Enhancing hydrogen positions in X-ray structures of transition metal hydride complexes with dynamic quantum crystallography

Hirshfeld atom refinement (HAR) is a method which enables the user to obtain more accurate positions of hydrogen atoms bonded to light chemical elements using X-ray data. When data quality permits, this method can be extended to hydrogen-bonded transition metals (TMs), as in hydride complexes. However, addressing hydrogen thermal motions with HAR, particularly in TM hydrides, presents a challenge. At the same time, proper description of thermal vibrations can be vital for determining hydrogen positions correctly. In this study, we employ tools such as SHADE3 and Normal Mode Refinement (NoMoRe) to estimate anisotropic displacement parameters (ADPs) for hydrogen atoms during HAR and IAM refinements performed for seven structures of TM (Fe, Ni, Cr, Nb, Rh and Os) and metalloid (Sb) hydride complexes for which both the neutron and the X-ray structures have been determined. A direct comparison between neutron and HAR/SHADE3/NoMoRe ADPs reveals that the similarity between neutron hydrogen ADPs and those estimated with NoMoRe or SHADE3 is significantly higher than when hydrogen ADPs are refined with HAR. Regarding TM—H bond lengths, traditional HAR exhibits a slight advantage over the other methods. However, combining NoMoRe/SHADE3 with HAR results in a minor decrease in agreement with neutron TM—H bond lengths. For the Cr complex, for which high-resolution X-ray data were collected, an investigation of resolution-related effects was possible.

1. Introduction

Transition metal (TM) bound hydrides are compounds which play a crucial role in important chemical reactions and have various potential applications. They serve as catalysts or intermediate compounds in energy conversion processes (Bullock et al., 2014; Rakowski Dubois & Dubois, 2009; Thoi et al., 2013), catalytic hydrogenation and reactions involving C—H bond activation (Hilt, 2014; Lyons & Sanford, 2010; Labinger & Bercaw, 2002; Choi et al., 2011). Additionally, many TM hydrides can be used as hydrogen storage materials (Schlapbach & Züttel, 2001; Fukuzumi & Suenobu, 2013; Langmi et al., 2014) and exhibit superconductivity or high-temperature superconductivity (Semenok et al., 2020; Du et al., 2021), e.g. Pd and Pd–Ni hydrides (Skoskiewicz, 1972), V hydrides (Li & Peng, 2017), Cr hydrides (Yu et al., 2015), Nb hydrides, Ta hydrides (Hubbard Horn & Ziegler, 1947), and Th hydrides (Satterthwaite & Toepke, 1970). This interesting class of compounds presents a challenge for X-ray crystallography and its most popular method, the Independent Atom Model (IAM) (Compton, 1915). The limitations arise from the simplified spherical electron density model, which cannot correctly describe aspherical electron density deformations due to the presence of lone electron pairs and bond formation, let alone other interactions between/within molecules in the crystals. Moreover, in TM hydrides, the weak X-ray diffraction signal from the hydrogen atom is screened by the strong signal from the electron-rich metal atom.

Hirshfeld atom refinement (HAR) (Jayatilaka & Dittrich, 2008; Capelli et al., 2014) is a method utilizing the Hirshfeld model of electron density (Hirshfeld, 1977) which accounts for the aspherical features of atomic electron density. HAR has evolved significantly in recent years, incorporating features like disorder refinement, solvent modelling to mimic the crystal environment (Kleemiss et al., 2021), various electron density partitioning methods (Chodkiewicz et al., 2020), fragmentation helpful in tackling large molecules and network compounds (Chodkiewicz et al., 2022), and finally periodic boundary conditions (Ruth et al., 2022). Compared with IAM, HAR shows remarkable improvement in accuracy and precision of positions of hydrogen atoms bonded to lighter chemical elements based on standard-resolution (d = 0.83 Å) good-quality X-ray data (data with hydrogen positions that can be freely refined with IAM). Although IAM underestimates the lengths of X—H bonds typical for crystals of organic compounds on average by 0.12 Å, compared with neutron bond lengths, mean X—H bond lengths obtained with HAR are underestimated by on average only 0.014 Å (Jha et al., 2020; Woińska et al., 2016). However, the ability of HAR to refine anisotropic displacement parameters (ADPs) of hydrogen atoms is subject to data quality (Malaspina et al., 2020; Woinska et al., 2019). HAR has been successfully used for processing X-ray data collected for TM complexes, including TM hydrides (Woińska et al., 2016, 2021, 2023; Kleemiss et al., 2021; Holsten et al., 2021). It allows modelling of electron density of the TM by means of very exact quantum mechanical calculations, with the possibility of including relativistic effects (Kleemiss et al., 2021; Holsten et al., 2021; Bučinský et al., 2016, 2019; Malaspina et al., 2019; Pawlędzio et al., 2021; Woińska et al., 2023).

Collecting high-quality X-ray data for crystals of TM hydride complexes is difficult due to high absorption and radiation damage. Neutron structures, crucial for validating hydrogen positions and thermal motions, are even scarcer. Nonetheless, in our previous work we refined ten X-ray datasets of TM hydride complexes deposited in the Cambridge Structural Database (CSD), each with the corresponding neutron structure. For five of the structures HAR outperformed IAM in terms of agreement of the TM—H bond lengths with the neutron values. We ranked the structures by quality of the X-ray and neutron data and quality of refinement, clearly showing the superiority of HAR for the higher-quality structures and the surprisingly good performance of IAM for the lowest-quality datasets. Our previous study also explored the impact of various DFT functionals, basis sets, relativistic effects and interactions with the surrounding molecules in the crystal. We tentatively considered the idea of estimating hydrogen ADPs using the SHADE2 server (Madsen, 2006) but successfully coupled it with HAR for only one structure. Using more advanced methods stemming from SHADE2, such as SHADE3 (Madsen & Hoser, 2014) and Normal Mode Refinement (NoMoRe) (Hoser & Madsen, 2016, 2017) was beyond the scope of our previous study due to computational demands. This work is a continuation of our previous study, focusing on SHADE3 and NoMoRe to estimate anisotropic thermal motions of hydrogen atoms and investigate their influence on positions of hydrogen atoms and compare ADPs obtained with various methods. Furthermore, we examine high-resolution X-ray data of a chromium complex (Macchi et al., 2005) with the neutron data collected at a similar temperature (Petersen et al., 1981). This allows us to investigate the impact of resolution on atomic thermal motions determined with HAR, IAM, SHADE3 and NoMoRe and the influence on the position of the hydrogen atom bonded to the TM atom. The latter issue has already been investigated by Kleemiss et al. (2021); however, there was no clear conclusion whether more information resulting from higher resolution was superior to better overall quality of low-resolution data.

The SHADE2 approach (Madsen, 2006) divides atomic thermal motion into the uncorrelated internal and external rigid body components. The external motion of hydrogen atoms is obtained from TLS (translation-libration-screw) analysis (Schomaker & Trueblood, 1968) of the non-hydrogen atom framework as a rigid body and the internal part comes from the library of internal mean square displacements (MSDs) derived from neutron data. ADPs estimated with SHADE2 are usually in good agreement with neutron-derived ADPs for hydrogen atoms involved in typical covalent bonds (Madsen & Hoser, 2014); however, inaccuracies can occur for atoms involved in medium and strong hydrogen bonds or hydrogen atoms bonded to TMs. SHADE3 (Madsen & Hoser, 2014) overcomes this problem by deriving the MSDs from normal-mode frequencies of the high-frequency vibrations obtained from periodic calculations at the Γ-point of the Brillouin zone or from spectroscopic experiments. NoMoRe (Hoser & Madsen, 2016, 2017) goes further, using all the normal-mode frequencies to estimate atomic thermal vibrations: the high-frequency ones are used to obtain the MSDs and the low-frequency ones, which are difficult to calculate accurately, are subject to NoMoRe. In this procedure, the scaling factors of the low-frequency normal modes are refined against diffraction data alternately with atomic coordinates in order to minimize wR₂. The TLS analysis assumes that 6Z (where Z is the number of asymmetric units in the unit cell) low-frequency normal modes correspond with the external vibrations; however, in practice, the number of refined low-frequency modes has to be adjusted.

NoMoRe has been successfully used to estimate hydrogen ADPs and thermodynamic properties for a number of crystal structures of simple organic compounds, such as urea (Hoser & Madsen, 2016); L-alanine, naphthalene and xylitol (Hoser & Madsen, 2017); yellow and white polymorphs of di­methyl 3,6-di­chloro-2,5-di­hydroxy­terephthalate (Kofoed et al., 2019); L-alanine (Sovago et al., 2020); urea, the α- and β-glycine polymorphs, benzoic acid, and 4′-hy­droxy­aceto­phenone (Hoser et al., 2021); and the pyrazinamide polymorphs (Hoser et al., 2022). SHADE3 has been applied to the crystal structures of 1-methyl­uracil, α -glycine, L-alanine, 2-methyl-4-nitro­aniline, xylitol and Proton Sponge (Madsen & Hoser, 2014). Both techniques have also been used to estimate hydrogen ADPs for HAR (Malaspina et al., 2020; Wanat et al., 2021). This work is an attempt to apply SHADE3 and NoMoRe to TM hydride complexes, aiming to improve hydrogen positions, especially for TM—H bonds, and compare the ADPs obtained with various methods to the neutron data. It also explores the computational feasibility of applying these methods to TM hydride complexes.

2. Results and discussion

2.1. Experimental data and previous results

In our previous research (Woińska et al., 2023), we performed HAR for ten metal–organic complexes featuring TM hydrogen bonds with both known X-ray structures and known neutron structures. The structures were ranked according to the quality of the neutron and X-ray datasets (based on resolution, completeness and R_int) and refinement (evaluated according to R, wR2, goodness of fit and residual density range) performed, leading to the final joint data- and refinement-quality X-ray (HAR)–neutron and X-ray (IAM)–neutron rankings. Structures were ordered from worst to best according to a given quantity and the score was equal to the position in the ranking. If a certain quantity used in the ranking procedure was unknown, the structure automatically obtained the lowest position in the ranking with respect to this quantity. The obtained scores were summed for each structure separately, leading to the data- and refinement-quality ranking, separate for the neutron and X-ray data. Next, the neutron and X-ray rankings were combined to form the final joint X-ray and neutron data and refinement quality ranking. For the top-ranked structures, HAR significantly improved agreement between the TM—H bond lengths and the neutron values compared with IAM. However, for half of the structures, particularly those lower in the ranking, HAR did not provide improvement and sometimes deteriorated the results in comparison with IAM. Consequently, one could ask whether further progression in the determination of positions of hydrogen atoms bonded to TMs is possible with HAR. Since refinement of hydrogen ADPs is often highlighted as a weakness of HAR, this study explores combining HAR with advanced models of hydrogen ADPs such as SHADE3 and NoMoRe. Six previously studied structures were chosen for this purpose. The selected structures are marked with the following REFCODEs: QOSZON (Ho et al., 2003) neutron, (Arion et al., 2001) X-ray; SITKUB (Lam et al., 2003), ZEYVAA (Bakhmutov et al., 2000) neutron, (Nikonov et al., 1995) X-ray; GOJNIF (Cammarota et al., 2019), TIWXOP (Schwamm et al., 2019), XAXMEP (Webster et al., 2005) neutron (Gross & Girolami, 2007) X-ray. Additionally, the high-resolution X-ray structure of the complex containing a Cr—H—Cr bridging bond, KCPTCR (Petersen et al., 1981) neutron, (Macchi et al., 2005) X-ray, was included to examine the role of data resolution. The ranking of structures from the previous study was supplemented with KCPTCR_std (refinement against dataset truncated to the resolution 0.59 Å⁻¹) and KCPTCR_max (refinement against the full dataset) structures. The order of structures in the joint X-ray and neutron data and refinement quality ranking, from best to worst, is as follows: (1) QOSZON, (2) KCPTCR_std, (3) GOJNIF, (4) SITKUB, (5) KCPTCR_max, (6) TIWXOP, (7) ZEYVAA, (8) XAXMEP. All the investigated structures are depicted in Fig. 1. One must bear in mind that this study is based on quite a small set of structures with varying quality of both neutron and X-ray datasets.

Figure 1 Schematic of the investigated structures with heavy metals bonded to hydrogen atoms marked.

2.2. Refinement types and theoretical calculations

The DiSCaMB library (Chodkiewicz et al., 2018) was used for HAR in various versions, all of which employed the same procedure of obtaining aspherical atomic scattering factors: the DFT method with B3LYP functional was used (Becke, 1988; Lee et al., 1988) and interactions within the crystal were included by surrounding the central molecule with a cluster of Hirshfeld partition-derived atomic charges and dipoles for all molecules with at least one atom within 8 Å from the central molecule. The basis set was chosen based on the TM atom to optimize TM—H bond lengths, as described in our previous study (Woińska et al., 2023) and detailed in Table 1. Convergence was reached when the maximum (parameter shift/sigma) was less than 0.001. Geometry optimization in the gas phase in previous work showed that the singlet state had the lowest energy for the compounds considered, so only this spin state was taken into account. In the case of KCPTCR, only geometry optimization for the singlet state was feasible. All refinements for this structure were performed against the full dataset (KCPTCR_max) and against the dataset truncated to a resolution of 0.59 Å⁻¹, which is equivalent to θ_max = 25° (KCPTCR_std) for Mo Kα radiation.

Table 1
Basis sets used in HAR and in normal-mode frequency calculations in CRYSTAL, temperatures of data collection and treatment of hydrogen thermal motions in the investigated structures

In the case of HAR, the basis sets in the table were used for all atoms in the structure (unless otherwise stated). In the case of CRYSTAL calculations the basis sets in the table were used for the heavy metal atoms only, and for the remaining atoms the 6-31G(d,p) basis set was used.

		Basis set		Temperature (K)		Hydrogen thermal motions
REFCODE	Metal	HAR	CRYSTAL	X-ray	Neutron	HAR	Neutron
KCPTCR	Cr	cc-pVDZ	TZP	28 (2)	20 (1)	Anisotropic	Anisotropic
	K	cc-pVDZ	TZP
QOSZON	Fe	cc-pVTZ	6-31G(d,p)	293 (2)	20 (2)	Anisotropic	Anisotropic
SITKUB	Rh	jorge-DZP	jorge-DZP	120.15	20 (2)	Anisotropic	Isotropic†
ZEYVAA	Nb	cc-pVTZ-DK	cc-pVTZ-DK	173 (2)	100	Isotropic	Anisotropic
XAXMEP	Os	jorge-DZP	jorge-DZP	199 (2)	20	Isotropic	Isotropic
TIWXOP	Sb	jorge-DZP	jorge-DZP	120.01 (10)	120	Isotropic	Anisotropic
GOJNIF	Ni	cc-pVTZ-DK	6-31G(d,p)	100 (2)	100 (2)	Anisotropic	Anisotropic
	In	cc-pVTZ-DK3	cc-pVTZ-DK3

Basis set used only for the In atom in HAR.
†Only the hydrogen atom bonded to Rh was refined anisotropically.

Various types of HAR were conducted with hydrogen ADPs fixed at the SHADE3/NoMoRe values. The refinements denoted HAR_SHADE3/HAR_NoMoRe involved using SHADE3/NoMoRe before each HAR cycle and refining until max(parameter shift/sigma) was below 1.0. The HAR_SHADE3 refinement for ZEYVAA was considered not converged since max(parameter shift/sigma) was oscillating and its values were much higher than 1.0. In refinements denoted HAR_SHADE3_1/HAR_NoMoRe_1, hydrogen ADPs were determined using SHADE3/NoMoRe only before the first HAR cycle and refinements continued until the maximum (parameter shift/sigma) was below 0.001. Additionally, IAM refinements using SHADE3 and NoMoRe were performed. Lastly, IAM and HAR with all hydrogen ADPs set to 0 (denoted IAM_0_HADPs and HAR_0_HADPs) were carried out. Although this is an unphysical model of thermal vibrations, it served as a boundary evaluation for the influence of the values of hydrogen ADPs on TM—H and X—H bond lengths and refinement statistics. Statistics describing all the refinements are provided in the supporting information (Figs. S1–S9 and Tables S2–S8) along with the computational details for SHADE3 and NoMoRe procedures.

2.3. Atomic thermal motions: similarity index

The similarity index S₁₂ (Whitten & Spackman, 2006) was used as a measure of similarity between thermal ellipsoids of a given atom obtained with different diffraction methods or models. S₁₂ quantifies the non-overlapping part of probability densities of a given atom (differing due to different thermal motions) and is given by

where R₁₂ is the overlap integral between the compared probability densities, calculated using only the values of the ADPs. S₁₂ = 0 indicates perfect agreement, whereas 100 denotes the highest possible difference. Notably, S₁₂ is more suitable for confirming high similarity between thermal motions, as even small differences at a level of 1 can result in noticeable visual differences in thermal ellipsoids. Moreover, depending on the estimated standard deviations (e.s.d.s) of ADPs, the e.s.d.s of S₁₂ can be very high, making S₁₂ an untrustworthy measure. Therefore, we use the mean S₁₂ calculated for all hydrogen or non-hydrogen atoms in the molecule, along with their estimated errors calculated using error propagation. The estimated error of the mean S₁₂ is lower meaning S₁₂ is a more reliable measure of thermal motion similarity. In the supporting information, the values of S₁₂ with e.s.d.s for individual atoms in all the structures are available (Figs. S10–S27), as well as the values of a mean S₁₂ with the corresponding e.s.d.s of the mean (Figs. S28–S45).

HAR with anisotropically refined hydrogen thermal motions was attainable for four of the crystal structures. However, a few hydrogen atoms in these structures had to be refined isotropically (Tables S2–S8). For TIWXOP, XAXMEP and ZEYVAA, only isotropic refinement was possible. The results of HAR for these structures have been published in a previous study (Woińska et al., 2023), with the exception of KCPTCR, which has not yet been treated with HAR, and GOJNIF, for which only isotropic HAR results were published. In the case of TIWXOP, the neutron dataset presented challenges, with large and distorted ellipsoids of anisotropically refined hydrogen atoms. One of the methyl groups in TIWXOP was significantly disordered, and only the hydrogen atoms of the largest component could be identified in the difference density map and refined isotropically, with the remaining nuclear density modelled as a ring of hydrogen nuclear density. The temperatures at which the neutron and the X-ray data for KCPTCR have been collected differ by only 8 K; therefore, we decided to compare the neutron thermal ellipsoids and those obtained from refinements against the X-ray data. Fig. 2 shows the structures of QOSZON and SITKUB obtained with HAR (anisotropic): HAR_NoMoRe and HAR_SHADE3. Fig. 3 displays the structures of XAXMEP and ZEYVAA obtained with HAR (isotropic): HAR_NoMoRe and HAR_SHADE3. Fig. 4 includes the X-ray-derived structures of TIWXOP, GOJNIF and KCPTCR along with the neutron structures.

Figure 2 Crystal structures of (a) QOSZON and (b) SITKUB obtained with HAR, HAR_NoMoRe and HAR_SHADE3. Thermal ellipsoids are depicted at the 50% probability level.

Figure 3 Crystal structures of (a) XAXMEP and (b) ZEYVAA obtained with HAR, HAR_NoMoRe and HAR_SHADE3 (HAR_SHADE3_1 for ZEYVAA). Thermal ellipsoids are depicted at the 50% probability level.

Figure 4 Crystal structures of (a) TIWXOP, (b) GOJNIF and (c) KCPTCR (high resolution) obtained based on the neutron and X-ray experiments (HAR, HAR_NoMoRe and HAR_SHADE3). Thermal ellipsoids are depicted at the 50% probability level.

2.3.1. Hydrogen ADPs from HAR_SHADE3(_1) versus HAR_NoMoRe(_1)

Average S₁₂ values are close to 0 when comparing hydrogen ADPs obtained from HAR_SHADE3 and HAR_SHADE3_1, as well as HAR_NoMoRe and HAR_ NoMoRe_1. This means that iterative application of SHADE3 or NoMoRe during HAR does not influence the estimated values of hydrogen ADPs. We will now focus on the results of HAR_SHADE3 and HAR_NoMoRe, with the HAR_SHADE3_1 and HAR_NoMoRe_1 results available in the supporting information (Figs. S10–S71). The averaged S₁₂ values, calculated between hydrogen ADPs obtained with HAR_SHADE3 and HAR_NoMoRe, are between 1 and 5 (see Table 2) and reflect the differences in hydrogen ADPs resulting from variations in internal vibrations estimated with NoMoRe using experimental data, and those obtained with SHADE3 are based on theoretical calculations. The variability of averaged S₁₂ for hydrogen atoms among the structures considered appears independent of the experimental temperature, position of the dataset in the ranking or the number of refined normal modes during NoMoRe. However, it noticeably decreases with the increasing number of hydrogen atoms in the structure.

Table 2
Averaged S₁₂ comparing hydrogen ADPs obtained with HAR_SHADE3 and HAR_NoMoRe

The structures are ordered according to their position in the X-ray (HAR) neutron data-refinement-quality ranking from best to worst.

	Averaged S12	X-ray Temperature (K)	Normal modes refined in NoMoRe
QOSZON	2.21	293 (2)	40
KCPTCR_std	1.25	28 (2)	20
GOJNIF	1.54	100 (2)	20
SITKUB	2.48	120.15	50
KCPTCR_max	1.28	28 (2)	20
TIWXOP	4.12	120.01 (10)	20
ZEYVAA	3.19†	173 (2)	20
XAXMEP	1.47	199 (2)	70

†Results for HAR_SHADE3_1 and HAR_NoMoRe _1 (HAR_SHADE3 and HAR_NoMoRe did not converge).

2.3.2. Hydrogen ADPs from HAR versus HAR_SHADE3 and HAR_NoMoRe

The average S₁₂ values between hydrogen ADPs obtained from HAR and HAR_NoMoRe are consistently lower than those from HAR and HAR_SHADE3. This is the consequence of the refinement of normal modes against experimental data (see Table 3). Only for QOSZON is the average S₁₂ value between hydrogen ADPs refined with HAR and those estimated with HAR_NoMoRe similar to the discrepancy between hydrogen ADPs from HAR_NoMoRe and HAR_SHADE3 (S₁₂ = 2.67). The differences between hydrogen ADPs in QOSZON from HAR and HAR_SHADE3 are slightly higher, with S₁₂ close to 5. For KCPTCR, SITKUB and GOJNIF, the S₁₂ values between hydrogen ADPs obtained from HAR and HAR_NoMoRe/HAR_SHADE3 are already relatively high, ranging from 6.50 to 8.51 and 8.69 to 9.87, respectively. It is also noticeable that among the presented structures, S₁₂ increases when the refinement of hydrogen ADPs with HAR becomes more problematic, i.e. the number of hydrogen atoms that have to be refined isotropically grows and also the shapes of refined hydrogen ellipsoids become more irregular. Refinement against high- and low-resolution data performed for KCPTCR reveals different behaviour of hydrogen ADPs from NoMoRe and SHADE3 – S₁₂ slightly increases with decreasing resolution for NoMoRe and slightly decreases for SHADE3.

Table 3
Averaged S₁₂ comparing hydrogen ADPs obtained with HAR and HAR_NoMoRe /HAR_SHADE3

Averaged S₁₂ is given with its estimated error.

	HAR_NoMoRe	HAR_ SHADE3
KCPTCR_max	6.00 ± 1.57	6.72 ± 1.61
KCPTCR_std	6.19 ± 1.46	6.66 ± 1.48
QOSZON	2.67 ± 0.77	4.75 ± 0.74
SITKUB	6.50 ± 2.16	8.51 ± 2.10
GOJNIF	8.69 ± 4.15	9.87 ± 4.08

2.3.3. Hydrogen and non-hydrogen ADPs from neutron versus HAR, HAR_SHADE3, HAR_NoMoRe and IAM

Based on the neutron data quality of KCPTCR, TIWXOP and GOJNIF, collected at the same or a similar temperature to the X-ray data, it was expected that TIWXOP would show the least favourable comparison (see Table 4). Indeed, the average S₁₂ for hydrogen atoms between neutron and HAR_NoMoRe is quite high, almost 9, and exceeds 11 between neutron and HAR_SHADE3. In the case of GOJNIF, for which the neutron structure is of much better quality, the average S₁₂ between neutron and HAR_NoMoRe/HAR_SHADE3 is similar to the level of discrepancy between hydrogen ADPs from HAR_NoMoRe and HAR_SHADE3. Averaged S₁₂ between the neutron and HAR hydrogen ADPs is high, almost 11. For KCPTCR, the results are better, with S₁₂ between neutron and HAR hydrogen ADPs being similar to S₁₂ between HAR and HAR_NoMoRe/HAR_SHADE3 hydrogen ADPs. These values indicate that for KCPTCR, NoMoRe in particular yields hydrogen thermal motions that are in quite good agreement with the neutron thermal motions, and their similarity is even higher on average than the similarity between NoMoRe and SHADE3. It can also be observed that S₁₂ between neutron and HAR or SHADE3 hydrogen ellipsoids slightly decreases with lower data resolution, whereas in the case of NoMoRe, there is either a small increase or no significant difference. This outcome is expected, as the scattering factor of hydrogen atoms is very low at high resolution and high-resolution data do not add much information about hydrogen atoms.

Table 4
Averaged S₁₂ comparing hydrogen ADPs obtained with neutron and HAR/HAR_NoMoRe/HAR_SHADE3

Averaged S₁₂ is given its estimated error.

	HAR	HAR_NoMoRe	HAR_ SHADE3
KCPTCR_max	6.30 ± 1.72	0.98 ± 0.08	1.43 ± 0.07
KCPTCR_std	5.74 ± 1.54	1.05 ± 0.08	1.36 ± 0.07
TIWXOP	–	8.93 ± 1.12	11.47 ± 0.95
GOJNIF	10.89 ± 4.26	2.80 ± 1.62	3.55 ± 1.63

For non-hydrogen atoms, the S₁₂ values between neutron ADPs and X-ray ADPs obtained with all investigated refinement techniques do not vary significantly across different structures (see Table 5). In the case of GOJNIF, the averaged S₁₂ reaches values up to 4. For GOJNIF, averaged S₁₂ is slightly lower for all the versions of IAM than in the case of HAR, and there is generally not much variability observed in averaged S₁₂ between different IAM or HAR versions [Fig. 4(b)]. In the case of TIWXOP, HAR (averaged S₁₂ between 4.24 and 4.3) results in non-hydrogen ADPs more similar to the neutron ones than IAM (averaged S₁₂ between 4.87 and 5.39) [Fig. 4(a)]. Regarding KCPTCR, using only low-resolution data significantly increases the S₁₂ values between neutron and IAM ADPs of non-hydrogen atoms (from around 1.33–1.36 to 2.87–3.04), whereas the increase for HAR is very small [Fig. 4(c)]. Note that IAM requires high-resolution data to achieve the same level of agreement of non-hydrogen thermal motions with the neutron results as HAR can provide with standard-resolution data. Further comparison of the ADPs for KCPTCR based on refinement against the full high-resolution dataset to those in the structure resulting from X-ray data cut to the resolution limit equivalent to 2θ = 50° can be found in the supporting information.

Table 5
Averaged S₁₂ comparing non-hydrogen ADPs obtained with neutron and HAR/HAR_NoMoRe/HAR_SHADE3

Averaged S₁₂ is given with its estimated error.

	IAM	IAM_NoMoRe	IAM_SHADE3	IAM_0_HADPs	HAR	HAR_NoMoRe	HAR_SHADE3	HAR_0_HADPs
KCPTCR_max	1.33 ± 0.52	1.36 ± 0.52	1.36 ± 0.52	1.36 ± 0.52	1.21 ± 0.52	1.22 ± 0.52	1.22 ± 0.52	1.23 ± 0.52
KCPTCR_std	2.96 ± 0.54	2.87 ± 0.54	2.88 ± 0.54	3.04 ± 0.55	1.32 ± 0.53	1.37 ± 0.52	1.37 ± 0.52	1.34 ± 0.53
TIWXOP	4.97 ± 0.59	4.87 ± 0.58	5.39 ± 0.59	5.20 ± 0.60	4.51 ± 0.56	4.24 ± 0.58	4.48 ± 0.55	4.83 ± 0.58
GOJNIF	3.84 ± 1.76	3.84 ± 1.76	3.88 ± 1.76	3.88 ± 1.77	3.98 ± 1.76	3.94 ± 1.77	3.99 ± 1.77	4.01 ± 1.78

2.4. The effect of data resolution on dynamic structure factors

Plotting the difference between the dynamic structure factor amplitudes [ΔF_calc = F_calc(model1) − F_calc(model2)] for the models allowed us to observe in which resolution ranges there are the highest differences between the models and how data truncation affects these differences. ΔF_calc between HAR and IAM for the full dataset [Fig. 5(a)] indicates the highest differences in low-resolution reflections (with a maximum between 0.2 and 0.3 Å⁻¹) and a sharp decrease at sin(θ)/λ = 0.6 Å⁻¹, which corresponds to the applied resolution cutoff. Applying the cutoff [Fig. 5(b)] has minimal effect on the low-resolution region, mainly reducing the concentration of diverging reflections, making HAR and IAM models slightly more similar. In both cases [Fig. 5(a) and 5(b)], ΔF_calc is quite symmetric relative to the x axis. Regarding how data trimming influences HAR and IAM individually [Figs. 5(c) and 5(d)], differences are less pronounced than between HAR and IAM, and the spread of ΔF_calc increases with higher resolution. HAR results in lower ΔF_calc compared with IAM. For both HAR and IAM, the KCPTCR_max structure tends to have slightly higher dynamic amplitudes of reflections than KCPTCR_std. The effect of thermal motions on dynamic structure factor amplitudes is very subtle; therefore, similar trends are observed for different techniques of estimating hydrogen thermal motion (Figs. S54–S59). Analogous effects for the remaining structures are presented in Figs. S60–S71.

Figure 5 The differences between the dynamic structure factors calculated in a given refinement versus resolution.

2.5. TM—H and X—H bond lengths obtained with various methods

The mean difference (MD) and mean absolute difference (MAD) between the neutron bond lengths and the X-ray bond lengths were calculated for the X—H and TM—H bonds (Fig. 6). Combined standard deviation (c.s.d.) averaged over the bond lengths was used as a measure for uncertainty of MD and MAD and was calculated according to the formula

where σ_X and σ_N are the estimated standard deviations of the X-ray and the neutron bond lengths, respectively. Aside from the plots, MD, MAD, MD/c.s.d. and MAD/c.s.d. values averaged for the X—H and TM—H bonds in all the structures are given in Tables 6 and 7. The two-tailed Welch's t-test (Welch, 1947) was employed to assess the statistical significance of these differences.

Table 6
MD, MAD, MD/c.s.d. and MAD/c.s.d. values calculated between the neutron and the X-ray/optimized bond lengths averaged for X—H bonds in all the structures

Bold: statistically significant. Italics: not significant.

Method	MD (Å)	MAD (Å)	MD/c.s.d.	MAD/c.s.d.	Mean c.s.d. (Å)
IAM	−0.121	0.122	−5.12	5.15	0.046
IAM_NoMoRe	−0.119	0.120	−3.98	4.00	0.039
IAM_SHADE3	−0.127	0.127	−4.93	4.95	0.031
IAM_0_HADPs	−0.134	0.135	−5.51	5.54	0.030
HAR	0.004	0.027	0.08	0.85	0.034
HAR_NoMoRe	0.005	0.032	0.03	0.89	0.038
HAR_NoMoRe_1	0.005	0.028	0.04	0.83	0.037
HAR_SHADE3	0.001	0.031	−0.01	0.92	0.035
HAR_SHADE3_1	0.000	0.035	−0.02	0.97	0.036
HAR_0_HADPs	0.003	0.042	0.00	1.47	0.030
Optimized	−0.001	0.014	−0.19	1.01	0.016

Table 7
MD, MAD, MD/c.s.d. and MAD/c.s.d. values calculated between the neutron and the X-ray/optimized bond lengths averaged for the TM—H bonds in all the structures

Since there are only 15 TM—H bond lengths in total, no statistical tests were performed on the averaged values.

Method	MD (Å)	MAD (Å)	MD/c.s.d.	MAD/c.s.d.	Mean c.s.d. (Å)
IAM	−0.028	0.046	−1.24	1.97	0.037
IAM_NoMoRe	−0.028	0.039	−1.25	1.65	0.039
IAM_SHADE3	−0.030	0.039	−1.44	1.76	0.034
IAM_0_HADPs	−0.023	0.038	−1.31	1.71	0.028
HAR	0.031	0.036	0.62	0.97	0.033
HAR_NoMoRe	0.025	0.043	0.29	1.31	0.038
HAR_NoMoRe_1	0.026	0.042	0.37	1.29	0.038
HAR_SHADE3	0.026	0.042	0.32	1.32	0.036
HAR_SHADE3_1	0.030	0.045	0.38	1.26	0.038
HAR_0_HADPs	0.032	0.052	0.55	1.64	0.031
Optimized	−0.005	0.017	−0.04	1.56	0.012

Figure 6 MAD between the X-ray/geometry-optimized and neutron values of the X—H and TM—H bond lengths with the c.s.d. averaged for the X—H/TM—H bonds in each structure as error bars. The X-ray values were obtained with various refinement methods. The structures are ordered according to their position in the X-ray (HAR)–neutron data- and refinement-quality ranking from best to worst.

The results indicate that tweaking HAR using more sophisticated methods for describing hydrogen thermal vibrations has minimal impact on the X—H and TM—H bond lengths in the investigated cases. As shown in Fig. 6, MAD between the HAR and the neutron bond lengths is fairly consistent across different hydrogen ADP estimation methods. Even setting hydrogen ADPs to 0 (IAM_0_HADPs/HAR_0_HADPs) does not significantly alter the X—H or TM—H bond lengths compared with conventional IAM/HAR, although some variability exists depending on the structure. MAD plots in Fig. 6 show that in the case of X—H bond lengths, the IAM values of MAD are consistently higher than 0.1 Å, with little variability related to different methods of estimating hydrogen ADPs. HAR generally yields lower MAD values for X—H bond lengths compared with IAM. Moreover, MAD obtained with HAR is the lowest for the structures from the top of the ranking and tends to increase with decreasing quality. For KCPTCR, pruning reflections has a minor effect on MAD for both HAR and IAM refinements.

For the TM—H bond lengths obtained with various HAR versions, it can also be observed that MAD tends to increase with lower position in the ranking and for some structures MAD is slightly higher than for the X—H bond lengths. Surprisingly, IAM yields lower MAD values for TM—H bond lengths compared with X—H bond lengths and, on average, MAD values are only slightly higher than those for HAR. For KCPTCR_std and KCPTCR_max, MAD is relatively consistent across various IAM and HAR types, although conventional HAR provides the best agreement of Cr—H bond lengths with the neutron structure.

The findings summarized in Tables 6 and 7 confirm the observations in the previous paragraph. All types of IAM, irrespective of the method of hydrogen thermal motion treatment, underestimate the X—H bond lengths in the investigated structures by on average 0.012–0.013 Å. In the case where all the variants of HAR and the geometry-optimized structure, MD is very close to 0. However, for HAR and HAR_NoMoRe(_1), MD is slightly different from 0 but still statistically significant. MAD values in these cases are significantly different from 0 but much lower compared with IAM. Geometry optimization results in the lowest MAD (0.014 Å). MAD is twice as high for HAR (0.027 Å) and HAR_NoMoRe_1 (0.028 Å). MAD increases slightly for HAR_NoMoRe (0.032 Å) and HAR_SHADE3(_1) (0.031 Å (0.035 Å), and finally for HAR_0_HADPs (0.042 Å) it is still much lower than in the case of IAM. The differences in MAD for X—H bond lengths for various types of IAM are quite small and the highest MAD is attained for IAM_0_HADPs.

Unfortunately, for TM—H bond lengths, statistical testing is impossible due to the small sample size of only 15 bonds. In this case, geometry optimization, which closely aligns with neutron values, slightly underestimates the bond lengths (MD = −0.005 Å and MAD = 0.017 Å). IAM tends to underestimate the TM—H bond lengths (MD ranging from −0.023 to −0.030 Å), resulting in MAD values of 0.038–0.046 Å, similar to what HAR achieves for X—H bond lengths. HAR, conversely, generally overestimates TM—H bond lengths (MD equal to 0.025–0.032 Å). The divergence of HAR values from neutron values, as estimated by MAD, has a similar range to IAM. However, in HAR the lowest MAD is obtained with standard HAR (0.036 Å) and the highest with HAR_0_HADPs (0.052 Å). In the case of IAM, IAM_0_HADPs results in the lowest MAD (0.038 Å) and standard IAM yields the highest MAD (0.046 Å). In summary, for the studied compounds, HAR performs slightly worse for TM—H bond lengths compared with the general case. The IAM performance for TM—H bond lengths is slightly worse than that of HAR and it appears to improve after using SHADE3 or NoMoRe, unlike the HAR performance for TM—H bond lengths. These conclusions are based on quite a small set of structures and the good agreement between the neutron and IAM TM—H bond lengths could be a coincidence. The role of high data quality, crucial for determining hydrogen positions with HAR in typical X—H bonds, seems to be even more critical for TM—H bond lengths, whereas this might not be an issue for IAM, perhaps accidentally.

3. Conclusions

This study aimed to combine HAR with sophisticated methods of estimating anisotropic thermal motions of hydrogen atoms – NoMoRe and SHADE3 – for seven X-ray datasets of TM/metalloid hydrides, with neutron structures serving as benchmarks. The primary objective was to investigate whether a more accurate estimation of hydrogen ADPs could enhance the positions of hydrogen atoms obtained from HAR, especially near heavy metals. The second goal was to assess the discrepancies between the thermal ellipsoids of hydrogen atoms obtained with various methods. Anisotropic HAR was feasible for only four structures. Neutron data were collected at the same temperature as the X-ray data for just two structures, one of which allowed anisotropic HAR. For one structure, a high-resolution X-ray dataset was collected and the neutron experiment was performed at a similar temperature, which enabled an examination of how data resolution affected atomic positions and thermal parameters.

The first observation regarding hydrogen ADPs is that, compared with SHADE3, NoMoRe yields hydrogen thermal ellipsoids in better agreement with those refined by HAR and this agreement correlates with the data-refinement quality ranking of the structure. Similarly, when comparing neutron hydrogen ADPs to those estimated by NoMoRe or SHADE3, the former results in smaller discrepancies with neutron ellipsoids and the corresponding S₁₂ values are strongly dependent on the specific structure. In comparisons between the neutron and the HAR hydrogen ADPs made for the only two structures for which it was feasible (GOJNIF and KCPTCR), a high discrepancy was also observed. For KCPTCR (standard resolution) averaged S₁₂ was slightly lower than for KCPTCR (high resolution) and significantly lower than for GOJNIF. Nonetheless, considering the high estimated error values of averaged S₁₂, these differences fall within the margin of error. As expected, NoMoRe yields hydrogen ADPs with the best agreement with neutron hydrogen ADPs, SHADE3 lags slightly behind, and HAR results in the most divergent hydrogen ADPs. Non-hydrogen ADPs are almost unaffected by hydrogen ADPs, even when those values are obviously erroneous (e.g. fixed at 0). Hydrogen ADPs obtained from HAR with high-resolution X-ray data are slightly more divergent from neutron hydrogen ADPs than in the case of standard-resolution X-ray data. It can be concluded that the information used by HAR to model hydrogen ADPs is mostly low-resolution data, with high-resolution data primarily introducing noise. The effect of data resolution on non-hydrogen atom ADPs differs for HAR and IAM. In HAR, using the high-resolution part of the data makes non-hydrogen ADPs only slightly more similar to neutron ones, whereas in IAM, it makes non-hydrogen ADPs much more similar to neutron ones. It appears that high-resolution X-ray data are needed to improve the description of thermal motion of non-hydrogen atoms with IAM, while standard resolution suffices for HAR.

The second issue addressed in this study was the impact of different methods of describing hydrogen thermal vibrations of X—H and, in particular, TM—H bond lengths. While there was some variability in X—H/TM—H bond lengths due to different hydrogen thermal motion estimation methods for individual structures, on average, the method of obtaining ADPs did not significantly influence hydrogen atom positions, even when the ADPs were set to 0 in IAM or HAR. In the case of IAM, the resulting average X—H bond lengths were very similar for all seven structures and they were underestimated by on average 0.121–0.134 Å. For HAR, discrepancies with mean neutron X—H bond lengths tended to increase with deteriorating position of the structure in the joint data-refinement quality X-ray–neutron ranking. HAR performed much better than IAM for X—H bond lengths, with discrepancies from neutron bond lengths varying depending on the hydrogen thermal motion treatment method, ranging from the lowest MAD in conventional HAR (0.027 Å) to slightly higher MAD in HAR_0_HADPs (0.042 Å). Surprisingly, IAM performed better for TM—H bond lengths, with average discrepancies from neutron bond lengths ranging from 0.038 Å (IAM_0_HADPs) to 0.046 Å (IAM). The IAM performance in terms of TM—H bond lengths was notably better for the structures with the worst position in the data and refinement quality ranking. In comparison, HAR yielded similar levels of discrepancy with neutron TM—H bonds as IAM, with MAD ranging from 0.036 Å (HAR) to 0.052 Å (HAR_0_HADPs). Note that geometry optimization resulted in high agreement with neutron positions, both for all X—H bond lengths (MAD = 0.014 Å) and for specifically TM—H bond lengths (MAD = 0.017 Å).

In conclusion, applying more precise and much more costly methods to describe hydrogen thermal motions did not improve hydrogen position determination in HAR. On the contrary, conventional HAR used to refine both hydrogen positions and thermal motions slightly outperformed HAR during which hydrogen thermal motions were fixed at the values estimated by sophisticated techniques such as NoMoRe and SHADE3. Nevertheless, this scientific problem certainly deserves more in-depth investigation.

Supporting information

Computing details

(GOJNIF_HAR_0_HADPs)

Crystal data

C39H62InN4NiP3	Dx = 1.415 Mg m^−3
Mr = 853.39	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, P212121	Cell parameters from 9537 reflections
a = 12.2127 (4) Å	θ = 2.3–36.4°
b = 14.5402 (5) Å	µ = 1.20 mm^−1
c = 22.5601 (8) Å	T = 100 K
V = 4006.1 (2) Å^3	Block, gold
Z = 4	0.14 × 0.08 × 0.06 mm
F(000) = 105.781

Data collection

Bruker Photon-II CMOS diffractometer	18741 reflections with I ≥ 2u(I)
φ and ω scans	Rint = 0.036
Absorption correction: multi-scan SADABS. R.Blessing, 1995	θmax = 36.4°, θmin = 2.3°
Tmin = 0.701, Tmax = 0.747	h = −20→20
237431 measured reflections	k = −24→24
19473 independent reflections	l = −37→37

Refinement

Refinement on F^2	0 constraints
Least-squares matrix: full	Only H-atom coordinates refined
R[F^2 > 2σ(F^2)] = 0.021	w = 1/[σ^2(Fo^2) + (0.1P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.078	(Δ/σ)max = 0.001
S = 0.69	Δρmax = 0.32 e Å^−3
19473 reflections	Δρmin = −0.99 e Å^−3
619 parameters	Absolute structure: Flack, H. D. (1983). Acta Cryst. A39, 876-881.
0 restraints	Absolute structure parameter: 0.004 (5)

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ni1	0.755794 (12)	0.598667 (10)	0.856158 (7)	0.00973 (3)
H1A	0.7244 (17)	0.5612 (15)	0.9258 (9)	0.000000
H1B	0.7516 (17)	0.6221 (15)	0.9292 (9)	0.000000
In1	0.798245 (6)	0.580828 (5)	0.749329 (3)	0.00865 (2)
P1	0.91843 (2)	0.52226 (2)	0.864349 (13)	0.00966 (5)
P2	0.59903 (2)	0.52856 (2)	0.829183 (13)	0.00973 (5)
P3	0.75364 (3)	0.75010 (2)	0.835663 (12)	0.00939 (4)
N1	0.96175 (7)	0.53390 (7)	0.74724 (5)	0.01104 (14)
N2	0.67674 (9)	0.48674 (7)	0.72031 (4)	0.01165 (16)
N3	0.78418 (9)	0.71637 (7)	0.71622 (4)	0.01086 (15)
N4	0.83414 (8)	0.56330 (7)	0.64680 (4)	0.00916 (14)
C1	0.95349 (9)	0.57155 (7)	0.64338 (5)	0.00953 (15)
C2	1.00508 (10)	0.59713 (9)	0.59111 (5)	0.01339 (18)
H2A	0.9635 (13)	0.6143 (11)	0.5554 (7)	0.000000
C3	1.11903 (11)	0.60875 (9)	0.58826 (6)	0.0150 (2)
H3A	1.1648 (15)	0.6210 (13)	0.5471 (7)	0.000000
C4	1.18058 (10)	0.59547 (9)	0.63983 (6)	0.01458 (19)
H4A	1.2641 (13)	0.6076 (11)	0.6377 (7)	0.000000
C5	1.12988 (10)	0.57046 (9)	0.69278 (5)	0.01301 (18)
H5A	1.1850 (16)	0.5651 (13)	0.7349 (8)	0.000000
C6	1.01529 (10)	0.55737 (8)	0.69636 (5)	0.01010 (17)
C7	1.01955 (10)	0.53667 (9)	0.80305 (5)	0.01191 (18)
H7A	1.0641 (13)	0.5966 (11)	0.8137 (7)	0.000000
H7B	1.0918 (15)	0.4849 (12)	0.8011 (7)	0.000000
C8	0.99537 (11)	0.56222 (9)	0.93123 (5)	0.01450 (19)
H8A	0.9835 (15)	0.6403 (13)	0.9306 (8)	0.000000
C9	0.91100 (10)	0.39466 (8)	0.87154 (6)	0.01448 (19)
H9A	0.8490 (14)	0.3821 (13)	0.9077 (7)	0.000000
C10	1.12048 (12)	0.55060 (12)	0.93058 (7)	0.0227 (3)
H10A	1.1499 (16)	0.4685 (14)	0.9324 (8)	0.000000
H10B	1.1541 (13)	0.5837 (11)	0.8967 (7)	0.000000
H10C	1.1561 (16)	0.5756 (14)	0.9845 (9)	0.000000
C11	0.94557 (16)	0.52140 (13)	0.98765 (6)	0.0265 (3)
H11A	1.0043 (14)	0.5499 (13)	1.0236 (8)	0.000000
H11B	0.8601 (13)	0.5341 (12)	0.9944 (7)	0.000000
H11C	0.9654 (15)	0.4443 (12)	0.9891 (7)	0.000000
C12	0.86437 (13)	0.35251 (9)	0.81442 (6)	0.0191 (2)
H12A	0.8582 (14)	0.2802 (12)	0.8228 (7)	0.000000
H12B	0.7822 (14)	0.3920 (13)	0.8025 (8)	0.000000
H12C	0.9247 (14)	0.3579 (12)	0.7807 (7)	0.000000
C13	1.01669 (13)	0.34492 (11)	0.88741 (8)	0.0242 (3)
H13A	1.0162 (14)	0.2730 (12)	0.8987 (7)	0.000000
H13B	1.0889 (14)	0.3649 (12)	0.8618 (7)	0.000000
H13C	1.0588 (15)	0.3643 (12)	0.9270 (7)	0.000000
C14	0.78942 (9)	0.47291 (7)	0.63335 (5)	0.01020 (16)
C15	0.82593 (10)	0.42283 (9)	0.58486 (5)	0.01245 (17)
H15A	0.8935 (15)	0.4560 (13)	0.5554 (8)	0.000000
C16	0.78534 (11)	0.33508 (9)	0.57252 (6)	0.0157 (2)
H16A	0.8118 (14)	0.2971 (12)	0.5337 (7)	0.000000
C17	0.70742 (11)	0.29751 (9)	0.61056 (6)	0.0162 (2)
H17A	0.6707 (15)	0.2273 (13)	0.5969 (8)	0.000000
C18	0.67030 (11)	0.34629 (9)	0.65972 (6)	0.01473 (19)
H18A	0.6169 (14)	0.3114 (12)	0.6898 (7)	0.000000
C19	0.70933 (9)	0.43559 (8)	0.67272 (5)	0.01066 (16)
C20	0.60332 (10)	0.44844 (8)	0.76429 (5)	0.01226 (17)
H20A	0.6198 (15)	0.3760 (12)	0.7836 (8)	0.000000
H20B	0.5220 (13)	0.4408 (12)	0.7434 (7)	0.000000
C21	0.53642 (10)	0.45616 (9)	0.88806 (5)	0.01363 (19)
H21A	0.4654 (14)	0.4161 (13)	0.8693 (7)	0.000000
C22	0.48067 (9)	0.60412 (9)	0.80772 (5)	0.01273 (18)
H22A	0.4859 (14)	0.6595 (12)	0.8402 (7)	0.000000
C23	0.61419 (12)	0.38126 (11)	0.91006 (6)	0.0204 (2)
H23A	0.5666 (15)	0.3404 (12)	0.9426 (7)	0.000000
H23B	0.6422 (14)	0.3323 (12)	0.8780 (7)	0.000000
H23C	0.6926 (16)	0.4200 (13)	0.9360 (8)	0.000000
C24	0.49899 (12)	0.51677 (10)	0.93996 (6)	0.0187 (2)
H24A	0.4354 (16)	0.5793 (14)	0.9243 (8)	0.000000
H24B	0.4538 (14)	0.4749 (12)	0.9719 (7)	0.000000
H24C	0.5624 (14)	0.5525 (12)	0.9646 (7)	0.000000
C25	0.49936 (11)	0.64734 (10)	0.74673 (7)	0.01745 (19)
H25A	0.4321 (14)	0.6971 (12)	0.7366 (7)	0.000000
H25B	0.5753 (13)	0.6754 (11)	0.7367 (7)	0.000000
H25C	0.4997 (14)	0.5910 (12)	0.7135 (7)	0.000000
C26	0.36782 (11)	0.55810 (11)	0.80854 (6)	0.0176 (2)
H26A	0.3036 (14)	0.6088 (12)	0.7971 (7)	0.000000
H26B	0.3681 (14)	0.5024 (11)	0.7801 (7)	0.000000
H26C	0.3400 (15)	0.5180 (13)	0.8480 (7)	0.000000
C27	0.77569 (10)	0.64133 (8)	0.62084 (5)	0.01049 (17)
C28	0.74244 (12)	0.64009 (8)	0.56206 (5)	0.01472 (19)
H28A	0.7512 (16)	0.5693 (13)	0.5388 (8)	0.000000
C29	0.69219 (13)	0.71640 (10)	0.53612 (6)	0.0185 (2)
H29A	0.6685 (13)	0.7124 (11)	0.4932 (7)	0.000000
C30	0.67558 (12)	0.79459 (9)	0.57063 (6)	0.0171 (2)
H30A	0.6348 (16)	0.8605 (14)	0.5438 (8)	0.000000
C31	0.70545 (11)	0.79585 (8)	0.63009 (5)	0.01365 (18)
H31A	0.6886 (13)	0.8510 (11)	0.6548 (7)	0.000000
C32	0.75548 (10)	0.71935 (8)	0.65747 (5)	0.01058 (16)
C33	0.74788 (10)	0.78795 (7)	0.75560 (5)	0.01177 (16)
H33A	0.6602 (14)	0.8074 (12)	0.7473 (8)	0.000000
H33B	0.7982 (12)	0.8508 (12)	0.7535 (7)	0.000000
C34	0.62768 (10)	0.80860 (8)	0.86330 (5)	0.01212 (17)
H34A	0.5633 (14)	0.7822 (12)	0.8355 (7)	0.000000
C35	0.86864 (10)	0.82268 (8)	0.86211 (6)	0.01360 (18)
H35A	0.8511 (13)	0.8906 (12)	0.8482 (7)	0.000000
C36	0.63050 (11)	0.91398 (9)	0.86001 (6)	0.0164 (2)
H36A	0.6580 (13)	0.9363 (11)	0.8210 (7)	0.000000
H36B	0.5464 (14)	0.9348 (12)	0.8686 (7)	0.000000
H36C	0.6793 (16)	0.9424 (13)	0.9009 (8)	0.000000
C37	0.59237 (12)	0.77684 (10)	0.92545 (6)	0.0182 (2)
H37A	0.5083 (14)	0.8042 (13)	0.9327 (8)	0.000000
H37B	0.6123 (13)	0.7113 (11)	0.9358 (7)	0.000000
H37C	0.6489 (13)	0.8014 (12)	0.9555 (7)	0.000000
C38	0.97438 (11)	0.79003 (10)	0.83210 (6)	0.0173 (2)
H38A	1.0317 (14)	0.8407 (11)	0.8344 (7)	0.000000
H38B	0.9913 (14)	0.7232 (12)	0.8532 (7)	0.000000
H38C	0.9638 (15)	0.7759 (13)	0.7812 (8)	0.000000
C39	0.88000 (12)	0.82434 (10)	0.92962 (6)	0.0184 (2)
H39A	0.9585 (16)	0.8568 (13)	0.9503 (8)	0.000000
H39B	0.8149 (15)	0.8679 (12)	0.9514 (7)	0.000000
H39C	0.8751 (15)	0.7527 (13)	0.9477 (7)	0.000000

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ni1	0.00899 (5)	0.00842 (5)	0.01178 (6)	−0.00032 (4)	0.00040 (4)	0.00001 (4)
H1A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
In1	0.00886 (3)	0.00814 (3)	0.00895 (3)	0.000085 (18)	0.00013 (2)	−0.00011 (2)
P1	0.01033 (11)	0.00983 (11)	0.00884 (11)	0.00072 (9)	−0.00064 (8)	0.00055 (8)
P2	0.00907 (10)	0.01103 (11)	0.00910 (10)	−0.00187 (9)	0.00045 (8)	−0.00029 (9)
P3	0.01131 (11)	0.00787 (10)	0.00898 (10)	−0.00032 (9)	−0.00060 (9)	−0.00082 (8)
N1	0.0097 (3)	0.0139 (4)	0.0095 (3)	0.0009 (3)	0.0002 (3)	0.0013 (3)
N2	0.0119 (4)	0.0124 (4)	0.0106 (4)	−0.0020 (3)	0.0015 (3)	−0.0026 (3)
N3	0.0148 (4)	0.0091 (3)	0.0087 (3)	0.0014 (3)	−0.0004 (3)	0.0002 (3)
N4	0.0110 (3)	0.0092 (3)	0.0073 (3)	0.0009 (3)	−0.0012 (3)	0.0000 (3)
C1	0.0098 (4)	0.0096 (4)	0.0093 (4)	0.0005 (3)	0.0020 (3)	0.0001 (3)
C2	0.0149 (4)	0.0141 (4)	0.0111 (4)	−0.0001 (4)	0.0033 (3)	0.0000 (3)
H2A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C3	0.0151 (5)	0.0162 (5)	0.0137 (5)	−0.0007 (4)	0.0039 (4)	0.0009 (4)
H3A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C4	0.0117 (4)	0.0157 (4)	0.0164 (5)	−0.0010 (4)	0.0035 (4)	0.0012 (4)
H4A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C5	0.0105 (4)	0.0157 (5)	0.0128 (4)	0.0001 (3)	0.0004 (3)	0.0008 (4)
H5A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C6	0.0098 (4)	0.0110 (4)	0.0094 (4)	0.0006 (3)	0.0014 (3)	0.0004 (3)
C7	0.0111 (4)	0.0142 (4)	0.0105 (4)	0.0007 (4)	−0.0001 (3)	0.0001 (3)
H7A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H7B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C8	0.0157 (5)	0.0167 (5)	0.0112 (4)	−0.0010 (4)	−0.0023 (4)	−0.0005 (4)
H8A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C9	0.0161 (5)	0.0111 (4)	0.0163 (5)	0.0015 (4)	−0.0003 (4)	0.0027 (4)
H9A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C10	0.0163 (5)	0.0298 (7)	0.0218 (6)	0.0005 (5)	−0.0075 (5)	−0.0035 (5)
H10A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H10B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H10C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C11	0.0339 (8)	0.0351 (8)	0.0105 (5)	−0.0097 (7)	0.0003 (5)	0.0009 (5)
H11A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H11B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H11C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C12	0.0257 (6)	0.0119 (5)	0.0198 (5)	−0.0001 (4)	−0.0019 (5)	−0.0027 (4)
H12A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H12B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H12C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C13	0.0201 (6)	0.0152 (5)	0.0372 (8)	0.0050 (5)	−0.0055 (6)	0.0058 (5)
H13A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H13B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H13C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C14	0.0130 (4)	0.0088 (4)	0.0088 (4)	0.0017 (3)	−0.0002 (3)	−0.0013 (3)
C15	0.0153 (4)	0.0126 (4)	0.0095 (4)	0.0001 (4)	0.0007 (3)	−0.0017 (3)
H15A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C16	0.0206 (5)	0.0130 (4)	0.0135 (4)	−0.0010 (4)	0.0012 (4)	−0.0055 (4)
H16A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C17	0.0182 (5)	0.0131 (4)	0.0173 (5)	−0.0033 (4)	0.0001 (4)	−0.0049 (4)
H17A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C18	0.0146 (4)	0.0120 (4)	0.0175 (5)	−0.0027 (4)	0.0009 (4)	−0.0039 (4)
H18A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C19	0.0109 (4)	0.0111 (4)	0.0100 (4)	−0.0006 (3)	0.0001 (3)	−0.0025 (3)
C20	0.0108 (4)	0.0135 (4)	0.0125 (4)	−0.0034 (3)	0.0018 (3)	−0.0016 (3)
H20A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H20B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C21	0.0135 (4)	0.0164 (5)	0.0110 (4)	−0.0036 (4)	0.0009 (3)	0.0011 (4)
H21A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C22	0.0099 (4)	0.0158 (4)	0.0125 (4)	0.0003 (4)	0.0009 (3)	−0.0022 (4)
H22A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C23	0.0214 (6)	0.0217 (6)	0.0180 (5)	0.0003 (5)	0.0031 (4)	0.0066 (4)
H23A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H23B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H23C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C24	0.0247 (6)	0.0215 (6)	0.0099 (4)	−0.0056 (5)	0.0026 (4)	−0.0014 (4)
H24A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H24B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H24C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C25	0.0170 (5)	0.0196 (5)	0.0157 (5)	0.0026 (4)	−0.0013 (4)	0.0033 (5)
H25A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H25B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H25C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C26	0.0108 (4)	0.0221 (6)	0.0198 (5)	−0.0021 (4)	−0.0013 (4)	−0.0028 (4)
H26A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H26B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H26C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C27	0.0149 (4)	0.0092 (4)	0.0074 (4)	0.0020 (3)	−0.0006 (3)	0.0004 (3)
C28	0.0214 (5)	0.0128 (4)	0.0100 (4)	0.0038 (4)	−0.0025 (4)	−0.0014 (3)
H28A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C29	0.0274 (6)	0.0175 (5)	0.0105 (4)	0.0084 (5)	−0.0061 (4)	−0.0003 (4)
H29A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C30	0.0241 (6)	0.0160 (5)	0.0111 (4)	0.0084 (4)	−0.0032 (4)	0.0009 (4)
H30A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C31	0.0177 (5)	0.0120 (4)	0.0112 (4)	0.0044 (4)	−0.0005 (4)	0.0006 (3)
H31A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C32	0.0125 (4)	0.0093 (4)	0.0099 (4)	0.0014 (3)	−0.0009 (3)	0.0003 (3)
C33	0.0163 (4)	0.0086 (3)	0.0104 (4)	0.0013 (3)	0.0004 (4)	−0.0006 (3)
H33A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H33B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C34	0.0146 (4)	0.0114 (4)	0.0104 (4)	0.0010 (3)	0.0002 (3)	−0.0008 (3)
H34A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C35	0.0156 (4)	0.0108 (4)	0.0144 (5)	−0.0019 (4)	−0.0005 (4)	−0.0021 (4)
H35A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C36	0.0202 (5)	0.0120 (4)	0.0169 (5)	0.0029 (4)	0.0012 (4)	−0.0010 (4)
H36A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H36B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H36C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C37	0.0242 (6)	0.0168 (5)	0.0137 (5)	−0.0008 (5)	0.0043 (4)	−0.0010 (4)
H37A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H37B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H37C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C38	0.0160 (5)	0.0192 (5)	0.0167 (5)	−0.0046 (4)	0.0015 (4)	−0.0034 (4)
H38A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H38B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H38C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C39	0.0194 (5)	0.0207 (5)	0.0151 (5)	−0.0033 (5)	−0.0032 (4)	−0.0041 (4)
H39A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H39B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H39C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000

Geometric parameters (Å, º)

Ni1—H1A	1.71 (2)	C14—C19	1.4282 (16)
Ni1—H1B	1.68 (2)	C15—H15A	1.164 (18)
Ni1—In1	2.4788 (2)	C15—C16	1.3968 (18)
Ni1—P1	2.2834 (3)	C16—H16A	1.086 (17)
Ni1—P2	2.2527 (3)	C16—C17	1.3931 (19)
Ni1—P3	2.2501 (3)	C17—H17A	1.156 (18)
H1A—H1B	0.95 (3)	C17—C18	1.3922 (18)
In1—N1	2.1108 (9)	C18—H18A	1.070 (17)
In1—N2	2.1218 (10)	C18—C19	1.4139 (17)
In1—N3	2.1146 (10)	C20—H20A	1.157 (18)
In1—N4	2.3681 (10)	C20—H20B	1.105 (16)
P1—C7	1.8658 (12)	C21—H21A	1.128 (18)
P1—C8	1.8702 (13)	C21—C23	1.528 (2)
P1—C9	1.8645 (13)	C21—C24	1.5353 (19)
P2—C20	1.8716 (12)	C22—H22A	1.090 (17)
P2—C21	1.8593 (12)	C22—C25	1.5299 (19)
P2—C22	1.8791 (12)	C22—C26	1.5322 (18)
P3—C33	1.8894 (12)	C23—H23A	1.110 (17)
P3—C34	1.8651 (12)	C23—H23B	1.070 (17)
P3—C35	1.8553 (12)	C23—H23C	1.256 (19)
N1—C6	1.3644 (15)	C24—H24A	1.25 (2)
N1—C7	1.4440 (16)	C24—H24B	1.093 (17)
N2—C19	1.3655 (15)	C24—H24C	1.085 (17)
N2—C20	1.4487 (15)	C25—H25A	1.118 (17)
N3—C32	1.3718 (14)	C25—H25B	1.038 (16)
N3—C33	1.4385 (15)	C25—H25C	1.110 (17)
N4—C1	1.4645 (15)	C26—H26A	1.107 (17)
N4—C14	1.4551 (15)	C26—H26B	1.033 (16)
N4—C27	1.4627 (14)	C26—H26C	1.117 (17)
C1—C2	1.3879 (16)	C27—C28	1.3871 (16)
C1—C6	1.4284 (16)	C27—C32	1.4250 (16)
C2—H2A	0.984 (15)	C28—H28A	1.161 (18)
C2—C3	1.4034 (18)	C28—C29	1.3965 (18)
C3—H3A	1.098 (17)	C29—H29A	1.013 (16)
C3—C4	1.3984 (18)	C29—C30	1.3928 (19)
C4—H4A	1.036 (16)	C30—H30A	1.238 (19)
C4—C5	1.3938 (17)	C30—C31	1.3903 (18)
C5—H5A	1.168 (18)	C31—H31A	0.998 (16)
C5—C6	1.4147 (17)	C31—C32	1.4113 (16)
C7—H7A	1.056 (16)	C33—H33A	1.124 (17)
C7—H7B	1.161 (18)	C33—H33B	1.102 (17)
C8—H8A	1.144 (18)	C34—H34A	1.077 (16)
C8—C10	1.537 (2)	C34—C36	1.5345 (18)
C8—C11	1.530 (2)	C34—C37	1.5380 (18)
C9—H9A	1.128 (17)	C35—H35A	1.059 (17)
C9—C12	1.5365 (19)	C35—C38	1.5335 (19)
C9—C13	1.5223 (19)	C35—C39	1.5296 (18)
C10—H10A	1.25 (2)	C36—H36A	0.997 (16)
C10—H10B	0.993 (15)	C36—H36B	1.088 (17)
C10—H10C	1.34 (2)	C36—H36C	1.174 (18)
C11—H11A	1.160 (18)	C37—H37A	1.113 (17)
C11—H11B	1.071 (16)	C37—H37B	1.011 (16)
C11—H11C	1.148 (18)	C37—H37C	1.031 (16)
C12—H12A	1.072 (18)	C38—H38A	1.018 (17)
C12—H12B	1.187 (18)	C38—H38B	1.101 (17)
C12—H12C	1.061 (16)	C38—H38C	1.173 (18)
C13—H13A	1.076 (18)	C39—H39A	1.166 (19)
C13—H13B	1.094 (17)	C39—H39B	1.129 (18)
C13—H13C	1.068 (17)	C39—H39C	1.120 (18)
C14—C15	1.3877 (16)
H1B—Ni1—H1A	32.5 (9)	C15—C14—N4	121.18 (10)
In1—Ni1—H1A	155.3 (7)	C19—C14—N4	118.08 (9)
In1—Ni1—H1B	168.3 (7)	C19—C14—C15	120.71 (10)
P1—Ni1—H1A	88.0 (7)	H15A—C15—C14	117.4 (9)
P1—Ni1—H1B	92.6 (7)	C16—C15—C14	121.50 (11)
P1—Ni1—In1	81.131 (9)	C16—C15—H15A	121.1 (9)
P2—Ni1—H1A	85.0 (7)	H16A—C16—C15	121.4 (9)
P2—Ni1—H1B	109.3 (7)	C17—C16—C15	118.54 (11)
P2—Ni1—In1	82.400 (9)	C17—C16—H16A	120.1 (9)
P2—Ni1—P1	122.750 (13)	H17A—C17—C16	116.6 (9)
P3—Ni1—H1A	119.9 (7)	C18—C17—C16	120.89 (11)
P3—Ni1—H1B	90.2 (7)	C18—C17—H17A	122.3 (9)
P3—Ni1—In1	84.552 (9)	H18A—C18—C17	117.6 (9)
P3—Ni1—P1	120.196 (13)	C19—C18—C17	121.55 (12)
P3—Ni1—P2	112.170 (13)	C19—C18—H18A	120.6 (9)
H1B—H1A—Ni1	72.5 (19)	C14—C19—N2	118.79 (10)
H1A—H1B—Ni1	75.0 (19)	C18—C19—N2	124.40 (11)
N1—In1—Ni1	104.68 (3)	C18—C19—C14	116.80 (10)
N2—In1—Ni1	102.78 (3)	N2—C20—P2	108.29 (8)
N2—In1—N1	116.51 (4)	H20A—C20—P2	106.1 (9)
N3—In1—Ni1	103.23 (3)	H20A—C20—N2	120.0 (9)
N3—In1—N1	111.73 (4)	H20B—C20—P2	111.7 (9)
N3—In1—N2	115.79 (4)	H20B—C20—N2	107.7 (9)
N4—In1—Ni1	178.59 (2)	H20B—C20—H20A	103.0 (13)
N4—In1—N1	76.60 (4)	H21A—C21—P2	109.9 (9)
N4—In1—N2	76.04 (4)	C23—C21—P2	112.34 (9)
N4—In1—N3	76.72 (3)	C23—C21—H21A	103.5 (9)
C7—P1—Ni1	117.46 (4)	C24—C21—P2	110.01 (9)
C8—P1—Ni1	110.56 (4)	C24—C21—H21A	110.7 (9)
C8—P1—C7	103.33 (6)	C24—C21—C23	110.27 (11)
C9—P1—Ni1	116.67 (4)	H22A—C22—P2	102.4 (9)
C9—P1—C7	102.03 (6)	C25—C22—P2	110.93 (8)
C9—P1—C8	105.27 (6)	C25—C22—H22A	107.0 (9)
C20—P2—Ni1	117.98 (4)	C26—C22—P2	115.69 (10)
C21—P2—Ni1	114.38 (4)	C26—C22—H22A	111.5 (9)
C21—P2—C20	102.58 (5)	C26—C22—C25	108.93 (10)
C22—P2—Ni1	117.31 (4)	H23A—C23—C21	105.8 (9)
C22—P2—C20	100.60 (6)	H23B—C23—C21	117.0 (9)
C22—P2—C21	101.46 (6)	H23B—C23—H23A	105.0 (13)
C33—P3—Ni1	118.81 (3)	H23C—C23—C21	107.8 (9)
C34—P3—Ni1	112.78 (4)	H23C—C23—H23A	109.3 (12)
C34—P3—C33	98.98 (5)	H23C—C23—H23B	111.6 (13)
C35—P3—Ni1	118.80 (4)	H24A—C24—C21	112.8 (9)
C35—P3—C33	99.78 (6)	H24B—C24—C21	109.5 (9)
C35—P3—C34	104.92 (5)	H24B—C24—H24A	106.1 (13)
C6—N1—In1	113.03 (8)	H24C—C24—C21	116.9 (9)
C7—N1—In1	115.72 (7)	H24C—C24—H24A	103.9 (13)
C7—N1—C6	119.50 (9)	H24C—C24—H24B	106.8 (12)
C19—N2—In1	112.95 (8)	H25A—C25—C22	109.9 (9)
C20—N2—In1	117.99 (7)	H25B—C25—C22	119.4 (9)
C20—N2—C19	120.64 (10)	H25B—C25—H25A	110.9 (13)
C32—N3—In1	113.05 (7)	H25C—C25—C22	107.7 (9)
C33—N3—In1	118.76 (7)	H25C—C25—H25A	110.0 (12)
C33—N3—C32	119.69 (10)	H25C—C25—H25B	98.1 (13)
C1—N4—In1	103.11 (7)	H26A—C26—C22	110.1 (9)
C14—N4—In1	103.38 (6)	H26B—C26—C22	109.4 (9)
C14—N4—C1	115.89 (9)	H26B—C26—H26A	112.3 (12)
C27—N4—In1	102.54 (6)	H26C—C26—C22	120.8 (9)
C27—N4—C1	113.65 (9)	H26C—C26—H26A	108.5 (13)
C27—N4—C14	115.72 (9)	H26C—C26—H26B	94.9 (13)
C2—C1—N4	121.23 (10)	C28—C27—N4	121.04 (10)
C6—C1—N4	118.04 (10)	C32—C27—N4	118.03 (9)
C6—C1—C2	120.65 (10)	C32—C27—C28	120.93 (10)
H2A—C2—C1	121.9 (9)	H28A—C28—C27	114.7 (9)
C3—C2—C1	121.42 (12)	C29—C28—C27	121.27 (11)
C3—C2—H2A	116.3 (9)	C29—C28—H28A	123.8 (9)
H3A—C3—C2	124.2 (9)	H29A—C29—C28	118.7 (9)
C4—C3—C2	118.58 (11)	C30—C29—C28	118.58 (11)
C4—C3—H3A	116.9 (9)	C30—C29—H29A	122.7 (9)
H4A—C4—C3	117.9 (9)	H30A—C30—C29	114.6 (9)
C5—C4—C3	120.68 (11)	C31—C30—C29	120.78 (11)
C5—C4—H4A	121.4 (9)	C31—C30—H30A	124.6 (9)
H5A—C5—C4	117.3 (9)	H31A—C31—C30	119.7 (9)
C6—C5—C4	121.56 (11)	C32—C31—C30	121.70 (11)
C6—C5—H5A	121.0 (9)	C32—C31—H31A	118.6 (9)
C1—C6—N1	119.13 (10)	C27—C32—N3	119.40 (10)
C5—C6—N1	123.76 (11)	C31—C32—N3	123.94 (10)
C5—C6—C1	117.10 (10)	C31—C32—C27	116.66 (10)
N1—C7—P1	108.64 (8)	N3—C33—P3	111.60 (7)
H7A—C7—P1	105.4 (9)	H33A—C33—P3	105.6 (9)
H7A—C7—N1	118.3 (9)	H33A—C33—N3	111.9 (9)
H7B—C7—P1	117.3 (8)	H33B—C33—P3	105.2 (8)
H7B—C7—N1	108.7 (8)	H33B—C33—N3	113.7 (8)
H7B—C7—H7A	98.8 (12)	H33B—C33—H33A	108.4 (12)
H8A—C8—P1	103.6 (9)	H34A—C34—P3	104.2 (9)
C10—C8—P1	117.22 (10)	C36—C34—P3	114.88 (9)
C10—C8—H8A	103.6 (9)	C36—C34—H34A	110.1 (9)
C11—C8—P1	110.53 (10)	C37—C34—P3	113.52 (9)
C11—C8—H8A	110.1 (9)	C37—C34—H34A	102.7 (9)
C11—C8—C10	111.12 (13)	C37—C34—C36	110.50 (10)
H9A—C9—P1	104.9 (9)	H35A—C35—P3	106.4 (9)
C12—C9—P1	110.00 (9)	C38—C35—P3	108.63 (8)
C12—C9—H9A	107.1 (9)	C38—C35—H35A	109.2 (9)
C13—C9—P1	116.87 (10)	C39—C35—P3	113.44 (9)
C13—C9—H9A	108.8 (9)	C39—C35—H35A	107.4 (9)
C13—C9—C12	108.78 (12)	C39—C35—C38	111.60 (11)
H10A—C10—C8	113.0 (9)	H36A—C36—C34	112.1 (9)
H10B—C10—C8	111.4 (9)	H36B—C36—C34	104.3 (9)
H10B—C10—H10A	111.8 (13)	H36B—C36—H36A	112.6 (13)
H10C—C10—C8	106.5 (9)	H36C—C36—C34	109.0 (9)
H10C—C10—H10A	97.8 (12)	H36C—C36—H36A	114.1 (13)
H10C—C10—H10B	115.6 (13)	H36C—C36—H36B	104.0 (13)
H11A—C11—C8	101.4 (9)	H37A—C37—C34	106.6 (9)
H11B—C11—C8	116.0 (9)	H37B—C37—C34	115.2 (9)
H11B—C11—H11A	116.2 (13)	H37B—C37—H37A	121.7 (13)
H11C—C11—C8	108.6 (9)	H37C—C37—C34	107.9 (9)
H11C—C11—H11A	101.5 (13)	H37C—C37—H37A	113.4 (13)
H11C—C11—H11B	111.7 (13)	H37C—C37—H37B	90.8 (13)
H12A—C12—C9	105.6 (9)	H38A—C38—C35	109.4 (9)
H12B—C12—C9	108.1 (9)	H38B—C38—C35	103.9 (9)
H12B—C12—H12A	117.1 (13)	H38B—C38—H38A	119.1 (13)
H12C—C12—C9	108.3 (9)	H38C—C38—C35	113.2 (9)
H12C—C12—H12A	104.4 (13)	H38C—C38—H38A	104.7 (13)
H12C—C12—H12B	112.9 (12)	H38C—C38—H38B	106.8 (13)
H13A—C13—C9	120.8 (10)	H39A—C39—C35	118.7 (9)
H13B—C13—C9	115.7 (9)	H39B—C39—C35	112.3 (9)
H13B—C13—H13A	112.8 (13)	H39B—C39—H39A	100.2 (13)
H13C—C13—C9	118.7 (10)	H39C—C39—C35	110.0 (9)
H13C—C13—H13A	93.5 (13)	H39C—C39—H39A	106.0 (13)
H13C—C13—H13B	89.1 (13)	H39C—C39—H39B	109.0 (13)
In1—N1—C6—C1	−26.68 (9)	N2—C19—C18—C17	−179.61 (12)
In1—N1—C6—C5	152.11 (8)	N3—C32—C27—N4	−4.50 (13)
In1—N1—C7—P1	29.22 (6)	N3—C32—C27—C28	176.52 (11)
In1—N2—C19—C14	−26.87 (9)	N3—C32—C31—C30	−178.45 (13)
In1—N2—C19—C18	152.11 (8)	N4—C1—C2—C3	177.38 (11)
In1—N2—C20—P2	23.25 (7)	N4—C1—C6—C5	−176.73 (10)
In1—N3—C32—C27	−21.98 (9)	N4—C14—C15—C16	178.39 (11)
In1—N3—C32—C31	157.58 (8)	N4—C14—C19—C18	−177.77 (10)
In1—N3—C33—P3	14.42 (7)	N4—C27—C28—C29	−176.31 (12)
In1—N4—C1—C2	−157.18 (7)	N4—C27—C32—C31	175.91 (10)
In1—N4—C1—C6	19.47 (7)	C1—C2—C3—C4	−1.06 (14)
In1—N4—C14—C15	−157.00 (7)	C1—C6—C5—C4	−0.44 (13)
In1—N4—C14—C19	20.86 (7)	C2—C3—C4—C5	0.55 (15)
In1—N4—C27—C28	−156.87 (8)	C3—C4—C5—C6	0.20 (15)
In1—N4—C27—C32	24.15 (8)	C14—C15—C16—C17	−0.76 (14)
P1—C7—N1—C6	169.70 (8)	C14—C19—C18—C17	−0.61 (13)
P2—C20—N2—C19	169.15 (7)	C15—C16—C17—C18	0.25 (15)
P3—C33—N3—C32	160.21 (8)	C16—C17—C18—C19	0.44 (16)
N1—C6—C1—N4	2.14 (12)	C27—C28—C29—C30	−0.13 (16)
N1—C6—C1—C2	178.81 (11)	C27—C32—C31—C30	1.12 (14)
N1—C6—C5—C4	−179.25 (12)	C28—C29—C30—C31	−1.84 (18)
N2—C19—C14—N4	1.30 (12)	C29—C30—C31—C32	1.32 (18)
N2—C19—C14—C15	179.17 (11)

(GOJNIF_HAR)

Crystal data

C39H62InN4NiP3	Dx = 1.415 Mg m^−3
Mr = 853.39	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, P212121	Cell parameters from 9537 reflections
a = 12.2127 (4) Å	θ = 2.3–36.4°
b = 14.5402 (5) Å	µ = 1.20 mm^−1
c = 22.5601 (8) Å	T = 100 K
V = 4006.1 (2) Å^3	Block, gold
Z = 4	0.14 × 0.08 × 0.06 mm
F(000) = 105.781

Data collection

Bruker Photon-II CMOS diffractometer	18741 reflections with I ≥ 2u(I)
φ and ω scans	Rint = 0.036
Absorption correction: multi-scan SADABS. R.Blessing, 1995	θmax = 36.4°, θmin = 2.3°
Tmin = 0.701, Tmax = 0.747	h = −20→20
237431 measured reflections	k = −24→24
19473 independent reflections	l = −37→37

Refinement

Refinement on F^2	0 constraints
Least-squares matrix: full	All H-atom parameters refined
R[F^2 > 2σ(F^2)] = 0.023	w = 1/[σ^2(Fo^2) + (0.0161P)^2 + 3.3112P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.051	(Δ/σ)max = 0.001
S = 1.04	Δρmax = 0.35 e Å^−3
19473 reflections	Δρmin = −0.62 e Å^−3
936 parameters	Absolute structure: Flack, H. D. (1983). Acta Cryst. A39, 876-881.
0 restraints	Absolute structure parameter: 0.234 (5)

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ni1	0.755807 (13)	0.598646 (10)	0.856159 (7)	0.00891 (3)
H1A	0.727 (3)	0.574 (3)	0.9266 (17)	0.056 (11)*
H1B	0.757 (4)	0.635 (3)	0.927 (2)	0.080 (15)*
In1	0.798239 (6)	0.580826 (5)	0.749330 (4)	0.008881 (15)
P1	0.91844 (3)	0.52225 (2)	0.864335 (14)	0.00896 (5)
P2	0.59903 (3)	0.52857 (2)	0.829180 (14)	0.00902 (5)
P3	0.75360 (3)	0.75011 (2)	0.835669 (14)	0.00874 (5)
N1	0.96178 (8)	0.53380 (7)	0.74730 (6)	0.01052 (15)
N2	0.67669 (9)	0.48662 (8)	0.72034 (5)	0.01092 (18)
N3	0.78428 (9)	0.71627 (7)	0.71617 (5)	0.01021 (17)
N4	0.83427 (9)	0.56334 (7)	0.64679 (5)	0.00848 (16)
C1	0.95348 (10)	0.57173 (8)	0.64334 (5)	0.00915 (17)
C2	1.00524 (11)	0.59716 (9)	0.59113 (6)	0.0125 (2)
H2A	0.957 (2)	0.6113 (18)	0.5529 (11)	0.025 (6)*
C3	1.11901 (12)	0.60861 (10)	0.58837 (6)	0.0143 (2)
H3A	1.160 (2)	0.629 (2)	0.5486 (13)	0.037 (7)*
C4	1.18033 (10)	0.59552 (9)	0.63977 (6)	0.0138 (2)
H4A	1.2671 (19)	0.6043 (18)	0.6379 (11)	0.029 (6)
C5	1.12975 (10)	0.57047 (9)	0.69269 (6)	0.0121 (2)
H5A	1.178 (2)	0.5614 (17)	0.7321 (10)	0.026 (6)
C6	1.01536 (11)	0.55741 (9)	0.69638 (6)	0.0095 (2)
C7	1.01939 (11)	0.53663 (10)	0.80307 (6)	0.0111 (2)
H7A	1.0632 (19)	0.6008 (17)	0.8120 (11)	0.025 (6)
H7B	1.082 (2)	0.4808 (19)	0.8063 (11)	0.031 (7)
C8	0.99541 (12)	0.56224 (10)	0.93122 (6)	0.0138 (2)
H8A	0.981 (2)	0.6375 (18)	0.9321 (12)	0.032 (7)
C9	0.91079 (11)	0.39464 (9)	0.87150 (6)	0.0135 (2)
H9A	0.852 (2)	0.3829 (18)	0.9081 (12)	0.029 (7)
C10	1.12044 (14)	0.55059 (13)	0.93045 (8)	0.0220 (3)
H10A	1.143 (3)	0.479 (2)	0.9271 (18)	0.067 (11)
H10B	1.160 (2)	0.587 (3)	0.8936 (13)	0.053 (9)
H10C	1.155 (2)	0.580 (3)	0.9722 (13)	0.049 (9)
C11	0.94556 (17)	0.52153 (15)	0.98765 (7)	0.0263 (3)
H11A	0.979 (4)	0.554 (3)	1.0251 (13)	0.084 (15)
H11B	0.862 (3)	0.535 (2)	0.9907 (14)	0.046 (8)*
H11C	0.953 (3)	0.447 (2)	0.9914 (14)	0.062 (12)
C12	0.86448 (14)	0.35267 (10)	0.81439 (7)	0.0182 (3)
H12A	0.849 (3)	0.2809 (17)	0.8216 (13)	0.048 (9)
H12B	0.786 (2)	0.3855 (19)	0.8018 (13)	0.040 (8)
H12C	0.924 (3)	0.362 (2)	0.7787 (11)	0.048 (10)
C13	1.01692 (15)	0.34496 (11)	0.88746 (9)	0.0234 (3)
H13A	1.005 (3)	0.272 (2)	0.8865 (14)	0.049 (9)*
H13B	1.083 (2)	0.3606 (19)	0.8545 (15)	0.042 (8)
H13C	1.048 (3)	0.362 (2)	0.9308 (15)	0.053 (10)
C14	0.78966 (10)	0.47284 (8)	0.63325 (5)	0.00964 (18)
C15	0.82602 (11)	0.42267 (10)	0.58484 (5)	0.01201 (19)
H15A	0.8904 (19)	0.4519 (16)	0.5573 (10)	0.019 (5)*
C16	0.78525 (12)	0.33496 (9)	0.57247 (6)	0.0147 (2)
H16A	0.815 (2)	0.2968 (17)	0.5338 (11)	0.030 (7)
C17	0.70729 (13)	0.29739 (9)	0.61049 (6)	0.0156 (2)
H17A	0.676 (3)	0.2291 (18)	0.6023 (12)	0.040 (8)
C18	0.67002 (12)	0.34631 (9)	0.65962 (6)	0.0138 (2)
H18A	0.612 (2)	0.3151 (19)	0.6913 (11)	0.027 (6)
C19	0.70909 (10)	0.43552 (8)	0.67264 (5)	0.01006 (18)
C20	0.60328 (11)	0.44849 (9)	0.76426 (6)	0.0115 (2)
H20A	0.628 (2)	0.3794 (18)	0.7806 (13)	0.033 (7)
H20B	0.5193 (18)	0.4393 (16)	0.7461 (13)	0.027 (6)
C21	0.53629 (11)	0.45621 (9)	0.88800 (6)	0.0128 (2)
H21A	0.465 (2)	0.422 (2)	0.8679 (11)	0.027 (6)*
C22	0.48065 (10)	0.60402 (10)	0.80768 (6)	0.0121 (2)
H22A	0.478 (2)	0.6577 (17)	0.8413 (11)	0.031 (7)
C23	0.61405 (14)	0.38130 (12)	0.91017 (7)	0.0202 (3)
H23A	0.573 (2)	0.337 (2)	0.9433 (13)	0.036 (7)*
H23B	0.640 (3)	0.3364 (19)	0.8756 (13)	0.042 (8)
H23C	0.684 (2)	0.414 (2)	0.9314 (12)	0.041 (8)
C24	0.49919 (14)	0.51662 (12)	0.94002 (6)	0.0183 (3)
H24A	0.443 (2)	0.574 (2)	0.9267 (11)	0.038 (8)
H24B	0.463 (3)	0.4754 (19)	0.9726 (11)	0.038 (8)
H24C	0.569 (2)	0.551 (2)	0.9607 (13)	0.040 (8)
C25	0.49935 (11)	0.64750 (10)	0.74678 (8)	0.0168 (2)
H25A	0.436 (2)	0.6986 (18)	0.7376 (11)	0.033 (7)
H25B	0.578 (2)	0.6809 (19)	0.7409 (10)	0.029 (6)
H25C	0.494 (2)	0.595 (2)	0.7130 (12)	0.039 (7)*
C26	0.36765 (12)	0.55815 (11)	0.80854 (7)	0.0171 (2)
H26A	0.306 (2)	0.6093 (18)	0.7969 (14)	0.037 (7)
H26B	0.364 (2)	0.5028 (19)	0.7777 (12)	0.037 (7)
H26C	0.344 (2)	0.534 (2)	0.8512 (12)	0.043 (8)
C27	0.77587 (10)	0.64131 (8)	0.62076 (5)	0.00994 (19)
C28	0.74260 (13)	0.64002 (9)	0.56205 (6)	0.0140 (2)
H28A	0.7542 (19)	0.5773 (16)	0.5369 (10)	0.021 (5)
C29	0.69212 (14)	0.71649 (10)	0.53620 (6)	0.0177 (2)
H29A	0.669 (3)	0.7150 (19)	0.4909 (12)	0.043 (9)
C30	0.67545 (13)	0.79434 (10)	0.57069 (6)	0.0165 (2)
H30A	0.638 (3)	0.8550 (18)	0.5518 (13)	0.036 (8)
C31	0.70546 (12)	0.79591 (9)	0.63023 (6)	0.0128 (2)
H31A	0.693 (3)	0.8574 (17)	0.6538 (13)	0.041 (8)
C32	0.75543 (11)	0.71946 (8)	0.65751 (5)	0.00952 (18)
C33	0.74804 (11)	0.78800 (8)	0.75567 (6)	0.01132 (18)
H33A	0.6630 (17)	0.8081 (17)	0.7469 (13)	0.029 (6)
H33B	0.797 (2)	0.8504 (15)	0.7520 (11)	0.029 (6)
C34	0.62754 (11)	0.80867 (9)	0.86343 (6)	0.0115 (2)
H34A	0.5636 (19)	0.7829 (17)	0.8332 (10)	0.021 (6)
C35	0.86861 (11)	0.82275 (9)	0.86203 (6)	0.0126 (2)
H35A	0.849 (2)	0.8921 (16)	0.8463 (12)	0.032 (7)
C36	0.63050 (12)	0.91388 (10)	0.85998 (6)	0.0158 (2)
H36A	0.657 (2)	0.937 (2)	0.8174 (12)	0.040 (8)
H36B	0.550 (2)	0.9423 (19)	0.8692 (13)	0.038 (8)
H36C	0.685 (3)	0.9425 (19)	0.8938 (13)	0.043 (8)
C37	0.59270 (14)	0.77704 (11)	0.92534 (7)	0.0174 (2)
H37A	0.514 (2)	0.805 (2)	0.9364 (15)	0.054 (10)
H37B	0.586 (3)	0.7045 (17)	0.9288 (13)	0.045 (9)
H37C	0.648 (2)	0.8012 (19)	0.9578 (11)	0.029 (6)
C38	0.97439 (12)	0.78990 (11)	0.83199 (7)	0.0166 (2)
H38A	1.036 (3)	0.840 (2)	0.8348 (16)	0.052 (10)
H38B	1.001 (2)	0.7265 (18)	0.8516 (12)	0.036 (7)
H38C	0.961 (2)	0.778 (2)	0.7844 (11)	0.032 (7)
C39	0.87995 (13)	0.82433 (11)	0.92965 (7)	0.0175 (2)
H39A	0.955 (3)	0.858 (3)	0.9429 (16)	0.063 (12)
H39B	0.817 (2)	0.862 (2)	0.9510 (12)	0.042 (8)
H39C	0.877 (2)	0.755 (2)	0.9479 (13)	0.038 (7)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ni1	0.00806 (6)	0.00781 (6)	0.01086 (6)	−0.00034 (5)	0.00038 (5)	0.00003 (5)
In1	0.00908 (3)	0.00840 (3)	0.00917 (3)	0.00011 (2)	0.00015 (3)	−0.00014 (3)
P1	0.00966 (12)	0.00914 (12)	0.00807 (12)	0.00075 (10)	−0.00067 (9)	0.00064 (10)
P2	0.00826 (12)	0.01045 (12)	0.00835 (12)	−0.00177 (10)	0.00046 (9)	−0.00026 (10)
P3	0.01059 (12)	0.00735 (11)	0.00828 (11)	−0.00014 (11)	−0.00058 (10)	−0.00085 (9)
N1	0.0089 (3)	0.0133 (4)	0.0093 (4)	0.0010 (3)	0.0001 (4)	0.0013 (4)
N2	0.0114 (4)	0.0112 (4)	0.0101 (4)	−0.0022 (3)	0.0012 (3)	−0.0025 (3)
N3	0.0138 (5)	0.0087 (4)	0.0081 (4)	0.0016 (3)	−0.0008 (3)	0.0002 (3)
N4	0.0100 (4)	0.0085 (4)	0.0070 (4)	0.0009 (3)	−0.0008 (3)	0.0001 (3)
C1	0.0098 (4)	0.0097 (4)	0.0079 (4)	0.0005 (4)	0.0014 (3)	0.0000 (4)
C2	0.0140 (5)	0.0132 (5)	0.0103 (5)	0.0000 (4)	0.0026 (4)	0.0007 (4)
C3	0.0144 (5)	0.0157 (5)	0.0129 (5)	−0.0011 (4)	0.0043 (4)	0.0012 (4)
C4	0.0108 (5)	0.0148 (5)	0.0156 (5)	−0.0008 (4)	0.0036 (4)	0.0006 (4)
H4A	0.017 (12)	0.042 (16)	0.028 (14)	−0.002 (12)	−0.005 (11)	−0.003 (13)
C5	0.0097 (5)	0.0145 (5)	0.0121 (5)	0.0002 (4)	0.0007 (4)	0.0005 (4)
H5A	0.025 (14)	0.026 (14)	0.026 (14)	0.007 (11)	−0.010 (11)	−0.013 (11)
C6	0.0091 (5)	0.0106 (5)	0.0088 (5)	0.0006 (4)	0.0011 (4)	0.0000 (4)
C7	0.0096 (5)	0.0140 (5)	0.0098 (5)	0.0011 (4)	−0.0003 (4)	0.0007 (4)
H7A	0.016 (13)	0.027 (15)	0.032 (15)	−0.007 (12)	−0.011 (11)	0.004 (12)
H7B	0.031 (16)	0.040 (17)	0.023 (14)	0.016 (14)	−0.014 (12)	−0.002 (13)
C8	0.0152 (5)	0.0162 (6)	0.0102 (5)	−0.0013 (4)	−0.0021 (4)	−0.0004 (4)
H8A	0.047 (19)	0.022 (14)	0.026 (16)	0.013 (14)	−0.009 (14)	0.007 (12)
C9	0.0145 (5)	0.0103 (5)	0.0156 (5)	0.0015 (4)	−0.0005 (4)	0.0027 (4)
H9A	0.030 (16)	0.025 (15)	0.033 (16)	−0.002 (12)	0.011 (13)	−0.017 (12)
C10	0.0162 (6)	0.0287 (8)	0.0212 (7)	0.0007 (6)	−0.0078 (5)	−0.0036 (6)
H10A	0.05 (2)	0.04 (2)	0.11 (3)	0.009 (19)	−0.03 (2)	−0.02 (2)
H10B	0.036 (19)	0.08 (3)	0.041 (19)	−0.01 (2)	0.002 (15)	0.02 (2)
H10C	0.039 (18)	0.08 (3)	0.032 (17)	−0.016 (19)	−0.009 (14)	−0.010 (18)
C11	0.0334 (9)	0.0344 (9)	0.0111 (6)	−0.0102 (7)	0.0003 (6)	0.0007 (6)
H11A	0.17 (5)	0.07 (3)	0.012 (16)	−0.02 (3)	−0.02 (2)	−0.010 (16)
H11C	0.12 (3)	0.025 (17)	0.04 (2)	−0.04 (2)	−0.02 (2)	0.003 (14)
C12	0.0241 (7)	0.0110 (5)	0.0194 (6)	−0.0006 (5)	−0.0019 (5)	−0.0018 (5)
H12A	0.08 (3)	0.007 (12)	0.05 (2)	0.006 (15)	−0.031 (19)	−0.001 (13)
H12B	0.037 (18)	0.034 (17)	0.048 (19)	0.003 (14)	−0.012 (15)	−0.013 (14)
H12C	0.09 (3)	0.05 (2)	0.003 (12)	−0.02 (2)	0.007 (15)	0.001 (13)
C13	0.0200 (7)	0.0139 (6)	0.0363 (9)	0.0054 (5)	−0.0056 (6)	0.0051 (6)
H13B	0.024 (16)	0.028 (16)	0.07 (2)	0.016 (13)	0.019 (17)	0.002 (17)
H13C	0.06 (2)	0.05 (2)	0.05 (2)	0.005 (19)	−0.029 (19)	0.026 (18)
C14	0.0117 (4)	0.0088 (4)	0.0084 (4)	0.0012 (4)	0.0000 (4)	−0.0014 (3)
C15	0.0149 (5)	0.0115 (5)	0.0097 (4)	0.0001 (4)	0.0011 (4)	−0.0020 (4)
C16	0.0182 (6)	0.0127 (5)	0.0133 (5)	−0.0007 (4)	0.0010 (4)	−0.0057 (4)
H16A	0.035 (16)	0.023 (14)	0.031 (15)	−0.005 (13)	0.009 (13)	−0.022 (12)
C17	0.0180 (6)	0.0120 (5)	0.0168 (5)	−0.0029 (5)	0.0007 (5)	−0.0055 (4)
H17A	0.06 (2)	0.028 (15)	0.029 (16)	−0.012 (15)	0.021 (15)	−0.016 (13)
C18	0.0142 (5)	0.0119 (5)	0.0154 (5)	−0.0030 (4)	0.0014 (4)	−0.0039 (4)
H18A	0.017 (13)	0.040 (17)	0.024 (14)	−0.019 (12)	−0.011 (11)	0.001 (12)
C19	0.0104 (4)	0.0099 (4)	0.0099 (4)	−0.0007 (4)	0.0002 (4)	−0.0023 (3)
C20	0.0106 (5)	0.0120 (4)	0.0118 (5)	−0.0027 (4)	0.0014 (4)	−0.0020 (3)
H20A	0.021 (15)	0.018 (14)	0.06 (2)	0.005 (12)	−0.002 (13)	0.005 (13)
H20B	0.019 (12)	0.032 (14)	0.030 (14)	−0.008 (10)	0.001 (14)	−0.013 (14)
C21	0.0125 (5)	0.0153 (5)	0.0106 (5)	−0.0039 (4)	0.0007 (4)	0.0010 (4)
C22	0.0093 (4)	0.0152 (5)	0.0117 (5)	0.0003 (4)	0.0005 (4)	−0.0020 (4)
H22A	0.046 (18)	0.025 (15)	0.022 (14)	0.008 (13)	0.000 (13)	−0.016 (11)
C23	0.0205 (7)	0.0218 (7)	0.0184 (6)	0.0002 (5)	0.0023 (5)	0.0075 (5)
H23B	0.05 (2)	0.030 (17)	0.044 (19)	0.020 (15)	−0.001 (16)	0.022 (14)
H23C	0.036 (17)	0.051 (19)	0.035 (16)	0.000 (16)	−0.023 (14)	0.000 (15)
C24	0.0236 (7)	0.0213 (6)	0.0100 (5)	−0.0057 (5)	0.0029 (5)	−0.0011 (5)
H24A	0.042 (18)	0.05 (2)	0.017 (14)	0.002 (17)	0.010 (13)	0.004 (15)
H24B	0.07 (2)	0.027 (16)	0.015 (13)	−0.021 (15)	0.015 (14)	0.009 (12)
H24C	0.026 (16)	0.05 (2)	0.041 (18)	−0.017 (14)	−0.012 (14)	0.000 (15)
C25	0.0166 (5)	0.0185 (5)	0.0151 (5)	0.0028 (4)	−0.0011 (5)	0.0024 (6)
H25A	0.034 (15)	0.044 (17)	0.021 (16)	0.019 (13)	−0.001 (12)	0.015 (13)
H25B	0.030 (14)	0.050 (17)	0.007 (13)	−0.012 (12)	−0.003 (11)	0.000 (12)
C26	0.0101 (5)	0.0228 (6)	0.0184 (6)	−0.0013 (5)	−0.0011 (4)	−0.0034 (5)
H26A	0.008 (12)	0.028 (15)	0.07 (2)	0.000 (12)	−0.017 (14)	0.006 (15)
H26B	0.031 (16)	0.039 (17)	0.041 (17)	−0.015 (14)	−0.005 (13)	−0.022 (14)
H26C	0.023 (15)	0.07 (2)	0.035 (17)	−0.005 (15)	0.013 (13)	−0.007 (16)
C27	0.0131 (5)	0.0091 (4)	0.0076 (4)	0.0015 (3)	−0.0007 (3)	0.0000 (3)
C28	0.0200 (6)	0.0125 (5)	0.0094 (5)	0.0041 (5)	−0.0029 (4)	−0.0014 (4)
H28A	0.016 (11)	0.018 (11)	0.030 (13)	0.007 (11)	0.008 (11)	−0.008 (11)
C29	0.0261 (7)	0.0169 (5)	0.0102 (5)	0.0083 (5)	−0.0056 (5)	−0.0006 (4)
H29A	0.06 (2)	0.040 (18)	0.028 (15)	0.017 (16)	−0.028 (15)	−0.021 (13)
C30	0.0237 (6)	0.0147 (5)	0.0110 (5)	0.0082 (5)	−0.0030 (4)	0.0012 (4)
H30A	0.05 (2)	0.020 (15)	0.040 (18)	0.014 (14)	0.002 (15)	−0.002 (13)
C31	0.0171 (5)	0.0111 (4)	0.0102 (5)	0.0046 (4)	−0.0011 (4)	0.0007 (4)
H31A	0.048 (19)	0.022 (14)	0.053 (19)	0.021 (14)	−0.007 (16)	−0.021 (13)
C32	0.0117 (5)	0.0084 (4)	0.0084 (4)	0.0018 (4)	−0.0008 (4)	0.0002 (3)
C33	0.0157 (5)	0.0084 (4)	0.0099 (5)	0.0013 (4)	−0.0002 (4)	−0.0005 (4)
H33A	0.013 (11)	0.039 (15)	0.036 (15)	0.018 (10)	−0.012 (14)	−0.013 (16)
H33B	0.044 (15)	0.029 (13)	0.015 (12)	−0.020 (12)	0.008 (15)	−0.012 (12)
C34	0.0134 (5)	0.0107 (5)	0.0104 (5)	0.0011 (4)	0.0005 (4)	−0.0010 (4)
H34A	0.015 (12)	0.031 (15)	0.016 (12)	0.009 (11)	0.002 (10)	−0.004 (11)
C35	0.0140 (5)	0.0104 (5)	0.0133 (5)	−0.0022 (4)	−0.0006 (4)	−0.0016 (4)
H35A	0.050 (19)	0.012 (13)	0.034 (16)	0.005 (12)	−0.009 (14)	0.006 (12)
C36	0.0202 (6)	0.0112 (5)	0.0160 (5)	0.0033 (4)	0.0009 (4)	−0.0008 (5)
H36A	0.039 (17)	0.045 (19)	0.037 (17)	0.012 (15)	0.016 (14)	0.013 (14)
H36B	0.029 (16)	0.034 (18)	0.05 (2)	0.005 (13)	0.019 (15)	−0.020 (15)
H36C	0.06 (2)	0.028 (16)	0.045 (19)	−0.007 (15)	−0.019 (16)	−0.001 (14)
C37	0.0220 (6)	0.0173 (6)	0.0129 (5)	−0.0012 (5)	0.0037 (5)	−0.0005 (4)
H37A	0.032 (18)	0.07 (3)	0.06 (2)	0.009 (18)	0.037 (16)	−0.002 (19)
H37B	0.08 (2)	0.007 (12)	0.047 (19)	0.005 (15)	0.024 (18)	0.000 (12)
H37C	0.035 (16)	0.034 (16)	0.020 (14)	−0.004 (13)	0.001 (12)	−0.002 (12)
C38	0.0142 (5)	0.0178 (6)	0.0177 (6)	−0.0041 (5)	0.0013 (5)	−0.0028 (5)
H38A	0.034 (18)	0.034 (18)	0.09 (3)	−0.017 (15)	−0.018 (18)	0.006 (17)
H38B	0.053 (19)	0.019 (14)	0.035 (17)	0.002 (13)	0.001 (15)	−0.003 (13)
H38C	0.029 (16)	0.05 (2)	0.012 (13)	−0.006 (14)	0.001 (12)	−0.008 (13)
C39	0.0188 (6)	0.0199 (6)	0.0137 (6)	−0.0030 (5)	−0.0027 (5)	−0.0039 (5)
H39A	0.05 (2)	0.09 (3)	0.06 (2)	−0.03 (2)	−0.018 (19)	0.00 (2)
H39B	0.036 (18)	0.05 (2)	0.036 (17)	0.018 (15)	0.014 (14)	−0.020 (15)

Geometric parameters (Å, º)

Ni1—H1A	1.67 (4)	C14—C19	1.4327 (17)
Ni1—H1B	1.68 (5)	C15—H15A	1.09 (2)
Ni1—In1	2.4787 (2)	C15—C16	1.3973 (19)
Ni1—P1	2.2832 (4)	C16—H16A	1.09 (2)
Ni1—P2	2.2527 (4)	C16—C17	1.393 (2)
Ni1—P3	2.2505 (4)	C17—H17A	1.08 (3)
H1A—H1B	0.96 (6)	C17—C18	1.3934 (19)
In1—N1	2.1116 (10)	C18—H18A	1.11 (2)
In1—N2	2.1231 (11)	C18—C19	1.4128 (18)
In1—N3	2.1136 (11)	C20—H20A	1.11 (3)
In1—N4	2.3684 (11)	C20—H20B	1.11 (2)
P1—C7	1.8639 (14)	C21—H21A	1.10 (3)
P1—C8	1.8704 (14)	C21—C23	1.529 (2)
P1—C9	1.8648 (14)	C21—C24	1.534 (2)
P2—C20	1.8717 (13)	C22—H22A	1.09 (2)
P2—C21	1.8587 (13)	C22—C25	1.529 (2)
P2—C22	1.8786 (14)	C22—C26	1.5328 (19)
P3—C33	1.8882 (13)	C23—H23A	1.11 (3)
P3—C34	1.8675 (13)	C23—H23B	1.06 (3)
P3—C35	1.8553 (13)	C23—H23C	1.09 (3)
N1—C6	1.3659 (18)	C24—H24A	1.12 (3)
N1—C7	1.4422 (18)	C24—H24B	1.05 (2)
N2—C19	1.3663 (16)	C24—H24C	1.09 (3)
N2—C20	1.4466 (17)	C25—H25A	1.10 (2)
N3—C32	1.3702 (16)	C25—H25B	1.08 (2)
N3—C33	1.4415 (16)	C25—H25C	1.08 (3)
N4—C1	1.4631 (16)	C26—H26A	1.09 (2)
N4—C14	1.4566 (16)	C26—H26B	1.06 (2)
N4—C27	1.4625 (16)	C26—H26C	1.06 (3)
C1—C2	1.3870 (17)	C27—C28	1.3854 (17)
C1—C6	1.4304 (18)	C27—C32	1.4287 (17)
C2—H2A	1.07 (2)	C28—H28A	1.08 (2)
C2—C3	1.4008 (19)	C28—C29	1.3988 (19)
C3—H3A	1.07 (3)	C29—H29A	1.06 (3)
C3—C4	1.394 (2)	C29—C30	1.389 (2)
C4—H4A	1.07 (2)	C30—H30A	1.08 (3)
C4—C5	1.3926 (19)	C30—C31	1.3925 (19)
C5—H5A	1.08 (2)	C31—H31A	1.05 (2)
C5—C6	1.4123 (19)	C31—C32	1.4095 (17)
C7—H7A	1.09 (2)	C33—H33A	1.10 (2)
C7—H7B	1.11 (3)	C33—H33B	1.09 (2)
C8—H8A	1.11 (3)	C34—H34A	1.10 (2)
C8—C10	1.536 (2)	C34—C36	1.5322 (19)
C8—C11	1.530 (2)	C34—C37	1.531 (2)
C9—H9A	1.11 (3)	C35—H35A	1.09 (2)
C9—C12	1.534 (2)	C35—C38	1.535 (2)
C9—C13	1.527 (2)	C35—C39	1.532 (2)
C10—H10A	1.08 (3)	C36—H36A	1.07 (3)
C10—H10B	1.10 (3)	C36—H36B	1.09 (3)
C10—H10C	1.12 (3)	C36—H36C	1.10 (3)
C11—H11A	1.05 (3)	C37—H37A	1.07 (3)
C11—H11B	1.04 (3)	C37—H37B	1.06 (2)
C11—H11C	1.09 (3)	C37—H37C	1.06 (3)
C12—H12A	1.07 (3)	C38—H38A	1.05 (3)
C12—H12B	1.11 (3)	C38—H38B	1.07 (3)
C12—H12C	1.09 (3)	C38—H38C	1.10 (2)
C13—H13A	1.07 (3)	C39—H39A	1.08 (3)
C13—H13B	1.12 (3)	C39—H39B	1.06 (2)
C13—H13C	1.08 (3)	C39—H39C	1.09 (3)
C14—C15	1.3864 (17)
H1B—Ni1—H1A	33.3 (19)	C15—C14—N4	121.38 (11)
In1—Ni1—H1A	161.8 (14)	C19—C14—N4	117.97 (10)
In1—Ni1—H1B	162.4 (17)	C19—C14—C15	120.62 (11)
P1—Ni1—H1A	90.2 (13)	H15A—C15—C14	118.4 (12)
P1—Ni1—H1B	94.1 (17)	C16—C15—C14	121.57 (12)
P1—Ni1—In1	81.131 (10)	C16—C15—H15A	120.0 (12)
P2—Ni1—H1A	89.0 (14)	H16A—C16—C15	120.3 (14)
P2—Ni1—H1B	114.0 (18)	C17—C16—C15	118.58 (12)
P2—Ni1—In1	82.397 (10)	C17—C16—H16A	121.1 (14)
P2—Ni1—P1	122.760 (14)	H17A—C17—C16	119.6 (14)
P3—Ni1—H1A	113.6 (14)	C18—C17—C16	120.85 (12)
P3—Ni1—H1B	83.3 (16)	C18—C17—H17A	119.5 (14)
P3—Ni1—In1	84.553 (10)	H18A—C18—C17	121.0 (14)
P3—Ni1—P1	120.206 (14)	C19—C18—C17	121.59 (13)
P3—Ni1—P2	112.148 (14)	C19—C18—H18A	117.4 (14)
H1B—H1A—Ni1	74 (4)	C14—C19—N2	118.78 (11)
H1A—H1B—Ni1	72 (4)	C18—C19—N2	124.42 (12)
N1—In1—Ni1	104.64 (4)	C18—C19—C14	116.79 (11)
N2—In1—Ni1	102.76 (3)	N2—C20—P2	108.35 (9)
N2—In1—N1	116.47 (4)	H20A—C20—P2	108.1 (15)
N3—In1—Ni1	103.29 (3)	H20A—C20—N2	114.1 (14)
N3—In1—N1	111.74 (4)	H20B—C20—P2	109.7 (13)
N3—In1—N2	115.83 (4)	H20B—C20—N2	111.4 (15)
N4—In1—Ni1	178.63 (3)	H20B—C20—H20A	105.0 (19)
N4—In1—N1	76.60 (4)	H21A—C21—P2	106.8 (14)
N4—In1—N2	76.10 (4)	C23—C21—P2	112.38 (10)
N4—In1—N3	76.66 (4)	C23—C21—H21A	107.4 (15)
C7—P1—Ni1	117.45 (5)	C24—C21—P2	110.11 (10)
C8—P1—Ni1	110.55 (5)	C24—C21—H21A	110.2 (13)
C8—P1—C7	103.35 (6)	C24—C21—C23	109.94 (12)
C9—P1—Ni1	116.58 (5)	H22A—C22—P2	105.3 (15)
C9—P1—C7	102.07 (6)	C25—C22—P2	111.00 (9)
C9—P1—C8	105.34 (6)	C25—C22—H22A	109.5 (14)
C20—P2—Ni1	117.98 (4)	C26—C22—P2	115.82 (10)
C21—P2—Ni1	114.42 (4)	C26—C22—H22A	105.9 (15)
C21—P2—C20	102.59 (6)	C26—C22—C25	109.01 (12)
C22—P2—Ni1	117.37 (4)	H23A—C23—C21	110.4 (16)
C22—P2—C20	100.52 (6)	H23B—C23—C21	112.3 (14)
C22—P2—C21	101.40 (6)	H23B—C23—H23A	106 (2)
C33—P3—Ni1	118.84 (4)	H23C—C23—C21	108.4 (16)
C34—P3—Ni1	112.78 (4)	H23C—C23—H23A	108 (2)
C34—P3—C33	99.08 (6)	H23C—C23—H23B	111 (2)
C35—P3—Ni1	118.83 (5)	H24A—C24—C21	113.7 (14)
C35—P3—C33	99.64 (6)	H24B—C24—C21	109.5 (15)
C35—P3—C34	104.90 (6)	H24B—C24—H24A	111 (2)
C6—N1—In1	112.96 (9)	H24C—C24—C21	111.0 (16)
C7—N1—In1	115.67 (9)	H24C—C24—H24A	105 (2)
C7—N1—C6	119.52 (10)	H24C—C24—H24B	107 (2)
C19—N2—In1	113.02 (8)	H25A—C25—C22	110.1 (13)
C20—N2—In1	118.00 (8)	H25B—C25—C22	115.3 (13)
C20—N2—C19	120.70 (11)	H25B—C25—H25A	107 (2)
C32—N3—In1	113.21 (8)	H25C—C25—C22	109.2 (15)
C33—N3—In1	118.69 (8)	H25C—C25—H25A	108 (2)
C33—N3—C32	119.57 (10)	H25C—C25—H25B	107 (2)
C1—N4—In1	103.17 (7)	H26A—C26—C22	108.7 (13)
C14—N4—In1	103.43 (7)	H26B—C26—C22	111.0 (15)
C14—N4—C1	115.87 (10)	H26B—C26—H26A	109 (2)
C27—N4—In1	102.62 (7)	H26C—C26—C22	113.7 (15)
C27—N4—C1	113.53 (10)	H26C—C26—H26A	105 (2)
C27—N4—C14	115.70 (10)	H26C—C26—H26B	109 (2)
C2—C1—N4	121.39 (11)	C28—C27—N4	121.09 (11)
C6—C1—N4	117.98 (11)	C32—C27—N4	117.95 (10)
C6—C1—C2	120.56 (11)	C32—C27—C28	120.96 (11)
H2A—C2—C1	119.0 (14)	H28A—C28—C27	118.3 (13)
C3—C2—C1	121.43 (12)	C29—C28—C27	121.14 (12)
C3—C2—H2A	119.5 (14)	C29—C28—H28A	120.6 (13)
H3A—C3—C2	122.6 (16)	H29A—C29—C28	120.3 (15)
C4—C3—C2	118.67 (12)	C30—C29—C28	118.61 (12)
C4—C3—H3A	118.7 (16)	C30—C29—H29A	121.1 (15)
H4A—C4—C3	119.0 (13)	H30A—C30—C29	120.4 (15)
C5—C4—C3	120.72 (12)	C31—C30—C29	121.02 (13)
C5—C4—H4A	120.3 (13)	C31—C30—H30A	118.6 (15)
H5A—C5—C4	119.6 (14)	H31A—C31—C30	117.5 (16)
C6—C5—C4	121.62 (12)	C32—C31—C30	121.49 (12)
C6—C5—H5A	118.7 (14)	C32—C31—H31A	120.9 (16)
C1—C6—N1	119.14 (12)	C27—C32—N3	119.25 (11)
C5—C6—N1	123.86 (12)	C31—C32—N3	124.05 (11)
C5—C6—C1	116.99 (12)	C31—C32—C27	116.70 (11)
N1—C7—P1	108.73 (9)	N3—C33—P3	111.64 (8)
H7A—C7—P1	106.4 (13)	H33A—C33—P3	106.5 (16)
H7A—C7—N1	115.0 (12)	H33A—C33—N3	111.8 (14)
H7B—C7—P1	108.7 (14)	H33B—C33—P3	107.2 (14)
H7B—C7—N1	111.6 (13)	H33B—C33—N3	112.7 (13)
H7B—C7—H7A	106.1 (19)	H33B—C33—H33A	106.6 (19)
H8A—C8—P1	104.1 (14)	H34A—C34—P3	102.9 (12)
C10—C8—P1	117.13 (11)	C36—C34—P3	114.75 (10)
C10—C8—H8A	105.3 (16)	C36—C34—H34A	108.9 (13)
C11—C8—P1	110.54 (11)	C37—C34—P3	113.46 (10)
C11—C8—H8A	107.8 (15)	C37—C34—H34A	105.3 (12)
C11—C8—C10	111.23 (14)	C37—C34—C36	110.67 (11)
H9A—C9—P1	104.5 (13)	H35A—C35—P3	104.8 (15)
C12—C9—P1	109.97 (9)	C38—C35—P3	108.57 (9)
C12—C9—H9A	108.9 (13)	C38—C35—H35A	109.0 (15)
C13—C9—P1	116.65 (11)	C39—C35—P3	113.34 (10)
C13—C9—H9A	107.7 (15)	C39—C35—H35A	109.2 (14)
C13—C9—C12	108.84 (13)	C39—C35—C38	111.61 (12)
H10A—C10—C8	111.3 (19)	H36A—C36—C34	111.6 (16)
H10B—C10—C8	113.1 (17)	H36B—C36—C34	110.4 (15)
H10B—C10—H10A	108 (3)	H36B—C36—H36A	109 (2)
H10C—C10—C8	109.1 (16)	H36C—C36—C34	111.0 (15)
H10C—C10—H10A	109 (3)	H36C—C36—H36A	108 (2)
H10C—C10—H10B	106 (2)	H36C—C36—H36B	106 (2)
H11A—C11—C8	110 (2)	H37A—C37—C34	110.3 (18)
H11B—C11—C8	111.7 (17)	H37B—C37—C34	112.8 (15)
H11B—C11—H11A	104 (3)	H37B—C37—H37A	107 (3)
H11C—C11—C8	114.6 (19)	H37C—C37—C34	110.7 (14)
H11C—C11—H11A	110 (3)	H37C—C37—H37A	107 (2)
H11C—C11—H11B	106 (3)	H37C—C37—H37B	109 (2)
H12A—C12—C9	108.9 (15)	H38A—C38—C35	110.7 (19)
H12B—C12—C9	111.3 (14)	H38B—C38—C35	110.1 (15)
H12B—C12—H12A	108 (2)	H38B—C38—H38A	111 (2)
H12C—C12—C9	108.7 (16)	H38C—C38—C35	110.9 (14)
H12C—C12—H12A	111 (2)	H38C—C38—H38A	106 (2)
H12C—C12—H12B	109 (2)	H38C—C38—H38B	108 (2)
H13A—C13—C9	110.4 (17)	H39A—C39—C35	111.1 (19)
H13B—C13—C9	111.1 (15)	H39B—C39—C35	113.2 (16)
H13B—C13—H13A	107 (2)	H39B—C39—H39A	105 (3)
H13C—C13—C9	113.9 (19)	H39C—C39—C35	111.0 (15)
H13C—C13—H13A	107 (2)	H39C—C39—H39A	110 (3)
H13C—C13—H13B	107 (3)	H39C—C39—H39B	107 (2)
In1—N1—C6—C1	−26.68 (9)	N2—C19—C18—C17	−179.33 (14)
In1—N1—C6—C5	152.14 (9)	N3—C32—C27—N4	−4.31 (14)
In1—N1—C7—P1	29.28 (6)	N3—C32—C27—C28	176.51 (12)
In1—N2—C19—C14	−26.52 (10)	N3—C32—C31—C30	−178.37 (14)
In1—N2—C19—C18	152.16 (9)	N4—C1—C2—C3	177.54 (12)
In1—N2—C20—P2	23.11 (8)	N4—C1—C6—C5	−176.85 (11)
In1—N3—C32—C27	−22.21 (10)	N4—C14—C15—C16	178.52 (12)
In1—N3—C32—C31	157.51 (9)	N4—C14—C19—C18	−177.85 (11)
In1—N3—C33—P3	14.30 (8)	N4—C27—C28—C29	−176.44 (13)
In1—N4—C1—C2	−157.31 (8)	N4—C27—C32—C31	175.96 (12)
In1—N4—C1—C6	19.60 (8)	C1—C2—C3—C4	−1.13 (15)
In1—N4—C14—C15	−157.01 (8)	C1—C6—C5—C4	−0.45 (14)
In1—N4—C14—C19	21.05 (8)	C2—C3—C4—C5	0.76 (16)
In1—N4—C27—C28	−156.75 (9)	C3—C4—C5—C6	0.03 (16)
In1—N4—C27—C32	24.07 (8)	C14—C15—C16—C17	−0.86 (16)
P1—C7—N1—C6	169.60 (8)	C14—C19—C18—C17	−0.62 (14)
P2—C20—N2—C19	169.29 (8)	C15—C16—C17—C18	0.46 (16)
P3—C33—N3—C32	160.12 (9)	C16—C17—C18—C19	0.29 (18)
N1—C6—C1—N4	2.06 (13)	C27—C28—C29—C30	−0.19 (18)
N1—C6—C1—C2	178.99 (12)	C27—C32—C31—C30	1.35 (15)
N1—C6—C5—C4	−179.30 (13)	C28—C29—C30—C31	−1.70 (19)
N2—C19—C14—N4	0.93 (13)	C29—C30—C31—C32	1.09 (19)
N2—C19—C14—C15	179.01 (12)

(GOJNIF_HAR_NoMoRe_1)

Crystal data

C39H62InN4NiP3	Dx = 1.415 Mg m^−3
Mr = 853.39	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, P212121	Cell parameters from 9537 reflections
a = 12.2127 (4) Å	θ = 2.3–36.4°
b = 14.5402 (5) Å	µ = 1.20 mm^−1
c = 22.5601 (8) Å	T = 100 K
V = 4006.1 (2) Å^3	Block, gold
Z = 4	0.14 × 0.08 × 0.06 mm
F(000) = 1784.150

Data collection

Bruker Photon-II CMOS diffractometer	18741 reflections with I ≥ 2u(I)
φ and ω scans	Rint = 0.036
Absorption correction: multi-scan SADABS. R.Blessing, 1995	θmax = 36.4°, θmin = 2.3°
Tmin = 0.701, Tmax = 0.747	h = −20→20
237431 measured reflections	k = −24→24
19473 independent reflections	l = −37→37

Refinement

Refinement on F^2	0 constraints
Least-squares matrix: full	Only H-atom coordinates refined
R[F^2 > 2σ(F^2)] = 0.016	w = 1/[σ^2(Fo^2) + (0.0103P)^2 + 0.7427P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.031	(Δ/σ)max = 0.0002
S = 1.05	Δρmax = 0.35 e Å^−3
19473 reflections	Δρmin = −0.50 e Å^−3
619 parameters	Absolute structure: Flack, H. D. (1983). Acta Cryst. A39, 876-881.
0 restraints	Absolute structure parameter: 0.004 (5)

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ni1	0.755816 (8)	0.598648 (6)	0.856146 (5)	0.009166 (17)
H1A	0.7290 (15)	0.5718 (13)	0.9262 (7)	0.036333
H1B	0.7578 (17)	0.6349 (12)	0.9268 (7)	0.035000
In1	0.798238 (4)	0.580829 (3)	0.749320 (3)	0.008179 (9)
P1	0.918447 (17)	0.522247 (14)	0.864340 (9)	0.00922 (3)
P2	0.599033 (17)	0.528563 (14)	0.829176 (9)	0.00932 (3)
P3	0.753610 (18)	0.750099 (14)	0.835675 (9)	0.00903 (3)
N1	0.96176 (5)	0.53380 (4)	0.74725 (4)	0.01081 (10)
N2	0.67664 (6)	0.48665 (5)	0.72035 (3)	0.01129 (12)
N3	0.78426 (6)	0.71631 (4)	0.71617 (3)	0.01057 (11)
N4	0.83423 (5)	0.56340 (4)	0.64679 (3)	0.00877 (10)
C1	0.95347 (6)	0.57173 (5)	0.64335 (3)	0.00949 (11)
C2	1.00529 (7)	0.59714 (6)	0.59112 (4)	0.01272 (13)
H2A	0.9563 (12)	0.6122 (10)	0.5535 (6)	0.028000
C3	1.11899 (7)	0.60859 (6)	0.58834 (4)	0.01462 (14)
H3A	1.1602 (12)	0.6282 (11)	0.5483 (6)	0.032000
C4	1.18035 (6)	0.59548 (6)	0.63979 (4)	0.01414 (14)
H4A	1.2687 (11)	0.6061 (10)	0.6382 (6)	0.030333
C5	1.12980 (6)	0.57045 (6)	0.69272 (4)	0.01235 (13)
H5A	1.1800 (11)	0.5618 (10)	0.7326 (6)	0.027667
C6	1.01533 (7)	0.55740 (6)	0.69641 (4)	0.00980 (13)
C7	1.01950 (7)	0.53659 (6)	0.80306 (4)	0.01149 (14)
H7A	1.0637 (12)	0.6015 (10)	0.8121 (6)	0.028000
H7B	1.0815 (12)	0.4811 (10)	0.8056 (6)	0.029000
C8	0.99545 (7)	0.56226 (6)	0.93121 (4)	0.01421 (14)
H8A	0.9795 (12)	0.6371 (10)	0.9324 (6)	0.027667
C9	0.91074 (7)	0.39464 (6)	0.87150 (4)	0.01382 (14)
H9A	0.8498 (12)	0.3827 (10)	0.9076 (6)	0.029000
C10	1.12036 (8)	0.55054 (8)	0.93050 (5)	0.02230 (19)
H10A	1.1449 (14)	0.4788 (12)	0.9259 (8)	0.049667
H10B	1.1554 (13)	0.5777 (15)	0.9727 (7)	0.051667
H10C	1.1594 (13)	0.5875 (13)	0.8930 (7)	0.041333
C11	0.94543 (10)	0.52162 (9)	0.98766 (4)	0.0271 (2)
H11A	0.9812 (15)	0.5542 (12)	1.0261 (7)	0.042000
H11B	0.9552 (13)	0.4465 (13)	0.9908 (7)	0.046333
H11C	0.8629 (15)	0.5370 (10)	0.9912 (7)	0.040000
C12	0.86443 (9)	0.35268 (6)	0.81444 (4)	0.01860 (16)
H12A	0.8490 (14)	0.2802 (10)	0.8217 (7)	0.040667
H12B	0.9251 (14)	0.3613 (11)	0.7792 (7)	0.042333
H12C	0.7874 (14)	0.3873 (12)	0.8029 (7)	0.045667
C13	1.01689 (9)	0.34488 (7)	0.88745 (6)	0.0237 (2)
H13A	1.0053 (14)	0.2707 (11)	0.8862 (8)	0.045333
H13B	1.0505 (15)	0.3631 (12)	0.9304 (9)	0.048000
H13C	1.0822 (16)	0.3596 (12)	0.8541 (8)	0.051333
C14	0.78969 (7)	0.47285 (5)	0.63325 (3)	0.01002 (12)
C15	0.82603 (7)	0.42270 (6)	0.58483 (3)	0.01233 (13)
H15A	0.8923 (12)	0.4523 (10)	0.5579 (6)	0.027000
C16	0.78524 (7)	0.33492 (6)	0.57248 (4)	0.01517 (15)
H16A	0.8133 (13)	0.2964 (10)	0.5337 (6)	0.035333
C17	0.70732 (8)	0.29738 (6)	0.61046 (4)	0.01602 (14)
H17A	0.6763 (13)	0.2279 (10)	0.6031 (7)	0.038667
C18	0.67003 (7)	0.34634 (6)	0.65963 (4)	0.01417 (14)
H18A	0.6108 (13)	0.3147 (10)	0.6903 (7)	0.033333
C19	0.70912 (7)	0.43550 (5)	0.67266 (3)	0.01037 (12)
C20	0.60329 (7)	0.44845 (6)	0.76421 (3)	0.01187 (13)
H20A	0.6274 (12)	0.3790 (9)	0.7804 (6)	0.026667
H20B	0.5195 (10)	0.4389 (9)	0.7460 (7)	0.026333
C21	0.53634 (7)	0.45617 (6)	0.88799 (4)	0.01315 (14)
H21A	0.4639 (11)	0.4213 (10)	0.8674 (6)	0.025000
C22	0.48064 (7)	0.60402 (6)	0.80771 (4)	0.01236 (13)
H22A	0.4785 (12)	0.6580 (9)	0.8420 (6)	0.025000
C23	0.61396 (8)	0.38123 (7)	0.91014 (4)	0.02053 (18)
H23A	0.5717 (14)	0.3371 (11)	0.9426 (7)	0.042333
H23B	0.6852 (14)	0.4149 (11)	0.9313 (7)	0.042333
H23C	0.6415 (13)	0.3359 (11)	0.8758 (7)	0.041667
C24	0.49925 (8)	0.51663 (7)	0.93998 (4)	0.01876 (17)
H24A	0.4407 (14)	0.5758 (12)	0.9264 (7)	0.036333
H24B	0.5692 (13)	0.5497 (11)	0.9614 (6)	0.035000
H24C	0.4614 (13)	0.4752 (11)	0.9734 (7)	0.038000
C25	0.49931 (7)	0.64751 (6)	0.74673 (5)	0.01704 (14)
H25A	0.4349 (12)	0.6996 (10)	0.7387 (7)	0.035667
H25B	0.4952 (12)	0.5946 (11)	0.7131 (7)	0.035333
H25C	0.5786 (13)	0.6811 (10)	0.7415 (7)	0.036333
C26	0.36756 (7)	0.55820 (7)	0.80854 (4)	0.01752 (16)
H26A	0.3053 (12)	0.6090 (10)	0.7960 (7)	0.036000
H26B	0.3449 (12)	0.5314 (11)	0.8522 (7)	0.037333
H26C	0.3630 (12)	0.5018 (11)	0.7775 (6)	0.034667
C27	0.77595 (6)	0.64129 (5)	0.62074 (3)	0.01012 (13)
C28	0.74256 (8)	0.64003 (6)	0.56205 (4)	0.01431 (14)
H28A	0.7562 (13)	0.5766 (10)	0.5369 (6)	0.029333
C29	0.69218 (8)	0.71649 (6)	0.53616 (4)	0.01813 (16)
H29A	0.6692 (14)	0.7148 (10)	0.4907 (6)	0.038333
C30	0.67548 (8)	0.79432 (6)	0.57071 (4)	0.01677 (16)
H30A	0.6390 (14)	0.8561 (10)	0.5524 (6)	0.036333
C31	0.70550 (7)	0.79597 (5)	0.63025 (3)	0.01309 (13)
H31A	0.6908 (13)	0.8577 (9)	0.6537 (6)	0.029333
C32	0.75541 (7)	0.71942 (5)	0.65749 (3)	0.00988 (12)
C33	0.74815 (7)	0.78803 (5)	0.75568 (4)	0.01164 (12)
H33A	0.6632 (10)	0.8093 (9)	0.7458 (7)	0.026667
H33B	0.7982 (11)	0.8500 (8)	0.7517 (7)	0.028333
C34	0.62751 (7)	0.80867 (5)	0.86342 (4)	0.01183 (13)
H34A	0.5632 (11)	0.7828 (10)	0.8330 (6)	0.026000
C35	0.86864 (7)	0.82275 (6)	0.86200 (4)	0.01279 (13)
H35A	0.8494 (12)	0.8932 (9)	0.8470 (6)	0.028000
C36	0.63052 (7)	0.91393 (6)	0.85997 (4)	0.01616 (14)
H36A	0.6590 (13)	0.9383 (10)	0.8174 (6)	0.036000
H36B	0.6865 (13)	0.9422 (10)	0.8952 (7)	0.037333
H36C	0.5486 (13)	0.9427 (10)	0.8683 (7)	0.036000
C37	0.59270 (8)	0.77705 (7)	0.92536 (4)	0.01775 (16)
H37A	0.5123 (13)	0.8041 (11)	0.9364 (7)	0.036333
H37B	0.6501 (13)	0.8007 (10)	0.9576 (7)	0.032667
H37C	0.5858 (13)	0.7038 (11)	0.9291 (6)	0.036000
C38	0.97436 (7)	0.78993 (7)	0.83201 (4)	0.01691 (15)
H38A	1.0371 (13)	0.8418 (11)	0.8360 (8)	0.041000
H38B	0.9612 (13)	0.7792 (11)	0.7842 (7)	0.042000
H38C	1.0018 (13)	0.7242 (11)	0.8526 (7)	0.036000
C39	0.88001 (8)	0.82429 (7)	0.92964 (4)	0.01780 (16)
H39A	0.9557 (15)	0.8575 (12)	0.9433 (7)	0.043333
H39B	0.8770 (13)	0.7537 (12)	0.9476 (7)	0.040000
H39C	0.8159 (15)	0.8629 (11)	0.9514 (7)	0.038000

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ni1	0.00830 (4)	0.00808 (4)	0.01113 (4)	−0.00033 (3)	0.00037 (3)	0.00003 (3)
H1A	0.046000	0.039000	0.024000	−0.010000	0.003000	0.006000
H1B	0.049000	0.033000	0.023000	0.002000	−0.001000	−0.005000
In1	0.008364 (17)	0.007714 (17)	0.008460 (17)	0.000107 (15)	0.000162 (19)	−0.000133 (19)
P1	0.00994 (8)	0.00943 (8)	0.00829 (8)	0.00074 (6)	−0.00068 (6)	0.00063 (6)
P2	0.00855 (8)	0.01072 (8)	0.00868 (8)	−0.00177 (6)	0.00046 (6)	−0.00032 (6)
P3	0.01089 (8)	0.00767 (7)	0.00853 (7)	−0.00017 (7)	−0.00057 (7)	−0.00087 (6)
N1	0.0095 (2)	0.0137 (2)	0.0093 (2)	0.00094 (19)	−0.0002 (2)	0.0011 (3)
N2	0.0118 (3)	0.0116 (3)	0.0105 (3)	−0.0022 (2)	0.0014 (2)	−0.0027 (2)
N3	0.0142 (3)	0.0091 (2)	0.0085 (2)	0.0015 (2)	−0.0007 (2)	0.0000 (2)
N4	0.0103 (2)	0.0087 (3)	0.0073 (2)	0.0009 (2)	−0.0007 (2)	0.0001 (2)
C1	0.0101 (3)	0.0100 (3)	0.0084 (3)	0.0004 (2)	0.0012 (2)	−0.0002 (2)
C2	0.0142 (3)	0.0134 (3)	0.0105 (3)	−0.0001 (3)	0.0024 (2)	0.0007 (3)
H2A	0.027000	0.039000	0.018000	0.000000	−0.002000	0.005000
C3	0.0148 (3)	0.0158 (3)	0.0132 (3)	−0.0010 (3)	0.0044 (3)	0.0012 (3)
H3A	0.029000	0.045000	0.022000	−0.005000	0.009000	0.007000
C4	0.0114 (3)	0.0153 (3)	0.0157 (3)	−0.0008 (3)	0.0036 (3)	0.0006 (3)
H4A	0.017000	0.041000	0.033000	−0.004000	0.004000	0.002000
C5	0.0099 (3)	0.0148 (3)	0.0124 (3)	0.0002 (3)	0.0007 (2)	0.0005 (3)
H5A	0.020000	0.040000	0.023000	0.000000	−0.003000	0.004000
C6	0.0095 (3)	0.0108 (3)	0.0091 (3)	0.0008 (2)	0.0011 (2)	0.0001 (2)
C7	0.0101 (3)	0.0144 (4)	0.0099 (3)	0.0014 (3)	−0.0003 (2)	0.0008 (3)
H7A	0.026000	0.031000	0.027000	−0.009000	−0.001000	0.001000
H7B	0.024000	0.034000	0.029000	0.013000	0.001000	0.005000
C8	0.0159 (4)	0.0164 (4)	0.0104 (3)	−0.0014 (3)	−0.0020 (3)	−0.0003 (3)
H8A	0.034000	0.019000	0.030000	−0.001000	−0.004000	0.002000
C9	0.0149 (3)	0.0106 (3)	0.0159 (3)	0.0014 (3)	−0.0006 (3)	0.0025 (3)
H9A	0.033000	0.024000	0.030000	0.001000	0.010000	0.006000
C10	0.0167 (4)	0.0292 (5)	0.0209 (4)	0.0006 (4)	−0.0078 (3)	−0.0034 (4)
H10A	0.031000	0.046000	0.072000	0.013000	−0.009000	−0.015000
H10B	0.028000	0.089000	0.038000	−0.013000	0.001000	0.021000
H10C	0.031000	0.061000	0.032000	−0.004000	−0.011000	−0.008000
C11	0.0340 (6)	0.0353 (6)	0.0120 (4)	−0.0098 (5)	0.0003 (4)	0.0006 (4)
H11A	0.059000	0.047000	0.020000	−0.014000	−0.007000	−0.000000
H11B	0.029000	0.071000	0.039000	0.009000	0.010000	0.020000
H11C	0.063000	0.023000	0.034000	−0.002000	0.002000	0.008000
C12	0.0242 (4)	0.0114 (3)	0.0202 (4)	−0.0006 (3)	−0.0017 (3)	−0.0018 (3)
H12A	0.057000	0.016000	0.049000	−0.003000	−0.005000	−0.002000
H12B	0.038000	0.032000	0.057000	0.009000	−0.021000	−0.009000
H12C	0.052000	0.052000	0.033000	−0.012000	0.015000	−0.011000
C13	0.0203 (4)	0.0144 (4)	0.0364 (6)	0.0055 (3)	−0.0056 (4)	0.0050 (4)
H13A	0.049000	0.019000	0.068000	0.009000	−0.010000	0.004000
H13B	0.027000	0.044000	0.073000	0.011000	0.008000	0.007000
H13C	0.058000	0.044000	0.052000	0.018000	−0.027000	−0.004000
C14	0.0121 (3)	0.0091 (3)	0.0088 (3)	0.0011 (2)	0.0001 (2)	−0.0014 (2)
C15	0.0153 (3)	0.0117 (3)	0.0101 (3)	0.0002 (3)	0.0012 (2)	−0.0022 (3)
H15A	0.028000	0.029000	0.024000	−0.001000	0.009000	−0.002000
C16	0.0187 (4)	0.0131 (3)	0.0137 (3)	−0.0007 (3)	0.0009 (3)	−0.0060 (3)
H16A	0.041000	0.034000	0.031000	−0.001000	0.009000	−0.018000
C17	0.0184 (4)	0.0125 (3)	0.0172 (4)	−0.0028 (3)	0.0008 (3)	−0.0056 (3)
H17A	0.046000	0.026000	0.044000	−0.014000	0.007000	−0.017000
C18	0.0144 (3)	0.0124 (3)	0.0158 (4)	−0.0031 (3)	0.0016 (3)	−0.0041 (3)
H18A	0.037000	0.030000	0.033000	−0.015000	0.011000	−0.006000
C19	0.0106 (3)	0.0101 (3)	0.0104 (3)	−0.0007 (2)	0.0002 (2)	−0.0024 (2)
C20	0.0111 (3)	0.0124 (3)	0.0121 (3)	−0.0028 (3)	0.0014 (2)	−0.0020 (2)
H20A	0.032000	0.018000	0.030000	−0.000000	0.005000	0.003000
H20B	0.018000	0.035000	0.026000	−0.006000	−0.002000	−0.005000
C21	0.0131 (3)	0.0156 (3)	0.0108 (3)	−0.0038 (3)	0.0009 (3)	0.0012 (3)
H21A	0.023000	0.027000	0.025000	−0.008000	−0.001000	−0.002000
C22	0.0097 (3)	0.0155 (3)	0.0119 (3)	0.0004 (3)	0.0002 (2)	−0.0020 (3)
H22A	0.028000	0.023000	0.024000	0.000000	−0.001000	−0.007000
C23	0.0205 (4)	0.0223 (4)	0.0189 (4)	0.0001 (3)	0.0022 (3)	0.0076 (3)
H23A	0.045000	0.038000	0.044000	0.002000	0.011000	0.023000
H23B	0.053000	0.038000	0.036000	0.018000	0.007000	0.001000
H23C	0.031000	0.049000	0.045000	0.001000	−0.012000	0.008000
C24	0.0240 (4)	0.0220 (4)	0.0103 (3)	−0.0059 (3)	0.0030 (3)	−0.0014 (3)
H24A	0.047000	0.034000	0.028000	0.013000	0.002000	−0.001000
H24B	0.045000	0.036000	0.024000	−0.010000	0.012000	0.005000
H24C	0.035000	0.051000	0.028000	−0.017000	0.000000	−0.011000
C25	0.0169 (3)	0.0189 (3)	0.0153 (4)	0.0028 (3)	−0.0010 (3)	0.0018 (4)
H25A	0.033000	0.038000	0.036000	0.014000	−0.001000	0.010000
H25B	0.025000	0.044000	0.037000	−0.009000	0.000000	0.013000
H25C	0.054000	0.034000	0.021000	−0.000000	0.000000	−0.005000
C26	0.0106 (3)	0.0233 (4)	0.0186 (4)	−0.0014 (3)	−0.0011 (3)	−0.0036 (3)
H26A	0.021000	0.038000	0.049000	0.006000	−0.005000	0.007000
H26B	0.031000	0.039000	0.042000	−0.008000	−0.001000	−0.018000
H26C	0.027000	0.049000	0.028000	−0.007000	0.004000	0.008000
C27	0.0132 (3)	0.0094 (3)	0.0078 (3)	0.0014 (2)	−0.0007 (2)	0.0000 (2)
C28	0.0204 (4)	0.0131 (3)	0.0094 (3)	0.0043 (3)	−0.0032 (3)	−0.0013 (2)
H28A	0.043000	0.024000	0.021000	0.010000	−0.003000	−0.006000
C29	0.0268 (4)	0.0171 (4)	0.0105 (3)	0.0086 (3)	−0.0056 (3)	−0.0006 (3)
H29A	0.062000	0.035000	0.018000	0.016000	−0.011000	−0.000000
C30	0.0240 (4)	0.0153 (4)	0.0111 (3)	0.0084 (3)	−0.0028 (3)	0.0011 (3)
H30A	0.057000	0.025000	0.027000	0.018000	−0.006000	0.006000
C31	0.0173 (3)	0.0115 (3)	0.0105 (3)	0.0048 (3)	−0.0010 (3)	0.0006 (2)
H31A	0.044000	0.018000	0.026000	0.009000	−0.002000	−0.003000
C32	0.0123 (3)	0.0086 (3)	0.0088 (3)	0.0015 (3)	−0.0009 (2)	0.0001 (2)
C33	0.0162 (3)	0.0087 (2)	0.0101 (3)	0.0013 (2)	−0.0001 (3)	−0.0004 (2)
H33A	0.026000	0.028000	0.026000	0.011000	−0.002000	−0.002000
H33B	0.039000	0.017000	0.029000	−0.007000	0.002000	−0.000000
C34	0.0137 (3)	0.0112 (3)	0.0106 (3)	0.0013 (2)	0.0006 (3)	−0.0010 (3)
H34A	0.023000	0.029000	0.026000	0.000000	−0.005000	−0.005000
C35	0.0144 (3)	0.0108 (3)	0.0133 (3)	−0.0023 (3)	−0.0006 (3)	−0.0015 (3)
H35A	0.033000	0.017000	0.034000	−0.002000	−0.002000	−0.000000
C36	0.0206 (4)	0.0116 (3)	0.0162 (3)	0.0035 (3)	0.0009 (3)	−0.0008 (3)
H36A	0.052000	0.028000	0.028000	0.003000	0.010000	0.006000
H36B	0.034000	0.028000	0.050000	0.012000	0.009000	−0.000000
H36C	0.047000	0.024000	0.037000	−0.004000	−0.008000	−0.007000
C37	0.0221 (4)	0.0176 (4)	0.0136 (4)	−0.0014 (3)	0.0036 (3)	−0.0004 (3)
H37A	0.033000	0.038000	0.038000	0.012000	0.014000	0.002000
H37B	0.042000	0.019000	0.037000	−0.002000	0.009000	0.001000
H37C	0.043000	0.042000	0.023000	−0.009000	−0.004000	−0.001000
C38	0.0146 (4)	0.0182 (4)	0.0179 (4)	−0.0040 (3)	0.0011 (3)	−0.0027 (3)
H38A	0.027000	0.044000	0.052000	−0.016000	0.005000	−0.011000
H38B	0.039000	0.038000	0.049000	0.014000	0.009000	0.016000
H38C	0.033000	0.051000	0.024000	0.001000	0.001000	−0.007000
C39	0.0190 (4)	0.0203 (4)	0.0142 (4)	−0.0029 (3)	−0.0026 (3)	−0.0041 (3)
H39A	0.035000	0.060000	0.035000	−0.021000	−0.007000	−0.009000
H39B	0.040000	0.048000	0.032000	0.006000	0.004000	−0.013000
H39C	0.051000	0.034000	0.029000	−0.003000	−0.005000	0.005000

Geometric parameters (Å, º)

Ni1—H1A	1.660 (16)	C14—C19	1.4330 (11)
Ni1—H1B	1.680 (16)	C15—H15A	1.099 (14)
Ni1—In1	2.4787 (1)	C15—C16	1.3982 (12)
Ni1—P1	2.2832 (2)	C16—H16A	1.094 (14)
Ni1—P2	2.2528 (2)	C16—C17	1.3920 (13)
Ni1—P3	2.2502 (2)	C17—H17A	1.091 (14)
H1A—H1B	0.98 (2)	C17—C18	1.3945 (12)
In1—N1	2.1114 (6)	C18—H18A	1.101 (14)
In1—N2	2.1231 (7)	C18—C19	1.4124 (11)
In1—N3	2.1141 (7)	C20—H20A	1.113 (14)
In1—N4	2.3681 (7)	C20—H20B	1.112 (12)
P1—C7	1.8649 (9)	C21—H21A	1.120 (13)
P1—C8	1.8706 (9)	C21—C23	1.5283 (13)
P1—C9	1.8648 (8)	C21—C24	1.5342 (13)
P2—C20	1.8728 (8)	C22—H22A	1.103 (13)
P2—C21	1.8587 (8)	C22—C25	1.5312 (14)
P2—C22	1.8786 (8)	C22—C26	1.5334 (12)
P3—C33	1.8882 (8)	C23—H23A	1.102 (15)
P3—C34	1.8678 (8)	C23—H23B	1.107 (18)
P3—C35	1.8553 (8)	C23—H23C	1.072 (17)
N1—C6	1.3643 (11)	C24—H24A	1.160 (16)
N1—C7	1.4437 (11)	C24—H24B	1.093 (16)
N2—C19	1.3668 (10)	C24—H24C	1.071 (16)
N2—C20	1.4457 (10)	C25—H25A	1.107 (13)
N3—C32	1.3708 (10)	C25—H25B	1.081 (16)
N3—C33	1.4410 (10)	C25—H25C	1.090 (15)
N4—C1	1.4633 (10)	C26—H26A	1.096 (14)
N4—C14	1.4569 (10)	C26—H26B	1.094 (16)
N4—C27	1.4611 (10)	C26—H26C	1.079 (16)
C1—C2	1.3876 (11)	C27—C28	1.3854 (11)
C1—C6	1.4307 (11)	C27—C32	1.4285 (11)
C2—H2A	1.061 (13)	C28—H28A	1.096 (13)
C2—C3	1.4000 (12)	C28—C29	1.3985 (12)
C3—H3A	1.073 (13)	C29—H29A	1.063 (14)
C3—C4	1.3947 (12)	C29—C30	1.3890 (13)
C4—H4A	1.091 (13)	C30—H30A	1.084 (14)
C4—C5	1.3927 (11)	C30—C31	1.3925 (12)
C5—H5A	1.097 (13)	C31—H31A	1.057 (13)
C5—C6	1.4133 (11)	C31—C32	1.4101 (11)
C7—H7A	1.106 (14)	C33—H33A	1.106 (12)
C7—H7B	1.108 (14)	C33—H33B	1.093 (12)
C8—H8A	1.105 (14)	C34—H34A	1.109 (13)
C8—C10	1.5350 (13)	C34—C36	1.5328 (12)
C8—C11	1.5311 (14)	C34—C37	1.5313 (12)
C9—H9A	1.116 (14)	C35—H35A	1.104 (13)
C9—C12	1.5328 (13)	C35—C38	1.5340 (13)
C9—C13	1.5276 (13)	C35—C39	1.5324 (13)
C10—H10A	1.090 (16)	C36—H36A	1.081 (14)
C10—H10B	1.116 (17)	C36—H36B	1.125 (17)
C10—H10C	1.110 (17)	C36—H36C	1.101 (16)
C11—H11A	1.080 (15)	C37—H37A	1.086 (15)
C11—H11B	1.101 (18)	C37—H37B	1.067 (16)
C11—H11C	1.035 (17)	C37—H37C	1.072 (16)
C12—H12A	1.083 (14)	C38—H38A	1.080 (15)
C12—H12B	1.094 (18)	C38—H38B	1.102 (17)
C12—H12C	1.099 (18)	C38—H38C	1.115 (16)
C13—H13A	1.088 (15)	C39—H39A	1.087 (16)
C13—H13B	1.09 (2)	C39—H39B	1.105 (18)
C13—H13C	1.12 (2)	C39—H39C	1.081 (17)
C14—C15	1.3864 (11)
H1B—Ni1—H1A	34.2 (7)	C15—C14—N4	121.39 (7)
In1—Ni1—H1A	160.4 (6)	C19—C14—N4	117.96 (6)
In1—Ni1—H1B	162.3 (7)	C19—C14—C15	120.62 (7)
P1—Ni1—H1A	88.9 (6)	H15A—C15—C14	117.7 (7)
P1—Ni1—H1B	93.6 (7)	C16—C15—C14	121.54 (8)
P1—Ni1—In1	81.143 (6)	C16—C15—H15A	120.6 (7)
P2—Ni1—H1A	89.0 (6)	H16A—C16—C15	121.0 (8)
P2—Ni1—H1B	114.2 (7)	C17—C16—C15	118.61 (7)
P2—Ni1—In1	82.401 (6)	C17—C16—H16A	120.4 (8)
P2—Ni1—P1	122.762 (8)	H17A—C17—C16	120.5 (8)
P3—Ni1—H1A	115.0 (6)	C18—C17—C16	120.85 (8)
P3—Ni1—H1B	83.5 (6)	C18—C17—H17A	118.6 (8)
P3—Ni1—In1	84.563 (6)	H18A—C18—C17	120.1 (8)
P3—Ni1—P1	120.211 (9)	C19—C18—C17	121.58 (8)
P3—Ni1—P2	112.153 (9)	C19—C18—H18A	118.3 (8)
H1B—H1A—Ni1	74.0 (16)	C14—C19—N2	118.77 (7)
H1A—H1B—Ni1	71.8 (15)	C18—C19—N2	124.42 (7)
N1—In1—Ni1	104.66 (2)	C18—C19—C14	116.80 (7)
N2—In1—Ni1	102.740 (18)	N2—C20—P2	108.29 (5)
N2—In1—N1	116.48 (3)	H20A—C20—P2	108.3 (7)
N3—In1—Ni1	103.277 (18)	H20A—C20—N2	114.2 (7)
N3—In1—N1	111.74 (3)	H20B—C20—P2	110.0 (7)
N3—In1—N2	115.83 (3)	H20B—C20—N2	111.4 (8)
N4—In1—Ni1	178.627 (16)	H20B—C20—H20A	104.5 (10)
N4—In1—N1	76.59 (3)	H21A—C21—P2	106.6 (7)
N4—In1—N2	76.12 (2)	C23—C21—P2	112.44 (6)
N4—In1—N3	76.66 (2)	C23—C21—H21A	107.6 (8)
C7—P1—Ni1	117.47 (3)	C24—C21—P2	110.05 (6)
C8—P1—Ni1	110.57 (3)	C24—C21—H21A	110.1 (7)
C8—P1—C7	103.32 (4)	C24—C21—C23	109.97 (8)
C9—P1—Ni1	116.57 (3)	H22A—C22—P2	104.7 (7)
C9—P1—C7	102.06 (4)	C25—C22—P2	110.99 (6)
C9—P1—C8	105.36 (4)	C25—C22—H22A	109.9 (7)
C20—P2—Ni1	117.98 (3)	C26—C22—P2	115.87 (6)
C21—P2—Ni1	114.43 (3)	C26—C22—H22A	106.3 (7)
C21—P2—C20	102.58 (4)	C26—C22—C25	108.94 (7)
C22—P2—Ni1	117.37 (3)	H23A—C23—C21	110.0 (9)
C22—P2—C20	100.54 (4)	H23B—C23—C21	108.3 (8)
C22—P2—C21	101.40 (4)	H23B—C23—H23A	109.8 (12)
C33—P3—Ni1	118.84 (2)	H23C—C23—C21	113.4 (8)
C34—P3—Ni1	112.79 (3)	H23C—C23—H23A	105.6 (12)
C34—P3—C33	99.09 (4)	H23C—C23—H23B	109.8 (11)
C35—P3—Ni1	118.85 (3)	H24A—C24—C21	113.9 (8)
C35—P3—C33	99.58 (4)	H24B—C24—C21	111.1 (8)
C35—P3—C34	104.91 (4)	H24B—C24—H24A	105.8 (12)
C6—N1—In1	113.00 (5)	H24C—C24—C21	110.1 (8)
C7—N1—In1	115.69 (5)	H24C—C24—H24A	109.7 (12)
C7—N1—C6	119.47 (6)	H24C—C24—H24B	105.9 (11)
C19—N2—In1	112.98 (5)	H25A—C25—C22	108.9 (8)
C20—N2—In1	118.06 (5)	H25B—C25—C22	109.2 (8)
C20—N2—C19	120.63 (7)	H25B—C25—H25A	109.8 (11)
C32—N3—In1	113.14 (5)	H25C—C25—C22	114.4 (8)
C33—N3—In1	118.70 (5)	H25C—C25—H25A	107.9 (11)
C33—N3—C32	119.67 (6)	H25C—C25—H25B	106.5 (11)
C1—N4—In1	103.16 (5)	H26A—C26—C22	109.2 (8)
C14—N4—In1	103.42 (4)	H26B—C26—C22	113.2 (8)
C14—N4—C1	115.80 (6)	H26B—C26—H26A	107.3 (11)
C27—N4—In1	102.68 (4)	H26C—C26—C22	111.6 (8)
C27—N4—C1	113.54 (6)	H26C—C26—H26A	108.0 (11)
C27—N4—C14	115.74 (6)	H26C—C26—H26B	107.4 (11)
C2—C1—N4	121.39 (7)	C28—C27—N4	121.17 (7)
C6—C1—N4	117.98 (7)	C32—C27—N4	117.94 (6)
C6—C1—C2	120.56 (7)	C32—C27—C28	120.89 (7)
H2A—C2—C1	118.5 (8)	H28A—C28—C27	117.5 (7)
C3—C2—C1	121.47 (8)	C29—C28—C27	121.21 (8)
C3—C2—H2A	120.0 (8)	C29—C28—H28A	121.3 (7)
H3A—C3—C2	122.3 (8)	H29A—C29—C28	120.0 (8)
C4—C3—C2	118.65 (7)	C30—C29—C28	118.55 (8)
C4—C3—H3A	119.0 (8)	C30—C29—H29A	121.4 (8)
H4A—C4—C3	119.0 (7)	H30A—C30—C29	121.4 (8)
C5—C4—C3	120.74 (7)	C31—C30—C29	121.11 (8)
C5—C4—H4A	120.2 (8)	C31—C30—H30A	117.5 (8)
H5A—C5—C4	119.1 (7)	H31A—C31—C30	116.9 (7)
C6—C5—C4	121.60 (8)	C32—C31—C30	121.37 (7)
C6—C5—H5A	119.3 (7)	C32—C31—H31A	121.7 (7)
C1—C6—N1	119.13 (7)	C27—C32—N3	119.29 (7)
C5—C6—N1	123.89 (8)	C31—C32—N3	123.92 (7)
C5—C6—C1	116.98 (7)	C31—C32—C27	116.79 (7)
N1—C7—P1	108.68 (6)	N3—C33—P3	111.65 (5)
H7A—C7—P1	106.3 (7)	H33A—C33—P3	107.9 (8)
H7A—C7—N1	115.1 (7)	H33A—C33—N3	111.4 (7)
H7B—C7—P1	109.5 (7)	H33B—C33—P3	107.4 (8)
H7B—C7—N1	111.0 (7)	H33B—C33—N3	112.0 (7)
H7B—C7—H7A	106.1 (11)	H33B—C33—H33A	106.1 (10)
H8A—C8—P1	103.7 (8)	H34A—C34—P3	102.8 (7)
C10—C8—P1	117.17 (7)	C36—C34—P3	114.74 (6)
C10—C8—H8A	106.5 (8)	C36—C34—H34A	109.0 (7)
C11—C8—P1	110.50 (7)	C37—C34—P3	113.44 (6)
C11—C8—H8A	106.8 (8)	C37—C34—H34A	105.4 (7)
C11—C8—C10	111.25 (8)	C37—C34—C36	110.66 (7)
H9A—C9—P1	104.6 (7)	H35A—C35—P3	105.6 (8)
C12—C9—P1	109.99 (6)	C38—C35—P3	108.60 (6)
C12—C9—H9A	107.7 (8)	C38—C35—H35A	109.4 (8)
C13—C9—P1	116.67 (6)	C39—C35—P3	113.31 (6)
C13—C9—H9A	108.7 (8)	C39—C35—H35A	108.1 (7)
C13—C9—C12	108.81 (8)	C39—C35—C38	111.56 (7)
H10A—C10—C8	112.4 (9)	H36A—C36—C34	112.3 (8)
H10B—C10—C8	109.5 (9)	H36B—C36—C34	110.1 (8)
H10B—C10—H10A	108.4 (14)	H36B—C36—H36A	108.1 (11)
H10C—C10—C8	112.4 (8)	H36C—C36—C34	110.5 (8)
H10C—C10—H10A	105.8 (13)	H36C—C36—H36A	108.7 (12)
H10C—C10—H10B	108.3 (12)	H36C—C36—H36B	107.0 (11)
H11A—C11—C8	109.7 (9)	H37A—C37—C34	110.5 (8)
H11B—C11—C8	113.2 (8)	H37B—C37—C34	110.0 (8)
H11B—C11—H11A	109.8 (13)	H37B—C37—H37A	108.7 (12)
H11C—C11—C8	111.6 (8)	H37C—C37—C34	113.0 (8)
H11C—C11—H11A	103.8 (13)	H37C—C37—H37A	105.7 (12)
H11C—C11—H11B	108.4 (12)	H37C—C37—H37B	108.6 (11)
H12A—C12—C9	109.0 (9)	H38A—C38—C35	110.1 (9)
H12B—C12—C9	108.3 (8)	H38B—C38—C35	110.7 (8)
H12B—C12—H12A	109.8 (12)	H38B—C38—H38A	106.4 (12)
H12C—C12—C9	109.4 (8)	H38C—C38—C35	109.6 (8)
H12C—C12—H12A	109.4 (12)	H38C—C38—H38A	110.6 (12)
H12C—C12—H12B	110.8 (11)	H38C—C38—H38B	109.4 (11)
H13A—C13—C9	110.6 (9)	H39A—C39—C35	111.5 (9)
H13B—C13—C9	114.6 (9)	H39B—C39—C35	110.4 (8)
H13B—C13—H13A	108.3 (13)	H39B—C39—H39A	109.7 (13)
H13C—C13—C9	110.9 (8)	H39C—C39—C35	113.2 (8)
H13C—C13—H13A	105.4 (13)	H39C—C39—H39A	104.8 (12)
H13C—C13—H13B	106.6 (13)	H39C—C39—H39B	106.9 (11)
In1—N1—C6—C1	−26.71 (6)	N2—C19—C18—C17	−179.40 (8)
In1—N1—C6—C5	152.14 (5)	N3—C32—C27—N4	−4.20 (9)
In1—N1—C7—P1	29.24 (4)	N3—C32—C27—C28	176.48 (8)
In1—N2—C19—C14	−26.58 (6)	N3—C32—C31—C30	−178.37 (9)
In1—N2—C19—C18	152.20 (6)	N4—C1—C2—C3	177.50 (7)
In1—N2—C20—P2	23.16 (5)	N4—C1—C6—C5	−176.83 (7)
In1—N3—C32—C27	−22.26 (6)	N4—C14—C15—C16	178.54 (7)
In1—N3—C32—C31	157.58 (6)	N4—C14—C19—C18	−177.91 (7)
In1—N3—C33—P3	14.20 (5)	N4—C27—C28—C29	−176.42 (8)
In1—N4—C1—C2	−157.34 (5)	N4—C27—C32—C31	175.95 (7)
In1—N4—C1—C6	19.55 (5)	C1—C2—C3—C4	−1.10 (10)
In1—N4—C14—C15	−157.03 (5)	C1—C6—C5—C4	−0.45 (9)
In1—N4—C14—C19	21.07 (5)	C2—C3—C4—C5	0.73 (10)
In1—N4—C27—C28	−156.69 (5)	C3—C4—C5—C6	0.04 (10)
In1—N4—C27—C32	24.00 (5)	C14—C15—C16—C17	−0.78 (10)
P1—C7—N1—C6	169.58 (5)	C14—C19—C18—C17	−0.60 (9)
P2—C20—N2—C19	169.24 (5)	C15—C16—C17—C18	0.40 (10)
P3—C33—N3—C32	160.05 (6)	C16—C17—C18—C19	0.30 (11)
N1—C6—C1—N4	2.11 (8)	C27—C28—C29—C30	−0.33 (11)
N1—C6—C1—C2	179.03 (7)	C27—C32—C31—C30	1.47 (10)
N1—C6—C5—C4	−179.33 (8)	C28—C29—C30—C31	−1.60 (12)
N2—C19—C14—N4	0.96 (8)	C29—C30—C31—C32	0.99 (12)
N2—C19—C14—C15	179.08 (7)

(GOJNIF_HAR_NoMoRe)

Crystal data

C39H62InN4NiP3	Dx = 1.415 Mg m^−3
Mr = 853.39	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, P212121	Cell parameters from 9537 reflections
a = 12.2127 (4) Å	θ = 2.3–36.4°
b = 14.5402 (5) Å	µ = 1.20 mm^−1
c = 22.5601 (8) Å	T = 100 K
V = 4006.1 (2) Å^3	Block, gold
Z = 4	0.14 × 0.08 × 0.06 mm
F(000) = 1784.150

Data collection

Bruker Photon-II CMOS diffractometer	18741 reflections with I ≥ 2u(I)
φ and ω scans	Rint = 0.036
Absorption correction: multi-scan SADABS. R.Blessing, 1995	θmax = 36.4°, θmin = 2.3°
Tmin = 0.701, Tmax = 0.747	h = −20→20
237431 measured reflections	k = −24→24
19473 independent reflections	l = −37→37

Refinement

Refinement on F^2	0 constraints
Least-squares matrix: full	Only H-atom coordinates refined
R[F^2 > 2σ(F^2)] = 0.016	w = 1/[σ^2(Fo^2) + (0.0239P)^2 + 0.5897P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.040	(Δ/σ)max = 0.001
S = 0.96	Δρmax = 0.34 e Å^−3
19473 reflections	Δρmin = −0.55 e Å^−3
619 parameters	Absolute structure: Flack, H. D. (1983). Acta Cryst. A39, 876-881.
0 restraints	Absolute structure parameter: 0.003 (5)

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ni1	0.755816 (9)	0.598650 (7)	0.856150 (5)	0.009304 (19)
H1A	0.7315 (18)	0.5702 (15)	0.9260 (9)	0.037000
H1B	0.753 (2)	0.6337 (15)	0.9273 (9)	0.035333
In1	0.798239 (4)	0.580829 (3)	0.749322 (3)	0.008315 (11)
P1	0.918454 (18)	0.522248 (15)	0.864338 (9)	0.00934 (3)
P2	0.599028 (18)	0.528565 (15)	0.829176 (10)	0.00942 (3)
P3	0.753619 (19)	0.750093 (15)	0.835678 (9)	0.00916 (3)
N1	0.96176 (5)	0.53381 (5)	0.74727 (4)	0.01093 (10)
N2	0.67666 (6)	0.48666 (5)	0.72035 (3)	0.01136 (12)
N3	0.78427 (6)	0.71632 (5)	0.71619 (3)	0.01066 (11)
N4	0.83415 (6)	0.56338 (5)	0.64679 (3)	0.00883 (11)
C1	0.95346 (6)	0.57171 (5)	0.64336 (4)	0.00957 (12)
C2	1.00523 (7)	0.59713 (6)	0.59110 (4)	0.01287 (14)
H2A	0.9573 (14)	0.6117 (12)	0.5540 (6)	0.028333
C3	1.11901 (8)	0.60861 (6)	0.58831 (4)	0.01475 (15)
H3A	1.1608 (15)	0.6284 (13)	0.5481 (7)	0.032000
C4	1.18035 (7)	0.59547 (6)	0.63979 (4)	0.01430 (14)
H4A	1.2684 (13)	0.6058 (12)	0.6377 (8)	0.030333
C5	1.12982 (7)	0.57046 (6)	0.69273 (4)	0.01248 (14)
H5A	1.1801 (13)	0.5630 (12)	0.7329 (7)	0.028000
C6	1.01531 (7)	0.55739 (6)	0.69640 (4)	0.00990 (13)
C7	1.01947 (7)	0.53661 (6)	0.80306 (4)	0.01156 (14)
H7A	1.0634 (14)	0.6011 (12)	0.8127 (7)	0.028000
H7B	1.0828 (14)	0.4829 (12)	0.8052 (7)	0.029000
C8	0.99543 (8)	0.56223 (7)	0.93121 (4)	0.01429 (15)
H8A	0.9801 (15)	0.6381 (12)	0.9321 (7)	0.027667
C9	0.91080 (8)	0.39463 (6)	0.87150 (4)	0.01393 (14)
H9A	0.8502 (15)	0.3832 (11)	0.9078 (7)	0.029667
C10	1.12038 (9)	0.55058 (9)	0.93051 (5)	0.02237 (19)
H10A	1.1454 (16)	0.4783 (14)	0.9261 (10)	0.050333
H10B	1.1554 (16)	0.5768 (17)	0.9739 (9)	0.051667
H10C	1.1603 (15)	0.5854 (15)	0.8926 (8)	0.041667
C11	0.94552 (11)	0.52155 (10)	0.98768 (5)	0.0270 (2)
H11A	0.9871 (17)	0.5546 (14)	1.0255 (8)	0.042000
H11B	0.9561 (16)	0.4456 (15)	0.9906 (9)	0.046667
H11C	0.8635 (17)	0.5359 (12)	0.9916 (8)	0.040000
C12	0.86444 (9)	0.35268 (7)	0.81443 (5)	0.01864 (17)
H12A	0.8484 (17)	0.2809 (11)	0.8223 (9)	0.041333
H12B	0.9250 (17)	0.3606 (13)	0.7799 (9)	0.043000
H12C	0.7863 (17)	0.3887 (14)	0.8039 (8)	0.046000
C13	1.01684 (10)	0.34490 (7)	0.88744 (6)	0.0237 (2)
H13A	1.0056 (17)	0.2705 (12)	0.8869 (9)	0.045667
H13B	1.0515 (17)	0.3624 (15)	0.9296 (10)	0.048333
H13C	1.0830 (19)	0.3608 (14)	0.8551 (9)	0.051667
C14	0.78963 (7)	0.47286 (5)	0.63325 (3)	0.01011 (12)
C15	0.82600 (7)	0.42271 (6)	0.58483 (4)	0.01240 (13)
H15A	0.8929 (14)	0.4529 (12)	0.5581 (7)	0.027333
C16	0.78525 (8)	0.33492 (6)	0.57248 (4)	0.01526 (15)
H16A	0.8119 (16)	0.2970 (13)	0.5323 (8)	0.036000
C17	0.70728 (8)	0.29739 (6)	0.61048 (4)	0.01609 (15)
H17A	0.6752 (16)	0.2269 (12)	0.6027 (8)	0.039333
C18	0.67007 (8)	0.34633 (6)	0.65965 (4)	0.01425 (15)
H18A	0.6109 (15)	0.3151 (12)	0.6902 (8)	0.034000
C19	0.70913 (7)	0.43549 (5)	0.67266 (4)	0.01043 (12)
C20	0.60325 (7)	0.44845 (6)	0.76424 (4)	0.01194 (14)
H20A	0.6269 (14)	0.3788 (11)	0.7808 (7)	0.027000
H20B	0.5199 (12)	0.4394 (11)	0.7455 (7)	0.027000
C21	0.53633 (7)	0.45619 (6)	0.88799 (4)	0.01321 (14)
H21A	0.4653 (13)	0.4218 (12)	0.8680 (7)	0.025000
C22	0.48066 (7)	0.60401 (6)	0.80770 (4)	0.01243 (13)
H22A	0.4783 (14)	0.6577 (11)	0.8418 (7)	0.025333
C23	0.61403 (9)	0.38122 (8)	0.91014 (5)	0.02053 (18)
H23A	0.5723 (17)	0.3376 (13)	0.9429 (9)	0.043000
H23B	0.6857 (17)	0.4150 (14)	0.9322 (9)	0.042667
H23C	0.6414 (15)	0.3353 (14)	0.8759 (9)	0.042333
C24	0.49921 (9)	0.51666 (8)	0.93998 (4)	0.01882 (17)
H24A	0.4395 (17)	0.5763 (14)	0.9255 (8)	0.036667
H24B	0.5685 (16)	0.5499 (13)	0.9612 (7)	0.035333
H24C	0.4609 (16)	0.4765 (13)	0.9738 (8)	0.038333
C25	0.49929 (8)	0.64748 (7)	0.74674 (5)	0.01718 (15)
H25A	0.4347 (14)	0.6998 (12)	0.7385 (8)	0.036000
H25B	0.4947 (14)	0.5934 (13)	0.7135 (8)	0.035667
H25C	0.5788 (16)	0.6802 (12)	0.7410 (7)	0.036667
C26	0.36760 (8)	0.55818 (7)	0.80853 (5)	0.01755 (17)
H26A	0.3048 (14)	0.6098 (13)	0.7978 (8)	0.036667
H26B	0.3438 (15)	0.5299 (13)	0.8521 (8)	0.037667
H26C	0.3631 (14)	0.5020 (13)	0.7779 (7)	0.035333
C27	0.77588 (7)	0.64129 (6)	0.62077 (4)	0.01021 (13)
C28	0.74258 (8)	0.64005 (6)	0.56207 (4)	0.01443 (14)
H28A	0.7556 (16)	0.5753 (11)	0.5375 (7)	0.029333
C29	0.69218 (9)	0.71653 (7)	0.53615 (4)	0.01817 (17)
H29A	0.6692 (16)	0.7140 (12)	0.4909 (7)	0.038333
C30	0.67553 (8)	0.79432 (7)	0.57069 (4)	0.01690 (16)
H30A	0.6396 (17)	0.8561 (12)	0.5519 (8)	0.036667
C31	0.70552 (8)	0.79596 (6)	0.63024 (4)	0.01321 (13)
H31A	0.6910 (15)	0.8575 (10)	0.6524 (7)	0.029333
C32	0.75544 (7)	0.71940 (6)	0.65748 (3)	0.01000 (12)
C33	0.74812 (7)	0.78800 (5)	0.75566 (4)	0.01175 (12)
H33A	0.6623 (13)	0.8085 (11)	0.7459 (7)	0.027333
H33B	0.7982 (12)	0.8493 (10)	0.7518 (7)	0.028667
C34	0.62755 (7)	0.80867 (6)	0.86343 (4)	0.01191 (13)
H34A	0.5639 (13)	0.7830 (11)	0.8333 (7)	0.026000
C35	0.86864 (7)	0.82277 (6)	0.86198 (4)	0.01293 (14)
H35A	0.8485 (15)	0.8925 (11)	0.8472 (7)	0.028333
C36	0.63049 (8)	0.91393 (6)	0.85998 (4)	0.01625 (15)
H36A	0.6582 (16)	0.9379 (12)	0.8189 (8)	0.036333
H36B	0.6860 (16)	0.9435 (13)	0.8956 (9)	0.037667
H36C	0.5478 (16)	0.9421 (12)	0.8686 (8)	0.036000
C37	0.59270 (9)	0.77704 (7)	0.92539 (4)	0.01787 (16)
H37A	0.5123 (15)	0.8045 (14)	0.9364 (8)	0.036667
H37B	0.6498 (15)	0.8009 (12)	0.9568 (8)	0.032667
H37C	0.5859 (15)	0.7045 (13)	0.9295 (7)	0.036000
C38	0.97440 (8)	0.78990 (7)	0.83201 (5)	0.01697 (16)
H38A	1.0371 (15)	0.8411 (13)	0.8362 (9)	0.041000
H38B	0.9616 (16)	0.7800 (13)	0.7837 (9)	0.041667
H38C	1.0007 (15)	0.7238 (13)	0.8528 (8)	0.035667
C39	0.88002 (9)	0.82427 (7)	0.92964 (4)	0.01793 (17)
H39A	0.9530 (17)	0.8583 (15)	0.9448 (8)	0.043667
H39B	0.8752 (16)	0.7534 (14)	0.9474 (8)	0.040000
H39C	0.8164 (18)	0.8630 (13)	0.9515 (8)	0.038000

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ni1	0.00845 (4)	0.00819 (4)	0.01127 (4)	−0.00035 (3)	0.00037 (3)	0.00002 (3)
H1A	0.047000	0.040000	0.024000	−0.010000	0.003000	0.006000
H1B	0.049000	0.034000	0.023000	0.002000	−0.001000	−0.005000
In1	0.008502 (19)	0.007840 (19)	0.008604 (19)	0.000102 (15)	0.000154 (19)	−0.000134 (19)
P1	0.01006 (8)	0.00953 (8)	0.00843 (8)	0.00075 (7)	−0.00069 (6)	0.00060 (6)
P2	0.00865 (8)	0.01082 (8)	0.00878 (8)	−0.00176 (7)	0.00046 (6)	−0.00029 (7)
P3	0.01105 (8)	0.00777 (7)	0.00865 (8)	−0.00019 (7)	−0.00055 (7)	−0.00086 (6)
N1	0.0095 (2)	0.0137 (3)	0.0095 (3)	0.0010 (2)	−0.0002 (2)	0.0012 (3)
N2	0.0119 (3)	0.0117 (3)	0.0105 (3)	−0.0022 (2)	0.0012 (2)	−0.0027 (2)
N3	0.0144 (3)	0.0091 (3)	0.0086 (3)	0.0015 (2)	−0.0008 (2)	0.0001 (2)
N4	0.0105 (3)	0.0088 (3)	0.0072 (3)	0.0009 (2)	−0.0008 (2)	0.0001 (2)
C1	0.0102 (3)	0.0101 (3)	0.0084 (3)	0.0004 (2)	0.0012 (2)	−0.0003 (2)
C2	0.0143 (3)	0.0135 (3)	0.0107 (3)	−0.0002 (3)	0.0025 (3)	0.0007 (3)
H2A	0.027000	0.040000	0.018000	0.000000	−0.002000	0.005000
C3	0.0150 (4)	0.0159 (4)	0.0133 (3)	−0.0011 (3)	0.0044 (3)	0.0011 (3)
H3A	0.029000	0.045000	0.022000	−0.004000	0.009000	0.007000
C4	0.0114 (3)	0.0155 (3)	0.0160 (4)	−0.0008 (3)	0.0036 (3)	0.0006 (3)
H4A	0.017000	0.041000	0.033000	−0.004000	0.004000	0.002000
C5	0.0100 (3)	0.0150 (3)	0.0125 (3)	0.0002 (3)	0.0008 (3)	0.0007 (3)
H5A	0.021000	0.040000	0.023000	0.000000	−0.003000	0.004000
C6	0.0097 (3)	0.0109 (3)	0.0092 (3)	0.0007 (2)	0.0011 (2)	0.0001 (2)
C7	0.0102 (3)	0.0144 (4)	0.0101 (3)	0.0013 (3)	−0.0003 (2)	0.0008 (3)
H7A	0.026000	0.031000	0.027000	−0.009000	−0.001000	0.001000
H7B	0.024000	0.034000	0.029000	0.013000	0.001000	0.006000
C8	0.0159 (4)	0.0164 (4)	0.0105 (3)	−0.0014 (3)	−0.0020 (3)	−0.0003 (3)
H8A	0.034000	0.019000	0.030000	−0.001000	−0.004000	0.002000
C9	0.0151 (3)	0.0107 (3)	0.0160 (4)	0.0014 (3)	−0.0006 (3)	0.0026 (3)
H9A	0.034000	0.024000	0.031000	0.001000	0.010000	0.007000
C10	0.0167 (4)	0.0294 (5)	0.0210 (5)	0.0005 (4)	−0.0078 (3)	−0.0034 (4)
H10A	0.032000	0.046000	0.073000	0.013000	−0.009000	−0.015000
H10B	0.028000	0.089000	0.038000	−0.013000	0.001000	0.021000
H10C	0.032000	0.061000	0.032000	−0.004000	−0.011000	−0.008000
C11	0.0337 (6)	0.0352 (6)	0.0120 (4)	−0.0098 (5)	0.0003 (4)	0.0008 (4)
H11A	0.059000	0.047000	0.020000	−0.014000	−0.007000	−0.000000
H11B	0.029000	0.071000	0.040000	0.009000	0.010000	0.020000
H11C	0.063000	0.023000	0.034000	−0.002000	0.002000	0.008000
C12	0.0244 (5)	0.0116 (3)	0.0199 (4)	−0.0006 (3)	−0.0017 (3)	−0.0018 (3)
H12A	0.058000	0.016000	0.050000	−0.003000	−0.004000	−0.001000
H12B	0.039000	0.032000	0.058000	0.009000	−0.021000	−0.009000
H12C	0.053000	0.052000	0.033000	−0.012000	0.015000	−0.010000
C13	0.0202 (4)	0.0145 (4)	0.0365 (6)	0.0054 (3)	−0.0056 (4)	0.0050 (4)
H13A	0.050000	0.019000	0.068000	0.009000	−0.010000	0.004000
H13B	0.028000	0.044000	0.073000	0.012000	0.008000	0.007000
H13C	0.059000	0.044000	0.052000	0.018000	−0.027000	−0.003000
C14	0.0124 (3)	0.0090 (3)	0.0089 (3)	0.0012 (3)	0.0000 (2)	−0.0015 (2)
C15	0.0153 (3)	0.0118 (3)	0.0101 (3)	0.0000 (3)	0.0011 (2)	−0.0022 (3)
H15A	0.029000	0.029000	0.024000	−0.001000	0.009000	−0.002000
C16	0.0189 (4)	0.0132 (3)	0.0137 (3)	−0.0006 (3)	0.0009 (3)	−0.0059 (3)
H16A	0.042000	0.034000	0.032000	−0.001000	0.009000	−0.019000
C17	0.0184 (4)	0.0126 (3)	0.0172 (4)	−0.0028 (3)	0.0007 (3)	−0.0055 (3)
H17A	0.047000	0.026000	0.045000	−0.014000	0.007000	−0.017000
C18	0.0145 (3)	0.0123 (3)	0.0160 (4)	−0.0030 (3)	0.0015 (3)	−0.0041 (3)
H18A	0.038000	0.030000	0.034000	−0.015000	0.011000	−0.006000
C19	0.0107 (3)	0.0102 (3)	0.0104 (3)	−0.0006 (2)	0.0002 (2)	−0.0024 (2)
C20	0.0111 (3)	0.0126 (3)	0.0121 (3)	−0.0029 (3)	0.0015 (2)	−0.0018 (2)
H20A	0.033000	0.018000	0.030000	−0.001000	0.005000	0.003000
H20B	0.019000	0.036000	0.026000	−0.006000	−0.002000	−0.005000
C21	0.0132 (3)	0.0156 (4)	0.0108 (3)	−0.0037 (3)	0.0008 (3)	0.0012 (3)
H21A	0.023000	0.027000	0.025000	−0.008000	−0.001000	−0.002000
C22	0.0097 (3)	0.0156 (3)	0.0119 (3)	0.0004 (3)	0.0003 (2)	−0.0020 (3)
H22A	0.028000	0.024000	0.024000	0.000000	−0.001000	−0.007000
C23	0.0206 (4)	0.0223 (4)	0.0187 (4)	0.0001 (4)	0.0024 (3)	0.0075 (3)
H23A	0.045000	0.039000	0.045000	0.001000	0.011000	0.023000
H23B	0.053000	0.039000	0.036000	0.018000	0.007000	0.001000
H23C	0.032000	0.050000	0.045000	0.001000	−0.012000	0.008000
C24	0.0241 (5)	0.0221 (4)	0.0102 (4)	−0.0059 (4)	0.0031 (3)	−0.0015 (3)
H24A	0.047000	0.035000	0.028000	0.013000	0.002000	−0.001000
H24B	0.045000	0.037000	0.024000	−0.010000	0.012000	0.005000
H24C	0.035000	0.052000	0.028000	−0.018000	0.000000	−0.011000
C25	0.0170 (3)	0.0191 (3)	0.0155 (4)	0.0028 (3)	−0.0011 (3)	0.0020 (4)
H25A	0.033000	0.039000	0.036000	0.014000	−0.001000	0.010000
H25B	0.025000	0.045000	0.037000	−0.009000	0.000000	0.013000
H25C	0.054000	0.035000	0.021000	−0.000000	0.000000	−0.005000
C26	0.0107 (3)	0.0232 (4)	0.0188 (4)	−0.0015 (3)	−0.0011 (3)	−0.0035 (3)
H26A	0.021000	0.040000	0.049000	0.005000	−0.005000	0.006000
H26B	0.031000	0.040000	0.042000	−0.008000	−0.001000	−0.019000
H26C	0.028000	0.050000	0.028000	−0.008000	0.004000	0.008000
C27	0.0134 (3)	0.0094 (3)	0.0078 (3)	0.0014 (2)	−0.0006 (2)	0.0000 (2)
C28	0.0206 (4)	0.0130 (3)	0.0096 (3)	0.0041 (3)	−0.0030 (3)	−0.0013 (3)
H28A	0.043000	0.024000	0.021000	0.010000	−0.003000	−0.006000
C29	0.0269 (5)	0.0170 (4)	0.0106 (3)	0.0085 (3)	−0.0056 (3)	−0.0007 (3)
H29A	0.062000	0.035000	0.018000	0.015000	−0.012000	−0.000000
C30	0.0242 (4)	0.0153 (4)	0.0111 (3)	0.0084 (3)	−0.0029 (3)	0.0012 (3)
H30A	0.057000	0.026000	0.027000	0.018000	−0.007000	0.006000
C31	0.0175 (3)	0.0116 (3)	0.0105 (3)	0.0048 (3)	−0.0011 (3)	0.0006 (2)
H31A	0.044000	0.018000	0.026000	0.009000	−0.002000	−0.003000
C32	0.0123 (3)	0.0087 (3)	0.0090 (3)	0.0015 (3)	−0.0009 (3)	0.0002 (2)
C33	0.0163 (3)	0.0087 (3)	0.0103 (3)	0.0012 (3)	0.0000 (3)	−0.0005 (2)
H33A	0.027000	0.029000	0.026000	0.011000	−0.002000	−0.002000
H33B	0.040000	0.017000	0.029000	−0.007000	0.002000	−0.000000
C34	0.0138 (3)	0.0112 (3)	0.0107 (3)	0.0011 (3)	0.0006 (3)	−0.0008 (3)
H34A	0.023000	0.029000	0.026000	0.000000	−0.005000	−0.006000
C35	0.0145 (3)	0.0108 (3)	0.0134 (4)	−0.0022 (3)	−0.0005 (3)	−0.0015 (3)
H35A	0.034000	0.017000	0.034000	−0.002000	−0.002000	−0.000000
C36	0.0206 (4)	0.0118 (3)	0.0164 (4)	0.0035 (3)	0.0010 (3)	−0.0007 (3)
H36A	0.052000	0.028000	0.029000	0.004000	0.010000	0.006000
H36B	0.035000	0.028000	0.050000	0.013000	0.009000	−0.000000
H36C	0.047000	0.024000	0.037000	−0.004000	−0.008000	−0.007000
C37	0.0223 (4)	0.0175 (4)	0.0137 (4)	−0.0013 (3)	0.0037 (3)	−0.0005 (3)
H37A	0.034000	0.038000	0.038000	0.013000	0.014000	0.002000
H37B	0.042000	0.019000	0.037000	−0.002000	0.009000	0.001000
H37C	0.043000	0.042000	0.023000	−0.009000	−0.004000	−0.001000
C38	0.0147 (4)	0.0182 (4)	0.0180 (4)	−0.0041 (3)	0.0011 (3)	−0.0028 (3)
H38A	0.027000	0.044000	0.052000	−0.016000	0.005000	−0.010000
H38B	0.039000	0.037000	0.049000	0.014000	0.009000	0.016000
H38C	0.033000	0.050000	0.024000	−0.000000	0.002000	−0.007000
C39	0.0191 (4)	0.0204 (4)	0.0143 (4)	−0.0031 (3)	−0.0026 (3)	−0.0041 (3)
H39A	0.036000	0.060000	0.035000	−0.021000	−0.008000	−0.009000
H39B	0.040000	0.048000	0.032000	0.006000	0.004000	−0.013000
H39C	0.051000	0.034000	0.029000	−0.003000	−0.005000	0.005000

Geometric parameters (Å, º)

Ni1—H1A	1.66 (2)	C14—C19	1.4325 (12)
Ni1—H1B	1.686 (19)	C15—H15A	1.106 (16)
Ni1—In1	2.4787 (1)	C15—C16	1.3981 (13)
Ni1—P1	2.2833 (2)	C16—H16A	1.109 (16)
Ni1—P2	2.2528 (2)	C16—C17	1.3927 (14)
Ni1—P3	2.2501 (2)	C17—H17A	1.111 (17)
H1A—H1B	0.96 (3)	C17—C18	1.3940 (13)
In1—N1	2.1114 (7)	C18—H18A	1.097 (16)
In1—N2	2.1229 (7)	C18—C19	1.4122 (12)
In1—N3	2.1140 (7)	C20—H20A	1.117 (16)
In1—N4	2.3680 (7)	C20—H20B	1.110 (15)
P1—C7	1.8646 (9)	C21—H21A	1.098 (16)
P1—C8	1.8702 (9)	C21—C23	1.5292 (14)
P1—C9	1.8649 (9)	C21—C24	1.5345 (13)
P2—C20	1.8724 (9)	C22—H22A	1.096 (15)
P2—C21	1.8586 (9)	C22—C25	1.5305 (15)
P2—C22	1.8783 (9)	C22—C26	1.5333 (13)
P3—C33	1.8886 (9)	C23—H23A	1.099 (18)
P3—C34	1.8676 (9)	C23—H23B	1.12 (2)
P3—C35	1.8553 (9)	C23—H23C	1.07 (2)
N1—C6	1.3646 (12)	C24—H24A	1.180 (19)
N1—C7	1.4431 (12)	C24—H24B	1.086 (19)
N2—C19	1.3669 (11)	C24—H24C	1.069 (18)
N2—C20	1.4466 (11)	C25—H25A	1.112 (16)
N3—C32	1.3712 (10)	C25—H25B	1.09 (2)
N3—C33	1.4402 (11)	C25—H25C	1.088 (19)
N4—C1	1.4641 (10)	C26—H26A	1.100 (17)
N4—C14	1.4564 (11)	C26—H26B	1.103 (19)
N4—C27	1.4609 (10)	C26—H26C	1.071 (18)
C1—C2	1.3879 (12)	C27—C28	1.3855 (11)
C1—C6	1.4303 (12)	C27—C32	1.4277 (11)
C2—H2A	1.044 (15)	C28—H28A	1.104 (16)
C2—C3	1.4010 (13)	C28—C29	1.3990 (13)
C3—H3A	1.081 (16)	C29—H29A	1.058 (16)
C3—C4	1.3951 (13)	C29—C30	1.3885 (14)
C4—H4A	1.087 (16)	C30—H30A	1.086 (16)
C4—C5	1.3927 (12)	C30—C31	1.3928 (13)
C5—H5A	1.099 (15)	C31—H31A	1.039 (15)
C5—C6	1.4138 (12)	C31—C32	1.4102 (12)
C7—H7A	1.102 (16)	C33—H33A	1.112 (15)
C7—H7B	1.100 (16)	C33—H33B	1.084 (14)
C8—H8A	1.119 (17)	C34—H34A	1.098 (15)
C8—C10	1.5354 (14)	C34—C36	1.5329 (13)
C8—C11	1.5311 (15)	C34—C37	1.5319 (13)
C9—H9A	1.116 (16)	C35—H35A	1.095 (16)
C9—C12	1.5330 (14)	C35—C38	1.5342 (14)
C9—C13	1.5261 (14)	C35—C39	1.5328 (14)
C10—H10A	1.10 (2)	C36—H36A	1.045 (16)
C10—H10B	1.13 (2)	C36—H36B	1.13 (2)
C10—H10C	1.11 (2)	C36—H36C	1.11 (2)
C11—H11A	1.103 (18)	C37—H37A	1.088 (17)
C11—H11B	1.11 (2)	C37—H37B	1.054 (18)
C11—H11C	1.03 (2)	C37—H37C	1.062 (18)
C12—H12A	1.077 (17)	C38—H38A	1.072 (18)
C12—H12B	1.08 (2)	C38—H38B	1.11 (2)
C12—H12C	1.11 (2)	C38—H38C	1.116 (19)
C13—H13A	1.091 (18)	C39—H39A	1.075 (19)
C13—H13B	1.07 (2)	C39—H39B	1.11 (2)
C13—H13C	1.11 (2)	C39—H39C	1.08 (2)
C14—C15	1.3866 (11)
H1B—Ni1—H1A	33.4 (9)	C15—C14—N4	121.39 (8)
In1—Ni1—H1A	159.5 (8)	C19—C14—N4	117.97 (7)
In1—Ni1—H1B	164.3 (8)	C19—C14—C15	120.62 (7)
P1—Ni1—H1A	87.6 (8)	H15A—C15—C14	117.2 (9)
P1—Ni1—H1B	95.1 (8)	C16—C15—C14	121.54 (8)
P1—Ni1—In1	81.139 (6)	C16—C15—H15A	121.1 (9)
P2—Ni1—H1A	89.5 (8)	H16A—C16—C15	120.8 (10)
P2—Ni1—H1B	112.1 (8)	C17—C16—C15	118.58 (8)
P2—Ni1—In1	82.400 (7)	C17—C16—H16A	120.6 (10)
P2—Ni1—P1	122.762 (9)	H17A—C17—C16	120.3 (10)
P3—Ni1—H1A	115.9 (8)	C18—C17—C16	120.85 (8)
P3—Ni1—H1B	84.2 (7)	C18—C17—H17A	118.8 (10)
P3—Ni1—In1	84.562 (6)	H18A—C18—C17	120.3 (9)
P3—Ni1—P1	120.206 (9)	C19—C18—C17	121.59 (8)
P3—Ni1—P2	112.154 (9)	C19—C18—H18A	118.1 (9)
H1B—H1A—Ni1	75.1 (19)	C14—C19—N2	118.76 (7)
H1A—H1B—Ni1	71.6 (18)	C18—C19—N2	124.42 (8)
N1—In1—Ni1	104.65 (2)	C18—C19—C14	116.82 (7)
N2—In1—Ni1	102.74 (2)	N2—C20—P2	108.28 (6)
N2—In1—N1	116.49 (3)	H20A—C20—P2	108.1 (8)
N3—In1—Ni1	103.267 (19)	H20A—C20—N2	114.6 (9)
N3—In1—N1	111.73 (3)	H20B—C20—P2	110.3 (8)
N3—In1—N2	115.84 (3)	H20B—C20—N2	110.7 (9)
N4—In1—Ni1	178.604 (17)	H20B—C20—H20A	104.8 (12)
N4—In1—N1	76.63 (3)	H21A—C21—P2	106.9 (8)
N4—In1—N2	76.10 (3)	C23—C21—P2	112.41 (6)
N4—In1—N3	76.67 (2)	C23—C21—H21A	107.5 (9)
C7—P1—Ni1	117.46 (3)	C24—C21—P2	110.06 (6)
C8—P1—Ni1	110.57 (3)	C24—C21—H21A	109.9 (8)
C8—P1—C7	103.33 (4)	C24—C21—C23	110.00 (8)
C9—P1—Ni1	116.58 (3)	H22A—C22—P2	104.8 (9)
C9—P1—C7	102.05 (4)	C25—C22—P2	111.01 (6)
C9—P1—C8	105.35 (4)	C25—C22—H22A	109.9 (9)
C20—P2—Ni1	117.99 (3)	C26—C22—P2	115.85 (7)
C21—P2—Ni1	114.42 (3)	C26—C22—H22A	106.1 (9)
C21—P2—C20	102.57 (4)	C26—C22—C25	108.93 (8)
C22—P2—Ni1	117.36 (3)	H23A—C23—C21	110.1 (11)
C22—P2—C20	100.53 (4)	H23B—C23—C21	108.5 (10)
C22—P2—C21	101.41 (4)	H23B—C23—H23A	108.4 (15)
C33—P3—Ni1	118.83 (2)	H23C—C23—C21	113.7 (10)
C34—P3—Ni1	112.79 (3)	H23C—C23—H23A	105.6 (15)
C34—P3—C33	99.09 (4)	H23C—C23—H23B	110.4 (13)
C35—P3—Ni1	118.86 (3)	H24A—C24—C21	113.1 (9)
C35—P3—C33	99.58 (4)	H24B—C24—C21	111.2 (9)
C35—P3—C34	104.90 (4)	H24B—C24—H24A	106.1 (14)
C6—N1—In1	112.98 (6)	H24C—C24—C21	111.2 (10)
C7—N1—In1	115.70 (6)	H24C—C24—H24A	109.2 (15)
C7—N1—C6	119.50 (7)	H24C—C24—H24B	105.6 (12)
C19—N2—In1	112.98 (5)	H25A—C25—C22	109.1 (9)
C20—N2—In1	118.06 (5)	H25B—C25—C22	108.3 (9)
C20—N2—C19	120.63 (7)	H25B—C25—H25A	110.1 (13)
C32—N3—In1	113.12 (5)	H25C—C25—C22	114.8 (9)
C33—N3—In1	118.72 (5)	H25C—C25—H25A	108.3 (13)
C33—N3—C32	119.66 (7)	H25C—C25—H25B	106.2 (12)
C1—N4—In1	103.12 (5)	H26A—C26—C22	109.2 (9)
C14—N4—In1	103.44 (5)	H26B—C26—C22	114.2 (9)
C14—N4—C1	115.80 (6)	H26B—C26—H26A	105.5 (14)
C27—N4—In1	102.66 (5)	H26C—C26—C22	111.7 (9)
C27—N4—C1	113.54 (6)	H26C—C26—H26A	110.0 (13)
C27—N4—C14	115.76 (6)	H26C—C26—H26B	106.1 (13)
C2—C1—N4	121.35 (7)	C28—C27—N4	121.13 (7)
C6—C1—N4	117.99 (7)	C32—C27—N4	117.97 (7)
C6—C1—C2	120.59 (8)	C32—C27—C28	120.90 (7)
H2A—C2—C1	118.7 (9)	H28A—C28—C27	116.6 (8)
C3—C2—C1	121.45 (8)	C29—C28—C27	121.22 (8)
C3—C2—H2A	119.7 (9)	C29—C28—H28A	122.1 (8)
H3A—C3—C2	122.5 (10)	H29A—C29—C28	119.5 (9)
C4—C3—C2	118.62 (8)	C30—C29—C28	118.52 (8)
C4—C3—H3A	118.8 (10)	C30—C29—H29A	122.0 (9)
H4A—C4—C3	118.5 (9)	H30A—C30—C29	120.9 (9)
C5—C4—C3	120.78 (8)	C31—C30—C29	121.11 (8)
C5—C4—H4A	120.7 (9)	C31—C30—H30A	118.0 (9)
H5A—C5—C4	119.0 (9)	H31A—C31—C30	115.6 (9)
C6—C5—C4	121.57 (8)	C32—C31—C30	121.37 (8)
C6—C5—H5A	119.4 (9)	C32—C31—H31A	123.0 (9)
C1—C6—N1	119.15 (8)	C27—C32—N3	119.31 (7)
C5—C6—N1	123.85 (8)	C31—C32—N3	123.90 (7)
C5—C6—C1	116.99 (8)	C31—C32—C27	116.79 (7)
N1—C7—P1	108.68 (6)	N3—C33—P3	111.65 (5)
H7A—C7—P1	105.8 (9)	H33A—C33—P3	107.5 (9)
H7A—C7—N1	115.7 (8)	H33A—C33—N3	111.1 (9)
H7B—C7—P1	110.7 (8)	H33B—C33—P3	107.3 (9)
H7B—C7—N1	111.2 (9)	H33B—C33—N3	111.8 (8)
H7B—C7—H7A	104.6 (12)	H33B—C33—H33A	107.2 (12)
H8A—C8—P1	103.7 (9)	H34A—C34—P3	102.8 (8)
C10—C8—P1	117.20 (7)	C36—C34—P3	114.77 (6)
C10—C8—H8A	105.9 (9)	C36—C34—H34A	108.9 (9)
C11—C8—P1	110.55 (7)	C37—C34—P3	113.46 (6)
C11—C8—H8A	107.4 (9)	C37—C34—H34A	105.4 (9)
C11—C8—C10	111.19 (9)	C37—C34—C36	110.65 (7)
H9A—C9—P1	104.2 (9)	H35A—C35—P3	105.1 (9)
C12—C9—P1	109.98 (6)	C38—C35—P3	108.60 (6)
C12—C9—H9A	108.2 (9)	C38—C35—H35A	110.1 (9)
C13—C9—P1	116.70 (7)	C39—C35—P3	113.29 (6)
C13—C9—H9A	108.6 (9)	C39—C35—H35A	108.1 (9)
C13—C9—C12	108.83 (9)	C39—C35—C38	111.53 (8)
H10A—C10—C8	112.5 (11)	H36A—C36—C34	112.6 (10)
H10B—C10—C8	109.2 (10)	H36B—C36—C34	110.9 (9)
H10B—C10—H10A	107.1 (16)	H36B—C36—H36A	107.9 (14)
H10C—C10—C8	113.3 (10)	H36C—C36—C34	109.8 (9)
H10C—C10—H10A	104.1 (16)	H36C—C36—H36A	109.2 (14)
H10C—C10—H10B	110.3 (14)	H36C—C36—H36B	106.2 (13)
H11A—C11—C8	106.9 (10)	H37A—C37—C34	110.4 (10)
H11B—C11—C8	112.8 (10)	H37B—C37—C34	109.4 (9)
H11B—C11—H11A	109.4 (15)	H37B—C37—H37A	108.8 (14)
H11C—C11—C8	112.5 (10)	H37C—C37—C34	113.6 (9)
H11C—C11—H11A	107.1 (16)	H37C—C37—H37A	105.9 (15)
H11C—C11—H11B	108.0 (14)	H37C—C37—H37B	108.7 (13)
H12A—C12—C9	108.3 (10)	H38A—C38—C35	110.3 (10)
H12B—C12—C9	108.1 (10)	H38B—C38—C35	110.8 (10)
H12B—C12—H12A	110.3 (14)	H38B—C38—H38A	106.1 (15)
H12C—C12—C9	107.9 (10)	H38C—C38—C35	109.0 (9)
H12C—C12—H12A	109.5 (15)	H38C—C38—H38A	110.7 (14)
H12C—C12—H12B	112.5 (13)	H38C—C38—H38B	109.9 (13)
H13A—C13—C9	111.2 (11)	H39A—C39—C35	113.5 (10)
H13B—C13—C9	115.6 (11)	H39B—C39—C35	110.0 (9)
H13B—C13—H13A	107.2 (15)	H39B—C39—H39A	110.9 (16)
H13C—C13—C9	111.3 (10)	H39C—C39—C35	113.5 (10)
H13C—C13—H13A	106.8 (15)	H39C—C39—H39A	102.1 (15)
H13C—C13—H13B	104.2 (15)	H39C—C39—H39B	106.4 (13)

(GOJNIF_HAR_SHADE3_1)

Crystal data

C39H62InN4NiP3	Dx = 1.415 Mg m^−3
Mr = 853.39	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, P212121	Cell parameters from 9537 reflections
a = 12.2127 (4) Å	θ = 2.3–36.4°
b = 14.5402 (5) Å	µ = 1.20 mm^−1
c = 22.5601 (8) Å	T = 100 K
V = 4006.1 (2) Å^3	Block, gold
Z = 4	0.14 × 0.08 × 0.06 mm
F(000) = 105.781

Data collection

Bruker Photon-II CMOS diffractometer	18741 reflections with I ≥ 2u(I)
φ and ω scans	Rint = 0.036
Absorption correction: multi-scan SADABS. R.Blessing, 1995	θmax = 36.4°, θmin = 2.3°
Tmin = 0.701, Tmax = 0.747	h = −20→20
237431 measured reflections	k = −24→24
19473 independent reflections	l = −37→37

Refinement

Refinement on F^2	0 constraints
Least-squares matrix: full	Only H-atom coordinates refined
R[F^2 > 2σ(F^2)] = 0.025	w = 1/[σ^2(Fo^2) + (0.1P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.091	(Δ/σ)max = 0.001
S = 0.81	Δρmax = 0.28 e Å^−3
19473 reflections	Δρmin = −1.33 e Å^−3
619 parameters	Absolute structure: Flack, H. D. (1983). Acta Cryst. A39, 876-881.
0 restraints	Absolute structure parameter: 0.231 (5)

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ni1	0.755786 (14)	0.598658 (12)	0.856175 (8)	0.00943 (3)
H1A	0.732 (4)	0.560 (3)	0.9253 (17)	0.032933
H1B	0.740 (4)	0.624 (3)	0.9285 (16)	0.032963
In1	0.798243 (7)	0.580827 (5)	0.749338 (4)	0.00930 (2)
P1	0.91844 (3)	0.52223 (2)	0.864360 (15)	0.00939 (5)
P2	0.59901 (3)	0.52857 (2)	0.829156 (15)	0.00947 (5)
P3	0.75363 (3)	0.75012 (2)	0.835668 (15)	0.00918 (5)
N1	0.96186 (9)	0.53386 (8)	0.74739 (6)	0.01099 (16)
N2	0.67673 (10)	0.48664 (9)	0.72030 (5)	0.01135 (18)
N3	0.78426 (10)	0.71625 (8)	0.71621 (5)	0.01067 (17)
N4	0.83422 (9)	0.56334 (8)	0.64688 (5)	0.00898 (16)
C1	0.95346 (10)	0.57160 (9)	0.64333 (6)	0.00938 (18)
C2	1.00509 (12)	0.59718 (10)	0.59116 (6)	0.0132 (2)
H2A	0.956 (3)	0.611 (2)	0.5552 (12)	0.026173
C3	1.11903 (12)	0.60874 (11)	0.58828 (6)	0.0148 (2)
H3A	1.172 (3)	0.630 (2)	0.5556 (13)	0.029180
C4	1.18048 (12)	0.59553 (10)	0.63980 (7)	0.0146 (2)
H4A	1.262 (2)	0.605 (2)	0.6377 (13)	0.029900
C5	1.12989 (11)	0.57056 (10)	0.69278 (6)	0.0128 (2)
H5A	1.180 (3)	0.564 (2)	0.7317 (13)	0.026790
C6	1.01537 (11)	0.55736 (9)	0.69641 (6)	0.0100 (2)
C7	1.01944 (12)	0.53670 (10)	0.80310 (6)	0.0116 (2)
H7A	1.059 (3)	0.600 (2)	0.8133 (13)	0.025617
H7B	1.085 (3)	0.483 (2)	0.8057 (13)	0.026373
C8	0.99550 (13)	0.56223 (11)	0.93117 (6)	0.0142 (2)
H8A	0.983 (2)	0.635 (2)	0.9291 (13)	0.023160
C9	0.91098 (12)	0.39470 (10)	0.87153 (7)	0.0139 (2)
H9A	0.851 (3)	0.382 (2)	0.9082 (13)	0.024073
C10	1.12026 (15)	0.55058 (15)	0.93054 (9)	0.0227 (3)
H10A	1.149 (3)	0.474 (2)	0.9294 (16)	0.032013
H10B	1.164 (3)	0.580 (2)	0.8972 (13)	0.029943
H10C	1.149 (3)	0.579 (3)	0.9806 (16)	0.033943
C11	0.94535 (18)	0.52143 (16)	0.98759 (8)	0.0262 (4)
H11A	0.998 (3)	0.550 (3)	1.0198 (13)	0.032467
H11B	0.860 (2)	0.528 (2)	0.9952 (14)	0.028553
H11C	0.960 (3)	0.448 (2)	0.9894 (14)	0.033707
C12	0.86456 (15)	0.35257 (11)	0.81432 (8)	0.0186 (3)
H12A	0.852 (3)	0.283 (2)	0.8258 (14)	0.030940
H12B	0.779 (3)	0.390 (2)	0.8026 (14)	0.028060
H12C	0.925 (3)	0.360 (2)	0.7813 (13)	0.029693
C13	1.01659 (16)	0.34496 (13)	0.88744 (10)	0.0239 (3)
H13A	1.004 (3)	0.272 (2)	0.8915 (15)	0.033140
H13B	1.087 (3)	0.367 (3)	0.8607 (14)	0.032587
H13C	1.054 (3)	0.355 (2)	0.9235 (13)	0.032957
C14	0.78948 (11)	0.47295 (9)	0.63327 (6)	0.00992 (18)
C15	0.82591 (12)	0.42276 (10)	0.58484 (6)	0.0123 (2)
H15A	0.896 (3)	0.456 (2)	0.5564 (13)	0.025920
C16	0.78539 (13)	0.33499 (10)	0.57248 (7)	0.0153 (2)
H16A	0.810 (3)	0.301 (2)	0.5314 (14)	0.029147
C17	0.70733 (13)	0.29742 (10)	0.61055 (7)	0.0158 (2)
H17A	0.668 (3)	0.229 (2)	0.5970 (15)	0.030350
C18	0.67022 (13)	0.34625 (10)	0.65968 (7)	0.0142 (2)
H18A	0.615 (3)	0.315 (2)	0.6915 (13)	0.027480
C19	0.70911 (11)	0.43560 (9)	0.67263 (6)	0.01043 (19)
C20	0.60314 (11)	0.44849 (10)	0.76429 (6)	0.0118 (2)
H20A	0.628 (3)	0.376 (2)	0.7803 (14)	0.026297
H20B	0.520 (2)	0.440 (2)	0.7453 (13)	0.027083
C21	0.53637 (12)	0.45618 (10)	0.88806 (6)	0.0134 (2)
H21A	0.463 (3)	0.421 (2)	0.8675 (13)	0.026133
C22	0.48074 (11)	0.60408 (10)	0.80768 (6)	0.0123 (2)
H22A	0.480 (3)	0.659 (2)	0.8417 (13)	0.023530
C23	0.61423 (15)	0.38117 (13)	0.91011 (7)	0.0203 (3)
H23A	0.574 (3)	0.341 (2)	0.9450 (14)	0.033403
H23B	0.635 (3)	0.329 (2)	0.8733 (14)	0.030193
H23C	0.684 (3)	0.414 (2)	0.9314 (15)	0.030337
C24	0.49905 (15)	0.51671 (12)	0.94003 (7)	0.0186 (3)
H24A	0.440 (3)	0.575 (3)	0.9219 (15)	0.030587
H24B	0.458 (3)	0.476 (2)	0.9703 (13)	0.033750
H24C	0.565 (3)	0.551 (2)	0.9633 (14)	0.029967
C25	0.49927 (13)	0.64744 (12)	0.74684 (8)	0.0173 (2)
H25A	0.439 (3)	0.699 (2)	0.7355 (14)	0.031203
H25B	0.574 (2)	0.678 (2)	0.7386 (13)	0.027960
H25C	0.497 (3)	0.589 (2)	0.7157 (14)	0.030697
C26	0.36780 (12)	0.55804 (12)	0.80856 (8)	0.0171 (3)
H26A	0.301 (3)	0.607 (2)	0.8026 (15)	0.034020
H26B	0.365 (3)	0.503 (2)	0.7761 (14)	0.033997
H26C	0.337 (3)	0.527 (3)	0.8488 (13)	0.033143
C27	0.77563 (11)	0.64134 (9)	0.62082 (6)	0.01047 (19)
C28	0.74267 (14)	0.63999 (10)	0.56205 (6)	0.0144 (2)
H28A	0.750 (3)	0.574 (2)	0.5366 (13)	0.026503
C29	0.69216 (15)	0.71651 (11)	0.53615 (7)	0.0182 (3)
H29A	0.663 (3)	0.708 (2)	0.4939 (12)	0.030493
C30	0.67555 (14)	0.79446 (11)	0.57063 (7)	0.0170 (3)
H30A	0.637 (3)	0.859 (3)	0.5432 (15)	0.031337
C31	0.70544 (12)	0.79587 (10)	0.63021 (6)	0.0134 (2)
H31A	0.692 (3)	0.856 (2)	0.6470 (12)	0.027447
C32	0.75541 (11)	0.71941 (9)	0.65751 (6)	0.01039 (19)
C33	0.74806 (12)	0.78793 (8)	0.75563 (6)	0.01161 (19)
H33A	0.658 (3)	0.804 (2)	0.7483 (14)	0.025540
H33B	0.801 (2)	0.848 (2)	0.7508 (12)	0.026013
C34	0.62768 (12)	0.80867 (10)	0.86343 (6)	0.0119 (2)
H34A	0.562 (3)	0.783 (2)	0.8335 (13)	0.023143
C35	0.86861 (12)	0.82273 (10)	0.86214 (7)	0.0132 (2)
H35A	0.845 (3)	0.889 (2)	0.8459 (13)	0.024117
C36	0.63049 (13)	0.91382 (10)	0.85994 (7)	0.0163 (2)
H36A	0.658 (3)	0.940 (2)	0.8265 (12)	0.031200
H36B	0.547 (3)	0.932 (2)	0.8720 (16)	0.031940
H36C	0.683 (3)	0.940 (2)	0.8946 (14)	0.031447
C37	0.59266 (15)	0.77694 (11)	0.92545 (7)	0.0180 (3)
H37A	0.516 (3)	0.807 (3)	0.9352 (14)	0.029693
H37B	0.589 (3)	0.706 (2)	0.9319 (13)	0.027917
H37C	0.645 (3)	0.799 (2)	0.9556 (12)	0.029467
C38	0.97448 (13)	0.78997 (12)	0.83206 (7)	0.0170 (2)
H38A	1.032 (3)	0.838 (2)	0.8393 (14)	0.030140
H38B	0.993 (3)	0.727 (2)	0.8529 (14)	0.028413
H38C	0.963 (3)	0.777 (2)	0.7811 (14)	0.028310
C39	0.87987 (14)	0.82434 (12)	0.92961 (7)	0.0181 (3)
H39A	0.943 (3)	0.870 (3)	0.9479 (14)	0.031073
H39B	0.814 (3)	0.858 (2)	0.9492 (13)	0.031150
H39C	0.876 (3)	0.755 (2)	0.9479 (14)	0.029307

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ni1	0.00868 (6)	0.00821 (6)	0.01140 (7)	−0.00034 (5)	0.00037 (5)	−0.00001 (5)
H1A	0.043840	0.032000	0.022960	−0.006910	0.003470	0.004980
H1B	0.046820	0.029800	0.022270	−0.002710	0.000520	−0.005120
In1	0.00952 (4)	0.00876 (4)	0.00961 (4)	0.00009 (2)	0.00013 (3)	−0.00013 (3)
P1	0.01007 (12)	0.00966 (12)	0.00844 (12)	0.00076 (10)	−0.00067 (10)	0.00063 (10)
P2	0.00875 (12)	0.01086 (13)	0.00881 (12)	−0.00171 (10)	0.00051 (10)	−0.00018 (10)
P3	0.01108 (13)	0.00768 (11)	0.00876 (12)	−0.00026 (11)	−0.00057 (10)	−0.00083 (9)
N1	0.0093 (4)	0.0137 (4)	0.0100 (4)	0.0009 (3)	0.0001 (4)	0.0015 (4)
N2	0.0119 (4)	0.0122 (4)	0.0099 (4)	−0.0018 (4)	0.0014 (3)	−0.0024 (3)
N3	0.0146 (5)	0.0088 (4)	0.0086 (4)	0.0017 (4)	−0.0010 (3)	0.0004 (3)
N4	0.0107 (4)	0.0090 (4)	0.0073 (4)	0.0011 (3)	−0.0013 (3)	0.0001 (3)
C1	0.0096 (4)	0.0096 (4)	0.0090 (4)	0.0005 (4)	0.0020 (4)	0.0002 (4)
C2	0.0144 (5)	0.0136 (5)	0.0115 (5)	−0.0001 (4)	0.0031 (4)	0.0002 (4)
H2A	0.026740	0.032290	0.019490	0.001230	−0.001140	0.002660
C3	0.0146 (5)	0.0165 (6)	0.0133 (5)	−0.0013 (5)	0.0041 (4)	0.0011 (4)
H3A	0.028530	0.036710	0.022300	−0.002590	0.008720	0.002720
C4	0.0114 (5)	0.0154 (5)	0.0169 (5)	−0.0009 (4)	0.0038 (4)	0.0009 (5)
H4A	0.017840	0.040640	0.031220	−0.003270	0.004440	−0.000140
C5	0.0101 (5)	0.0155 (5)	0.0128 (5)	0.0002 (4)	0.0008 (4)	0.0007 (4)
H5A	0.020880	0.036310	0.023180	−0.000220	−0.002380	0.001550
C6	0.0096 (5)	0.0108 (5)	0.0096 (5)	0.0006 (4)	0.0014 (4)	0.0004 (4)
C7	0.0107 (5)	0.0143 (5)	0.0099 (5)	0.0005 (4)	0.0004 (4)	0.0004 (4)
H7A	0.024920	0.025410	0.026520	−0.007350	−0.001590	−0.001430
H7B	0.023130	0.028200	0.027790	0.009260	−0.000810	0.001380
C8	0.0154 (5)	0.0160 (6)	0.0112 (5)	−0.0014 (4)	−0.0020 (4)	−0.0006 (4)
H8A	0.023880	0.020980	0.024620	0.000790	−0.001660	−0.000460
C9	0.0154 (5)	0.0108 (5)	0.0154 (5)	0.0016 (4)	−0.0001 (4)	0.0028 (4)
H9A	0.025820	0.025000	0.021400	0.000670	0.003690	0.003120
C10	0.0161 (6)	0.0298 (8)	0.0222 (7)	0.0002 (6)	−0.0083 (5)	−0.0036 (6)
H10A	0.028990	0.026710	0.040340	0.006980	−0.001360	0.001020
H10B	0.024340	0.036450	0.029040	0.000480	0.001980	0.008010
H10C	0.026650	0.049710	0.025470	0.001110	−0.008110	−0.007630
C11	0.0330 (9)	0.0343 (9)	0.0112 (6)	−0.0104 (8)	0.0003 (6)	0.0006 (6)
H11A	0.033260	0.044100	0.020040	−0.005870	−0.006750	−0.000640
H11B	0.020770	0.036000	0.028890	0.002880	0.000890	0.005010
H11C	0.045760	0.022630	0.032730	0.006210	0.004800	0.004840
C12	0.0250 (7)	0.0121 (5)	0.0187 (6)	−0.0007 (5)	−0.0016 (5)	−0.0024 (5)
H12A	0.046090	0.015950	0.030780	−0.003060	−0.002580	0.002690
H12B	0.024270	0.029780	0.030130	0.008170	−0.005390	−0.002730
H12C	0.026600	0.038900	0.023580	−0.004230	0.007180	−0.001680
C13	0.0195 (7)	0.0150 (6)	0.0373 (10)	0.0049 (5)	−0.0050 (7)	0.0054 (6)
H13A	0.037190	0.020260	0.041970	0.005270	−0.003980	0.003940
H13B	0.026460	0.040480	0.030820	0.006680	0.005990	0.009580
H13C	0.035720	0.040150	0.023000	0.008980	−0.007740	−0.002200
C14	0.0123 (5)	0.0086 (4)	0.0089 (4)	0.0016 (4)	0.0001 (4)	−0.0012 (4)
C15	0.0154 (5)	0.0119 (5)	0.0097 (5)	−0.0002 (4)	0.0007 (4)	−0.0018 (4)
H15A	0.028030	0.025870	0.023860	−0.003020	0.006990	−0.001480
C16	0.0195 (6)	0.0131 (5)	0.0133 (5)	−0.0009 (5)	0.0012 (4)	−0.0055 (4)
H16A	0.036300	0.026870	0.024270	−0.000720	0.005700	−0.009510
C17	0.0178 (6)	0.0124 (5)	0.0172 (6)	−0.0031 (5)	0.0003 (5)	−0.0049 (4)
H17A	0.037560	0.021450	0.032040	−0.008320	0.003230	−0.008260
C18	0.0146 (5)	0.0121 (5)	0.0160 (5)	−0.0029 (4)	0.0008 (4)	−0.0040 (4)
H18A	0.029490	0.025630	0.027320	−0.007940	0.006820	−0.002860
C19	0.0107 (5)	0.0109 (5)	0.0097 (4)	−0.0005 (4)	0.0003 (4)	−0.0022 (4)
C20	0.0107 (5)	0.0131 (5)	0.0117 (5)	−0.0032 (4)	0.0017 (4)	−0.0016 (4)
H20A	0.031780	0.018810	0.028300	−0.000250	0.002950	0.002210
H20B	0.018840	0.034450	0.027960	−0.005470	−0.002300	−0.004060
C21	0.0129 (5)	0.0161 (6)	0.0113 (5)	−0.0036 (4)	0.0007 (4)	0.0011 (4)
H21A	0.021880	0.028310	0.028210	−0.007420	−0.000160	−0.003290
C22	0.0095 (4)	0.0155 (5)	0.0120 (5)	0.0005 (4)	0.0010 (4)	−0.0021 (4)
H22A	0.023290	0.025250	0.022050	0.000210	0.000980	−0.005670
C23	0.0213 (7)	0.0220 (7)	0.0175 (6)	0.0002 (6)	0.0027 (5)	0.0070 (5)
H23A	0.034620	0.030250	0.035340	−0.005040	0.010730	0.011730
H23B	0.036770	0.028370	0.025440	0.003660	0.003760	−0.005620
H23C	0.028730	0.025530	0.036750	−0.004660	−0.008490	−0.002600
C24	0.0244 (7)	0.0213 (7)	0.0102 (5)	−0.0060 (6)	0.0030 (5)	−0.0013 (5)
H24A	0.028520	0.031680	0.031560	0.006840	−0.001560	−0.002660
H24B	0.041060	0.031660	0.028530	−0.008630	0.014170	0.001890
H24C	0.022040	0.036950	0.030910	−0.005740	−0.001150	−0.009110
C25	0.0167 (5)	0.0196 (6)	0.0156 (6)	0.0027 (4)	−0.0016 (5)	0.0025 (5)
H25A	0.026690	0.036660	0.030260	0.013970	0.000250	0.003440
H25B	0.020000	0.036130	0.027750	−0.006680	−0.000690	0.002270
H25C	0.041860	0.027410	0.022820	−0.002800	−0.000310	−0.008220
C26	0.0104 (5)	0.0222 (7)	0.0187 (6)	−0.0020 (5)	−0.0011 (4)	−0.0028 (5)
H26A	0.019680	0.037190	0.045190	0.003670	−0.002970	0.000680
H26B	0.027840	0.037740	0.036410	−0.006710	0.004290	−0.017020
H26C	0.027980	0.046420	0.025030	−0.008930	0.004290	0.002010
C27	0.0143 (5)	0.0092 (4)	0.0079 (4)	0.0017 (4)	−0.0007 (4)	0.0000 (4)
C28	0.0210 (6)	0.0128 (5)	0.0095 (5)	0.0039 (5)	−0.0024 (4)	−0.0012 (4)
H28A	0.034740	0.023440	0.021330	0.005780	−0.001050	−0.005150
C29	0.0270 (7)	0.0173 (6)	0.0104 (5)	0.0080 (5)	−0.0059 (5)	−0.0007 (4)
H29A	0.041440	0.033560	0.016480	0.008330	−0.004910	0.000270
C30	0.0244 (7)	0.0151 (6)	0.0114 (5)	0.0081 (5)	−0.0036 (5)	0.0008 (4)
H30A	0.043580	0.025880	0.024550	0.013290	−0.003390	0.004630
C31	0.0180 (6)	0.0112 (5)	0.0109 (5)	0.0047 (4)	−0.0008 (4)	0.0007 (4)
H31A	0.038770	0.020490	0.023080	0.007920	−0.000530	−0.002830
C32	0.0122 (5)	0.0094 (4)	0.0096 (4)	0.0015 (4)	−0.0007 (4)	0.0005 (3)
C33	0.0160 (5)	0.0084 (4)	0.0104 (5)	0.0011 (4)	0.0003 (4)	−0.0006 (4)
H33A	0.023710	0.027880	0.025030	0.008280	−0.001490	−0.000790
H33B	0.033370	0.018100	0.026570	−0.005110	0.003520	−0.000060
C34	0.0141 (5)	0.0111 (5)	0.0104 (5)	0.0008 (4)	0.0004 (4)	−0.0006 (4)
H34A	0.023160	0.024730	0.021540	0.001030	−0.002700	−0.002790
C35	0.0149 (5)	0.0109 (5)	0.0139 (5)	−0.0019 (4)	−0.0005 (4)	−0.0018 (4)
H35A	0.030700	0.016710	0.024940	−0.000010	0.001460	0.000540
C36	0.0199 (6)	0.0121 (5)	0.0167 (6)	0.0031 (5)	0.0016 (5)	−0.0005 (4)
H36A	0.046120	0.025110	0.022370	0.001250	0.007700	0.002240
H36B	0.028490	0.026150	0.041180	0.008620	0.004860	−0.002530
H36C	0.039600	0.025130	0.029610	−0.001690	−0.009670	−0.004310
C37	0.0238 (7)	0.0167 (6)	0.0134 (5)	−0.0009 (5)	0.0042 (5)	−0.0008 (5)
H37A	0.024520	0.036080	0.028480	0.009870	0.005920	0.000070
H37B	0.037740	0.018650	0.027360	−0.002000	0.003910	−0.000780
H37C	0.029190	0.037100	0.022110	−0.007190	−0.004980	−0.002480
C38	0.0153 (6)	0.0185 (6)	0.0172 (6)	−0.0046 (5)	0.0014 (5)	−0.0035 (5)
H38A	0.025710	0.024790	0.039920	−0.010640	0.004210	−0.007270
H38B	0.031210	0.022530	0.031500	0.003840	0.004460	0.007100
H38C	0.030190	0.036580	0.018160	0.001290	−0.000160	−0.004690
C39	0.0192 (6)	0.0202 (6)	0.0149 (6)	−0.0031 (5)	−0.0030 (5)	−0.0043 (5)
H39A	0.028660	0.036800	0.027760	−0.013140	−0.002870	−0.004160
H39B	0.032180	0.035400	0.025870	0.009220	0.004590	−0.005160
H39C	0.043460	0.018950	0.025510	−0.002380	−0.001140	0.002110

Geometric parameters (Å, º)

Ni1—H1A	1.68 (4)	C14—C19	1.4306 (19)
Ni1—H1B	1.68 (4)	C15—H15A	1.18 (3)
Ni1—In1	2.4790 (2)	C15—C16	1.397 (2)
Ni1—P1	2.2836 (4)	C16—H16A	1.09 (3)
Ni1—P2	2.2530 (4)	C16—C17	1.395 (2)
Ni1—P3	2.2505 (4)	C17—H17A	1.15 (3)
H1A—H1B	0.94 (5)	C17—C18	1.392 (2)
In1—N1	2.1121 (11)	C18—H18A	1.09 (3)
In1—N2	2.1230 (12)	C18—C19	1.414 (2)
In1—N3	2.1131 (12)	C20—H20A	1.15 (3)
In1—N4	2.3667 (11)	C20—H20B	1.11 (3)
P1—C7	1.8643 (14)	C21—H21A	1.13 (3)
P1—C8	1.8697 (15)	C21—C23	1.530 (2)
P1—C9	1.8636 (15)	C21—C24	1.535 (2)
P2—C20	1.8707 (14)	C22—H22A	1.11 (3)
P2—C21	1.8599 (14)	C22—C25	1.527 (2)
P2—C22	1.8780 (14)	C22—C26	1.533 (2)
P3—C33	1.8888 (14)	C23—H23A	1.10 (3)
P3—C34	1.8664 (14)	C23—H23B	1.15 (3)
P3—C35	1.8555 (15)	C23—H23C	1.09 (3)
N1—C6	1.3662 (18)	C24—H24A	1.19 (4)
N1—C7	1.4408 (19)	C24—H24B	1.03 (3)
N2—C19	1.3652 (17)	C24—H24C	1.09 (3)
N2—C20	1.4492 (18)	C25—H25A	1.09 (3)
N3—C32	1.3713 (17)	C25—H25B	1.03 (3)
N3—C33	1.4395 (17)	C25—H25C	1.10 (3)
N4—C1	1.4633 (17)	C26—H26A	1.09 (3)
N4—C14	1.4561 (17)	C26—H26B	1.08 (3)
N4—C27	1.4642 (17)	C26—H26C	1.08 (3)
C1—C2	1.3860 (19)	C27—C28	1.3858 (19)
C1—C6	1.4314 (19)	C27—C32	1.4264 (19)
C2—H2A	1.03 (3)	C28—H28A	1.12 (3)
C2—C3	1.403 (2)	C28—C29	1.400 (2)
C3—H3A	1.03 (3)	C29—H29A	1.03 (3)
C3—C4	1.397 (2)	C29—C30	1.390 (2)
C4—H4A	1.00 (3)	C30—H30A	1.22 (3)
C4—C5	1.394 (2)	C30—C31	1.393 (2)
C5—H5A	1.07 (3)	C31—H31A	0.97 (3)
C5—C6	1.414 (2)	C31—C32	1.4098 (19)
C7—H7A	1.06 (3)	C33—H33A	1.13 (3)
C7—H7B	1.12 (3)	C33—H33B	1.09 (3)
C8—H8A	1.07 (3)	C34—H34A	1.12 (3)
C8—C10	1.533 (2)	C34—C36	1.531 (2)
C8—C11	1.532 (2)	C34—C37	1.534 (2)
C9—H9A	1.12 (3)	C35—H35A	1.08 (3)
C9—C12	1.537 (2)	C35—C38	1.536 (2)
C9—C13	1.522 (2)	C35—C39	1.528 (2)
C10—H10A	1.16 (3)	C36—H36A	0.92 (3)
C10—H10B	1.01 (3)	C36—H36B	1.09 (3)
C10—H10C	1.26 (3)	C36—H36C	1.08 (3)
C11—H11A	1.06 (3)	C37—H37A	1.06 (3)
C11—H11B	1.06 (3)	C37—H37B	1.04 (3)
C11—H11C	1.08 (3)	C37—H37C	0.99 (3)
C12—H12A	1.05 (3)	C38—H38A	1.01 (3)
C12—H12B	1.20 (3)	C38—H38B	1.06 (3)
C12—H12C	1.05 (3)	C38—H38C	1.17 (3)
C13—H13A	1.07 (3)	C39—H39A	1.09 (3)
C13—H13B	1.10 (3)	C39—H39B	1.04 (3)
C13—H13C	0.94 (3)	C39—H39C	1.10 (3)
C14—C15	1.3872 (18)
H1B—Ni1—H1A	32.5 (17)	C15—C14—N4	121.37 (12)
In1—Ni1—H1A	154.5 (14)	C19—C14—N4	117.98 (11)
In1—Ni1—H1B	171.3 (15)	C19—C14—C15	120.62 (12)
P1—Ni1—H1A	85.1 (16)	H15A—C15—C14	116.4 (16)
P1—Ni1—H1B	97.5 (16)	C16—C15—C14	121.61 (13)
P1—Ni1—In1	81.129 (10)	C16—C15—H15A	121.9 (16)
P2—Ni1—H1A	87.3 (15)	H16A—C16—C15	119.2 (17)
P2—Ni1—H1B	105.4 (16)	C17—C16—C15	118.50 (13)
P2—Ni1—In1	82.380 (10)	C17—C16—H16A	122.0 (17)
P2—Ni1—P1	122.749 (15)	H17A—C17—C16	117.5 (17)
P3—Ni1—H1A	120.9 (14)	C18—C17—C16	120.87 (13)
P3—Ni1—H1B	88.8 (14)	C18—C17—H17A	121.2 (17)
P3—Ni1—In1	84.544 (10)	H18A—C18—C17	120.8 (17)
P3—Ni1—P1	120.198 (15)	C19—C18—C17	121.59 (14)
P3—Ni1—P2	112.155 (15)	C19—C18—H18A	117.4 (17)
H1B—H1A—Ni1	74 (4)	C14—C19—N2	118.78 (12)
H1A—H1B—Ni1	74 (4)	C18—C19—N2	124.40 (13)
N1—In1—Ni1	104.59 (3)	C18—C19—C14	116.81 (12)
N2—In1—Ni1	102.78 (3)	N2—C20—P2	108.31 (9)
N2—In1—N1	116.51 (5)	H20A—C20—P2	109.3 (16)
N3—In1—Ni1	103.27 (3)	H20A—C20—N2	113.7 (16)
N3—In1—N1	111.74 (5)	H20B—C20—P2	110.4 (16)
N3—In1—N2	115.82 (5)	H20B—C20—N2	110.3 (16)
N4—In1—Ni1	178.62 (3)	H20B—C20—H20A	105 (3)
N4—In1—N1	76.66 (4)	H21A—C21—P2	106.7 (16)
N4—In1—N2	76.06 (4)	C23—C21—P2	112.33 (10)
N4—In1—N3	76.69 (4)	C23—C21—H21A	107.7 (17)
C7—P1—Ni1	117.43 (5)	C24—C21—P2	110.09 (11)
C8—P1—Ni1	110.59 (5)	C24—C21—H21A	109.8 (16)
C8—P1—C7	103.27 (7)	C24—C21—C23	110.18 (13)
C9—P1—Ni1	116.66 (5)	H22A—C22—P2	104.5 (16)
C9—P1—C7	102.06 (7)	C25—C22—P2	111.05 (10)
C9—P1—C8	105.32 (7)	C25—C22—H22A	108.9 (16)
C20—P2—Ni1	118.05 (5)	C26—C22—P2	115.67 (11)
C21—P2—Ni1	114.34 (5)	C26—C22—H22A	107.4 (17)
C21—P2—C20	102.58 (6)	C26—C22—C25	108.97 (12)
C22—P2—Ni1	117.32 (5)	H23A—C23—C21	109.5 (19)
C22—P2—C20	100.54 (6)	H23B—C23—C21	111.9 (17)
C22—P2—C21	101.47 (7)	H23B—C23—H23A	105 (2)
C33—P3—Ni1	118.80 (4)	H23C—C23—C21	108.3 (18)
C34—P3—Ni1	112.77 (5)	H23C—C23—H23A	106 (3)
C34—P3—C33	99.11 (6)	H23C—C23—H23B	116 (3)
C35—P3—Ni1	118.80 (5)	H24A—C24—C21	109.2 (17)
C35—P3—C33	99.75 (6)	H24B—C24—C21	108.6 (18)
C35—P3—C34	104.84 (6)	H24B—C24—H24A	110 (3)
C6—N1—In1	112.91 (9)	H24C—C24—C21	114.5 (17)
C7—N1—In1	115.74 (9)	H24C—C24—H24A	106 (3)
C7—N1—C6	119.58 (11)	H24C—C24—H24B	108 (3)
C19—N2—In1	113.03 (9)	H25A—C25—C22	113.4 (17)
C20—N2—In1	117.97 (8)	H25B—C25—C22	118.0 (17)
C20—N2—C19	120.74 (12)	H25B—C25—H25A	105 (3)
C32—N3—In1	113.18 (9)	H25C—C25—C22	104.7 (17)
C33—N3—In1	118.75 (8)	H25C—C25—H25A	111 (3)
C33—N3—C32	119.57 (11)	H25C—C25—H25B	104 (2)
C1—N4—In1	103.26 (8)	H26A—C26—C22	112.8 (18)
C14—N4—In1	103.49 (8)	H26B—C26—C22	109.8 (18)
C14—N4—C1	115.85 (10)	H26B—C26—H26A	112 (3)
C27—N4—In1	102.60 (7)	H26C—C26—C22	120.5 (18)
C27—N4—C1	113.63 (11)	H26C—C26—H26A	96 (3)
C27—N4—C14	115.54 (10)	H26C—C26—H26B	105 (3)
C2—C1—N4	121.42 (12)	C28—C27—N4	121.00 (12)
C6—C1—N4	117.91 (11)	C32—C27—N4	117.92 (11)
C6—C1—C2	120.59 (12)	C32—C27—C28	121.07 (12)
H2A—C2—C1	117.0 (17)	H28A—C28—C27	118.5 (16)
C3—C2—C1	121.51 (14)	C29—C28—C27	121.07 (13)
C3—C2—H2A	121.4 (17)	C29—C28—H28A	120.2 (16)
H3A—C3—C2	133.7 (19)	H29A—C29—C28	116.3 (17)
C4—C3—C2	118.55 (13)	C30—C29—C28	118.62 (13)
C4—C3—H3A	107.6 (18)	C30—C29—H29A	124.7 (17)
H4A—C4—C3	118.3 (17)	H30A—C30—C29	113.5 (17)
C5—C4—C3	120.75 (13)	C31—C30—C29	120.93 (13)
C5—C4—H4A	121.0 (17)	C31—C30—H30A	125.6 (17)
H5A—C5—C4	118.2 (17)	H31A—C31—C30	110.2 (17)
C6—C5—C4	121.57 (13)	C32—C31—C30	121.55 (13)
C6—C5—H5A	120.1 (17)	C32—C31—H31A	128.0 (17)
C1—C6—N1	119.19 (12)	C27—C32—N3	119.29 (11)
C5—C6—N1	123.77 (13)	C31—C32—N3	124.02 (12)
C5—C6—C1	117.02 (12)	C31—C32—C27	116.69 (11)
N1—C7—P1	108.70 (9)	N3—C33—P3	111.64 (9)
H7A—C7—P1	103.5 (17)	H33A—C33—P3	103.5 (16)
H7A—C7—N1	115.7 (16)	H33A—C33—N3	110.7 (16)
H7B—C7—P1	110.8 (15)	H33B—C33—P3	107.9 (15)
H7B—C7—N1	112.0 (16)	H33B—C33—N3	109.7 (15)
H7B—C7—H7A	106 (2)	H33B—C33—H33A	113 (2)
H8A—C8—P1	101.6 (15)	H34A—C34—P3	103.6 (16)
C10—C8—P1	117.28 (12)	C36—C34—P3	114.82 (10)
C10—C8—H8A	104.5 (16)	C36—C34—H34A	108.9 (16)
C11—C8—P1	110.37 (11)	C37—C34—P3	113.49 (10)
C11—C8—H8A	111.2 (16)	C37—C34—H34A	104.5 (16)
C11—C8—C10	111.24 (15)	C37—C34—C36	110.70 (12)
H9A—C9—P1	104.7 (17)	H35A—C35—P3	101.5 (17)
C12—C9—P1	109.98 (10)	C38—C35—P3	108.56 (10)
C12—C9—H9A	108.4 (16)	C38—C35—H35A	110.8 (16)
C13—C9—P1	116.87 (12)	C39—C35—P3	113.41 (11)
C13—C9—H9A	107.8 (16)	C39—C35—H35A	110.5 (16)
C13—C9—C12	108.74 (14)	C39—C35—C38	111.66 (13)
H10A—C10—C8	113.7 (18)	H36A—C36—C34	118.3 (19)
H10B—C10—C8	118.8 (18)	H36B—C36—C34	102.2 (19)
H10B—C10—H10A	103 (3)	H36B—C36—H36A	117 (3)
H10C—C10—C8	103.6 (17)	H36C—C36—C34	109.4 (18)
H10C—C10—H10A	105 (3)	H36C—C36—H36A	103 (3)
H10C—C10—H10B	112 (3)	H36C—C36—H36B	107 (3)
H11A—C11—C8	100.1 (18)	H37A—C37—C34	108.2 (18)
H11B—C11—C8	119.7 (17)	H37B—C37—C34	115.9 (16)
H11B—C11—H11A	117 (3)	H37B—C37—H37A	110 (3)
H11C—C11—C8	110.3 (17)	H37C—C37—C34	110.4 (18)
H11C—C11—H11A	105 (3)	H37C—C37—H37A	107 (3)
H11C—C11—H11B	104 (3)	H37C—C37—H37B	105 (3)
H12A—C12—C9	103.3 (17)	H38A—C38—C35	107.2 (18)
H12B—C12—C9	108.9 (16)	H38B—C38—C35	104.5 (17)
H12B—C12—H12A	111 (3)	H38B—C38—H38A	113 (3)
H12C—C12—C9	107.3 (18)	H38C—C38—C35	112.4 (17)
H12C—C12—H12A	112 (3)	H38C—C38—H38A	111 (3)
H12C—C12—H12B	114 (2)	H38C—C38—H38B	109 (2)
H13A—C13—C9	111.8 (19)	H39A—C39—C35	116.7 (17)
H13B—C13—C9	113.2 (17)	H39B—C39—C35	111.2 (17)
H13B—C13—H13A	117 (3)	H39B—C39—H39A	96 (3)
H13C—C13—C9	122 (2)	H39C—C39—C35	110.9 (17)
H13C—C13—H13A	99 (3)	H39C—C39—H39A	117 (3)
H13C—C13—H13B	93 (3)	H39C—C39—H39B	104 (3)
In1—N1—C6—C1	−26.60 (10)	N2—C19—C18—C17	−179.40 (14)
In1—N1—C6—C5	152.09 (9)	N3—C32—C27—N4	−4.49 (15)
In1—N1—C7—P1	29.30 (7)	N3—C32—C27—C28	176.68 (13)
In1—N2—C19—C14	−26.60 (11)	N3—C32—C31—C30	−178.48 (15)
In1—N2—C19—C18	151.99 (10)	N4—C1—C2—C3	177.39 (13)
In1—N2—C20—P2	23.07 (8)	N4—C1—C6—C5	−176.65 (12)
In1—N3—C32—C27	−22.08 (11)	N4—C14—C15—C16	178.26 (13)
In1—N3—C32—C31	157.54 (10)	N4—C14—C19—C18	−177.58 (12)
In1—N3—C33—P3	14.31 (9)	N4—C27—C28—C29	−176.35 (15)
In1—N4—C1—C2	−157.14 (8)	N4—C27—C32—C31	175.86 (12)
In1—N4—C1—C6	19.47 (9)	C1—C2—C3—C4	−1.17 (17)
In1—N4—C14—C15	−156.94 (8)	C1—C6—C5—C4	−0.55 (15)
In1—N4—C14—C19	20.89 (9)	C2—C3—C4—C5	0.61 (17)
In1—N4—C27—C28	−156.96 (9)	C3—C4—C5—C6	0.25 (17)
In1—N4—C27—C32	24.22 (9)	C14—C15—C16—C17	−0.72 (17)
P1—C7—N1—C6	169.71 (9)	C14—C19—C18—C17	−0.79 (15)
P2—C20—N2—C19	169.29 (9)	C15—C16—C17—C18	0.20 (18)
P3—C33—N3—C32	160.14 (9)	C16—C17—C18—C19	0.56 (19)
N1—C6—C1—N4	2.13 (15)	C27—C28—C29—C30	0.03 (19)
N1—C6—C1—C2	178.78 (13)	C27—C32—C31—C30	1.14 (16)
N1—C6—C5—C4	−179.27 (14)	C28—C29—C30—C31	−1.9 (2)
N2—C19—C14—N4	1.12 (14)	C29—C30—C31—C32	1.3 (2)
N2—C19—C14—C15	178.97 (12)

(GOJNIF_HAR_SHADE3)

Crystal data

C39H62InN4NiP3	Dx = 1.415 Mg m^−3
Mr = 853.39	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, P212121	Cell parameters from 9537 reflections
a = 12.2127 (4) Å	θ = 2.3–36.4°
b = 14.5402 (5) Å	µ = 1.20 mm^−1
c = 22.5601 (8) Å	T = 100 K
V = 4006.1 (2) Å^3	Block, gold
Z = 4	0.14 × 0.08 × 0.06 mm
F(000) = 1787.122

Data collection

Bruker Photon-II CMOS diffractometer	18741 reflections with I ≥ 2u(I)
φ and ω scans	Rint = 0.036
Absorption correction: multi-scan SADABS. R.Blessing, 1995	θmax = 36.4°, θmin = 2.3°
Tmin = 0.701, Tmax = 0.747	h = −20→20
237431 measured reflections	k = −24→24
19473 independent reflections	l = −37→37

Refinement

Refinement on F^2	0 constraints
Least-squares matrix: full	Only H-atom coordinates refined
R[F^2 > 2σ(F^2)] = 0.025	w = 1/[σ^2(Fo^2) + (0.1P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.091	(Δ/σ)max = 0.001
S = 0.81	Δρmax = 0.28 e Å^−3
19473 reflections	Δρmin = −1.33 e Å^−3
619 parameters	Absolute structure: Flack, H. D. (1983). Acta Cryst. A39, 876-881.
0 restraints	Absolute structure parameter: 0.231 (5)

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ni1	0.755786 (14)	0.598658 (12)	0.856175 (8)	0.00943 (3)
H1A	0.732 (4)	0.560 (3)	0.9253 (17)	0.032777
H1B	0.740 (4)	0.624 (3)	0.9284 (16)	0.032880
In1	0.798243 (7)	0.580827 (5)	0.749338 (4)	0.00930 (2)
P1	0.91844 (3)	0.52223 (2)	0.864360 (15)	0.00939 (5)
P2	0.59901 (3)	0.52856 (2)	0.829156 (15)	0.00947 (5)
P3	0.75363 (3)	0.75012 (2)	0.835668 (15)	0.00918 (5)
N1	0.96186 (9)	0.53386 (8)	0.74739 (6)	0.01099 (16)
N2	0.67672 (10)	0.48664 (9)	0.72030 (5)	0.01135 (18)
N3	0.78425 (10)	0.71625 (8)	0.71621 (5)	0.01067 (17)
N4	0.83422 (9)	0.56334 (8)	0.64688 (5)	0.00897 (16)
C1	0.95346 (10)	0.57160 (9)	0.64333 (6)	0.00939 (18)
C2	1.00509 (12)	0.59718 (10)	0.59116 (6)	0.0132 (2)
H2A	0.955 (3)	0.611 (2)	0.5552 (12)	0.026547
C3	1.11903 (12)	0.60874 (11)	0.58829 (6)	0.0148 (2)
H3A	1.172 (3)	0.630 (2)	0.5556 (13)	0.029823
C4	1.18047 (12)	0.59553 (10)	0.63980 (7)	0.0146 (2)
H4A	1.262 (2)	0.605 (2)	0.6376 (14)	0.030597
C5	1.12989 (11)	0.57056 (10)	0.69277 (6)	0.0128 (2)
H5A	1.180 (3)	0.565 (2)	0.7316 (13)	0.027547
C6	1.01536 (11)	0.55736 (9)	0.69641 (6)	0.0100 (2)
C7	1.01943 (12)	0.53670 (10)	0.80310 (6)	0.0116 (2)
H7A	1.058 (3)	0.600 (2)	0.8134 (13)	0.026160
H7B	1.085 (3)	0.483 (2)	0.8057 (13)	0.027077
C8	0.99550 (13)	0.56223 (11)	0.93117 (6)	0.0142 (2)
H8A	0.983 (2)	0.635 (2)	0.9291 (13)	0.023010
C9	0.91098 (12)	0.39470 (10)	0.87153 (7)	0.0139 (2)
H9A	0.851 (3)	0.382 (2)	0.9080 (13)	0.023980
C10	1.12026 (15)	0.55058 (15)	0.93054 (9)	0.0227 (3)
H10A	1.149 (3)	0.474 (2)	0.9294 (16)	0.032437
H10B	1.164 (3)	0.580 (2)	0.8972 (13)	0.030493
H10C	1.149 (3)	0.579 (3)	0.9806 (16)	0.034073
C11	0.94534 (18)	0.52143 (16)	0.98760 (8)	0.0262 (4)
H11A	0.999 (3)	0.550 (3)	1.0198 (14)	0.031947
H11B	0.860 (2)	0.528 (2)	0.9952 (14)	0.028190
H11C	0.960 (3)	0.448 (2)	0.9894 (14)	0.033387
C12	0.86456 (15)	0.35257 (11)	0.81432 (8)	0.0186 (3)
H12A	0.852 (3)	0.283 (2)	0.8258 (14)	0.031280
H12B	0.779 (3)	0.390 (2)	0.8026 (14)	0.028247
H12C	0.925 (3)	0.360 (2)	0.7813 (13)	0.030097
C13	1.01659 (16)	0.34496 (13)	0.88744 (10)	0.0239 (3)
H13A	1.005 (3)	0.272 (2)	0.8916 (15)	0.033360
H13B	1.087 (3)	0.367 (3)	0.8608 (14)	0.032930
H13C	1.054 (3)	0.355 (2)	0.9237 (13)	0.033173
C14	0.78948 (11)	0.47295 (9)	0.63327 (6)	0.00992 (18)
C15	0.82591 (12)	0.42276 (10)	0.58484 (6)	0.0123 (2)
H15A	0.896 (3)	0.456 (2)	0.5564 (13)	0.026317
C16	0.78539 (13)	0.33498 (10)	0.57248 (7)	0.0153 (2)
H16A	0.810 (3)	0.301 (2)	0.5312 (14)	0.029527
C17	0.70733 (13)	0.29742 (10)	0.61055 (7)	0.0158 (2)
H17A	0.668 (3)	0.229 (2)	0.5969 (15)	0.031103
C18	0.67022 (13)	0.34625 (10)	0.65968 (7)	0.0142 (2)
H18A	0.615 (3)	0.315 (2)	0.6915 (13)	0.027867
C19	0.70911 (11)	0.43560 (9)	0.67263 (6)	0.01044 (19)
C20	0.60314 (11)	0.44849 (10)	0.76429 (6)	0.0118 (2)
H20A	0.628 (3)	0.376 (2)	0.7803 (14)	0.026797
H20B	0.520 (2)	0.440 (2)	0.7452 (13)	0.027590
C21	0.53637 (12)	0.45618 (10)	0.88807 (6)	0.0134 (2)
H21A	0.464 (3)	0.421 (2)	0.8675 (13)	0.026070
C22	0.48074 (11)	0.60409 (10)	0.80768 (6)	0.0123 (2)
H22A	0.480 (3)	0.659 (2)	0.8417 (13)	0.023520
C23	0.61422 (15)	0.38117 (13)	0.91011 (7)	0.0203 (3)
H23A	0.574 (3)	0.340 (2)	0.9450 (14)	0.032970
H23B	0.635 (3)	0.329 (2)	0.8733 (14)	0.030373
H23C	0.684 (3)	0.414 (2)	0.9314 (15)	0.029870
C24	0.49905 (15)	0.51670 (12)	0.94003 (7)	0.0186 (3)
H24A	0.440 (3)	0.575 (3)	0.9220 (15)	0.030083
H24B	0.458 (3)	0.476 (2)	0.9703 (13)	0.033003
H24C	0.565 (3)	0.551 (2)	0.9633 (14)	0.029380
C25	0.49926 (13)	0.64744 (12)	0.74684 (8)	0.0173 (2)
H25A	0.439 (3)	0.699 (2)	0.7355 (14)	0.031697
H25B	0.574 (2)	0.677 (2)	0.7386 (13)	0.028417
H25C	0.497 (3)	0.589 (2)	0.7157 (14)	0.031093
C26	0.36780 (12)	0.55803 (12)	0.80856 (8)	0.0171 (3)
H26A	0.301 (3)	0.607 (2)	0.8027 (15)	0.034310
H26B	0.365 (3)	0.504 (2)	0.7763 (14)	0.034193
H26C	0.337 (3)	0.527 (3)	0.8488 (13)	0.033460
C27	0.77563 (11)	0.64134 (9)	0.62082 (6)	0.01046 (19)
C28	0.74267 (14)	0.63999 (10)	0.56205 (6)	0.0144 (2)
H28A	0.750 (3)	0.574 (2)	0.5367 (13)	0.026897
C29	0.69216 (15)	0.71651 (11)	0.53615 (7)	0.0182 (3)
H29A	0.663 (3)	0.708 (2)	0.4939 (12)	0.030690
C30	0.67556 (14)	0.79446 (11)	0.57063 (7)	0.0170 (3)
H30A	0.637 (3)	0.859 (3)	0.5432 (15)	0.032427
C31	0.70544 (12)	0.79587 (10)	0.63021 (6)	0.0134 (2)
H31A	0.693 (3)	0.857 (2)	0.6468 (12)	0.028243
C32	0.75541 (11)	0.71941 (9)	0.65751 (6)	0.01039 (19)
C33	0.74806 (12)	0.78793 (8)	0.75563 (6)	0.01161 (19)
H33A	0.659 (3)	0.804 (2)	0.7483 (14)	0.026027
H33B	0.801 (2)	0.848 (2)	0.7508 (12)	0.026610
C34	0.62768 (12)	0.80867 (10)	0.86343 (6)	0.0119 (2)
H34A	0.562 (3)	0.783 (2)	0.8336 (13)	0.023220
C35	0.86861 (12)	0.82272 (10)	0.86214 (7)	0.0132 (2)
H35A	0.845 (3)	0.890 (2)	0.8461 (13)	0.024307
C36	0.63049 (13)	0.91382 (10)	0.85994 (7)	0.0162 (2)
H36A	0.658 (3)	0.940 (2)	0.8266 (12)	0.031530
H36B	0.547 (3)	0.932 (2)	0.8723 (16)	0.031720
H36C	0.683 (3)	0.941 (2)	0.8945 (14)	0.031390
C37	0.59267 (15)	0.77694 (11)	0.92546 (7)	0.0180 (3)
H37A	0.515 (3)	0.807 (3)	0.9354 (14)	0.029330
H37B	0.588 (3)	0.706 (2)	0.9317 (13)	0.027593
H37C	0.645 (3)	0.799 (2)	0.9555 (12)	0.029013
C38	0.97448 (13)	0.78997 (12)	0.83205 (7)	0.0170 (2)
H38A	1.032 (3)	0.838 (2)	0.8395 (15)	0.030563
H38B	0.993 (3)	0.727 (2)	0.8529 (14)	0.028607
H38C	0.963 (3)	0.776 (2)	0.7812 (14)	0.028790
C39	0.87987 (14)	0.82434 (12)	0.92961 (7)	0.0181 (3)
H39A	0.942 (3)	0.869 (3)	0.9481 (14)	0.031313
H39B	0.814 (3)	0.858 (2)	0.9492 (13)	0.030753
H39C	0.875 (3)	0.755 (2)	0.9479 (14)	0.029063

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ni1	0.00868 (6)	0.00822 (6)	0.01140 (7)	−0.00034 (5)	0.00037 (5)	−0.00001 (5)
H1A	0.043510	0.031290	0.023530	−0.006860	0.003280	0.005010
H1B	0.046490	0.029330	0.022820	−0.002750	0.000500	−0.005040
In1	0.00952 (4)	0.00876 (4)	0.00961 (4)	0.00009 (2)	0.00013 (3)	−0.00013 (3)
P1	0.01007 (12)	0.00966 (12)	0.00844 (12)	0.00076 (10)	−0.00067 (10)	0.00063 (10)
P2	0.00875 (12)	0.01086 (13)	0.00881 (12)	−0.00171 (10)	0.00051 (10)	−0.00018 (10)
P3	0.01108 (13)	0.00768 (11)	0.00877 (12)	−0.00026 (11)	−0.00057 (10)	−0.00083 (9)
N1	0.0093 (4)	0.0137 (4)	0.0099 (4)	0.0009 (3)	0.0001 (4)	0.0015 (4)
N2	0.0119 (4)	0.0122 (4)	0.0099 (4)	−0.0018 (4)	0.0013 (3)	−0.0024 (3)
N3	0.0146 (5)	0.0088 (4)	0.0086 (4)	0.0017 (4)	−0.0010 (3)	0.0004 (3)
N4	0.0107 (4)	0.0090 (4)	0.0073 (4)	0.0011 (3)	−0.0013 (3)	0.0002 (3)
C1	0.0096 (4)	0.0096 (4)	0.0090 (4)	0.0005 (4)	0.0020 (4)	0.0002 (4)
C2	0.0144 (5)	0.0136 (5)	0.0115 (5)	−0.0001 (4)	0.0031 (4)	0.0002 (4)
H2A	0.027520	0.032280	0.019840	0.001190	−0.001340	0.002790
C3	0.0146 (5)	0.0165 (6)	0.0133 (5)	−0.0013 (5)	0.0041 (4)	0.0011 (4)
H3A	0.029090	0.037640	0.022740	−0.003020	0.008670	0.002790
C4	0.0113 (5)	0.0155 (5)	0.0169 (5)	−0.0009 (4)	0.0038 (4)	0.0009 (5)
H4A	0.018680	0.042130	0.030980	−0.003450	0.004510	0.000090
C5	0.0101 (5)	0.0155 (5)	0.0128 (5)	0.0002 (4)	0.0008 (4)	0.0007 (4)
H5A	0.021470	0.037930	0.023240	−0.000320	−0.002130	0.001720
C6	0.0096 (5)	0.0108 (5)	0.0097 (5)	0.0006 (4)	0.0014 (4)	0.0004 (4)
C7	0.0108 (5)	0.0143 (5)	0.0099 (5)	0.0005 (4)	0.0004 (4)	0.0004 (4)
H7A	0.025280	0.026400	0.026800	−0.007490	−0.001310	−0.001330
H7B	0.023590	0.029550	0.028090	0.009580	−0.000340	0.001420
C8	0.0154 (5)	0.0160 (6)	0.0112 (5)	−0.0014 (4)	−0.0020 (4)	−0.0006 (4)
H8A	0.023230	0.020750	0.025050	0.000580	−0.001170	−0.000360
C9	0.0154 (5)	0.0108 (5)	0.0155 (5)	0.0016 (4)	−0.0002 (4)	0.0028 (4)
H9A	0.025670	0.024820	0.021450	0.000870	0.004100	0.002590
C10	0.0161 (6)	0.0298 (8)	0.0222 (7)	0.0002 (6)	−0.0083 (5)	−0.0036 (6)
H10A	0.028840	0.027930	0.040540	0.007710	−0.000520	0.001030
H10B	0.024130	0.038030	0.029320	0.000600	0.002660	0.008090
H10C	0.026170	0.050630	0.025420	0.001110	−0.007370	−0.007580
C11	0.0330 (9)	0.0343 (9)	0.0112 (6)	−0.0104 (8)	0.0003 (6)	0.0006 (6)
H11A	0.031520	0.043680	0.020640	−0.005690	−0.006330	−0.000880
H11B	0.020050	0.035120	0.029400	0.003060	0.001200	0.004910
H11C	0.044930	0.022140	0.033090	0.006700	0.005370	0.004490
C12	0.0250 (7)	0.0121 (5)	0.0187 (6)	−0.0007 (5)	−0.0016 (5)	−0.0025 (5)
H12A	0.046990	0.016320	0.030530	−0.002600	−0.002040	0.002380
H12B	0.024510	0.030060	0.030170	0.008030	−0.005140	−0.003150
H12C	0.027170	0.039560	0.023560	−0.003880	0.007610	−0.001800
C13	0.0195 (7)	0.0150 (6)	0.0372 (10)	0.0049 (5)	−0.0050 (7)	0.0054 (6)
H13A	0.037820	0.020720	0.041540	0.006020	−0.003050	0.003520
H13B	0.026340	0.041850	0.030600	0.007210	0.006660	0.009300
H13C	0.035670	0.040750	0.023100	0.009920	−0.006870	−0.002620
C14	0.0123 (5)	0.0086 (4)	0.0089 (4)	0.0016 (4)	0.0001 (4)	−0.0012 (4)
C15	0.0154 (5)	0.0119 (5)	0.0098 (5)	−0.0002 (4)	0.0007 (4)	−0.0018 (4)
H15A	0.028780	0.026000	0.024170	−0.002960	0.007310	−0.000950
C16	0.0195 (6)	0.0131 (5)	0.0133 (5)	−0.0009 (5)	0.0012 (4)	−0.0056 (4)
H16A	0.037530	0.027050	0.024000	−0.000790	0.006130	−0.008930
C17	0.0179 (6)	0.0124 (5)	0.0172 (6)	−0.0032 (5)	0.0003 (5)	−0.0049 (4)
H17A	0.039420	0.022230	0.031660	−0.008880	0.003850	−0.008260
C18	0.0146 (5)	0.0121 (5)	0.0160 (5)	−0.0029 (4)	0.0008 (4)	−0.0040 (4)
H18A	0.030600	0.025930	0.027070	−0.008160	0.007250	−0.002870
C19	0.0106 (5)	0.0109 (5)	0.0097 (4)	−0.0005 (4)	0.0003 (4)	−0.0022 (4)
C20	0.0107 (5)	0.0131 (5)	0.0117 (5)	−0.0032 (4)	0.0017 (4)	−0.0016 (4)
H20A	0.032860	0.019040	0.028490	−0.000400	0.003150	0.001870
H20B	0.019540	0.035190	0.028040	−0.005610	−0.002420	−0.004490
C21	0.0129 (5)	0.0161 (6)	0.0113 (5)	−0.0036 (4)	0.0007 (4)	0.0011 (4)
H21A	0.021960	0.028160	0.028090	−0.007540	−0.000640	−0.004060
C22	0.0095 (4)	0.0155 (5)	0.0120 (5)	0.0005 (4)	0.0009 (4)	−0.0021 (4)
H22A	0.023570	0.024990	0.022000	0.000280	0.000460	−0.005630
C23	0.0213 (7)	0.0220 (7)	0.0175 (6)	0.0002 (6)	0.0027 (5)	0.0070 (5)
H23A	0.034490	0.029340	0.035080	−0.004880	0.010570	0.010790
H23B	0.037510	0.028030	0.025580	0.003620	0.003910	−0.006420
H23C	0.028140	0.024730	0.036740	−0.004310	−0.008700	−0.003240
C24	0.0244 (7)	0.0213 (7)	0.0102 (5)	−0.0060 (6)	0.0030 (5)	−0.0013 (5)
H24A	0.027770	0.031000	0.031480	0.007250	−0.002560	−0.003080
H24B	0.040170	0.030370	0.028470	−0.008610	0.013360	0.001160
H24C	0.021340	0.035740	0.031060	−0.005590	−0.001770	−0.009410
C25	0.0167 (5)	0.0196 (6)	0.0156 (6)	0.0027 (4)	−0.0016 (5)	0.0025 (5)
H25A	0.027630	0.037320	0.030140	0.014330	−0.000150	0.003440
H25B	0.020820	0.036490	0.027940	−0.006580	−0.000980	0.002290
H25C	0.042510	0.027840	0.022930	−0.003090	−0.000450	−0.008420
C26	0.0104 (5)	0.0222 (7)	0.0187 (6)	−0.0020 (5)	−0.0011 (4)	−0.0027 (5)
H26A	0.020090	0.038060	0.044780	0.003810	−0.003530	0.000420
H26B	0.028390	0.038210	0.035980	−0.006820	0.003780	−0.017430
H26C	0.028200	0.047180	0.025000	−0.009260	0.003650	0.001410
C27	0.0143 (5)	0.0092 (4)	0.0079 (4)	0.0017 (4)	−0.0008 (4)	0.0000 (4)
C28	0.0210 (6)	0.0128 (5)	0.0095 (5)	0.0039 (5)	−0.0024 (4)	−0.0012 (4)
H28A	0.035270	0.023500	0.021920	0.005610	−0.001060	−0.005320
C29	0.0270 (7)	0.0173 (6)	0.0104 (5)	0.0080 (5)	−0.0059 (5)	−0.0007 (4)
H29A	0.041720	0.033520	0.016830	0.008330	−0.004920	−0.000220
C30	0.0244 (7)	0.0151 (6)	0.0114 (5)	0.0081 (5)	−0.0036 (5)	0.0008 (4)
H30A	0.045990	0.026630	0.024660	0.014040	−0.003280	0.004410
C31	0.0180 (6)	0.0112 (5)	0.0109 (5)	0.0047 (4)	−0.0008 (4)	0.0006 (4)
H31A	0.040550	0.021030	0.023150	0.008090	−0.000480	−0.002870
C32	0.0122 (5)	0.0094 (4)	0.0096 (4)	0.0015 (4)	−0.0007 (4)	0.0005 (3)
C33	0.0160 (5)	0.0084 (4)	0.0104 (5)	0.0011 (4)	0.0003 (4)	−0.0006 (4)
H33A	0.024430	0.028470	0.025180	0.008400	−0.001730	−0.000760
H33B	0.034570	0.018510	0.026750	−0.005440	0.003590	0.000060
C34	0.0141 (5)	0.0111 (5)	0.0104 (5)	0.0008 (4)	0.0005 (4)	−0.0006 (4)
H34A	0.023370	0.024780	0.021510	0.001020	−0.003190	−0.002490
C35	0.0149 (5)	0.0109 (5)	0.0139 (5)	−0.0019 (4)	−0.0005 (4)	−0.0018 (4)
H35A	0.031410	0.016740	0.024770	−0.000150	0.001560	0.001140
C36	0.0198 (6)	0.0121 (5)	0.0167 (6)	0.0031 (5)	0.0016 (5)	−0.0005 (4)
H36A	0.047460	0.025080	0.022050	0.000970	0.007660	0.002680
H36B	0.028620	0.026110	0.040430	0.008610	0.004400	−0.001850
H36C	0.040240	0.024740	0.029190	−0.002050	−0.009830	−0.003550
C37	0.0237 (7)	0.0167 (6)	0.0135 (5)	−0.0009 (5)	0.0042 (5)	−0.0008 (5)
H37A	0.024360	0.035230	0.028400	0.010010	0.005200	0.000630
H37B	0.037390	0.017830	0.027560	−0.002110	0.003360	−0.000510
H37C	0.028770	0.036030	0.022240	−0.007300	−0.005440	−0.001870
C38	0.0153 (6)	0.0185 (6)	0.0172 (6)	−0.0046 (5)	0.0014 (5)	−0.0035 (5)
H38A	0.026320	0.025540	0.039830	−0.011200	0.004530	−0.006930
H38B	0.031310	0.022900	0.031610	0.003720	0.004680	0.007450
H38C	0.030850	0.037180	0.018340	0.001060	0.000070	−0.004390
C39	0.0192 (6)	0.0201 (6)	0.0150 (6)	−0.0031 (5)	−0.0030 (5)	−0.0043 (5)
H39A	0.029400	0.036590	0.027950	−0.013870	−0.002370	−0.003670
H39B	0.031770	0.034720	0.025770	0.008970	0.004580	−0.004320
H39C	0.042870	0.018540	0.025780	−0.002600	−0.001070	0.002650

Geometric parameters (Å, º)

Ni1—H1A	1.68 (4)	C14—C19	1.4306 (19)
Ni1—H1B	1.68 (4)	C15—H15A	1.17 (3)
Ni1—In1	2.4790 (2)	C15—C16	1.397 (2)
Ni1—P1	2.2836 (4)	C16—H16A	1.10 (3)
Ni1—P2	2.2530 (4)	C16—C17	1.395 (2)
Ni1—P3	2.2505 (4)	C17—H17A	1.15 (3)
H1A—H1B	0.94 (5)	C17—C18	1.392 (2)
In1—N1	2.1121 (11)	C18—H18A	1.08 (3)
In1—N2	2.1230 (12)	C18—C19	1.414 (2)
In1—N3	2.1131 (12)	C20—H20A	1.15 (3)
In1—N4	2.3666 (11)	C20—H20B	1.11 (3)
P1—C7	1.8643 (14)	C21—H21A	1.12 (3)
P1—C8	1.8696 (15)	C21—C23	1.530 (2)
P1—C9	1.8636 (15)	C21—C24	1.535 (2)
P2—C20	1.8708 (14)	C22—H22A	1.11 (3)
P2—C21	1.8599 (14)	C22—C25	1.527 (2)
P2—C22	1.8780 (14)	C22—C26	1.533 (2)
P3—C33	1.8888 (14)	C23—H23A	1.10 (3)
P3—C34	1.8664 (14)	C23—H23B	1.16 (3)
P3—C35	1.8554 (15)	C23—H23C	1.09 (3)
N1—C6	1.3662 (18)	C24—H24A	1.19 (3)
N1—C7	1.4408 (19)	C24—H24B	1.03 (3)
N2—C19	1.3652 (17)	C24—H24C	1.09 (3)
N2—C20	1.4492 (18)	C25—H25A	1.08 (3)
N3—C32	1.3712 (17)	C25—H25B	1.03 (3)
N3—C33	1.4395 (17)	C25—H25C	1.10 (3)
N4—C1	1.4634 (17)	C26—H26A	1.10 (3)
N4—C14	1.4561 (17)	C26—H26B	1.08 (3)
N4—C27	1.4641 (17)	C26—H26C	1.08 (3)
C1—C2	1.3861 (19)	C27—C28	1.3858 (19)
C1—C6	1.4313 (19)	C27—C32	1.4264 (19)
C2—H2A	1.03 (3)	C28—H28A	1.12 (3)
C2—C3	1.403 (2)	C28—C29	1.400 (2)
C3—H3A	1.03 (3)	C29—H29A	1.03 (3)
C3—C4	1.397 (2)	C29—C30	1.390 (2)
C4—H4A	1.01 (3)	C30—H30A	1.22 (3)
C4—C5	1.394 (2)	C30—C31	1.393 (2)
C5—H5A	1.07 (3)	C31—H31A	0.97 (3)
C5—C6	1.414 (2)	C31—C32	1.4098 (19)
C7—H7A	1.06 (3)	C33—H33A	1.13 (3)
C7—H7B	1.12 (3)	C33—H33B	1.09 (3)
C8—H8A	1.07 (3)	C34—H34A	1.11 (3)
C8—C10	1.533 (2)	C34—C36	1.531 (2)
C8—C11	1.532 (2)	C34—C37	1.534 (2)
C9—H9A	1.12 (3)	C35—H35A	1.08 (3)
C9—C12	1.537 (2)	C35—C38	1.536 (2)
C9—C13	1.522 (2)	C35—C39	1.528 (2)
C10—H10A	1.16 (3)	C36—H36A	0.91 (3)
C10—H10B	1.01 (3)	C36—H36B	1.09 (3)
C10—H10C	1.26 (3)	C36—H36C	1.08 (3)
C11—H11A	1.06 (3)	C37—H37A	1.07 (3)
C11—H11B	1.06 (3)	C37—H37B	1.04 (3)
C11—H11C	1.09 (3)	C37—H37C	0.98 (3)
C12—H12A	1.05 (3)	C38—H38A	1.01 (3)
C12—H12B	1.20 (3)	C38—H38B	1.06 (3)
C12—H12C	1.05 (3)	C38—H38C	1.17 (3)
C13—H13A	1.07 (3)	C39—H39A	1.09 (3)
C13—H13B	1.10 (3)	C39—H39B	1.04 (3)
C13—H13C	0.95 (3)	C39—H39C	1.09 (3)
C14—C15	1.3872 (18)
H1B—Ni1—H1A	32.5 (17)	C15—C14—N4	121.36 (12)
In1—Ni1—H1A	154.5 (14)	C19—C14—N4	117.98 (11)
In1—Ni1—H1B	171.5 (15)	C19—C14—C15	120.62 (12)
P1—Ni1—H1A	85.1 (15)	H15A—C15—C14	116.4 (16)
P1—Ni1—H1B	97.5 (16)	C16—C15—C14	121.61 (13)
P1—Ni1—In1	81.128 (10)	C16—C15—H15A	121.9 (16)
P2—Ni1—H1A	87.3 (14)	H16A—C16—C15	119.2 (18)
P2—Ni1—H1B	105.2 (16)	C17—C16—C15	118.50 (13)
P2—Ni1—In1	82.380 (10)	C17—C16—H16A	122.0 (17)
P2—Ni1—P1	122.749 (15)	H17A—C17—C16	117.3 (17)
P3—Ni1—H1A	121.0 (14)	C18—C17—C16	120.88 (13)
P3—Ni1—H1B	88.9 (14)	C18—C17—H17A	121.4 (17)
P3—Ni1—In1	84.544 (10)	H18A—C18—C17	120.8 (17)
P3—Ni1—P1	120.197 (15)	C19—C18—C17	121.59 (14)
P3—Ni1—P2	112.156 (15)	C19—C18—H18A	117.4 (17)
H1B—H1A—Ni1	74 (4)	C14—C19—N2	118.78 (12)
H1A—H1B—Ni1	74 (4)	C18—C19—N2	124.40 (13)
N1—In1—Ni1	104.59 (3)	C18—C19—C14	116.81 (12)
N2—In1—Ni1	102.78 (3)	N2—C20—P2	108.31 (9)
N2—In1—N1	116.51 (5)	H20A—C20—P2	109.2 (16)
N3—In1—Ni1	103.27 (3)	H20A—C20—N2	113.7 (16)
N3—In1—N1	111.74 (5)	H20B—C20—P2	110.4 (16)
N3—In1—N2	115.82 (5)	H20B—C20—N2	110.2 (16)
N4—In1—Ni1	178.62 (3)	H20B—C20—H20A	105 (3)
N4—In1—N1	76.66 (4)	H21A—C21—P2	106.5 (16)
N4—In1—N2	76.06 (4)	C23—C21—P2	112.34 (10)
N4—In1—N3	76.69 (4)	C23—C21—H21A	107.8 (17)
C7—P1—Ni1	117.43 (5)	C24—C21—P2	110.09 (11)
C8—P1—Ni1	110.59 (5)	C24—C21—H21A	109.8 (16)
C8—P1—C7	103.27 (7)	C24—C21—C23	110.18 (13)
C9—P1—Ni1	116.66 (5)	H22A—C22—P2	104.5 (16)
C9—P1—C7	102.06 (7)	C25—C22—P2	111.05 (10)
C9—P1—C8	105.32 (7)	C25—C22—H22A	108.8 (16)
C20—P2—Ni1	118.05 (5)	C26—C22—P2	115.67 (11)
C21—P2—Ni1	114.34 (5)	C26—C22—H22A	107.6 (17)
C21—P2—C20	102.58 (6)	C26—C22—C25	108.98 (12)
C22—P2—Ni1	117.32 (5)	H23A—C23—C21	109.8 (19)
C22—P2—C20	100.53 (6)	H23B—C23—C21	111.8 (17)
C22—P2—C21	101.47 (7)	H23B—C23—H23A	105 (2)
C33—P3—Ni1	118.80 (4)	H23C—C23—C21	108.4 (18)
C34—P3—Ni1	112.77 (5)	H23C—C23—H23A	106 (3)
C34—P3—C33	99.12 (6)	H23C—C23—H23B	116 (3)
C35—P3—Ni1	118.80 (5)	H24A—C24—C21	109.2 (17)
C35—P3—C33	99.75 (6)	H24B—C24—C21	108.9 (18)
C35—P3—C34	104.84 (6)	H24B—C24—H24A	110 (3)
C6—N1—In1	112.91 (9)	H24C—C24—C21	114.5 (17)
C7—N1—In1	115.74 (9)	H24C—C24—H24A	106 (3)
C7—N1—C6	119.59 (11)	H24C—C24—H24B	108 (3)
C19—N2—In1	113.03 (9)	H25A—C25—C22	113.4 (17)
C20—N2—In1	117.98 (8)	H25B—C25—C22	118.0 (17)
C20—N2—C19	120.74 (12)	H25B—C25—H25A	105 (3)
C32—N3—In1	113.18 (9)	H25C—C25—C22	104.7 (17)
C33—N3—In1	118.75 (8)	H25C—C25—H25A	111 (3)
C33—N3—C32	119.57 (11)	H25C—C25—H25B	104 (3)
C1—N4—In1	103.26 (8)	H26A—C26—C22	112.8 (18)
C14—N4—In1	103.49 (8)	H26B—C26—C22	109.8 (18)
C14—N4—C1	115.85 (10)	H26B—C26—H26A	112 (3)
C27—N4—In1	102.60 (7)	H26C—C26—C22	120.5 (18)
C27—N4—C1	113.63 (11)	H26C—C26—H26A	96 (3)
C27—N4—C14	115.54 (10)	H26C—C26—H26B	105 (3)
C2—C1—N4	121.42 (12)	C28—C27—N4	121.00 (12)
C6—C1—N4	117.91 (11)	C32—C27—N4	117.92 (11)
C6—C1—C2	120.59 (12)	C32—C27—C28	121.07 (12)
H2A—C2—C1	116.8 (17)	H28A—C28—C27	118.5 (16)
C3—C2—C1	121.51 (14)	C29—C28—C27	121.07 (13)
C3—C2—H2A	121.6 (17)	C29—C28—H28A	120.2 (17)
H3A—C3—C2	134.0 (19)	H29A—C29—C28	116.4 (17)
C4—C3—C2	118.55 (13)	C30—C29—C28	118.62 (13)
C4—C3—H3A	107.3 (19)	C30—C29—H29A	124.7 (17)
H4A—C4—C3	118.1 (18)	H30A—C30—C29	113.5 (17)
C5—C4—C3	120.75 (13)	C31—C30—C29	120.93 (13)
C5—C4—H4A	121.1 (18)	C31—C30—H30A	125.5 (17)
H5A—C5—C4	118.0 (17)	H31A—C31—C30	110.1 (17)
C6—C5—C4	121.57 (13)	C32—C31—C30	121.55 (13)
C6—C5—H5A	120.4 (17)	C32—C31—H31A	128.2 (17)
C1—C6—N1	119.20 (12)	C27—C32—N3	119.29 (11)
C5—C6—N1	123.77 (13)	C31—C32—N3	124.02 (12)
C5—C6—C1	117.02 (12)	C31—C32—C27	116.69 (11)
N1—C7—P1	108.70 (9)	N3—C33—P3	111.64 (9)
H7A—C7—P1	103.4 (17)	H33A—C33—P3	103.5 (16)
H7A—C7—N1	115.7 (16)	H33A—C33—N3	110.7 (16)
H7B—C7—P1	110.8 (16)	H33B—C33—P3	107.8 (15)
H7B—C7—N1	112.0 (16)	H33B—C33—N3	109.7 (15)
H7B—C7—H7A	106 (2)	H33B—C33—H33A	113 (2)
H8A—C8—P1	101.6 (15)	H34A—C34—P3	103.6 (16)
C10—C8—P1	117.29 (12)	C36—C34—P3	114.81 (10)
C10—C8—H8A	104.5 (16)	C36—C34—H34A	108.9 (16)
C11—C8—P1	110.37 (11)	C37—C34—P3	113.49 (10)
C11—C8—H8A	111.2 (16)	C37—C34—H34A	104.4 (16)
C11—C8—C10	111.24 (15)	C37—C34—C36	110.70 (12)
H9A—C9—P1	104.8 (17)	H35A—C35—P3	101.5 (17)
C12—C9—P1	109.98 (10)	C38—C35—P3	108.57 (10)
C12—C9—H9A	108.3 (16)	C38—C35—H35A	111.1 (16)
C13—C9—P1	116.87 (12)	C39—C35—P3	113.42 (11)
C13—C9—H9A	107.8 (16)	C39—C35—H35A	110.2 (16)
C13—C9—C12	108.75 (14)	C39—C35—C38	111.66 (13)
H10A—C10—C8	113.9 (18)	H36A—C36—C34	118.4 (19)
H10B—C10—C8	118.9 (18)	H36B—C36—C34	102.3 (19)
H10B—C10—H10A	103 (3)	H36B—C36—H36A	117 (3)
H10C—C10—C8	103.7 (17)	H36C—C36—C34	109.6 (18)
H10C—C10—H10A	105 (3)	H36C—C36—H36A	103 (3)
H10C—C10—H10B	112 (3)	H36C—C36—H36B	106 (3)
H11A—C11—C8	99.9 (18)	H37A—C37—C34	108.3 (18)
H11B—C11—C8	119.7 (17)	H37B—C37—C34	115.9 (16)
H11B—C11—H11A	118 (3)	H37B—C37—H37A	109 (3)
H11C—C11—C8	110.2 (17)	H37C—C37—C34	110.4 (18)
H11C—C11—H11A	105 (3)	H37C—C37—H37A	107 (3)
H11C—C11—H11B	104 (3)	H37C—C37—H37B	106 (3)
H12A—C12—C9	103.3 (17)	H38A—C38—C35	107.2 (19)
H12B—C12—C9	108.9 (16)	H38B—C38—C35	104.4 (17)
H12B—C12—H12A	111 (3)	H38B—C38—H38A	113 (3)
H12C—C12—C9	107.3 (18)	H38C—C38—C35	112.4 (17)
H12C—C12—H12A	112 (3)	H38C—C38—H38A	111 (3)
H12C—C12—H12B	114 (2)	H38C—C38—H38B	108 (2)
H13A—C13—C9	112.3 (19)	H39A—C39—C35	117.0 (17)
H13B—C13—C9	113.3 (17)	H39B—C39—C35	111.2 (17)
H13B—C13—H13A	116 (3)	H39B—C39—H39A	95 (3)
H13C—C13—C9	122 (2)	H39C—C39—C35	110.9 (17)
H13C—C13—H13A	98 (3)	H39C—C39—H39A	116 (3)
H13C—C13—H13B	93 (3)	H39C—C39—H39B	104 (3)

(GOJNIF_IAM_0_HADPs)

Crystal data

C39H62InN4NiP3	Dx = 1.415 Mg m^−3
Mr = 853.39	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, P212121	Cell parameters from 9537 reflections
a = 12.2127 (4) Å	θ = 2.3–36.4°
b = 14.5402 (5) Å	µ = 1.20 mm^−1
c = 22.5601 (8) Å	T = 100 K
V = 4006.1 (2) Å^3	Block, gold
Z = 4	0.14 × 0.08 × 0.06 mm
F(000) = 105.805

Data collection

Bruker Photon-II CMOS diffractometer	18741 reflections with I ≥ 2u(I)
φ and ω scans	Rint = 0.036
Absorption correction: multi-scan SADABS. R.Blessing, 1995	θmax = 36.4°, θmin = 2.3°
Tmin = 0.701, Tmax = 0.747	h = −20→20
237431 measured reflections	k = −24→24
19473 independent reflections	l = −37→37

Refinement

Refinement on F^2	0 constraints
Least-squares matrix: full	Only H-atom coordinates refined
R[F^2 > 2σ(F^2)] = 0.019	w = 1/[σ^2(Fo^2) + (0.0146P)^2 + 1.8877P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.043	(Δ/σ)max = 0.001
S = 1.05	Δρmax = 0.40 e Å^−3
19473 reflections	Δρmin = −0.59 e Å^−3
619 parameters	Absolute structure: Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.
0 restraints	Absolute structure parameter: −0.0095 (17)

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ni1	0.755796 (11)	0.598654 (9)	0.856163 (6)	0.00938 (2)
Ha	0.7260 (11)	0.5766 (10)	0.9247 (6)	0.000000
Hb	0.7616 (12)	0.6325 (10)	0.9232 (6)	0.000000
In1	0.798243 (5)	0.580828 (4)	0.749323 (3)	0.008341 (12)
P1	0.91843 (2)	0.522271 (19)	0.864329 (12)	0.00938 (4)
P2	0.59907 (2)	0.528580 (19)	0.829182 (12)	0.00943 (4)
P3	0.75361 (2)	0.750090 (18)	0.835685 (11)	0.00916 (4)
N1	0.96160 (7)	0.53379 (6)	0.74726 (5)	0.01061 (13)
N2	0.67672 (8)	0.48679 (7)	0.72033 (4)	0.01127 (15)
N3	0.78431 (8)	0.71619 (6)	0.71614 (4)	0.01044 (14)
N4	0.83419 (7)	0.56338 (6)	0.64690 (4)	0.00869 (13)
C1	0.95366 (8)	0.57172 (7)	0.64335 (4)	0.00937 (15)
C2	1.00532 (9)	0.59715 (8)	0.59114 (5)	0.01291 (17)
H2	0.9638 (12)	0.6087 (10)	0.5560 (6)	0.000000
C3	1.11899 (10)	0.60859 (8)	0.58844 (5)	0.01473 (18)
H3	1.1552 (12)	0.6248 (10)	0.5549 (6)	0.000000
C4	1.18023 (8)	0.59547 (8)	0.63980 (5)	0.01397 (17)
H4	1.2595 (12)	0.6040 (9)	0.6371 (6)	0.000000
C5	1.12981 (9)	0.57034 (8)	0.69260 (5)	0.01243 (17)
H5	1.1718 (12)	0.5611 (10)	0.7277 (6)	0.000000
C6	1.01545 (9)	0.55745 (7)	0.69632 (5)	0.00990 (17)
C7	1.01944 (9)	0.53673 (8)	0.80313 (5)	0.01138 (18)
H7a	1.0596 (11)	0.5917 (10)	0.8101 (6)	0.000000
H7b	1.0756 (12)	0.4873 (10)	0.8052 (6)	0.000000
C8	0.99542 (10)	0.56229 (8)	0.93126 (5)	0.01418 (18)
H8	0.9810 (12)	0.6279 (10)	0.9307 (6)	0.000000
C9	0.91074 (9)	0.39460 (8)	0.87149 (5)	0.01383 (18)
H9	0.8587 (12)	0.3840 (10)	0.9047 (6)	0.000000
C10	1.12032 (11)	0.55057 (11)	0.93042 (6)	0.0226 (2)
H10a	1.1474 (12)	0.4853 (10)	0.9273 (6)	0.000000
H10b	1.1541 (11)	0.5828 (10)	0.8977 (6)	0.000000
H10c	1.1500 (11)	0.5776 (10)	0.9682 (6)	0.000000
C11	0.94528 (14)	0.52142 (12)	0.98763 (6)	0.0266 (3)
H11a	0.9790 (12)	0.5480 (10)	1.0205 (6)	0.000000
H11b	0.8705 (12)	0.5358 (10)	0.9904 (6)	0.000000
H11c	0.9546 (12)	0.4534 (10)	0.9897 (6)	0.000000
C12	0.86458 (12)	0.35268 (8)	0.81442 (6)	0.0186 (2)
H12a	0.8499 (12)	0.2888 (10)	0.8206 (6)	0.000000
H12b	0.7919 (12)	0.3829 (9)	0.8026 (6)	0.000000
H12c	0.9179 (12)	0.3589 (10)	0.7842 (6)	0.000000
C13	1.01693 (12)	0.34496 (9)	0.88757 (7)	0.0235 (3)
H13a	1.0043 (12)	0.2815 (10)	0.8878 (6)	0.000000
H13b	1.0744 (12)	0.3595 (10)	0.8592 (6)	0.000000
H13c	1.0462 (12)	0.3642 (10)	0.9247 (6)	0.000000
C14	0.78952 (9)	0.47270 (7)	0.63327 (4)	0.00998 (15)
C15	0.82592 (9)	0.42270 (8)	0.58481 (4)	0.01227 (16)
H15	0.8836 (12)	0.4444 (10)	0.5618 (6)	0.000000
C16	0.78510 (10)	0.33494 (8)	0.57256 (5)	0.01507 (19)
H16	0.8128 (12)	0.2976 (10)	0.5388 (6)	0.000000
C17	0.70729 (11)	0.29763 (8)	0.61045 (5)	0.01581 (18)
H17	0.6801 (11)	0.2367 (10)	0.6039 (6)	0.000000
C18	0.67000 (10)	0.34622 (8)	0.65958 (5)	0.01406 (18)
H18	0.6192 (12)	0.3160 (10)	0.6869 (6)	0.000000
C19	0.70909 (9)	0.43555 (7)	0.67262 (4)	0.01031 (15)
C20	0.60325 (9)	0.44849 (8)	0.76424 (5)	0.01193 (17)
H20a	0.6229 (12)	0.3866 (10)	0.7792 (6)	0.000000
H20b	0.5268 (10)	0.4402 (9)	0.7488 (7)	0.000000
C21	0.53629 (9)	0.45614 (8)	0.88800 (5)	0.01311 (18)
H21	0.4724 (11)	0.4263 (10)	0.8704 (6)	0.000000
C22	0.48061 (9)	0.60404 (8)	0.80768 (5)	0.01231 (17)
H22	0.4805 (12)	0.6529 (10)	0.8376 (6)	0.000000
C23	0.61392 (11)	0.38123 (9)	0.91002 (6)	0.0204 (2)
H23a	0.5759 (12)	0.3410 (10)	0.9388 (6)	0.000000
H23b	0.6378 (12)	0.3428 (10)	0.8778 (6)	0.000000
H23c	0.6770 (11)	0.4090 (10)	0.9298 (6)	0.000000
C24	0.49921 (11)	0.51660 (9)	0.93994 (5)	0.0185 (2)
H24a	0.4497 (12)	0.5635 (10)	0.9286 (6)	0.000000
H24b	0.4687 (12)	0.4794 (10)	0.9690 (6)	0.000000
H24c	0.5593 (12)	0.5461 (10)	0.9591 (6)	0.000000
C25	0.49935 (9)	0.64746 (8)	0.74666 (7)	0.01698 (18)
H25a	0.4425 (11)	0.6918 (9)	0.7375 (6)	0.000000
H25b	0.5700 (11)	0.6763 (9)	0.7413 (6)	0.000000
H25c	0.4961 (12)	0.6020 (10)	0.7172 (6)	0.000000
C26	0.36768 (10)	0.55817 (9)	0.80855 (6)	0.0171 (2)
H26a	0.3129 (12)	0.6050 (10)	0.7982 (6)	0.000000
H26b	0.3643 (12)	0.5087 (10)	0.7808 (6)	0.000000
H26c	0.3479 (12)	0.5374 (10)	0.8454 (6)	0.000000
C27	0.77592 (8)	0.64147 (7)	0.62070 (4)	0.01026 (16)
C28	0.74247 (11)	0.64021 (8)	0.56208 (5)	0.01440 (18)
H28	0.7563 (12)	0.5835 (10)	0.5378 (6)	0.000000
C29	0.69203 (11)	0.71654 (8)	0.53624 (5)	0.0178 (2)
H29	0.6722 (12)	0.7142 (10)	0.4980 (6)	0.000000
C30	0.67556 (11)	0.79426 (8)	0.57074 (5)	0.0168 (2)
H30	0.6443 (12)	0.8474 (10)	0.5552 (6)	0.000000
C31	0.70535 (10)	0.79577 (7)	0.63025 (5)	0.01299 (17)
H31	0.6925 (12)	0.8500 (9)	0.6531 (6)	0.000000
C32	0.75538 (9)	0.71943 (7)	0.65745 (4)	0.00976 (15)
C33	0.74807 (9)	0.78807 (6)	0.75562 (5)	0.01182 (15)
H33a	0.6711 (10)	0.8065 (9)	0.7486 (7)	0.000000
H33b	0.7900 (10)	0.8442 (9)	0.7526 (7)	0.000000
C34	0.62759 (9)	0.80863 (7)	0.86334 (5)	0.01205 (17)
H34	0.5705 (12)	0.7876 (10)	0.8375 (6)	0.000000
C35	0.86862 (9)	0.82265 (7)	0.86207 (5)	0.01288 (17)
H35	0.8529 (12)	0.8830 (10)	0.8478 (6)	0.000000
C36	0.63057 (10)	0.91388 (8)	0.85995 (5)	0.01597 (18)
H36a	0.6544 (12)	0.9338 (10)	0.8233 (6)	0.000000
H36b	0.5567 (12)	0.9378 (10)	0.8681 (6)	0.000000
H36c	0.6828 (12)	0.9408 (10)	0.8923 (6)	0.000000
C37	0.59279 (11)	0.77702 (9)	0.92533 (5)	0.0175 (2)
H37a	0.5197 (12)	0.8037 (10)	0.9330 (6)	0.000000
H37b	0.5874 (12)	0.7113 (10)	0.9283 (6)	0.000000
H37c	0.6426 (12)	0.7981 (10)	0.9529 (6)	0.000000
C38	0.97439 (10)	0.78989 (9)	0.83202 (6)	0.0168 (2)
H38a	1.0297 (12)	0.8332 (10)	0.8362 (6)	0.000000
H38b	1.0001 (12)	0.7363 (10)	0.8487 (6)	0.000000
H38c	0.9622 (12)	0.7786 (10)	0.7889 (6)	0.000000
C39	0.87992 (11)	0.82439 (9)	0.92961 (6)	0.0178 (2)
H39a	0.9476 (12)	0.8487 (10)	0.9422 (6)	0.000000
H39b	0.8237 (12)	0.8581 (10)	0.9478 (6)	0.000000
H39c	0.8745 (12)	0.7591 (10)	0.9474 (6)	0.000000

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ni1	0.00867 (5)	0.00828 (5)	0.01119 (5)	−0.00038 (4)	0.00040 (4)	0.00007 (4)
Ha	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
Hb	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
In1	0.00852 (2)	0.00788 (2)	0.00862 (2)	0.000100 (19)	0.00017 (2)	−0.00012 (2)
P1	0.01020 (10)	0.00953 (10)	0.00842 (10)	0.00072 (8)	−0.00059 (8)	0.00063 (8)
P2	0.00868 (10)	0.01080 (10)	0.00882 (10)	−0.00174 (8)	0.00042 (8)	−0.00031 (8)
P3	0.01096 (10)	0.00781 (9)	0.00872 (9)	−0.00021 (9)	−0.00060 (9)	−0.00076 (8)
N1	0.0093 (3)	0.0139 (3)	0.0087 (3)	0.0010 (2)	−0.0003 (3)	0.0009 (3)
N2	0.0117 (4)	0.0123 (4)	0.0099 (3)	−0.0024 (3)	0.0017 (3)	−0.0025 (3)
N3	0.0145 (4)	0.0090 (3)	0.0079 (3)	0.0016 (3)	−0.0004 (3)	−0.0003 (3)
N4	0.0097 (3)	0.0080 (3)	0.0083 (3)	0.0007 (3)	−0.0009 (3)	0.0003 (3)
C1	0.0097 (3)	0.0090 (4)	0.0094 (4)	0.0003 (3)	0.0012 (3)	−0.0004 (3)
C2	0.0152 (4)	0.0123 (4)	0.0112 (4)	0.0005 (3)	0.0023 (3)	0.0001 (3)
H2	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C3	0.0156 (5)	0.0146 (4)	0.0139 (4)	−0.0006 (4)	0.0048 (4)	0.0009 (4)
H3	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C4	0.0116 (4)	0.0134 (4)	0.0169 (4)	−0.0009 (3)	0.0035 (3)	0.0001 (4)
H4	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C5	0.0103 (4)	0.0139 (4)	0.0131 (4)	0.0004 (3)	0.0001 (3)	−0.0001 (3)
H5	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C6	0.0101 (4)	0.0096 (4)	0.0100 (4)	0.0009 (3)	0.0012 (3)	−0.0006 (3)
C7	0.0104 (4)	0.0138 (4)	0.0099 (4)	0.0009 (3)	−0.0005 (3)	0.0008 (3)
H7a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H7b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C8	0.0154 (5)	0.0163 (5)	0.0109 (4)	−0.0013 (4)	−0.0024 (3)	−0.0005 (3)
H8	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C9	0.0150 (4)	0.0105 (4)	0.0160 (4)	0.0013 (3)	−0.0005 (3)	0.0026 (3)
H9	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C10	0.0169 (5)	0.0296 (6)	0.0215 (6)	0.0003 (5)	−0.0080 (4)	−0.0037 (5)
H10a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H10b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H10c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C11	0.0341 (7)	0.0340 (7)	0.0116 (5)	−0.0099 (6)	0.0002 (5)	0.0009 (5)
H11a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H11b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H11c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C12	0.0252 (6)	0.0106 (4)	0.0201 (5)	−0.0008 (4)	−0.0017 (4)	−0.0022 (4)
H12a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H12b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H12c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C13	0.0198 (6)	0.0146 (5)	0.0361 (7)	0.0053 (4)	−0.0061 (5)	0.0049 (5)
H13a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H13b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H13c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C14	0.0120 (4)	0.0087 (3)	0.0092 (4)	0.0015 (3)	−0.0012 (3)	−0.0011 (3)
C15	0.0147 (4)	0.0123 (4)	0.0097 (4)	0.0007 (3)	0.0005 (3)	−0.0012 (3)
H15	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C16	0.0182 (5)	0.0134 (4)	0.0136 (4)	0.0001 (4)	0.0001 (4)	−0.0056 (3)
H16	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C17	0.0180 (5)	0.0121 (4)	0.0173 (5)	−0.0023 (4)	−0.0007 (4)	−0.0051 (3)
H17	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C18	0.0138 (4)	0.0123 (4)	0.0160 (5)	−0.0029 (3)	0.0008 (4)	−0.0032 (3)
H18	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C19	0.0103 (4)	0.0105 (4)	0.0101 (4)	0.0000 (3)	−0.0009 (3)	−0.0020 (3)
C20	0.0113 (4)	0.0125 (4)	0.0120 (4)	−0.0026 (3)	0.0015 (3)	−0.0020 (3)
H20a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H20b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C21	0.0129 (4)	0.0157 (4)	0.0108 (4)	−0.0040 (3)	0.0009 (3)	0.0011 (3)
H21	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C22	0.0098 (4)	0.0155 (4)	0.0116 (4)	0.0005 (3)	0.0003 (3)	−0.0019 (3)
H22	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C23	0.0202 (5)	0.0221 (6)	0.0189 (5)	0.0003 (4)	0.0026 (4)	0.0077 (4)
H23a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H23b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H23c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C24	0.0235 (6)	0.0215 (5)	0.0105 (4)	−0.0057 (4)	0.0030 (4)	−0.0012 (4)
H24a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H24b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H24c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C25	0.0171 (4)	0.0188 (4)	0.0150 (5)	0.0027 (3)	−0.0009 (4)	0.0026 (5)
H25a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H25b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H25c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C26	0.0104 (4)	0.0224 (5)	0.0185 (5)	−0.0012 (4)	−0.0010 (4)	−0.0032 (4)
H26a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H26b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H26c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C27	0.0131 (4)	0.0090 (4)	0.0087 (4)	0.0014 (3)	−0.0004 (3)	0.0007 (3)
C28	0.0196 (5)	0.0136 (4)	0.0099 (4)	0.0038 (4)	−0.0029 (4)	−0.0012 (3)
H28	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C29	0.0249 (6)	0.0179 (5)	0.0107 (4)	0.0076 (4)	−0.0054 (4)	−0.0002 (4)
H29	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C30	0.0223 (5)	0.0162 (5)	0.0118 (4)	0.0076 (4)	−0.0025 (4)	0.0018 (4)
H30	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C31	0.0164 (4)	0.0117 (4)	0.0109 (4)	0.0038 (4)	−0.0006 (4)	0.0005 (3)
H31	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C32	0.0108 (4)	0.0094 (3)	0.0090 (4)	0.0006 (3)	−0.0004 (3)	0.0003 (3)
C33	0.0162 (4)	0.0087 (3)	0.0106 (4)	0.0015 (3)	−0.0004 (4)	−0.0005 (3)
H33a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H33b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C34	0.0139 (4)	0.0113 (4)	0.0109 (4)	0.0013 (3)	0.0003 (3)	−0.0012 (3)
H34	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C35	0.0143 (4)	0.0107 (4)	0.0136 (4)	−0.0024 (3)	−0.0004 (3)	−0.0015 (3)
H35	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C36	0.0203 (5)	0.0110 (4)	0.0166 (4)	0.0034 (4)	0.0009 (4)	−0.0010 (4)
H36a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H36b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H36c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C37	0.0220 (5)	0.0173 (5)	0.0133 (5)	−0.0013 (4)	0.0039 (4)	−0.0003 (4)
H37a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H37b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H37c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C38	0.0146 (5)	0.0179 (5)	0.0179 (5)	−0.0037 (4)	0.0013 (4)	−0.0029 (4)
H38a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H38b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H38c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C39	0.0191 (5)	0.0199 (5)	0.0143 (5)	−0.0027 (4)	−0.0026 (4)	−0.0042 (4)
H39a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H39b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H39c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000

Geometric parameters (Å, º)

Ni1—Ha	1.620 (14)	C14—C19	1.4298 (15)
Ni1—Hb	1.593 (14)	C15—H15	0.931 (14)
Ni1—In1	2.4790 (2)	C15—C16	1.3976 (16)
Ni1—P1	2.2831 (3)	C16—H16	0.995 (14)
Ni1—P2	2.2521 (3)	C16—C17	1.3885 (17)
Ni1—P3	2.2500 (3)	C17—H17	0.958 (14)
Ha—Hb	0.922 (18)	C17—C18	1.3910 (16)
In1—N1	2.1095 (8)	C18—H18	0.979 (14)
In1—N2	2.1213 (9)	C18—C19	1.4148 (15)
In1—N3	2.1127 (9)	C20—H20a	0.991 (14)
In1—N4	2.3656 (9)	C20—H20b	1.003 (13)
P1—C7	1.8634 (12)	C21—H21	0.977 (14)
P1—C8	1.8716 (11)	C21—C23	1.5272 (18)
P1—C9	1.8657 (11)	C21—C24	1.5333 (17)
P2—C20	1.8723 (11)	C22—H22	0.979 (14)
P2—C21	1.8596 (11)	C22—C25	1.5317 (18)
P2—C22	1.8795 (11)	C22—C26	1.5321 (16)
P3—C33	1.8900 (11)	C23—H23a	0.989 (14)
P3—C34	1.8662 (11)	C23—H23b	0.963 (14)
P3—C35	1.8547 (11)	C23—H23c	0.977 (14)
N1—C6	1.3680 (15)	C24—H24a	0.946 (14)
N1—C7	1.4454 (15)	C24—H24b	0.927 (14)
N2—C19	1.3675 (13)	C24—H24c	0.954 (14)
N2—C20	1.4479 (14)	C25—H25a	0.970 (14)
N3—C32	1.3711 (13)	C25—H25b	0.967 (13)
N3—C33	1.4428 (13)	C25—H25c	0.938 (14)
N4—C1	1.4663 (13)	C26—H26a	0.983 (14)
N4—C14	1.4597 (13)	C26—H26b	0.954 (14)
N4—C27	1.4646 (13)	C26—H26c	0.916 (14)
C1—C2	1.3864 (15)	C27—C28	1.3844 (14)
C1—C6	1.4286 (15)	C27—C32	1.4266 (14)
C2—H2	0.955 (14)	C28—H28	1.004 (14)
C2—C3	1.3995 (16)	C28—C29	1.3967 (16)
C3—H3	0.908 (14)	C29—H29	0.897 (14)
C3—C4	1.3923 (17)	C29—C30	1.3868 (17)
C4—H4	0.978 (14)	C30—H30	0.930 (14)
C4—C5	1.3899 (15)	C30—C31	1.3913 (16)
C5—H5	0.954 (14)	C31—H31	0.955 (14)
C5—C6	1.4117 (15)	C31—C32	1.4078 (14)
C7—H7a	0.951 (14)	C33—H33a	0.990 (13)
C7—H7b	0.995 (15)	C33—H33b	0.966 (12)
C8—H8	0.970 (15)	C34—H34	0.959 (14)
C8—C10	1.5350 (18)	C34—C36	1.5327 (16)
C8—C11	1.5315 (18)	C34—C37	1.5322 (16)
C9—H9	0.994 (14)	C35—H35	0.955 (14)
C9—C12	1.5320 (17)	C35—C38	1.5346 (17)
C9—C13	1.5277 (17)	C35—C39	1.5302 (17)
C10—H10a	1.007 (14)	C36—H36a	0.923 (14)
C10—H10b	0.967 (14)	C36—H36b	0.985 (14)
C10—H10c	1.007 (14)	C36—H36c	1.045 (14)
C11—H11a	0.932 (14)	C37—H37a	0.988 (15)
C11—H11b	0.939 (14)	C37—H37b	0.960 (14)
C11—H11c	0.997 (14)	C37—H37c	0.923 (15)
C12—H12a	0.957 (14)	C38—H38a	0.928 (15)
C12—H12b	1.025 (14)	C38—H38b	0.920 (14)
C12—H12c	0.948 (15)	C38—H38c	0.998 (14)
C13—H13a	0.936 (15)	C39—H39a	0.942 (15)
C13—H13b	0.974 (15)	C39—H39b	0.938 (14)
C13—H13c	0.953 (15)	C39—H39c	1.032 (15)
C14—C15	1.3862 (14)
Hb—Ni1—Ha	33.3 (6)	C15—C14—N4	121.33 (9)
In1—Ni1—Ha	162.5 (5)	C19—C14—N4	117.86 (8)
In1—Ni1—Hb	161.2 (5)	C19—C14—C15	120.79 (9)
P1—Ni1—Ha	91.2 (5)	H15—C15—C14	120.4 (9)
P1—Ni1—Hb	92.0 (5)	C16—C15—C14	121.36 (10)
P1—Ni1—In1	81.122 (8)	C16—C15—H15	117.9 (9)
P2—Ni1—Ha	88.7 (5)	H16—C16—C15	121.9 (8)
P2—Ni1—Hb	115.8 (5)	C17—C16—C15	118.63 (10)
P2—Ni1—In1	82.393 (8)	C17—C16—H16	119.5 (8)
P2—Ni1—P1	122.758 (11)	H17—C17—C16	120.3 (8)
P3—Ni1—Ha	112.8 (5)	C18—C17—C16	121.08 (10)
P3—Ni1—Hb	83.9 (5)	C18—C17—H17	118.6 (8)
P3—Ni1—In1	84.558 (8)	H18—C18—C17	118.8 (8)
P3—Ni1—P1	120.195 (12)	C19—C18—C17	121.43 (10)
P3—Ni1—P2	112.158 (12)	C19—C18—H18	119.7 (8)
Hb—Ha—Ni1	71.7 (13)	C14—C19—N2	118.78 (9)
Ha—Hb—Ni1	74.9 (13)	C18—C19—N2	124.50 (10)
N1—In1—Ni1	104.66 (3)	C18—C19—C14	116.71 (9)
N2—In1—Ni1	102.76 (2)	N2—C20—P2	108.24 (7)
N2—In1—N1	116.48 (4)	H20a—C20—P2	107.7 (8)
N3—In1—Ni1	103.32 (2)	H20a—C20—N2	115.6 (8)
N3—In1—N1	111.74 (3)	H20b—C20—P2	108.7 (8)
N3—In1—N2	115.78 (4)	H20b—C20—N2	112.6 (9)
N4—In1—Ni1	178.62 (2)	H20b—C20—H20a	103.6 (11)
N4—In1—N1	76.60 (4)	H21—C21—P2	107.0 (8)
N4—In1—N2	76.09 (3)	C23—C21—P2	112.34 (8)
N4—In1—N3	76.63 (3)	C23—C21—H21	108.1 (9)
C7—P1—Ni1	117.47 (4)	C24—C21—P2	110.02 (8)
C8—P1—Ni1	110.54 (4)	C24—C21—H21	109.2 (8)
C8—P1—C7	103.31 (5)	C24—C21—C23	110.09 (10)
C9—P1—Ni1	116.56 (4)	H22—C22—P2	104.3 (8)
C9—P1—C7	102.11 (5)	C25—C22—P2	110.95 (7)
C9—P1—C8	105.35 (5)	C25—C22—H22	108.7 (8)
C20—P2—Ni1	118.02 (4)	C26—C22—P2	115.81 (8)
C21—P2—Ni1	114.45 (4)	C26—C22—H22	107.8 (9)
C21—P2—C20	102.55 (5)	C26—C22—C25	109.00 (9)
C22—P2—Ni1	117.38 (4)	H23a—C23—C21	110.1 (8)
C22—P2—C20	100.49 (5)	H23b—C23—C21	110.9 (9)
C22—P2—C21	101.39 (5)	H23b—C23—H23a	107.1 (12)
C33—P3—Ni1	118.86 (3)	H23c—C23—C21	110.0 (9)
C34—P3—Ni1	112.80 (4)	H23c—C23—H23a	108.4 (12)
C34—P3—C33	99.02 (5)	H23c—C23—H23b	110.2 (12)
C35—P3—Ni1	118.80 (4)	H24a—C24—C21	113.3 (9)
C35—P3—C33	99.65 (5)	H24b—C24—C21	108.9 (9)
C35—P3—C34	104.94 (5)	H24b—C24—H24a	110.7 (13)
C6—N1—In1	113.05 (7)	H24c—C24—C21	112.1 (9)
C7—N1—In1	115.68 (7)	H24c—C24—H24a	106.9 (12)
C7—N1—C6	119.35 (8)	H24c—C24—H24b	104.5 (12)
C19—N2—In1	113.06 (7)	H25a—C25—C22	111.1 (8)
C20—N2—In1	118.07 (7)	H25b—C25—C22	115.0 (8)
C20—N2—C19	120.53 (9)	H25b—C25—H25a	109.0 (11)
C32—N3—In1	113.26 (7)	H25c—C25—C22	109.9 (9)
C33—N3—In1	118.74 (6)	H25c—C25—H25a	106.7 (12)
C33—N3—C32	119.49 (9)	H25c—C25—H25b	104.8 (12)
C1—N4—In1	103.25 (6)	H26a—C26—C22	108.0 (8)
C14—N4—In1	103.48 (6)	H26b—C26—C22	111.0 (9)
C14—N4—C1	115.79 (8)	H26b—C26—H26a	109.7 (12)
C27—N4—In1	102.76 (6)	H26c—C26—C22	113.1 (9)
C27—N4—C1	113.41 (8)	H26c—C26—H26a	105.4 (12)
C27—N4—C14	115.70 (8)	H26c—C26—H26b	109.5 (12)
C2—C1—N4	121.42 (9)	C28—C27—N4	121.25 (9)
C6—C1—N4	117.90 (9)	C32—C27—N4	117.83 (8)
C6—C1—C2	120.61 (9)	C32—C27—C28	120.92 (9)
H2—C2—C1	120.6 (9)	H28—C28—C27	118.8 (8)
C3—C2—C1	121.34 (10)	C29—C28—C27	121.22 (10)
C3—C2—H2	118.0 (9)	C29—C28—H28	119.9 (8)
H3—C3—C2	123.4 (9)	H29—C29—C28	119.4 (9)
C4—C3—C2	118.71 (10)	C30—C29—C28	118.50 (10)
C4—C3—H3	117.9 (9)	C30—C29—H29	122.1 (9)
H4—C4—C3	117.6 (8)	H30—C30—C29	121.6 (9)
C5—C4—C3	120.75 (10)	C31—C30—C29	121.11 (10)
C5—C4—H4	121.7 (8)	C31—C30—H30	117.3 (9)
H5—C5—C4	120.7 (9)	H31—C31—C30	119.4 (8)
C6—C5—C4	121.62 (10)	C32—C31—C30	121.44 (10)
C6—C5—H5	117.6 (9)	C32—C31—H31	119.1 (8)
C1—C6—N1	119.04 (10)	C27—C32—N3	119.25 (9)
C5—C6—N1	123.98 (10)	C31—C32—N3	124.04 (9)
C5—C6—C1	116.97 (10)	C31—C32—C27	116.71 (9)
N1—C7—P1	108.62 (8)	N3—C33—P3	111.55 (7)
H7a—C7—P1	108.3 (8)	H33a—C33—P3	105.5 (9)
H7a—C7—N1	114.8 (8)	H33a—C33—N3	112.8 (9)
H7b—C7—P1	109.9 (8)	H33b—C33—P3	107.2 (9)
H7b—C7—N1	110.9 (8)	H33b—C33—N3	114.0 (8)
H7b—C7—H7a	104.1 (12)	H33b—C33—H33a	105.3 (11)
H8—C8—P1	101.8 (9)	H34—C34—P3	104.6 (9)
C10—C8—P1	117.04 (9)	C36—C34—P3	114.77 (8)
C10—C8—H8	106.8 (9)	C36—C34—H34	107.8 (9)
C11—C8—P1	110.40 (9)	C37—C34—P3	113.40 (8)
C11—C8—H8	108.6 (9)	C37—C34—H34	104.9 (9)
C11—C8—C10	111.38 (11)	C37—C34—C36	110.59 (9)
H9—C9—P1	104.6 (8)	H35—C35—P3	105.2 (9)
C12—C9—P1	109.97 (8)	C38—C35—P3	108.61 (8)
C12—C9—H9	109.6 (8)	C38—C35—H35	107.8 (9)
C13—C9—P1	116.61 (9)	C39—C35—P3	113.41 (8)
C13—C9—H9	106.9 (8)	C39—C35—H35	109.8 (9)
C13—C9—C12	108.90 (11)	C39—C35—C38	111.66 (10)
H10a—C10—C8	115.6 (8)	H36a—C36—C34	111.5 (9)
H10b—C10—C8	112.3 (8)	H36b—C36—C34	108.8 (8)
H10b—C10—H10a	105.3 (12)	H36b—C36—H36a	110.2 (12)
H10c—C10—C8	107.7 (8)	H36c—C36—C34	110.7 (8)
H10c—C10—H10a	108.0 (12)	H36c—C36—H36a	108.4 (12)
H10c—C10—H10b	107.7 (12)	H36c—C36—H36b	107.3 (11)
H11a—C11—C8	108.8 (9)	H37a—C37—C34	107.0 (9)
H11b—C11—C8	110.9 (9)	H37b—C37—C34	112.4 (9)
H11b—C11—H11a	106.5 (13)	H37b—C37—H37a	108.5 (12)
H11c—C11—C8	112.2 (8)	H37c—C37—C34	109.4 (9)
H11c—C11—H11a	109.0 (12)	H37c—C37—H37a	110.3 (12)
H11c—C11—H11b	109.2 (12)	H37c—C37—H37b	109.3 (13)
H12a—C12—C9	109.4 (9)	H38a—C38—C35	110.9 (9)
H12b—C12—C9	111.5 (8)	H38b—C38—C35	111.6 (9)
H12b—C12—H12a	107.0 (12)	H38b—C38—H38a	106.5 (13)
H12c—C12—C9	108.3 (9)	H38c—C38—C35	110.9 (8)
H12c—C12—H12a	109.1 (12)	H38c—C38—H38a	108.6 (12)
H12c—C12—H12b	111.5 (11)	H38c—C38—H38b	108.1 (12)
H13a—C13—C9	109.1 (9)	H39a—C39—C35	112.7 (9)
H13b—C13—C9	110.7 (8)	H39b—C39—C35	112.2 (9)
H13b—C13—H13a	109.7 (12)	H39b—C39—H39a	108.3 (12)
H13c—C13—C9	112.9 (9)	H39c—C39—C35	111.5 (8)
H13c—C13—H13a	110.2 (12)	H39c—C39—H39a	106.5 (12)
H13c—C13—H13b	104.2 (12)	H39c—C39—H39b	105.3 (12)
In1—N1—C6—C1	−26.77 (8)	N2—C19—C18—C17	−179.43 (11)
In1—N1—C6—C5	152.23 (7)	N3—C32—C27—N4	−4.06 (12)
In1—N1—C7—P1	29.39 (5)	N3—C32—C27—C28	176.42 (10)
In1—N2—C19—C14	−26.58 (8)	N3—C32—C31—C30	−178.51 (12)
In1—N2—C19—C18	152.09 (7)	N4—C1—C2—C3	177.45 (10)
In1—N2—C20—P2	23.17 (6)	N4—C1—C6—C5	−176.91 (9)
In1—N3—C32—C27	−22.34 (8)	N4—C14—C15—C16	178.43 (10)
In1—N3—C32—C31	157.41 (8)	N4—C14—C19—C18	−177.81 (9)
In1—N3—C33—P3	14.25 (6)	N4—C27—C28—C29	−176.60 (11)
In1—N4—C1—C2	−157.28 (6)	N4—C27—C32—C31	176.17 (10)
In1—N4—C1—C6	19.53 (7)	C1—C2—C3—C4	−1.10 (13)
In1—N4—C14—C15	−157.05 (6)	C1—C6—C5—C4	−0.20 (12)
In1—N4—C14—C19	21.06 (7)	C2—C3—C4—C5	0.82 (13)
In1—N4—C27—C28	−156.60 (7)	C3—C4—C5—C6	−0.18 (13)
In1—N4—C27—C32	23.89 (7)	C14—C15—C16—C17	−0.64 (13)
P1—C7—N1—C6	169.64 (7)	C14—C19—C18—C17	−0.73 (12)
P2—C20—N2—C19	169.26 (7)	C15—C16—C17—C18	0.22 (14)
P3—C33—N3—C32	160.10 (7)	C16—C17—C18—C19	0.48 (15)
N1—C6—C1—N4	2.16 (11)	C27—C28—C29—C30	−0.21 (15)
N1—C6—C1—C2	179.00 (10)	C27—C32—C31—C30	1.25 (13)
N1—C6—C5—C4	−179.22 (11)	C28—C29—C30—C31	−1.91 (16)
N2—C19—C14—N4	0.97 (11)	C29—C30—C31—C32	1.36 (16)
N2—C19—C14—C15	179.08 (10)

(GOJNIF_IAM_NoMoRe)

Crystal data

C39H62InN4NiP3	Dx = 1.415 Mg m^−3
Mr = 853.39	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, P212121	Cell parameters from 9537 reflections
a = 12.2127 (4) Å	θ = 2.3–36.4°
b = 14.5402 (5) Å	µ = 1.20 mm^−1
c = 22.5601 (8) Å	T = 100 K
V = 4006.1 (2) Å^3	Block, gold
Z = 4	0.14 × 0.08 × 0.06 mm
F(000) = 1784.150

Data collection

Bruker Photon-II CMOS diffractometer	18741 reflections with I ≥ 2u(I)
φ and ω scans	Rint = 0.036
Absorption correction: multi-scan SADABS. R.Blessing, 1995	θmax = 36.4°, θmin = 2.3°
Tmin = 0.701, Tmax = 0.747	h = −20→20
237431 measured reflections	k = −24→24
19473 independent reflections	l = −37→37

Refinement

Refinement on F^2	0 constraints
Least-squares matrix: full	Only H-atom coordinates refined
R[F^2 > 2σ(F^2)] = 0.018	w = 1/[σ^2(Fo^2) + (0.0167P)^2 + 1.352P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.042	(Δ/σ)max = 0.001
S = 1.05	Δρmax = 0.43 e Å^−3
19473 reflections	Δρmin = −0.51 e Å^−3
619 parameters	Absolute structure: Flack, H. D. (1983). Acta Cryst. A39, 876-881.
0 restraints	Absolute structure parameter: 0.003 (5)

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ni1	0.755800 (10)	0.598649 (8)	0.856160 (6)	0.00937 (2)
H1A	0.7243 (18)	0.5783 (15)	0.9261 (9)	0.036333
H1B	0.756 (2)	0.6348 (14)	0.9218 (9)	0.035000
In1	0.798245 (5)	0.580830 (4)	0.749321 (3)	0.008364 (12)
P1	0.91844 (2)	0.522268 (17)	0.864329 (11)	0.00941 (4)
P2	0.59906 (2)	0.528573 (18)	0.829180 (11)	0.00948 (4)
P3	0.75362 (2)	0.750099 (17)	0.835687 (11)	0.00922 (4)
N1	0.96165 (6)	0.53377 (5)	0.74728 (4)	0.01070 (12)
N2	0.67671 (7)	0.48677 (6)	0.72033 (4)	0.01115 (14)
N3	0.78435 (7)	0.71620 (6)	0.71617 (4)	0.01051 (13)
N4	0.83420 (7)	0.56341 (5)	0.64689 (4)	0.00871 (12)
C1	0.95358 (7)	0.57174 (6)	0.64336 (4)	0.00949 (14)
C2	1.00522 (9)	0.59712 (7)	0.59113 (4)	0.01295 (16)
H2A	0.9640 (16)	0.6099 (14)	0.5564 (8)	0.028000
C3	1.11905 (9)	0.60854 (8)	0.58846 (5)	0.01474 (17)
H3A	1.1562 (17)	0.6241 (14)	0.5539 (8)	0.032000
C4	1.18017 (8)	0.59543 (7)	0.63981 (5)	0.01408 (16)
H4A	1.2571 (15)	0.6047 (13)	0.6377 (8)	0.030333
C5	1.12984 (8)	0.57038 (7)	0.69263 (5)	0.01239 (16)
H5A	1.1712 (15)	0.5607 (14)	0.7270 (8)	0.027667
C6	1.01548 (9)	0.55745 (7)	0.69637 (5)	0.00993 (16)
C7	1.01941 (9)	0.53661 (8)	0.80312 (5)	0.01143 (17)
H7A	1.0593 (15)	0.5949 (14)	0.8099 (8)	0.028000
H7B	1.0747 (16)	0.4860 (13)	0.8053 (8)	0.029000
C8	0.99550 (9)	0.56229 (8)	0.93122 (5)	0.01423 (17)
H8A	0.9806 (17)	0.6292 (13)	0.9309 (9)	0.027667
C9	0.91069 (9)	0.39460 (7)	0.87149 (5)	0.01391 (16)
H9A	0.8605 (17)	0.3851 (13)	0.9031 (9)	0.029000
C10	1.12034 (11)	0.55057 (10)	0.93044 (6)	0.0226 (2)
H10A	1.1430 (18)	0.4836 (16)	0.9283 (11)	0.049667
H10B	1.1533 (17)	0.5820 (19)	0.9695 (10)	0.051667
H10C	1.1559 (17)	0.5823 (17)	0.8971 (9)	0.041333
C11	0.94526 (13)	0.52148 (11)	0.98764 (6)	0.0268 (3)
H11A	0.981 (2)	0.5492 (16)	1.0220 (9)	0.042000
H11B	0.9546 (18)	0.4548 (18)	0.9915 (10)	0.046333
H11C	0.870 (2)	0.5359 (14)	0.9898 (9)	0.040000
C12	0.86451 (11)	0.35281 (8)	0.81440 (6)	0.0186 (2)
H12A	0.8484 (19)	0.2868 (13)	0.8213 (10)	0.040667
H12B	0.9200 (19)	0.3577 (14)	0.7844 (10)	0.042333
H12C	0.7940 (19)	0.3837 (16)	0.8027 (9)	0.045667
C13	1.01691 (11)	0.34496 (9)	0.88755 (7)	0.0238 (2)
H13A	1.0028 (19)	0.2779 (14)	0.8865 (11)	0.045333
H13B	1.045 (2)	0.3620 (16)	0.9274 (12)	0.048000
H13C	1.076 (2)	0.3600 (16)	0.8574 (11)	0.051333
C14	0.78955 (8)	0.47272 (6)	0.63324 (4)	0.00997 (14)
C15	0.82596 (8)	0.42271 (7)	0.58486 (4)	0.01225 (15)
H15A	0.8817 (16)	0.4448 (13)	0.5618 (8)	0.027000
C16	0.78504 (9)	0.33491 (7)	0.57255 (5)	0.01515 (18)
H16A	0.8146 (17)	0.2987 (14)	0.5386 (9)	0.035333
C17	0.70734 (10)	0.29757 (7)	0.61044 (5)	0.01590 (17)
H17A	0.6802 (18)	0.2360 (14)	0.6044 (9)	0.038667
C18	0.66995 (9)	0.34621 (7)	0.65958 (5)	0.01408 (17)
H18A	0.6175 (17)	0.3178 (14)	0.6868 (9)	0.033333
C19	0.70905 (8)	0.43550 (6)	0.67261 (4)	0.01038 (14)
C20	0.60328 (8)	0.44847 (7)	0.76427 (4)	0.01195 (16)
H20A	0.6212 (16)	0.3867 (12)	0.7790 (8)	0.026667
H20B	0.5266 (13)	0.4406 (12)	0.7498 (9)	0.026333
C21	0.53622 (9)	0.45616 (7)	0.88799 (5)	0.01315 (16)
H21A	0.4715 (15)	0.4268 (13)	0.8697 (8)	0.025000
C22	0.48067 (8)	0.60398 (7)	0.80768 (4)	0.01244 (16)
H22A	0.4789 (16)	0.6525 (13)	0.8378 (8)	0.025000
C23	0.61393 (11)	0.38118 (9)	0.91008 (6)	0.0207 (2)
H23A	0.5747 (19)	0.3414 (15)	0.9374 (10)	0.042333
H23B	0.6769 (19)	0.4074 (15)	0.9283 (9)	0.042333
H23C	0.6368 (17)	0.3434 (15)	0.8772 (10)	0.041667
C24	0.49920 (11)	0.51668 (9)	0.93993 (5)	0.0187 (2)
H24A	0.4503 (18)	0.5642 (15)	0.9290 (9)	0.036333
H24B	0.5606 (18)	0.5463 (15)	0.9583 (9)	0.035000
H24C	0.4665 (18)	0.4813 (16)	0.9704 (9)	0.038000
C25	0.49931 (9)	0.64751 (8)	0.74674 (6)	0.01710 (17)
H25A	0.4423 (16)	0.6930 (14)	0.7389 (9)	0.035667
H25B	0.4945 (16)	0.6014 (15)	0.7182 (9)	0.035333
H25C	0.5683 (17)	0.6788 (13)	0.7431 (9)	0.036333
C26	0.36762 (9)	0.55817 (9)	0.80854 (6)	0.01740 (19)
H26A	0.3139 (16)	0.6050 (14)	0.7992 (9)	0.036000
H26B	0.3457 (17)	0.5383 (14)	0.8461 (9)	0.037333
H26C	0.3630 (16)	0.5091 (15)	0.7810 (9)	0.034667
C27	0.77583 (8)	0.64150 (6)	0.62070 (4)	0.01023 (15)
C28	0.74274 (10)	0.64020 (7)	0.56206 (4)	0.01442 (17)
H28A	0.7551 (17)	0.5839 (13)	0.5376 (8)	0.029333
C29	0.69208 (11)	0.71658 (8)	0.53622 (5)	0.01791 (19)
H29A	0.6705 (18)	0.7128 (14)	0.4977 (9)	0.038333
C30	0.67549 (10)	0.79423 (8)	0.57069 (5)	0.01666 (19)
H30A	0.6446 (19)	0.8466 (14)	0.5549 (9)	0.036333
C31	0.70538 (9)	0.79583 (7)	0.63022 (4)	0.01306 (15)
H31A	0.6915 (18)	0.8509 (12)	0.6512 (8)	0.029333
C32	0.75536 (8)	0.71941 (6)	0.65746 (4)	0.00982 (14)
C33	0.74808 (9)	0.78805 (6)	0.75562 (4)	0.01187 (14)
H33A	0.6714 (14)	0.8061 (12)	0.7492 (9)	0.026667
H33B	0.7923 (14)	0.8433 (11)	0.7508 (9)	0.028333
C34	0.62752 (8)	0.80867 (7)	0.86344 (5)	0.01196 (16)
H34A	0.5712 (15)	0.7885 (13)	0.8367 (8)	0.026000
C35	0.86858 (9)	0.82270 (7)	0.86199 (5)	0.01280 (16)
H35A	0.8513 (16)	0.8834 (12)	0.8475 (9)	0.028000
C36	0.63058 (9)	0.91391 (7)	0.85994 (5)	0.01623 (17)
H36A	0.6540 (18)	0.9336 (14)	0.8227 (9)	0.036000
H36B	0.6827 (18)	0.9399 (14)	0.8919 (10)	0.037333
H36C	0.5541 (18)	0.9365 (14)	0.8676 (9)	0.036000
C37	0.59283 (11)	0.77707 (8)	0.92536 (5)	0.01771 (19)
H37A	0.5230 (17)	0.8044 (15)	0.9353 (9)	0.036333
H37B	0.6437 (18)	0.7986 (14)	0.9535 (9)	0.032667
H37C	0.5884 (18)	0.7119 (15)	0.9272 (9)	0.036000
C38	0.97443 (9)	0.78985 (8)	0.83204 (5)	0.01688 (19)
H38A	1.0296 (17)	0.8349 (15)	0.8357 (10)	0.041000
H38B	0.9635 (18)	0.7785 (15)	0.7882 (10)	0.042000
H38C	1.0005 (17)	0.7355 (16)	0.8490 (9)	0.036000
C39	0.87996 (10)	0.82426 (9)	0.92959 (5)	0.01781 (19)
H39A	0.948 (2)	0.8528 (17)	0.9397 (9)	0.043333
H39B	0.8716 (18)	0.7615 (16)	0.9463 (9)	0.040000
H39C	0.824 (2)	0.8585 (15)	0.9488 (9)	0.038000

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ni1	0.00865 (5)	0.00830 (5)	0.01117 (5)	−0.00038 (4)	0.00038 (4)	0.00007 (4)
H1A	0.046000	0.039000	0.024000	−0.010000	0.003000	0.006000
H1B	0.049000	0.033000	0.023000	0.002000	−0.001000	−0.005000
In1	0.00855 (2)	0.00790 (2)	0.00864 (2)	0.000111 (18)	0.00018 (2)	−0.00013 (2)
P1	0.01022 (10)	0.00961 (9)	0.00841 (10)	0.00073 (8)	−0.00063 (7)	0.00065 (8)
P2	0.00873 (9)	0.01083 (9)	0.00889 (9)	−0.00167 (8)	0.00041 (8)	−0.00026 (8)
P3	0.01105 (10)	0.00785 (8)	0.00876 (9)	−0.00024 (9)	−0.00057 (8)	−0.00081 (7)
N1	0.0093 (3)	0.0140 (3)	0.0088 (3)	0.0010 (2)	−0.0005 (3)	0.0011 (3)
N2	0.0114 (3)	0.0120 (3)	0.0100 (3)	−0.0025 (3)	0.0017 (3)	−0.0025 (3)
N3	0.0146 (4)	0.0091 (3)	0.0079 (3)	0.0016 (3)	−0.0005 (3)	−0.0003 (2)
N4	0.0097 (3)	0.0081 (3)	0.0084 (3)	0.0008 (2)	−0.0012 (2)	0.0002 (2)
C1	0.0099 (3)	0.0092 (3)	0.0093 (3)	0.0004 (3)	0.0011 (3)	−0.0005 (3)
C2	0.0154 (4)	0.0122 (4)	0.0113 (4)	0.0004 (3)	0.0024 (3)	0.0001 (3)
H2A	0.027000	0.039000	0.018000	0.000000	−0.002000	0.005000
C3	0.0157 (4)	0.0146 (4)	0.0140 (4)	−0.0009 (3)	0.0049 (3)	0.0007 (3)
H3A	0.029000	0.045000	0.022000	−0.005000	0.009000	0.007000
C4	0.0118 (4)	0.0135 (4)	0.0170 (4)	−0.0008 (3)	0.0035 (3)	−0.0002 (3)
H4A	0.017000	0.041000	0.033000	−0.004000	0.004000	0.002000
C5	0.0101 (4)	0.0138 (4)	0.0133 (4)	0.0004 (3)	0.0004 (3)	0.0000 (3)
H5A	0.020000	0.040000	0.023000	0.000000	−0.003000	0.004000
C6	0.0102 (4)	0.0095 (4)	0.0101 (4)	0.0010 (3)	0.0013 (3)	−0.0006 (3)
C7	0.0102 (4)	0.0141 (4)	0.0101 (4)	0.0010 (3)	−0.0002 (3)	0.0009 (3)
H7A	0.026000	0.031000	0.027000	−0.009000	−0.001000	0.001000
H7B	0.024000	0.034000	0.029000	0.013000	0.001000	0.005000
C8	0.0158 (4)	0.0164 (4)	0.0105 (4)	−0.0014 (3)	−0.0023 (3)	−0.0006 (3)
H8A	0.034000	0.019000	0.030000	−0.001000	−0.004000	0.002000
C9	0.0150 (4)	0.0107 (4)	0.0161 (4)	0.0015 (3)	−0.0003 (3)	0.0028 (3)
H9A	0.033000	0.024000	0.030000	0.001000	0.010000	0.006000
C10	0.0171 (5)	0.0297 (6)	0.0209 (5)	0.0006 (4)	−0.0082 (4)	−0.0037 (4)
H10A	0.031000	0.046000	0.072000	0.013000	−0.009000	−0.015000
H10B	0.028000	0.089000	0.038000	−0.013000	0.001000	0.021000
H10C	0.031000	0.061000	0.032000	−0.004000	−0.011000	−0.008000
C11	0.0342 (7)	0.0344 (7)	0.0116 (5)	−0.0096 (6)	0.0001 (4)	0.0007 (5)
H11A	0.059000	0.047000	0.020000	−0.014000	−0.007000	−0.000000
H11B	0.029000	0.071000	0.039000	0.009000	0.010000	0.020000
H11C	0.063000	0.023000	0.034000	−0.002000	0.002000	0.008000
C12	0.0244 (5)	0.0114 (4)	0.0200 (5)	−0.0007 (4)	−0.0017 (4)	−0.0020 (4)
H12A	0.057000	0.016000	0.049000	−0.003000	−0.005000	−0.002000
H12B	0.038000	0.032000	0.057000	0.009000	−0.021000	−0.009000
H12C	0.052000	0.052000	0.033000	−0.012000	0.015000	−0.011000
C13	0.0203 (5)	0.0146 (5)	0.0364 (7)	0.0057 (4)	−0.0054 (5)	0.0050 (5)
H13A	0.049000	0.019000	0.068000	0.009000	−0.010000	0.004000
H13B	0.027000	0.044000	0.073000	0.011000	0.008000	0.007000
H13C	0.058000	0.044000	0.052000	0.018000	−0.027000	−0.004000
C14	0.0118 (4)	0.0089 (3)	0.0092 (3)	0.0014 (3)	−0.0011 (3)	−0.0011 (3)
C15	0.0148 (4)	0.0124 (4)	0.0095 (3)	0.0006 (3)	0.0006 (3)	−0.0013 (3)
H15A	0.028000	0.029000	0.024000	−0.001000	0.009000	−0.002000
C16	0.0182 (5)	0.0135 (4)	0.0138 (4)	0.0002 (3)	0.0001 (3)	−0.0057 (3)
H16A	0.041000	0.034000	0.031000	−0.001000	0.009000	−0.018000
C17	0.0178 (4)	0.0123 (4)	0.0176 (4)	−0.0022 (4)	−0.0007 (4)	−0.0052 (3)
H17A	0.046000	0.026000	0.044000	−0.014000	0.007000	−0.017000
C18	0.0140 (4)	0.0123 (4)	0.0159 (4)	−0.0028 (3)	0.0006 (3)	−0.0031 (3)
H18A	0.037000	0.030000	0.033000	−0.015000	0.011000	−0.006000
C19	0.0103 (3)	0.0106 (3)	0.0103 (3)	0.0001 (3)	−0.0006 (3)	−0.0020 (3)
C20	0.0113 (4)	0.0125 (4)	0.0120 (4)	−0.0026 (3)	0.0016 (3)	−0.0020 (3)
H20A	0.032000	0.018000	0.030000	−0.000000	0.005000	0.003000
H20B	0.018000	0.035000	0.026000	−0.006000	−0.002000	−0.005000
C21	0.0129 (4)	0.0156 (4)	0.0110 (4)	−0.0039 (3)	0.0009 (3)	0.0011 (3)
H21A	0.023000	0.027000	0.025000	−0.008000	−0.001000	−0.002000
C22	0.0099 (4)	0.0154 (4)	0.0120 (4)	0.0006 (3)	0.0002 (3)	−0.0019 (3)
H22A	0.028000	0.023000	0.024000	0.000000	−0.001000	−0.007000
C23	0.0203 (5)	0.0223 (5)	0.0194 (5)	0.0003 (4)	0.0023 (4)	0.0077 (4)
H23A	0.045000	0.038000	0.044000	0.002000	0.011000	0.023000
H23B	0.053000	0.038000	0.036000	0.018000	0.007000	0.001000
H23C	0.031000	0.049000	0.045000	0.001000	−0.012000	0.008000
C24	0.0236 (5)	0.0219 (5)	0.0106 (4)	−0.0057 (4)	0.0030 (4)	−0.0013 (4)
H24A	0.047000	0.034000	0.028000	0.013000	0.002000	−0.001000
H24B	0.045000	0.036000	0.024000	−0.010000	0.012000	0.005000
H24C	0.035000	0.051000	0.028000	−0.017000	0.000000	−0.011000
C25	0.0171 (4)	0.0188 (4)	0.0154 (4)	0.0028 (3)	−0.0007 (4)	0.0021 (4)
H25A	0.033000	0.038000	0.036000	0.014000	−0.001000	0.010000
H25B	0.025000	0.044000	0.037000	−0.009000	0.000000	0.013000
H25C	0.054000	0.034000	0.021000	−0.000000	0.000000	−0.005000
C26	0.0106 (4)	0.0231 (5)	0.0184 (5)	−0.0013 (4)	−0.0009 (3)	−0.0033 (4)
H26A	0.021000	0.038000	0.049000	0.006000	−0.005000	0.007000
H26B	0.031000	0.039000	0.042000	−0.008000	−0.001000	−0.018000
H26C	0.027000	0.049000	0.028000	−0.007000	0.004000	0.008000
C27	0.0129 (4)	0.0090 (3)	0.0087 (3)	0.0013 (3)	−0.0005 (3)	0.0006 (3)
C28	0.0197 (4)	0.0135 (4)	0.0101 (4)	0.0035 (4)	−0.0024 (3)	−0.0013 (3)
H28A	0.043000	0.024000	0.021000	0.010000	−0.003000	−0.006000
C29	0.0251 (5)	0.0178 (4)	0.0108 (4)	0.0075 (4)	−0.0053 (4)	−0.0003 (3)
H29A	0.062000	0.035000	0.018000	0.016000	−0.011000	−0.000000
C30	0.0221 (5)	0.0157 (4)	0.0122 (4)	0.0075 (4)	−0.0023 (3)	0.0017 (3)
H30A	0.057000	0.025000	0.027000	0.018000	−0.006000	0.006000
C31	0.0164 (4)	0.0117 (4)	0.0110 (4)	0.0042 (3)	−0.0007 (3)	0.0006 (3)
H31A	0.044000	0.018000	0.026000	0.009000	−0.002000	−0.003000
C32	0.0109 (4)	0.0096 (3)	0.0090 (3)	0.0005 (3)	−0.0003 (3)	0.0005 (3)
C33	0.0163 (4)	0.0089 (3)	0.0104 (4)	0.0014 (3)	0.0000 (4)	−0.0007 (3)
H33A	0.026000	0.028000	0.026000	0.011000	−0.002000	−0.002000
H33B	0.039000	0.017000	0.029000	−0.007000	0.002000	−0.000000
C34	0.0136 (4)	0.0112 (4)	0.0110 (4)	0.0012 (3)	0.0005 (3)	−0.0009 (3)
H34A	0.023000	0.029000	0.026000	0.000000	−0.005000	−0.005000
C35	0.0143 (4)	0.0107 (4)	0.0134 (4)	−0.0022 (3)	−0.0006 (3)	−0.0014 (3)
H35A	0.033000	0.017000	0.034000	−0.002000	−0.002000	−0.000000
C36	0.0207 (4)	0.0114 (4)	0.0166 (4)	0.0036 (3)	0.0009 (3)	−0.0008 (4)
H36A	0.052000	0.028000	0.028000	0.003000	0.010000	0.006000
H36B	0.034000	0.028000	0.050000	0.012000	0.009000	−0.000000
H36C	0.047000	0.024000	0.037000	−0.004000	−0.008000	−0.007000
C37	0.0223 (5)	0.0174 (4)	0.0134 (4)	−0.0014 (4)	0.0038 (4)	−0.0002 (3)
H37A	0.033000	0.038000	0.038000	0.012000	0.014000	0.002000
H37B	0.042000	0.019000	0.037000	−0.002000	0.009000	0.001000
H37C	0.043000	0.042000	0.023000	−0.009000	−0.004000	−0.001000
C38	0.0147 (4)	0.0179 (5)	0.0180 (5)	−0.0039 (4)	0.0013 (4)	−0.0026 (4)
H38A	0.027000	0.044000	0.052000	−0.016000	0.005000	−0.011000
H38B	0.039000	0.038000	0.049000	0.014000	0.009000	0.016000
H38C	0.033000	0.051000	0.024000	0.001000	0.001000	−0.007000
C39	0.0190 (5)	0.0201 (5)	0.0143 (4)	−0.0027 (4)	−0.0026 (4)	−0.0042 (4)
H39A	0.035000	0.060000	0.035000	−0.021000	−0.007000	−0.009000
H39B	0.040000	0.048000	0.032000	0.006000	0.004000	−0.013000
H39C	0.051000	0.034000	0.029000	−0.003000	−0.005000	0.005000

Geometric parameters (Å, º)

Ni1—H1A	1.652 (19)	C14—C19	1.4311 (14)
Ni1—H1B	1.572 (19)	C15—H15A	0.915 (18)
Ni1—In1	2.4790 (2)	C15—C16	1.3988 (15)
Ni1—P1	2.2831 (3)	C16—H16A	0.997 (19)
Ni1—P2	2.2523 (3)	C16—C17	1.3879 (16)
Ni1—P3	2.2502 (3)	C17—H17A	0.964 (19)
H1A—H1B	0.92 (2)	C17—C18	1.3919 (15)
In1—N1	2.1102 (7)	C18—H18A	0.978 (19)
In1—N2	2.1216 (8)	C18—C19	1.4141 (14)
In1—N3	2.1124 (8)	C20—H20A	0.982 (18)
In1—N4	2.3657 (8)	C20—H20B	0.999 (17)
P1—C7	1.8631 (11)	C21—H21A	0.988 (18)
P1—C8	1.8712 (11)	C21—C23	1.5289 (17)
P1—C9	1.8658 (11)	C21—C24	1.5335 (16)
P2—C20	1.8718 (10)	C22—H22A	0.979 (18)
P2—C21	1.8595 (10)	C22—C25	1.5307 (17)
P2—C22	1.8783 (11)	C22—C26	1.5331 (15)
P3—C33	1.8900 (10)	C23—H23A	0.97 (2)
P3—C34	1.8677 (10)	C23—H23B	0.95 (2)
P3—C35	1.8540 (10)	C23—H23C	0.96 (2)
N1—C6	1.3675 (14)	C24—H24A	0.95 (2)
N1—C7	1.4444 (14)	C24—H24B	0.96 (2)
N2—C19	1.3679 (12)	C24—H24C	0.95 (2)
N2—C20	1.4480 (13)	C25—H25A	0.977 (19)
N3—C32	1.3718 (12)	C25—H25B	0.93 (2)
N3—C33	1.4420 (12)	C25—H25C	0.96 (2)
N4—C1	1.4652 (12)	C26—H26A	0.97 (2)
N4—C14	1.4598 (12)	C26—H26B	0.94 (2)
N4—C27	1.4651 (12)	C26—H26C	0.95 (2)
C1—C2	1.3866 (14)	C27—C28	1.3834 (13)
C1—C6	1.4298 (14)	C27—C32	1.4261 (13)
C2—H2A	0.950 (18)	C28—H28A	0.998 (18)
C2—C3	1.4014 (15)	C28—C29	1.3986 (15)
C3—H3A	0.930 (18)	C29—H29A	0.911 (19)
C3—C4	1.3912 (16)	C29—C30	1.3857 (16)
C4—H4A	0.950 (18)	C30—H30A	0.921 (19)
C4—C5	1.3893 (14)	C30—C31	1.3919 (15)
C5—H5A	0.936 (18)	C31—H31A	0.945 (18)
C5—C6	1.4118 (14)	C31—C32	1.4089 (13)
C7—H7A	0.990 (19)	C33—H33A	0.984 (17)
C7—H7B	1.000 (19)	C33—H33B	0.974 (16)
C8—H8A	0.990 (19)	C34—H34A	0.961 (18)
C8—C10	1.5342 (17)	C34—C36	1.5327 (15)
C8—C11	1.5325 (17)	C34—C37	1.5305 (15)
C9—H9A	0.949 (19)	C35—H35A	0.964 (18)
C9—C12	1.5319 (16)	C35—C38	1.5349 (16)
C9—C13	1.5280 (16)	C35—C39	1.5317 (16)
C10—H10A	1.01 (2)	C36—H36A	0.933 (19)
C10—H10B	1.07 (2)	C36—H36B	1.03 (2)
C10—H10C	0.98 (2)	C36—H36C	1.00 (2)
C11—H11A	0.98 (2)	C37—H37A	0.97 (2)
C11—H11B	0.98 (2)	C37—H37B	0.94 (2)
C11—H11C	0.95 (2)	C37—H37C	0.95 (2)
C12—H12A	0.99 (2)	C38—H38A	0.94 (2)
C12—H12B	0.96 (3)	C38—H38B	1.01 (2)
C12—H12C	1.01 (2)	C38—H38C	0.93 (2)
C13—H13A	0.99 (2)	C39—H39A	0.96 (2)
C13—H13B	0.99 (3)	C39—H39B	0.99 (2)
C13—H13C	1.01 (3)	C39—H39C	0.95 (2)
C14—C15	1.3848 (13)
H1B—Ni1—H1A	32.9 (9)	C15—C14—N4	121.38 (9)
In1—Ni1—H1A	163.6 (8)	C19—C14—N4	117.85 (8)
In1—Ni1—H1B	161.9 (8)	C19—C14—C15	120.74 (9)
P1—Ni1—H1A	92.2 (8)	H15A—C15—C14	120.2 (12)
P1—Ni1—H1B	94.7 (8)	C16—C15—C14	121.40 (9)
P1—Ni1—In1	81.125 (7)	C16—C15—H15A	118.2 (12)
P2—Ni1—H1A	88.8 (7)	H16A—C16—C15	120.3 (12)
P2—Ni1—H1B	114.2 (9)	C17—C16—C15	118.62 (9)
P2—Ni1—In1	82.396 (8)	C17—C16—H16A	120.9 (12)
P2—Ni1—P1	122.761 (11)	H17A—C17—C16	120.8 (12)
P3—Ni1—H1A	111.6 (8)	C18—C17—C16	121.06 (10)
P3—Ni1—H1B	82.3 (8)	C18—C17—H17A	118.1 (12)
P3—Ni1—In1	84.560 (7)	H18A—C18—C17	120.0 (12)
P3—Ni1—P1	120.194 (11)	C19—C18—C17	121.42 (10)
P3—Ni1—P2	112.159 (11)	C19—C18—H18A	118.6 (12)
H1B—H1A—Ni1	68.8 (18)	C14—C19—N2	118.73 (8)
H1A—H1B—Ni1	78.3 (19)	C18—C19—N2	124.50 (9)
N1—In1—Ni1	104.65 (3)	C18—C19—C14	116.75 (9)
N2—In1—Ni1	102.76 (2)	N2—C20—P2	108.26 (7)
N2—In1—N1	116.48 (3)	H20A—C20—P2	108.0 (11)
N3—In1—Ni1	103.30 (2)	H20A—C20—N2	116.4 (11)
N3—In1—N1	111.74 (3)	H20B—C20—P2	107.5 (11)
N3—In1—N2	115.81 (3)	H20B—C20—N2	113.6 (12)
N4—In1—Ni1	178.62 (2)	H20B—C20—H20A	102.5 (15)
N4—In1—N1	76.61 (3)	H21A—C21—P2	106.1 (11)
N4—In1—N2	76.10 (3)	C23—C21—P2	112.35 (8)
N4—In1—N3	76.64 (3)	C23—C21—H21A	108.9 (11)
C7—P1—Ni1	117.48 (3)	C24—C21—P2	110.00 (8)
C8—P1—Ni1	110.57 (4)	C24—C21—H21A	109.3 (11)
C8—P1—C7	103.30 (5)	C24—C21—C23	110.07 (10)
C9—P1—Ni1	116.54 (4)	H22A—C22—P2	105.0 (11)
C9—P1—C7	102.07 (5)	C25—C22—P2	111.03 (7)
C9—P1—C8	105.37 (5)	C25—C22—H22A	109.2 (11)
C20—P2—Ni1	118.00 (3)	C26—C22—P2	115.87 (8)
C21—P2—Ni1	114.46 (3)	C26—C22—H22A	106.5 (11)
C21—P2—C20	102.55 (5)	C26—C22—C25	108.96 (9)
C22—P2—Ni1	117.38 (3)	H23A—C23—C21	109.0 (13)
C22—P2—C20	100.51 (5)	H23B—C23—C21	110.8 (13)
C22—P2—C21	101.37 (5)	H23B—C23—H23A	111.4 (19)
C33—P3—Ni1	118.84 (3)	H23C—C23—C21	109.6 (12)
C34—P3—Ni1	112.78 (3)	H23C—C23—H23A	107.0 (18)
C34—P3—C33	99.07 (5)	H23C—C23—H23B	109.0 (17)
C35—P3—Ni1	118.85 (4)	H24A—C24—C21	114.0 (12)
C35—P3—C33	99.60 (5)	H24B—C24—C21	111.0 (12)
C35—P3—C34	104.92 (5)	H24B—C24—H24A	106.1 (18)
C6—N1—In1	113.04 (7)	H24C—C24—C21	111.6 (13)
C7—N1—In1	115.69 (7)	H24C—C24—H24A	108.7 (19)
C7—N1—C6	119.37 (8)	H24C—C24—H24B	105.0 (16)
C19—N2—In1	113.08 (6)	H25A—C25—C22	109.7 (12)
C20—N2—In1	118.05 (6)	H25B—C25—C22	108.3 (12)
C20—N2—C19	120.53 (8)	H25B—C25—H25A	108.4 (17)
C32—N3—In1	113.22 (6)	H25C—C25—C22	113.8 (12)
C33—N3—In1	118.76 (6)	H25C—C25—H25A	106.8 (16)
C33—N3—C32	119.47 (8)	H25C—C25—H25B	109.7 (16)
C1—N4—In1	103.24 (6)	H26A—C26—C22	107.6 (12)
C14—N4—In1	103.51 (5)	H26B—C26—C22	113.8 (12)
C14—N4—C1	115.78 (7)	H26B—C26—H26A	102.7 (17)
C27—N4—In1	102.75 (5)	H26C—C26—C22	111.9 (12)
C27—N4—C1	113.46 (7)	H26C—C26—H26A	110.3 (17)
C27—N4—C14	115.67 (7)	H26C—C26—H26B	110.2 (17)
C2—C1—N4	121.38 (9)	C28—C27—N4	121.15 (8)
C6—C1—N4	117.94 (8)	C32—C27—N4	117.80 (8)
C6—C1—C2	120.60 (9)	C32—C27—C28	121.05 (9)
H2A—C2—C1	120.8 (12)	H28A—C28—C27	119.7 (10)
C3—C2—C1	121.27 (10)	C29—C28—C27	121.13 (9)
C3—C2—H2A	117.8 (12)	C29—C28—H28A	119.2 (10)
H3A—C3—C2	123.3 (13)	H29A—C29—C28	118.5 (13)
C4—C3—C2	118.71 (9)	C30—C29—C28	118.54 (10)
C4—C3—H3A	118.0 (13)	C30—C29—H29A	122.9 (13)
H4A—C4—C3	118.0 (11)	H30A—C30—C29	121.1 (13)
C5—C4—C3	120.84 (9)	C31—C30—C29	121.12 (10)
C5—C4—H4A	121.2 (11)	C31—C30—H30A	117.8 (13)
H5A—C5—C4	120.7 (11)	H31A—C31—C30	116.8 (11)
C6—C5—C4	121.59 (9)	C32—C31—C30	121.42 (9)
C6—C5—H5A	117.7 (11)	C32—C31—H31A	121.8 (11)
C1—C6—N1	119.00 (9)	C27—C32—N3	119.29 (8)
C5—C6—N1	124.01 (9)	C31—C32—N3	124.04 (9)
C5—C6—C1	116.98 (9)	C31—C32—C27	116.67 (8)
N1—C7—P1	108.67 (7)	N3—C33—P3	111.55 (6)
H7A—C7—P1	107.9 (11)	H33A—C33—P3	104.7 (12)
H7A—C7—N1	113.5 (11)	H33A—C33—N3	113.2 (11)
H7B—C7—P1	109.2 (11)	H33B—C33—P3	109.2 (12)
H7B—C7—N1	110.5 (11)	H33B—C33—N3	111.0 (11)
H7B—C7—H7A	106.9 (16)	H33B—C33—H33A	106.9 (15)
H8A—C8—P1	102.0 (11)	H34A—C34—P3	103.9 (11)
C10—C8—P1	117.13 (8)	C36—C34—P3	114.70 (7)
C10—C8—H8A	107.0 (12)	C36—C34—H34A	106.8 (11)
C11—C8—P1	110.37 (8)	C37—C34—P3	113.41 (8)
C11—C8—H8A	108.2 (12)	C37—C34—H34A	106.5 (11)
C11—C8—C10	111.37 (11)	C37—C34—C36	110.70 (9)
H9A—C9—P1	104.1 (12)	H35A—C35—P3	104.3 (12)
C12—C9—P1	109.91 (7)	C38—C35—P3	108.65 (7)
C12—C9—H9A	109.6 (12)	C38—C35—H35A	108.7 (12)
C13—C9—P1	116.58 (8)	C39—C35—P3	113.32 (8)
C13—C9—H9A	107.5 (12)	C39—C35—H35A	110.0 (11)
C13—C9—C12	108.94 (10)	C39—C35—C38	111.49 (9)
H10A—C10—C8	112.2 (13)	H36A—C36—C34	111.1 (13)
H10B—C10—C8	108.5 (12)	H36B—C36—C34	110.1 (11)
H10B—C10—H10A	110.3 (19)	H36B—C36—H36A	109.2 (17)
H10C—C10—C8	113.3 (12)	H36C—C36—C34	107.2 (11)
H10C—C10—H10A	107.1 (19)	H36C—C36—H36A	109.8 (17)
H10C—C10—H10B	105.2 (17)	H36C—C36—H36B	109.4 (15)
H11A—C11—C8	108.6 (13)	H37A—C37—C34	109.5 (13)
H11B—C11—C8	114.2 (12)	H37B—C37—C34	109.5 (12)
H11B—C11—H11A	106.5 (19)	H37B—C37—H37A	106.8 (17)
H11C—C11—C8	110.3 (12)	H37C—C37—C34	110.7 (12)
H11C—C11—H11A	107.9 (19)	H37C—C37—H37A	110.5 (19)
H11C—C11—H11B	109.2 (18)	H37C—C37—H37B	109.9 (17)
H12A—C12—C9	108.9 (13)	H38A—C38—C35	110.3 (13)
H12B—C12—C9	107.6 (12)	H38B—C38—C35	111.8 (12)
H12B—C12—H12A	108.8 (17)	H38B—C38—H38A	107.0 (18)
H12C—C12—C9	111.1 (12)	H38C—C38—C35	111.7 (12)
H12C—C12—H12A	107.7 (18)	H38C—C38—H38A	108.0 (18)
H12C—C12—H12B	112.7 (17)	H38C—C38—H38B	107.9 (17)
H13A—C13—C9	108.2 (13)	H39A—C39—C35	108.8 (13)
H13B—C13—C9	113.2 (13)	H39B—C39—C35	110.8 (12)
H13B—C13—H13A	109.1 (18)	H39B—C39—H39A	113.5 (19)
H13C—C13—C9	109.9 (12)	H39C—C39—C35	113.2 (12)
H13C—C13—H13A	108.6 (19)	H39C—C39—H39A	107.1 (19)
H13C—C13—H13B	107.8 (19)	H39C—C39—H39B	103.5 (17)
In1—N1—C6—C1	−26.77 (7)	N2—C19—C18—C17	−179.37 (10)
In1—N1—C6—C5	152.20 (7)	N3—C32—C27—N4	−4.09 (11)
In1—N1—C7—P1	29.30 (5)	N3—C32—C27—C28	176.63 (10)
In1—N2—C19—C14	−26.58 (8)	N3—C32—C31—C30	−178.48 (11)
In1—N2—C19—C18	152.11 (7)	N4—C1—C2—C3	177.47 (9)
In1—N2—C20—P2	23.21 (6)	N4—C1—C6—C5	−176.88 (9)
In1—N3—C32—C27	−22.35 (8)	N4—C14—C15—C16	178.48 (9)
In1—N3—C32—C31	157.47 (7)	N4—C14—C19—C18	−177.82 (9)
In1—N3—C33—P3	14.31 (6)	N4—C27—C28—C29	−176.65 (10)
In1—N4—C1—C2	−157.33 (6)	N4—C27—C32—C31	176.07 (9)
In1—N4—C1—C6	19.53 (6)	C1—C2—C3—C4	−1.08 (12)
In1—N4—C14—C15	−156.98 (6)	C1—C6—C5—C4	−0.30 (11)
In1—N4—C14—C19	21.05 (6)	C2—C3—C4—C5	0.79 (12)
In1—N4—C27—C28	−156.78 (7)	C3—C4—C5—C6	−0.10 (12)
In1—N4—C27—C32	23.94 (6)	C14—C15—C16—C17	−0.81 (12)
P1—C7—N1—C6	169.58 (6)	C14—C19—C18—C17	−0.66 (11)
P2—C20—N2—C19	169.29 (6)	C15—C16—C17—C18	0.39 (13)
P3—C33—N3—C32	160.07 (7)	C16—C17—C18—C19	0.36 (14)
N1—C6—C1—N4	2.17 (10)	C27—C28—C29—C30	0.00 (14)
N1—C6—C1—C2	179.06 (9)	C27—C32—C31—C30	1.35 (12)
N1—C6—C5—C4	−179.29 (10)	C28—C29—C30—C31	−1.87 (15)
N2—C19—C14—N4	0.97 (10)	C29—C30—C31—C32	1.17 (15)
N2—C19—C14—C15	179.02 (9)

(GOJNIF_IAM_SHADE3)

Crystal data

C39H62InN4NiP3	Dx = 1.415 Mg m^−3
Mr = 853.39	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, P212121	Cell parameters from 9537 reflections
a = 12.2127 (4) Å	θ = 2.3–36.4°
b = 14.5402 (5) Å	µ = 1.20 mm^−1
c = 22.5601 (8) Å	T = 100 K
V = 4006.1 (2) Å^3	Block, gold
Z = 4	0.14 × 0.08 × 0.06 mm
F(000) = 105.781

Data collection

Bruker Photon-II CMOS diffractometer	18741 reflections with I ≥ 2u(I)
φ and ω scans	Rint = 0.036
Absorption correction: multi-scan SADABS. R.Blessing, 1995	θmax = 36.4°, θmin = 2.3°
Tmin = 0.701, Tmax = 0.747	h = −20→20
237431 measured reflections	k = −24→24
19473 independent reflections	l = −37→37

Refinement

Refinement on F^2	0 constraints
Least-squares matrix: full	Only H-atom coordinates refined
R[F^2 > 2σ(F^2)] = 0.025	w = 1/[σ^2(Fo^2) + (0.0265P)^2 + 3.4362P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.060	(Δ/σ)max = 0.001
S = 1.04	Δρmax = 0.44 e Å^−3
19473 reflections	Δρmin = −0.75 e Å^−3
619 parameters	Absolute structure: Flack, H. D. (1983). Acta Cryst. A39, 876-881.
0 restraints	Absolute structure parameter: 0.233 (5)

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ni1	0.755794 (14)	0.598648 (11)	0.856169 (8)	0.00909 (3)
H1A	0.724 (3)	0.577 (2)	0.9261 (13)	0.032933
H1B	0.753 (3)	0.634 (2)	0.9225 (13)	0.032963
In1	0.798243 (6)	0.580827 (5)	0.749329 (4)	0.009039 (17)
P1	0.91843 (3)	0.52227 (2)	0.864327 (15)	0.00912 (5)
P2	0.59905 (3)	0.52857 (2)	0.829181 (15)	0.00918 (5)
P3	0.75361 (3)	0.75011 (2)	0.835685 (15)	0.00892 (5)
N1	0.96166 (8)	0.53378 (8)	0.74731 (6)	0.01045 (16)
N2	0.67672 (10)	0.48675 (8)	0.72033 (5)	0.01087 (19)
N3	0.78434 (10)	0.71615 (8)	0.71617 (5)	0.01019 (18)
N4	0.83422 (9)	0.56337 (7)	0.64689 (5)	0.00850 (17)
C1	0.95358 (10)	0.57173 (9)	0.64335 (6)	0.00919 (18)
C2	1.00521 (12)	0.59713 (10)	0.59113 (6)	0.0127 (2)
H2A	0.964 (2)	0.609 (2)	0.5563 (12)	0.026173
C3	1.11907 (12)	0.60859 (11)	0.58846 (7)	0.0145 (2)
H3A	1.156 (3)	0.625 (2)	0.5544 (13)	0.029180
C4	1.18021 (11)	0.59547 (10)	0.63979 (7)	0.0138 (2)
H4A	1.256 (2)	0.603 (2)	0.6378 (12)	0.029900
C5	1.12981 (11)	0.57041 (10)	0.69263 (6)	0.0122 (2)
H5A	1.169 (2)	0.560 (2)	0.7262 (12)	0.026790
C6	1.01547 (12)	0.55744 (10)	0.69635 (6)	0.0097 (2)
C7	1.01937 (12)	0.53666 (10)	0.80311 (6)	0.0112 (2)
H7A	1.059 (2)	0.594 (2)	0.8099 (12)	0.025617
H7B	1.074 (2)	0.486 (2)	0.8058 (12)	0.026373
C8	0.99545 (13)	0.56226 (11)	0.93123 (6)	0.0139 (2)
H8A	0.982 (2)	0.6280 (19)	0.9306 (12)	0.023160
C9	0.91076 (12)	0.39462 (10)	0.87149 (7)	0.0136 (2)
H9A	0.861 (2)	0.3851 (19)	0.9036 (12)	0.024073
C10	1.12039 (15)	0.55064 (14)	0.93040 (8)	0.0223 (3)
H10A	1.143 (2)	0.484 (2)	0.9299 (14)	0.032013
H10B	1.156 (2)	0.582 (2)	0.8977 (13)	0.029943
H10C	1.152 (2)	0.583 (2)	0.9695 (13)	0.033943
C11	0.94528 (19)	0.52142 (16)	0.98763 (8)	0.0262 (4)
H11A	0.981 (3)	0.548 (2)	1.0214 (13)	0.032467
H11B	0.870 (2)	0.534 (2)	0.9901 (13)	0.028553
H11C	0.954 (3)	0.454 (2)	0.9915 (13)	0.033707
C12	0.86453 (15)	0.35277 (11)	0.81437 (8)	0.0183 (3)
H12A	0.849 (3)	0.2882 (19)	0.8215 (13)	0.030940
H12B	0.793 (2)	0.383 (2)	0.8021 (12)	0.028060
H12C	0.919 (3)	0.358 (2)	0.7841 (12)	0.029693
C13	1.01695 (16)	0.34500 (12)	0.88756 (10)	0.0233 (3)
H13A	1.003 (3)	0.280 (2)	0.8875 (14)	0.033140
H13B	1.076 (2)	0.360 (2)	0.8587 (13)	0.032587
H13C	1.044 (3)	0.362 (2)	0.9266 (13)	0.032957
C14	0.78954 (11)	0.47275 (9)	0.63324 (5)	0.00967 (19)
C15	0.82598 (12)	0.42271 (10)	0.58485 (6)	0.0120 (2)
H15A	0.881 (2)	0.445 (2)	0.5612 (12)	0.025920
C16	0.78508 (13)	0.33493 (10)	0.57253 (7)	0.0148 (2)
H16A	0.814 (3)	0.299 (2)	0.5383 (12)	0.029147
C17	0.70731 (14)	0.29756 (10)	0.61046 (7)	0.0155 (2)
H17A	0.680 (2)	0.2370 (19)	0.6034 (13)	0.030350
C18	0.66994 (12)	0.34620 (10)	0.65960 (7)	0.0138 (2)
H18A	0.618 (2)	0.319 (2)	0.6875 (12)	0.027480
C19	0.70905 (11)	0.43551 (9)	0.67261 (6)	0.01013 (19)
C20	0.60327 (12)	0.44850 (10)	0.76428 (6)	0.0116 (2)
H20A	0.622 (2)	0.3879 (19)	0.7786 (12)	0.026297
H20B	0.527 (2)	0.4406 (18)	0.7499 (14)	0.027083
C21	0.53619 (12)	0.45618 (10)	0.88800 (6)	0.0129 (2)
H21A	0.472 (2)	0.428 (2)	0.8702 (12)	0.026133
C22	0.48068 (11)	0.60398 (10)	0.80766 (6)	0.0121 (2)
H22A	0.479 (2)	0.6519 (19)	0.8371 (12)	0.023530
C23	0.61401 (15)	0.38119 (13)	0.91010 (8)	0.0203 (3)
H23A	0.575 (3)	0.343 (2)	0.9380 (14)	0.033403
H23B	0.635 (3)	0.344 (2)	0.8775 (13)	0.030193
H23C	0.676 (2)	0.407 (2)	0.9289 (13)	0.030337
C24	0.49916 (15)	0.51669 (12)	0.93997 (7)	0.0183 (3)
H24A	0.451 (2)	0.562 (2)	0.9291 (13)	0.030587
H24B	0.467 (3)	0.481 (2)	0.9697 (13)	0.033750
H24C	0.560 (2)	0.547 (2)	0.9581 (13)	0.029967
C25	0.49936 (12)	0.64749 (11)	0.74676 (9)	0.0168 (2)
H25A	0.443 (2)	0.692 (2)	0.7387 (13)	0.031203
H25B	0.568 (2)	0.6786 (19)	0.7431 (13)	0.027960
H25C	0.493 (3)	0.602 (2)	0.7178 (12)	0.030697
C26	0.36767 (13)	0.55811 (12)	0.80856 (8)	0.0170 (3)
H26A	0.314 (2)	0.605 (2)	0.7996 (14)	0.034020
H26B	0.364 (2)	0.510 (2)	0.7808 (13)	0.033997
H26C	0.345 (2)	0.540 (2)	0.8452 (13)	0.033143
C27	0.77581 (11)	0.64148 (9)	0.62073 (6)	0.0101 (2)
C28	0.74272 (14)	0.64017 (10)	0.56204 (6)	0.0142 (2)
H28A	0.753 (3)	0.5847 (19)	0.5377 (11)	0.026503
C29	0.69206 (15)	0.71656 (11)	0.53624 (7)	0.0176 (3)
H29A	0.671 (3)	0.712 (2)	0.4980 (12)	0.030493
C30	0.67544 (14)	0.79426 (11)	0.57067 (7)	0.0164 (3)
H30A	0.645 (3)	0.846 (2)	0.5546 (13)	0.031337
C31	0.70535 (13)	0.79579 (9)	0.63021 (6)	0.0128 (2)
H31A	0.692 (3)	0.8500 (18)	0.6514 (12)	0.027447
C32	0.75539 (12)	0.71946 (9)	0.65749 (5)	0.00957 (19)
C33	0.74802 (12)	0.78802 (8)	0.75564 (6)	0.01155 (19)
H33A	0.671 (2)	0.8052 (18)	0.7497 (13)	0.025540
H33B	0.791 (2)	0.8430 (17)	0.7511 (13)	0.026013
C34	0.62755 (12)	0.80866 (9)	0.86342 (6)	0.0117 (2)
H34A	0.572 (2)	0.7884 (19)	0.8369 (12)	0.023143
C35	0.86858 (12)	0.82269 (10)	0.86203 (7)	0.0126 (2)
H35A	0.851 (2)	0.8824 (18)	0.8475 (12)	0.024117
C36	0.63056 (13)	0.91387 (10)	0.85996 (7)	0.0159 (2)
H36A	0.653 (3)	0.933 (2)	0.8232 (13)	0.031200
H36B	0.555 (2)	0.936 (2)	0.8688 (13)	0.031940
H36C	0.682 (3)	0.940 (2)	0.8913 (13)	0.031447
C37	0.59282 (15)	0.77707 (11)	0.92537 (7)	0.0173 (3)
H37A	0.524 (2)	0.805 (2)	0.9345 (13)	0.029693
H37B	0.587 (3)	0.7120 (19)	0.9270 (12)	0.027917
H37C	0.642 (2)	0.799 (2)	0.9534 (13)	0.029467
C38	0.97448 (13)	0.78982 (12)	0.83203 (8)	0.0166 (3)
H38A	1.027 (2)	0.832 (2)	0.8350 (14)	0.030140
H38B	1.000 (2)	0.737 (2)	0.8486 (13)	0.028413
H38C	0.964 (2)	0.777 (2)	0.7887 (12)	0.028310
C39	0.87988 (14)	0.82430 (12)	0.92961 (7)	0.0175 (3)
H39A	0.946 (3)	0.853 (2)	0.9395 (13)	0.031073
H39B	0.823 (3)	0.857 (2)	0.9487 (13)	0.031150
H39C	0.872 (3)	0.761 (2)	0.9467 (13)	0.029307

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ni1	0.00836 (6)	0.00801 (6)	0.01090 (6)	−0.00038 (5)	0.00039 (5)	0.00006 (5)
H1A	0.043840	0.032000	0.022960	−0.006910	0.003470	0.004980
H1B	0.046820	0.029800	0.022270	−0.002710	0.000520	−0.005120
In1	0.00924 (3)	0.00855 (3)	0.00932 (3)	0.00011 (2)	0.00017 (3)	−0.00013 (3)
P1	0.00988 (13)	0.00931 (13)	0.00818 (13)	0.00073 (10)	−0.00061 (10)	0.00065 (10)
P2	0.00843 (12)	0.01055 (13)	0.00855 (13)	−0.00169 (10)	0.00042 (10)	−0.00023 (10)
P3	0.01076 (13)	0.00752 (11)	0.00849 (12)	−0.00021 (12)	−0.00057 (11)	−0.00081 (10)
N1	0.0089 (4)	0.0137 (4)	0.0087 (4)	0.0011 (3)	−0.0003 (4)	0.0012 (4)
N2	0.0111 (4)	0.0118 (4)	0.0097 (4)	−0.0025 (4)	0.0016 (3)	−0.0025 (3)
N3	0.0143 (5)	0.0087 (4)	0.0076 (4)	0.0017 (4)	−0.0007 (3)	−0.0001 (3)
N4	0.0094 (4)	0.0080 (4)	0.0081 (4)	0.0008 (3)	−0.0012 (3)	0.0003 (3)
C1	0.0096 (4)	0.0091 (5)	0.0088 (4)	0.0005 (4)	0.0013 (4)	−0.0003 (4)
C2	0.0149 (5)	0.0122 (5)	0.0110 (5)	0.0003 (4)	0.0025 (4)	0.0001 (4)
H2A	0.026740	0.032290	0.019490	0.001230	−0.001140	0.002660
C3	0.0151 (6)	0.0147 (5)	0.0136 (5)	−0.0009 (5)	0.0046 (4)	0.0008 (4)
H3A	0.028530	0.036710	0.022300	−0.002590	0.008720	0.002720
C4	0.0113 (5)	0.0134 (5)	0.0166 (5)	−0.0007 (4)	0.0036 (4)	−0.0001 (4)
H4A	0.017840	0.040640	0.031220	−0.003270	0.004440	−0.000140
C5	0.0099 (5)	0.0137 (5)	0.0129 (5)	0.0004 (4)	0.0004 (4)	0.0001 (4)
H5A	0.020880	0.036310	0.023180	−0.000220	−0.002380	0.001550
C6	0.0099 (5)	0.0095 (5)	0.0096 (5)	0.0008 (4)	0.0013 (4)	−0.0005 (4)
C7	0.0099 (5)	0.0138 (6)	0.0098 (5)	0.0008 (4)	−0.0002 (4)	0.0007 (4)
H7A	0.024920	0.025410	0.026520	−0.007350	−0.001590	−0.001430
H7B	0.023130	0.028200	0.027790	0.009260	−0.000810	0.001380
C8	0.0153 (6)	0.0162 (6)	0.0103 (5)	−0.0013 (4)	−0.0024 (4)	−0.0006 (4)
H8A	0.023880	0.020980	0.024620	0.000790	−0.001660	−0.000460
C9	0.0147 (5)	0.0103 (5)	0.0158 (6)	0.0014 (4)	−0.0003 (4)	0.0028 (4)
H9A	0.025820	0.025000	0.021400	0.000670	0.003690	0.003120
C10	0.0166 (7)	0.0291 (8)	0.0212 (7)	0.0006 (6)	−0.0082 (5)	−0.0037 (6)
H10A	0.028990	0.026710	0.040340	0.006980	−0.001360	0.001020
H10B	0.024340	0.036450	0.029040	0.000480	0.001980	0.008010
H10C	0.026650	0.049710	0.025470	0.001110	−0.008110	−0.007630
C11	0.0338 (9)	0.0337 (10)	0.0110 (6)	−0.0099 (8)	0.0001 (6)	0.0008 (6)
H11A	0.033260	0.044100	0.020040	−0.005870	−0.006750	−0.000640
H11B	0.020770	0.036000	0.028890	0.002880	0.000890	0.005010
H11C	0.045760	0.022630	0.032730	0.006210	0.004800	0.004840
C12	0.0244 (7)	0.0110 (5)	0.0194 (7)	−0.0008 (5)	−0.0016 (5)	−0.0021 (5)
H12A	0.046090	0.015950	0.030780	−0.003060	−0.002580	0.002690
H12B	0.024270	0.029780	0.030130	0.008170	−0.005390	−0.002730
H12C	0.026600	0.038900	0.023580	−0.004230	0.007180	−0.001680
C13	0.0198 (7)	0.0141 (6)	0.0361 (10)	0.0055 (5)	−0.0053 (7)	0.0051 (6)
H13A	0.037190	0.020260	0.041970	0.005270	−0.003980	0.003940
H13B	0.026460	0.040480	0.030820	0.006680	0.005990	0.009580
H13C	0.035720	0.040150	0.023000	0.008980	−0.007740	−0.002200
C14	0.0115 (5)	0.0086 (4)	0.0089 (4)	0.0014 (4)	−0.0010 (4)	−0.0011 (4)
C15	0.0147 (5)	0.0121 (5)	0.0093 (5)	0.0006 (4)	0.0006 (4)	−0.0013 (4)
H15A	0.028030	0.025870	0.023860	−0.003020	0.006990	−0.001480
C16	0.0179 (6)	0.0131 (5)	0.0134 (5)	0.0001 (5)	0.0003 (5)	−0.0054 (4)
H16A	0.036300	0.026870	0.024270	−0.000720	0.005700	−0.009510
C17	0.0175 (6)	0.0120 (5)	0.0171 (6)	−0.0023 (5)	−0.0006 (5)	−0.0051 (4)
H17A	0.037560	0.021450	0.032040	−0.008320	0.003230	−0.008260
C18	0.0139 (5)	0.0119 (5)	0.0156 (6)	−0.0029 (4)	0.0006 (4)	−0.0031 (4)
H18A	0.029490	0.025630	0.027320	−0.007940	0.006820	−0.002860
C19	0.0101 (5)	0.0104 (5)	0.0099 (5)	−0.0001 (4)	−0.0004 (4)	−0.0020 (4)
C20	0.0109 (5)	0.0122 (5)	0.0117 (5)	−0.0026 (4)	0.0016 (4)	−0.0020 (4)
H20A	0.031780	0.018810	0.028300	−0.000250	0.002950	0.002210
H20B	0.018840	0.034450	0.027960	−0.005470	−0.002300	−0.004060
C21	0.0126 (5)	0.0154 (6)	0.0107 (5)	−0.0039 (4)	0.0008 (4)	0.0010 (4)
H21A	0.021880	0.028310	0.028210	−0.007420	−0.000160	−0.003290
C22	0.0095 (5)	0.0152 (5)	0.0117 (5)	0.0005 (4)	0.0004 (4)	−0.0018 (4)
H22A	0.023290	0.025250	0.022050	0.000210	0.000980	−0.005670
C23	0.0202 (7)	0.0218 (7)	0.0188 (7)	0.0004 (6)	0.0023 (5)	0.0076 (5)
H23A	0.034620	0.030250	0.035340	−0.005040	0.010730	0.011730
H23B	0.036770	0.028370	0.025440	0.003660	0.003760	−0.005620
H23C	0.028730	0.025530	0.036750	−0.004660	−0.008490	−0.002600
C24	0.0233 (7)	0.0214 (7)	0.0102 (5)	−0.0056 (6)	0.0030 (5)	−0.0012 (5)
H24A	0.028520	0.031680	0.031560	0.006840	−0.001560	−0.002660
H24B	0.041060	0.031660	0.028530	−0.008630	0.014170	0.001890
H24C	0.022040	0.036950	0.030910	−0.005740	−0.001150	−0.009110
C25	0.0168 (5)	0.0186 (5)	0.0151 (6)	0.0028 (4)	−0.0009 (5)	0.0024 (6)
H25A	0.026690	0.036660	0.030260	0.013970	0.000250	0.003440
H25B	0.020000	0.036130	0.027750	−0.006680	−0.000690	0.002270
H25C	0.041860	0.027410	0.022820	−0.002800	−0.000310	−0.008220
C26	0.0101 (5)	0.0226 (7)	0.0184 (6)	−0.0013 (5)	−0.0010 (5)	−0.0031 (5)
H26A	0.019680	0.037190	0.045190	0.003670	−0.002970	0.000680
H26B	0.027840	0.037740	0.036410	−0.006710	0.004290	−0.017020
H26C	0.027980	0.046420	0.025030	−0.008930	0.004290	0.002010
C27	0.0129 (5)	0.0088 (5)	0.0085 (5)	0.0014 (4)	−0.0005 (4)	0.0005 (4)
C28	0.0195 (6)	0.0131 (5)	0.0099 (5)	0.0036 (5)	−0.0024 (5)	−0.0013 (4)
H28A	0.034740	0.023440	0.021330	0.005780	−0.001050	−0.005150
C29	0.0248 (7)	0.0174 (6)	0.0105 (5)	0.0074 (5)	−0.0053 (5)	−0.0003 (4)
H29A	0.041440	0.033560	0.016480	0.008330	−0.004910	0.000270
C30	0.0222 (7)	0.0152 (6)	0.0119 (5)	0.0075 (5)	−0.0025 (5)	0.0016 (4)
H30A	0.043580	0.025880	0.024550	0.013290	−0.003390	0.004630
C31	0.0165 (5)	0.0113 (5)	0.0106 (5)	0.0041 (5)	−0.0008 (4)	0.0007 (4)
H31A	0.038770	0.020490	0.023080	0.007920	−0.000530	−0.002830
C32	0.0107 (5)	0.0093 (4)	0.0088 (4)	0.0009 (4)	−0.0004 (4)	0.0005 (4)
C33	0.0158 (5)	0.0086 (4)	0.0102 (5)	0.0014 (4)	0.0000 (5)	−0.0007 (4)
H33A	0.023710	0.027880	0.025030	0.008280	−0.001490	−0.000790
H33B	0.033370	0.018100	0.026570	−0.005110	0.003520	−0.000060
C34	0.0135 (5)	0.0110 (5)	0.0107 (5)	0.0012 (4)	0.0005 (4)	−0.0009 (4)
H34A	0.023160	0.024730	0.021540	0.001030	−0.002700	−0.002790
C35	0.0141 (5)	0.0105 (5)	0.0133 (5)	−0.0022 (4)	−0.0006 (4)	−0.0015 (4)
H35A	0.030700	0.016710	0.024940	−0.000010	0.001460	0.000540
C36	0.0203 (6)	0.0110 (5)	0.0164 (6)	0.0035 (5)	0.0010 (5)	−0.0008 (5)
H36A	0.046120	0.025110	0.022370	0.001250	0.007700	0.002240
H36B	0.028490	0.026150	0.041180	0.008620	0.004860	−0.002530
H36C	0.039600	0.025130	0.029610	−0.001690	−0.009670	−0.004310
C37	0.0221 (7)	0.0171 (6)	0.0129 (6)	−0.0011 (5)	0.0039 (5)	−0.0002 (5)
H37A	0.024520	0.036080	0.028480	0.009870	0.005920	0.000070
H37B	0.037740	0.018650	0.027360	−0.002000	0.003910	−0.000780
H37C	0.029190	0.037100	0.022110	−0.007190	−0.004980	−0.002480
C38	0.0144 (6)	0.0177 (6)	0.0177 (6)	−0.0039 (5)	0.0014 (5)	−0.0028 (5)
H38A	0.025710	0.024790	0.039920	−0.010640	0.004210	−0.007270
H38B	0.031210	0.022530	0.031500	0.003840	0.004460	0.007100
H38C	0.030190	0.036580	0.018160	0.001290	−0.000160	−0.004690
C39	0.0188 (6)	0.0198 (6)	0.0140 (6)	−0.0026 (5)	−0.0028 (5)	−0.0041 (5)
H39A	0.028660	0.036800	0.027760	−0.013140	−0.002870	−0.004160
H39B	0.032180	0.035400	0.025870	0.009220	0.004590	−0.005160
H39C	0.043460	0.018950	0.025510	−0.002380	−0.001140	0.002110

Geometric parameters (Å, º)

Ni1—H1A	1.65 (3)	C14—C19	1.4311 (19)
Ni1—H1B	1.58 (3)	C15—H15A	0.92 (3)
Ni1—In1	2.4790 (2)	C15—C16	1.398 (2)
Ni1—P1	2.2831 (4)	C16—H16A	1.00 (3)
Ni1—P2	2.2523 (4)	C16—C17	1.389 (2)
Ni1—P3	2.2504 (4)	C17—H17A	0.95 (3)
H1A—H1B	0.91 (4)	C17—C18	1.392 (2)
In1—N1	2.1102 (10)	C18—H18A	0.98 (3)
In1—N2	2.1216 (12)	C18—C19	1.4145 (19)
In1—N3	2.1119 (11)	C20—H20A	0.97 (3)
In1—N4	2.3661 (11)	C20—H20B	1.00 (3)
P1—C7	1.8630 (15)	C21—H21A	0.98 (3)
P1—C8	1.8710 (15)	C21—C23	1.530 (2)
P1—C9	1.8654 (15)	C21—C24	1.534 (2)
P2—C20	1.8714 (14)	C22—H22A	0.96 (3)
P2—C21	1.8597 (14)	C22—C25	1.530 (2)
P2—C22	1.8783 (15)	C22—C26	1.533 (2)
P3—C33	1.8894 (14)	C23—H23A	0.97 (3)
P3—C34	1.8673 (14)	C23—H23B	0.95 (3)
P3—C35	1.8543 (14)	C23—H23C	0.95 (3)
N1—C6	1.3683 (19)	C24—H24A	0.92 (3)
N1—C7	1.443 (2)	C24—H24B	0.93 (3)
N2—C19	1.3676 (17)	C24—H24C	0.96 (3)
N2—C20	1.4481 (18)	C25—H25A	0.96 (3)
N3—C32	1.3710 (17)	C25—H25B	0.95 (3)
N3—C33	1.4428 (17)	C25—H25C	0.93 (3)
N4—C1	1.4650 (17)	C26—H26A	0.97 (3)
N4—C14	1.4590 (17)	C26—H26B	0.94 (3)
N4—C27	1.4652 (17)	C26—H26C	0.91 (3)
C1—C2	1.3864 (19)	C27—C28	1.3845 (19)
C1—C6	1.4297 (19)	C27—C32	1.4267 (18)
C2—H2A	0.95 (3)	C28—H28A	0.98 (3)
C2—C3	1.402 (2)	C28—C29	1.398 (2)
C3—H3A	0.92 (3)	C29—H29A	0.90 (3)
C3—C4	1.391 (2)	C29—C30	1.386 (2)
C4—H4A	0.93 (3)	C30—H30A	0.91 (3)
C4—C5	1.390 (2)	C30—C31	1.392 (2)
C5—H5A	0.91 (3)	C31—H31A	0.94 (3)
C5—C6	1.412 (2)	C31—C32	1.4085 (19)
C7—H7A	0.97 (3)	C33—H33A	0.98 (3)
C7—H7B	0.99 (3)	C33—H33B	0.96 (2)
C8—H8A	0.97 (3)	C34—H34A	0.96 (3)
C8—C10	1.535 (2)	C34—C36	1.532 (2)
C8—C11	1.532 (2)	C34—C37	1.531 (2)
C9—H9A	0.95 (3)	C35—H35A	0.95 (3)
C9—C12	1.533 (2)	C35—C38	1.536 (2)
C9—C13	1.528 (2)	C35—C39	1.531 (2)
C10—H10A	1.01 (3)	C36—H36A	0.92 (3)
C10—H10B	0.97 (3)	C36—H36B	1.00 (3)
C10—H10C	1.07 (3)	C36—H36C	1.02 (3)
C11—H11A	0.96 (3)	C37—H37A	0.96 (3)
C11—H11B	0.94 (3)	C37—H37B	0.95 (3)
C11—H11C	0.99 (3)	C37—H37C	0.93 (3)
C12—H12A	0.97 (3)	C38—H38A	0.90 (3)
C12—H12B	1.02 (3)	C38—H38B	0.91 (3)
C12—H12C	0.96 (3)	C38—H38C	1.00 (3)
C13—H13A	0.96 (3)	C39—H39A	0.94 (3)
C13—H13B	1.00 (3)	C39—H39B	0.95 (3)
C13—H13C	0.97 (3)	C39—H39C	1.00 (3)
C14—C15	1.3855 (18)
H1B—Ni1—H1A	32.6 (13)	C15—C14—N4	121.36 (12)
In1—Ni1—H1A	163.0 (11)	C19—C14—N4	117.88 (11)
In1—Ni1—H1B	163.1 (12)	C19—C14—C15	120.73 (12)
P1—Ni1—H1A	92.1 (11)	H15A—C15—C14	120.8 (17)
P1—Ni1—H1B	95.7 (12)	C16—C15—C14	121.41 (13)
P1—Ni1—In1	81.118 (10)	C16—C15—H15A	117.7 (18)
P2—Ni1—H1A	88.3 (11)	H16A—C16—C15	120.2 (17)
P2—Ni1—H1B	112.8 (13)	C17—C16—C15	118.61 (13)
P2—Ni1—In1	82.393 (11)	C17—C16—H16A	121.2 (17)
P2—Ni1—P1	122.760 (15)	H17A—C17—C16	119.7 (17)
P3—Ni1—H1A	112.3 (11)	C18—C17—C16	121.07 (13)
P3—Ni1—H1B	82.7 (11)	C18—C17—H17A	119.3 (17)
P3—Ni1—In1	84.554 (10)	H18A—C18—C17	121.1 (17)
P3—Ni1—P1	120.191 (15)	C19—C18—C17	121.40 (14)
P3—Ni1—P2	112.156 (15)	C19—C18—H18A	117.4 (17)
H1B—H1A—Ni1	69 (3)	C14—C19—N2	118.73 (11)
H1A—H1B—Ni1	78 (3)	C18—C19—N2	124.48 (13)
N1—In1—Ni1	104.63 (4)	C18—C19—C14	116.78 (12)
N2—In1—Ni1	102.76 (3)	N2—C20—P2	108.28 (9)
N2—In1—N1	116.48 (5)	H20A—C20—P2	108.2 (16)
N3—In1—Ni1	103.31 (3)	H20A—C20—N2	115.8 (17)
N3—In1—N1	111.74 (5)	H20B—C20—P2	107.5 (17)
N3—In1—N2	115.80 (5)	H20B—C20—N2	113.8 (18)
N4—In1—Ni1	178.62 (3)	H20B—C20—H20A	103 (2)
N4—In1—N1	76.62 (5)	H21A—C21—P2	106.2 (17)
N4—In1—N2	76.09 (4)	C23—C21—P2	112.30 (10)
N4—In1—N3	76.64 (4)	C23—C21—H21A	109.3 (18)
C7—P1—Ni1	117.47 (5)	C24—C21—P2	110.02 (10)
C8—P1—Ni1	110.56 (5)	C24—C21—H21A	108.8 (16)
C8—P1—C7	103.32 (7)	C24—C21—C23	110.06 (13)
C9—P1—Ni1	116.57 (5)	H22A—C22—P2	105.1 (17)
C9—P1—C7	102.08 (7)	C25—C22—P2	111.03 (10)
C9—P1—C8	105.34 (7)	C25—C22—H22A	108.9 (17)
C20—P2—Ni1	118.01 (5)	C26—C22—P2	115.82 (11)
C21—P2—Ni1	114.46 (5)	C26—C22—H22A	106.7 (17)
C21—P2—C20	102.56 (6)	C26—C22—C25	109.03 (12)
C22—P2—Ni1	117.38 (5)	H23A—C23—C21	108.7 (19)
C22—P2—C20	100.49 (6)	H23B—C23—C21	109.1 (18)
C22—P2—C21	101.37 (7)	H23B—C23—H23A	108 (3)
C33—P3—Ni1	118.83 (4)	H23C—C23—C21	111.0 (18)
C34—P3—Ni1	112.78 (5)	H23C—C23—H23A	110 (3)
C34—P3—C33	99.06 (6)	H23C—C23—H23B	111 (3)
C35—P3—Ni1	118.83 (5)	H24A—C24—C21	113.4 (19)
C35—P3—C33	99.65 (6)	H24B—C24—C21	110.8 (19)
C35—P3—C34	104.91 (6)	H24B—C24—H24A	108 (3)
C6—N1—In1	113.01 (9)	H24C—C24—C21	111.2 (17)
C7—N1—In1	115.70 (9)	H24C—C24—H24A	106 (3)
C7—N1—C6	119.40 (10)	H24C—C24—H24B	106 (3)
C19—N2—In1	113.08 (9)	H25A—C25—C22	110.0 (17)
C20—N2—In1	118.03 (9)	H25B—C25—C22	113.9 (18)
C20—N2—C19	120.57 (11)	H25B—C25—H25A	107 (2)
C32—N3—In1	113.29 (9)	H25C—C25—C22	108.9 (18)
C33—N3—In1	118.74 (8)	H25C—C25—H25A	107 (2)
C33—N3—C32	119.42 (11)	H25C—C25—H25B	110 (3)
C1—N4—In1	103.24 (8)	H26A—C26—C22	107.6 (18)
C14—N4—In1	103.51 (8)	H26B—C26—C22	111.4 (18)
C14—N4—C1	115.82 (10)	H26B—C26—H26A	111 (3)
C27—N4—In1	102.70 (8)	H26C—C26—C22	114.1 (19)
C27—N4—C1	113.46 (10)	H26C—C26—H26A	101 (3)
C27—N4—C14	115.66 (10)	H26C—C26—H26B	112 (3)
C2—C1—N4	121.39 (12)	C28—C27—N4	121.11 (12)
C6—C1—N4	117.93 (11)	C32—C27—N4	117.84 (11)
C6—C1—C2	120.60 (12)	C32—C27—C28	121.04 (12)
H2A—C2—C1	120.5 (17)	H28A—C28—C27	120.6 (16)
C3—C2—C1	121.28 (13)	C29—C28—C27	121.09 (13)
C3—C2—H2A	118.2 (17)	C29—C28—H28A	118.3 (16)
H3A—C3—C2	123.4 (19)	H29A—C29—C28	118.2 (19)
C4—C3—C2	118.72 (13)	C30—C29—C28	118.62 (13)
C4—C3—H3A	117.9 (19)	C30—C29—H29A	123.1 (19)
H4A—C4—C3	118.3 (18)	H30A—C30—C29	120.5 (19)
C5—C4—C3	120.80 (13)	C31—C30—C29	121.02 (14)
C5—C4—H4A	120.9 (18)	C31—C30—H30A	118.5 (19)
H5A—C5—C4	121.4 (18)	H31A—C31—C30	117.4 (17)
C6—C5—C4	121.60 (13)	C32—C31—C30	121.53 (13)
C6—C5—H5A	116.9 (18)	C32—C31—H31A	121.1 (17)
C1—C6—N1	119.03 (12)	C27—C32—N3	119.23 (11)
C5—C6—N1	123.97 (13)	C31—C32—N3	124.15 (12)
C5—C6—C1	116.99 (12)	C31—C32—C27	116.62 (11)
N1—C7—P1	108.67 (10)	N3—C33—P3	111.56 (8)
H7A—C7—P1	107.8 (17)	H33A—C33—P3	103.8 (18)
H7A—C7—N1	113.9 (16)	H33A—C33—N3	113.2 (17)
H7B—C7—P1	108.3 (16)	H33B—C33—P3	109.0 (17)
H7B—C7—N1	111.1 (16)	H33B—C33—N3	111.7 (16)
H7B—C7—H7A	107 (2)	H33B—C33—H33A	107 (2)
H8A—C8—P1	101.9 (17)	H34A—C34—P3	103.9 (16)
C10—C8—P1	117.10 (11)	C36—C34—P3	114.73 (10)
C10—C8—H8A	106.3 (17)	C36—C34—H34A	107.1 (17)
C11—C8—P1	110.39 (11)	C37—C34—P3	113.42 (10)
C11—C8—H8A	109.0 (17)	C37—C34—H34A	106.3 (17)
C11—C8—C10	111.40 (15)	C37—C34—C36	110.66 (12)
H9A—C9—P1	104.0 (17)	H35A—C35—P3	103.9 (17)
C12—C9—P1	109.92 (10)	C38—C35—P3	108.61 (10)
C12—C9—H9A	110.2 (17)	C38—C35—H35A	108.6 (17)
C13—C9—P1	116.60 (11)	C39—C35—P3	113.34 (11)
C13—C9—H9A	106.9 (17)	C39—C35—H35A	110.4 (16)
C13—C9—C12	108.94 (14)	C39—C35—C38	111.57 (13)
H10A—C10—C8	111.9 (18)	H36A—C36—C34	111.1 (18)
H10B—C10—C8	113.5 (17)	H36B—C36—C34	106.9 (17)
H10B—C10—H10A	109 (3)	H36B—C36—H36A	111 (3)
H10C—C10—C8	107.7 (16)	H36C—C36—C34	110.3 (17)
H10C—C10—H10A	109 (2)	H36C—C36—H36A	109 (3)
H10C—C10—H10B	105 (2)	H36C—C36—H36B	108 (2)
H11A—C11—C8	108.8 (19)	H37A—C37—C34	108.3 (18)
H11B—C11—C8	111.2 (18)	H37B—C37—C34	110.7 (17)
H11B—C11—H11A	109 (3)	H37B—C37—H37A	110 (3)
H11C—C11—C8	114.5 (18)	H37C—C37—C34	110.0 (18)
H11C—C11—H11A	106 (3)	H37C—C37—H37A	107 (3)
H11C—C11—H11B	107 (3)	H37C—C37—H37B	111 (3)
H12A—C12—C9	108.4 (17)	H38A—C38—C35	111.1 (19)
H12B—C12—C9	112.0 (16)	H38B—C38—C35	111.7 (18)
H12B—C12—H12A	107 (2)	H38B—C38—H38A	108 (3)
H12C—C12—C9	108.3 (18)	H38C—C38—C35	111.9 (17)
H12C—C12—H12A	109 (3)	H38C—C38—H38A	107 (3)
H12C—C12—H12B	112 (2)	H38C—C38—H38B	107 (3)
H13A—C13—C9	108.2 (19)	H39A—C39—C35	108.8 (18)
H13B—C13—C9	110.8 (17)	H39B—C39—C35	113.3 (18)
H13B—C13—H13A	111 (3)	H39B—C39—H39A	107 (3)
H13C—C13—C9	112.6 (19)	H39C—C39—C35	111.3 (17)
H13C—C13—H13A	108 (3)	H39C—C39—H39A	113 (3)
H13C—C13—H13B	107 (3)	H39C—C39—H39B	103 (3)
In1—N1—C6—C1	−26.73 (10)	N2—C19—C18—C17	−179.35 (15)
In1—N1—C6—C5	152.18 (9)	N3—C32—C27—N4	−4.18 (15)
In1—N1—C7—P1	29.34 (7)	N3—C32—C27—C28	176.62 (13)
In1—N2—C19—C14	−26.56 (11)	N3—C32—C31—C30	−178.45 (15)
In1—N2—C19—C18	152.10 (10)	N4—C1—C2—C3	177.47 (13)
In1—N2—C20—P2	23.18 (8)	N4—C1—C6—C5	−176.87 (12)
In1—N3—C32—C27	−22.30 (11)	N4—C14—C15—C16	178.46 (13)
In1—N3—C32—C31	157.41 (10)	N4—C14—C19—C18	−177.78 (12)
In1—N3—C33—P3	14.34 (8)	N4—C27—C28—C29	−176.64 (14)
In1—N4—C1—C2	−157.31 (8)	N4—C27—C32—C31	176.09 (12)
In1—N4—C1—C6	19.56 (9)	C1—C2—C3—C4	−1.08 (16)
In1—N4—C14—C15	−156.97 (8)	C1—C6—C5—C4	−0.33 (15)
In1—N4—C14—C19	21.02 (9)	C2—C3—C4—C5	0.77 (17)
In1—N4—C27—C28	−156.81 (9)	C3—C4—C5—C6	−0.07 (17)
In1—N4—C27—C32	23.99 (9)	C14—C15—C16—C17	−0.83 (17)
P1—C7—N1—C6	169.62 (9)	C14—C19—C18—C17	−0.67 (15)
P2—C20—N2—C19	169.30 (9)	C15—C16—C17—C18	0.38 (18)
P3—C33—N3—C32	160.13 (9)	C16—C17—C18—C19	0.37 (19)
N1—C6—C1—N4	2.12 (14)	C27—C28—C29—C30	0.03 (19)
N1—C6—C1—C2	179.01 (12)	C27—C32—C31—C30	1.27 (16)
N1—C6—C5—C4	−179.26 (14)	C28—C29—C30—C31	−1.9 (2)
N2—C19—C14—N4	0.98 (14)	C29—C30—C31—C32	1.2 (2)
N2—C19—C14—C15	178.99 (12)

 

(KCPTCR_HAR_0_HADPs)

Crystal data

C28H37Cr2KN2O16	F(000) = 1660.306
Mr = 800.70	Dx = 1.489 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71069 Å
a = 10.458 Å	Cell parameters from 1024 reflections
b = 14.417 Å	θ = 47.5–1.5°
c = 23.882 Å	µ = 0.80 mm^−1
β = 97.26°	T = 28 K
V = 3571.89 Å^3	Ellipsoidal, yellow
Z = 4	0.3 × 0.25 × 0.2 mm

Data collection

SMART CCD diffractometer	22531 reflections with I ≥ 2u(I)
ω scan	Rint = 0.0000
Absorption correction: empirical (using intensity measurements)	θmax = 48.7°, θmin = 2.4°
Tmin = 0.890, Tmax = 0.903	h = −19→20
27917 measured reflections	k = 0→30
27917 independent reflections	l = 0→50

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.032	Only H-atom coordinates refined
wR(F^2) = 0.104	w = 1/[σ^2(Fo^2) + (0.1P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 0.72	(Δ/σ)max = 0.0002
27917 reflections	Δρmax = 0.76 e Å^−3
553 parameters	Δρmin = −1.17 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Cr1	0.163874 (10)	0.002349 (6)	0.236375 (4)	0.005207 (18)
Cr2	0.018762 (11)	0.177452 (6)	0.165108 (4)	0.005772 (18)
K1	0.463717 (13)	0.199293 (8)	0.418000 (5)	0.00654 (2)
O1	0.25209 (6)	0.13809 (4)	0.33121 (2)	0.01180 (8)
O2	−0.08353 (6)	−0.04365 (4)	0.28575 (3)	0.01417 (9)
O3	0.10466 (6)	−0.12659 (4)	0.13547 (2)	0.01253 (9)
O4	0.39545 (6)	0.05450 (4)	0.17751 (3)	0.01359 (9)
O5	0.30034 (6)	−0.15033 (4)	0.30579 (3)	0.01230 (9)
O6	−0.25957 (6)	0.12167 (4)	0.17223 (2)	0.01233 (9)
O7	0.01680 (6)	0.05855 (4)	0.05955 (2)	0.01260 (9)
O8	0.28637 (6)	0.25363 (4)	0.15524 (3)	0.01338 (9)
O9	0.02670 (7)	0.26566 (4)	0.28174 (3)	0.01766 (11)
O10	−0.07201 (7)	0.34766 (4)	0.09923 (3)	0.01448 (10)
O11	0.28571 (5)	0.09214 (3)	0.47314 (2)	0.00780 (7)
O12	0.44342 (5)	0.00265 (3)	0.40246 (2)	0.00833 (7)
O13	0.31317 (5)	0.34096 (3)	0.36293 (2)	0.00873 (7)
O14	0.52821 (5)	0.26679 (3)	0.31528 (2)	0.00888 (7)
O15	0.55089 (5)	0.32678 (4)	0.50766 (2)	0.00926 (7)
O16	0.72730 (5)	0.20516 (3)	0.46497 (2)	0.00821 (7)
N1	0.27305 (6)	0.30200 (4)	0.47985 (2)	0.00781 (8)
N2	0.66189 (6)	0.09452 (4)	0.36196 (2)	0.00692 (7)
C1	0.21620 (7)	0.08860 (4)	0.29508 (3)	0.00814 (9)
C2	0.01010 (7)	−0.02689 (4)	0.26770 (3)	0.00876 (9)
C3	0.12293 (7)	−0.07915 (4)	0.17412 (3)	0.00847 (9)
C4	0.30810 (7)	0.03662 (4)	0.20002 (3)	0.00897 (9)
C5	0.25021 (7)	−0.09118 (4)	0.27863 (3)	0.00842 (9)
C6	−0.15453 (7)	0.14179 (4)	0.16995 (3)	0.00870 (9)
C7	0.01878 (7)	0.10405 (4)	0.09913 (3)	0.00825 (9)
C8	0.18815 (7)	0.22109 (4)	0.16011 (3)	0.00896 (9)
C9	0.02388 (8)	0.23370 (5)	0.23776 (3)	0.01106 (10)
C10	−0.03870 (7)	0.28242 (4)	0.12526 (3)	0.00929 (9)
C11	0.20815 (7)	0.23294 (4)	0.51163 (3)	0.00902 (9)
C12	0.17310 (7)	0.14344 (4)	0.47988 (3)	0.00863 (9)
C13	0.25207 (7)	0.00543 (4)	0.44643 (3)	0.00781 (9)
C14	0.37236 (7)	−0.04781 (4)	0.43910 (3)	0.00815 (9)
C15	0.54822 (7)	−0.04991 (4)	0.38674 (3)	0.00805 (9)
C16	0.60989 (7)	0.00369 (4)	0.34255 (3)	0.00813 (9)
C17	0.17935 (7)	0.34654 (5)	0.43700 (3)	0.00924 (9)
C18	0.24062 (7)	0.40164 (4)	0.39331 (3)	0.00968 (9)
C19	0.37490 (8)	0.38881 (5)	0.32182 (3)	0.01084 (10)
C20	0.42820 (8)	0.31882 (5)	0.28403 (3)	0.01079 (10)
C21	0.57211 (7)	0.19483 (4)	0.28134 (3)	0.00943 (9)
C22	0.69038 (7)	0.14949 (4)	0.31300 (3)	0.00919 (9)
C23	0.33593 (7)	0.37155 (5)	0.51923 (3)	0.01008 (10)
C24	0.46539 (7)	0.34038 (5)	0.54888 (3)	0.01026 (10)
C25	0.68009 (7)	0.31745 (4)	0.53319 (3)	0.00875 (9)
C26	0.76442 (7)	0.29314 (4)	0.48874 (3)	0.00913 (9)
C27	0.82386 (7)	0.16972 (5)	0.43396 (3)	0.00908 (9)
C28	0.77753 (7)	0.08189 (4)	0.40292 (3)	0.00833 (9)
H	0.0487 (12)	0.0771 (9)	0.2000 (5)	0.000000
H1A	0.1187 (12)	0.2627 (8)	0.5261 (5)	0.000000
H1B	0.2745 (12)	0.2156 (8)	0.5499 (5)	0.000000
H1C	0.1186 (12)	0.1570 (8)	0.4365 (5)	0.000000
H1D	0.1093 (11)	0.1027 (8)	0.5038 (5)	0.000000
H1E	0.1947 (12)	0.0161 (8)	0.4056 (5)	0.000000
H1F	0.1921 (12)	−0.0353 (8)	0.4720 (5)	0.000000
H1G	0.3422 (11)	−0.1149 (8)	0.4210 (5)	0.000000
H1H	0.4276 (11)	−0.0578 (8)	0.4804 (5)	0.000000
H1I	0.5113 (12)	−0.1161 (8)	0.3678 (5)	0.000000
H1J	0.6130 (11)	−0.0694 (8)	0.4241 (5)	0.000000
H1K	0.5370 (12)	0.0182 (8)	0.3071 (5)	0.000000
H1L	0.6850 (12)	−0.0387 (8)	0.3280 (5)	0.000000
H1M	0.1241 (12)	0.2924 (8)	0.4142 (5)	0.000000
H1N	0.1135 (11)	0.3914 (8)	0.4561 (5)	0.000000
H1O	0.1638 (12)	0.4367 (8)	0.3629 (5)	0.000000
H1P	0.3029 (11)	0.4577 (8)	0.4123 (5)	0.000000
H1Q	0.4515 (12)	0.4318 (8)	0.3427 (5)	0.000000
H1R	0.3069 (11)	0.4331 (8)	0.2962 (5)	0.000000
H2A	0.3500 (11)	0.2736 (8)	0.2666 (5)	0.000000
H2B	0.4684 (12)	0.3539 (8)	0.2493 (5)	0.000000
H2C	0.5955 (12)	0.2242 (9)	0.2405 (5)	0.000000
H2D	0.4967 (11)	0.1463 (8)	0.2693 (5)	0.000000
H2E	0.7351 (12)	0.1051 (8)	0.2837 (5)	0.000000
H2F	0.7558 (12)	0.2075 (8)	0.3274 (5)	0.000000
H2G	0.3558 (11)	0.4334 (8)	0.4974 (5)	0.000000
H2H	0.2732 (12)	0.3954 (9)	0.5512 (5)	0.000000
H2I	0.4571 (12)	0.2739 (9)	0.5739 (5)	0.000000
H2J	0.5079 (12)	0.3937 (8)	0.5787 (5)	0.000000
H2K	0.7142 (11)	0.3810 (8)	0.5544 (5)	0.000000
H2L	0.6878 (12)	0.2636 (8)	0.5666 (5)	0.000000
H2M	0.7587 (12)	0.3477 (8)	0.4548 (5)	0.000000
H2N	0.8637 (11)	0.2922 (8)	0.5086 (5)	0.000000
H2O	0.8500 (12)	0.2236 (8)	0.4061 (5)	0.000000
H2P	0.9112 (12)	0.1517 (8)	0.4658 (5)	0.000000
H2Q	0.8587 (12)	0.0527 (8)	0.3833 (5)	0.000000
H2R	0.7550 (11)	0.0325 (8)	0.4335 (5)	0.000000

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cr1	0.00566 (4)	0.00461 (3)	0.00533 (4)	0.00020 (2)	0.00060 (3)	−0.00016 (2)
Cr2	0.00676 (4)	0.00531 (3)	0.00511 (4)	0.00087 (3)	0.00021 (3)	0.00018 (2)
K1	0.00624 (5)	0.00669 (4)	0.00663 (5)	0.00019 (3)	0.00058 (3)	−0.00004 (3)
O1	0.0155 (2)	0.00917 (16)	0.0097 (2)	−0.00008 (16)	−0.00230 (16)	−0.00282 (14)
O2	0.0105 (2)	0.0167 (2)	0.0166 (2)	−0.00024 (18)	0.00654 (18)	0.00139 (17)
O3	0.0152 (2)	0.01220 (18)	0.0102 (2)	−0.00197 (17)	0.00164 (16)	−0.00496 (15)
O4	0.0108 (2)	0.01394 (19)	0.0173 (2)	−0.00099 (18)	0.00691 (18)	0.00010 (17)
O5	0.0136 (2)	0.00915 (16)	0.0135 (2)	0.00353 (16)	−0.00099 (16)	0.00245 (15)
O6	0.0096 (2)	0.01497 (19)	0.0130 (2)	−0.00108 (17)	0.00340 (16)	0.00016 (16)
O7	0.0169 (3)	0.01222 (18)	0.0090 (2)	−0.00136 (17)	0.00288 (17)	−0.00339 (14)
O8	0.0110 (2)	0.0161 (2)	0.0129 (2)	−0.00540 (18)	0.00069 (16)	0.00073 (16)
O9	0.0261 (3)	0.0172 (2)	0.0089 (2)	0.0096 (2)	−0.0010 (2)	−0.00483 (17)
O10	0.0177 (3)	0.00946 (17)	0.0152 (2)	0.00298 (17)	−0.00219 (18)	0.00423 (16)
O11	0.00644 (19)	0.00765 (14)	0.00926 (18)	−0.00018 (13)	0.00081 (13)	−0.00095 (12)
O12	0.0089 (2)	0.00665 (14)	0.00989 (19)	0.00079 (13)	0.00284 (14)	0.00101 (12)
O13	0.0096 (2)	0.00708 (14)	0.00983 (19)	0.00084 (14)	0.00233 (14)	0.00114 (12)
O14	0.0101 (2)	0.00880 (15)	0.00766 (18)	0.00178 (14)	0.00083 (14)	0.00055 (12)
O15	0.0075 (2)	0.01242 (17)	0.00766 (18)	0.00117 (15)	0.00029 (13)	−0.00174 (13)
O16	0.00612 (19)	0.00872 (15)	0.00983 (19)	−0.00103 (13)	0.00121 (13)	−0.00237 (13)
N1	0.0069 (2)	0.00787 (16)	0.0087 (2)	0.00122 (15)	0.00098 (15)	−0.00052 (13)
N2	0.0072 (2)	0.00694 (15)	0.00674 (18)	−0.00007 (14)	0.00133 (14)	−0.00015 (13)
C1	0.0096 (2)	0.00679 (17)	0.0077 (2)	−0.00001 (17)	−0.00030 (17)	−0.00076 (15)
C2	0.0082 (3)	0.00892 (18)	0.0095 (2)	0.00038 (18)	0.00269 (17)	0.00050 (16)
C3	0.0093 (2)	0.00800 (18)	0.0081 (2)	−0.00027 (17)	0.00110 (17)	−0.00150 (15)
C4	0.0081 (3)	0.00912 (19)	0.0100 (2)	−0.00054 (18)	0.00257 (17)	−0.00038 (16)
C5	0.0088 (2)	0.00688 (17)	0.0094 (2)	0.00119 (17)	0.00031 (17)	0.00045 (15)
C6	0.0089 (3)	0.00945 (18)	0.0078 (2)	0.00080 (18)	0.00143 (17)	0.00025 (15)
C7	0.0095 (2)	0.00820 (18)	0.0071 (2)	−0.00039 (17)	0.00113 (17)	−0.00119 (15)
C8	0.0094 (3)	0.00888 (18)	0.0084 (2)	−0.00115 (18)	0.00009 (17)	0.00013 (16)
C9	0.0144 (3)	0.0103 (2)	0.0081 (2)	0.0038 (2)	−0.00017 (19)	−0.00178 (17)
C10	0.0111 (3)	0.00712 (17)	0.0092 (2)	0.00145 (18)	−0.00031 (18)	0.00134 (16)
C11	0.0094 (3)	0.00980 (19)	0.0081 (2)	0.00139 (18)	0.00229 (17)	−0.00032 (16)
C12	0.0065 (2)	0.00932 (19)	0.0102 (2)	0.00005 (17)	0.00157 (17)	0.00007 (16)
C13	0.0072 (2)	0.00793 (18)	0.0084 (2)	−0.00154 (16)	0.00151 (16)	−0.00027 (15)
C14	0.0095 (3)	0.00667 (17)	0.0085 (2)	−0.00024 (17)	0.00208 (17)	0.00074 (15)
C15	0.0079 (2)	0.00658 (17)	0.0097 (2)	0.00065 (17)	0.00127 (17)	0.00038 (15)
C16	0.0093 (3)	0.00757 (17)	0.0076 (2)	−0.00024 (17)	0.00122 (17)	−0.00078 (15)
C17	0.0073 (2)	0.0101 (2)	0.0105 (2)	0.00177 (18)	0.00170 (17)	0.00127 (17)
C18	0.0102 (3)	0.00774 (18)	0.0115 (2)	0.00187 (18)	0.00299 (19)	0.00150 (16)
C19	0.0124 (3)	0.00808 (19)	0.0126 (3)	0.00222 (19)	0.0039 (2)	0.00306 (17)
C20	0.0123 (3)	0.0117 (2)	0.0085 (2)	0.0030 (2)	0.00197 (19)	0.00313 (17)
C21	0.0120 (3)	0.00888 (19)	0.0073 (2)	0.00165 (18)	0.00096 (18)	0.00047 (16)
C22	0.0096 (3)	0.00967 (19)	0.0089 (2)	0.00099 (18)	0.00335 (18)	0.00170 (16)
C23	0.0086 (3)	0.0098 (2)	0.0117 (2)	0.00137 (18)	0.00068 (18)	−0.00329 (17)
C24	0.0079 (3)	0.0138 (2)	0.0089 (2)	0.00042 (19)	0.00081 (18)	−0.00303 (18)
C25	0.0082 (2)	0.00950 (19)	0.0083 (2)	−0.00049 (18)	0.00005 (17)	−0.00192 (16)
C26	0.0075 (3)	0.00887 (19)	0.0110 (2)	−0.00130 (17)	0.00131 (18)	−0.00206 (16)
C27	0.0074 (2)	0.0099 (2)	0.0100 (2)	−0.00086 (18)	0.00141 (17)	−0.00199 (16)
C28	0.0075 (2)	0.00827 (18)	0.0092 (2)	0.00082 (17)	0.00094 (17)	−0.00062 (16)
H	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1D	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1E	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1F	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1G	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1H	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1I	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1J	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1K	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1L	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1M	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1N	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1O	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1P	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1Q	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1R	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2D	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2E	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2F	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2G	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2H	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2I	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2J	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2K	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2L	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2M	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2N	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2O	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2P	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2Q	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2R	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000

Geometric parameters (Å, º)

Cr1—C1	1.9020 (6)	N2—C22	1.4738 (8)
Cr1—C2	1.9046 (7)	N2—C28	1.4676 (9)
Cr1—C3	1.9009 (6)	C11—C12	1.5179 (9)
Cr1—C4	1.8984 (7)	C11—H1A	1.123 (12)
Cr1—C5	1.8498 (6)	C11—H1B	1.105 (12)
Cr1—H	1.761 (13)	C12—H1C	1.134 (12)
Cr2—C6	1.9014 (7)	C12—H1D	1.102 (12)
Cr2—C7	1.8980 (6)	C13—C14	1.5027 (10)
Cr2—C8	1.8978 (7)	C13—H1E	1.088 (12)
Cr2—C9	1.9099 (7)	C13—H1F	1.099 (12)
Cr2—C10	1.8473 (6)	C14—H1G	1.090 (12)
Cr2—H	1.679 (13)	C14—H1H	1.089 (12)
K1—O1	2.9688 (6)	C15—C16	1.5161 (9)
K1—O11	2.8646 (5)	C15—H1I	1.104 (12)
K1—O12	2.8636 (5)	C15—H1J	1.087 (12)
K1—O13	2.8030 (5)	C16—H1K	1.086 (12)
K1—O14	2.7996 (5)	C16—H1L	1.087 (12)
K1—O15	2.8810 (5)	C17—C18	1.5163 (10)
K1—O16	2.8430 (5)	C17—H1M	1.076 (12)
K1—N1	3.0158 (6)	C17—H1N	1.086 (12)
K1—N2	3.0115 (6)	C18—H1O	1.132 (12)
O1—C1	1.1456 (8)	C18—H1P	1.100 (12)
O2—C2	1.1443 (9)	C19—C20	1.5068 (10)
O3—C3	1.1453 (8)	C19—H1Q	1.083 (12)
O4—C4	1.1463 (9)	C19—H1R	1.085 (12)
O5—C5	1.1561 (8)	C20—H2A	1.086 (12)
O6—C6	1.1441 (9)	C20—H2B	1.099 (12)
O7—C7	1.1487 (8)	C21—C22	1.5141 (10)
O8—C8	1.1485 (9)	C21—H2C	1.117 (12)
O9—C9	1.1438 (9)	C21—H2D	1.067 (12)
O10—C10	1.1566 (8)	C22—H2E	1.096 (12)
O11—C12	1.4169 (8)	C22—H2F	1.107 (12)
O11—C13	1.4272 (8)	C23—C24	1.5146 (10)
O12—C14	1.4183 (8)	C23—H2G	1.066 (11)
O12—C15	1.4214 (8)	C23—H2H	1.121 (12)
O13—C18	1.4165 (8)	C24—H2I	1.138 (12)
O13—C19	1.4202 (8)	C24—H2J	1.103 (12)
O14—C20	1.4200 (9)	C25—C26	1.5047 (10)
O14—C21	1.4277 (8)	C25—H2K	1.085 (12)
O15—C24	1.4247 (9)	C25—H2L	1.110 (12)
O15—C25	1.4168 (9)	C26—H2M	1.126 (12)
O16—C26	1.4234 (8)	C26—H2N	1.086 (12)
O16—C27	1.4206 (9)	C27—C28	1.5155 (9)
N1—C11	1.4691 (9)	C27—H2O	1.079 (11)
N1—C17	1.4718 (9)	C27—H2P	1.143 (12)
N1—C23	1.4718 (9)	C28—H2Q	1.104 (12)
N2—C16	1.4702 (8)	C28—H2R	1.068 (11)
C2—Cr1—C1	91.93 (3)	H1A—C11—N1	110.9 (6)
C3—Cr1—C1	174.90 (3)	H1A—C11—C12	108.7 (6)
C3—Cr1—C2	93.01 (3)	H1B—C11—N1	107.4 (6)
C4—Cr1—C1	89.76 (3)	H1B—C11—C12	107.9 (6)
C4—Cr1—C2	175.08 (3)	H1B—C11—H1A	107.0 (9)
C4—Cr1—C3	85.22 (3)	C11—C12—O11	110.41 (6)
C5—Cr1—C1	89.96 (3)	H1C—C12—O11	108.4 (6)
C5—Cr1—C2	90.15 (3)	H1C—C12—C11	111.8 (6)
C5—Cr1—C3	91.28 (3)	H1D—C12—O11	110.3 (6)
C5—Cr1—C4	94.47 (3)	H1D—C12—C11	108.6 (6)
H—Cr1—C1	94.5 (4)	H1D—C12—H1C	107.3 (9)
H—Cr1—C2	76.7 (4)	C14—C13—O11	109.68 (6)
H—Cr1—C3	85.4 (4)	H1E—C13—O11	110.7 (6)
H—Cr1—C4	98.5 (4)	H1E—C13—C14	110.0 (7)
H—Cr1—C5	166.2 (4)	H1F—C13—O11	110.2 (6)
C7—Cr2—C6	89.99 (3)	H1F—C13—C14	109.7 (6)
C8—Cr2—C6	176.32 (3)	H1F—C13—H1E	106.6 (9)
C8—Cr2—C7	91.98 (3)	C13—C14—O12	108.76 (5)
C9—Cr2—C6	88.68 (3)	H1G—C14—O12	111.0 (6)
C9—Cr2—C7	171.11 (3)	H1G—C14—C13	107.2 (6)
C9—Cr2—C8	89.84 (3)	H1H—C14—O12	111.6 (6)
C10—Cr2—C6	90.14 (3)	H1H—C14—C13	108.5 (6)
C10—Cr2—C7	93.62 (3)	H1H—C14—H1G	109.6 (9)
C10—Cr2—C8	86.65 (3)	C16—C15—O12	108.79 (5)
C10—Cr2—C9	95.17 (3)	H1I—C15—O12	109.1 (6)
H—Cr2—C6	81.7 (4)	H1I—C15—C16	108.2 (6)
H—Cr2—C7	84.9 (4)	H1J—C15—O12	110.0 (6)
H—Cr2—C8	101.5 (4)	H1J—C15—C16	115.3 (6)
H—Cr2—C9	86.2 (4)	H1J—C15—H1I	105.2 (9)
H—Cr2—C10	171.7 (4)	C15—C16—N2	114.05 (5)
O11—K1—O1	71.956 (16)	H1K—C16—N2	105.6 (6)
O12—K1—O1	65.088 (16)	H1K—C16—C15	108.8 (6)
O12—K1—O11	58.927 (14)	H1L—C16—N2	110.4 (6)
O13—K1—O1	64.150 (15)	H1L—C16—C15	108.9 (6)
O13—K1—O11	104.449 (15)	H1L—C16—H1K	108.9 (9)
O13—K1—O12	129.238 (16)	C18—C17—N1	113.88 (6)
O14—K1—O1	74.479 (17)	H1M—C17—N1	107.6 (6)
O14—K1—O11	146.385 (16)	H1M—C17—C18	106.1 (6)
O14—K1—O12	104.635 (15)	H1N—C17—N1	111.7 (6)
O14—K1—O13	61.237 (15)	H1N—C17—C18	108.8 (6)
O15—K1—O1	147.827 (16)	H1N—C17—H1M	108.4 (9)
O15—K1—O11	99.519 (15)	C17—C18—O13	109.22 (5)
O15—K1—O12	137.665 (16)	H1O—C18—O13	109.2 (6)
O15—K1—O13	89.431 (15)	H1O—C18—C17	110.4 (6)
O15—K1—O14	109.926 (16)	H1P—C18—O13	109.7 (6)
O16—K1—O1	152.181 (16)	H1P—C18—C17	112.4 (6)
O16—K1—O11	119.255 (15)	H1P—C18—H1O	105.8 (9)
O16—K1—O12	97.635 (15)	C20—C19—O13	108.89 (5)
O16—K1—O13	128.504 (16)	H1Q—C19—O13	109.5 (6)
O16—K1—O14	90.370 (16)	H1Q—C19—C20	110.5 (6)
O16—K1—O15	59.191 (15)	H1R—C19—O13	110.6 (6)
N1—K1—O1	90.411 (16)	H1R—C19—C20	108.8 (6)
N1—K1—O11	62.050 (15)	H1R—C19—H1Q	108.5 (9)
N1—K1—O12	120.453 (16)	C19—C20—O14	110.03 (6)
N1—K1—O13	60.336 (15)	H2A—C20—O14	110.7 (6)
N1—K1—O14	120.391 (15)	H2A—C20—C19	108.3 (6)
N1—K1—O15	59.301 (16)	H2B—C20—O14	108.3 (6)
N1—K1—O16	117.406 (15)	H2B—C20—C19	110.5 (6)
N2—K1—O1	91.995 (16)	H2B—C20—H2A	109.2 (9)
N2—K1—O11	117.229 (15)	C22—C21—O14	109.35 (6)
N2—K1—O12	59.317 (15)	H2C—C21—O14	109.9 (6)
N2—K1—O13	122.292 (15)	H2C—C21—C22	110.1 (6)
N2—K1—O14	61.926 (15)	H2D—C21—O14	110.5 (6)
N2—K1—O15	118.645 (16)	H2D—C21—C22	112.4 (6)
N2—K1—O16	60.190 (15)	H2D—C21—H2C	104.5 (9)
N2—K1—N1	177.086 (16)	C21—C22—N2	113.20 (6)
C1—O1—K1	148.79 (5)	H2E—C22—N2	109.8 (6)
C12—O11—K1	111.62 (4)	H2E—C22—C21	108.7 (6)
C13—O11—K1	113.87 (4)	H2F—C22—N2	109.7 (6)
C13—O11—C12	110.28 (5)	H2F—C22—C21	105.3 (6)
C14—O12—K1	117.64 (4)	H2F—C22—H2E	110.1 (9)
C15—O12—K1	121.00 (4)	C24—C23—N1	113.42 (5)
C15—O12—C14	111.79 (5)	H2G—C23—N1	110.9 (6)
C18—O13—K1	121.01 (4)	H2G—C23—C24	105.0 (6)
C19—O13—K1	113.63 (4)	H2H—C23—N1	113.0 (6)
C19—O13—C18	111.96 (5)	H2H—C23—C24	109.8 (6)
C20—O14—K1	113.66 (4)	H2H—C23—H2G	104.1 (9)
C21—O14—K1	112.04 (4)	C23—C24—O15	108.65 (6)
C21—O14—C20	110.72 (5)	H2I—C24—O15	110.1 (6)
C24—O15—K1	115.73 (4)	H2I—C24—C23	111.9 (6)
C25—O15—K1	117.02 (4)	H2J—C24—O15	107.8 (6)
C25—O15—C24	111.30 (5)	H2J—C24—C23	111.0 (6)
C26—O16—K1	112.69 (4)	H2J—C24—H2I	107.4 (9)
C27—O16—K1	120.08 (4)	C26—C25—O15	109.31 (5)
C27—O16—C26	110.63 (5)	H2K—C25—O15	111.1 (6)
C11—N1—K1	107.31 (4)	H2K—C25—C26	109.8 (6)
C17—N1—K1	107.27 (4)	H2L—C25—O15	110.8 (6)
C17—N1—C11	110.15 (6)	H2L—C25—C26	110.4 (6)
C23—N1—K1	112.20 (4)	H2L—C25—H2K	105.4 (9)
C23—N1—C11	109.26 (5)	C25—C26—O16	109.53 (5)
C23—N1—C17	110.59 (5)	H2M—C26—O16	110.4 (6)
C16—N2—K1	109.81 (4)	H2M—C26—C25	111.3 (6)
C22—N2—K1	107.60 (4)	H2N—C26—O16	111.1 (6)
C22—N2—C16	109.43 (5)	H2N—C26—C25	108.0 (6)
C28—N2—K1	108.74 (4)	H2N—C26—H2M	106.5 (9)
C28—N2—C16	109.90 (5)	C28—C27—O16	110.55 (6)
C28—N2—C22	111.31 (5)	H2O—C27—O16	108.3 (6)
O1—C1—Cr1	177.05 (6)	H2O—C27—C28	112.9 (6)
O2—C2—Cr1	178.79 (6)	H2P—C27—O16	107.2 (6)
O3—C3—Cr1	176.04 (6)	H2P—C27—C28	108.4 (6)
O4—C4—Cr1	177.85 (6)	H2P—C27—H2O	109.3 (9)
O5—C5—Cr1	177.68 (7)	C27—C28—N2	114.08 (5)
O6—C6—Cr2	178.73 (6)	H2Q—C28—N2	112.2 (6)
O7—C7—Cr2	178.59 (6)	H2Q—C28—C27	108.1 (6)
O8—C8—Cr2	174.70 (6)	H2R—C28—N2	107.7 (6)
O9—C9—Cr2	178.63 (7)	H2R—C28—C27	107.9 (6)
O10—C10—Cr2	177.98 (7)	H2R—C28—H2Q	106.5 (9)
C12—C11—N1	114.59 (5)	Cr2—H—Cr1	147.6 (8)

(KCPTCR_HAR)

Crystal data

C28H37Cr2KN2O16	F(000) = 1660.306
Mr = 800.70	Dx = 1.489 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71069 Å
a = 10.458 Å	Cell parameters from 1024 reflections
b = 14.417 Å	θ = 47.5–1.5°
c = 23.882 Å	µ = 0.80 mm^−1
β = 97.26°	T = 28 K
V = 3571.89 Å^3	Ellipsoidal, yellow
Z = 4	0.3 × 0.25 × 0.2 mm

Data collection

SMART CCD diffractometer	22531 reflections with I ≥ 2u(I)
ω scan	Rint = 0.0000
Absorption correction: empirical (using intensity measurements)	θmax = 48.7°, θmin = 2.4°
Tmin = 0.890, Tmax = 0.903	h = −19→20
27917 measured reflections	k = 0→30
27917 independent reflections	l = 0→50

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.030	All H-atom parameters refined
wR(F^2) = 0.057	w = 1/[σ^2(Fo^2) + (0.0214P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 0.99	(Δ/σ)max = 0.0002
27917 reflections	Δρmax = 0.70 e Å^−3
750 parameters	Δρmin = −0.63 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Cr1	0.163872 (8)	0.002350 (5)	0.236369 (3)	0.005184 (13)
Cr2	0.018765 (8)	0.177460 (5)	0.165108 (3)	0.005744 (13)
K1	0.463721 (11)	0.199293 (7)	0.418002 (4)	0.006508 (16)
O1	0.25206 (4)	0.13807 (3)	0.331203 (18)	0.01180 (7)
O2	−0.08348 (4)	−0.04363 (3)	0.285743 (19)	0.01419 (8)
O3	0.10472 (5)	−0.12656 (3)	0.135491 (18)	0.01260 (7)
O4	0.39546 (4)	0.05450 (3)	0.177511 (19)	0.01362 (7)
O5	0.30035 (4)	−0.15031 (3)	0.305771 (19)	0.01228 (7)
O6	−0.25957 (4)	0.12166 (3)	0.172260 (18)	0.01239 (7)
O7	0.01688 (4)	0.05855 (3)	0.059592 (17)	0.01254 (7)
O8	0.28629 (4)	0.25364 (3)	0.155254 (19)	0.01331 (7)
O9	0.02672 (5)	0.26560 (3)	0.281716 (19)	0.01772 (9)
O10	−0.07203 (5)	0.34762 (3)	0.099218 (19)	0.01463 (8)
O11	0.28569 (4)	0.09214 (2)	0.473111 (17)	0.00779 (6)
O12	0.44350 (4)	0.00267 (2)	0.402458 (17)	0.00831 (6)
O13	0.31323 (4)	0.34097 (2)	0.362952 (17)	0.00878 (6)
O14	0.52819 (4)	0.26681 (3)	0.315264 (16)	0.00891 (6)
O15	0.55093 (4)	0.32679 (3)	0.507659 (16)	0.00931 (6)
O16	0.72729 (4)	0.20517 (3)	0.464988 (17)	0.00817 (6)
N1	0.27302 (5)	0.30198 (3)	0.479836 (19)	0.00787 (7)
N2	0.66191 (4)	0.09454 (3)	0.361945 (18)	0.00690 (6)
C1	0.21628 (5)	0.08859 (3)	0.29507 (2)	0.00805 (7)
C2	0.01000 (6)	−0.02688 (3)	0.26771 (2)	0.00879 (8)
C3	0.12291 (5)	−0.07921 (3)	0.17415 (2)	0.00838 (8)
C4	0.30807 (6)	0.03664 (3)	0.20004 (2)	0.00894 (8)
C5	0.25026 (5)	−0.09120 (3)	0.27865 (2)	0.00835 (8)
C6	−0.15457 (6)	0.14176 (3)	0.16994 (2)	0.00867 (8)
C7	0.01880 (5)	0.10403 (3)	0.09912 (2)	0.00824 (8)
C8	0.18824 (6)	0.22113 (3)	0.16011 (2)	0.00906 (8)
C9	0.02390 (6)	0.23372 (4)	0.23780 (2)	0.01096 (9)
C10	−0.03870 (6)	0.28242 (3)	0.12528 (2)	0.00935 (8)
C11	0.20813 (6)	0.23292 (3)	0.51162 (2)	0.00902 (8)
C12	0.17304 (5)	0.14347 (3)	0.47989 (2)	0.00856 (8)
C13	0.25207 (5)	0.00545 (3)	0.44644 (2)	0.00783 (7)
C14	0.37232 (5)	−0.04780 (3)	0.43910 (2)	0.00816 (8)
C15	0.54817 (5)	−0.04995 (3)	0.38671 (2)	0.00794 (7)
C16	0.60987 (5)	0.00367 (3)	0.34254 (2)	0.00806 (7)
C17	0.17926 (6)	0.34658 (4)	0.43698 (2)	0.00935 (8)
C18	0.24062 (6)	0.40163 (3)	0.39329 (2)	0.00973 (8)
C19	0.37488 (6)	0.38877 (4)	0.32181 (2)	0.01088 (9)
C20	0.42820 (6)	0.31883 (4)	0.28402 (2)	0.01074 (8)
C21	0.57214 (6)	0.19485 (3)	0.28133 (2)	0.00943 (8)
C22	0.69036 (6)	0.14950 (4)	0.31299 (2)	0.00911 (8)
C23	0.33597 (6)	0.37155 (4)	0.51922 (2)	0.01011 (8)
C24	0.46534 (6)	0.34035 (4)	0.54885 (2)	0.01029 (8)
C25	0.68006 (5)	0.31750 (3)	0.53316 (2)	0.00872 (8)
C26	0.76440 (6)	0.29312 (3)	0.48871 (2)	0.00910 (8)
C27	0.82391 (6)	0.16971 (4)	0.43398 (2)	0.00901 (8)
C28	0.77747 (5)	0.08193 (3)	0.40289 (2)	0.00835 (8)
H	0.0483 (11)	0.0741 (8)	0.2000 (5)	0.039 (3)
H1A	0.1185 (10)	0.2622 (7)	0.5253 (4)	0.022 (3)
H1B	0.2726 (10)	0.2158 (7)	0.5495 (4)	0.023 (3)
H1C	0.1176 (10)	0.1573 (7)	0.4377 (4)	0.021 (2)
H1D	0.1092 (9)	0.1026 (7)	0.5037 (4)	0.022 (2)
H1E	0.1929 (10)	0.0162 (7)	0.4054 (4)	0.020 (2)
H1F	0.1934 (10)	−0.0364 (7)	0.4719 (4)	0.022 (2)
H1G	0.3439 (9)	−0.1155 (6)	0.4208 (4)	0.019 (2)
H1H	0.4286 (8)	−0.0588 (7)	0.4805 (4)	0.015 (2)
H1I	0.5130 (9)	−0.1161 (7)	0.3677 (4)	0.023 (3)
H1J	0.6157 (9)	−0.0683 (7)	0.4244 (4)	0.021 (2)
H1K	0.5386 (10)	0.0168 (7)	0.3065 (4)	0.024 (3)*
H1L	0.6861 (10)	−0.0394 (7)	0.3279 (4)	0.024 (3)
H1M	0.1231 (10)	0.2921 (7)	0.4139 (4)	0.023 (2)*
H1N	0.1134 (10)	0.3921 (7)	0.4563 (4)	0.022 (2)
H1O	0.1641 (10)	0.4348 (8)	0.3634 (5)	0.028 (3)
H1P	0.3029 (10)	0.4573 (7)	0.4131 (4)	0.024 (2)*
H1Q	0.4495 (10)	0.4326 (7)	0.3425 (4)	0.026 (3)
H1R	0.3072 (10)	0.4334 (8)	0.2959 (5)	0.036 (3)
H2A	0.3498 (10)	0.2744 (8)	0.2662 (4)	0.030 (3)
H2B	0.4654 (11)	0.3541 (8)	0.2495 (4)	0.033 (3)
H2C	0.5963 (10)	0.2246 (7)	0.2416 (4)	0.021 (2)
H2D	0.4958 (10)	0.1455 (6)	0.2698 (5)	0.027 (3)
H2E	0.7366 (10)	0.1055 (7)	0.2831 (4)	0.024 (3)
H2F	0.7575 (10)	0.2052 (7)	0.3269 (4)	0.020 (2)
H2G	0.3535 (9)	0.4328 (7)	0.4957 (5)	0.025 (3)
H2H	0.2732 (9)	0.3934 (7)	0.5511 (4)	0.026 (3)
H2I	0.4570 (10)	0.2752 (7)	0.5742 (4)	0.023 (3)
H2J	0.5048 (10)	0.3929 (8)	0.5795 (4)	0.032 (3)
H2K	0.7160 (9)	0.3821 (7)	0.5542 (4)	0.020 (2)*
H2L	0.6886 (10)	0.2625 (7)	0.5663 (4)	0.020 (2)*
H2M	0.7582 (10)	0.3472 (7)	0.4554 (4)	0.025 (3)
H2N	0.8638 (10)	0.2909 (7)	0.5091 (5)	0.028 (3)
H2O	0.8492 (10)	0.2226 (6)	0.4053 (4)	0.025 (3)
H2P	0.9103 (9)	0.1521 (7)	0.4646 (4)	0.021 (2)
H2Q	0.8586 (9)	0.0548 (7)	0.3827 (4)	0.021 (2)
H2R	0.7535 (10)	0.0314 (6)	0.4329 (4)	0.021 (2)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cr1	0.00561 (3)	0.00458 (2)	0.00533 (3)	0.00019 (2)	0.00058 (2)	−0.00015 (2)
Cr2	0.00669 (3)	0.00528 (2)	0.00512 (3)	0.00087 (2)	0.00018 (2)	0.00016 (2)
K1	0.00615 (4)	0.00669 (3)	0.00663 (4)	0.00020 (3)	0.00057 (3)	−0.00004 (3)
O1	0.0154 (2)	0.00914 (13)	0.00987 (17)	−0.00014 (13)	−0.00231 (13)	−0.00267 (12)
O2	0.0104 (2)	0.01668 (17)	0.01673 (19)	−0.00005 (15)	0.00652 (15)	0.00154 (14)
O3	0.0153 (2)	0.01240 (15)	0.01009 (17)	−0.00237 (14)	0.00167 (14)	−0.00485 (12)
O4	0.0108 (2)	0.01386 (15)	0.0175 (2)	−0.00103 (14)	0.00681 (15)	−0.00012 (14)
O5	0.0135 (2)	0.00896 (13)	0.01365 (18)	0.00345 (13)	−0.00094 (14)	0.00252 (12)
O6	0.00979 (19)	0.01500 (15)	0.01287 (18)	−0.00107 (14)	0.00339 (13)	0.00018 (13)
O7	0.0168 (2)	0.01228 (15)	0.00882 (16)	−0.00157 (14)	0.00275 (14)	−0.00336 (12)
O8	0.0112 (2)	0.01589 (16)	0.01262 (18)	−0.00525 (14)	0.00066 (14)	0.00072 (13)
O9	0.0260 (3)	0.01717 (17)	0.00906 (18)	0.00959 (17)	−0.00127 (16)	−0.00491 (14)
O10	0.0178 (2)	0.00961 (14)	0.01542 (19)	0.00303 (14)	−0.00206 (15)	0.00440 (13)
O11	0.00641 (16)	0.00764 (12)	0.00928 (15)	−0.00023 (11)	0.00082 (11)	−0.00093 (10)
O12	0.00876 (17)	0.00665 (11)	0.00995 (15)	0.00072 (11)	0.00290 (12)	0.00109 (11)
O13	0.00958 (18)	0.00710 (12)	0.00991 (16)	0.00100 (12)	0.00218 (12)	0.00118 (11)
O14	0.01003 (18)	0.00895 (12)	0.00772 (15)	0.00159 (12)	0.00099 (12)	0.00056 (11)
O15	0.00764 (16)	0.01237 (14)	0.00773 (15)	0.00126 (13)	0.00023 (11)	−0.00173 (11)
O16	0.00600 (16)	0.00889 (12)	0.00965 (15)	−0.00094 (11)	0.00110 (11)	−0.00218 (11)
N1	0.00687 (18)	0.00813 (13)	0.00860 (17)	0.00120 (13)	0.00096 (13)	−0.00048 (12)
N2	0.00712 (18)	0.00691 (13)	0.00682 (16)	0.00013 (12)	0.00143 (12)	−0.00005 (11)
C1	0.0093 (2)	0.00694 (14)	0.00753 (19)	−0.00005 (14)	−0.00020 (14)	−0.00071 (13)
C2	0.0083 (2)	0.00903 (15)	0.0095 (2)	0.00053 (15)	0.00277 (15)	0.00068 (13)
C3	0.0090 (2)	0.00811 (15)	0.00798 (19)	−0.00052 (15)	0.00095 (15)	−0.00158 (13)
C4	0.0080 (2)	0.00889 (16)	0.0102 (2)	−0.00053 (15)	0.00241 (15)	−0.00046 (14)
C5	0.0086 (2)	0.00680 (15)	0.00946 (19)	0.00120 (14)	0.00030 (15)	0.00052 (13)
C6	0.0088 (2)	0.00949 (16)	0.00785 (19)	0.00073 (15)	0.00144 (15)	0.00041 (13)
C7	0.0094 (2)	0.00826 (15)	0.00710 (19)	−0.00039 (15)	0.00135 (14)	−0.00098 (13)
C8	0.0095 (2)	0.00908 (16)	0.00828 (19)	−0.00119 (15)	0.00015 (15)	0.00003 (13)
C9	0.0142 (2)	0.01024 (17)	0.0081 (2)	0.00388 (16)	−0.00014 (16)	−0.00179 (14)
C10	0.0112 (2)	0.00722 (15)	0.0092 (2)	0.00148 (15)	−0.00029 (15)	0.00131 (13)
C11	0.0095 (2)	0.00968 (16)	0.0082 (2)	0.00143 (15)	0.00219 (15)	−0.00019 (14)
C12	0.0065 (2)	0.00905 (16)	0.0102 (2)	−0.00011 (15)	0.00129 (15)	0.00014 (14)
C13	0.0073 (2)	0.00779 (15)	0.00855 (19)	−0.00153 (14)	0.00147 (14)	−0.00028 (13)
C14	0.0094 (2)	0.00681 (15)	0.00848 (19)	−0.00021 (15)	0.00201 (15)	0.00070 (13)
C15	0.0077 (2)	0.00648 (14)	0.0097 (2)	0.00061 (14)	0.00141 (15)	0.00043 (13)
C16	0.0090 (2)	0.00779 (15)	0.00744 (18)	−0.00022 (15)	0.00128 (14)	−0.00083 (13)
C17	0.0077 (2)	0.00998 (16)	0.0105 (2)	0.00196 (15)	0.00177 (15)	0.00134 (14)
C18	0.0101 (2)	0.00785 (15)	0.0117 (2)	0.00180 (16)	0.00282 (16)	0.00146 (14)
C19	0.0123 (2)	0.00815 (16)	0.0128 (2)	0.00215 (16)	0.00388 (17)	0.00296 (15)
C20	0.0120 (2)	0.01177 (17)	0.0086 (2)	0.00297 (17)	0.00198 (16)	0.00313 (15)
C21	0.0122 (2)	0.00896 (16)	0.00710 (19)	0.00161 (16)	0.00105 (15)	0.00066 (13)
C22	0.0094 (2)	0.00946 (16)	0.0090 (2)	0.00105 (16)	0.00320 (15)	0.00181 (14)
C23	0.0084 (2)	0.00985 (17)	0.0120 (2)	0.00145 (16)	0.00085 (16)	−0.00329 (15)
C24	0.0078 (2)	0.01391 (19)	0.0090 (2)	0.00048 (17)	0.00073 (15)	−0.00303 (15)
C25	0.0081 (2)	0.00954 (16)	0.00821 (19)	−0.00047 (15)	−0.00006 (14)	−0.00193 (14)
C26	0.0077 (2)	0.00903 (16)	0.0106 (2)	−0.00128 (15)	0.00126 (15)	−0.00196 (14)
C27	0.0071 (2)	0.00994 (17)	0.0101 (2)	−0.00079 (15)	0.00133 (15)	−0.00189 (14)
C28	0.0075 (2)	0.00835 (15)	0.0091 (2)	0.00073 (15)	0.00078 (15)	−0.00070 (13)
H	0.037 (8)	0.022 (7)	0.058 (9)	0.006 (6)	0.003 (7)	0.008 (7)
H1A	0.017 (6)	0.026 (6)	0.027 (6)	0.002 (5)	0.017 (5)	−0.007 (5)
H1B	0.026 (7)	0.023 (6)	0.019 (6)	−0.003 (5)	−0.005 (5)	−0.002 (5)
H1C	0.020 (6)	0.026 (6)	0.016 (6)	0.002 (5)	−0.002 (5)	−0.001 (5)
H1D	0.024 (6)	0.014 (5)	0.029 (6)	0.006 (5)	0.008 (5)	0.003 (5)
H1E	0.019 (6)	0.025 (6)	0.013 (5)	0.010 (5)	−0.004 (4)	−0.003 (5)
H1F	0.025 (6)	0.024 (6)	0.018 (6)	−0.009 (5)	0.004 (5)	−0.004 (5)
H1G	0.024 (6)	0.005 (5)	0.029 (6)	−0.007 (4)	0.013 (5)	−0.004 (4)
H1H	0.011 (5)	0.022 (6)	0.013 (5)	0.002 (4)	0.007 (4)	0.006 (4)
H1I	0.015 (6)	0.031 (6)	0.024 (6)	−0.005 (5)	0.000 (5)	−0.003 (5)
H1J	0.015 (6)	0.029 (6)	0.020 (6)	−0.009 (5)	0.001 (5)	0.006 (5)
H1L	0.025 (6)	0.022 (6)	0.025 (6)	0.004 (5)	0.006 (5)	−0.005 (5)
H1N	0.023 (6)	0.027 (6)	0.018 (6)	0.004 (5)	0.010 (5)	0.012 (5)
H1O	0.019 (6)	0.033 (7)	0.035 (7)	0.001 (5)	0.010 (5)	0.015 (6)
H1Q	0.021 (6)	0.017 (6)	0.040 (7)	−0.011 (5)	0.005 (5)	−0.004 (5)
H1R	0.028 (7)	0.039 (7)	0.043 (8)	0.016 (6)	0.014 (6)	0.031 (6)
H2A	0.027 (7)	0.033 (7)	0.025 (7)	−0.001 (5)	−0.018 (5)	0.006 (5)
H2B	0.043 (8)	0.040 (7)	0.017 (6)	0.005 (6)	0.006 (5)	0.015 (5)
H2C	0.028 (7)	0.024 (6)	0.013 (5)	0.007 (5)	0.008 (5)	0.011 (5)
H2D	0.026 (7)	0.012 (5)	0.048 (7)	−0.003 (5)	0.019 (5)	−0.007 (5)
H2E	0.027 (7)	0.025 (6)	0.022 (6)	0.000 (5)	0.012 (5)	−0.006 (5)
H2F	0.024 (6)	0.020 (6)	0.016 (6)	−0.001 (5)	0.000 (5)	−0.003 (5)
H2G	0.014 (6)	0.020 (6)	0.040 (7)	0.003 (5)	0.003 (5)	0.007 (5)
H2H	0.014 (6)	0.035 (7)	0.029 (7)	−0.007 (5)	0.012 (5)	−0.014 (5)
H2I	0.026 (7)	0.022 (6)	0.021 (6)	0.001 (5)	0.004 (5)	0.005 (5)
H2J	0.032 (7)	0.053 (8)	0.011 (6)	0.003 (6)	0.003 (5)	−0.017 (6)
H2M	0.018 (6)	0.027 (6)	0.031 (7)	0.009 (5)	0.012 (5)	0.001 (5)
H2N	0.025 (7)	0.025 (6)	0.036 (7)	−0.004 (5)	0.003 (5)	−0.014 (5)
H2O	0.038 (7)	0.006 (5)	0.028 (6)	0.005 (5)	−0.007 (5)	−0.003 (4)
H2P	0.014 (6)	0.021 (6)	0.026 (6)	−0.001 (5)	−0.003 (5)	−0.009 (5)
H2Q	0.017 (6)	0.019 (6)	0.027 (6)	0.007 (5)	0.002 (5)	−0.010 (5)
H2R	0.034 (7)	0.010 (5)	0.018 (6)	−0.001 (5)	0.000 (5)	0.008 (4)

Geometric parameters (Å, º)

Cr1—C1	1.9019 (5)	N2—C22	1.4735 (6)
Cr1—C2	1.9056 (6)	N2—C28	1.4667 (7)
Cr1—C3	1.9009 (5)	C11—C12	1.5172 (7)
Cr1—C4	1.8980 (6)	C11—H1A	1.113 (9)
Cr1—C5	1.8505 (5)	C11—H1B	1.086 (10)
Cr1—H	1.738 (11)	C12—H1C	1.115 (10)
Cr2—C6	1.9018 (6)	C12—H1D	1.100 (10)
Cr2—C7	1.8985 (5)	C13—C14	1.5025 (8)
Cr2—C8	1.8988 (6)	C13—H1E	1.102 (9)
Cr2—C9	1.9108 (5)	C13—H1F	1.097 (10)
Cr2—C10	1.8469 (5)	C14—H1G	1.095 (9)
Cr2—H	1.716 (11)	C14—H1H	1.096 (9)
K1—O1	2.9692 (4)	C15—C16	1.5162 (7)
K1—O11	2.8643 (4)	C15—H1I	1.100 (10)
K1—O12	2.8632 (4)	C15—H1J	1.104 (10)
K1—O13	2.8026 (4)	C16—H1K	1.081 (10)
K1—O14	2.8000 (4)	C16—H1L	1.102 (10)
K1—O15	2.8812 (4)	C17—C18	1.5164 (7)
K1—O16	2.8430 (4)	C17—H1M	1.089 (10)
K1—N1	3.0156 (5)	C17—H1N	1.095 (10)
K1—N2	3.0117 (4)	C18—H1O	1.111 (10)
O1—C1	1.1455 (6)	C18—H1P	1.101 (10)
O2—C2	1.1429 (7)	C19—C20	1.5064 (8)
O3—C3	1.1446 (6)	C19—H1Q	1.075 (9)
O4—C4	1.1468 (7)	C19—H1R	1.089 (10)
O5—C5	1.1551 (6)	C20—H2A	1.084 (10)
O6—C6	1.1438 (7)	C20—H2B	1.081 (10)
O7—C7	1.1475 (6)	C21—C22	1.5138 (8)
O8—C8	1.1466 (7)	C21—H2C	1.099 (9)
O9—C9	1.1420 (7)	C21—H2D	1.079 (10)
O10—C10	1.1567 (6)	C22—H2E	1.111 (10)
O11—C12	1.4177 (7)	C22—H2F	1.090 (10)
O11—C13	1.4263 (6)	C23—C24	1.5138 (8)
O12—C14	1.4192 (6)	C23—H2G	1.074 (10)
O12—C15	1.4211 (6)	C23—H2H	1.113 (10)
O13—C18	1.4162 (6)	C24—H2I	1.126 (10)
O13—C19	1.4198 (6)	C24—H2J	1.097 (10)
O14—C20	1.4197 (7)	C25—C26	1.5050 (8)
O14—C21	1.4278 (6)	C25—H2K	1.101 (10)
O15—C24	1.4247 (7)	C25—H2L	1.116 (10)
O15—C25	1.4159 (7)	C26—H2M	1.111 (10)
O16—C26	1.4225 (6)	C26—H2N	1.091 (11)
O16—C27	1.4211 (7)	C27—C28	1.5158 (7)
N1—C11	1.4691 (7)	C27—H2O	1.080 (10)
N1—C17	1.4727 (7)	C27—H2P	1.117 (10)
N1—C23	1.4723 (7)	C28—H2Q	1.100 (9)
N2—C16	1.4709 (6)	C28—H2R	1.074 (9)
C2—Cr1—C1	91.95 (2)	H1A—C11—N1	110.8 (5)
C3—Cr1—C1	174.91 (2)	H1A—C11—C12	108.0 (5)
C3—Cr1—C2	92.99 (2)	H1B—C11—N1	107.8 (5)
C4—Cr1—C1	89.72 (2)	H1B—C11—C12	107.9 (5)
C4—Cr1—C2	175.08 (2)	H1B—C11—H1A	107.4 (8)
C4—Cr1—C3	85.26 (2)	C11—C12—O11	110.41 (4)
C5—Cr1—C1	89.94 (2)	H1C—C12—O11	109.6 (5)
C5—Cr1—C2	90.16 (2)	H1C—C12—C11	111.4 (5)
C5—Cr1—C3	91.26 (2)	H1D—C12—O11	110.3 (5)
C5—Cr1—C4	94.47 (2)	H1D—C12—C11	108.8 (5)
H—Cr1—C1	95.6 (4)	H1D—C12—H1C	106.4 (7)
H—Cr1—C2	76.1 (4)	C14—C13—O11	109.70 (4)
H—Cr1—C3	84.5 (4)	H1E—C13—O11	110.7 (5)
H—Cr1—C4	99.1 (4)	H1E—C13—C14	110.6 (5)
H—Cr1—C5	165.3 (4)	H1F—C13—O11	111.0 (5)
C7—Cr2—C6	89.98 (2)	H1F—C13—C14	108.5 (5)
C8—Cr2—C6	176.33 (2)	H1F—C13—H1E	106.3 (8)
C8—Cr2—C7	91.99 (2)	C13—C14—O12	108.78 (4)
C9—Cr2—C6	88.70 (2)	H1G—C14—O12	110.4 (5)
C9—Cr2—C7	171.10 (2)	H1G—C14—C13	108.2 (5)
C9—Cr2—C8	89.83 (2)	H1H—C14—O12	111.5 (5)
C10—Cr2—C6	90.13 (2)	H1H—C14—C13	109.3 (5)
C10—Cr2—C7	93.64 (2)	H1H—C14—H1G	108.6 (7)
C10—Cr2—C8	86.65 (2)	C16—C15—O12	108.77 (4)
C10—Cr2—C9	95.16 (2)	H1I—C15—O12	110.1 (5)
H—Cr2—C6	81.4 (4)	H1I—C15—C16	107.7 (5)
H—Cr2—C7	84.3 (4)	H1J—C15—O12	110.3 (5)
H—Cr2—C8	101.9 (4)	H1J—C15—C16	113.9 (5)
H—Cr2—C9	86.8 (4)	H1J—C15—H1I	106.0 (7)
H—Cr2—C10	171.2 (4)	C15—C16—N2	114.07 (4)
O11—K1—O1	71.938 (12)	H1K—C16—N2	106.6 (5)
O12—K1—O1	65.093 (12)	H1K—C16—C15	109.3 (6)
O12—K1—O11	58.933 (11)	H1L—C16—N2	110.4 (5)
O13—K1—O1	64.167 (11)	H1L—C16—C15	108.8 (5)
O13—K1—O11	104.451 (12)	H1L—C16—H1K	107.4 (8)
O13—K1—O12	129.260 (12)	C18—C17—N1	113.84 (5)
O14—K1—O1	74.477 (12)	H1M—C17—N1	107.8 (5)
O14—K1—O11	146.366 (12)	H1M—C17—C18	106.1 (5)
O14—K1—O12	104.631 (11)	H1N—C17—N1	111.6 (5)
O14—K1—O13	61.229 (11)	H1N—C17—C18	108.7 (5)
O15—K1—O1	147.833 (12)	H1N—C17—H1M	108.6 (8)
O15—K1—O11	99.537 (11)	C17—C18—O13	109.26 (4)
O15—K1—O12	137.664 (12)	H1O—C18—O13	109.0 (6)
O15—K1—O13	89.421 (12)	H1O—C18—C17	109.5 (5)
O15—K1—O14	109.924 (12)	H1P—C18—O13	110.1 (5)
O16—K1—O1	152.191 (12)	H1P—C18—C17	111.4 (5)
O16—K1—O11	119.263 (12)	H1P—C18—H1O	107.5 (8)
O16—K1—O12	97.628 (12)	C20—C19—O13	108.94 (4)
O16—K1—O13	128.491 (12)	H1Q—C19—O13	109.5 (6)
O16—K1—O14	90.383 (12)	H1Q—C19—C20	111.5 (6)
O16—K1—O15	59.176 (11)	H1R—C19—O13	111.1 (5)
N1—K1—O1	90.401 (12)	H1R—C19—C20	108.5 (6)
N1—K1—O11	62.048 (11)	H1R—C19—H1Q	107.2 (8)
N1—K1—O12	120.459 (12)	C19—C20—O14	110.03 (5)
N1—K1—O13	60.331 (12)	H2A—C20—O14	111.4 (6)
N1—K1—O14	120.385 (12)	H2A—C20—C19	108.2 (6)
N1—K1—O15	59.317 (12)	H2B—C20—O14	109.7 (6)
N1—K1—O16	117.406 (12)	H2B—C20—C19	109.7 (6)
N2—K1—O1	91.996 (12)	H2B—C20—H2A	107.7 (8)
N2—K1—O11	117.233 (11)	C22—C21—O14	109.36 (4)
N2—K1—O12	59.312 (11)	H2C—C21—O14	109.4 (5)
N2—K1—O13	122.286 (12)	H2C—C21—C22	109.7 (5)
N2—K1—O14	61.924 (11)	H2D—C21—O14	110.1 (5)
N2—K1—O15	118.637 (12)	H2D—C21—C22	111.9 (6)
N2—K1—O16	60.199 (11)	H2D—C21—H2C	106.3 (8)
N2—K1—N1	177.097 (13)	C21—C22—N2	113.23 (5)
C1—O1—K1	148.74 (4)	H2E—C22—N2	110.6 (5)
C12—O11—K1	111.64 (3)	H2E—C22—C21	108.7 (6)
C13—O11—K1	113.91 (3)	H2F—C22—N2	109.9 (5)
C13—O11—C12	110.29 (4)	H2F—C22—C21	106.7 (5)
C14—O12—K1	117.62 (3)	H2F—C22—H2E	107.5 (8)
C15—O12—K1	121.07 (3)	C24—C23—N1	113.41 (4)
C15—O12—C14	111.78 (4)	H2G—C23—N1	108.6 (6)
C18—O13—K1	121.04 (3)	H2G—C23—C24	106.7 (5)
C19—O13—K1	113.65 (3)	H2H—C23—N1	112.1 (5)
C19—O13—C18	111.97 (4)	H2H—C23—C24	109.5 (6)
C20—O14—K1	113.66 (3)	H2H—C23—H2G	106.2 (8)
C21—O14—K1	112.04 (3)	C23—C24—O15	108.68 (4)
C21—O14—C20	110.74 (4)	H2I—C24—O15	110.8 (5)
C24—O15—K1	115.67 (3)	H2I—C24—C23	111.9 (5)
C25—O15—K1	117.03 (3)	H2J—C24—O15	109.8 (5)
C25—O15—C24	111.37 (4)	H2J—C24—C23	110.2 (6)
C26—O16—K1	112.70 (3)	H2J—C24—H2I	105.4 (8)
C27—O16—K1	120.09 (3)	C26—C25—O15	109.32 (4)
C27—O16—C26	110.61 (4)	H2K—C25—O15	111.6 (5)
C11—N1—K1	107.31 (3)	H2K—C25—C26	108.8 (5)
C17—N1—K1	107.31 (3)	H2L—C25—O15	111.0 (5)
C17—N1—C11	110.15 (4)	H2L—C25—C26	109.5 (5)
C23—N1—K1	112.17 (3)	H2L—C25—H2K	106.5 (7)
C23—N1—C11	109.27 (4)	C25—C26—O16	109.53 (4)
C23—N1—C17	110.56 (4)	H2M—C26—O16	110.6 (6)
C16—N2—K1	109.80 (3)	H2M—C26—C25	110.8 (5)
C22—N2—K1	107.60 (3)	H2N—C26—O16	110.4 (5)
C22—N2—C16	109.43 (4)	H2N—C26—C25	107.6 (6)
C28—N2—K1	108.74 (3)	H2N—C26—H2M	107.8 (8)
C28—N2—C16	109.91 (4)	C28—C27—O16	110.53 (4)
C28—N2—C22	111.32 (4)	H2O—C27—O16	108.9 (5)
O1—C1—Cr1	177.11 (5)	H2O—C27—C28	111.6 (5)
O2—C2—Cr1	178.82 (5)	H2P—C27—O16	108.0 (5)
O3—C3—Cr1	175.95 (5)	H2P—C27—C28	108.3 (5)
O4—C4—Cr1	177.82 (4)	H2P—C27—H2O	109.4 (8)
O5—C5—Cr1	177.68 (5)	C27—C28—N2	114.15 (4)
O6—C6—Cr2	178.76 (5)	H2Q—C28—N2	111.6 (5)
O7—C7—Cr2	178.60 (5)	H2Q—C28—C27	107.1 (5)
O8—C8—Cr2	174.70 (5)	H2R—C28—N2	106.7 (5)
O9—C9—Cr2	178.60 (5)	H2R—C28—C27	109.0 (5)
O10—C10—Cr2	177.93 (5)	H2R—C28—H2Q	108.1 (8)
C12—C11—N1	114.60 (4)	Cr2—H—Cr1	146.2 (7)
K1—O11—C12—C11	−55.95 (3)	K1—N1—C23—C24	−37.52 (3)
K1—O11—C13—C14	53.09 (3)	K1—N2—C16—C15	−48.51 (3)
K1—O12—C14—C13	42.24 (3)	K1—N2—C22—C21	−39.24 (3)
K1—O12—C15—C16	−41.05 (3)	K1—N2—C28—C27	−48.56 (3)
K1—O13—C18—C17	−40.73 (3)	O11—C12—C11—N1	69.73 (5)
K1—O13—C19—C20	49.26 (3)	O11—C13—C14—O12	−63.24 (4)
K1—O14—C20—C19	47.79 (3)	O12—C15—C16—N2	60.67 (5)
K1—O14—C21—C22	−59.77 (3)	O13—C18—C17—N1	62.37 (5)
K1—O15—C24—C23	−56.04 (3)	O13—C19—C20—O14	−65.92 (5)
K1—O15—C25—C26	37.73 (3)	O14—C21—C22—N2	69.60 (4)
K1—O16—C26—C25	57.35 (3)	O15—C24—C23—N1	63.15 (5)
K1—O16—C27—C28	−39.11 (3)	O15—C25—C26—O16	−63.63 (4)
K1—N1—C11—C12	−41.25 (3)	O16—C27—C28—N2	60.49 (5)
K1—N1—C17—C18	−49.78 (3)

(KCPTCR_HAR_NoMoRe_1)

Crystal data

C28H37Cr2KN2O16	F(000) = 1660.306
Mr = 800.70	Dx = 1.489 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71069 Å
a = 10.458 Å	Cell parameters from 1024 reflections
b = 14.417 Å	θ = 47.5–1.5°
c = 23.882 Å	µ = 0.80 mm^−1
β = 97.26°	T = 28 K
V = 3571.89 Å^3	Ellipsoidal, yellow
Z = 4	0.3 × 0.25 × 0.2 mm

Data collection

SMART CCD diffractometer	22531 reflections with I ≥ 2u(I)
ω scan	Rint = 0.0000
Absorption correction: empirical (using intensity measurements)	θmax = 48.7°, θmin = 2.4°
Tmin = 0.890, Tmax = 0.903	h = −19→20
27917 measured reflections	k = 0→30
27917 independent reflections	l = 0→50

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.031	Only H-atom coordinates refined
wR(F^2) = 0.100	w = 1/[σ^2(Fo^2) + (0.1P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 0.69	(Δ/σ)max = 0.0001
27917 reflections	Δρmax = 0.73 e Å^−3
553 parameters	Δρmin = −1.27 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Cr1	0.163875 (10)	0.002347 (6)	0.236375 (4)	0.005245 (17)
Cr2	0.018764 (10)	0.177450 (6)	0.165109 (4)	0.005811 (18)
K1	0.463713 (13)	0.199294 (8)	0.418001 (5)	0.00657 (2)
O1	0.25208 (6)	0.13810 (3)	0.33122 (2)	0.01184 (8)
O2	−0.08355 (6)	−0.04362 (4)	0.28576 (3)	0.01424 (9)
O3	0.10469 (6)	−0.12659 (4)	0.13548 (2)	0.01260 (8)
O4	0.39549 (6)	0.05450 (4)	0.17751 (3)	0.01366 (9)
O5	0.30038 (6)	−0.15033 (4)	0.30580 (2)	0.01236 (8)
O6	−0.25958 (6)	0.12167 (4)	0.17223 (2)	0.01235 (8)
O7	0.01687 (6)	0.05854 (4)	0.05958 (2)	0.01265 (8)
O8	0.28635 (6)	0.25364 (4)	0.15524 (2)	0.01343 (9)
O9	0.02671 (7)	0.26561 (4)	0.28173 (3)	0.01788 (11)
O10	−0.07206 (6)	0.34766 (4)	0.09922 (3)	0.01458 (9)
O11	0.28570 (5)	0.09214 (3)	0.47314 (2)	0.00784 (7)
O12	0.44346 (5)	0.00267 (3)	0.40246 (2)	0.00837 (7)
O13	0.31318 (5)	0.34097 (3)	0.36294 (2)	0.00878 (7)
O14	0.52819 (5)	0.26678 (3)	0.31528 (2)	0.00893 (7)
O15	0.55089 (5)	0.32676 (4)	0.50766 (2)	0.00929 (7)
O16	0.72730 (5)	0.20515 (3)	0.46498 (2)	0.00825 (7)
N1	0.27305 (6)	0.30198 (4)	0.47984 (2)	0.00785 (7)
N2	0.66187 (5)	0.09454 (3)	0.36195 (2)	0.00696 (7)
C1	0.21620 (7)	0.08861 (4)	0.29509 (3)	0.00816 (8)
C2	0.01011 (7)	−0.02688 (4)	0.26769 (3)	0.00880 (9)
C3	0.12292 (7)	−0.07914 (4)	0.17414 (3)	0.00848 (8)
C4	0.30807 (7)	0.03663 (4)	0.20003 (3)	0.00900 (9)
C5	0.25021 (7)	−0.09118 (4)	0.27863 (3)	0.00847 (8)
C6	−0.15452 (7)	0.14180 (4)	0.16996 (3)	0.00873 (9)
C7	0.01879 (7)	0.10406 (4)	0.09913 (3)	0.00830 (8)
C8	0.18818 (7)	0.22110 (4)	0.16012 (3)	0.00901 (9)
C9	0.02397 (7)	0.23368 (4)	0.23776 (3)	0.01109 (10)
C10	−0.03870 (7)	0.28241 (4)	0.12526 (3)	0.00937 (9)
C11	0.20814 (7)	0.23292 (4)	0.51163 (3)	0.00904 (9)
C12	0.17312 (6)	0.14345 (4)	0.47988 (3)	0.00867 (9)
C13	0.25204 (7)	0.00543 (4)	0.44641 (3)	0.00786 (8)
C14	0.37237 (7)	−0.04780 (4)	0.43910 (3)	0.00820 (8)
C15	0.54819 (6)	−0.04991 (4)	0.38672 (3)	0.00804 (8)
C16	0.60989 (7)	0.00369 (4)	0.34255 (3)	0.00813 (8)
C17	0.17934 (7)	0.34655 (4)	0.43701 (3)	0.00930 (9)
C18	0.24065 (7)	0.40165 (4)	0.39330 (3)	0.00976 (9)
C19	0.37488 (7)	0.38881 (4)	0.32182 (3)	0.01091 (10)
C20	0.42815 (7)	0.31883 (5)	0.28403 (3)	0.01081 (10)
C21	0.57213 (7)	0.19482 (4)	0.28134 (3)	0.00947 (9)
C22	0.69036 (7)	0.14948 (4)	0.31299 (3)	0.00920 (9)
C23	0.33590 (7)	0.37152 (4)	0.51924 (3)	0.01014 (9)
C24	0.46543 (7)	0.34034 (5)	0.54889 (3)	0.01030 (9)
C25	0.68009 (7)	0.31747 (4)	0.53319 (3)	0.00879 (9)
C26	0.76441 (7)	0.29313 (4)	0.48874 (3)	0.00917 (9)
C27	0.82389 (7)	0.16973 (4)	0.43397 (3)	0.00908 (9)
C28	0.77753 (6)	0.08188 (4)	0.40292 (3)	0.00838 (8)
H	0.0489 (17)	0.0757 (13)	0.1996 (8)	0.033652
H1A	0.1189 (16)	0.2624 (11)	0.5257 (8)	0.025013
H1B	0.2731 (16)	0.2162 (12)	0.5496 (7)	0.023076
H1C	0.1182 (16)	0.1563 (12)	0.4377 (7)	0.023746
H1D	0.1086 (15)	0.1021 (12)	0.5035 (7)	0.024598
H1E	0.1938 (16)	0.0155 (12)	0.4053 (7)	0.022215
H1F	0.1927 (16)	−0.0360 (11)	0.4720 (7)	0.023329
H1G	0.3431 (16)	−0.1158 (11)	0.4209 (7)	0.025071
H1H	0.4290 (16)	−0.0575 (12)	0.4804 (6)	0.024233
H1I	0.5128 (16)	−0.1161 (11)	0.3676 (7)	0.022451
H1J	0.6148 (15)	−0.0686 (11)	0.4237 (6)	0.021710
H1K	0.5375 (16)	0.0168 (11)	0.3062 (7)	0.022322
H1L	0.6867 (16)	−0.0389 (11)	0.3285 (7)	0.023001
H1M	0.1249 (16)	0.2929 (11)	0.4142 (7)	0.024511
H1N	0.1146 (16)	0.3921 (12)	0.4564 (7)	0.026678
H1O	0.1635 (16)	0.4348 (12)	0.3630 (7)	0.027525
H1P	0.3024 (16)	0.4572 (11)	0.4130 (7)	0.026323
H1Q	0.4495 (17)	0.4327 (12)	0.3433 (7)	0.027823
H1R	0.3064 (16)	0.4328 (12)	0.2959 (7)	0.029725
H2A	0.3500 (16)	0.2734 (13)	0.2658 (7)	0.026016
H2B	0.4674 (17)	0.3546 (13)	0.2497 (7)	0.028356
H2C	0.5961 (17)	0.2245 (12)	0.2414 (7)	0.025505
H2D	0.4958 (16)	0.1455 (11)	0.2692 (7)	0.024538
H2E	0.7377 (17)	0.1058 (12)	0.2834 (7)	0.025760
H2F	0.7573 (16)	0.2064 (12)	0.3274 (7)	0.024185
H2G	0.3546 (16)	0.4328 (11)	0.4960 (7)	0.025234
H2H	0.2738 (16)	0.3935 (13)	0.5521 (7)	0.026839
H2I	0.4573 (17)	0.2747 (13)	0.5745 (7)	0.026520
H2J	0.5069 (16)	0.3937 (12)	0.5789 (7)	0.027507
H2K	0.7154 (16)	0.3810 (11)	0.5542 (7)	0.024028
H2L	0.6876 (16)	0.2637 (12)	0.5665 (7)	0.023835
H2M	0.7581 (18)	0.3474 (11)	0.4549 (7)	0.025301
H2N	0.8641 (15)	0.2908 (12)	0.5089 (7)	0.026087
H2O	0.8494 (16)	0.2232 (12)	0.4057 (7)	0.025953
H2P	0.9104 (16)	0.1519 (12)	0.4651 (8)	0.027682
H2Q	0.8593 (15)	0.0542 (12)	0.3825 (7)	0.024815
H2R	0.7534 (15)	0.0328 (11)	0.4334 (6)	0.022425

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cr1	0.00570 (4)	0.00465 (3)	0.00537 (3)	0.00020 (2)	0.00060 (2)	−0.00015 (2)
Cr2	0.00681 (4)	0.00534 (3)	0.00515 (3)	0.00087 (2)	0.00021 (2)	0.00017 (2)
K1	0.00627 (5)	0.00672 (4)	0.00667 (4)	0.00020 (3)	0.00060 (3)	−0.00005 (3)
O1	0.0156 (2)	0.00918 (15)	0.00979 (19)	−0.00010 (15)	−0.00223 (15)	−0.00278 (13)
O2	0.0106 (2)	0.0167 (2)	0.0167 (2)	−0.00016 (17)	0.00650 (17)	0.00149 (17)
O3	0.0153 (2)	0.01230 (17)	0.01023 (19)	−0.00204 (16)	0.00162 (16)	−0.00501 (14)
O4	0.0110 (2)	0.01397 (18)	0.0173 (2)	−0.00091 (17)	0.00693 (17)	0.00011 (16)
O5	0.0136 (2)	0.00923 (15)	0.0135 (2)	0.00351 (15)	−0.00096 (16)	0.00256 (14)
O6	0.0096 (2)	0.01501 (18)	0.0130 (2)	−0.00104 (16)	0.00346 (15)	0.00016 (15)
O7	0.0169 (2)	0.01230 (17)	0.00905 (19)	−0.00135 (17)	0.00292 (16)	−0.00336 (14)
O8	0.0111 (2)	0.01615 (19)	0.0129 (2)	−0.00546 (17)	0.00069 (16)	0.00072 (16)
O9	0.0265 (3)	0.0174 (2)	0.0089 (2)	0.0097 (2)	−0.00111 (19)	−0.00491 (16)
O10	0.0179 (3)	0.00951 (16)	0.0152 (2)	0.00299 (16)	−0.00220 (18)	0.00423 (15)
O11	0.00643 (18)	0.00771 (13)	0.00933 (17)	−0.00020 (13)	0.00085 (13)	−0.00098 (12)
O12	0.00898 (19)	0.00666 (13)	0.00988 (18)	0.00077 (13)	0.00284 (14)	0.00105 (12)
O13	0.0096 (2)	0.00715 (13)	0.00986 (18)	0.00085 (13)	0.00237 (14)	0.00118 (12)
O14	0.0101 (2)	0.00885 (14)	0.00775 (17)	0.00180 (14)	0.00085 (13)	0.00055 (12)
O15	0.00757 (19)	0.01245 (17)	0.00769 (17)	0.00119 (14)	0.00030 (13)	−0.00175 (13)
O16	0.00614 (18)	0.00879 (14)	0.00987 (18)	−0.00101 (13)	0.00127 (13)	−0.00238 (12)
N1	0.0069 (2)	0.00793 (15)	0.00868 (19)	0.00124 (14)	0.00098 (14)	−0.00052 (13)
N2	0.0073 (2)	0.00700 (14)	0.00674 (18)	−0.00005 (14)	0.00132 (13)	−0.00013 (12)
C1	0.0096 (2)	0.00688 (16)	0.0076 (2)	0.00001 (16)	−0.00037 (16)	−0.00072 (14)
C2	0.0082 (2)	0.00898 (18)	0.0096 (2)	0.00044 (17)	0.00268 (17)	0.00053 (15)
C3	0.0093 (2)	0.00801 (17)	0.0081 (2)	−0.00032 (16)	0.00113 (16)	−0.00149 (15)
C4	0.0081 (2)	0.00919 (18)	0.0100 (2)	−0.00055 (17)	0.00255 (17)	−0.00041 (15)
C5	0.0088 (2)	0.00691 (16)	0.0094 (2)	0.00112 (16)	0.00021 (16)	0.00041 (15)
C6	0.0091 (2)	0.00949 (18)	0.0077 (2)	0.00082 (17)	0.00147 (16)	0.00023 (15)
C7	0.0095 (2)	0.00826 (17)	0.0072 (2)	−0.00036 (16)	0.00116 (16)	−0.00120 (15)
C8	0.0094 (2)	0.00889 (18)	0.0084 (2)	−0.00111 (17)	0.00013 (16)	0.00015 (15)
C9	0.0145 (3)	0.01029 (19)	0.0081 (2)	0.00387 (19)	−0.00012 (18)	−0.00181 (16)
C10	0.0112 (3)	0.00720 (17)	0.0093 (2)	0.00142 (17)	−0.00032 (17)	0.00141 (15)
C11	0.0094 (2)	0.00983 (18)	0.0082 (2)	0.00140 (17)	0.00226 (17)	−0.00030 (15)
C12	0.0066 (2)	0.00930 (18)	0.0103 (2)	0.00006 (16)	0.00156 (16)	0.00010 (15)
C13	0.0073 (2)	0.00795 (17)	0.0084 (2)	−0.00159 (16)	0.00149 (16)	−0.00034 (14)
C14	0.0096 (2)	0.00667 (16)	0.0086 (2)	−0.00028 (16)	0.00214 (16)	0.00076 (14)
C15	0.0078 (2)	0.00662 (16)	0.0098 (2)	0.00067 (16)	0.00127 (16)	0.00043 (15)
C16	0.0092 (2)	0.00758 (17)	0.0076 (2)	−0.00023 (16)	0.00120 (16)	−0.00079 (14)
C17	0.0074 (2)	0.01011 (19)	0.0105 (2)	0.00182 (17)	0.00168 (17)	0.00131 (16)
C18	0.0103 (3)	0.00774 (17)	0.0116 (2)	0.00190 (17)	0.00299 (18)	0.00151 (16)
C19	0.0125 (3)	0.00809 (18)	0.0127 (2)	0.00226 (18)	0.00390 (19)	0.00307 (16)
C20	0.0123 (3)	0.0118 (2)	0.0085 (2)	0.00294 (19)	0.00184 (18)	0.00318 (16)
C21	0.0122 (3)	0.00891 (18)	0.0073 (2)	0.00172 (18)	0.00096 (17)	0.00053 (15)
C22	0.0095 (2)	0.00971 (19)	0.0090 (2)	0.00107 (17)	0.00339 (17)	0.00167 (15)
C23	0.0087 (2)	0.00980 (19)	0.0118 (2)	0.00134 (17)	0.00071 (18)	−0.00333 (16)
C24	0.0080 (2)	0.0139 (2)	0.0089 (2)	0.00035 (19)	0.00083 (17)	−0.00298 (17)
C25	0.0083 (2)	0.00949 (18)	0.0083 (2)	−0.00049 (17)	0.00003 (16)	−0.00189 (15)
C26	0.0077 (2)	0.00891 (18)	0.0110 (2)	−0.00132 (17)	0.00133 (17)	−0.00200 (16)
C27	0.0073 (2)	0.00997 (19)	0.0101 (2)	−0.00080 (17)	0.00139 (16)	−0.00194 (16)
C28	0.0074 (2)	0.00832 (17)	0.0093 (2)	0.00083 (16)	0.00091 (16)	−0.00065 (15)
H	0.027000	0.026000	0.046000	0.004000	−0.003000	0.018000
H1A	0.023000	0.023000	0.032000	0.005000	0.015000	−0.000000
H1B	0.028000	0.024000	0.016000	0.000000	−0.002000	0.003000
H1C	0.022000	0.026000	0.021000	0.004000	−0.006000	0.001000
H1D	0.021000	0.022000	0.033000	−0.003000	0.012000	0.003000
H1E	0.022000	0.027000	0.016000	0.000000	−0.004000	−0.001000
H1F	0.026000	0.022000	0.024000	−0.009000	0.011000	−0.000000
H1G	0.033000	0.013000	0.031000	−0.006000	0.011000	−0.005000
H1H	0.026000	0.029000	0.017000	0.005000	0.000000	0.007000
H1I	0.027000	0.013000	0.028000	−0.003000	0.006000	−0.005000
H1J	0.019000	0.026000	0.019000	0.004000	−0.002000	0.006000
H1K	0.025000	0.023000	0.017000	−0.002000	−0.005000	0.001000
H1L	0.024000	0.020000	0.027000	0.004000	0.011000	−0.005000
H1M	0.021000	0.025000	0.026000	−0.006000	−0.003000	0.004000
H1N	0.025000	0.029000	0.028000	0.013000	0.011000	0.005000
H1O	0.025000	0.030000	0.028000	0.013000	0.005000	0.012000
H1P	0.034000	0.017000	0.029000	−0.006000	0.008000	−0.005000
H1Q	0.028000	0.021000	0.036000	−0.009000	0.010000	−0.005000
H1R	0.032000	0.030000	0.028000	0.016000	0.007000	0.014000
H2A	0.021000	0.029000	0.026000	−0.002000	−0.005000	−0.005000
H2B	0.035000	0.032000	0.020000	0.009000	0.011000	0.012000
H2C	0.036000	0.027000	0.015000	0.006000	0.009000	0.006000
H2D	0.024000	0.020000	0.028000	−0.004000	−0.003000	−0.004000
H2E	0.032000	0.026000	0.022000	0.010000	0.014000	0.001000
H2F	0.021000	0.022000	0.029000	−0.007000	0.001000	0.004000
H2G	0.028000	0.016000	0.031000	−0.002000	0.001000	0.003000
H2H	0.024000	0.031000	0.027000	0.003000	0.009000	−0.011000
H2I	0.027000	0.028000	0.025000	0.002000	0.005000	0.010000
H2J	0.026000	0.034000	0.022000	−0.002000	0.001000	−0.014000
H2K	0.025000	0.020000	0.026000	−0.003000	−0.001000	−0.010000
H2L	0.028000	0.024000	0.019000	0.003000	0.001000	0.007000
H2M	0.035000	0.018000	0.024000	−0.002000	0.008000	0.004000
H2N	0.014000	0.031000	0.032000	−0.002000	−0.002000	−0.010000
H2O	0.031000	0.022000	0.027000	−0.007000	0.012000	−0.000000
H2P	0.014000	0.034000	0.033000	0.004000	−0.005000	−0.009000
H2Q	0.017000	0.030000	0.028000	0.006000	0.005000	−0.008000
H2R	0.027000	0.019000	0.020000	−0.002000	−0.002000	0.005000

Geometric parameters (Å, º)

Cr1—C1	1.9022 (6)	N2—C22	1.4737 (8)
Cr1—C2	1.9044 (7)	N2—C28	1.4678 (9)
Cr1—C3	1.9005 (6)	C11—C12	1.5175 (9)
Cr1—C4	1.8980 (7)	C11—H1A	1.115 (16)
Cr1—C5	1.8497 (6)	C11—H1B	1.088 (16)
Cr1—H	1.752 (17)	C12—H1C	1.111 (15)
Cr2—C6	1.9013 (7)	C12—H1D	1.107 (15)
Cr2—C7	1.8980 (6)	C13—C14	1.5028 (9)
Cr2—C8	1.8981 (7)	C13—H1E	1.097 (15)
Cr2—C9	1.9097 (7)	C13—H1F	1.102 (15)
Cr2—C10	1.8472 (6)	C14—H1G	1.100 (15)
Cr2—H	1.692 (17)	C14—H1H	1.093 (15)
K1—O1	2.9686 (6)	C15—C16	1.5161 (9)
K1—O11	2.8646 (5)	C15—H1I	1.102 (15)
K1—O12	2.8632 (5)	C15—H1J	1.087 (15)
K1—O13	2.8029 (5)	C16—H1K	1.093 (15)
K1—O14	2.7995 (5)	C16—H1L	1.097 (15)
K1—O15	2.8809 (5)	C17—C18	1.5169 (9)
K1—O16	2.8430 (5)	C17—H1M	1.068 (16)
K1—N1	3.0155 (6)	C17—H1N	1.088 (16)
K1—N2	3.0114 (6)	C18—H1O	1.120 (16)
O1—C1	1.1457 (8)	C18—H1P	1.097 (16)
O2—C2	1.1448 (9)	C19—C20	1.5065 (10)
O3—C3	1.1455 (8)	C19—H1Q	1.083 (16)
O4—C4	1.1470 (9)	C19—H1R	1.089 (15)
O5—C5	1.1564 (8)	C20—H2A	1.094 (16)
O6—C6	1.1443 (9)	C20—H2B	1.092 (16)
O7—C7	1.1483 (8)	C21—C22	1.5137 (10)
O8—C8	1.1480 (9)	C21—H2C	1.103 (15)
O9—C9	1.1434 (9)	C21—H2D	1.081 (16)
O10—C10	1.1569 (8)	C22—H2E	1.108 (16)
O11—C12	1.4167 (8)	C22—H2F	1.105 (16)
O11—C13	1.4274 (7)	C23—C24	1.5152 (10)
O12—C14	1.4186 (8)	C23—H2G	1.074 (16)
O12—C15	1.4211 (8)	C23—H2H	1.126 (16)
O13—C18	1.4162 (8)	C24—H2I	1.135 (17)
O13—C19	1.4201 (8)	C24—H2J	1.103 (16)
O14—C20	1.4204 (8)	C25—C26	1.5049 (9)
O14—C21	1.4279 (8)	C25—H2K	1.086 (15)
O15—C24	1.4246 (8)	C25—H2L	1.106 (16)
O15—C25	1.4168 (9)	C26—H2M	1.120 (16)
O16—C26	1.4233 (7)	C26—H2N	1.092 (15)
O16—C27	1.4208 (8)	C27—C28	1.5160 (9)
N1—C11	1.4693 (8)	C27—H2O	1.081 (16)
N1—C17	1.4718 (9)	C27—H2P	1.126 (16)
N1—C23	1.4716 (8)	C28—H2Q	1.111 (15)
N2—C16	1.4704 (8)	C28—H2R	1.068 (15)
C2—Cr1—C1	91.93 (3)	H1A—C11—N1	110.8 (9)
C3—Cr1—C1	174.91 (3)	H1A—C11—C12	108.4 (9)
C3—Cr1—C2	92.99 (3)	H1B—C11—N1	107.4 (9)
C4—Cr1—C1	89.76 (3)	H1B—C11—C12	108.2 (9)
C4—Cr1—C2	175.07 (3)	H1B—C11—H1A	107.0 (13)
C4—Cr1—C3	85.23 (3)	C11—C12—O11	110.43 (5)
C5—Cr1—C1	89.96 (3)	H1C—C12—O11	109.0 (9)
C5—Cr1—C2	90.15 (3)	H1C—C12—C11	112.1 (9)
C5—Cr1—C3	91.28 (3)	H1D—C12—O11	110.2 (9)
C5—Cr1—C4	94.48 (3)	H1D—C12—C11	109.1 (9)
H—Cr1—C1	95.2 (7)	H1D—C12—H1C	105.9 (13)
H—Cr1—C2	76.7 (6)	C14—C13—O11	109.65 (5)
H—Cr1—C3	84.8 (7)	H1E—C13—O11	111.2 (9)
H—Cr1—C4	98.5 (6)	H1E—C13—C14	110.0 (9)
H—Cr1—C5	166.0 (6)	H1F—C13—O11	110.6 (9)
C7—Cr2—C6	90.00 (3)	H1F—C13—C14	109.1 (9)
C8—Cr2—C6	176.31 (3)	H1F—C13—H1E	106.3 (13)
C8—Cr2—C7	91.99 (3)	C13—C14—O12	108.76 (5)
C9—Cr2—C6	88.70 (3)	H1G—C14—O12	110.7 (9)
C9—Cr2—C7	171.10 (3)	H1G—C14—C13	107.8 (9)
C9—Cr2—C8	89.81 (3)	H1H—C14—O12	110.8 (9)
C10—Cr2—C6	90.13 (3)	H1H—C14—C13	109.1 (9)
C10—Cr2—C7	93.62 (3)	H1H—C14—H1G	109.6 (13)
C10—Cr2—C8	86.65 (3)	C16—C15—O12	108.80 (5)
C10—Cr2—C9	95.19 (3)	H1I—C15—O12	110.0 (9)
H—Cr2—C6	81.7 (6)	H1I—C15—C16	107.7 (9)
H—Cr2—C7	84.3 (7)	H1J—C15—O12	110.8 (9)
H—Cr2—C8	101.5 (6)	H1J—C15—C16	113.9 (8)
H—Cr2—C9	86.8 (7)	H1J—C15—H1I	105.5 (12)
H—Cr2—C10	171.6 (6)	C15—C16—N2	114.05 (5)
O11—K1—O1	71.951 (15)	H1K—C16—N2	106.7 (9)
O12—K1—O1	65.096 (15)	H1K—C16—C15	109.1 (9)
O12—K1—O11	58.934 (14)	H1L—C16—N2	109.8 (9)
O13—K1—O1	64.153 (15)	H1L—C16—C15	108.7 (9)
O13—K1—O11	104.448 (15)	H1L—C16—H1K	108.3 (13)
O13—K1—O12	129.248 (16)	C18—C17—N1	113.87 (6)
O14—K1—O1	74.478 (16)	H1M—C17—N1	107.7 (9)
O14—K1—O11	146.380 (15)	H1M—C17—C18	105.8 (9)
O14—K1—O12	104.629 (14)	H1N—C17—N1	111.3 (9)
O14—K1—O13	61.240 (14)	H1N—C17—C18	108.5 (9)
O15—K1—O1	147.825 (16)	H1N—C17—H1M	109.5 (13)
O15—K1—O11	99.517 (15)	C17—C18—O13	109.22 (5)
O15—K1—O12	137.659 (15)	H1O—C18—O13	108.8 (9)
O15—K1—O13	89.430 (15)	H1O—C18—C17	109.6 (9)
O15—K1—O14	109.934 (15)	H1P—C18—O13	110.3 (9)
O16—K1—O1	152.187 (15)	H1P—C18—C17	111.3 (9)
O16—K1—O11	119.252 (15)	H1P—C18—H1O	107.6 (13)
O16—K1—O12	97.626 (15)	C20—C19—O13	108.89 (5)
O16—K1—O13	128.505 (15)	H1Q—C19—O13	108.6 (9)
O16—K1—O14	90.377 (15)	H1Q—C19—C20	112.1 (9)
O16—K1—O15	59.189 (14)	H1R—C19—O13	110.6 (9)
N1—K1—O1	90.403 (16)	H1R—C19—C20	108.4 (9)
N1—K1—O11	62.045 (14)	H1R—C19—H1Q	108.2 (14)
N1—K1—O12	120.456 (15)	C19—C20—O14	110.03 (6)
N1—K1—O13	60.334 (15)	H2A—C20—O14	110.8 (9)
N1—K1—O14	120.395 (15)	H2A—C20—C19	109.0 (9)
N1—K1—O15	59.305 (15)	H2B—C20—O14	108.8 (9)
N1—K1—O16	117.407 (15)	H2B—C20—C19	109.6 (9)
N2—K1—O1	91.998 (15)	H2B—C20—H2A	108.5 (13)
N2—K1—O11	117.233 (14)	C22—C21—O14	109.35 (5)
N2—K1—O12	59.314 (14)	H2C—C21—O14	109.5 (9)
N2—K1—O13	122.290 (15)	H2C—C21—C22	109.8 (9)
N2—K1—O14	61.919 (14)	H2D—C21—O14	110.5 (9)
N2—K1—O15	118.645 (15)	H2D—C21—C22	112.3 (9)
N2—K1—O16	60.193 (14)	H2D—C21—H2C	105.4 (13)
N2—K1—N1	177.091 (15)	C21—C22—N2	113.20 (6)
C1—O1—K1	148.78 (5)	H2E—C22—N2	110.6 (9)
C12—O11—K1	111.61 (4)	H2E—C22—C21	109.2 (9)
C13—O11—K1	113.87 (4)	H2F—C22—N2	109.6 (9)
C13—O11—C12	110.28 (5)	H2F—C22—C21	106.3 (9)
C14—O12—K1	117.63 (3)	H2F—C22—H2E	107.7 (13)
C15—O12—K1	121.03 (4)	C24—C23—N1	113.42 (5)
C15—O12—C14	111.78 (5)	H2G—C23—N1	109.0 (9)
C18—O13—K1	121.02 (4)	H2G—C23—C24	106.0 (9)
C19—O13—K1	113.64 (4)	H2H—C23—N1	112.8 (9)
C19—O13—C18	111.94 (5)	H2H—C23—C24	108.6 (9)
C20—O14—K1	113.65 (4)	H2H—C23—H2G	106.7 (13)
C21—O14—K1	112.05 (4)	C23—C24—O15	108.63 (5)
C21—O14—C20	110.73 (5)	H2I—C24—O15	110.7 (9)
C24—O15—K1	115.73 (4)	H2I—C24—C23	112.0 (9)
C25—O15—K1	117.04 (4)	H2J—C24—O15	108.4 (9)
C25—O15—C24	111.28 (5)	H2J—C24—C23	110.6 (9)
C26—O16—K1	112.69 (4)	H2J—C24—H2I	106.4 (13)
C27—O16—K1	120.09 (4)	C26—C25—O15	109.29 (5)
C27—O16—C26	110.61 (5)	H2K—C25—O15	111.7 (9)
C11—N1—K1	107.32 (3)	H2K—C25—C26	109.1 (9)
C17—N1—K1	107.30 (4)	H2L—C25—O15	110.7 (9)
C17—N1—C11	110.14 (5)	H2L—C25—C26	110.5 (9)
C23—N1—K1	112.21 (4)	H2L—C25—H2K	105.6 (13)
C23—N1—C11	109.24 (5)	C25—C26—O16	109.54 (5)
C23—N1—C17	110.57 (5)	H2M—C26—O16	110.3 (9)
C16—N2—K1	109.82 (4)	H2M—C26—C25	111.1 (9)
C22—N2—K1	107.62 (4)	H2N—C26—O16	110.2 (9)
C22—N2—C16	109.42 (5)	H2N—C26—C25	108.0 (9)
C28—N2—K1	108.75 (4)	H2N—C26—H2M	107.8 (13)
C28—N2—C16	109.87 (5)	C28—C27—O16	110.53 (5)
C28—N2—C22	111.32 (5)	H2O—C27—O16	108.5 (9)
O1—C1—Cr1	177.05 (6)	H2O—C27—C28	112.3 (9)
O2—C2—Cr1	178.81 (6)	H2P—C27—O16	107.6 (9)
O3—C3—Cr1	176.01 (6)	H2P—C27—C28	108.2 (9)
O4—C4—Cr1	177.84 (6)	H2P—C27—H2O	109.6 (13)
O5—C5—Cr1	177.69 (6)	C27—C28—N2	114.07 (5)
O6—C6—Cr2	178.73 (6)	H2Q—C28—N2	111.6 (9)
O7—C7—Cr2	178.60 (6)	H2Q—C28—C27	107.4 (9)
O8—C8—Cr2	174.69 (6)	H2R—C28—N2	106.9 (8)
O9—C9—Cr2	178.61 (6)	H2R—C28—C27	108.0 (9)
O10—C10—Cr2	177.98 (6)	H2R—C28—H2Q	108.8 (13)
C12—C11—N1	114.57 (5)	Cr2—H—Cr1	147.3 (12)

(KCPTCR_HAR_NoMoRe)

Crystal data

C28H37Cr2KN2O16	F(000) = 1660.306
Mr = 800.70	Dx = 1.489 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71069 Å
a = 10.458 Å	Cell parameters from 1024 reflections
b = 14.417 Å	θ = 47.5–1.5°
c = 23.882 Å	µ = 0.80 mm^−1
β = 97.26°	T = 28 K
V = 3571.89 Å^3	Ellipsoidal, yellow
Z = 4	0.3 × 0.25 × 0.2 mm

Data collection

SMART CCD diffractometer	22531 reflections with I ≥ 2u(I)
ω scan	Rint = 0.0000
Absorption correction: empirical (using intensity measurements)	θmax = 48.7°, θmin = 2.4°
Tmin = 0.890, Tmax = 0.903	h = −19→20
27917 measured reflections	k = 0→30
27917 independent reflections	l = 0→50

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.031	Only H-atom coordinates refined
wR(F^2) = 0.100	w = 1/[σ^2(Fo^2) + (0.1P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 0.69	(Δ/σ)max = 0.001
27917 reflections	Δρmax = 0.73 e Å^−3
553 parameters	Δρmin = −1.27 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Cr1	0.163876 (10)	0.002347 (6)	0.236375 (4)	0.005245 (17)
Cr2	0.018763 (10)	0.177450 (6)	0.165108 (4)	0.005810 (18)
K1	0.463713 (13)	0.199294 (8)	0.418001 (5)	0.00657 (2)
O1	0.25208 (6)	0.13810 (3)	0.33122 (2)	0.01184 (8)
O2	−0.08355 (6)	−0.04362 (4)	0.28576 (3)	0.01424 (9)
O3	0.10469 (6)	−0.12659 (4)	0.13548 (2)	0.01260 (8)
O4	0.39548 (6)	0.05450 (4)	0.17751 (3)	0.01366 (9)
O5	0.30038 (6)	−0.15033 (4)	0.30580 (2)	0.01236 (8)
O6	−0.25958 (6)	0.12167 (4)	0.17223 (2)	0.01235 (8)
O7	0.01687 (6)	0.05854 (4)	0.05958 (2)	0.01265 (8)
O8	0.28636 (6)	0.25364 (4)	0.15524 (2)	0.01343 (9)
O9	0.02671 (7)	0.26561 (4)	0.28173 (3)	0.01788 (11)
O10	−0.07205 (6)	0.34765 (4)	0.09922 (3)	0.01457 (9)
O11	0.28570 (5)	0.09215 (3)	0.47314 (2)	0.00784 (7)
O12	0.44346 (5)	0.00268 (3)	0.40246 (2)	0.00837 (7)
O13	0.31318 (5)	0.34097 (3)	0.36294 (2)	0.00878 (7)
O14	0.52819 (5)	0.26678 (3)	0.31528 (2)	0.00893 (7)
O15	0.55089 (5)	0.32676 (4)	0.50766 (2)	0.00929 (7)
O16	0.72730 (5)	0.20516 (3)	0.46498 (2)	0.00824 (7)
N1	0.27305 (6)	0.30199 (4)	0.47985 (2)	0.00785 (7)
N2	0.66187 (5)	0.09454 (3)	0.36195 (2)	0.00696 (7)
C1	0.21620 (7)	0.08861 (4)	0.29509 (3)	0.00815 (8)
C2	0.01010 (7)	−0.02689 (4)	0.26769 (3)	0.00879 (9)
C3	0.12292 (7)	−0.07914 (4)	0.17414 (3)	0.00848 (8)
C4	0.30806 (7)	0.03663 (4)	0.20002 (3)	0.00900 (9)
C5	0.25021 (7)	−0.09119 (4)	0.27863 (3)	0.00846 (8)
C6	−0.15452 (7)	0.14180 (4)	0.16996 (3)	0.00873 (9)
C7	0.01878 (7)	0.10405 (4)	0.09913 (3)	0.00830 (8)
C8	0.18818 (7)	0.22110 (4)	0.16012 (3)	0.00901 (9)
C9	0.02397 (7)	0.23368 (4)	0.23777 (3)	0.01109 (10)
C10	−0.03870 (7)	0.28241 (4)	0.12526 (3)	0.00938 (9)
C11	0.20814 (7)	0.23292 (4)	0.51164 (3)	0.00904 (9)
C12	0.17313 (6)	0.14345 (4)	0.47988 (3)	0.00867 (9)
C13	0.25204 (7)	0.00543 (4)	0.44641 (3)	0.00786 (8)
C14	0.37236 (7)	−0.04780 (4)	0.43910 (3)	0.00820 (8)
C15	0.54819 (6)	−0.04991 (4)	0.38672 (3)	0.00804 (8)
C16	0.60989 (7)	0.00369 (4)	0.34255 (3)	0.00812 (8)
C17	0.17934 (7)	0.34655 (4)	0.43702 (3)	0.00930 (9)
C18	0.24064 (7)	0.40165 (4)	0.39331 (3)	0.00976 (9)
C19	0.37487 (7)	0.38881 (4)	0.32182 (3)	0.01091 (10)
C20	0.42815 (7)	0.31884 (5)	0.28403 (3)	0.01081 (10)
C21	0.57213 (7)	0.19482 (4)	0.28134 (3)	0.00947 (9)
C22	0.69037 (7)	0.14948 (4)	0.31299 (3)	0.00920 (9)
C23	0.33590 (7)	0.37151 (4)	0.51924 (3)	0.01014 (9)
C24	0.46543 (7)	0.34034 (5)	0.54889 (3)	0.01030 (9)
C25	0.68009 (7)	0.31747 (4)	0.53319 (3)	0.00878 (9)
C26	0.76441 (7)	0.29314 (4)	0.48874 (3)	0.00917 (9)
C27	0.82389 (7)	0.16973 (4)	0.43397 (3)	0.00907 (9)
C28	0.77753 (6)	0.08188 (4)	0.40292 (3)	0.00838 (8)
H	0.0490 (18)	0.0761 (13)	0.1997 (8)	0.033990
H1A	0.1191 (16)	0.2623 (12)	0.5257 (7)	0.025008
H1B	0.2731 (16)	0.2161 (12)	0.5495 (7)	0.023076
H1C	0.1177 (16)	0.1563 (12)	0.4374 (7)	0.024080
H1D	0.1085 (15)	0.1020 (12)	0.5034 (7)	0.024846
H1E	0.1940 (16)	0.0156 (12)	0.4054 (7)	0.022548
H1F	0.1926 (16)	−0.0363 (11)	0.4721 (7)	0.022990
H1G	0.3432 (16)	−0.1160 (11)	0.4209 (7)	0.025071
H1H	0.4293 (16)	−0.0575 (12)	0.4806 (7)	0.024233
H1I	0.5126 (16)	−0.1161 (11)	0.3675 (7)	0.022451
H1J	0.6148 (15)	−0.0684 (11)	0.4238 (6)	0.021710
H1K	0.5372 (16)	0.0167 (11)	0.3061 (7)	0.021983
H1L	0.6863 (16)	−0.0390 (11)	0.3283 (7)	0.023086
H1M	0.1246 (16)	0.2928 (11)	0.4142 (7)	0.024172
H1N	0.1145 (16)	0.3919 (12)	0.4562 (7)	0.026678
H1O	0.1637 (16)	0.4348 (12)	0.3631 (7)	0.027859
H1P	0.3025 (16)	0.4572 (11)	0.4130 (7)	0.026323
H1Q	0.4495 (16)	0.4327 (11)	0.3433 (7)	0.027823
H1R	0.3069 (16)	0.4326 (12)	0.2960 (7)	0.029387
H2A	0.3498 (16)	0.2731 (13)	0.2658 (7)	0.026016
H2B	0.4675 (17)	0.3545 (13)	0.2495 (7)	0.028356
H2C	0.5962 (17)	0.2244 (12)	0.2414 (7)	0.025839
H2D	0.4956 (16)	0.1453 (11)	0.2692 (7)	0.024199
H2E	0.7375 (16)	0.1059 (12)	0.2835 (7)	0.025421
H2F	0.7572 (16)	0.2062 (12)	0.3275 (7)	0.024185
H2G	0.3545 (16)	0.4331 (11)	0.4960 (7)	0.025234
H2H	0.2740 (16)	0.3934 (13)	0.5519 (7)	0.026839
H2I	0.4572 (17)	0.2744 (13)	0.5743 (7)	0.026181
H2J	0.5066 (16)	0.3938 (12)	0.5788 (7)	0.027841
H2K	0.7152 (16)	0.3808 (11)	0.5542 (7)	0.024028
H2L	0.6874 (16)	0.2636 (12)	0.5664 (7)	0.023835
H2M	0.7578 (18)	0.3471 (11)	0.4549 (7)	0.025301
H2N	0.8636 (15)	0.2907 (12)	0.5087 (7)	0.026087
H2O	0.8492 (16)	0.2229 (11)	0.4058 (7)	0.025614
H2P	0.9109 (16)	0.1515 (13)	0.4652 (8)	0.027677
H2Q	0.8592 (15)	0.0541 (12)	0.3826 (7)	0.024477
H2R	0.7532 (16)	0.0325 (11)	0.4337 (6)	0.022425

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cr1	0.00569 (4)	0.00465 (3)	0.00537 (3)	0.00020 (2)	0.00060 (2)	−0.00015 (2)
Cr2	0.00680 (4)	0.00533 (3)	0.00515 (3)	0.00087 (2)	0.00021 (2)	0.00017 (2)
K1	0.00627 (5)	0.00672 (4)	0.00667 (4)	0.00020 (3)	0.00060 (3)	−0.00005 (3)
O1	0.0156 (2)	0.00918 (15)	0.00979 (19)	−0.00009 (15)	−0.00223 (15)	−0.00277 (13)
O2	0.0106 (2)	0.0167 (2)	0.0166 (2)	−0.00015 (17)	0.00648 (17)	0.00149 (17)
O3	0.0153 (2)	0.01230 (17)	0.01023 (19)	−0.00204 (16)	0.00161 (16)	−0.00502 (14)
O4	0.0110 (2)	0.01397 (18)	0.0173 (2)	−0.00092 (17)	0.00695 (17)	0.00012 (16)
O5	0.0136 (2)	0.00923 (15)	0.0135 (2)	0.00351 (15)	−0.00095 (16)	0.00256 (14)
O6	0.0095 (2)	0.01503 (18)	0.0130 (2)	−0.00105 (16)	0.00346 (15)	0.00016 (15)
O7	0.0169 (2)	0.01230 (17)	0.00906 (19)	−0.00135 (17)	0.00292 (16)	−0.00336 (14)
O8	0.0111 (2)	0.01615 (19)	0.0129 (2)	−0.00546 (17)	0.00069 (16)	0.00072 (16)
O9	0.0264 (3)	0.0174 (2)	0.0090 (2)	0.0097 (2)	−0.00111 (19)	−0.00489 (16)
O10	0.0179 (3)	0.00947 (16)	0.0152 (2)	0.00300 (16)	−0.00220 (18)	0.00426 (15)
O11	0.00644 (18)	0.00770 (13)	0.00933 (17)	−0.00021 (13)	0.00083 (13)	−0.00098 (12)
O12	0.00899 (19)	0.00667 (13)	0.00987 (18)	0.00075 (13)	0.00284 (14)	0.00106 (12)
O13	0.0096 (2)	0.00715 (13)	0.00986 (18)	0.00085 (13)	0.00236 (14)	0.00118 (12)
O14	0.0101 (2)	0.00884 (14)	0.00775 (17)	0.00180 (14)	0.00085 (13)	0.00055 (12)
O15	0.00759 (19)	0.01243 (17)	0.00769 (17)	0.00119 (14)	0.00032 (13)	−0.00175 (13)
O16	0.00612 (18)	0.00882 (14)	0.00986 (18)	−0.00098 (13)	0.00129 (13)	−0.00235 (12)
N1	0.0069 (2)	0.00793 (15)	0.00869 (19)	0.00124 (14)	0.00099 (14)	−0.00051 (13)
N2	0.0073 (2)	0.00698 (14)	0.00675 (18)	−0.00005 (14)	0.00130 (13)	−0.00014 (12)
C1	0.0096 (2)	0.00688 (16)	0.0076 (2)	0.00002 (16)	−0.00037 (16)	−0.00072 (14)
C2	0.0082 (2)	0.00897 (18)	0.0096 (2)	0.00044 (17)	0.00268 (17)	0.00053 (15)
C3	0.0093 (2)	0.00801 (17)	0.0082 (2)	−0.00032 (16)	0.00113 (16)	−0.00150 (15)
C4	0.0081 (2)	0.00919 (18)	0.0100 (2)	−0.00056 (17)	0.00255 (17)	−0.00041 (15)
C5	0.0088 (2)	0.00691 (16)	0.0094 (2)	0.00112 (16)	0.00021 (16)	0.00041 (15)
C6	0.0091 (2)	0.00948 (18)	0.0078 (2)	0.00081 (17)	0.00148 (16)	0.00023 (15)
C7	0.0095 (2)	0.00826 (17)	0.0072 (2)	−0.00036 (16)	0.00116 (16)	−0.00121 (15)
C8	0.0094 (2)	0.00889 (18)	0.0084 (2)	−0.00110 (17)	0.00012 (16)	0.00015 (15)
C9	0.0145 (3)	0.01028 (19)	0.0081 (2)	0.00387 (19)	−0.00013 (18)	−0.00181 (16)
C10	0.0112 (3)	0.00720 (17)	0.0093 (2)	0.00141 (17)	−0.00031 (17)	0.00142 (15)
C11	0.0094 (2)	0.00982 (18)	0.0082 (2)	0.00140 (17)	0.00224 (17)	−0.00032 (15)
C12	0.0066 (2)	0.00933 (18)	0.0102 (2)	0.00007 (16)	0.00153 (16)	0.00011 (15)
C13	0.0073 (2)	0.00795 (17)	0.0084 (2)	−0.00159 (16)	0.00150 (16)	−0.00033 (14)
C14	0.0096 (2)	0.00668 (16)	0.0086 (2)	−0.00028 (16)	0.00211 (16)	0.00077 (14)
C15	0.0078 (2)	0.00662 (16)	0.0098 (2)	0.00067 (16)	0.00126 (16)	0.00042 (15)
C16	0.0092 (2)	0.00760 (17)	0.0076 (2)	−0.00022 (16)	0.00119 (16)	−0.00077 (14)
C17	0.0074 (2)	0.01011 (19)	0.0105 (2)	0.00181 (17)	0.00168 (17)	0.00130 (16)
C18	0.0103 (3)	0.00774 (17)	0.0116 (2)	0.00190 (17)	0.00298 (18)	0.00150 (16)
C19	0.0125 (3)	0.00808 (18)	0.0127 (2)	0.00225 (18)	0.00391 (19)	0.00305 (16)
C20	0.0123 (3)	0.0118 (2)	0.0085 (2)	0.00291 (19)	0.00182 (18)	0.00318 (16)
C21	0.0121 (3)	0.00891 (18)	0.0073 (2)	0.00168 (18)	0.00095 (17)	0.00053 (15)
C22	0.0095 (2)	0.00971 (19)	0.0090 (2)	0.00107 (17)	0.00339 (17)	0.00169 (15)
C23	0.0087 (2)	0.00978 (19)	0.0118 (2)	0.00132 (17)	0.00069 (18)	−0.00332 (16)
C24	0.0080 (2)	0.0139 (2)	0.0089 (2)	0.00035 (19)	0.00083 (17)	−0.00297 (17)
C25	0.0083 (2)	0.00949 (18)	0.0083 (2)	−0.00049 (17)	0.00003 (16)	−0.00188 (15)
C26	0.0077 (2)	0.00888 (18)	0.0110 (2)	−0.00133 (17)	0.00133 (17)	−0.00203 (16)
C27	0.0073 (2)	0.00997 (19)	0.0101 (2)	−0.00080 (17)	0.00137 (16)	−0.00195 (16)
C28	0.0075 (2)	0.00831 (17)	0.0093 (2)	0.00081 (16)	0.00091 (16)	−0.00062 (15)
H	0.028000	0.026000	0.046000	0.004000	−0.003000	0.018000
H1A	0.023000	0.024000	0.031000	0.006000	0.015000	−0.000000
H1B	0.028000	0.024000	0.016000	0.001000	−0.002000	0.003000
H1C	0.022000	0.027000	0.021000	0.004000	−0.006000	0.001000
H1D	0.021000	0.023000	0.033000	−0.003000	0.013000	0.004000
H1E	0.022000	0.028000	0.016000	0.000000	−0.004000	−0.001000
H1F	0.025000	0.022000	0.024000	−0.009000	0.011000	−0.000000
H1G	0.033000	0.013000	0.031000	−0.006000	0.011000	−0.005000
H1H	0.026000	0.029000	0.017000	0.004000	0.000000	0.006000
H1I	0.027000	0.013000	0.028000	−0.003000	0.006000	−0.005000
H1J	0.019000	0.026000	0.019000	0.004000	−0.002000	0.006000
H1K	0.024000	0.023000	0.017000	−0.002000	−0.005000	0.001000
H1L	0.024000	0.020000	0.027000	0.004000	0.010000	−0.006000
H1M	0.021000	0.025000	0.025000	−0.005000	−0.003000	0.004000
H1N	0.025000	0.029000	0.028000	0.014000	0.011000	0.005000
H1O	0.025000	0.031000	0.028000	0.013000	0.005000	0.012000
H1P	0.034000	0.017000	0.029000	−0.006000	0.008000	−0.005000
H1Q	0.028000	0.021000	0.036000	−0.009000	0.010000	−0.005000
H1R	0.032000	0.030000	0.027000	0.016000	0.007000	0.014000
H2A	0.021000	0.029000	0.026000	−0.001000	−0.005000	−0.005000
H2B	0.035000	0.032000	0.020000	0.009000	0.011000	0.012000
H2C	0.036000	0.028000	0.015000	0.006000	0.009000	0.006000
H2D	0.023000	0.020000	0.028000	−0.003000	−0.003000	−0.004000
H2E	0.031000	0.026000	0.022000	0.009000	0.014000	0.001000
H2F	0.021000	0.022000	0.029000	−0.007000	0.001000	0.004000
H2G	0.029000	0.016000	0.030000	−0.001000	0.001000	0.003000
H2H	0.024000	0.031000	0.027000	0.004000	0.009000	−0.011000
H2I	0.026000	0.028000	0.025000	0.002000	0.005000	0.010000
H2J	0.026000	0.035000	0.022000	−0.001000	0.001000	−0.014000
H2K	0.025000	0.020000	0.026000	−0.003000	−0.001000	−0.010000
H2L	0.028000	0.024000	0.019000	0.003000	0.001000	0.007000
H2M	0.035000	0.018000	0.024000	−0.002000	0.008000	0.004000
H2N	0.014000	0.031000	0.032000	−0.002000	−0.002000	−0.010000
H2O	0.031000	0.022000	0.026000	−0.007000	0.012000	−0.000000
H2P	0.014000	0.035000	0.032000	0.004000	−0.005000	−0.010000
H2Q	0.017000	0.030000	0.027000	0.006000	0.005000	−0.009000
H2R	0.027000	0.019000	0.020000	−0.002000	−0.002000	0.005000

Geometric parameters (Å, º)

Cr1—C1	1.9022 (6)	N2—C22	1.4736 (8)
Cr1—C2	1.9044 (7)	N2—C28	1.4679 (9)
Cr1—C3	1.9005 (6)	C11—C12	1.5175 (9)
Cr1—C4	1.8980 (7)	C11—H1A	1.113 (16)
Cr1—C5	1.8497 (6)	C11—H1B	1.088 (16)
Cr1—H	1.754 (17)	C12—H1C	1.118 (16)
Cr2—C6	1.9012 (7)	C12—H1D	1.106 (15)
Cr2—C7	1.8980 (6)	C13—C14	1.5028 (9)
Cr2—C8	1.8981 (7)	C13—H1E	1.096 (15)
Cr2—C9	1.9098 (7)	C13—H1F	1.105 (15)
Cr2—C10	1.8472 (6)	C14—H1G	1.102 (15)
Cr2—H	1.689 (17)	C14—H1H	1.099 (15)
K1—O1	2.9686 (6)	C15—C16	1.5160 (9)
K1—O11	2.8646 (5)	C15—H1I	1.103 (15)
K1—O12	2.8632 (5)	C15—H1J	1.089 (15)
K1—O13	2.8029 (5)	C16—H1K	1.096 (15)
K1—O14	2.7995 (5)	C16—H1L	1.096 (15)
K1—O15	2.8809 (5)	C17—C18	1.5168 (9)
K1—O16	2.8431 (5)	C17—H1M	1.071 (16)
K1—N1	3.0156 (6)	C17—H1N	1.084 (15)
K1—N2	3.0114 (6)	C18—H1O	1.117 (16)
O1—C1	1.1458 (8)	C18—H1P	1.097 (16)
O2—C2	1.1448 (9)	C19—C20	1.5064 (10)
O3—C3	1.1455 (8)	C19—H1Q	1.082 (16)
O4—C4	1.1470 (9)	C19—H1R	1.083 (15)
O5—C5	1.1564 (8)	C20—H2A	1.098 (16)
O6—C6	1.1443 (9)	C20—H2B	1.094 (16)
O7—C7	1.1483 (8)	C21—C22	1.5137 (10)
O8—C8	1.1480 (9)	C21—H2C	1.102 (15)
O9—C9	1.1435 (9)	C21—H2D	1.084 (16)
O10—C10	1.1568 (8)	C22—H2E	1.105 (16)
O11—C12	1.4166 (8)	C22—H2F	1.103 (16)
O11—C13	1.4274 (7)	C23—C24	1.5152 (10)
O12—C14	1.4187 (8)	C23—H2G	1.077 (16)
O12—C15	1.4211 (8)	C23—H2H	1.120 (16)
O13—C18	1.4162 (8)	C24—H2I	1.137 (17)
O13—C19	1.4201 (8)	C24—H2J	1.101 (16)
O14—C20	1.4204 (8)	C25—C26	1.5049 (9)
O14—C21	1.4278 (8)	C25—H2K	1.083 (15)
O15—C24	1.4245 (8)	C25—H2L	1.105 (16)
O15—C25	1.4168 (9)	C26—H2M	1.118 (16)
O16—C26	1.4233 (7)	C26—H2N	1.086 (15)
O16—C27	1.4208 (8)	C27—C28	1.5159 (9)
N1—C11	1.4693 (8)	C27—H2O	1.075 (16)
N1—C17	1.4718 (9)	C27—H2P	1.132 (16)
N1—C23	1.4716 (8)	C28—H2Q	1.109 (15)
N2—C16	1.4704 (8)	C28—H2R	1.077 (15)
C2—Cr1—C1	91.93 (3)	H1A—C11—N1	111.0 (9)
C3—Cr1—C1	174.91 (3)	H1A—C11—C12	108.4 (9)
C3—Cr1—C2	92.99 (3)	H1B—C11—N1	107.5 (9)
C4—Cr1—C1	89.76 (3)	H1B—C11—C12	108.1 (9)
C4—Cr1—C2	175.07 (3)	H1B—C11—H1A	107.0 (13)
C4—Cr1—C3	85.23 (3)	C11—C12—O11	110.43 (5)
C5—Cr1—C1	89.96 (3)	H1C—C12—O11	109.1 (9)
C5—Cr1—C2	90.15 (3)	H1C—C12—C11	112.1 (9)
C5—Cr1—C3	91.27 (3)	H1D—C12—O11	110.2 (9)
C5—Cr1—C4	94.48 (3)	H1D—C12—C11	109.2 (9)
H—Cr1—C1	95.0 (7)	H1D—C12—H1C	105.7 (13)
H—Cr1—C2	76.8 (6)	C14—C13—O11	109.66 (5)
H—Cr1—C3	84.9 (7)	H1E—C13—O11	111.1 (9)
H—Cr1—C4	98.5 (6)	H1E—C13—C14	110.0 (9)
H—Cr1—C5	166.1 (6)	H1F—C13—O11	110.6 (9)
C7—Cr2—C6	90.00 (3)	H1F—C13—C14	109.0 (9)
C8—Cr2—C6	176.32 (3)	H1F—C13—H1E	106.4 (13)
C8—Cr2—C7	91.99 (3)	C13—C14—O12	108.76 (5)
C9—Cr2—C6	88.70 (3)	H1G—C14—O12	110.8 (9)
C9—Cr2—C7	171.09 (3)	H1G—C14—C13	107.9 (9)
C9—Cr2—C8	89.81 (3)	H1H—C14—O12	110.8 (9)
C10—Cr2—C6	90.13 (3)	H1H—C14—C13	109.1 (9)
C10—Cr2—C7	93.62 (3)	H1H—C14—H1G	109.4 (13)
C10—Cr2—C8	86.65 (3)	C16—C15—O12	108.80 (5)
C10—Cr2—C9	95.19 (3)	H1I—C15—O12	109.9 (9)
H—Cr2—C6	81.8 (6)	H1I—C15—C16	107.6 (9)
H—Cr2—C7	84.5 (7)	H1J—C15—O12	110.5 (9)
H—Cr2—C8	101.5 (6)	H1J—C15—C16	114.0 (9)
H—Cr2—C9	86.6 (7)	H1J—C15—H1I	105.9 (12)
H—Cr2—C10	171.7 (6)	C15—C16—N2	114.06 (5)
O11—K1—O1	71.951 (15)	H1K—C16—N2	106.8 (9)
O12—K1—O1	65.095 (15)	H1K—C16—C15	109.0 (9)
O12—K1—O11	58.935 (14)	H1L—C16—N2	110.1 (9)
O13—K1—O1	64.153 (15)	H1L—C16—C15	108.7 (9)
O13—K1—O11	104.447 (15)	H1L—C16—H1K	108.0 (13)
O13—K1—O12	129.248 (16)	C18—C17—N1	113.87 (6)
O14—K1—O1	74.480 (16)	H1M—C17—N1	107.7 (9)
O14—K1—O11	146.381 (15)	H1M—C17—C18	105.9 (9)
O14—K1—O12	104.628 (14)	H1N—C17—N1	111.5 (9)
O14—K1—O13	61.241 (14)	H1N—C17—C18	108.4 (9)
O15—K1—O1	147.825 (16)	H1N—C17—H1M	109.2 (13)
O15—K1—O11	99.517 (15)	C17—C18—O13	109.22 (5)
O15—K1—O12	137.659 (15)	H1O—C18—O13	108.8 (9)
O15—K1—O13	89.430 (15)	H1O—C18—C17	109.6 (9)
O15—K1—O14	109.934 (15)	H1P—C18—O13	110.2 (9)
O16—K1—O1	152.188 (15)	H1P—C18—C17	111.4 (9)
O16—K1—O11	119.255 (15)	H1P—C18—H1O	107.6 (13)
O16—K1—O12	97.628 (15)	C20—C19—O13	108.89 (5)
O16—K1—O13	128.503 (15)	H1Q—C19—O13	108.6 (9)
O16—K1—O14	90.374 (15)	H1Q—C19—C20	112.1 (9)
O16—K1—O15	59.187 (14)	H1R—C19—O13	110.7 (9)
N1—K1—O1	90.404 (16)	H1R—C19—C20	108.4 (9)
N1—K1—O11	62.046 (14)	H1R—C19—H1Q	108.1 (14)
N1—K1—O12	120.457 (15)	C19—C20—O14	110.05 (6)
N1—K1—O13	60.333 (15)	H2A—C20—O14	110.8 (9)
N1—K1—O14	120.395 (15)	H2A—C20—C19	109.0 (9)
N1—K1—O15	59.304 (15)	H2B—C20—O14	108.8 (9)
N1—K1—O16	117.405 (15)	H2B—C20—C19	109.8 (9)
N2—K1—O1	91.998 (15)	H2B—C20—H2A	108.4 (13)
N2—K1—O11	117.235 (14)	C22—C21—O14	109.36 (5)
N2—K1—O12	59.314 (14)	H2C—C21—O14	109.6 (9)
N2—K1—O13	122.289 (15)	H2C—C21—C22	109.8 (9)
N2—K1—O14	61.918 (14)	H2D—C21—O14	110.5 (9)
N2—K1—O15	118.645 (15)	H2D—C21—C22	112.3 (9)
N2—K1—O16	60.194 (14)	H2D—C21—H2C	105.3 (13)
N2—K1—N1	177.091 (15)	C21—C22—N2	113.20 (6)
C1—O1—K1	148.78 (5)	H2E—C22—N2	110.6 (9)
C12—O11—K1	111.62 (4)	H2E—C22—C21	109.2 (9)
C13—O11—K1	113.87 (4)	H2F—C22—N2	109.5 (9)
C13—O11—C12	110.28 (5)	H2F—C22—C21	106.4 (9)
C14—O12—K1	117.63 (3)	H2F—C22—H2E	107.8 (13)
C15—O12—K1	121.03 (4)	C24—C23—N1	113.42 (5)
C15—O12—C14	111.78 (5)	H2G—C23—N1	109.1 (9)
C18—O13—K1	121.02 (4)	H2G—C23—C24	106.0 (9)
C19—O13—K1	113.64 (4)	H2H—C23—N1	112.7 (9)
C19—O13—C18	111.94 (5)	H2H—C23—C24	108.6 (9)
C20—O14—K1	113.64 (4)	H2H—C23—H2G	106.5 (13)
C21—O14—K1	112.05 (4)	C23—C24—O15	108.64 (5)
C21—O14—C20	110.74 (5)	H2I—C24—O15	110.5 (9)
C24—O15—K1	115.73 (4)	H2I—C24—C23	112.0 (9)
C25—O15—K1	117.04 (4)	H2J—C24—O15	108.5 (9)
C25—O15—C24	111.28 (5)	H2J—C24—C23	110.5 (9)
C26—O16—K1	112.69 (4)	H2J—C24—H2I	106.7 (13)
C27—O16—K1	120.09 (4)	C26—C25—O15	109.29 (5)
C27—O16—C26	110.62 (5)	H2K—C25—O15	111.7 (9)
C11—N1—K1	107.32 (3)	H2K—C25—C26	109.2 (9)
C17—N1—K1	107.30 (4)	H2L—C25—O15	110.5 (9)
C17—N1—C11	110.14 (5)	H2L—C25—C26	110.4 (9)
C23—N1—K1	112.21 (4)	H2L—C25—H2K	105.8 (13)
C23—N1—C11	109.23 (5)	C25—C26—O16	109.54 (5)
C23—N1—C17	110.57 (5)	H2M—C26—O16	110.1 (9)
C16—N2—K1	109.82 (4)	H2M—C26—C25	111.1 (9)
C22—N2—K1	107.62 (4)	H2N—C26—O16	110.1 (9)
C22—N2—C16	109.42 (5)	H2N—C26—C25	108.1 (9)
C28—N2—K1	108.75 (4)	H2N—C26—H2M	107.9 (13)
C28—N2—C16	109.87 (5)	C28—C27—O16	110.54 (5)
C28—N2—C22	111.32 (5)	H2O—C27—O16	108.5 (9)
O1—C1—Cr1	177.05 (6)	H2O—C27—C28	112.2 (9)
O2—C2—Cr1	178.81 (6)	H2P—C27—O16	107.8 (9)
O3—C3—Cr1	176.01 (6)	H2P—C27—C28	108.0 (9)
O4—C4—Cr1	177.84 (6)	H2P—C27—H2O	109.6 (13)
O5—C5—Cr1	177.69 (6)	C27—C28—N2	114.07 (5)
O6—C6—Cr2	178.73 (6)	H2Q—C28—N2	111.7 (8)
O7—C7—Cr2	178.60 (6)	H2Q—C28—C27	107.4 (9)
O8—C8—Cr2	174.69 (6)	H2R—C28—N2	106.9 (8)
O9—C9—Cr2	178.61 (6)	H2R—C28—C27	107.9 (9)
O10—C10—Cr2	177.99 (6)	H2R—C28—H2Q	108.8 (13)
C12—C11—N1	114.58 (5)	Cr2—H—Cr1	147.4 (12)
K1—O11—C12—C11	−56.01 (4)	K1—N1—C23—C24	−37.46 (4)
K1—O11—C13—C14	53.15 (4)	K1—N2—C16—C15	−48.50 (4)
K1—O12—C14—C13	42.30 (4)	K1—N2—C22—C21	−39.24 (4)
K1—O12—C15—C16	−41.07 (4)	K1—N2—C28—C27	−48.58 (4)
K1—O13—C18—C17	−40.76 (4)	O11—C12—C11—N1	69.75 (6)
K1—O13—C19—C20	49.30 (4)	O11—C13—C14—O12	−63.32 (5)
K1—O14—C20—C19	47.81 (4)	O12—C15—C16—N2	60.68 (6)
K1—O14—C21—C22	−59.79 (4)	O13—C18—C17—N1	62.42 (6)
K1—O15—C24—C23	−56.01 (4)	O13—C19—C20—O14	−65.96 (6)
K1—O15—C25—C26	37.76 (4)	O14—C21—C22—N2	69.59 (5)
K1—O16—C26—C25	57.35 (4)	O15—C24—C23—N1	63.05 (6)
K1—O16—C27—C28	−39.20 (4)	O15—C25—C26—O16	−63.64 (5)
K1—N1—C11—C12	−41.21 (4)	O16—C27—C28—N2	60.54 (6)
K1—N1—C17—C18	−49.81 (4)

(KCPTCR_HAR_SHADE3_1)

Crystal data

C28H37Cr2KN2O16	F(000) = 1660.306
Mr = 800.70	Dx = 1.489 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71069 Å
a = 10.458 Å	Cell parameters from 1024 reflections
b = 14.417 Å	θ = 47.5–1.5°
c = 23.882 Å	µ = 0.80 mm^−1
β = 97.26°	T = 28 K
V = 3571.89 Å^3	Ellipsoidal, yellow
Z = 4	0.3 × 0.25 × 0.2 mm

Data collection

SMART CCD diffractometer	22531 reflections with I ≥ 2u(I)
ω scan	Rint = 0.0000
Absorption correction: empirical (using intensity measurements)	θmax = 48.7°, θmin = 2.4°
Tmin = 0.890, Tmax = 0.903	h = −19→20
27917 measured reflections	k = 0→30
27917 independent reflections	l = 0→50

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.031	Only H-atom coordinates refined
wR(F^2) = 0.100	w = 1/[σ^2(Fo^2) + (0.1P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 0.69	(Δ/σ)max = 0.0001
27917 reflections	Δρmax = 0.73 e Å^−3
553 parameters	Δρmin = −1.25 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Cr1	0.163876 (10)	0.002348 (6)	0.236375 (4)	0.005243 (17)
Cr2	0.018764 (10)	0.177450 (6)	0.165109 (4)	0.005809 (18)
K1	0.463713 (13)	0.199294 (8)	0.418000 (5)	0.00657 (2)
O1	0.25208 (6)	0.13810 (3)	0.33122 (2)	0.01184 (8)
O2	−0.08354 (6)	−0.04363 (4)	0.28576 (3)	0.01423 (9)
O3	0.10469 (6)	−0.12659 (4)	0.13548 (2)	0.01260 (8)
O4	0.39549 (6)	0.05450 (4)	0.17751 (3)	0.01366 (9)
O5	0.30038 (6)	−0.15033 (4)	0.30579 (2)	0.01236 (8)
O6	−0.25958 (6)	0.12167 (4)	0.17223 (2)	0.01235 (8)
O7	0.01686 (6)	0.05854 (4)	0.05958 (2)	0.01264 (8)
O8	0.28636 (6)	0.25364 (4)	0.15524 (2)	0.01343 (9)
O9	0.02671 (7)	0.26562 (4)	0.28173 (3)	0.01786 (11)
O10	−0.07205 (6)	0.34766 (4)	0.09922 (3)	0.01458 (9)
O11	0.28570 (5)	0.09215 (3)	0.47314 (2)	0.00784 (7)
O12	0.44346 (5)	0.00267 (3)	0.40246 (2)	0.00836 (7)
O13	0.31318 (5)	0.34097 (3)	0.36294 (2)	0.00878 (7)
O14	0.52819 (5)	0.26678 (3)	0.31528 (2)	0.00893 (7)
O15	0.55089 (5)	0.32676 (4)	0.50765 (2)	0.00929 (7)
O16	0.72730 (5)	0.20515 (3)	0.46498 (2)	0.00824 (7)
N1	0.27305 (6)	0.30199 (4)	0.47985 (2)	0.00785 (7)
N2	0.66187 (5)	0.09454 (3)	0.36195 (2)	0.00696 (7)
C1	0.21620 (7)	0.08861 (4)	0.29509 (3)	0.00816 (8)
C2	0.01010 (7)	−0.02689 (4)	0.26769 (3)	0.00879 (9)
C3	0.12292 (7)	−0.07914 (4)	0.17414 (3)	0.00849 (8)
C4	0.30807 (7)	0.03663 (4)	0.20003 (3)	0.00900 (9)
C5	0.25021 (7)	−0.09119 (4)	0.27863 (3)	0.00846 (8)
C6	−0.15453 (7)	0.14180 (4)	0.16996 (3)	0.00873 (9)
C7	0.01879 (7)	0.10405 (4)	0.09913 (3)	0.00830 (8)
C8	0.18817 (7)	0.22110 (4)	0.16012 (3)	0.00901 (9)
C9	0.02396 (7)	0.23368 (4)	0.23776 (3)	0.01109 (10)
C10	−0.03870 (7)	0.28241 (4)	0.12526 (3)	0.00937 (9)
C11	0.20814 (7)	0.23292 (4)	0.51163 (3)	0.00904 (9)
C12	0.17312 (6)	0.14345 (4)	0.47988 (3)	0.00867 (9)
C13	0.25204 (7)	0.00543 (4)	0.44642 (3)	0.00786 (8)
C14	0.37237 (7)	−0.04780 (4)	0.43910 (3)	0.00820 (8)
C15	0.54819 (6)	−0.04991 (4)	0.38673 (3)	0.00804 (8)
C16	0.60989 (7)	0.00369 (4)	0.34255 (3)	0.00813 (8)
C17	0.17934 (7)	0.34654 (4)	0.43701 (3)	0.00930 (9)
C18	0.24064 (7)	0.40165 (4)	0.39330 (3)	0.00975 (9)
C19	0.37488 (7)	0.38881 (4)	0.32182 (3)	0.01091 (10)
C20	0.42815 (7)	0.31883 (5)	0.28403 (3)	0.01082 (10)
C21	0.57213 (7)	0.19482 (4)	0.28134 (3)	0.00947 (9)
C22	0.69036 (7)	0.14948 (4)	0.31298 (3)	0.00920 (9)
C23	0.33591 (7)	0.37152 (4)	0.51924 (3)	0.01014 (9)
C24	0.46542 (7)	0.34035 (5)	0.54889 (3)	0.01029 (9)
C25	0.68009 (7)	0.31747 (4)	0.53319 (3)	0.00879 (9)
C26	0.76441 (7)	0.29313 (4)	0.48874 (3)	0.00917 (9)
C27	0.82388 (7)	0.16973 (4)	0.43397 (3)	0.00908 (9)
C28	0.77753 (6)	0.08188 (4)	0.40292 (3)	0.00838 (8)
H	0.0490 (17)	0.0760 (12)	0.1997 (8)	0.029921
H1A	0.1187 (16)	0.2623 (12)	0.5257 (7)	0.023023
H1B	0.2730 (15)	0.2160 (12)	0.5496 (7)	0.022016
H1C	0.1183 (16)	0.1564 (12)	0.4376 (6)	0.020440
H1D	0.1089 (15)	0.1022 (12)	0.5034 (7)	0.021942
H1E	0.1938 (16)	0.0154 (11)	0.4055 (7)	0.020147
H1F	0.1929 (15)	−0.0359 (11)	0.4720 (7)	0.021496
H1G	0.3426 (15)	−0.1157 (11)	0.4209 (7)	0.020240
H1H	0.4285 (15)	−0.0577 (11)	0.4805 (6)	0.020490
H1I	0.5126 (15)	−0.1160 (11)	0.3676 (7)	0.021436
H1J	0.6145 (15)	−0.0687 (11)	0.4236 (6)	0.021077
H1K	0.5376 (15)	0.0172 (11)	0.3063 (7)	0.020388
H1L	0.6863 (15)	−0.0389 (11)	0.3286 (7)	0.022019
H1M	0.1248 (16)	0.2925 (11)	0.4141 (7)	0.021287
H1N	0.1143 (15)	0.3919 (12)	0.4564 (7)	0.023007
H1O	0.1636 (16)	0.4349 (11)	0.3629 (7)	0.022432
H1P	0.3025 (15)	0.4572 (11)	0.4130 (7)	0.022225
H1Q	0.4499 (15)	0.4328 (11)	0.3433 (6)	0.021477
H1R	0.3066 (15)	0.4331 (11)	0.2959 (7)	0.021586
H2A	0.3502 (15)	0.2735 (11)	0.2659 (7)	0.019926
H2B	0.4677 (16)	0.3544 (11)	0.2496 (6)	0.021449
H2C	0.5960 (16)	0.2244 (12)	0.2412 (6)	0.021626
H2D	0.4959 (15)	0.1456 (11)	0.2691 (7)	0.020024
H2E	0.7372 (16)	0.1057 (12)	0.2835 (7)	0.022041
H2F	0.7572 (15)	0.2065 (11)	0.3273 (7)	0.021862
H2G	0.3549 (15)	0.4330 (11)	0.4962 (7)	0.022708
H2H	0.2735 (16)	0.3936 (12)	0.5519 (7)	0.023541
H2I	0.4571 (16)	0.2746 (12)	0.5744 (7)	0.021522
H2J	0.5069 (15)	0.3936 (12)	0.5789 (7)	0.022847
H2K	0.7154 (15)	0.3810 (11)	0.5544 (7)	0.022041
H2L	0.6877 (15)	0.2637 (12)	0.5664 (7)	0.021426
H2M	0.7582 (17)	0.3475 (11)	0.4550 (7)	0.021454
H2N	0.8639 (15)	0.2908 (12)	0.5088 (7)	0.021617
H2O	0.8498 (15)	0.2231 (11)	0.4058 (7)	0.021560
H2P	0.9105 (15)	0.1518 (12)	0.4652 (7)	0.022180
H2Q	0.8594 (15)	0.0541 (12)	0.3826 (7)	0.022814
H2R	0.7536 (15)	0.0328 (11)	0.4334 (6)	0.021435

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cr1	0.00570 (4)	0.00465 (3)	0.00536 (3)	0.00020 (2)	0.00060 (2)	−0.00015 (2)
Cr2	0.00680 (4)	0.00533 (3)	0.00515 (3)	0.00087 (2)	0.00021 (2)	0.00017 (2)
K1	0.00627 (5)	0.00672 (4)	0.00667 (4)	0.00020 (3)	0.00060 (3)	−0.00005 (3)
O1	0.0156 (2)	0.00918 (15)	0.00978 (19)	−0.00009 (15)	−0.00224 (15)	−0.00279 (13)
O2	0.0106 (2)	0.0167 (2)	0.0167 (2)	−0.00016 (17)	0.00651 (17)	0.00147 (17)
O3	0.0153 (2)	0.01229 (17)	0.01024 (19)	−0.00203 (16)	0.00162 (16)	−0.00501 (14)
O4	0.0110 (2)	0.01397 (18)	0.0173 (2)	−0.00093 (17)	0.00693 (17)	0.00010 (16)
O5	0.0136 (2)	0.00922 (15)	0.0135 (2)	0.00351 (15)	−0.00096 (16)	0.00255 (14)
O6	0.0096 (2)	0.01501 (18)	0.0130 (2)	−0.00105 (16)	0.00345 (15)	0.00016 (15)
O7	0.0169 (2)	0.01228 (17)	0.00905 (19)	−0.00136 (17)	0.00292 (16)	−0.00336 (14)
O8	0.0111 (2)	0.01615 (19)	0.0129 (2)	−0.00546 (17)	0.00069 (16)	0.00073 (16)
O9	0.0264 (3)	0.0174 (2)	0.0089 (2)	0.0097 (2)	−0.00110 (19)	−0.00490 (16)
O10	0.0179 (3)	0.00951 (16)	0.0152 (2)	0.00298 (16)	−0.00221 (18)	0.00424 (15)
O11	0.00643 (18)	0.00770 (13)	0.00933 (17)	−0.00020 (13)	0.00084 (13)	−0.00097 (12)
O12	0.00897 (19)	0.00666 (13)	0.00989 (18)	0.00077 (13)	0.00284 (14)	0.00105 (12)
O13	0.0096 (2)	0.00715 (13)	0.00986 (18)	0.00086 (13)	0.00237 (14)	0.00119 (12)
O14	0.0101 (2)	0.00884 (14)	0.00775 (17)	0.00180 (14)	0.00085 (13)	0.00055 (12)
O15	0.00756 (19)	0.01245 (17)	0.00768 (17)	0.00119 (14)	0.00030 (13)	−0.00176 (13)
O16	0.00613 (18)	0.00879 (14)	0.00987 (18)	−0.00101 (13)	0.00126 (13)	−0.00237 (12)
N1	0.0069 (2)	0.00793 (15)	0.00869 (19)	0.00124 (14)	0.00098 (14)	−0.00052 (13)
N2	0.0073 (2)	0.00699 (14)	0.00674 (18)	−0.00005 (14)	0.00132 (13)	−0.00013 (12)
C1	0.0096 (2)	0.00688 (16)	0.0076 (2)	0.00001 (16)	−0.00036 (16)	−0.00072 (14)
C2	0.0082 (2)	0.00898 (18)	0.0096 (2)	0.00043 (17)	0.00269 (17)	0.00052 (15)
C3	0.0093 (2)	0.00802 (17)	0.0081 (2)	−0.00032 (17)	0.00112 (16)	−0.00149 (15)
C4	0.0081 (2)	0.00919 (18)	0.0100 (2)	−0.00055 (17)	0.00255 (17)	−0.00040 (15)
C5	0.0088 (2)	0.00690 (17)	0.0094 (2)	0.00112 (16)	0.00023 (16)	0.00042 (15)
C6	0.0090 (2)	0.00949 (18)	0.0077 (2)	0.00081 (17)	0.00147 (16)	0.00023 (15)
C7	0.0095 (2)	0.00825 (17)	0.0072 (2)	−0.00036 (16)	0.00116 (16)	−0.00120 (15)
C8	0.0094 (2)	0.00888 (18)	0.0084 (2)	−0.00112 (17)	0.00013 (16)	0.00015 (15)
C9	0.0145 (3)	0.01029 (19)	0.0081 (2)	0.00385 (19)	−0.00014 (18)	−0.00181 (16)
C10	0.0112 (3)	0.00719 (17)	0.0093 (2)	0.00142 (17)	−0.00032 (17)	0.00140 (15)
C11	0.0094 (2)	0.00982 (18)	0.0082 (2)	0.00139 (17)	0.00226 (17)	−0.00031 (15)
C12	0.0066 (2)	0.00930 (18)	0.0103 (2)	0.00005 (16)	0.00157 (16)	0.00010 (15)
C13	0.0073 (2)	0.00795 (17)	0.0084 (2)	−0.00159 (16)	0.00149 (16)	−0.00033 (14)
C14	0.0096 (2)	0.00667 (16)	0.0086 (2)	−0.00029 (16)	0.00212 (16)	0.00076 (14)
C15	0.0078 (2)	0.00661 (16)	0.0097 (2)	0.00067 (16)	0.00126 (16)	0.00043 (15)
C16	0.0092 (2)	0.00758 (17)	0.0076 (2)	−0.00022 (16)	0.00121 (16)	−0.00078 (14)
C17	0.0074 (2)	0.01011 (19)	0.0105 (2)	0.00183 (17)	0.00168 (17)	0.00131 (16)
C18	0.0103 (3)	0.00774 (17)	0.0116 (2)	0.00190 (17)	0.00299 (18)	0.00151 (16)
C19	0.0125 (3)	0.00809 (18)	0.0127 (2)	0.00227 (18)	0.00389 (19)	0.00306 (16)
C20	0.0123 (3)	0.0118 (2)	0.0085 (2)	0.00293 (19)	0.00186 (18)	0.00318 (16)
C21	0.0121 (3)	0.00890 (18)	0.0073 (2)	0.00172 (18)	0.00096 (17)	0.00054 (15)
C22	0.0095 (2)	0.00970 (19)	0.0090 (2)	0.00107 (18)	0.00339 (17)	0.00167 (15)
C23	0.0087 (2)	0.00980 (19)	0.0118 (2)	0.00135 (17)	0.00070 (18)	−0.00332 (16)
C24	0.0080 (2)	0.0139 (2)	0.0089 (2)	0.00035 (19)	0.00083 (17)	−0.00298 (17)
C25	0.0083 (2)	0.00950 (18)	0.0083 (2)	−0.00050 (17)	0.00005 (16)	−0.00189 (15)
C26	0.0077 (2)	0.00891 (18)	0.0110 (2)	−0.00131 (17)	0.00133 (17)	−0.00201 (16)
C27	0.0073 (2)	0.00998 (19)	0.0100 (2)	−0.00081 (17)	0.00139 (16)	−0.00194 (16)
C28	0.0075 (2)	0.00832 (17)	0.0093 (2)	0.00082 (16)	0.00091 (16)	−0.00064 (15)
H	0.026290	0.023490	0.038610	0.003460	−0.001240	0.011980
H1A	0.017820	0.027050	0.025490	0.003500	0.007760	−0.004370
H1B	0.021170	0.027300	0.016190	−0.000740	−0.003040	0.001360
H1C	0.019760	0.025730	0.014770	0.003900	−0.001940	−0.000730
H1D	0.019570	0.025160	0.022480	−0.003390	0.008050	0.001390
H1E	0.021570	0.021640	0.015700	0.002370	−0.003600	0.000750
H1F	0.021710	0.021790	0.022180	−0.004980	0.007410	0.003180
H1G	0.024250	0.014390	0.021880	−0.002540	0.002140	−0.001160
H1H	0.018890	0.025310	0.016030	−0.000330	−0.002620	0.004520
H1I	0.023620	0.014700	0.026080	−0.001330	0.003500	−0.003730
H1J	0.018640	0.024620	0.018910	0.005010	−0.001760	0.002570
H1K	0.019210	0.021460	0.018930	−0.000080	−0.003680	0.001470
H1L	0.019100	0.020910	0.027180	0.004670	0.007330	−0.003990
H1M	0.021810	0.019650	0.021050	−0.002900	−0.002550	−0.002970
H1N	0.022540	0.024800	0.022240	0.008720	0.005010	−0.004240
H1O	0.022460	0.022100	0.021570	0.007430	−0.001760	0.001380
H1P	0.023610	0.017640	0.024950	−0.002890	0.001220	−0.006520
H1Q	0.023340	0.019560	0.020860	−0.007390	0.000180	−0.002760
H1R	0.023180	0.018730	0.021920	0.004550	−0.000760	0.004000
H2A	0.018400	0.015870	0.024430	−0.003500	−0.001490	−0.002080
H2B	0.025450	0.021570	0.018040	−0.001490	0.005520	0.005190
H2C	0.024880	0.024790	0.016260	0.000380	0.006690	0.003650
H2D	0.016430	0.018400	0.025110	−0.003810	0.002110	−0.004270
H2E	0.022510	0.024870	0.019950	0.004210	0.007380	−0.003420
H2F	0.019850	0.022430	0.022610	−0.007340	−0.000030	−0.000770
H2G	0.026040	0.018650	0.022510	−0.001220	−0.000530	0.001350
H2H	0.020050	0.030410	0.020750	0.003500	0.004860	−0.008200
H2I	0.022340	0.021250	0.021620	0.001760	0.005280	0.003480
H2J	0.021520	0.025440	0.020820	−0.001020	−0.000290	−0.009450
H2K	0.021500	0.020400	0.023550	−0.002650	0.000230	−0.007210
H2L	0.020370	0.023980	0.019810	0.000570	0.002080	0.005640
H2M	0.027810	0.018690	0.017750	−0.002200	0.002440	0.002340
H2N	0.013980	0.026010	0.023980	−0.000700	−0.001030	−0.003050
H2O	0.023470	0.021050	0.021220	−0.002050	0.006950	0.002120
H2P	0.014520	0.029010	0.021960	0.002500	−0.001780	−0.002580
H2Q	0.016150	0.028860	0.024060	0.004080	0.004990	−0.006060
H2R	0.021840	0.021330	0.020670	−0.001820	0.000880	0.004530

Geometric parameters (Å, º)

Cr1—C1	1.9022 (6)	N2—C22	1.4737 (8)
Cr1—C2	1.9044 (7)	N2—C28	1.4678 (9)
Cr1—C3	1.9006 (6)	C11—C12	1.5176 (9)
Cr1—C4	1.8981 (7)	C11—H1A	1.117 (16)
Cr1—C5	1.8498 (6)	C11—H1B	1.090 (15)
Cr1—H	1.752 (17)	C12—H1C	1.112 (15)
Cr2—C6	1.9013 (7)	C12—H1D	1.102 (15)
Cr2—C7	1.8980 (6)	C13—C14	1.5029 (9)
Cr2—C8	1.8980 (7)	C13—H1E	1.094 (15)
Cr2—C9	1.9097 (7)	C13—H1F	1.098 (15)
Cr2—C10	1.8473 (6)	C14—H1G	1.100 (15)
Cr2—H	1.690 (17)	C14—H1H	1.093 (14)
K1—O1	2.9687 (6)	C15—C16	1.5161 (9)
K1—O11	2.8646 (5)	C15—H1I	1.102 (15)
K1—O12	2.8633 (5)	C15—H1J	1.085 (15)
K1—O13	2.8029 (5)	C16—H1K	1.093 (15)
K1—O14	2.7995 (5)	C16—H1L	1.093 (15)
K1—O15	2.8809 (5)	C17—C18	1.5169 (9)
K1—O16	2.8430 (5)	C17—H1M	1.074 (15)
K1—N1	3.0156 (6)	C17—H1N	1.087 (15)
K1—N2	3.0114 (6)	C18—H1O	1.121 (15)
O1—C1	1.1457 (8)	C18—H1P	1.098 (15)
O2—C2	1.1447 (9)	C19—C20	1.5066 (10)
O3—C3	1.1455 (8)	C19—H1Q	1.085 (15)
O4—C4	1.1470 (9)	C19—H1R	1.091 (15)
O5—C5	1.1563 (8)	C20—H2A	1.091 (15)
O6—C6	1.1442 (9)	C20—H2B	1.093 (15)
O7—C7	1.1483 (8)	C21—C22	1.5137 (10)
O8—C8	1.1482 (9)	C21—H2C	1.106 (15)
O9—C9	1.1436 (9)	C21—H2D	1.079 (15)
O10—C10	1.1568 (8)	C22—H2E	1.105 (15)
O11—C12	1.4167 (8)	C22—H2F	1.105 (15)
O11—C13	1.4275 (7)	C23—C24	1.5151 (10)
O12—C14	1.4185 (8)	C23—H2G	1.074 (16)
O12—C15	1.4212 (8)	C23—H2H	1.124 (16)
O13—C18	1.4163 (8)	C24—H2I	1.136 (16)
O13—C19	1.4201 (8)	C24—H2J	1.102 (15)
O14—C20	1.4204 (8)	C25—C26	1.5048 (9)
O14—C21	1.4279 (8)	C25—H2K	1.088 (15)
O15—C24	1.4246 (8)	C25—H2L	1.105 (16)
O15—C25	1.4168 (9)	C26—H2M	1.119 (16)
O16—C26	1.4233 (7)	C26—H2N	1.090 (15)
O16—C27	1.4208 (8)	C27—C28	1.5160 (9)
N1—C11	1.4693 (8)	C27—H2O	1.078 (15)
N1—C17	1.4718 (9)	C27—H2P	1.129 (15)
N1—C23	1.4717 (8)	C28—H2Q	1.111 (15)
N2—C16	1.4704 (8)	C28—H2R	1.066 (15)
C2—Cr1—C1	91.94 (3)	H1A—C11—N1	111.0 (9)
C3—Cr1—C1	174.91 (3)	H1A—C11—C12	108.4 (9)
C3—Cr1—C2	92.99 (3)	H1B—C11—N1	107.6 (9)
C4—Cr1—C1	89.76 (3)	H1B—C11—C12	108.1 (9)
C4—Cr1—C2	175.07 (3)	H1B—C11—H1A	106.9 (13)
C4—Cr1—C3	85.23 (3)	C11—C12—O11	110.42 (5)
C5—Cr1—C1	89.96 (3)	H1C—C12—O11	109.0 (8)
C5—Cr1—C2	90.15 (3)	H1C—C12—C11	112.0 (9)
C5—Cr1—C3	91.28 (3)	H1D—C12—O11	110.2 (9)
C5—Cr1—C4	94.48 (3)	H1D—C12—C11	109.1 (9)
H—Cr1—C1	95.0 (6)	H1D—C12—H1C	106.1 (12)
H—Cr1—C2	76.7 (6)	C14—C13—O11	109.65 (5)
H—Cr1—C3	84.9 (6)	H1E—C13—O11	111.2 (8)
H—Cr1—C4	98.5 (6)	H1E—C13—C14	110.1 (9)
H—Cr1—C5	166.1 (6)	H1F—C13—O11	110.5 (9)
C7—Cr2—C6	90.00 (3)	H1F—C13—C14	109.0 (9)
C8—Cr2—C6	176.32 (3)	H1F—C13—H1E	106.3 (13)
C8—Cr2—C7	91.99 (3)	C13—C14—O12	108.76 (5)
C9—Cr2—C6	88.70 (3)	H1G—C14—O12	110.9 (8)
C9—Cr2—C7	171.10 (3)	H1G—C14—C13	107.5 (8)
C9—Cr2—C8	89.81 (3)	H1H—C14—O12	111.1 (8)
C10—Cr2—C6	90.13 (3)	H1H—C14—C13	108.9 (9)
C10—Cr2—C7	93.62 (3)	H1H—C14—H1G	109.5 (12)
C10—Cr2—C8	86.65 (3)	C16—C15—O12	108.80 (5)
C10—Cr2—C9	95.19 (3)	H1I—C15—O12	109.9 (8)
H—Cr2—C6	81.8 (6)	H1I—C15—C16	107.6 (9)
H—Cr2—C7	84.5 (7)	H1J—C15—O12	110.7 (8)
H—Cr2—C8	101.5 (6)	H1J—C15—C16	114.1 (9)
H—Cr2—C9	86.6 (7)	H1J—C15—H1I	105.6 (12)
H—Cr2—C10	171.7 (6)	C15—C16—N2	114.05 (5)
O11—K1—O1	71.953 (15)	H1K—C16—N2	106.4 (8)
O12—K1—O1	65.096 (15)	H1K—C16—C15	109.2 (9)
O12—K1—O11	58.933 (14)	H1L—C16—N2	109.9 (9)
O13—K1—O1	64.152 (15)	H1L—C16—C15	108.5 (9)
O13—K1—O11	104.449 (15)	H1L—C16—H1K	108.6 (13)
O13—K1—O12	129.248 (16)	C18—C17—N1	113.87 (6)
O14—K1—O1	74.477 (16)	H1M—C17—N1	107.6 (8)
O14—K1—O11	146.381 (15)	H1M—C17—C18	105.8 (9)
O14—K1—O12	104.630 (14)	H1N—C17—N1	111.4 (8)
O14—K1—O13	61.238 (14)	H1N—C17—C18	108.6 (9)
O15—K1—O1	147.826 (16)	H1N—C17—H1M	109.4 (13)
O15—K1—O11	99.517 (15)	C17—C18—O13	109.22 (5)
O15—K1—O12	137.659 (15)	H1O—C18—O13	108.7 (8)
O15—K1—O13	89.431 (15)	H1O—C18—C17	109.7 (9)
O15—K1—O14	109.933 (15)	H1P—C18—O13	110.2 (8)
O16—K1—O1	152.187 (15)	H1P—C18—C17	111.4 (9)
O16—K1—O11	119.252 (15)	H1P—C18—H1O	107.5 (12)
O16—K1—O12	97.627 (15)	C20—C19—O13	108.89 (5)
O16—K1—O13	128.505 (15)	H1Q—C19—O13	108.8 (8)
O16—K1—O14	90.377 (15)	H1Q—C19—C20	111.9 (9)
O16—K1—O15	59.188 (14)	H1R—C19—O13	110.8 (8)
N1—K1—O1	90.404 (16)	H1R—C19—C20	108.5 (9)
N1—K1—O11	62.046 (14)	H1R—C19—H1Q	108.0 (12)
N1—K1—O12	120.455 (15)	C19—C20—O14	110.03 (6)
N1—K1—O13	60.335 (15)	H2A—C20—O14	110.8 (8)
N1—K1—O14	120.395 (15)	H2A—C20—C19	109.0 (9)
N1—K1—O15	59.305 (15)	H2B—C20—O14	108.6 (8)
N1—K1—O16	117.406 (15)	H2B—C20—C19	109.9 (9)
N2—K1—O1	91.998 (15)	H2B—C20—H2A	108.5 (12)
N2—K1—O11	117.233 (14)	C22—C21—O14	109.36 (5)
N2—K1—O12	59.315 (14)	H2C—C21—O14	109.6 (9)
N2—K1—O13	122.289 (15)	H2C—C21—C22	109.9 (8)
N2—K1—O14	61.920 (14)	H2D—C21—O14	110.6 (8)
N2—K1—O15	118.644 (15)	H2D—C21—C22	112.3 (8)
N2—K1—O16	60.193 (14)	H2D—C21—H2C	105.0 (12)
N2—K1—N1	177.090 (15)	C21—C22—N2	113.21 (6)
C1—O1—K1	148.78 (5)	H2E—C22—N2	110.4 (9)
C12—O11—K1	111.62 (4)	H2E—C22—C21	109.2 (8)
C13—O11—K1	113.87 (4)	H2F—C22—N2	109.7 (8)
C13—O11—C12	110.27 (5)	H2F—C22—C21	106.2 (9)
C14—O12—K1	117.64 (3)	H2F—C22—H2E	108.0 (12)
C15—O12—K1	121.03 (4)	C24—C23—N1	113.42 (5)
C15—O12—C14	111.78 (5)	H2G—C23—N1	109.4 (8)
C18—O13—K1	121.02 (4)	H2G—C23—C24	105.8 (9)
C19—O13—K1	113.64 (4)	H2H—C23—N1	112.6 (9)
C19—O13—C18	111.94 (5)	H2H—C23—C24	108.8 (8)
C20—O14—K1	113.65 (4)	H2H—C23—H2G	106.3 (13)
C21—O14—K1	112.05 (4)	C23—C24—O15	108.64 (5)
C21—O14—C20	110.73 (5)	H2I—C24—O15	110.7 (8)
C24—O15—K1	115.73 (4)	H2I—C24—C23	112.0 (8)
C25—O15—K1	117.04 (4)	H2J—C24—O15	108.4 (9)
C25—O15—C24	111.28 (5)	H2J—C24—C23	110.7 (8)
C26—O16—K1	112.69 (4)	H2J—C24—H2I	106.4 (12)
C27—O16—K1	120.09 (4)	C26—C25—O15	109.29 (5)
C27—O16—C26	110.62 (5)	H2K—C25—O15	111.7 (8)
C11—N1—K1	107.31 (3)	H2K—C25—C26	109.3 (9)
C17—N1—K1	107.30 (4)	H2L—C25—O15	110.7 (8)
C17—N1—C11	110.14 (5)	H2L—C25—C26	110.3 (9)
C23—N1—K1	112.21 (4)	H2L—C25—H2K	105.5 (12)
C23—N1—C11	109.24 (5)	C25—C26—O16	109.54 (5)
C23—N1—C17	110.57 (5)	H2M—C26—O16	110.4 (8)
C16—N2—K1	109.82 (4)	H2M—C26—C25	111.0 (9)
C22—N2—K1	107.61 (4)	H2N—C26—O16	110.2 (9)
C22—N2—C16	109.42 (5)	H2N—C26—C25	108.0 (9)
C28—N2—K1	108.75 (4)	H2N—C26—H2M	107.6 (13)
C28—N2—C16	109.88 (5)	C28—C27—O16	110.53 (5)
C28—N2—C22	111.32 (5)	H2O—C27—O16	108.6 (9)
O1—C1—Cr1	177.05 (6)	H2O—C27—C28	112.4 (9)
O2—C2—Cr1	178.81 (6)	H2P—C27—O16	107.5 (8)
O3—C3—Cr1	176.01 (6)	H2P—C27—C28	108.2 (8)
O4—C4—Cr1	177.84 (6)	H2P—C27—H2O	109.4 (12)
O5—C5—Cr1	177.69 (6)	C27—C28—N2	114.07 (5)
O6—C6—Cr2	178.73 (6)	H2Q—C28—N2	111.7 (8)
O7—C7—Cr2	178.60 (6)	H2Q—C28—C27	107.4 (9)
O8—C8—Cr2	174.69 (6)	H2R—C28—N2	107.0 (8)
O9—C9—Cr2	178.61 (6)	H2R—C28—C27	108.0 (9)
O10—C10—Cr2	177.99 (6)	H2R—C28—H2Q	108.6 (13)
C12—C11—N1	114.58 (5)	Cr2—H—Cr1	147.4 (11)
K1—O11—C12—C11	−56.01 (4)	K1—N1—C23—C24	−37.47 (4)
K1—O11—C13—C14	53.14 (4)	K1—N2—C16—C15	−48.50 (4)
K1—O12—C14—C13	42.30 (4)	K1—N2—C22—C21	−39.24 (4)
K1—O12—C15—C16	−41.08 (4)	K1—N2—C28—C27	−48.58 (4)
K1—O13—C18—C17	−40.76 (4)	O11—C12—C11—N1	69.76 (6)
K1—O13—C19—C20	49.32 (4)	O11—C13—C14—O12	−63.32 (5)
K1—O14—C20—C19	47.82 (4)	O12—C15—C16—N2	60.69 (6)
K1—O14—C21—C22	−59.79 (4)	O13—C18—C17—N1	62.43 (6)
K1—O15—C24—C23	−56.01 (4)	O13—C19—C20—O14	−65.97 (6)
K1—O15—C25—C26	37.76 (4)	O14—C21—C22—N2	69.59 (5)
K1—O16—C26—C25	57.35 (4)	O15—C24—C23—N1	63.06 (6)
K1—O16—C27—C28	−39.20 (4)	O15—C25—C26—O16	−63.64 (5)
K1—N1—C11—C12	−41.22 (4)	O16—C27—C28—N2	60.54 (6)
K1—N1—C17—C18	−49.82 (4)

(KCPTCR_HAR_SHADE3)

Crystal data

4(C28H37Cr2KN2O16)	F(000) = 1660.306
Mr = 3202.80	Dx = 1.489 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71069 Å
a = 10.458 Å	Cell parameters from 1024 reflections
b = 14.417 Å	θ = 47.5–1.5°
c = 23.882 Å	µ = 0.80 mm^−1
β = 97.26°	T = 28 K
V = 3571.89 Å^3	Ellipsoidal, yellow
Z = 1	0.3 × 0.25 × 0.2 mm

Data collection

SMART CCD diffractometer	22531 reflections with I ≥ 2u(I)
ω scan	Rint = 0.0000
Absorption correction: empirical (using intensity measurements)	θmax = 48.7°, θmin = 2.4°
Tmin = 0.890, Tmax = 0.903	h = −19→20
27917 measured reflections	k = 0→30
27917 independent reflections	l = 0→50

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.031	Only H-atom coordinates refined
wR(F^2) = 0.100	w = 1/[σ^2(Fo^2) + (0.1P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 0.69	(Δ/σ)max = 0.0002
27917 reflections	Δρmax = 0.73 e Å^−3
553 parameters	Δρmin = −1.26 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Cr1	0.163876 (10)	0.002348 (6)	0.236375 (4)	0.005243 (17)
Cr2	0.018763 (10)	0.177450 (6)	0.165108 (4)	0.005808 (18)
K1	0.463713 (13)	0.199294 (8)	0.418000 (5)	0.00657 (2)
O1	0.25208 (6)	0.13810 (3)	0.33122 (2)	0.01184 (8)
O2	−0.08354 (6)	−0.04363 (4)	0.28576 (3)	0.01423 (9)
O3	0.10469 (6)	−0.12659 (4)	0.13548 (2)	0.01260 (8)
O4	0.39548 (6)	0.05450 (4)	0.17751 (3)	0.01365 (9)
O5	0.30038 (6)	−0.15033 (4)	0.30579 (2)	0.01236 (8)
O6	−0.25957 (6)	0.12167 (4)	0.17223 (2)	0.01235 (8)
O7	0.01686 (6)	0.05854 (4)	0.05957 (2)	0.01264 (8)
O8	0.28636 (6)	0.25364 (4)	0.15524 (2)	0.01343 (9)
O9	0.02670 (7)	0.26562 (4)	0.28173 (3)	0.01786 (11)
O10	−0.07205 (6)	0.34765 (4)	0.09923 (3)	0.01457 (9)
O11	0.28570 (5)	0.09215 (3)	0.47314 (2)	0.00784 (7)
O12	0.44346 (5)	0.00267 (3)	0.40246 (2)	0.00837 (7)
O13	0.31318 (5)	0.34097 (3)	0.36294 (2)	0.00878 (7)
O14	0.52819 (5)	0.26678 (3)	0.31528 (2)	0.00893 (7)
O15	0.55089 (5)	0.32677 (4)	0.50766 (2)	0.00929 (7)
O16	0.72730 (5)	0.20516 (3)	0.46498 (2)	0.00824 (7)
N1	0.27305 (6)	0.30199 (4)	0.47985 (2)	0.00785 (7)
N2	0.66188 (5)	0.09454 (3)	0.36195 (2)	0.00696 (7)
C1	0.21620 (7)	0.08861 (4)	0.29509 (3)	0.00816 (8)
C2	0.01010 (7)	−0.02689 (4)	0.26769 (3)	0.00879 (9)
C3	0.12292 (7)	−0.07914 (4)	0.17414 (3)	0.00849 (8)
C4	0.30806 (7)	0.03662 (4)	0.20002 (3)	0.00900 (9)
C5	0.25021 (7)	−0.09119 (4)	0.27863 (3)	0.00846 (8)
C6	−0.15452 (7)	0.14180 (4)	0.16996 (3)	0.00873 (9)
C7	0.01879 (7)	0.10405 (4)	0.09913 (3)	0.00830 (8)
C8	0.18817 (7)	0.22110 (4)	0.16012 (3)	0.00901 (9)
C9	0.02396 (7)	0.23368 (4)	0.23776 (3)	0.01108 (10)
C10	−0.03870 (7)	0.28241 (4)	0.12526 (3)	0.00937 (9)
C11	0.20814 (7)	0.23292 (4)	0.51164 (3)	0.00904 (9)
C12	0.17312 (6)	0.14345 (4)	0.47988 (3)	0.00866 (9)
C13	0.25204 (7)	0.00543 (4)	0.44642 (3)	0.00785 (8)
C14	0.37236 (7)	−0.04780 (4)	0.43910 (3)	0.00820 (8)
C15	0.54819 (6)	−0.04991 (4)	0.38672 (3)	0.00804 (8)
C16	0.60990 (7)	0.00369 (4)	0.34255 (3)	0.00813 (8)
C17	0.17934 (7)	0.34655 (4)	0.43701 (3)	0.00930 (9)
C18	0.24064 (7)	0.40165 (4)	0.39331 (3)	0.00975 (9)
C19	0.37488 (7)	0.38881 (4)	0.32182 (3)	0.01090 (10)
C20	0.42815 (7)	0.31883 (5)	0.28403 (3)	0.01081 (10)
C21	0.57213 (7)	0.19482 (4)	0.28134 (3)	0.00947 (9)
C22	0.69036 (7)	0.14948 (4)	0.31299 (3)	0.00920 (9)
C23	0.33591 (7)	0.37152 (4)	0.51924 (3)	0.01013 (9)
C24	0.46542 (7)	0.34035 (5)	0.54889 (3)	0.01029 (9)
C25	0.68009 (7)	0.31747 (4)	0.53319 (3)	0.00878 (9)
C26	0.76441 (7)	0.29313 (4)	0.48874 (3)	0.00917 (9)
C27	0.82388 (7)	0.16973 (4)	0.43397 (3)	0.00908 (9)
C28	0.77753 (6)	0.08188 (4)	0.40292 (3)	0.00838 (8)
H	0.0490 (17)	0.0763 (12)	0.1998 (8)	0.029887
H1A	0.1188 (16)	0.2621 (12)	0.5258 (7)	0.023252
H1B	0.2730 (15)	0.2159 (12)	0.5495 (7)	0.022070
H1C	0.1178 (16)	0.1564 (12)	0.4374 (6)	0.020331
H1D	0.1089 (15)	0.1022 (12)	0.5033 (7)	0.022071
H1E	0.1940 (16)	0.0155 (11)	0.4055 (7)	0.020019
H1F	0.1928 (16)	−0.0361 (11)	0.4721 (7)	0.021652
H1G	0.3427 (15)	−0.1159 (11)	0.4209 (7)	0.020315
H1H	0.4288 (15)	−0.0578 (11)	0.4807 (6)	0.020580
H1I	0.5123 (16)	−0.1160 (11)	0.3674 (7)	0.021564
H1J	0.6145 (15)	−0.0685 (11)	0.4238 (6)	0.021149
H1K	0.5373 (15)	0.0171 (11)	0.3062 (7)	0.020351
H1L	0.6859 (15)	−0.0390 (11)	0.3285 (7)	0.022207
H1M	0.1246 (16)	0.2924 (11)	0.4141 (7)	0.021184
H1N	0.1142 (15)	0.3917 (12)	0.4562 (7)	0.023194
H1O	0.1638 (16)	0.4349 (11)	0.3630 (7)	0.022433
H1P	0.3025 (15)	0.4573 (11)	0.4130 (7)	0.022338
H1Q	0.4498 (15)	0.4327 (11)	0.3432 (6)	0.021604
H1R	0.3071 (15)	0.4329 (11)	0.2960 (7)	0.021628
H2A	0.3500 (15)	0.2733 (11)	0.2658 (7)	0.019770
H2B	0.4677 (16)	0.3543 (11)	0.2495 (6)	0.021561
H2C	0.5961 (16)	0.2243 (12)	0.2413 (7)	0.021867
H2D	0.4957 (15)	0.1455 (11)	0.2690 (7)	0.019958
H2E	0.7370 (16)	0.1057 (12)	0.2835 (7)	0.022329
H2F	0.7570 (15)	0.2063 (11)	0.3273 (7)	0.022019
H2G	0.3548 (16)	0.4333 (11)	0.4963 (7)	0.022903
H2H	0.2737 (16)	0.3936 (12)	0.5517 (7)	0.023787
H2I	0.4571 (16)	0.2743 (12)	0.5743 (7)	0.021688
H2J	0.5068 (15)	0.3936 (12)	0.5789 (7)	0.023228
H2K	0.7152 (15)	0.3807 (11)	0.5544 (7)	0.022421
H2L	0.6873 (15)	0.2635 (12)	0.5663 (7)	0.021569
H2M	0.7580 (17)	0.3472 (11)	0.4550 (7)	0.021680
H2N	0.8634 (15)	0.2907 (12)	0.5086 (7)	0.021950
H2O	0.8495 (15)	0.2227 (11)	0.4059 (7)	0.021759
H2P	0.9110 (15)	0.1515 (12)	0.4653 (7)	0.022440
H2Q	0.8593 (15)	0.0541 (12)	0.3827 (7)	0.023097
H2R	0.7534 (15)	0.0326 (11)	0.4337 (6)	0.021440

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cr1	0.00569 (4)	0.00465 (3)	0.00536 (3)	0.00020 (2)	0.00060 (2)	−0.00015 (2)
Cr2	0.00680 (4)	0.00533 (3)	0.00515 (3)	0.00087 (2)	0.00021 (2)	0.00017 (2)
K1	0.00627 (5)	0.00672 (4)	0.00667 (4)	0.00020 (3)	0.00060 (3)	−0.00005 (3)
O1	0.0156 (2)	0.00918 (15)	0.00978 (19)	−0.00008 (15)	−0.00224 (15)	−0.00277 (13)
O2	0.0106 (2)	0.0167 (2)	0.0166 (2)	−0.00016 (17)	0.00649 (17)	0.00147 (17)
O3	0.0153 (2)	0.01229 (17)	0.01024 (19)	−0.00203 (16)	0.00161 (16)	−0.00502 (14)
O4	0.0110 (2)	0.01398 (18)	0.0173 (2)	−0.00094 (17)	0.00695 (17)	0.00011 (16)
O5	0.0136 (2)	0.00922 (15)	0.0135 (2)	0.00351 (15)	−0.00095 (16)	0.00255 (14)
O6	0.0095 (2)	0.01503 (18)	0.0130 (2)	−0.00106 (16)	0.00346 (15)	0.00016 (15)
O7	0.0169 (2)	0.01229 (17)	0.00906 (19)	−0.00135 (17)	0.00292 (16)	−0.00336 (14)
O8	0.0111 (2)	0.01614 (19)	0.0129 (2)	−0.00546 (17)	0.00069 (16)	0.00073 (16)
O9	0.0264 (3)	0.0174 (2)	0.0090 (2)	0.0097 (2)	−0.00110 (19)	−0.00489 (16)
O10	0.0179 (3)	0.00947 (16)	0.0152 (2)	0.00299 (16)	−0.00221 (18)	0.00426 (15)
O11	0.00644 (18)	0.00770 (13)	0.00933 (17)	−0.00021 (13)	0.00084 (13)	−0.00097 (12)
O12	0.00898 (19)	0.00666 (13)	0.00988 (18)	0.00075 (13)	0.00284 (14)	0.00106 (12)
O13	0.0096 (2)	0.00715 (13)	0.00985 (18)	0.00085 (13)	0.00236 (14)	0.00118 (12)
O14	0.0101 (2)	0.00884 (14)	0.00774 (17)	0.00179 (14)	0.00086 (13)	0.00055 (12)
O15	0.00758 (19)	0.01243 (17)	0.00768 (17)	0.00119 (14)	0.00031 (13)	−0.00175 (13)
O16	0.00611 (18)	0.00882 (14)	0.00986 (18)	−0.00098 (13)	0.00127 (13)	−0.00235 (12)
N1	0.0069 (2)	0.00793 (15)	0.00870 (19)	0.00123 (14)	0.00099 (14)	−0.00051 (13)
N2	0.0073 (2)	0.00697 (14)	0.00675 (18)	−0.00005 (14)	0.00131 (13)	−0.00015 (12)
C1	0.0096 (2)	0.00688 (16)	0.0076 (2)	0.00001 (16)	−0.00036 (16)	−0.00072 (14)
C2	0.0082 (2)	0.00897 (18)	0.0096 (2)	0.00043 (17)	0.00269 (17)	0.00052 (15)
C3	0.0093 (2)	0.00801 (17)	0.0081 (2)	−0.00032 (17)	0.00112 (16)	−0.00150 (15)
C4	0.0081 (2)	0.00919 (18)	0.0100 (2)	−0.00055 (17)	0.00255 (17)	−0.00040 (15)
C5	0.0088 (2)	0.00690 (17)	0.0094 (2)	0.00112 (16)	0.00023 (16)	0.00042 (15)
C6	0.0090 (2)	0.00949 (18)	0.0078 (2)	0.00081 (17)	0.00148 (16)	0.00023 (15)
C7	0.0095 (2)	0.00825 (17)	0.0072 (2)	−0.00036 (16)	0.00117 (16)	−0.00120 (15)
C8	0.0094 (2)	0.00888 (18)	0.0084 (2)	−0.00111 (17)	0.00012 (16)	0.00015 (15)
C9	0.0145 (3)	0.01029 (19)	0.0081 (2)	0.00386 (19)	−0.00014 (18)	−0.00180 (16)
C10	0.0112 (3)	0.00719 (17)	0.0093 (2)	0.00141 (17)	−0.00032 (17)	0.00141 (15)
C11	0.0094 (2)	0.00981 (18)	0.0082 (2)	0.00139 (17)	0.00224 (17)	−0.00032 (15)
C12	0.0066 (2)	0.00933 (18)	0.0102 (2)	0.00007 (16)	0.00154 (16)	0.00012 (15)
C13	0.0073 (2)	0.00796 (17)	0.0084 (2)	−0.00158 (16)	0.00150 (16)	−0.00032 (14)
C14	0.0096 (2)	0.00668 (16)	0.0086 (2)	−0.00029 (16)	0.00210 (16)	0.00076 (14)
C15	0.0078 (2)	0.00661 (16)	0.0097 (2)	0.00067 (16)	0.00125 (16)	0.00042 (15)
C16	0.0092 (2)	0.00760 (17)	0.0076 (2)	−0.00021 (16)	0.00120 (16)	−0.00077 (14)
C17	0.0074 (2)	0.01011 (19)	0.0105 (2)	0.00182 (17)	0.00168 (17)	0.00129 (16)
C18	0.0103 (3)	0.00774 (17)	0.0116 (2)	0.00190 (17)	0.00298 (18)	0.00150 (16)
C19	0.0125 (3)	0.00808 (18)	0.0127 (2)	0.00226 (18)	0.00390 (19)	0.00305 (16)
C20	0.0123 (3)	0.0118 (2)	0.0085 (2)	0.00290 (19)	0.00185 (18)	0.00318 (16)
C21	0.0121 (3)	0.00890 (18)	0.0073 (2)	0.00168 (18)	0.00095 (17)	0.00053 (15)
C22	0.0095 (2)	0.00970 (19)	0.0089 (2)	0.00108 (18)	0.00340 (17)	0.00169 (15)
C23	0.0087 (2)	0.00978 (19)	0.0118 (2)	0.00133 (17)	0.00069 (18)	−0.00331 (16)
C24	0.0080 (2)	0.0139 (2)	0.0089 (2)	0.00035 (19)	0.00083 (17)	−0.00296 (17)
C25	0.0083 (2)	0.00950 (18)	0.0083 (2)	−0.00050 (17)	0.00004 (16)	−0.00187 (15)
C26	0.0077 (2)	0.00888 (18)	0.0110 (2)	−0.00132 (17)	0.00133 (17)	−0.00204 (16)
C27	0.0073 (2)	0.00998 (19)	0.0100 (2)	−0.00080 (17)	0.00137 (16)	−0.00196 (16)
C28	0.0075 (2)	0.00831 (17)	0.0093 (2)	0.00081 (16)	0.00092 (16)	−0.00060 (15)
H	0.026370	0.023490	0.038400	0.003390	−0.001360	0.011980
H1A	0.018040	0.027600	0.025410	0.003440	0.007780	−0.004630
H1B	0.021450	0.027330	0.016020	−0.000860	−0.003120	0.001260
H1C	0.019780	0.025580	0.014580	0.003710	−0.001930	−0.000790
H1D	0.019850	0.025480	0.022280	−0.003710	0.008100	0.001400
H1E	0.021680	0.021420	0.015420	0.002150	−0.003640	0.000680
H1F	0.022150	0.022020	0.021960	−0.005410	0.007360	0.003260
H1G	0.024820	0.014140	0.021720	−0.002730	0.001910	−0.001170
H1H	0.019400	0.025230	0.015810	−0.000510	−0.002840	0.004560
H1I	0.024240	0.014510	0.025960	−0.001250	0.003240	−0.003760
H1J	0.019040	0.024540	0.018740	0.005090	−0.002000	0.002590
H1K	0.019340	0.021480	0.018670	0.000020	−0.003680	0.001540
H1L	0.019410	0.021150	0.027160	0.005020	0.007220	−0.003980
H1M	0.021630	0.019660	0.020920	−0.003050	−0.002540	−0.003040
H1N	0.022650	0.025000	0.022450	0.008790	0.004870	−0.004580
H1O	0.022370	0.021910	0.021810	0.007380	−0.001920	0.001400
H1P	0.023580	0.017510	0.025380	−0.002950	0.000970	−0.006650
H1Q	0.023190	0.019480	0.021420	−0.007590	0.000010	−0.002560
H1R	0.023010	0.018620	0.022290	0.004490	−0.000890	0.004220
H2A	0.018060	0.015820	0.024370	−0.003440	−0.001450	−0.001890
H2B	0.025210	0.021870	0.018340	−0.001590	0.005620	0.005630
H2C	0.024880	0.025310	0.016490	0.000420	0.006820	0.004090
H2D	0.016340	0.018400	0.025010	−0.003620	0.002130	−0.004080
H2E	0.022530	0.025510	0.020170	0.004520	0.007460	−0.003190
H2F	0.019720	0.022650	0.022980	−0.007270	−0.000050	−0.000390
H2G	0.026330	0.018390	0.022960	−0.001250	−0.000890	0.001120
H2H	0.020350	0.030630	0.020900	0.003580	0.004630	−0.008570
H2I	0.022620	0.021450	0.021570	0.001730	0.005030	0.003300
H2J	0.022000	0.025490	0.021290	−0.000990	−0.000780	−0.009880
H2K	0.021830	0.020320	0.024270	−0.002730	−0.000370	−0.007450
H2L	0.020540	0.023900	0.020030	0.000600	0.001640	0.005570
H2M	0.027870	0.018470	0.018480	−0.002370	0.002070	0.002510
H2N	0.013960	0.026150	0.024730	−0.000750	−0.001490	−0.003010
H2O	0.023390	0.021160	0.021740	−0.002110	0.006790	0.002410
H2P	0.014530	0.029190	0.022460	0.002610	−0.002100	−0.002450
H2Q	0.016220	0.029320	0.024350	0.004340	0.004890	−0.005950
H2R	0.022040	0.021100	0.020650	−0.001680	0.000630	0.004680

Geometric parameters (Å, º)

Cr1—C1	1.9022 (6)	N2—C22	1.4736 (8)
Cr1—C2	1.9045 (7)	N2—C28	1.4678 (9)
Cr1—C3	1.9006 (6)	C11—C12	1.5176 (9)
Cr1—C4	1.8980 (7)	C11—H1A	1.115 (16)
Cr1—C5	1.8498 (6)	C11—H1B	1.088 (15)
Cr1—H	1.754 (17)	C12—H1C	1.119 (15)
Cr2—C6	1.9012 (7)	C12—H1D	1.101 (15)
Cr2—C7	1.8980 (6)	C13—C14	1.5028 (9)
Cr2—C8	1.8980 (7)	C13—H1E	1.093 (15)
Cr2—C9	1.9097 (7)	C13—H1F	1.102 (15)
Cr2—C10	1.8472 (6)	C14—H1G	1.102 (15)
Cr2—H	1.688 (17)	C14—H1H	1.099 (15)
K1—O1	2.9686 (6)	C15—C16	1.5161 (9)
K1—O11	2.8646 (5)	C15—H1I	1.103 (15)
K1—O12	2.8633 (5)	C15—H1J	1.087 (15)
K1—O13	2.8029 (5)	C16—H1K	1.096 (15)
K1—O14	2.7996 (5)	C16—H1L	1.092 (15)
K1—O15	2.8809 (5)	C17—C18	1.5168 (9)
K1—O16	2.8431 (5)	C17—H1M	1.076 (15)
K1—N1	3.0156 (6)	C17—H1N	1.084 (15)
K1—N2	3.0114 (6)	C18—H1O	1.119 (15)
O1—C1	1.1457 (8)	C18—H1P	1.098 (15)
O2—C2	1.1447 (9)	C19—C20	1.5065 (10)
O3—C3	1.1455 (8)	C19—H1Q	1.084 (15)
O4—C4	1.1469 (9)	C19—H1R	1.084 (15)
O5—C5	1.1563 (8)	C20—H2A	1.095 (15)
O6—C6	1.1442 (9)	C20—H2B	1.095 (15)
O7—C7	1.1483 (8)	C21—C22	1.5136 (10)
O8—C8	1.1482 (9)	C21—H2C	1.105 (15)
O9—C9	1.1436 (9)	C21—H2D	1.082 (15)
O10—C10	1.1567 (8)	C22—H2E	1.103 (15)
O11—C12	1.4167 (8)	C22—H2F	1.102 (15)
O11—C13	1.4275 (7)	C23—C24	1.5151 (10)
O12—C14	1.4185 (8)	C23—H2G	1.078 (16)
O12—C15	1.4212 (8)	C23—H2H	1.119 (16)
O13—C18	1.4163 (8)	C24—H2I	1.139 (17)
O13—C19	1.4201 (8)	C24—H2J	1.101 (15)
O14—C20	1.4203 (8)	C25—C26	1.5048 (9)
O14—C21	1.4278 (8)	C25—H2K	1.084 (15)
O15—C24	1.4246 (8)	C25—H2L	1.105 (16)
O15—C25	1.4168 (9)	C26—H2M	1.117 (16)
O16—C26	1.4232 (7)	C26—H2N	1.084 (15)
O16—C27	1.4207 (8)	C27—C28	1.5159 (9)
N1—C11	1.4693 (8)	C27—H2O	1.072 (15)
N1—C17	1.4718 (9)	C27—H2P	1.134 (16)
N1—C23	1.4716 (8)	C28—H2Q	1.108 (15)
N2—C16	1.4704 (8)	C28—H2R	1.076 (15)
C2—Cr1—C1	91.94 (3)	H1A—C11—N1	111.1 (9)
C3—Cr1—C1	174.91 (3)	H1A—C11—C12	108.3 (9)
C3—Cr1—C2	92.99 (3)	H1B—C11—N1	107.6 (9)
C4—Cr1—C1	89.76 (3)	H1B—C11—C12	108.1 (9)
C4—Cr1—C2	175.07 (3)	H1B—C11—H1A	106.9 (13)
C4—Cr1—C3	85.23 (3)	C11—C12—O11	110.43 (5)
C5—Cr1—C1	89.96 (3)	H1C—C12—O11	109.0 (8)
C5—Cr1—C2	90.15 (3)	H1C—C12—C11	112.1 (9)
C5—Cr1—C3	91.27 (3)	H1D—C12—O11	110.2 (9)
C5—Cr1—C4	94.48 (3)	H1D—C12—C11	109.2 (9)
H—Cr1—C1	94.9 (6)	H1D—C12—H1C	105.8 (12)
H—Cr1—C2	76.8 (6)	C14—C13—O11	109.66 (5)
H—Cr1—C3	85.1 (6)	H1E—C13—O11	111.2 (8)
H—Cr1—C4	98.5 (6)	H1E—C13—C14	110.0 (9)
H—Cr1—C5	166.2 (6)	H1F—C13—O11	110.6 (9)
C7—Cr2—C6	90.00 (3)	H1F—C13—C14	109.0 (9)
C8—Cr2—C6	176.32 (3)	H1F—C13—H1E	106.4 (13)
C8—Cr2—C7	91.99 (3)	C13—C14—O12	108.76 (5)
C9—Cr2—C6	88.70 (3)	H1G—C14—O12	111.0 (8)
C9—Cr2—C7	171.09 (3)	H1G—C14—C13	107.6 (8)
C9—Cr2—C8	89.81 (3)	H1H—C14—O12	111.2 (8)
C10—Cr2—C6	90.13 (3)	H1H—C14—C13	108.9 (9)
C10—Cr2—C7	93.62 (3)	H1H—C14—H1G	109.4 (12)
C10—Cr2—C8	86.65 (3)	C16—C15—O12	108.80 (5)
C10—Cr2—C9	95.19 (3)	H1I—C15—O12	109.8 (8)
H—Cr2—C6	81.8 (6)	H1I—C15—C16	107.5 (9)
H—Cr2—C7	84.6 (7)	H1J—C15—O12	110.4 (8)
H—Cr2—C8	101.5 (6)	H1J—C15—C16	114.1 (9)
H—Cr2—C9	86.5 (7)	H1J—C15—H1I	106.0 (12)
H—Cr2—C10	171.7 (6)	C15—C16—N2	114.06 (5)
O11—K1—O1	71.952 (15)	H1K—C16—N2	106.5 (8)
O12—K1—O1	65.095 (15)	H1K—C16—C15	109.1 (9)
O12—K1—O11	58.934 (14)	H1L—C16—N2	110.2 (9)
O13—K1—O1	64.152 (15)	H1L—C16—C15	108.5 (9)
O13—K1—O11	104.449 (15)	H1L—C16—H1K	108.3 (13)
O13—K1—O12	129.247 (16)	C18—C17—N1	113.87 (6)
O14—K1—O1	74.479 (16)	H1M—C17—N1	107.6 (9)
O14—K1—O11	146.382 (15)	H1M—C17—C18	105.9 (9)
O14—K1—O12	104.630 (14)	H1N—C17—N1	111.6 (8)
O14—K1—O13	61.239 (14)	H1N—C17—C18	108.6 (9)
O15—K1—O1	147.825 (16)	H1N—C17—H1M	109.2 (13)
O15—K1—O11	99.516 (15)	C17—C18—O13	109.22 (5)
O15—K1—O12	137.659 (15)	H1O—C18—O13	108.7 (8)
O15—K1—O13	89.431 (15)	H1O—C18—C17	109.7 (9)
O15—K1—O14	109.933 (15)	H1P—C18—O13	110.2 (8)
O16—K1—O1	152.188 (15)	H1P—C18—C17	111.5 (9)
O16—K1—O11	119.254 (15)	H1P—C18—H1O	107.5 (12)
O16—K1—O12	97.629 (15)	C20—C19—O13	108.89 (5)
O16—K1—O13	128.502 (15)	H1Q—C19—O13	108.8 (8)
O16—K1—O14	90.375 (15)	H1Q—C19—C20	111.9 (9)
O16—K1—O15	59.187 (14)	H1R—C19—O13	110.9 (8)
N1—K1—O1	90.404 (16)	H1R—C19—C20	108.5 (9)
N1—K1—O11	62.046 (14)	H1R—C19—H1Q	107.9 (12)
N1—K1—O12	120.456 (15)	C19—C20—O14	110.04 (6)
N1—K1—O13	60.334 (15)	H2A—C20—O14	110.8 (8)
N1—K1—O14	120.394 (15)	H2A—C20—C19	109.0 (9)
N1—K1—O15	59.304 (15)	H2B—C20—O14	108.6 (8)
N1—K1—O16	117.405 (15)	H2B—C20—C19	110.0 (9)
N2—K1—O1	91.999 (15)	H2B—C20—H2A	108.4 (12)
N2—K1—O11	117.235 (14)	C22—C21—O14	109.36 (5)
N2—K1—O12	59.315 (14)	H2C—C21—O14	109.7 (9)
N2—K1—O13	122.289 (15)	H2C—C21—C22	109.8 (9)
N2—K1—O14	61.919 (14)	H2D—C21—O14	110.6 (8)
N2—K1—O15	118.644 (15)	H2D—C21—C22	112.3 (9)
N2—K1—O16	60.194 (14)	H2D—C21—H2C	105.0 (12)
N2—K1—N1	177.090 (15)	C21—C22—N2	113.21 (6)
C1—O1—K1	148.78 (5)	H2E—C22—N2	110.4 (9)
C12—O11—K1	111.62 (4)	H2E—C22—C21	109.1 (8)
C13—O11—K1	113.87 (4)	H2F—C22—N2	109.6 (8)
C13—O11—C12	110.28 (5)	H2F—C22—C21	106.2 (9)
C14—O12—K1	117.63 (4)	H2F—C22—H2E	108.1 (13)
C15—O12—K1	121.03 (4)	C24—C23—N1	113.42 (5)
C15—O12—C14	111.78 (5)	H2G—C23—N1	109.5 (8)
C18—O13—K1	121.02 (4)	H2G—C23—C24	105.8 (9)
C19—O13—K1	113.64 (4)	H2H—C23—N1	112.6 (9)
C19—O13—C18	111.94 (5)	H2H—C23—C24	108.9 (8)
C20—O14—K1	113.64 (4)	H2H—C23—H2G	106.1 (13)
C21—O14—K1	112.05 (4)	C23—C24—O15	108.65 (5)
C21—O14—C20	110.74 (5)	H2I—C24—O15	110.5 (8)
C24—O15—K1	115.73 (4)	H2I—C24—C23	111.9 (8)
C25—O15—K1	117.04 (4)	H2J—C24—O15	108.5 (9)
C25—O15—C24	111.29 (5)	H2J—C24—C23	110.6 (8)
C26—O16—K1	112.69 (4)	H2J—C24—H2I	106.7 (12)
C27—O16—K1	120.09 (4)	C26—C25—O15	109.29 (5)
C27—O16—C26	110.62 (5)	H2K—C25—O15	111.7 (8)
C11—N1—K1	107.31 (3)	H2K—C25—C26	109.3 (9)
C17—N1—K1	107.30 (4)	H2L—C25—O15	110.5 (8)
C17—N1—C11	110.14 (5)	H2L—C25—C26	110.3 (9)
C23—N1—K1	112.21 (4)	H2L—C25—H2K	105.7 (12)
C23—N1—C11	109.23 (5)	C25—C26—O16	109.54 (5)
C23—N1—C17	110.58 (5)	H2M—C26—O16	110.2 (8)
C16—N2—K1	109.82 (4)	H2M—C26—C25	111.0 (9)
C22—N2—K1	107.62 (4)	H2N—C26—O16	110.1 (9)
C22—N2—C16	109.42 (5)	H2N—C26—C25	108.1 (9)
C28—N2—K1	108.75 (4)	H2N—C26—H2M	107.8 (13)
C28—N2—C16	109.88 (5)	C28—C27—O16	110.54 (5)
C28—N2—C22	111.32 (5)	H2O—C27—O16	108.7 (9)
O1—C1—Cr1	177.05 (6)	H2O—C27—C28	112.3 (9)
O2—C2—Cr1	178.81 (6)	H2P—C27—O16	107.7 (9)
O3—C3—Cr1	176.01 (6)	H2P—C27—C28	108.0 (9)
O4—C4—Cr1	177.84 (6)	H2P—C27—H2O	109.4 (12)
O5—C5—Cr1	177.69 (6)	C27—C28—N2	114.07 (5)
O6—C6—Cr2	178.73 (6)	H2Q—C28—N2	111.8 (8)
O7—C7—Cr2	178.60 (6)	H2Q—C28—C27	107.4 (9)
O8—C8—Cr2	174.69 (6)	H2R—C28—N2	107.0 (8)
O9—C9—Cr2	178.62 (6)	H2R—C28—C27	107.8 (9)
O10—C10—Cr2	177.99 (6)	H2R—C28—H2Q	108.6 (13)
C12—C11—N1	114.58 (5)	Cr2—H—Cr1	147.6 (12)

(KCPTCR_IAM_0_HADPs)

Crystal data

C28H37Cr2KN2O16	F(000) = 1660.538
Mr = 800.70	Dx = 1.489 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71069 Å
a = 10.458 Å	Cell parameters from 1024 reflections
b = 14.417 Å	θ = 47.5–1.5°
c = 23.882 Å	µ = 0.80 mm^−1
β = 97.26°	T = 28 K
V = 3571.89 Å^3	Ellipsoidal, yellow
Z = 4	0.3 × 0.25 × 0.2 mm

Data collection

SMART CCD diffractometer	22531 reflections with I ≥ 2u(I)
ω scan	Rint = 0.0000
Absorption correction: empirical (using intensity measurements)	θmax = 48.7°, θmin = 2.4°
Tmin = 0.890, Tmax = 0.903	h = −19→20
27917 measured reflections	k = 0→30
27917 independent reflections	l = 0→50

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.036	Only H-atom coordinates refined
wR(F^2) = 0.085	w = 1/[σ^2(Fo^2) + (0.0367P)^2 + 0.9231P] where P = (Fo^2 + 2Fc^2)/3
S = 1.00	(Δ/σ)max = 0.001
27917 reflections	Δρmax = 0.85 e Å^−3
553 parameters	Δρmin = −0.82 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Cr1	0.163868 (11)	0.002358 (7)	0.236370 (4)	0.005240 (17)
Cr2	0.018767 (11)	0.177452 (7)	0.165108 (5)	0.005798 (18)
K1	0.463723 (14)	0.199286 (9)	0.418002 (6)	0.00648 (2)
O1	0.25214 (6)	0.13814 (4)	0.33124 (3)	0.01179 (9)
O2	−0.08359 (6)	−0.04363 (5)	0.28578 (3)	0.01419 (10)
O3	0.10471 (6)	−0.12664 (4)	0.13543 (3)	0.01251 (9)
O4	0.39535 (6)	0.05455 (4)	0.17748 (3)	0.01362 (10)
O5	0.30039 (6)	−0.15038 (4)	0.30580 (3)	0.01216 (9)
O6	−0.25965 (6)	0.12158 (4)	0.17223 (3)	0.01244 (9)
O7	0.01688 (6)	0.05853 (4)	0.05955 (2)	0.01252 (9)
O8	0.28638 (6)	0.25367 (4)	0.15524 (3)	0.01337 (10)
O9	0.02668 (8)	0.26560 (5)	0.28175 (3)	0.01759 (12)
O10	−0.07206 (7)	0.34770 (4)	0.09919 (3)	0.01448 (10)
O11	0.28603 (5)	0.09223 (3)	0.47319 (2)	0.00778 (8)
O12	0.44334 (6)	0.00286 (3)	0.40242 (2)	0.00835 (8)
O13	0.31320 (6)	0.34079 (4)	0.36297 (2)	0.00875 (8)
O14	0.52830 (6)	0.26685 (4)	0.31543 (2)	0.00890 (8)
O15	0.55088 (6)	0.32678 (4)	0.50749 (2)	0.00921 (8)
O16	0.72699 (5)	0.20502 (4)	0.46501 (2)	0.00819 (8)
N1	0.27325 (6)	0.30194 (4)	0.47980 (3)	0.00787 (8)
N2	0.66165 (6)	0.09466 (4)	0.36197 (2)	0.00696 (8)
C1	0.21616 (7)	0.08852 (4)	0.29500 (3)	0.00811 (10)
C2	0.01016 (8)	−0.02687 (5)	0.26765 (3)	0.00898 (10)
C3	0.12293 (7)	−0.07908 (5)	0.17421 (3)	0.00843 (10)
C4	0.30792 (8)	0.03663 (5)	0.20003 (3)	0.00919 (10)
C5	0.25012 (7)	−0.09109 (5)	0.27860 (3)	0.00838 (10)
C6	−0.15430 (8)	0.14182 (5)	0.16995 (3)	0.00896 (10)
C7	0.01872 (7)	0.10414 (5)	0.09918 (3)	0.00829 (10)
C8	0.18801 (8)	0.22110 (5)	0.16011 (3)	0.00931 (10)
C9	0.02392 (8)	0.23364 (5)	0.23772 (3)	0.01107 (11)
C10	−0.03864 (8)	0.28231 (5)	0.12532 (3)	0.00927 (10)
C11	0.20813 (8)	0.23293 (5)	0.51164 (3)	0.00913 (10)
C12	0.17306 (7)	0.14352 (5)	0.47990 (3)	0.00867 (10)
C13	0.25208 (7)	0.00541 (4)	0.44641 (3)	0.00797 (9)
C14	0.37225 (7)	−0.04781 (4)	0.43913 (3)	0.00827 (10)
C15	0.54832 (7)	−0.04995 (4)	0.38670 (3)	0.00808 (10)
C16	0.60990 (7)	0.00363 (5)	0.34255 (3)	0.00822 (10)
C17	0.17929 (7)	0.34658 (5)	0.43696 (3)	0.00941 (10)
C18	0.24063 (8)	0.40169 (5)	0.39333 (3)	0.00983 (10)
C19	0.37497 (8)	0.38880 (5)	0.32178 (3)	0.01090 (11)
C20	0.42802 (8)	0.31884 (5)	0.28400 (3)	0.01088 (11)
C21	0.57214 (8)	0.19478 (5)	0.28131 (3)	0.00952 (10)
C22	0.69029 (8)	0.14952 (5)	0.31296 (3)	0.00927 (10)
C23	0.33602 (8)	0.37155 (5)	0.51922 (3)	0.01021 (11)
C24	0.46519 (8)	0.34035 (5)	0.54887 (3)	0.01030 (11)
C25	0.68016 (7)	0.31745 (5)	0.53317 (3)	0.00879 (10)
C26	0.76442 (7)	0.29320 (5)	0.48874 (3)	0.00917 (10)
C27	0.82397 (7)	0.16968 (5)	0.43394 (3)	0.00904 (10)
C28	0.77750 (7)	0.08191 (5)	0.40291 (3)	0.00838 (10)
H	0.0504 (11)	0.0762 (8)	0.2000 (5)	0.000000
H11a	0.1272 (12)	0.2600 (8)	0.5234 (5)	0.000000
H11b	0.2652 (11)	0.2182 (8)	0.5467 (5)	0.000000
H12a	0.1261 (11)	0.1562 (8)	0.4424 (5)	0.000000
H12b	0.1147 (11)	0.1066 (8)	0.5021 (5)	0.000000
H13a	0.2011 (12)	0.0146 (8)	0.4104 (5)	0.000000
H13b	0.1993 (11)	−0.0317 (8)	0.4687 (5)	0.000000
H14a	0.3443 (11)	−0.1089 (8)	0.4228 (5)	0.000000
H14b	0.4225 (11)	−0.0561 (8)	0.4766 (5)	0.000000
H15a	0.5169 (11)	−0.1076 (8)	0.3698 (5)	0.000000
H15b	0.6082 (11)	−0.0656 (8)	0.4197 (5)	0.000000
H16a	0.5442 (12)	0.0135 (8)	0.3113 (5)	0.000000
H16b	0.6774 (11)	−0.0344 (8)	0.3291 (5)	0.000000
H17a	0.1298 (11)	0.2982 (8)	0.4167 (5)	0.000000
H17b	0.1212 (11)	0.3854 (8)	0.4540 (5)	0.000000
H18a	0.1719 (11)	0.4304 (8)	0.3685 (5)	0.000000
H18b	0.2988 (11)	0.4511 (8)	0.4117 (5)	0.000000
H19a	0.4420 (11)	0.4264 (8)	0.3398 (5)	0.000000
H19b	0.3127 (11)	0.4278 (8)	0.2983 (5)	0.000000
H20a	0.3599 (11)	0.2804 (8)	0.2691 (5)	0.000000
H20b	0.4606 (11)	0.3513 (8)	0.2544 (5)	0.000000
H21a	0.5927 (11)	0.2199 (8)	0.2450 (5)	0.000000
H21b	0.5054 (12)	0.1520 (8)	0.2718 (5)	0.000000
H22a	0.7295 (11)	0.1090 (8)	0.2857 (5)	0.000000
H22b	0.7505 (11)	0.2003 (8)	0.3253 (5)	0.000000
H23a	0.3484 (11)	0.4256 (8)	0.4984 (5)	0.000000
H23b	0.2773 (11)	0.3921 (8)	0.5479 (5)	0.000000
H24a	0.4604 (11)	0.2821 (8)	0.5706 (5)	0.000000
H24b	0.4966 (11)	0.3863 (8)	0.5751 (5)	0.000000
H25a	0.7122 (11)	0.3743 (8)	0.5516 (5)	0.000000
H25b	0.6866 (11)	0.2701 (8)	0.5625 (5)	0.000000
H26a	0.7622 (11)	0.3391 (8)	0.4595 (5)	0.000000
H26b	0.8526 (11)	0.2921 (8)	0.5073 (5)	0.000000
H27a	0.8485 (11)	0.2164 (8)	0.4084 (5)	0.000000
H27b	0.9033 (11)	0.1543 (8)	0.4620 (5)	0.000000
H28a	0.8477 (11)	0.0552 (8)	0.3850 (5)	0.000000
H28b	0.7617 (11)	0.0365 (8)	0.4296 (5)	0.000000

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cr1	0.00568 (4)	0.00465 (3)	0.00537 (4)	0.00014 (3)	0.00063 (3)	−0.00017 (3)
Cr2	0.00671 (4)	0.00537 (3)	0.00518 (4)	0.00077 (3)	0.00023 (3)	0.00014 (3)
K1	0.00616 (5)	0.00665 (4)	0.00657 (5)	0.00019 (4)	0.00056 (4)	−0.00004 (3)
O1	0.0151 (3)	0.00927 (17)	0.0101 (2)	0.00002 (17)	−0.00211 (17)	−0.00225 (15)
O2	0.0111 (3)	0.0163 (2)	0.0162 (3)	0.0003 (2)	0.00563 (19)	0.00134 (19)
O3	0.0146 (3)	0.0123 (2)	0.0107 (2)	−0.00206 (18)	0.00177 (18)	−0.00438 (16)
O4	0.0114 (3)	0.0136 (2)	0.0169 (3)	−0.00070 (19)	0.00614 (19)	−0.00016 (18)
O5	0.0132 (3)	0.00925 (18)	0.0134 (2)	0.00314 (17)	−0.00060 (18)	0.00208 (16)
O6	0.0108 (2)	0.0146 (2)	0.0124 (2)	−0.00067 (19)	0.00330 (18)	0.00010 (17)
O7	0.0162 (3)	0.0123 (2)	0.0093 (2)	−0.00152 (19)	0.00264 (18)	−0.00279 (16)
O8	0.0120 (3)	0.0158 (2)	0.0120 (2)	−0.00447 (19)	0.00030 (18)	0.00057 (18)
O9	0.0254 (3)	0.0169 (2)	0.0096 (2)	0.0096 (2)	−0.0012 (2)	−0.00439 (18)
O10	0.0175 (3)	0.00994 (19)	0.0150 (3)	0.00287 (19)	−0.0018 (2)	0.00386 (17)
O11	0.0059 (2)	0.00712 (15)	0.0103 (2)	0.00008 (14)	0.00088 (15)	−0.00169 (14)
O12	0.0085 (2)	0.00670 (15)	0.0105 (2)	0.00107 (15)	0.00399 (15)	0.00143 (14)
O13	0.0098 (2)	0.00708 (15)	0.0099 (2)	0.00118 (15)	0.00347 (16)	0.00125 (14)
O14	0.0102 (2)	0.00873 (16)	0.00767 (19)	0.00281 (16)	0.00058 (15)	0.00030 (14)
O15	0.0065 (2)	0.01357 (19)	0.00744 (19)	0.00152 (16)	0.00028 (14)	−0.00175 (15)
O16	0.0060 (2)	0.00845 (16)	0.0103 (2)	−0.00112 (15)	0.00186 (15)	−0.00322 (14)
N1	0.0072 (2)	0.00792 (17)	0.0084 (2)	0.00064 (17)	0.00033 (16)	−0.00016 (15)
N2	0.0074 (2)	0.00684 (16)	0.0066 (2)	−0.00051 (16)	0.00079 (16)	0.00019 (14)
C1	0.0087 (3)	0.00702 (19)	0.0084 (2)	0.00044 (19)	0.00038 (18)	0.00019 (17)
C2	0.0100 (3)	0.0084 (2)	0.0087 (2)	0.0010 (2)	0.00157 (19)	0.00047 (17)
C3	0.0080 (3)	0.0082 (2)	0.0091 (2)	−0.00010 (19)	0.00139 (19)	−0.00042 (17)
C4	0.0094 (3)	0.0085 (2)	0.0097 (3)	−0.00002 (19)	0.0012 (2)	−0.00069 (18)
C5	0.0081 (3)	0.00735 (19)	0.0096 (2)	0.00042 (19)	0.00095 (19)	−0.00039 (17)
C6	0.0112 (3)	0.0090 (2)	0.0067 (2)	0.0016 (2)	0.00102 (19)	0.00033 (17)
C7	0.0084 (3)	0.0084 (2)	0.0082 (2)	−0.00050 (19)	0.00146 (19)	0.00010 (17)
C8	0.0114 (3)	0.0089 (2)	0.0072 (2)	−0.0001 (2)	−0.00045 (19)	−0.00007 (17)
C9	0.0131 (3)	0.0100 (2)	0.0097 (3)	0.0038 (2)	0.0000 (2)	−0.00088 (19)
C10	0.0104 (3)	0.0080 (2)	0.0091 (3)	0.0010 (2)	−0.00002 (19)	0.00039 (17)
C11	0.0096 (3)	0.0099 (2)	0.0082 (2)	0.0014 (2)	0.00228 (19)	−0.00005 (17)
C12	0.0063 (3)	0.0094 (2)	0.0105 (3)	0.00041 (19)	0.00150 (19)	0.00010 (18)
C13	0.0077 (3)	0.00767 (19)	0.0087 (2)	−0.00183 (19)	0.00146 (18)	−0.00056 (17)
C14	0.0094 (3)	0.00705 (19)	0.0087 (2)	−0.00047 (19)	0.00245 (19)	0.00093 (17)
C15	0.0075 (3)	0.00668 (19)	0.0102 (3)	0.00109 (18)	0.00159 (19)	0.00033 (17)
C16	0.0094 (3)	0.00774 (19)	0.0076 (2)	−0.00025 (19)	0.00127 (18)	−0.00102 (17)
C17	0.0076 (3)	0.0101 (2)	0.0107 (3)	0.0021 (2)	0.00159 (19)	0.00140 (18)
C18	0.0103 (3)	0.0079 (2)	0.0118 (3)	0.0023 (2)	0.0031 (2)	0.00121 (18)
C19	0.0125 (3)	0.0083 (2)	0.0125 (3)	0.0019 (2)	0.0042 (2)	0.00325 (19)
C20	0.0121 (3)	0.0120 (2)	0.0087 (3)	0.0032 (2)	0.0017 (2)	0.00339 (19)
C21	0.0124 (3)	0.0089 (2)	0.0072 (2)	0.0018 (2)	0.0012 (2)	0.00021 (17)
C22	0.0096 (3)	0.0097 (2)	0.0090 (3)	0.0009 (2)	0.0033 (2)	0.00188 (18)
C23	0.0087 (3)	0.0099 (2)	0.0119 (3)	0.0013 (2)	0.0008 (2)	−0.00350 (19)
C24	0.0080 (3)	0.0141 (2)	0.0089 (3)	0.0003 (2)	0.00130 (19)	−0.00307 (19)
C25	0.0078 (3)	0.0098 (2)	0.0084 (2)	−0.00043 (19)	−0.00028 (18)	−0.00192 (18)
C26	0.0079 (3)	0.0087 (2)	0.0109 (3)	−0.00155 (19)	0.00123 (19)	−0.00219 (18)
C27	0.0069 (3)	0.0102 (2)	0.0102 (3)	−0.00049 (19)	0.00176 (19)	−0.00205 (18)
C28	0.0073 (3)	0.0085 (2)	0.0092 (2)	0.00094 (19)	0.00067 (18)	−0.00069 (17)
H	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H11a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H11b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H12a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H12b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H13a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H13b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H14a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H14b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H15a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H15b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H16a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H16b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H17a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H17b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H18a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H18b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H19a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H19b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H20a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H20b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H21a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H21b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H22a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H22b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H23a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H23b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H24a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H24b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H25a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H25b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H26a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H26b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H27a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H27b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H28a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H28b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000

Geometric parameters (Å, º)

Cr1—C1	1.8997 (7)	N2—C22	1.4744 (9)
Cr1—C2	1.9034 (8)	N2—C28	1.4690 (10)
Cr1—C3	1.8986 (7)	C11—C12	1.5168 (10)
Cr1—C4	1.8966 (8)	C11—H11a	1.004 (12)
Cr1—C5	1.8482 (7)	C11—H11b	0.989 (12)
Cr1—H	1.742 (12)	C12—H12a	0.981 (12)
Cr2—C6	1.8989 (8)	C12—H12b	1.009 (11)
Cr2—C7	1.8962 (7)	C13—C14	1.5013 (10)
Cr2—C8	1.8964 (8)	C13—H13a	0.962 (12)
Cr2—C9	1.9085 (8)	C13—H13b	0.974 (12)
Cr2—C10	1.8452 (7)	C14—H14a	0.993 (11)
Cr2—H	1.693 (12)	C14—H14b	0.986 (12)
K1—O1	2.9678 (6)	C15—C16	1.5149 (10)
K1—O11	2.8621 (6)	C15—H15a	0.963 (12)
K1—O12	2.8606 (5)	C15—H15b	0.970 (12)
K1—O13	2.8008 (6)	C16—H16a	0.959 (12)
K1—O14	2.7970 (6)	C16—H16b	0.979 (12)
K1—O15	2.8782 (6)	C17—C18	1.5157 (10)
K1—O16	2.8401 (6)	C17—H17a	0.962 (12)
K1—N1	3.0132 (6)	C17—H17b	0.954 (12)
K1—N2	3.0084 (6)	C18—H18a	0.965 (12)
O1—C1	1.1491 (9)	C18—H18b	1.001 (12)
O2—C2	1.1465 (10)	C19—C20	1.5052 (11)
O3—C3	1.1488 (9)	C19—H19a	0.946 (12)
O4—C4	1.1477 (10)	C19—H19b	0.981 (12)
O5—C5	1.1587 (9)	C20—H20a	0.937 (12)
O6—C6	1.1477 (10)	C20—H20b	0.946 (12)
O7—C7	1.1507 (9)	C21—C22	1.5126 (11)
O8—C8	1.1501 (10)	C21—H21a	0.987 (12)
O9—C9	1.1451 (10)	C21—H21b	0.937 (12)
O10—C10	1.1598 (9)	C22—H22a	1.000 (11)
O11—C12	1.4199 (9)	C22—H22b	0.986 (12)
O11—C13	1.4297 (8)	C23—C24	1.5123 (11)
O12—C14	1.4213 (8)	C23—H23a	0.942 (12)
O12—C15	1.4248 (9)	C23—H23b	1.020 (12)
O13—C18	1.4183 (9)	C24—H24a	0.992 (12)
O13—C19	1.4229 (9)	C24—H24b	0.943 (12)
O14—C20	1.4234 (9)	C25—C26	1.5037 (10)
O14—C21	1.4312 (9)	C25—H25a	0.970 (12)
O15—C24	1.4290 (9)	C25—H25b	0.974 (12)
O15—C25	1.4186 (9)	C26—H26a	0.960 (12)
O16—C26	1.4264 (8)	C26—H26b	0.971 (12)
O16—C27	1.4244 (9)	C27—C28	1.5150 (10)
N1—C11	1.4705 (9)	C27—H27a	0.965 (12)
N1—C17	1.4739 (10)	C27—H27b	1.022 (12)
N1—C23	1.4725 (9)	C28—H28a	0.974 (12)
N2—C16	1.4720 (9)	C28—H28b	0.942 (11)
C2—Cr1—C1	91.96 (3)	H11a—C11—N1	110.1 (7)
C3—Cr1—C1	174.92 (3)	H11a—C11—C12	108.2 (7)
C3—Cr1—C2	92.96 (3)	H11b—C11—N1	108.3 (7)
C4—Cr1—C1	89.75 (3)	H11b—C11—C12	108.8 (7)
C4—Cr1—C2	175.05 (3)	H11b—C11—H11a	106.6 (10)
C4—Cr1—C3	85.24 (3)	C11—C12—O11	110.29 (6)
C5—Cr1—C1	89.96 (3)	H12a—C12—O11	108.8 (7)
C5—Cr1—C2	90.15 (3)	H12a—C12—C11	111.0 (7)
C5—Cr1—C3	91.27 (3)	H12b—C12—O11	110.6 (7)
C5—Cr1—C4	94.50 (3)	H12b—C12—C11	108.1 (7)
H—Cr1—C1	94.7 (4)	H12b—C12—H12a	108.2 (10)
H—Cr1—C2	77.0 (4)	C14—C13—O11	109.57 (6)
H—Cr1—C3	85.2 (4)	H13a—C13—O11	110.9 (7)
H—Cr1—C4	98.2 (4)	H13a—C13—C14	110.2 (7)
H—Cr1—C5	166.4 (4)	H13b—C13—O11	111.3 (7)
C7—Cr2—C6	89.97 (3)	H13b—C13—C14	108.8 (7)
C8—Cr2—C6	176.31 (3)	H13b—C13—H13a	106.0 (10)
C8—Cr2—C7	92.01 (3)	C13—C14—O12	108.64 (5)
C9—Cr2—C6	88.69 (3)	H14a—C14—O12	111.4 (7)
C9—Cr2—C7	171.11 (3)	H14a—C14—C13	106.8 (7)
C9—Cr2—C8	89.82 (3)	H14b—C14—O12	111.2 (7)
C10—Cr2—C6	90.14 (3)	H14b—C14—C13	108.3 (7)
C10—Cr2—C7	93.62 (3)	H14b—C14—H14a	110.3 (10)
C10—Cr2—C8	86.63 (3)	C16—C15—O12	108.69 (5)
C10—Cr2—C9	95.17 (3)	H15a—C15—O12	109.7 (7)
H—Cr2—C6	82.2 (4)	H15a—C15—C16	107.6 (7)
H—Cr2—C7	84.7 (4)	H15b—C15—O12	110.5 (7)
H—Cr2—C8	101.0 (4)	H15b—C15—C16	113.4 (7)
H—Cr2—C9	86.4 (4)	H15b—C15—H15a	106.9 (10)
H—Cr2—C10	172.2 (4)	C15—C16—N2	114.01 (6)
O11—K1—O1	72.006 (17)	H16a—C16—N2	108.2 (7)
O12—K1—O1	65.064 (16)	H16a—C16—C15	106.9 (7)
O12—K1—O11	58.938 (15)	H16b—C16—N2	110.6 (7)
O13—K1—O1	64.117 (16)	H16b—C16—C15	109.2 (7)
O13—K1—O11	104.463 (16)	H16b—C16—H16a	107.7 (10)
O13—K1—O12	129.181 (17)	C18—C17—N1	113.78 (6)
O14—K1—O1	74.530 (17)	H17a—C17—N1	107.6 (7)
O14—K1—O11	146.486 (17)	H17a—C17—C18	106.4 (7)
O14—K1—O12	104.657 (16)	H17b—C17—N1	111.3 (7)
O14—K1—O13	61.247 (16)	H17b—C17—C18	109.5 (7)
O15—K1—O1	147.810 (17)	H17b—C17—H17a	108.0 (10)
O15—K1—O11	99.533 (16)	C17—C18—O13	109.10 (6)
O15—K1—O12	137.748 (17)	H18a—C18—O13	110.9 (7)
O15—K1—O13	89.413 (16)	H18a—C18—C17	107.5 (7)
O15—K1—O14	109.817 (17)	H18b—C18—O13	109.3 (7)
O16—K1—O1	152.206 (17)	H18b—C18—C17	111.0 (7)
O16—K1—O11	119.151 (16)	H18b—C18—H18a	109.1 (10)
O16—K1—O12	97.633 (16)	C20—C19—O13	108.80 (6)
O16—K1—O13	128.578 (17)	H19a—C19—O13	109.8 (7)
O16—K1—O14	90.385 (17)	H19a—C19—C20	110.4 (7)
O16—K1—O15	59.183 (15)	H19b—C19—O13	110.4 (7)
N1—K1—O1	90.406 (17)	H19b—C19—C20	108.0 (7)
N1—K1—O11	62.059 (16)	H19b—C19—H19a	109.4 (10)
N1—K1—O12	120.460 (17)	C19—C20—O14	109.85 (6)
N1—K1—O13	60.326 (16)	H20a—C20—O14	111.3 (7)
N1—K1—O14	120.374 (16)	H20a—C20—C19	107.7 (7)
N1—K1—O15	59.310 (17)	H20b—C20—O14	110.1 (7)
N1—K1—O16	117.385 (17)	H20b—C20—C19	108.2 (7)
N2—K1—O1	91.993 (17)	H20b—C20—H20a	109.7 (10)
N2—K1—O11	117.237 (15)	C22—C21—O14	109.20 (6)
N2—K1—O12	59.329 (16)	H21a—C21—O14	110.8 (7)
N2—K1—O13	122.277 (16)	H21a—C21—C22	110.0 (7)
N2—K1—O14	61.916 (16)	H21b—C21—O14	109.5 (7)
N2—K1—O15	118.641 (17)	H21b—C21—C22	111.9 (7)
N2—K1—O16	60.216 (16)	H21b—C21—H21a	105.4 (10)
N2—K1—N1	177.105 (17)	C21—C22—N2	113.15 (6)
C1—O1—K1	148.77 (6)	H22a—C22—N2	110.2 (7)
C12—O11—K1	111.66 (4)	H22a—C22—C21	107.6 (7)
C13—O11—K1	113.90 (4)	H22b—C22—N2	110.3 (7)
C13—O11—C12	110.07 (6)	H22b—C22—C21	106.2 (7)
C14—O12—K1	117.69 (4)	H22b—C22—H22a	109.2 (10)
C15—O12—K1	121.07 (4)	C24—C23—N1	113.35 (6)
C15—O12—C14	111.62 (5)	H23a—C23—N1	107.8 (7)
C18—O13—K1	121.09 (4)	H23a—C23—C24	108.6 (7)
C19—O13—K1	113.66 (4)	H23b—C23—N1	111.7 (7)
C19—O13—C18	111.79 (5)	H23b—C23—C24	110.4 (7)
C20—O14—K1	113.69 (4)	H23b—C23—H23a	104.5 (9)
C21—O14—K1	112.09 (4)	C23—C24—O15	108.54 (6)
C21—O14—C20	110.47 (6)	H24a—C24—O15	108.9 (7)
C24—O15—K1	115.69 (4)	H24a—C24—C23	113.3 (7)
C25—O15—K1	117.10 (4)	H24b—C24—O15	111.1 (7)
C25—O15—C24	111.14 (6)	H24b—C24—C23	108.5 (7)
C26—O16—K1	112.75 (4)	H24b—C24—H24a	106.4 (10)
C27—O16—K1	120.14 (4)	C26—C25—O15	109.18 (6)
C27—O16—C26	110.37 (6)	H25a—C25—O15	111.8 (7)
C11—N1—K1	107.39 (4)	H25a—C25—C26	108.5 (7)
C17—N1—K1	107.36 (4)	H25b—C25—O15	110.6 (7)
C17—N1—C11	110.04 (6)	H25b—C25—C26	110.5 (7)
C23—N1—K1	112.27 (4)	H25b—C25—H25a	106.2 (10)
C23—N1—C11	109.19 (6)	C25—C26—O16	109.37 (6)
C23—N1—C17	110.51 (6)	H26a—C26—O16	110.2 (7)
C16—N2—K1	109.94 (4)	H26a—C26—C25	113.0 (7)
C22—N2—K1	107.72 (4)	H26b—C26—O16	111.3 (7)
C22—N2—C16	109.36 (5)	H26b—C26—C25	106.8 (7)
C28—N2—K1	108.82 (4)	H26b—C26—H26a	106.1 (10)
C28—N2—C16	109.74 (5)	C28—C27—O16	110.36 (6)
C28—N2—C22	111.24 (6)	H27a—C27—O16	110.1 (7)
O1—C1—Cr1	177.05 (6)	H27a—C27—C28	111.6 (7)
O2—C2—Cr1	178.85 (7)	H27b—C27—O16	108.0 (7)
O3—C3—Cr1	175.95 (7)	H27b—C27—C28	108.8 (7)
O4—C4—Cr1	177.85 (6)	H27b—C27—H27a	107.9 (10)
O5—C5—Cr1	177.70 (7)	C27—C28—N2	114.06 (6)
O6—C6—Cr2	178.76 (6)	H28a—C28—N2	111.1 (7)
O7—C7—Cr2	178.64 (6)	H28a—C28—C27	109.4 (7)
O8—C8—Cr2	174.74 (7)	H28b—C28—N2	109.7 (7)
O9—C9—Cr2	178.60 (7)	H28b—C28—C27	108.8 (7)
O10—C10—Cr2	177.94 (7)	H28b—C28—H28a	103.2 (10)
C12—C11—N1	114.53 (6)	Cr2—H—Cr1	148.3 (7)
K1—O11—C12—C11	−56.09 (4)	K1—N1—C23—C24	−37.55 (5)
K1—O11—C13—C14	53.26 (4)	K1—N2—C16—C15	−48.45 (4)
K1—O12—C14—C13	42.37 (4)	K1—N2—C22—C21	−39.26 (4)
K1—O12—C15—C16	−41.17 (5)	K1—N2—C28—C27	−48.60 (4)
K1—O13—C18—C17	−40.89 (5)	O11—C12—C11—N1	69.68 (6)
K1—O13—C19—C20	49.42 (5)	O11—C13—C14—O12	−63.32 (6)
K1—O14—C20—C19	48.02 (4)	O12—C15—C16—N2	60.59 (6)
K1—O14—C21—C22	−59.88 (4)	O13—C18—C17—N1	62.43 (7)
K1—O15—C24—C23	−56.15 (4)	O13—C19—C20—O14	−66.05 (7)
K1—O15—C25—C26	37.93 (4)	O14—C21—C22—N2	69.53 (6)
K1—O16—C26—C25	57.46 (4)	O15—C24—C23—N1	63.12 (6)
K1—O16—C27—C28	−39.29 (4)	O15—C25—C26—O16	−63.69 (6)
K1—N1—C11—C12	−41.20 (4)	O16—C27—C28—N2	60.51 (6)
K1—N1—C17—C18	−49.87 (4)

(KCPTCR_IAM)

Crystal data

C28H37Cr2KN2O16	F(000) = 1656
Mr = 800.69	Dx = 1.489 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71069 Å
a = 10.458 Å	Cell parameters from 1024 reflections
b = 14.417 Å	θ = 47.5–1.5°
c = 23.882 Å	µ = 0.80 mm^−1
β = 97.26°	T = 28 K
V = 3571.9 Å^3	Ellipsoidal, yellow
Z = 4	0.3 × 0.25 × 0.2 mm

Data collection

SMART CCD diffractometer	27917 independent reflections
ω scan	22536 reflections with I > 2σ(I)
Absorption correction: empirical (using intensity measurements)	Rint = 0.0000
Tmin = 0.890, Tmax = 0.903	θmax = 48.7°, θmin = 2.4°
27917 measured reflections

Refinement

Refinement on F^2	Primary atom site location: dual
Least-squares matrix: full	Hydrogen site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.036	All H-atom parameters refined
wR(F^2) = 0.115	w = 1/[σ^2(Fo^2) + (0.1P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 0.79	(Δ/σ)max = 0.001
27917 reflections	Δρmax = 0.94 e Å^−3
590 parameters	Δρmin = −1.47 e Å^−3
0 restraints

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Cr1	0.16387 (2)	0.00235 (2)	0.23637 (2)	0.00530 (2)
Cr2	0.01877 (2)	0.17745 (2)	0.16510 (2)	0.00585 (2)
K1	0.46372 (2)	0.19929 (2)	0.41800 (2)	0.00655 (2)
O1	0.25216 (7)	0.13817 (4)	0.33127 (3)	0.01187 (9)
O2	−0.08369 (7)	−0.04362 (5)	0.28579 (3)	0.01435 (10)
O3	0.10464 (7)	−0.12663 (4)	0.13540 (3)	0.01260 (10)
O4	0.39538 (7)	0.05452 (5)	0.17747 (3)	0.01375 (10)
O5	0.30046 (7)	−0.15040 (4)	0.30578 (3)	0.01223 (9)
O6	−0.25964 (7)	0.12161 (5)	0.17221 (3)	0.01248 (9)
O7	0.01696 (7)	0.05853 (4)	0.05954 (3)	0.01265 (10)
O8	0.28643 (7)	0.25368 (5)	0.15522 (3)	0.01347 (10)
O9	0.02663 (8)	0.26556 (5)	0.28173 (3)	0.01791 (13)
O10	−0.07211 (7)	0.34774 (4)	0.09917 (3)	0.01455 (11)
O11	0.28594 (6)	0.09223 (4)	0.47322 (2)	0.00788 (8)
O12	0.44336 (6)	0.00283 (4)	0.40243 (2)	0.00842 (8)
O13	0.31313 (6)	0.34081 (4)	0.36294 (2)	0.00880 (8)
O14	0.52824 (6)	0.26682 (4)	0.31540 (2)	0.00897 (8)
O15	0.55084 (6)	0.32675 (4)	0.50748 (2)	0.00924 (8)
O16	0.72702 (6)	0.20502 (4)	0.46499 (2)	0.00825 (8)
N1	0.27330 (6)	0.30193 (4)	0.47979 (3)	0.00794 (8)
N2	0.66168 (6)	0.09464 (4)	0.36196 (3)	0.00703 (8)
C1	0.21610 (8)	0.08854 (5)	0.29503 (3)	0.00821 (10)
C2	0.01017 (8)	−0.02686 (5)	0.26762 (3)	0.00900 (10)
C3	0.12300 (8)	−0.07907 (5)	0.17421 (3)	0.00853 (10)
C4	0.30796 (8)	0.03659 (5)	0.20003 (3)	0.00925 (10)
C5	0.25015 (8)	−0.09111 (5)	0.27863 (3)	0.00851 (10)
C6	−0.15434 (8)	0.14182 (5)	0.16995 (3)	0.00896 (10)
C7	0.01871 (8)	0.10414 (5)	0.09917 (3)	0.00838 (10)
C8	0.18802 (8)	0.22108 (5)	0.16011 (3)	0.00925 (10)
C9	0.02402 (8)	0.23363 (5)	0.23768 (3)	0.01116 (11)
C10	−0.03860 (8)	0.28233 (5)	0.12530 (3)	0.00936 (10)
C11	0.20809 (8)	0.23293 (5)	0.51163 (3)	0.00912 (10)
C12	0.17310 (7)	0.14347 (5)	0.47988 (3)	0.00878 (10)
C13	0.25210 (8)	0.00539 (5)	0.44637 (3)	0.00801 (9)
C14	0.37230 (8)	−0.04780 (5)	0.43910 (3)	0.00834 (10)
C15	0.54821 (7)	−0.04992 (5)	0.38669 (3)	0.00816 (9)
C16	0.60994 (8)	0.00364 (5)	0.34255 (3)	0.00831 (10)
C17	0.17936 (8)	0.34656 (5)	0.43699 (3)	0.00945 (10)
C18	0.24064 (8)	0.40171 (5)	0.39332 (3)	0.00989 (10)
C19	0.37489 (8)	0.38881 (5)	0.32182 (3)	0.01099 (11)
C20	0.42804 (8)	0.31883 (5)	0.28402 (3)	0.01095 (11)
C21	0.57209 (8)	0.19478 (5)	0.28133 (3)	0.00959 (10)
C22	0.69033 (8)	0.14950 (5)	0.31295 (3)	0.00936 (10)
C23	0.33591 (8)	0.37155 (5)	0.51918 (3)	0.01028 (11)
C24	0.46533 (8)	0.34031 (6)	0.54888 (3)	0.01035 (11)
C25	0.68014 (8)	0.31744 (5)	0.53319 (3)	0.00888 (10)
C26	0.76443 (8)	0.29319 (5)	0.48875 (3)	0.00924 (10)
C27	0.82395 (8)	0.16969 (5)	0.43394 (3)	0.00912 (10)
C28	0.77746 (7)	0.08191 (5)	0.40293 (3)	0.00846 (10)
H	0.051 (2)	0.0803 (15)	0.1969 (9)	0.032 (5)*
H1A	0.1285 (17)	0.2612 (12)	0.5240 (7)	0.016 (4)*
H1B	0.2640 (16)	0.2180 (11)	0.5471 (7)	0.012 (3)*
H1C	0.1260 (16)	0.1562 (11)	0.4438 (7)	0.013 (3)*
H1D	0.1132 (15)	0.1052 (11)	0.5020 (7)	0.012 (3)*
H1E	0.2016 (17)	0.0126 (12)	0.4112 (7)	0.015 (4)*
H1F	0.2001 (15)	−0.0338 (11)	0.4691 (7)	0.012 (3)*
H1G	0.3441 (15)	−0.1099 (11)	0.4233 (7)	0.013 (3)*
H1H	0.4241 (14)	−0.0546 (11)	0.4767 (6)	0.008 (3)*
H1I	0.5182 (15)	−0.1063 (11)	0.3699 (7)	0.011 (3)*
H1J	0.6087 (16)	−0.0667 (12)	0.4199 (7)	0.017 (4)*
H1K	0.5419 (16)	0.0130 (11)	0.3112 (7)	0.012 (3)*
H1L	0.6800 (16)	−0.0352 (12)	0.3299 (7)	0.015 (4)*
H1M	0.1335 (14)	0.2971 (10)	0.4159 (6)	0.005 (3)*
H1N	0.1206 (17)	0.3850 (12)	0.4551 (7)	0.018 (4)*
H1O	0.1724 (17)	0.4322 (12)	0.3692 (8)	0.019 (4)*
H1P	0.2998 (14)	0.4520 (10)	0.4105 (6)	0.005 (3)*
H1Q	0.4406 (16)	0.4270 (11)	0.3410 (7)	0.012 (3)*
H1R	0.3125 (17)	0.4292 (13)	0.2991 (8)	0.023 (4)*
H2A	0.3590 (17)	0.2800 (13)	0.2687 (7)	0.019 (4)*
H2B	0.4623 (18)	0.3555 (13)	0.2547 (8)	0.023 (4)*
H2C	0.5928 (17)	0.2190 (13)	0.2459 (7)	0.019 (4)*
H2D	0.5047 (16)	0.1514 (11)	0.2721 (7)	0.011 (3)*
H2E	0.7285 (16)	0.1082 (12)	0.2861 (7)	0.016 (4)*
H2F	0.7538 (15)	0.2012 (11)	0.3253 (6)	0.009 (3)*
H2G	0.3506 (15)	0.4246 (11)	0.4985 (7)	0.013 (3)*
H2H	0.2746 (18)	0.3922 (13)	0.5494 (8)	0.025 (4)*
H2I	0.4626 (17)	0.2819 (13)	0.5701 (7)	0.017 (4)*
H2J	0.4982 (18)	0.3856 (13)	0.5748 (8)	0.022 (4)*
H2K	0.7126 (16)	0.3727 (12)	0.5514 (7)	0.017 (4)*
H2L	0.6867 (14)	0.2732 (10)	0.5632 (6)	0.007 (3)*
H2M	0.7639 (17)	0.3384 (12)	0.4590 (7)	0.018 (4)*
H2N	0.8501 (16)	0.2927 (12)	0.5064 (7)	0.015 (4)*
H2O	0.8494 (16)	0.2172 (12)	0.4082 (7)	0.013 (3)*
H2P	0.9031 (16)	0.1529 (11)	0.4619 (7)	0.012 (3)*
H2Q	0.8485 (17)	0.0544 (12)	0.3833 (7)	0.018 (4)*
H2R	0.7607 (14)	0.0374 (10)	0.4303 (6)	0.008 (3)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cr1	0.00576 (4)	0.00471 (3)	0.00542 (4)	0.00013 (3)	0.00064 (3)	−0.00017 (2)
Cr2	0.00678 (5)	0.00542 (3)	0.00523 (4)	0.00076 (3)	0.00025 (3)	0.00013 (2)
K1	0.00626 (6)	0.00670 (4)	0.00663 (5)	0.00020 (4)	0.00058 (4)	−0.00005 (3)
O1	0.0154 (3)	0.00930 (17)	0.0100 (2)	0.00015 (17)	−0.00216 (17)	−0.00237 (15)
O2	0.0112 (3)	0.0164 (2)	0.0165 (3)	0.0002 (2)	0.0058 (2)	0.00138 (19)
O3	0.0148 (3)	0.0123 (2)	0.0107 (2)	−0.00196 (19)	0.00176 (18)	−0.00464 (16)
O4	0.0117 (3)	0.0137 (2)	0.0170 (3)	−0.00062 (19)	0.0064 (2)	0.00002 (18)
O5	0.0134 (3)	0.00943 (18)	0.0133 (2)	0.00326 (17)	−0.00067 (18)	0.00216 (16)
O6	0.0106 (2)	0.0148 (2)	0.0125 (2)	−0.00070 (19)	0.00334 (18)	0.00017 (17)
O7	0.0164 (3)	0.0124 (2)	0.0094 (2)	−0.00144 (19)	0.00282 (18)	−0.00291 (16)
O8	0.0118 (3)	0.0159 (2)	0.0124 (2)	−0.00474 (19)	0.00034 (18)	0.00060 (18)
O9	0.0263 (4)	0.0172 (2)	0.0094 (2)	0.0098 (2)	−0.0012 (2)	−0.00453 (19)
O10	0.0177 (3)	0.00981 (19)	0.0151 (3)	0.00285 (19)	−0.0020 (2)	0.00384 (17)
O11	0.0062 (2)	0.00720 (15)	0.0102 (2)	0.00006 (14)	0.00091 (14)	−0.00165 (14)
O12	0.0087 (2)	0.00677 (15)	0.0105 (2)	0.00108 (15)	0.00384 (16)	0.00138 (13)
O13	0.0099 (2)	0.00714 (15)	0.0100 (2)	0.00111 (15)	0.00352 (16)	0.00122 (14)
O14	0.0102 (2)	0.00871 (16)	0.0078 (2)	0.00283 (16)	0.00056 (15)	0.00028 (14)
O15	0.0066 (2)	0.01356 (19)	0.00748 (19)	0.00152 (16)	0.00037 (14)	−0.00173 (15)
O16	0.0061 (2)	0.00849 (16)	0.0103 (2)	−0.00113 (15)	0.00190 (15)	−0.00327 (14)
N1	0.0072 (2)	0.00792 (17)	0.0086 (2)	0.00072 (16)	0.00047 (16)	−0.00023 (15)
N2	0.0075 (2)	0.00694 (16)	0.0066 (2)	−0.00058 (16)	0.00081 (15)	0.00014 (14)
C1	0.0090 (3)	0.00697 (19)	0.0084 (2)	0.00046 (18)	0.00024 (18)	0.00005 (16)
C2	0.0097 (3)	0.0085 (2)	0.0089 (2)	0.00086 (19)	0.00172 (19)	0.00043 (17)
C3	0.0084 (3)	0.0081 (2)	0.0092 (2)	0.00001 (19)	0.00145 (19)	−0.00051 (17)
C4	0.0093 (3)	0.0087 (2)	0.0098 (3)	−0.00013 (19)	0.00159 (19)	−0.00063 (17)
C5	0.0083 (3)	0.00747 (19)	0.0096 (3)	0.00043 (19)	0.00079 (19)	−0.00031 (17)
C6	0.0110 (3)	0.0091 (2)	0.0068 (2)	0.0016 (2)	0.00107 (19)	0.00019 (17)
C7	0.0087 (3)	0.0083 (2)	0.0081 (2)	−0.00037 (19)	0.00128 (18)	−0.00026 (17)
C8	0.0111 (3)	0.0088 (2)	0.0075 (2)	−0.0002 (2)	−0.00033 (19)	0.00010 (17)
C9	0.0134 (3)	0.0101 (2)	0.0096 (3)	0.0039 (2)	0.0001 (2)	−0.00108 (19)
C10	0.0106 (3)	0.0079 (2)	0.0093 (3)	0.00107 (19)	−0.00006 (19)	0.00055 (17)
C11	0.0094 (3)	0.0100 (2)	0.0082 (2)	0.0014 (2)	0.00231 (19)	−0.00013 (17)
C12	0.0064 (3)	0.0095 (2)	0.0106 (3)	0.00048 (19)	0.00168 (19)	0.00009 (18)
C13	0.0077 (3)	0.00783 (19)	0.0087 (2)	−0.00184 (18)	0.00153 (18)	−0.00061 (16)
C14	0.0096 (3)	0.00705 (19)	0.0087 (2)	−0.00052 (19)	0.00240 (19)	0.00100 (16)
C15	0.0076 (3)	0.00671 (19)	0.0103 (3)	0.00104 (18)	0.00149 (19)	0.00030 (17)
C16	0.0096 (3)	0.00767 (19)	0.0077 (2)	−0.00027 (18)	0.00125 (19)	−0.00098 (16)
C17	0.0075 (3)	0.0102 (2)	0.0107 (3)	0.0020 (2)	0.00155 (19)	0.00138 (18)
C18	0.0105 (3)	0.0079 (2)	0.0117 (3)	0.0023 (2)	0.0032 (2)	0.00128 (18)
C19	0.0126 (3)	0.0083 (2)	0.0128 (3)	0.0020 (2)	0.0042 (2)	0.00326 (19)
C20	0.0122 (3)	0.0120 (2)	0.0086 (3)	0.0032 (2)	0.0016 (2)	0.00339 (19)
C21	0.0124 (3)	0.0090 (2)	0.0074 (2)	0.0018 (2)	0.0012 (2)	0.00024 (17)
C22	0.0097 (3)	0.0100 (2)	0.0090 (2)	0.0010 (2)	0.00341 (19)	0.00176 (18)
C23	0.0090 (3)	0.0099 (2)	0.0118 (3)	0.0012 (2)	0.0008 (2)	−0.00348 (19)
C24	0.0081 (3)	0.0141 (2)	0.0088 (3)	0.0002 (2)	0.00127 (19)	−0.00302 (19)
C25	0.0080 (3)	0.0098 (2)	0.0086 (2)	−0.00045 (19)	−0.00017 (18)	−0.00194 (18)
C26	0.0080 (3)	0.0087 (2)	0.0111 (3)	−0.00156 (19)	0.00127 (19)	−0.00210 (18)
C27	0.0071 (3)	0.0102 (2)	0.0103 (3)	−0.00060 (19)	0.00176 (19)	−0.00207 (18)
C28	0.0073 (3)	0.0085 (2)	0.0095 (2)	0.00091 (19)	0.00077 (18)	−0.00069 (17)

Geometric parameters (Å, º)

Cr1—C1	1.9002 (7)	N2—C22	1.4744 (9)
Cr1—C2	1.9029 (8)	N2—C28	1.4688 (10)
Cr1—C3	1.8985 (7)	C11—C12	1.5173 (10)
Cr1—C4	1.8970 (8)	C11—H1A	1.004 (17)
Cr1—C5	1.8487 (7)	C11—H1B	0.989 (16)
Cr1—H	1.81 (2)	C12—H1C	0.955 (16)
Cr2—C6	1.8994 (8)	C12—H1D	1.029 (16)
Cr2—C7	1.8964 (7)	C13—C14	1.5011 (11)
Cr2—C8	1.8964 (8)	C13—H1E	0.940 (17)
Cr2—C9	1.9077 (8)	C13—H1F	0.992 (16)
Cr2—C10	1.8456 (7)	C14—H1G	1.002 (16)
Cr2—H	1.61 (2)	C14—H1H	0.993 (15)
K1—O1	2.9670 (6)	C15—C16	1.5154 (10)
K1—O11	2.8633 (6)	C15—H1I	0.942 (16)
K1—O12	2.8611 (5)	C15—H1J	0.981 (17)
K1—O13	2.8015 (6)	C16—H1K	0.975 (16)
K1—O14	2.7975 (6)	C16—H1L	0.999 (17)
K1—O15	2.8777 (6)	C17—C18	1.5166 (11)
K1—O16	2.8402 (6)	C17—H1M	0.965 (14)
K1—N1	3.0127 (7)	C17—H1N	0.969 (17)
K1—N2	3.0091 (6)	C18—H1O	0.965 (18)
O1—C1	1.1493 (9)	C18—H1P	1.006 (14)
O2—C2	1.1481 (10)	C19—C20	1.5062 (11)
O3—C3	1.1494 (9)	C19—H1Q	0.952 (16)
O4—C4	1.1478 (10)	C19—H1R	0.985 (18)
O5—C5	1.1582 (9)	C20—H2A	0.950 (18)
O6—C6	1.1469 (10)	C20—H2B	0.981 (19)
O7—C7	1.1507 (9)	C21—C22	1.5130 (11)
O8—C8	1.1507 (10)	C21—H2C	0.965 (18)
O9—C9	1.1456 (10)	C21—H2D	0.947 (16)
O10—C10	1.1601 (9)	C22—H2E	0.994 (17)
O11—C12	1.4181 (9)	C22—H2F	1.017 (15)
O11—C13	1.4305 (8)	C23—C24	1.5150 (12)
O12—C14	1.4201 (9)	C23—H2G	0.934 (16)
O12—C15	1.4234 (9)	C23—H2H	1.066 (19)
O13—C18	1.4181 (9)	C24—H2I	0.985 (18)
O13—C19	1.4216 (9)	C24—H2J	0.935 (19)
O14—C20	1.4224 (10)	C25—C26	1.5041 (11)
O14—C21	1.4303 (9)	C25—H2K	0.950 (18)
O15—C24	1.4280 (10)	C25—H2L	0.955 (15)
O15—C25	1.4190 (10)	C26—H2M	0.964 (18)
O16—C26	1.4264 (9)	C26—H2N	0.941 (17)
O16—C27	1.4237 (9)	C27—C28	1.5151 (10)
N1—C11	1.4711 (10)	C27—H2O	0.980 (16)
N1—C17	1.4731 (10)	C27—H2P	1.025 (16)
N1—C23	1.4714 (10)	C28—H2Q	1.008 (17)
N2—C16	1.4716 (9)	C28—H2R	0.949 (15)
C1—Cr1—C2	91.95 (3)	N1—C11—H1A	109.5 (10)
C1—Cr1—H	95.0 (7)	N1—C11—H1B	109.0 (10)
C2—Cr1—H	79.2 (7)	C12—C11—H1A	109.6 (10)
C3—Cr1—C1	174.92 (3)	C12—C11—H1B	108.8 (10)
C3—Cr1—C2	92.98 (3)	H1A—C11—H1B	105.0 (14)
C3—Cr1—H	84.7 (7)	O11—C12—C11	110.33 (6)
C4—Cr1—C1	89.79 (3)	O11—C12—H1C	109.9 (10)
C4—Cr1—C2	175.04 (3)	O11—C12—H1D	110.3 (9)
C4—Cr1—C3	85.20 (3)	C11—C12—H1C	110.6 (10)
C4—Cr1—H	96.0 (7)	C11—C12—H1D	108.8 (9)
C5—Cr1—C1	89.95 (3)	H1C—C12—H1D	106.8 (13)
C5—Cr1—C2	90.16 (3)	O11—C13—C14	109.61 (6)
C5—Cr1—C3	91.28 (3)	O11—C13—H1E	112.6 (10)
C5—Cr1—C4	94.49 (3)	O11—C13—H1F	112.1 (9)
C5—Cr1—H	168.4 (7)	C14—C13—H1E	109.7 (11)
C6—Cr2—C9	88.72 (3)	C14—C13—H1F	107.3 (9)
C6—Cr2—H	83.0 (7)	H1E—C13—H1F	105.4 (14)
C7—Cr2—C6	89.98 (3)	O12—C14—C13	108.66 (6)
C7—Cr2—C8	92.00 (3)	O12—C14—H1G	112.2 (9)
C7—Cr2—C9	171.12 (3)	O12—C14—H1H	109.9 (9)
C7—Cr2—H	83.4 (7)	C13—C14—H1G	106.8 (9)
C8—Cr2—C6	176.31 (3)	C13—C14—H1H	108.4 (9)
C8—Cr2—C9	89.79 (3)	H1G—C14—H1H	110.8 (13)
C8—Cr2—H	100.3 (7)	O12—C15—C16	108.76 (6)
C9—Cr2—H	87.8 (7)	O12—C15—H1I	110.3 (10)
C10—Cr2—C6	90.15 (3)	O12—C15—H1J	111.0 (10)
C10—Cr2—C7	93.60 (3)	C16—C15—H1I	107.0 (10)
C10—Cr2—C8	86.62 (3)	C16—C15—H1J	113.6 (10)
C10—Cr2—C9	95.18 (3)	H1I—C15—H1J	106.1 (14)
C10—Cr2—H	172.5 (8)	N2—C16—C15	114.02 (6)
O1—K1—N1	90.405 (18)	N2—C16—H1K	108.8 (10)
O1—K1—N2	91.997 (18)	N2—C16—H1L	109.9 (10)
O11—K1—O1	72.008 (18)	C15—C16—H1K	105.8 (10)
O11—K1—O15	99.512 (17)	C15—C16—H1L	108.5 (10)
O11—K1—N1	62.046 (16)	H1K—C16—H1L	109.6 (14)
O11—K1—N2	117.254 (16)	N1—C17—C18	113.80 (7)
O12—K1—O1	65.078 (17)	N1—C17—H1M	106.4 (9)
O12—K1—O11	58.952 (16)	N1—C17—H1N	110.2 (10)
O12—K1—O15	137.735 (18)	C18—C17—H1M	104.8 (9)
O12—K1—N1	120.463 (18)	C18—C17—H1N	110.8 (10)
O12—K1—N2	59.330 (16)	H1M—C17—H1N	110.7 (14)
O13—K1—O1	64.103 (17)	O13—C18—C17	109.09 (6)
O13—K1—O11	104.451 (17)	O13—C18—H1O	112.3 (11)
O13—K1—O12	129.180 (18)	O13—C18—H1P	108.3 (8)
O13—K1—O15	89.424 (17)	C17—C18—H1O	107.7 (11)
O13—K1—O16	128.585 (17)	C17—C18—H1P	112.8 (8)
O13—K1—N1	60.334 (17)	H1O—C18—H1P	106.7 (13)
O13—K1—N2	122.268 (17)	O13—C19—C20	108.80 (6)
O14—K1—O1	74.515 (18)	O13—C19—H1Q	108.3 (10)
O14—K1—O11	146.474 (18)	O13—C19—H1R	110.0 (11)
O14—K1—O12	104.650 (17)	C20—C19—H1Q	112.1 (10)
O14—K1—O13	61.242 (17)	C20—C19—H1R	109.5 (11)
O14—K1—O15	109.843 (18)	H1Q—C19—H1R	108.1 (15)
O14—K1—O16	90.390 (18)	O14—C20—C19	109.89 (6)
O14—K1—N1	120.378 (17)	O14—C20—H2A	111.4 (11)
O14—K1—N2	61.911 (16)	O14—C20—H2B	110.4 (11)
O15—K1—O1	147.800 (18)	C19—C20—H2A	107.7 (11)
O15—K1—N1	59.298 (17)	C19—C20—H2B	105.3 (11)
O15—K1—N2	118.648 (18)	H2A—C20—H2B	111.8 (15)
O16—K1—O1	152.202 (18)	O14—C21—C22	109.26 (6)
O16—K1—O11	119.159 (17)	O14—C21—H2C	111.1 (11)
O16—K1—O12	97.621 (17)	O14—C21—H2D	109.2 (10)
O16—K1—O15	59.198 (16)	C22—C21—H2C	109.5 (11)
O16—K1—N1	117.390 (17)	C22—C21—H2D	111.6 (10)
O16—K1—N2	60.208 (16)	H2C—C21—H2D	106.1 (14)
N2—K1—N1	177.104 (18)	N2—C22—C21	113.11 (6)
C1—O1—K1	148.80 (6)	N2—C22—H2E	109.2 (10)
C12—O11—K1	111.64 (4)	N2—C22—H2F	110.7 (9)
C12—O11—C13	110.12 (6)	C21—C22—H2E	107.8 (10)
C13—O11—K1	113.80 (4)	C21—C22—H2F	106.9 (9)
C14—O12—K1	117.70 (4)	H2E—C22—H2F	109.0 (13)
C14—O12—C15	111.65 (5)	N1—C23—C24	113.30 (6)
C15—O12—K1	121.07 (4)	N1—C23—H2G	108.1 (10)
C18—O13—K1	121.06 (4)	N1—C23—H2H	111.5 (10)
C18—O13—C19	111.78 (5)	C24—C23—H2G	107.1 (10)
C19—O13—K1	113.66 (4)	C24—C23—H2H	110.2 (10)
C20—O14—K1	113.69 (4)	H2G—C23—H2H	106.4 (14)
C20—O14—C21	110.54 (6)	O15—C24—C23	108.48 (6)
C21—O14—K1	112.07 (4)	O15—C24—H2I	107.4 (10)
C24—O15—K1	115.75 (5)	O15—C24—H2J	110.2 (12)
C25—O15—K1	117.12 (4)	C23—C24—H2I	114.4 (10)
C25—O15—C24	111.05 (6)	C23—C24—H2J	109.5 (11)
C26—O16—K1	112.74 (4)	H2I—C24—H2J	106.8 (15)
C27—O16—K1	120.16 (4)	O15—C25—C26	109.15 (6)
C27—O16—C26	110.39 (6)	O15—C25—H2K	112.7 (10)
C11—N1—K1	107.42 (4)	O15—C25—H2L	111.2 (9)
C11—N1—C17	110.00 (6)	C26—C25—H2K	108.1 (10)
C11—N1—C23	109.19 (6)	C26—C25—H2L	112.4 (9)
C17—N1—K1	107.38 (4)	H2K—C25—H2L	103.2 (14)
C23—N1—K1	112.33 (5)	O16—C26—C25	109.39 (6)
C23—N1—C17	110.46 (6)	O16—C26—H2M	109.5 (10)
C16—N2—K1	109.93 (4)	O16—C26—H2N	111.7 (10)
C16—N2—C22	109.37 (6)	C25—C26—H2M	114.4 (11)
C22—N2—K1	107.72 (4)	C25—C26—H2N	107.2 (10)
C28—N2—K1	108.78 (4)	H2M—C26—H2N	104.5 (15)
C28—N2—C16	109.74 (6)	O16—C27—C28	110.35 (6)
C28—N2—C22	111.27 (6)	O16—C27—H2O	110.2 (10)
O1—C1—Cr1	177.01 (7)	O16—C27—H2P	108.3 (9)
O2—C2—Cr1	178.87 (7)	C28—C27—H2O	111.9 (10)
O3—C3—Cr1	176.02 (7)	C28—C27—H2P	107.7 (9)
O4—C4—Cr1	177.88 (7)	H2O—C27—H2P	108.3 (13)
O5—C5—Cr1	177.76 (7)	N2—C28—C27	114.07 (6)
O6—C6—Cr2	178.73 (7)	N2—C28—H2Q	109.5 (10)
O7—C7—Cr2	178.66 (7)	N2—C28—H2R	109.6 (9)
O8—C8—Cr2	174.71 (7)	C27—C28—H2Q	110.2 (10)
O9—C9—Cr2	178.54 (8)	C27—C28—H2R	107.7 (9)
O10—C10—Cr2	178.00 (8)	H2Q—C28—H2R	105.4 (13)
N1—C11—C12	114.50 (6)
K1—O11—C12—C11	−56.13 (6)	N1—C23—C24—O15	63.08 (8)
K1—O11—C13—C14	53.28 (6)	C11—N1—C17—C18	−166.46 (6)
K1—O12—C14—C13	42.37 (7)	C11—N1—C23—C24	81.51 (8)
K1—O12—C15—C16	−41.10 (7)	C12—O11—C13—C14	179.50 (6)
K1—O13—C18—C17	−40.89 (8)	C13—O11—C12—C11	176.44 (6)
K1—O13—C19—C20	49.43 (8)	C14—O12—C15—C16	173.52 (6)
K1—O14—C20—C19	47.95 (7)	C15—O12—C14—C13	−170.96 (6)
K1—O14—C21—C22	−59.88 (7)	C16—N2—C22—C21	80.21 (7)
K1—O15—C24—C23	−56.15 (7)	C16—N2—C28—C27	−168.94 (6)
K1—O15—C25—C26	37.93 (7)	C17—N1—C11—C12	75.44 (8)
K1—O16—C26—C25	57.45 (7)	C17—N1—C23—C24	−157.40 (7)
K1—O16—C27—C28	−39.30 (7)	C18—O13—C19—C20	−169.17 (7)
K1—N1—C11—C12	−41.13 (7)	C19—O13—C18—C17	−179.04 (7)
K1—N1—C17—C18	−49.86 (7)	C20—O14—C21—C22	172.17 (6)
K1—N1—C23—C24	−37.54 (8)	C21—O14—C20—C19	175.00 (6)
K1—N2—C16—C15	−48.38 (7)	C22—N2—C16—C15	−166.46 (6)
K1—N2—C22—C21	−39.24 (7)	C22—N2—C28—C27	69.87 (8)
K1—N2—C28—C27	−48.64 (7)	C23—N1—C11—C12	−163.19 (6)
O11—C13—C14—O12	−63.39 (7)	C23—N1—C17—C18	72.94 (8)
O12—C15—C16—N2	60.52 (8)	C24—O15—C25—C26	173.99 (6)
O13—C19—C20—O14	−66.04 (9)	C25—O15—C24—C23	167.14 (6)
O14—C21—C22—N2	69.54 (8)	C26—O16—C27—C28	−173.15 (6)
O15—C25—C26—O16	−63.68 (8)	C27—O16—C26—C25	−165.09 (6)
O16—C27—C28—N2	60.55 (8)	C28—N2—C16—C15	71.21 (8)
N1—C11—C12—O11	69.67 (8)	C28—N2—C22—C21	−158.39 (6)
N1—C17—C18—O13	62.44 (8)

(KCPTCR_IAM_NoMoRe)

Crystal data

C28H37Cr2KN2O16	F(000) = 1660.538
Mr = 800.70	Dx = 1.489 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71069 Å
a = 10.458 Å	Cell parameters from 1024 reflections
b = 14.417 Å	θ = 47.5–1.5°
c = 23.882 Å	µ = 0.80 mm^−1
β = 97.26°	T = 28 K
V = 3571.89 Å^3	Ellipsoidal, yellow
Z = 4	0.3 × 0.25 × 0.2 mm

Data collection

SMART CCD diffractometer	22531 reflections with I ≥ 2u(I)
ω scan	Rint = 0.0000
Absorption correction: empirical (using intensity measurements)	θmax = 48.7°, θmin = 2.4°
Tmin = 0.890, Tmax = 0.903	h = −19→20
27917 measured reflections	k = 0→30
27917 independent reflections	l = 0→50

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.036	Only H-atom coordinates refined
wR(F^2) = 0.086	w = 1/[σ^2(Fo^2) + (0.0385P)^2 + 0.7612P] where P = (Fo^2 + 2Fc^2)/3
S = 1.00	(Δ/σ)max = 0.001
27917 reflections	Δρmax = 0.88 e Å^−3
553 parameters	Δρmin = −0.94 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Cr1	0.163871 (11)	0.002357 (7)	0.236370 (4)	0.005266 (17)
Cr2	0.018768 (11)	0.177450 (7)	0.165109 (4)	0.005822 (18)
K1	0.463722 (14)	0.199287 (9)	0.418003 (6)	0.00651 (2)
O1	0.25211 (6)	0.13817 (4)	0.33124 (2)	0.01182 (9)
O2	−0.08359 (6)	−0.04363 (4)	0.28579 (3)	0.01424 (10)
O3	0.10475 (6)	−0.12663 (4)	0.13543 (3)	0.01256 (9)
O4	0.39537 (6)	0.05453 (4)	0.17748 (3)	0.01366 (10)
O5	0.30040 (6)	−0.15038 (4)	0.30579 (3)	0.01221 (9)
O6	−0.25967 (6)	0.12160 (4)	0.17224 (3)	0.01248 (9)
O7	0.01690 (6)	0.05854 (4)	0.05956 (2)	0.01256 (9)
O8	0.28638 (6)	0.25368 (4)	0.15523 (3)	0.01339 (10)
O9	0.02666 (8)	0.26557 (5)	0.28175 (3)	0.01773 (12)
O10	−0.07209 (7)	0.34768 (4)	0.09918 (3)	0.01453 (10)
O11	0.28601 (5)	0.09223 (3)	0.47319 (2)	0.00782 (7)
O12	0.44336 (6)	0.00289 (3)	0.40242 (2)	0.00835 (8)
O13	0.31320 (6)	0.34079 (3)	0.36297 (2)	0.00877 (8)
O14	0.52829 (6)	0.26684 (4)	0.31543 (2)	0.00895 (8)
O15	0.55084 (5)	0.32677 (4)	0.50748 (2)	0.00926 (8)
O16	0.72701 (5)	0.20502 (4)	0.46502 (2)	0.00822 (8)
N1	0.27326 (6)	0.30193 (4)	0.47979 (3)	0.00792 (8)
N2	0.66164 (6)	0.09467 (4)	0.36197 (2)	0.00697 (8)
C1	0.21615 (7)	0.08852 (4)	0.29500 (3)	0.00811 (9)
C2	0.01018 (7)	−0.02685 (5)	0.26764 (3)	0.00901 (10)
C3	0.12293 (7)	−0.07908 (5)	0.17422 (3)	0.00845 (10)
C4	0.30792 (8)	0.03662 (5)	0.20004 (3)	0.00922 (10)
C5	0.25013 (7)	−0.09110 (4)	0.27860 (3)	0.00841 (10)
C6	−0.15430 (8)	0.14184 (5)	0.16996 (3)	0.00897 (10)
C7	0.01871 (7)	0.10415 (5)	0.09919 (3)	0.00834 (10)
C8	0.18802 (8)	0.22109 (5)	0.16012 (3)	0.00935 (10)
C9	0.02398 (8)	0.23361 (5)	0.23771 (3)	0.01110 (11)
C10	−0.03864 (8)	0.28232 (5)	0.12531 (3)	0.00933 (10)
C11	0.20813 (8)	0.23292 (5)	0.51164 (3)	0.00912 (10)
C12	0.17306 (7)	0.14352 (5)	0.47990 (3)	0.00870 (10)
C13	0.25206 (7)	0.00540 (4)	0.44640 (3)	0.00801 (9)
C14	0.37225 (7)	−0.04782 (4)	0.43913 (3)	0.00831 (10)
C15	0.54827 (7)	−0.04995 (4)	0.38669 (3)	0.00809 (9)
C16	0.60989 (7)	0.00363 (4)	0.34253 (3)	0.00821 (9)
C17	0.17928 (7)	0.34656 (5)	0.43697 (3)	0.00946 (10)
C18	0.24064 (8)	0.40169 (5)	0.39332 (3)	0.00989 (10)
C19	0.37497 (8)	0.38880 (5)	0.32178 (3)	0.01096 (11)
C20	0.42797 (8)	0.31883 (5)	0.28400 (3)	0.01090 (11)
C21	0.57214 (8)	0.19476 (5)	0.28131 (3)	0.00953 (10)
C22	0.69030 (8)	0.14951 (5)	0.31296 (3)	0.00930 (10)
C23	0.33599 (8)	0.37154 (5)	0.51921 (3)	0.01025 (10)
C24	0.46522 (8)	0.34033 (5)	0.54888 (3)	0.01037 (10)
C25	0.68014 (7)	0.31745 (5)	0.53317 (3)	0.00882 (10)
C26	0.76442 (7)	0.29320 (5)	0.48874 (3)	0.00922 (10)
C27	0.82399 (7)	0.16969 (5)	0.43395 (3)	0.00904 (10)
C28	0.77750 (7)	0.08192 (5)	0.40291 (3)	0.00843 (10)
H	0.0509 (16)	0.0771 (12)	0.1996 (8)	0.033652
H1A	0.1264 (16)	0.2602 (11)	0.5230 (7)	0.025013
H1B	0.2640 (16)	0.2184 (11)	0.5468 (7)	0.023076
H1C	0.1261 (15)	0.1559 (11)	0.4426 (7)	0.023746
H1D	0.1131 (15)	0.1061 (11)	0.5023 (7)	0.024598
H1E	0.2009 (16)	0.0142 (11)	0.4101 (7)	0.022215
H1F	0.1988 (15)	−0.0319 (11)	0.4683 (7)	0.023329
H1G	0.3438 (16)	−0.1095 (11)	0.4227 (7)	0.025071
H1H	0.4233 (15)	−0.0555 (11)	0.4771 (7)	0.024233
H1I	0.5173 (15)	−0.1075 (11)	0.3701 (7)	0.022451
H1J	0.6092 (15)	−0.0656 (11)	0.4203 (7)	0.021710
H1K	0.5434 (16)	0.0132 (11)	0.3109 (7)	0.022322
H1L	0.6781 (15)	−0.0348 (11)	0.3289 (7)	0.023001
H1M	0.1297 (15)	0.2983 (11)	0.4165 (7)	0.024511
H1N	0.1208 (16)	0.3856 (12)	0.4541 (7)	0.026678
H1O	0.1718 (16)	0.4294 (12)	0.3687 (7)	0.027525
H1P	0.2999 (16)	0.4515 (11)	0.4123 (7)	0.026323
H1Q	0.4421 (16)	0.4264 (11)	0.3403 (7)	0.027823
H1R	0.3111 (16)	0.4279 (12)	0.2977 (7)	0.029725
H2A	0.3601 (16)	0.2801 (12)	0.2690 (7)	0.026016
H2B	0.4618 (16)	0.3525 (12)	0.2542 (7)	0.028356
H2C	0.5924 (16)	0.2200 (12)	0.2450 (7)	0.025505
H2D	0.5063 (16)	0.1519 (11)	0.2723 (7)	0.024538
H2E	0.7304 (16)	0.1082 (11)	0.2854 (7)	0.025760
H2F	0.7512 (15)	0.2006 (11)	0.3256 (7)	0.024185
H2G	0.3487 (15)	0.4259 (11)	0.4977 (7)	0.025234
H2H	0.2768 (16)	0.3915 (12)	0.5487 (7)	0.026839
H2I	0.4614 (16)	0.2823 (12)	0.5709 (7)	0.026520
H2J	0.4955 (16)	0.3870 (12)	0.5752 (7)	0.027507
H2K	0.7122 (15)	0.3742 (11)	0.5513 (7)	0.024028
H2L	0.6877 (16)	0.2707 (11)	0.5627 (7)	0.023835
H2M	0.7620 (17)	0.3391 (11)	0.4590 (7)	0.025301
H2N	0.8540 (15)	0.2914 (12)	0.5076 (7)	0.026087
H2O	0.8490 (16)	0.2168 (11)	0.4080 (7)	0.025953
H2P	0.9037 (15)	0.1544 (12)	0.4615 (7)	0.027682
H2Q	0.8465 (15)	0.0550 (12)	0.3843 (7)	0.024815
H2R	0.7610 (15)	0.0362 (11)	0.4297 (7)	0.022425

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cr1	0.00571 (4)	0.00467 (3)	0.00540 (4)	0.00013 (3)	0.00063 (3)	−0.00017 (3)
Cr2	0.00674 (4)	0.00538 (3)	0.00521 (4)	0.00077 (3)	0.00024 (3)	0.00014 (3)
K1	0.00619 (5)	0.00667 (4)	0.00659 (5)	0.00019 (4)	0.00057 (4)	−0.00005 (3)
O1	0.0151 (3)	0.00928 (17)	0.0101 (2)	0.00005 (17)	−0.00208 (17)	−0.00223 (15)
O2	0.0112 (3)	0.0163 (2)	0.0162 (3)	0.00030 (19)	0.00561 (19)	0.00138 (19)
O3	0.0146 (3)	0.01241 (19)	0.0107 (2)	−0.00208 (18)	0.00173 (18)	−0.00445 (16)
O4	0.0115 (3)	0.0136 (2)	0.0170 (3)	−0.00063 (19)	0.00617 (19)	−0.00014 (18)
O5	0.0133 (3)	0.00929 (17)	0.0135 (2)	0.00317 (17)	−0.00057 (18)	0.00215 (16)
O6	0.0108 (2)	0.0147 (2)	0.0124 (2)	−0.00063 (18)	0.00335 (18)	0.00010 (17)
O7	0.0163 (3)	0.01234 (19)	0.0093 (2)	−0.00155 (19)	0.00270 (18)	−0.00279 (16)
O8	0.0120 (3)	0.0158 (2)	0.0121 (2)	−0.00449 (19)	0.00027 (18)	0.00057 (17)
O9	0.0256 (3)	0.0171 (2)	0.0096 (2)	0.0097 (2)	−0.0012 (2)	−0.00446 (18)
O10	0.0176 (3)	0.00996 (19)	0.0151 (3)	0.00287 (19)	−0.0018 (2)	0.00387 (17)
O11	0.0060 (2)	0.00716 (15)	0.0103 (2)	0.00006 (14)	0.00092 (14)	−0.00173 (14)
O12	0.0085 (2)	0.00670 (15)	0.0106 (2)	0.00104 (15)	0.00396 (15)	0.00145 (14)
O13	0.0098 (2)	0.00710 (15)	0.0099 (2)	0.00116 (15)	0.00348 (16)	0.00124 (14)
O14	0.0102 (2)	0.00875 (16)	0.00780 (19)	0.00286 (15)	0.00062 (15)	0.00027 (14)
O15	0.0066 (2)	0.01359 (19)	0.00748 (19)	0.00154 (16)	0.00031 (14)	−0.00174 (15)
O16	0.0061 (2)	0.00852 (16)	0.0103 (2)	−0.00111 (15)	0.00187 (15)	−0.00323 (14)
N1	0.0073 (2)	0.00793 (17)	0.0084 (2)	0.00065 (16)	0.00032 (16)	−0.00019 (15)
N2	0.0075 (2)	0.00689 (16)	0.0065 (2)	−0.00050 (16)	0.00076 (15)	0.00021 (14)
C1	0.0087 (3)	0.00708 (19)	0.0084 (2)	0.00045 (18)	0.00040 (18)	0.00021 (16)
C2	0.0100 (3)	0.0084 (2)	0.0087 (2)	0.00109 (19)	0.00160 (19)	0.00050 (17)
C3	0.0081 (3)	0.0082 (2)	0.0092 (2)	−0.00011 (19)	0.00138 (19)	−0.00040 (17)
C4	0.0094 (3)	0.0085 (2)	0.0098 (3)	0.00000 (19)	0.00115 (19)	−0.00072 (17)
C5	0.0081 (3)	0.00741 (19)	0.0096 (2)	0.00039 (18)	0.00087 (19)	−0.00040 (17)
C6	0.0113 (3)	0.0090 (2)	0.0066 (2)	0.0016 (2)	0.00101 (19)	0.00032 (17)
C7	0.0085 (3)	0.0084 (2)	0.0083 (2)	−0.00046 (19)	0.00147 (18)	0.00010 (17)
C8	0.0115 (3)	0.0089 (2)	0.0073 (2)	−0.0001 (2)	−0.00044 (19)	−0.00004 (17)
C9	0.0132 (3)	0.0100 (2)	0.0098 (3)	0.0038 (2)	0.0000 (2)	−0.00090 (19)
C10	0.0105 (3)	0.0080 (2)	0.0091 (3)	0.00094 (19)	−0.00004 (19)	0.00041 (17)
C11	0.0095 (3)	0.0099 (2)	0.0082 (2)	0.0014 (2)	0.00231 (19)	−0.00008 (17)
C12	0.0063 (3)	0.0094 (2)	0.0106 (3)	0.00041 (19)	0.00151 (19)	0.00010 (18)
C13	0.0077 (3)	0.00768 (19)	0.0087 (2)	−0.00183 (18)	0.00146 (18)	−0.00062 (17)
C14	0.0094 (3)	0.00707 (19)	0.0088 (2)	−0.00043 (19)	0.00248 (19)	0.00098 (17)
C15	0.0075 (3)	0.00670 (18)	0.0102 (3)	0.00114 (18)	0.00163 (19)	0.00036 (17)
C16	0.0093 (3)	0.00772 (19)	0.0077 (2)	−0.00025 (19)	0.00133 (18)	−0.00101 (16)
C17	0.0076 (3)	0.0102 (2)	0.0107 (3)	0.0021 (2)	0.00158 (19)	0.00144 (18)
C18	0.0104 (3)	0.0079 (2)	0.0118 (3)	0.0023 (2)	0.0031 (2)	0.00120 (18)
C19	0.0125 (3)	0.0083 (2)	0.0127 (3)	0.0019 (2)	0.0042 (2)	0.00328 (19)
C20	0.0121 (3)	0.0120 (2)	0.0087 (3)	0.0033 (2)	0.0017 (2)	0.00343 (19)
C21	0.0125 (3)	0.0089 (2)	0.0072 (2)	0.0018 (2)	0.00121 (19)	0.00024 (17)
C22	0.0096 (3)	0.0098 (2)	0.0090 (2)	0.0010 (2)	0.00335 (19)	0.00187 (18)
C23	0.0088 (3)	0.0099 (2)	0.0120 (3)	0.0013 (2)	0.0008 (2)	−0.00353 (19)
C24	0.0081 (3)	0.0142 (2)	0.0089 (3)	0.0004 (2)	0.00126 (19)	−0.00307 (19)
C25	0.0078 (3)	0.0099 (2)	0.0084 (2)	−0.00041 (19)	−0.00026 (18)	−0.00191 (18)
C26	0.0081 (3)	0.0087 (2)	0.0109 (3)	−0.00156 (19)	0.00127 (19)	−0.00218 (18)
C27	0.0068 (3)	0.0103 (2)	0.0102 (3)	−0.00049 (19)	0.00177 (19)	−0.00202 (18)
C28	0.0073 (3)	0.0086 (2)	0.0093 (2)	0.00095 (19)	0.00064 (18)	−0.00070 (17)
H	0.027000	0.026000	0.046000	0.004000	−0.003000	0.018000
H1A	0.023000	0.023000	0.032000	0.005000	0.015000	−0.000000
H1B	0.028000	0.024000	0.016000	0.000000	−0.002000	0.003000
H1C	0.022000	0.026000	0.021000	0.004000	−0.006000	0.001000
H1D	0.021000	0.022000	0.033000	−0.003000	0.012000	0.003000
H1E	0.022000	0.027000	0.016000	0.000000	−0.004000	−0.001000
H1F	0.026000	0.022000	0.024000	−0.009000	0.011000	−0.000000
H1G	0.033000	0.013000	0.031000	−0.006000	0.011000	−0.005000
H1H	0.026000	0.029000	0.017000	0.005000	0.000000	0.007000
H1I	0.027000	0.013000	0.028000	−0.003000	0.006000	−0.005000
H1J	0.019000	0.026000	0.019000	0.004000	−0.002000	0.006000
H1K	0.025000	0.023000	0.017000	−0.002000	−0.005000	0.001000
H1L	0.024000	0.020000	0.027000	0.004000	0.011000	−0.005000
H1M	0.021000	0.025000	0.026000	−0.006000	−0.003000	0.004000
H1N	0.025000	0.029000	0.028000	0.013000	0.011000	0.005000
H1O	0.025000	0.030000	0.028000	0.013000	0.005000	0.012000
H1P	0.034000	0.017000	0.029000	−0.006000	0.008000	−0.005000
H1Q	0.028000	0.021000	0.036000	−0.009000	0.010000	−0.005000
H1R	0.032000	0.030000	0.028000	0.016000	0.007000	0.014000
H2A	0.021000	0.029000	0.026000	−0.002000	−0.005000	−0.005000
H2B	0.035000	0.032000	0.020000	0.009000	0.011000	0.012000
H2C	0.036000	0.027000	0.015000	0.006000	0.009000	0.006000
H2D	0.024000	0.020000	0.028000	−0.004000	−0.003000	−0.004000
H2E	0.032000	0.026000	0.022000	0.010000	0.014000	0.001000
H2F	0.021000	0.022000	0.029000	−0.007000	0.001000	0.004000
H2G	0.028000	0.016000	0.031000	−0.002000	0.001000	0.003000
H2H	0.024000	0.031000	0.027000	0.003000	0.009000	−0.011000
H2I	0.027000	0.028000	0.025000	0.002000	0.005000	0.010000
H2J	0.026000	0.034000	0.022000	−0.002000	0.001000	−0.014000
H2K	0.025000	0.020000	0.026000	−0.003000	−0.001000	−0.010000
H2L	0.028000	0.024000	0.019000	0.003000	0.001000	0.007000
H2M	0.035000	0.018000	0.024000	−0.002000	0.008000	0.004000
H2N	0.014000	0.031000	0.032000	−0.002000	−0.002000	−0.010000
H2O	0.031000	0.022000	0.027000	−0.007000	0.012000	−0.000000
H2P	0.014000	0.034000	0.033000	0.004000	−0.005000	−0.009000
H2Q	0.017000	0.030000	0.028000	0.006000	0.005000	−0.008000
H2R	0.027000	0.019000	0.020000	−0.002000	−0.002000	0.005000

Geometric parameters (Å, º)

Cr1—C1	1.8997 (7)	N2—C22	1.4742 (9)
Cr1—C2	1.9031 (8)	N2—C28	1.4692 (9)
Cr1—C3	1.8984 (7)	C11—C12	1.5166 (10)
Cr1—C4	1.8965 (8)	C11—H1A	1.009 (16)
Cr1—C5	1.8483 (7)	C11—H1B	0.983 (15)
Cr1—H	1.751 (16)	C12—H1C	0.978 (15)
Cr2—C6	1.8989 (8)	C12—H1D	1.028 (15)
Cr2—C7	1.8961 (7)	C13—C14	1.5013 (10)
Cr2—C8	1.8964 (8)	C13—H1E	0.967 (16)
Cr2—C9	1.9081 (7)	C13—H1F	0.974 (15)
Cr2—C10	1.8454 (7)	C14—H1G	1.002 (15)
Cr2—H	1.678 (16)	C14—H1H	0.998 (15)
K1—O1	2.9679 (6)	C15—C16	1.5152 (10)
K1—O11	2.8622 (6)	C15—H1I	0.957 (15)
K1—O12	2.8603 (5)	C15—H1J	0.985 (15)
K1—O13	2.8008 (6)	C16—H1K	0.970 (15)
K1—O14	2.7970 (6)	C16—H1L	0.991 (15)
K1—O15	2.8779 (6)	C17—C18	1.5164 (10)
K1—O16	2.8403 (6)	C17—H1M	0.964 (16)
K1—N1	3.0129 (6)	C17—H1N	0.959 (16)
K1—N2	3.0083 (6)	C18—H1O	0.957 (16)
O1—C1	1.1492 (9)	C18—H1P	1.017 (16)
O2—C2	1.1470 (10)	C19—C20	1.5051 (11)
O3—C3	1.1488 (9)	C19—H1Q	0.951 (16)
O4—C4	1.1480 (10)	C19—H1R	0.999 (16)
O5—C5	1.1586 (9)	C20—H2A	0.939 (16)
O6—C6	1.1478 (10)	C20—H2B	0.964 (16)
O7—C7	1.1505 (9)	C21—C22	1.5126 (11)
O8—C8	1.1502 (10)	C21—H2C	0.988 (15)
O9—C9	1.1453 (10)	C21—H2D	0.930 (16)
O10—C10	1.1595 (9)	C22—H2E	1.016 (15)
O11—C12	1.4198 (9)	C22—H2F	0.995 (15)
O11—C13	1.4300 (8)	C23—C24	1.5128 (11)
O12—C14	1.4215 (8)	C23—H2G	0.956 (16)
O12—C15	1.4246 (9)	C23—H2H	1.037 (16)
O13—C18	1.4180 (9)	C24—H2I	0.992 (16)
O13—C19	1.4227 (9)	C24—H2J	0.947 (16)
O14—C20	1.4237 (9)	C25—C26	1.5039 (10)
O14—C21	1.4313 (9)	C25—H2K	0.965 (15)
O15—C24	1.4288 (9)	C25—H2L	0.970 (16)
O15—C25	1.4188 (9)	C26—H2M	0.968 (16)
O16—C26	1.4262 (8)	C26—H2N	0.987 (16)
O16—C27	1.4243 (9)	C27—C28	1.5153 (10)
N1—C11	1.4708 (9)	C27—H2O	0.977 (16)
N1—C17	1.4736 (10)	C27—H2P	1.019 (16)
N1—C23	1.4724 (9)	C28—H2Q	0.975 (15)
N2—C16	1.4722 (9)	C28—H2R	0.950 (15)
C2—Cr1—C1	91.96 (3)	H1A—C11—N1	109.8 (9)
C3—Cr1—C1	174.93 (3)	H1A—C11—C12	107.8 (10)
C3—Cr1—C2	92.96 (3)	H1B—C11—N1	108.8 (10)
C4—Cr1—C1	89.75 (3)	H1B—C11—C12	109.0 (10)
C4—Cr1—C2	175.04 (3)	H1B—C11—H1A	106.6 (14)
C4—Cr1—C3	85.25 (3)	C11—C12—O11	110.30 (6)
C5—Cr1—C1	89.96 (3)	H1C—C12—O11	108.8 (10)
C5—Cr1—C2	90.16 (3)	H1C—C12—C11	111.2 (10)
C5—Cr1—C3	91.26 (3)	H1D—C12—O11	110.9 (9)
C5—Cr1—C4	94.50 (3)	H1D—C12—C11	108.1 (9)
H—Cr1—C1	94.6 (6)	H1D—C12—H1C	107.5 (13)
H—Cr1—C2	77.5 (6)	C14—C13—O11	109.57 (6)
H—Cr1—C3	85.3 (6)	H1E—C13—O11	111.4 (10)
H—Cr1—C4	97.8 (6)	H1E—C13—C14	109.8 (10)
H—Cr1—C5	166.9 (6)	H1F—C13—O11	111.7 (9)
C7—Cr2—C6	89.98 (3)	H1F—C13—C14	108.9 (10)
C8—Cr2—C6	176.31 (3)	H1F—C13—H1E	105.4 (14)
C8—Cr2—C7	92.01 (3)	C13—C14—O12	108.63 (5)
C9—Cr2—C6	88.70 (3)	H1G—C14—O12	111.5 (9)
C9—Cr2—C7	171.10 (3)	H1G—C14—C13	106.7 (9)
C9—Cr2—C8	89.81 (3)	H1H—C14—O12	110.8 (9)
C10—Cr2—C6	90.13 (3)	H1H—C14—C13	108.1 (9)
C10—Cr2—C7	93.61 (3)	H1H—C14—H1G	110.9 (14)
C10—Cr2—C8	86.64 (3)	C16—C15—O12	108.68 (5)
C10—Cr2—C9	95.19 (3)	H1I—C15—O12	109.9 (10)
H—Cr2—C6	82.5 (6)	H1I—C15—C16	107.7 (10)
H—Cr2—C7	84.6 (7)	H1J—C15—O12	110.4 (9)
H—Cr2—C8	100.7 (6)	H1J—C15—C16	113.2 (9)
H—Cr2—C9	86.5 (7)	H1J—C15—H1I	106.8 (13)
H—Cr2—C10	172.4 (6)	C15—C16—N2	114.01 (6)
O11—K1—O1	72.005 (16)	H1K—C16—N2	108.5 (9)
O12—K1—O1	65.075 (16)	H1K—C16—C15	106.7 (10)
O12—K1—O11	58.941 (15)	H1L—C16—N2	110.6 (9)
O13—K1—O1	64.110 (16)	H1L—C16—C15	109.3 (9)
O13—K1—O11	104.461 (16)	H1L—C16—H1K	107.4 (14)
O13—K1—O12	129.185 (17)	C18—C17—N1	113.76 (6)
O14—K1—O1	74.524 (17)	H1M—C17—N1	107.8 (10)
O14—K1—O11	146.480 (17)	H1M—C17—C18	106.0 (10)
O14—K1—O12	104.652 (16)	H1N—C17—N1	111.5 (10)
O14—K1—O13	61.247 (16)	H1N—C17—C18	109.5 (10)
O15—K1—O1	147.797 (17)	H1N—C17—H1M	107.9 (14)
O15—K1—O11	99.530 (16)	C17—C18—O13	109.10 (5)
O15—K1—O12	137.749 (17)	H1O—C18—O13	110.7 (10)
O15—K1—O13	89.408 (16)	H1O—C18—C17	106.9 (10)
O15—K1—O14	109.824 (17)	H1P—C18—O13	109.2 (9)
O16—K1—O1	152.213 (17)	H1P—C18—C17	110.5 (9)
O16—K1—O11	119.151 (16)	H1P—C18—H1O	110.4 (14)
O16—K1—O12	97.629 (16)	C20—C19—O13	108.80 (6)
O16—K1—O13	128.578 (17)	H1Q—C19—O13	109.3 (10)
O16—K1—O14	90.390 (17)	H1Q—C19—C20	110.7 (10)
O16—K1—O15	59.189 (15)	H1R—C19—O13	110.1 (10)
N1—K1—O1	90.398 (17)	H1R—C19—C20	107.6 (10)
N1—K1—O11	62.059 (15)	H1R—C19—H1Q	110.3 (15)
N1—K1—O12	120.464 (17)	C19—C20—O14	109.85 (6)
N1—K1—O13	60.324 (16)	H2A—C20—O14	111.1 (10)
N1—K1—O14	120.373 (16)	H2A—C20—C19	108.1 (10)
N1—K1—O15	59.305 (16)	H2B—C20—O14	109.8 (10)
N1—K1—O16	117.386 (16)	H2B—C20—C19	107.6 (10)
N2—K1—O1	91.996 (17)	H2B—C20—H2A	110.4 (15)
N2—K1—O11	117.242 (15)	C22—C21—O14	109.20 (6)
N2—K1—O12	59.329 (16)	H2C—C21—O14	110.7 (10)
N2—K1—O13	122.271 (16)	H2C—C21—C22	110.2 (10)
N2—K1—O14	61.909 (16)	H2D—C21—O14	109.5 (10)
N2—K1—O15	118.649 (17)	H2D—C21—C22	111.3 (10)
N2—K1—O16	60.220 (16)	H2D—C21—H2C	106.0 (14)
N2—K1—N1	177.114 (17)	C21—C22—N2	113.13 (6)
C1—O1—K1	148.75 (5)	H2E—C22—N2	110.0 (9)
C12—O11—K1	111.66 (4)	H2E—C22—C21	107.9 (9)
C13—O11—K1	113.89 (4)	H2F—C22—N2	110.0 (9)
C13—O11—C12	110.08 (5)	H2F—C22—C21	106.5 (9)
C14—O12—K1	117.71 (4)	H2F—C22—H2E	109.2 (14)
C15—O12—K1	121.10 (4)	C24—C23—N1	113.35 (6)
C15—O12—C14	111.59 (5)	H2G—C23—N1	107.2 (10)
C18—O13—K1	121.09 (4)	H2G—C23—C24	108.6 (10)
C19—O13—K1	113.67 (4)	H2H—C23—N1	111.6 (9)
C19—O13—C18	111.79 (5)	H2H—C23—C24	109.8 (9)
C20—O14—K1	113.68 (4)	H2H—C23—H2G	105.9 (14)
C21—O14—K1	112.09 (4)	C23—C24—O15	108.51 (6)
C21—O14—C20	110.48 (6)	H2I—C24—O15	108.8 (10)
C24—O15—K1	115.72 (4)	H2I—C24—C23	114.0 (10)
C25—O15—K1	117.10 (4)	H2J—C24—O15	111.7 (10)
C25—O15—C24	111.10 (6)	H2J—C24—C23	107.7 (10)
C26—O16—K1	112.74 (4)	H2J—C24—H2I	106.3 (14)
C27—O16—K1	120.15 (4)	C26—C25—O15	109.17 (6)
C27—O16—C26	110.36 (5)	H2K—C25—O15	111.8 (10)
C11—N1—K1	107.40 (4)	H2K—C25—C26	108.1 (10)
C17—N1—K1	107.39 (4)	H2L—C25—O15	111.4 (10)
C17—N1—C11	110.02 (6)	H2L—C25—C26	110.5 (10)
C23—N1—K1	112.29 (4)	H2L—C25—H2K	105.7 (14)
C23—N1—C11	109.17 (6)	C25—C26—O16	109.37 (6)
C23—N1—C17	110.51 (6)	H2M—C26—O16	109.7 (10)
C16—N2—K1	109.94 (4)	H2M—C26—C25	113.3 (10)
C22—N2—K1	107.73 (4)	H2N—C26—O16	110.8 (10)
C22—N2—C16	109.35 (5)	H2N—C26—C25	106.9 (10)
C28—N2—K1	108.82 (4)	H2N—C26—H2M	106.7 (14)
C28—N2—C16	109.73 (5)	C28—C27—O16	110.36 (6)
C28—N2—C22	111.23 (6)	H2O—C27—O16	110.3 (10)
O1—C1—Cr1	177.07 (6)	H2O—C27—C28	111.4 (10)
O2—C2—Cr1	178.88 (7)	H2P—C27—O16	108.6 (10)
O3—C3—Cr1	175.93 (7)	H2P—C27—C28	108.7 (10)
O4—C4—Cr1	177.84 (6)	H2P—C27—H2O	107.3 (14)
O5—C5—Cr1	177.70 (7)	C27—C28—N2	114.07 (6)
O6—C6—Cr2	178.76 (6)	H2Q—C28—N2	110.0 (10)
O7—C7—Cr2	178.65 (6)	H2Q—C28—C27	110.2 (10)
O8—C8—Cr2	174.71 (6)	H2R—C28—N2	109.3 (9)
O9—C9—Cr2	178.58 (7)	H2R—C28—C27	108.9 (10)
O10—C10—Cr2	177.95 (7)	H2R—C28—H2Q	103.8 (14)
C12—C11—N1	114.52 (6)	Cr2—H—Cr1	149.0 (11)
K1—O11—C12—C11	−56.09 (4)	K1—N1—C23—C24	−37.53 (5)
K1—O11—C13—C14	53.27 (4)	K1—N2—C16—C15	−48.43 (4)
K1—O12—C14—C13	42.37 (4)	K1—N2—C22—C21	−39.27 (4)
K1—O12—C15—C16	−41.14 (5)	K1—N2—C28—C27	−48.60 (4)
K1—O13—C18—C17	−40.88 (5)	O11—C12—C11—N1	69.68 (6)
K1—O13—C19—C20	49.43 (5)	O11—C13—C14—O12	−63.32 (6)
K1—O14—C20—C19	48.03 (4)	O12—C15—C16—N2	60.54 (6)
K1—O14—C21—C22	−59.88 (4)	O13—C18—C17—N1	62.41 (7)
K1—O15—C24—C23	−56.15 (4)	O13—C19—C20—O14	−66.06 (7)
K1—O15—C25—C26	37.93 (4)	O14—C21—C22—N2	69.53 (6)
K1—O16—C26—C25	57.47 (4)	O15—C24—C23—N1	63.09 (6)
K1—O16—C27—C28	−39.28 (4)	O15—C25—C26—O16	−63.70 (6)
K1—N1—C11—C12	−41.21 (4)	O16—C27—C28—N2	60.50 (6)
K1—N1—C17—C18	−49.86 (4)

(KCPTCR_IAM_SHADE3)

Crystal data

C28H37Cr2KN2O16	F(000) = 1660.538
Mr = 800.70	Dx = 1.489 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71069 Å
a = 10.458 Å	Cell parameters from 1024 reflections
b = 14.417 Å	θ = 47.5–1.5°
c = 23.882 Å	µ = 0.80 mm^−1
β = 97.26°	T = 28 K
V = 3571.89 Å^3	Ellipsoidal, yellow
Z = 4	0.3 × 0.25 × 0.2 mm

Data collection

SMART CCD diffractometer	22531 reflections with I ≥ 2u(I)
ω scan	Rint = 0.0000
Absorption correction: empirical (using intensity measurements)	θmax = 48.7°, θmin = 2.4°
Tmin = 0.890, Tmax = 0.903	h = −19→20
27917 measured reflections	k = 0→30
27917 independent reflections	l = 0→50

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.036	Only H-atom coordinates refined
wR(F^2) = 0.085	w = 1/[σ^2(Fo^2) + (0.0383P)^2 + 0.7446P] where P = (Fo^2 + 2Fc^2)/3
S = 1.00	(Δ/σ)max = 0.0002
27917 reflections	Δρmax = 0.88 e Å^−3
553 parameters	Δρmin = −0.94 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Cr1	0.163871 (11)	0.002357 (7)	0.236370 (4)	0.005265 (17)
Cr2	0.018768 (11)	0.177451 (7)	0.165108 (4)	0.005821 (18)
K1	0.463722 (14)	0.199287 (9)	0.418003 (6)	0.00650 (2)
O1	0.25211 (6)	0.13816 (4)	0.33124 (2)	0.01182 (9)
O2	−0.08359 (6)	−0.04363 (4)	0.28579 (3)	0.01423 (10)
O3	0.10474 (6)	−0.12663 (4)	0.13543 (3)	0.01256 (9)
O4	0.39537 (6)	0.05453 (4)	0.17748 (3)	0.01365 (10)
O5	0.30040 (6)	−0.15038 (4)	0.30579 (3)	0.01220 (9)
O6	−0.25966 (6)	0.12160 (4)	0.17224 (3)	0.01248 (9)
O7	0.01690 (6)	0.05854 (4)	0.05956 (2)	0.01256 (9)
O8	0.28638 (6)	0.25368 (4)	0.15523 (3)	0.01339 (10)
O9	0.02666 (8)	0.26557 (5)	0.28175 (3)	0.01772 (12)
O10	−0.07208 (7)	0.34768 (4)	0.09919 (3)	0.01453 (10)
O11	0.28601 (5)	0.09223 (3)	0.47319 (2)	0.00782 (7)
O12	0.44336 (6)	0.00288 (3)	0.40242 (2)	0.00835 (8)
O13	0.31320 (6)	0.34079 (3)	0.36297 (2)	0.00877 (8)
O14	0.52829 (6)	0.26684 (4)	0.31543 (2)	0.00895 (8)
O15	0.55085 (5)	0.32677 (4)	0.50748 (2)	0.00925 (8)
O16	0.72701 (5)	0.20502 (4)	0.46501 (2)	0.00821 (8)
N1	0.27326 (6)	0.30193 (4)	0.47979 (3)	0.00792 (8)
N2	0.66164 (6)	0.09467 (4)	0.36197 (2)	0.00698 (8)
C1	0.21615 (7)	0.08851 (4)	0.29500 (3)	0.00812 (9)
C2	0.01017 (7)	−0.02686 (5)	0.26764 (3)	0.00901 (10)
C3	0.12293 (7)	−0.07907 (5)	0.17422 (3)	0.00845 (10)
C4	0.30792 (7)	0.03662 (5)	0.20004 (3)	0.00922 (10)
C5	0.25013 (7)	−0.09110 (4)	0.27860 (3)	0.00841 (10)
C6	−0.15430 (8)	0.14184 (5)	0.16996 (3)	0.00897 (10)
C7	0.01871 (7)	0.10415 (5)	0.09918 (3)	0.00833 (10)
C8	0.18801 (8)	0.22109 (5)	0.16012 (3)	0.00934 (10)
C9	0.02397 (8)	0.23362 (5)	0.23771 (3)	0.01110 (11)
C10	−0.03864 (8)	0.28232 (5)	0.12531 (3)	0.00933 (10)
C11	0.20813 (8)	0.23292 (5)	0.51164 (3)	0.00912 (10)
C12	0.17305 (7)	0.14352 (5)	0.47990 (3)	0.00870 (10)
C13	0.25207 (7)	0.00540 (4)	0.44640 (3)	0.00801 (9)
C14	0.37225 (7)	−0.04781 (4)	0.43913 (3)	0.00831 (10)
C15	0.54828 (7)	−0.04995 (4)	0.38669 (3)	0.00810 (9)
C16	0.60989 (7)	0.00363 (4)	0.34254 (3)	0.00821 (9)
C17	0.17927 (7)	0.34656 (5)	0.43697 (3)	0.00946 (10)
C18	0.24064 (8)	0.40169 (5)	0.39332 (3)	0.00988 (10)
C19	0.37497 (8)	0.38880 (5)	0.32179 (3)	0.01095 (11)
C20	0.42797 (8)	0.31883 (5)	0.28400 (3)	0.01090 (11)
C21	0.57215 (8)	0.19476 (5)	0.28131 (3)	0.00953 (10)
C22	0.69030 (8)	0.14951 (5)	0.31296 (3)	0.00930 (10)
C23	0.33600 (8)	0.37154 (5)	0.51922 (3)	0.01025 (10)
C24	0.46521 (8)	0.34034 (5)	0.54888 (3)	0.01036 (10)
C25	0.68014 (7)	0.31745 (5)	0.53317 (3)	0.00882 (10)
C26	0.76442 (7)	0.29320 (5)	0.48874 (3)	0.00922 (10)
C27	0.82399 (7)	0.16969 (5)	0.43395 (3)	0.00905 (10)
C28	0.77750 (7)	0.08192 (5)	0.40291 (3)	0.00842 (10)
H	0.0507 (16)	0.0770 (12)	0.1996 (7)	0.029921
H1A	0.1264 (15)	0.2603 (11)	0.5231 (7)	0.023023
H1B	0.2640 (15)	0.2182 (11)	0.5468 (7)	0.022016
H1C	0.1261 (15)	0.1559 (11)	0.4427 (6)	0.020436
H1D	0.1135 (15)	0.1063 (11)	0.5022 (7)	0.021942
H1E	0.2008 (15)	0.0142 (11)	0.4102 (7)	0.020147
H1F	0.1991 (15)	−0.0319 (11)	0.4684 (7)	0.021496
H1G	0.3436 (15)	−0.1094 (10)	0.4227 (7)	0.020240
H1H	0.4229 (14)	−0.0556 (11)	0.4770 (6)	0.020490
H1I	0.5173 (15)	−0.1074 (11)	0.3700 (7)	0.021436
H1J	0.6090 (15)	−0.0656 (11)	0.4202 (6)	0.021077
H1K	0.5434 (15)	0.0133 (11)	0.3109 (7)	0.020388
H1L	0.6779 (15)	−0.0348 (11)	0.3289 (7)	0.022019
H1M	0.1296 (15)	0.2982 (11)	0.4164 (7)	0.021287
H1N	0.1209 (15)	0.3855 (11)	0.4541 (7)	0.023003
H1O	0.1719 (15)	0.4294 (11)	0.3688 (7)	0.022432
H1P	0.2995 (15)	0.4515 (11)	0.4122 (7)	0.022225
H1Q	0.4421 (15)	0.4265 (11)	0.3401 (6)	0.021477
H1R	0.3116 (15)	0.4278 (11)	0.2978 (7)	0.021586
H2A	0.3600 (15)	0.2802 (11)	0.2689 (7)	0.019926
H2B	0.4614 (15)	0.3521 (11)	0.2542 (6)	0.021449
H2C	0.5925 (15)	0.2198 (11)	0.2450 (6)	0.021626
H2D	0.5062 (15)	0.1520 (11)	0.2721 (7)	0.020024
H2E	0.7302 (15)	0.1084 (11)	0.2856 (6)	0.022042
H2F	0.7511 (15)	0.2006 (11)	0.3255 (7)	0.021862
H2G	0.3487 (15)	0.4260 (11)	0.4978 (7)	0.022708
H2H	0.2767 (15)	0.3916 (11)	0.5486 (7)	0.023541
H2I	0.4613 (15)	0.2823 (11)	0.5708 (7)	0.021522
H2J	0.4956 (15)	0.3869 (11)	0.5752 (7)	0.022844
H2K	0.7123 (15)	0.3743 (11)	0.5514 (7)	0.022041
H2L	0.6874 (15)	0.2706 (11)	0.5626 (7)	0.021423
H2M	0.7622 (16)	0.3391 (11)	0.4592 (6)	0.021454
H2N	0.8537 (15)	0.2915 (11)	0.5075 (7)	0.021617
H2O	0.8489 (15)	0.2167 (11)	0.4081 (7)	0.021560
H2P	0.9035 (15)	0.1544 (11)	0.4616 (7)	0.022180
H2Q	0.8467 (14)	0.0551 (11)	0.3844 (7)	0.022814
H2R	0.7612 (15)	0.0363 (11)	0.4297 (6)	0.021435

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cr1	0.00571 (4)	0.00467 (3)	0.00539 (4)	0.00013 (3)	0.00063 (3)	−0.00017 (2)
Cr2	0.00674 (4)	0.00538 (3)	0.00521 (4)	0.00077 (3)	0.00024 (3)	0.00014 (3)
K1	0.00619 (5)	0.00667 (4)	0.00659 (5)	0.00019 (4)	0.00056 (4)	−0.00005 (3)
O1	0.0151 (3)	0.00928 (17)	0.0101 (2)	0.00006 (17)	−0.00208 (17)	−0.00223 (15)
O2	0.0111 (3)	0.0163 (2)	0.0162 (3)	0.00029 (19)	0.00561 (19)	0.00137 (18)
O3	0.0146 (3)	0.01241 (19)	0.0107 (2)	−0.00208 (18)	0.00173 (18)	−0.00444 (16)
O4	0.0115 (3)	0.0136 (2)	0.0170 (3)	−0.00064 (19)	0.00616 (19)	−0.00015 (18)
O5	0.0133 (3)	0.00929 (17)	0.0135 (2)	0.00316 (17)	−0.00057 (18)	0.00215 (16)
O6	0.0108 (2)	0.0147 (2)	0.0124 (2)	−0.00064 (18)	0.00334 (18)	0.00010 (17)
O7	0.0163 (3)	0.01234 (19)	0.0093 (2)	−0.00155 (19)	0.00269 (18)	−0.00278 (16)
O8	0.0120 (3)	0.0158 (2)	0.0121 (2)	−0.00448 (19)	0.00027 (18)	0.00058 (17)
O9	0.0256 (3)	0.0171 (2)	0.0096 (2)	0.0097 (2)	−0.0012 (2)	−0.00445 (18)
O10	0.0176 (3)	0.00996 (18)	0.0151 (3)	0.00286 (19)	−0.0018 (2)	0.00386 (17)
O11	0.0059 (2)	0.00717 (15)	0.0103 (2)	0.00007 (14)	0.00092 (14)	−0.00173 (13)
O12	0.0085 (2)	0.00671 (15)	0.0106 (2)	0.00104 (15)	0.00396 (15)	0.00145 (14)
O13	0.0099 (2)	0.00710 (15)	0.0099 (2)	0.00117 (15)	0.00348 (16)	0.00124 (14)
O14	0.0102 (2)	0.00874 (16)	0.00779 (19)	0.00286 (15)	0.00062 (15)	0.00027 (14)
O15	0.0065 (2)	0.01358 (19)	0.00748 (19)	0.00154 (16)	0.00030 (14)	−0.00174 (15)
O16	0.0060 (2)	0.00851 (16)	0.0103 (2)	−0.00111 (15)	0.00187 (15)	−0.00323 (14)
N1	0.0072 (2)	0.00794 (17)	0.0084 (2)	0.00065 (16)	0.00032 (16)	−0.00019 (15)
N2	0.0075 (2)	0.00689 (16)	0.0065 (2)	−0.00050 (16)	0.00076 (15)	0.00021 (14)
C1	0.0087 (3)	0.00708 (19)	0.0084 (2)	0.00045 (18)	0.00041 (18)	0.00022 (16)
C2	0.0100 (3)	0.0084 (2)	0.0087 (2)	0.00108 (19)	0.00160 (19)	0.00050 (17)
C3	0.0081 (3)	0.0082 (2)	0.0092 (2)	−0.00011 (19)	0.00138 (18)	−0.00040 (17)
C4	0.0094 (3)	0.0085 (2)	0.0098 (3)	0.00000 (19)	0.00115 (19)	−0.00072 (17)
C5	0.0081 (3)	0.00741 (19)	0.0096 (2)	0.00039 (18)	0.00089 (19)	−0.00040 (17)
C6	0.0113 (3)	0.0090 (2)	0.0066 (2)	0.0016 (2)	0.00101 (19)	0.00032 (17)
C7	0.0085 (3)	0.0084 (2)	0.0083 (2)	−0.00047 (19)	0.00147 (18)	0.00011 (17)
C8	0.0115 (3)	0.0089 (2)	0.0073 (2)	−0.0001 (2)	−0.00045 (19)	−0.00004 (17)
C9	0.0132 (3)	0.0100 (2)	0.0098 (3)	0.0038 (2)	0.0000 (2)	−0.00090 (18)
C10	0.0105 (3)	0.00804 (19)	0.0091 (3)	0.00094 (19)	−0.00003 (19)	0.00040 (17)
C11	0.0095 (3)	0.0099 (2)	0.0083 (2)	0.0014 (2)	0.00231 (19)	−0.00009 (17)
C12	0.0063 (3)	0.0094 (2)	0.0106 (3)	0.00040 (19)	0.00152 (19)	0.00010 (18)
C13	0.0077 (3)	0.00768 (19)	0.0087 (2)	−0.00184 (18)	0.00146 (18)	−0.00061 (17)
C14	0.0094 (3)	0.00707 (19)	0.0088 (2)	−0.00045 (19)	0.00247 (19)	0.00096 (17)
C15	0.0075 (3)	0.00669 (18)	0.0102 (2)	0.00113 (18)	0.00162 (19)	0.00036 (17)
C16	0.0093 (3)	0.00772 (19)	0.0077 (2)	−0.00024 (19)	0.00132 (18)	−0.00100 (16)
C17	0.0076 (3)	0.0102 (2)	0.0106 (3)	0.0021 (2)	0.00159 (19)	0.00143 (18)
C18	0.0104 (3)	0.0079 (2)	0.0118 (3)	0.0023 (2)	0.0031 (2)	0.00121 (18)
C19	0.0125 (3)	0.0083 (2)	0.0127 (3)	0.0019 (2)	0.0042 (2)	0.00327 (18)
C20	0.0121 (3)	0.0120 (2)	0.0087 (3)	0.0032 (2)	0.0017 (2)	0.00344 (19)
C21	0.0125 (3)	0.0089 (2)	0.0072 (2)	0.0018 (2)	0.00123 (19)	0.00025 (17)
C22	0.0096 (3)	0.0098 (2)	0.0090 (2)	0.0010 (2)	0.00334 (19)	0.00186 (18)
C23	0.0088 (3)	0.0099 (2)	0.0119 (3)	0.0013 (2)	0.0009 (2)	−0.00352 (19)
C24	0.0081 (3)	0.0142 (2)	0.0089 (3)	0.0004 (2)	0.00126 (19)	−0.00307 (19)
C25	0.0078 (3)	0.0099 (2)	0.0084 (2)	−0.00042 (19)	−0.00026 (18)	−0.00192 (17)
C26	0.0081 (3)	0.0087 (2)	0.0109 (3)	−0.00155 (19)	0.00126 (19)	−0.00218 (18)
C27	0.0068 (3)	0.0103 (2)	0.0102 (3)	−0.00048 (19)	0.00176 (19)	−0.00201 (18)
C28	0.0073 (3)	0.0086 (2)	0.0093 (2)	0.00094 (19)	0.00064 (18)	−0.00070 (17)
H	0.026290	0.023490	0.038610	0.003460	−0.001240	0.011980
H1A	0.017820	0.027050	0.025490	0.003500	0.007760	−0.004370
H1B	0.021170	0.027300	0.016190	−0.000740	−0.003040	0.001360
H1C	0.019760	0.025720	0.014770	0.003890	−0.001940	−0.000730
H1D	0.019570	0.025160	0.022480	−0.003380	0.008050	0.001390
H1E	0.021570	0.021640	0.015700	0.002370	−0.003600	0.000750
H1F	0.021710	0.021790	0.022180	−0.004980	0.007410	0.003180
H1G	0.024250	0.014390	0.021880	−0.002530	0.002140	−0.001160
H1H	0.018890	0.025310	0.016030	−0.000330	−0.002620	0.004510
H1I	0.023620	0.014700	0.026080	−0.001330	0.003500	−0.003730
H1J	0.018640	0.024620	0.018910	0.005010	−0.001760	0.002570
H1K	0.019210	0.021460	0.018930	−0.000080	−0.003680	0.001470
H1L	0.019100	0.020910	0.027180	0.004670	0.007330	−0.003990
H1M	0.021810	0.019650	0.021050	−0.002900	−0.002550	−0.002970
H1N	0.022530	0.024800	0.022240	0.008720	0.005010	−0.004240
H1O	0.022460	0.022100	0.021570	0.007420	−0.001760	0.001380
H1P	0.023610	0.017640	0.024950	−0.002890	0.001220	−0.006520
H1Q	0.023340	0.019560	0.020860	−0.007390	0.000180	−0.002760
H1R	0.023180	0.018730	0.021920	0.004550	−0.000760	0.004000
H2A	0.018400	0.015870	0.024430	−0.003500	−0.001490	−0.002080
H2B	0.025450	0.021570	0.018040	−0.001490	0.005520	0.005190
H2C	0.024880	0.024790	0.016260	0.000380	0.006690	0.003650
H2D	0.016430	0.018400	0.025110	−0.003810	0.002110	−0.004270
H2E	0.022510	0.024870	0.019950	0.004210	0.007370	−0.003420
H2F	0.019850	0.022430	0.022610	−0.007340	−0.000030	−0.000770
H2G	0.026040	0.018650	0.022510	−0.001220	−0.000530	0.001350
H2H	0.020050	0.030410	0.020750	0.003500	0.004860	−0.008200
H2I	0.022340	0.021250	0.021620	0.001760	0.005280	0.003480
H2J	0.021520	0.025430	0.020820	−0.001020	−0.000290	−0.009450
H2K	0.021500	0.020400	0.023550	−0.002650	0.000230	−0.007210
H2L	0.020360	0.023980	0.019810	0.000570	0.002080	0.005640
H2M	0.027810	0.018690	0.017750	−0.002200	0.002440	0.002340
H2N	0.013980	0.026010	0.023980	−0.000700	−0.001030	−0.003050
H2O	0.023470	0.021050	0.021220	−0.002050	0.006950	0.002120
H2P	0.014520	0.029010	0.021960	0.002500	−0.001780	−0.002580
H2Q	0.016150	0.028860	0.024060	0.004080	0.004990	−0.006060
H2R	0.021840	0.021330	0.020670	−0.001820	0.000880	0.004530

Geometric parameters (Å, º)

Cr1—C1	1.8997 (7)	N2—C22	1.4742 (9)
Cr1—C2	1.9032 (8)	N2—C28	1.4691 (9)
Cr1—C3	1.8984 (7)	C11—C12	1.5166 (10)
Cr1—C4	1.8965 (8)	C11—H1A	1.010 (15)
Cr1—C5	1.8483 (7)	C11—H1B	0.984 (15)
Cr1—H	1.752 (16)	C12—H1C	0.976 (15)
Cr2—C6	1.8990 (8)	C12—H1D	1.021 (15)
Cr2—C7	1.8962 (7)	C13—C14	1.5013 (10)
Cr2—C8	1.8963 (8)	C13—H1E	0.967 (15)
Cr2—C9	1.9081 (7)	C13—H1F	0.973 (15)
Cr2—C10	1.8453 (7)	C14—H1G	1.001 (15)
Cr2—H	1.678 (16)	C14—H1H	0.996 (14)
K1—O1	2.9679 (6)	C15—C16	1.5152 (10)
K1—O11	2.8622 (5)	C15—H1I	0.958 (15)
K1—O12	2.8603 (5)	C15—H1J	0.982 (15)
K1—O13	2.8008 (5)	C16—H1K	0.969 (15)
K1—O14	2.7970 (6)	C16—H1L	0.988 (15)
K1—O15	2.8779 (6)	C17—C18	1.5164 (10)
K1—O16	2.8403 (6)	C17—H1M	0.966 (15)
K1—N1	3.0129 (6)	C17—H1N	0.958 (15)
K1—N2	3.0083 (6)	C18—H1O	0.956 (15)
O1—C1	1.1492 (9)	C18—H1P	1.014 (15)
O2—C2	1.1469 (10)	C19—C20	1.5051 (11)
O3—C3	1.1488 (9)	C19—H1Q	0.951 (15)
O4—C4	1.1480 (10)	C19—H1R	0.993 (15)
O5—C5	1.1586 (9)	C20—H2A	0.938 (15)
O6—C6	1.1477 (10)	C20—H2B	0.960 (15)
O7—C7	1.1505 (9)	C21—C22	1.5125 (11)
O8—C8	1.1502 (10)	C21—H2C	0.986 (15)
O9—C9	1.1453 (9)	C21—H2D	0.931 (15)
O10—C10	1.1595 (9)	C22—H2E	1.012 (15)
O11—C12	1.4198 (9)	C22—H2F	0.994 (15)
O11—C13	1.4300 (8)	C23—C24	1.5127 (11)
O12—C14	1.4215 (8)	C23—H2G	0.955 (16)
O12—C15	1.4246 (9)	C23—H2H	1.035 (15)
O13—C18	1.4181 (9)	C24—H2I	0.991 (16)
O13—C19	1.4228 (9)	C24—H2J	0.947 (15)
O14—C20	1.4237 (9)	C25—C26	1.5038 (10)
O14—C21	1.4313 (9)	C25—H2K	0.968 (15)
O15—C24	1.4289 (9)	C25—H2L	0.971 (15)
O15—C25	1.4188 (9)	C26—H2M	0.964 (15)
O16—C26	1.4263 (8)	C26—H2N	0.983 (15)
O16—C27	1.4243 (9)	C27—C28	1.5153 (10)
N1—C11	1.4708 (9)	C27—H2O	0.974 (15)
N1—C17	1.4737 (9)	C27—H2P	1.018 (15)
N1—C23	1.4724 (9)	C28—H2Q	0.975 (15)
N2—C16	1.4722 (9)	C28—H2R	0.948 (15)
C2—Cr1—C1	91.96 (3)	H1A—C11—N1	109.8 (9)
C3—Cr1—C1	174.93 (3)	H1A—C11—C12	107.9 (9)
C3—Cr1—C2	92.96 (3)	H1B—C11—N1	108.9 (9)
C4—Cr1—C1	89.75 (3)	H1B—C11—C12	108.9 (10)
C4—Cr1—C2	175.04 (3)	H1B—C11—H1A	106.6 (13)
C4—Cr1—C3	85.25 (3)	C11—C12—O11	110.30 (6)
C5—Cr1—C1	89.96 (3)	H1C—C12—O11	108.8 (9)
C5—Cr1—C2	90.16 (3)	H1C—C12—C11	111.2 (9)
C5—Cr1—C3	91.27 (3)	H1D—C12—O11	110.9 (9)
C5—Cr1—C4	94.50 (3)	H1D—C12—C11	108.1 (9)
H—Cr1—C1	94.7 (6)	H1D—C12—H1C	107.6 (13)
H—Cr1—C2	77.4 (6)	C14—C13—O11	109.57 (6)
H—Cr1—C3	85.2 (6)	H1E—C13—O11	111.4 (9)
H—Cr1—C4	97.8 (6)	H1E—C13—C14	109.9 (9)
H—Cr1—C5	166.9 (5)	H1F—C13—O11	111.6 (9)
C7—Cr2—C6	89.98 (3)	H1F—C13—C14	108.8 (9)
C8—Cr2—C6	176.31 (3)	H1F—C13—H1E	105.5 (13)
C8—Cr2—C7	92.01 (3)	C13—C14—O12	108.63 (5)
C9—Cr2—C6	88.70 (3)	H1G—C14—O12	111.6 (9)
C9—Cr2—C7	171.10 (3)	H1G—C14—C13	106.6 (9)
C9—Cr2—C8	89.81 (3)	H1H—C14—O12	111.1 (9)
C10—Cr2—C6	90.13 (3)	H1H—C14—C13	108.0 (9)
C10—Cr2—C7	93.61 (3)	H1H—C14—H1G	110.8 (13)
C10—Cr2—C8	86.64 (3)	C16—C15—O12	108.68 (5)
C10—Cr2—C9	95.19 (3)	H1I—C15—O12	109.9 (9)
H—Cr2—C6	82.5 (6)	H1I—C15—C16	107.6 (9)
H—Cr2—C7	84.6 (6)	H1J—C15—O12	110.4 (9)
H—Cr2—C8	100.8 (6)	H1J—C15—C16	113.3 (9)
H—Cr2—C9	86.5 (6)	H1J—C15—H1I	106.9 (13)
H—Cr2—C10	172.4 (6)	C15—C16—N2	114.01 (5)
O11—K1—O1	72.006 (16)	H1K—C16—N2	108.4 (9)
O12—K1—O1	65.074 (16)	H1K—C16—C15	106.8 (9)
O12—K1—O11	58.942 (15)	H1L—C16—N2	110.6 (9)
O13—K1—O1	64.111 (16)	H1L—C16—C15	109.3 (9)
O13—K1—O11	104.462 (16)	H1L—C16—H1K	107.5 (13)
O13—K1—O12	129.185 (17)	C18—C17—N1	113.75 (6)
O14—K1—O1	74.524 (17)	H1M—C17—N1	107.8 (9)
O14—K1—O11	146.481 (17)	H1M—C17—C18	106.1 (10)
O14—K1—O12	104.653 (16)	H1N—C17—N1	111.4 (10)
O14—K1—O13	61.246 (16)	H1N—C17—C18	109.5 (10)
O15—K1—O1	147.798 (17)	H1N—C17—H1M	108.0 (13)
O15—K1—O11	99.530 (16)	C17—C18—O13	109.10 (5)
O15—K1—O12	137.749 (17)	H1O—C18—O13	110.8 (9)
O15—K1—O13	89.408 (16)	H1O—C18—C17	106.8 (10)
O15—K1—O14	109.823 (17)	H1P—C18—O13	109.4 (9)
O16—K1—O1	152.212 (17)	H1P—C18—C17	110.6 (9)
O16—K1—O11	119.151 (16)	H1P—C18—H1O	110.2 (13)
O16—K1—O12	97.629 (16)	C20—C19—O13	108.80 (6)
O16—K1—O13	128.577 (16)	H1Q—C19—O13	109.5 (9)
O16—K1—O14	90.390 (17)	H1Q—C19—C20	110.7 (10)
O16—K1—O15	59.188 (15)	H1R—C19—O13	110.2 (9)
N1—K1—O1	90.399 (17)	H1R—C19—C20	107.7 (9)
N1—K1—O11	62.058 (15)	H1R—C19—H1Q	110.0 (13)
N1—K1—O12	120.464 (16)	C19—C20—O14	109.84 (6)
N1—K1—O13	60.324 (16)	H2A—C20—O14	111.2 (9)
N1—K1—O14	120.372 (16)	H2A—C20—C19	108.0 (10)
N1—K1—O15	59.306 (16)	H2B—C20—O14	109.9 (9)
N1—K1—O16	117.386 (16)	H2B—C20—C19	107.8 (9)
N2—K1—O1	91.995 (17)	H2B—C20—H2A	109.9 (13)
N2—K1—O11	117.243 (15)	C22—C21—O14	109.20 (6)
N2—K1—O12	59.329 (15)	H2C—C21—O14	110.8 (9)
N2—K1—O13	122.271 (16)	H2C—C21—C22	110.1 (9)
N2—K1—O14	61.910 (15)	H2D—C21—O14	109.5 (10)
N2—K1—O15	118.648 (17)	H2D—C21—C22	111.5 (10)
N2—K1—O16	60.220 (16)	H2D—C21—H2C	105.7 (13)
N2—K1—N1	177.113 (17)	C21—C22—N2	113.14 (6)
C1—O1—K1	148.75 (5)	H2E—C22—N2	109.9 (9)
C12—O11—K1	111.66 (4)	H2E—C22—C21	107.9 (9)
C13—O11—K1	113.89 (4)	H2F—C22—N2	110.1 (9)
C13—O11—C12	110.08 (5)	H2F—C22—C21	106.4 (9)
C14—O12—K1	117.71 (4)	H2F—C22—H2E	109.2 (13)
C15—O12—K1	121.10 (4)	C24—C23—N1	113.35 (6)
C15—O12—C14	111.60 (5)	H2G—C23—N1	107.4 (9)
C18—O13—K1	121.09 (4)	H2G—C23—C24	108.6 (9)
C19—O13—K1	113.66 (4)	H2H—C23—N1	111.6 (9)
C19—O13—C18	111.79 (5)	H2H—C23—C24	110.0 (9)
C20—O14—K1	113.68 (4)	H2H—C23—H2G	105.6 (13)
C21—O14—K1	112.09 (4)	C23—C24—O15	108.52 (6)
C21—O14—C20	110.48 (6)	H2I—C24—O15	108.8 (9)
C24—O15—K1	115.71 (4)	H2I—C24—C23	113.8 (9)
C25—O15—K1	117.10 (4)	H2J—C24—O15	111.7 (10)
C25—O15—C24	111.11 (6)	H2J—C24—C23	107.8 (10)
C26—O16—K1	112.74 (4)	H2J—C24—H2I	106.3 (13)
C27—O16—K1	120.15 (4)	C26—C25—O15	109.17 (6)
C27—O16—C26	110.36 (5)	H2K—C25—O15	111.9 (9)
C11—N1—K1	107.40 (4)	H2K—C25—C26	108.2 (9)
C17—N1—K1	107.39 (4)	H2L—C25—O15	111.2 (9)
C17—N1—C11	110.02 (6)	H2L—C25—C26	110.4 (9)
C23—N1—K1	112.28 (4)	H2L—C25—H2K	105.8 (13)
C23—N1—C11	109.17 (6)	C25—C26—O16	109.37 (6)
C23—N1—C17	110.52 (5)	H2M—C26—O16	109.9 (9)
C16—N2—K1	109.94 (4)	H2M—C26—C25	113.2 (10)
C22—N2—K1	107.73 (4)	H2N—C26—O16	110.9 (9)
C22—N2—C16	109.35 (5)	H2N—C26—C25	106.9 (9)
C28—N2—K1	108.82 (4)	H2N—C26—H2M	106.5 (13)
C28—N2—C16	109.74 (5)	C28—C27—O16	110.36 (6)
C28—N2—C22	111.23 (6)	H2O—C27—O16	110.3 (9)
O1—C1—Cr1	177.07 (6)	H2O—C27—C28	111.4 (9)
O2—C2—Cr1	178.88 (7)	H2P—C27—O16	108.4 (9)
O3—C3—Cr1	175.93 (7)	H2P—C27—C28	108.8 (9)
O4—C4—Cr1	177.84 (6)	H2P—C27—H2O	107.4 (13)
O5—C5—Cr1	177.71 (7)	C27—C28—N2	114.06 (6)
O6—C6—Cr2	178.76 (6)	H2Q—C28—N2	110.1 (9)
O7—C7—Cr2	178.65 (6)	H2Q—C28—C27	110.1 (9)
O8—C8—Cr2	174.71 (6)	H2R—C28—N2	109.4 (9)
O9—C9—Cr2	178.59 (7)	H2R—C28—C27	108.8 (10)
O10—C10—Cr2	177.96 (7)	H2R—C28—H2Q	103.8 (13)
C12—C11—N1	114.52 (6)	Cr2—H—Cr1	148.9 (11)
K1—O11—C12—C11	−56.09 (4)	K1—N1—C23—C24	−37.53 (5)
K1—O11—C13—C14	53.27 (4)	K1—N2—C16—C15	−48.44 (4)
K1—O12—C14—C13	42.37 (4)	K1—N2—C22—C21	−39.27 (4)
K1—O12—C15—C16	−41.14 (5)	K1—N2—C28—C27	−48.60 (4)
K1—O13—C18—C17	−40.89 (5)	O11—C12—C11—N1	69.69 (6)
K1—O13—C19—C20	49.44 (5)	O11—C13—C14—O12	−63.32 (6)
K1—O14—C20—C19	48.03 (4)	O12—C15—C16—N2	60.55 (6)
K1—O14—C21—C22	−59.87 (4)	O13—C18—C17—N1	62.42 (7)
K1—O15—C24—C23	−56.15 (4)	O13—C19—C20—O14	−66.07 (7)
K1—O15—C25—C26	37.93 (4)	O14—C21—C22—N2	69.53 (6)
K1—O16—C26—C25	57.47 (4)	O15—C24—C23—N1	63.09 (6)
K1—O16—C27—C28	−39.29 (4)	O15—C25—C26—O16	−63.69 (6)
K1—N1—C11—C12	−41.21 (4)	O16—C27—C28—N2	60.50 (6)
K1—N1—C17—C18	−49.86 (4)

(KCPTCR_standard_HAR_0_HADPs)

Crystal data

C28H37Cr2KN2O16	F(000) = 1660.306
Mr = 800.70	Dx = 1.489 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71069 Å
a = 10.458 Å	Cell parameters from 1024 reflections
b = 14.417 Å	θ = 47.5–1.5°
c = 23.882 Å	µ = 0.80 mm^−1
β = 97.26°	T = 28 K
V = 3571.89 Å^3	Ellipsoidal, yellow
Z = 4	0.3 × 0.25 × 0.2 mm

Data collection

SMART CCD diffractometer	5667 reflections with I ≥ 2u(I)
ω scan	Rint = 0.0000
Absorption correction: empirical (using intensity measurements)	θmax = 25.0°, θmin = 2.4°
Tmin = 0.890, Tmax = 0.903	h = −19→20
27917 measured reflections	k = 0→30
5993 independent reflections	l = 0→50

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.018	Only H-atom coordinates refined
wR(F^2) = 0.042	w = 1/[σ^2(Fo^2) + (0.0174P)^2 + 1.1731P] where P = (Fo^2 + 2Fc^2)/3
S = 1.04	(Δ/σ)max = 0.001
5993 reflections	Δρmax = 0.22 e Å^−3
553 parameters	Δρmin = −0.29 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Cr1	0.163857 (17)	0.002356 (12)	0.236360 (7)	0.00542 (5)
Cr2	0.018769 (17)	0.177467 (12)	0.165104 (7)	0.00593 (5)
K1	0.46374 (2)	0.199296 (16)	0.418009 (10)	0.00672 (6)
O1	0.25201 (8)	0.13802 (5)	0.33120 (3)	0.01227 (18)
O2	−0.08338 (8)	−0.04361 (6)	0.28572 (3)	0.01438 (18)
O3	0.10472 (8)	−0.12656 (6)	0.13551 (3)	0.01296 (18)
O4	0.39542 (8)	0.05450 (6)	0.17754 (4)	0.01393 (18)
O5	0.30035 (8)	−0.15025 (5)	0.30579 (3)	0.01276 (18)
O6	−0.25958 (8)	0.12166 (6)	0.17227 (3)	0.01265 (18)
O7	0.01683 (8)	0.05854 (6)	0.05961 (3)	0.01265 (18)
O8	0.28630 (8)	0.25364 (6)	0.15527 (3)	0.01332 (18)
O9	0.02671 (9)	0.26557 (6)	0.28168 (4)	0.01762 (19)
O10	−0.07200 (8)	0.34763 (6)	0.09920 (3)	0.01479 (18)
O11	0.28564 (7)	0.09218 (5)	0.47310 (3)	0.00806 (16)
O12	0.44351 (8)	0.00261 (5)	0.40247 (3)	0.00846 (16)
O13	0.31322 (8)	0.34103 (5)	0.36298 (3)	0.00920 (17)
O14	0.52822 (8)	0.26683 (5)	0.31527 (3)	0.00935 (16)
O15	0.55096 (7)	0.32681 (5)	0.50766 (3)	0.00983 (17)
O16	0.72726 (7)	0.20520 (5)	0.46500 (3)	0.00864 (16)
N1	0.27297 (9)	0.30201 (6)	0.47985 (4)	0.00814 (19)
N2	0.66195 (9)	0.09452 (6)	0.36194 (4)	0.00755 (19)
C1	0.21631 (11)	0.08864 (8)	0.29510 (5)	0.0081 (2)
C2	0.00991 (11)	−0.02698 (8)	0.26777 (5)	0.0090 (2)
C3	0.12293 (11)	−0.07936 (8)	0.17418 (5)	0.0086 (2)
C4	0.30822 (11)	0.03672 (8)	0.19996 (5)	0.0092 (2)
C5	0.25035 (11)	−0.09129 (8)	0.27869 (5)	0.0082 (2)
C6	−0.15487 (11)	0.14172 (8)	0.16986 (5)	0.0087 (2)
C7	0.01887 (11)	0.10391 (8)	0.09903 (5)	0.0084 (2)
C8	0.18840 (11)	0.22125 (8)	0.16007 (5)	0.0092 (2)
C9	0.02380 (11)	0.23382 (8)	0.23788 (5)	0.0110 (2)
C10	−0.03869 (11)	0.28250 (8)	0.12528 (5)	0.0097 (2)
C11	0.20815 (11)	0.23289 (8)	0.51159 (5)	0.0092 (2)
C12	0.17296 (11)	0.14345 (8)	0.47991 (5)	0.0089 (2)
C13	0.25202 (11)	0.00550 (8)	0.44645 (5)	0.0084 (2)
C14	0.37231 (11)	−0.04770 (8)	0.43915 (5)	0.0083 (2)
C15	0.54823 (11)	−0.04997 (8)	0.38673 (5)	0.0081 (2)
C16	0.60997 (11)	0.00365 (8)	0.34261 (5)	0.0085 (2)
C17	0.17922 (11)	0.34656 (8)	0.43699 (5)	0.0097 (2)
C18	0.24063 (11)	0.40157 (8)	0.39328 (5)	0.0099 (2)
C19	0.37487 (12)	0.38870 (8)	0.32183 (5)	0.0112 (2)
C20	0.42825 (12)	0.31889 (8)	0.28397 (5)	0.0110 (2)
C21	0.57225 (11)	0.19494 (8)	0.28135 (5)	0.0097 (2)
C22	0.69046 (11)	0.14955 (8)	0.31304 (5)	0.0092 (2)
C23	0.33601 (11)	0.37156 (8)	0.51918 (5)	0.0106 (2)
C24	0.46526 (11)	0.34034 (8)	0.54884 (5)	0.0106 (2)
C25	0.68005 (11)	0.31754 (8)	0.53315 (5)	0.0088 (2)
C26	0.76448 (11)	0.29313 (8)	0.48869 (5)	0.0094 (2)
C27	0.82387 (11)	0.16974 (8)	0.43398 (5)	0.0093 (2)
C28	0.77740 (11)	0.08197 (8)	0.40283 (5)	0.0084 (2)
H	0.0487 (11)	0.0732 (8)	0.1996 (5)	0.000000
H1A	0.1204 (12)	0.2629 (8)	0.5254 (5)	0.000000
H1B	0.2725 (11)	0.2161 (8)	0.5497 (5)	0.000000
H1C	0.1171 (11)	0.1574 (8)	0.4376 (5)	0.000000
H1D	0.1092 (11)	0.1027 (8)	0.5038 (5)	0.000000
H1E	0.1934 (12)	0.0166 (8)	0.4052 (5)	0.000000
H1F	0.1940 (11)	−0.0358 (8)	0.4716 (5)	0.000000
H1G	0.3441 (11)	−0.1150 (8)	0.4212 (5)	0.000000
H1H	0.4282 (11)	−0.0594 (8)	0.4804 (5)	0.000000
H1I	0.5124 (11)	−0.1154 (8)	0.3680 (5)	0.000000
H1J	0.6155 (11)	−0.0678 (8)	0.4241 (5)	0.000000
H1K	0.5392 (11)	0.0158 (8)	0.3069 (5)	0.000000
H1L	0.6859 (11)	−0.0399 (8)	0.3282 (5)	0.000000
H1M	0.1231 (11)	0.2923 (8)	0.4142 (5)	0.000000
H1N	0.1142 (11)	0.3924 (8)	0.4568 (5)	0.000000
H1O	0.1634 (11)	0.4346 (8)	0.3628 (5)	0.000000
H1P	0.3020 (11)	0.4563 (8)	0.4124 (5)	0.000000
H1Q	0.4506 (11)	0.4328 (8)	0.3422 (5)	0.000000
H1R	0.3071 (11)	0.4327 (8)	0.2961 (5)	0.000000
H2A	0.3505 (11)	0.2739 (8)	0.2661 (5)	0.000000
H2B	0.4653 (11)	0.3538 (8)	0.2492 (5)	0.000000
H2C	0.5974 (11)	0.2239 (8)	0.2418 (5)	0.000000
H2D	0.4956 (11)	0.1456 (8)	0.2695 (5)	0.000000
H2E	0.7376 (11)	0.1057 (8)	0.2830 (5)	0.000000
H2F	0.7581 (11)	0.2052 (8)	0.3267 (5)	0.000000
H2G	0.3528 (11)	0.4332 (8)	0.4960 (5)	0.000000
H2H	0.2742 (11)	0.3936 (8)	0.5507 (5)	0.000000
H2I	0.4572 (11)	0.2752 (8)	0.5741 (5)	0.000000
H2J	0.5049 (11)	0.3919 (8)	0.5794 (5)	0.000000
H2K	0.7159 (11)	0.3828 (8)	0.5540 (5)	0.000000
H2L	0.6877 (11)	0.2624 (8)	0.5660 (5)	0.000000
H2M	0.7591 (11)	0.3465 (8)	0.4558 (5)	0.000000
H2N	0.8631 (12)	0.2920 (8)	0.5093 (5)	0.000000
H2O	0.8501 (11)	0.2220 (8)	0.4048 (5)	0.000000
H2P	0.9102 (12)	0.1527 (8)	0.4645 (5)	0.000000
H2Q	0.8592 (11)	0.0543 (8)	0.3830 (5)	0.000000
H2R	0.7555 (11)	0.0317 (8)	0.4326 (5)	0.000000

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cr1	0.00572 (10)	0.00477 (9)	0.00569 (9)	0.00012 (6)	0.00046 (7)	−0.00013 (7)
Cr2	0.00685 (10)	0.00540 (9)	0.00534 (9)	0.00085 (7)	−0.00003 (7)	0.00016 (7)
K1	0.00618 (12)	0.00678 (11)	0.00709 (12)	0.00026 (9)	0.00040 (9)	−0.00006 (9)
O1	0.0156 (4)	0.0096 (4)	0.0106 (4)	−0.0004 (3)	−0.0027 (3)	−0.0020 (3)
O2	0.0108 (5)	0.0166 (4)	0.0170 (4)	−0.0002 (3)	0.0069 (4)	0.0013 (3)
O3	0.0153 (4)	0.0129 (4)	0.0107 (4)	−0.0026 (3)	0.0020 (3)	−0.0046 (4)
O4	0.0110 (5)	0.0141 (4)	0.0178 (4)	−0.0012 (3)	0.0066 (4)	−0.0005 (3)
O5	0.0134 (4)	0.0096 (4)	0.0145 (4)	0.0033 (3)	−0.0012 (3)	0.0021 (3)
O6	0.0100 (5)	0.0152 (4)	0.0133 (4)	−0.0014 (3)	0.0033 (3)	0.0005 (3)
O7	0.0170 (5)	0.0124 (4)	0.0088 (4)	−0.0019 (3)	0.0028 (3)	−0.0035 (3)
O8	0.0116 (5)	0.0154 (4)	0.0129 (4)	−0.0051 (4)	0.0011 (3)	0.0011 (3)
O9	0.0257 (5)	0.0172 (4)	0.0090 (5)	0.0094 (4)	−0.0014 (4)	−0.0049 (4)
O10	0.0183 (5)	0.0093 (4)	0.0157 (4)	0.0030 (3)	−0.0024 (4)	0.0044 (4)
O11	0.0064 (4)	0.0079 (4)	0.0097 (4)	−0.0002 (3)	0.0003 (3)	−0.0004 (3)
O12	0.0091 (4)	0.0064 (4)	0.0102 (4)	0.0004 (3)	0.0026 (3)	0.0012 (3)
O13	0.0098 (4)	0.0072 (4)	0.0106 (4)	0.0014 (3)	0.0013 (3)	0.0010 (3)
O14	0.0105 (4)	0.0095 (4)	0.0079 (4)	0.0011 (3)	0.0007 (3)	0.0007 (3)
O15	0.0083 (4)	0.0122 (4)	0.0087 (4)	0.0010 (3)	0.0004 (3)	−0.0019 (3)
O16	0.0064 (4)	0.0089 (4)	0.0105 (4)	−0.0008 (3)	0.0005 (3)	−0.0020 (3)
N1	0.0065 (5)	0.0086 (5)	0.0094 (5)	0.0014 (4)	0.0011 (4)	−0.0005 (4)
N2	0.0077 (5)	0.0072 (4)	0.0081 (5)	0.0003 (4)	0.0021 (4)	−0.0001 (4)
C1	0.0087 (6)	0.0069 (5)	0.0082 (6)	−0.0003 (4)	−0.0004 (4)	−0.0006 (5)
C2	0.0082 (6)	0.0092 (5)	0.0097 (5)	0.0001 (4)	0.0022 (5)	0.0002 (4)
C3	0.0085 (6)	0.0083 (5)	0.0089 (6)	−0.0007 (4)	0.0009 (4)	−0.0021 (5)
C4	0.0080 (6)	0.0089 (5)	0.0110 (6)	−0.0005 (4)	0.0022 (5)	−0.0004 (4)
C5	0.0086 (6)	0.0073 (5)	0.0086 (5)	0.0014 (4)	0.0004 (4)	0.0006 (5)
C6	0.0084 (7)	0.0096 (5)	0.0080 (5)	0.0003 (5)	0.0011 (4)	0.0007 (4)
C7	0.0090 (6)	0.0084 (5)	0.0076 (6)	−0.0005 (4)	0.0006 (4)	−0.0003 (5)
C8	0.0097 (7)	0.0095 (5)	0.0081 (5)	−0.0012 (5)	−0.0001 (4)	−0.0004 (4)
C9	0.0138 (6)	0.0102 (5)	0.0085 (6)	0.0039 (5)	−0.0007 (5)	−0.0011 (5)
C10	0.0110 (6)	0.0076 (6)	0.0101 (6)	0.0018 (4)	−0.0003 (4)	0.0007 (5)
C11	0.0094 (6)	0.0098 (5)	0.0085 (6)	0.0022 (5)	0.0020 (5)	0.0003 (4)
C12	0.0070 (6)	0.0093 (5)	0.0103 (6)	0.0001 (4)	0.0007 (5)	0.0008 (5)
C13	0.0083 (6)	0.0084 (5)	0.0084 (6)	−0.0022 (4)	0.0010 (5)	−0.0001 (4)
C14	0.0094 (6)	0.0070 (5)	0.0083 (6)	−0.0010 (4)	0.0010 (5)	0.0001 (4)
C15	0.0083 (6)	0.0066 (5)	0.0092 (6)	0.0003 (4)	0.0005 (5)	0.0001 (4)
C16	0.0094 (6)	0.0087 (5)	0.0073 (6)	−0.0001 (4)	0.0005 (5)	−0.0010 (4)
C17	0.0084 (6)	0.0092 (6)	0.0117 (6)	0.0021 (5)	0.0018 (5)	0.0012 (5)
C18	0.0101 (6)	0.0079 (5)	0.0116 (6)	0.0014 (5)	0.0014 (5)	0.0016 (5)
C19	0.0120 (6)	0.0089 (6)	0.0131 (6)	0.0025 (5)	0.0027 (5)	0.0030 (5)
C20	0.0122 (6)	0.0120 (6)	0.0090 (6)	0.0023 (5)	0.0020 (5)	0.0031 (5)
C21	0.0125 (6)	0.0087 (5)	0.0079 (6)	0.0018 (5)	0.0011 (5)	0.0015 (4)
C22	0.0093 (6)	0.0095 (5)	0.0093 (6)	0.0008 (5)	0.0031 (5)	0.0020 (5)
C23	0.0083 (6)	0.0111 (6)	0.0123 (6)	0.0017 (5)	0.0010 (5)	−0.0034 (5)
C24	0.0082 (6)	0.0139 (6)	0.0097 (6)	0.0007 (5)	0.0006 (5)	−0.0031 (5)
C25	0.0077 (6)	0.0093 (6)	0.0090 (6)	−0.0007 (4)	−0.0008 (4)	−0.0021 (5)
C26	0.0079 (6)	0.0097 (5)	0.0103 (6)	−0.0011 (4)	0.0003 (5)	−0.0016 (5)
C27	0.0069 (6)	0.0106 (6)	0.0104 (6)	−0.0013 (4)	0.0010 (5)	−0.0020 (5)
C28	0.0070 (6)	0.0086 (5)	0.0093 (6)	−0.0003 (4)	0.0007 (4)	−0.0010 (5)
H	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1D	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1E	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1F	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1G	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1H	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1I	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1J	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1K	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1L	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1M	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1N	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1O	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1P	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1Q	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H1R	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2D	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2E	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2F	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2G	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2H	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2I	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2J	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2K	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2L	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2M	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2N	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2O	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2P	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2Q	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2R	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000

Geometric parameters (Å, º)

Cr1—C1	1.9030 (12)	N2—C22	1.4733 (14)
Cr1—C2	1.9076 (12)	N2—C28	1.4649 (14)
Cr1—C3	1.9016 (12)	C11—C12	1.5166 (16)
Cr1—C4	1.9006 (12)	C11—H1A	1.102 (12)
Cr1—C5	1.8525 (12)	C11—H1B	1.088 (12)
Cr1—H	1.732 (12)	C12—H1C	1.120 (12)
Cr2—C6	1.9048 (12)	C12—H1D	1.101 (12)
Cr2—C7	1.9014 (12)	C13—C14	1.5022 (16)
Cr2—C8	1.9010 (12)	C13—H1E	1.104 (12)
Cr2—C9	1.9133 (12)	C13—H1F	1.085 (12)
Cr2—C10	1.8477 (12)	C14—H1G	1.086 (12)
Cr2—H	1.723 (12)	C14—H1H	1.094 (12)
K1—O1	2.9701 (8)	C15—C16	1.5155 (15)
K1—O11	2.8644 (8)	C15—H1I	1.091 (12)
K1—O12	2.8642 (8)	C15—H1J	1.096 (12)
K1—O13	2.8031 (8)	C16—H1K	1.071 (12)
K1—O14	2.8002 (8)	C16—H1L	1.101 (12)
K1—O15	2.8814 (8)	C17—C18	1.5167 (15)
K1—O16	2.8424 (8)	C17—H1M	1.083 (12)
K1—N1	3.0165 (10)	C17—H1N	1.096 (12)
K1—N2	3.0122 (9)	C18—H1O	1.123 (12)
O1—C1	1.1438 (14)	C18—H1P	1.081 (12)
O2—C2	1.1396 (14)	C19—C20	1.5065 (16)
O3—C3	1.1434 (14)	C19—H1Q	1.082 (12)
O4—C4	1.1435 (14)	C19—H1R	1.083 (12)
O5—C5	1.1529 (14)	C20—H2A	1.085 (12)
O6—C6	1.1410 (14)	C20—H2B	1.084 (12)
O7—C7	1.1442 (14)	C21—C22	1.5141 (16)
O8—C8	1.1442 (14)	C21—H2C	1.095 (12)
O9—C9	1.1386 (15)	C21—H2D	1.082 (12)
O10—C10	1.1560 (14)	C22—H2E	1.117 (12)
O11—C12	1.4177 (13)	C22—H2F	1.092 (12)
O11—C13	1.4261 (13)	C23—C24	1.5130 (16)
O12—C14	1.4187 (13)	C23—H2G	1.072 (12)
O12—C15	1.4210 (13)	C23—H2H	1.099 (12)
O13—C18	1.4144 (13)	C24—H2I	1.126 (12)
O13—C19	1.4190 (13)	C24—H2J	1.088 (12)
O14—C20	1.4204 (14)	C25—C26	1.5060 (15)
O14—C21	1.4273 (13)	C25—H2K	1.108 (12)
O15—C24	1.4251 (13)	C25—H2L	1.111 (12)
O15—C25	1.4153 (14)	C26—H2M	1.097 (12)
O16—C26	1.4224 (13)	C26—H2N	1.085 (12)
O16—C27	1.4213 (13)	C27—C28	1.5164 (15)
N1—C11	1.4687 (14)	C27—H2O	1.084 (12)
N1—C17	1.4724 (14)	C27—H2P	1.114 (12)
N1—C23	1.4717 (14)	C28—H2Q	1.103 (12)
N2—C16	1.4703 (14)	C28—H2R	1.061 (12)
C2—Cr1—C1	91.95 (5)	H1A—C11—N1	110.2 (6)
C3—Cr1—C1	174.95 (5)	H1A—C11—C12	108.9 (6)
C3—Cr1—C2	92.97 (5)	H1B—C11—N1	107.7 (6)
C4—Cr1—C1	89.72 (5)	H1B—C11—C12	108.3 (6)
C4—Cr1—C2	175.11 (5)	H1B—C11—H1A	106.7 (9)
C4—Cr1—C3	85.28 (5)	C11—C12—O11	110.35 (9)
C5—Cr1—C1	89.92 (5)	H1C—C12—O11	109.7 (6)
C5—Cr1—C2	90.11 (5)	H1C—C12—C11	111.3 (6)
C5—Cr1—C3	91.20 (5)	H1D—C12—O11	110.3 (6)
C5—Cr1—C4	94.49 (5)	H1D—C12—C11	108.6 (6)
H—Cr1—C1	96.0 (4)	H1D—C12—H1C	106.5 (9)
H—Cr1—C2	76.3 (4)	C14—C13—O11	109.66 (9)
H—Cr1—C3	84.0 (4)	H1E—C13—O11	110.5 (6)
H—Cr1—C4	99.0 (4)	H1E—C13—C14	110.4 (6)
H—Cr1—C5	165.3 (4)	H1F—C13—O11	111.0 (6)
C7—Cr2—C6	89.95 (5)	H1F—C13—C14	108.6 (6)
C8—Cr2—C6	176.30 (5)	H1F—C13—H1E	106.6 (9)
C8—Cr2—C7	91.97 (5)	C13—C14—O12	108.85 (9)
C9—Cr2—C6	88.72 (5)	H1G—C14—O12	110.5 (6)
C9—Cr2—C7	171.10 (5)	H1G—C14—C13	108.2 (6)
C9—Cr2—C8	89.87 (5)	H1H—C14—O12	111.9 (6)
C10—Cr2—C6	90.11 (5)	H1H—C14—C13	109.5 (6)
C10—Cr2—C7	93.68 (5)	H1H—C14—H1G	107.8 (9)
C10—Cr2—C8	86.60 (5)	C16—C15—O12	108.79 (9)
C10—Cr2—C9	95.13 (5)	H1I—C15—O12	109.5 (6)
H—Cr2—C6	81.5 (4)	H1I—C15—C16	108.1 (6)
H—Cr2—C7	83.7 (4)	H1J—C15—O12	110.3 (6)
H—Cr2—C8	101.8 (4)	H1J—C15—C16	113.6 (6)
H—Cr2—C9	87.3 (4)	H1J—C15—H1I	106.5 (9)
H—Cr2—C10	171.2 (4)	C15—C16—N2	114.16 (9)
O11—K1—O1	71.91 (2)	H1K—C16—N2	107.1 (6)
O12—K1—O1	65.08 (2)	H1K—C16—C15	109.0 (6)
O12—K1—O11	58.94 (2)	H1L—C16—N2	110.7 (6)
O13—K1—O1	64.19 (2)	H1L—C16—C15	108.3 (6)
O13—K1—O11	104.42 (2)	H1L—C16—H1K	107.3 (9)
O13—K1—O12	129.27 (2)	C18—C17—N1	113.82 (9)
O14—K1—O1	74.49 (2)	H1M—C17—N1	107.8 (6)
O14—K1—O11	146.36 (2)	H1M—C17—C18	106.3 (6)
O14—K1—O12	104.64 (2)	H1N—C17—N1	111.0 (6)
O14—K1—O13	61.24 (2)	H1N—C17—C18	108.7 (6)
O15—K1—O1	147.84 (2)	H1N—C17—H1M	109.0 (9)
O15—K1—O11	99.54 (2)	C17—C18—O13	109.31 (9)
O15—K1—O12	137.67 (2)	H1O—C18—O13	108.6 (6)
O15—K1—O13	89.40 (2)	H1O—C18—C17	109.6 (6)
O15—K1—O14	109.91 (2)	H1P—C18—O13	109.7 (6)
O16—K1—O1	152.20 (2)	H1P—C18—C17	111.8 (6)
O16—K1—O11	119.28 (2)	H1P—C18—H1O	107.7 (9)
O16—K1—O12	97.63 (2)	C20—C19—O13	109.11 (9)
O16—K1—O13	128.48 (2)	H1Q—C19—O13	110.2 (6)
O16—K1—O14	90.39 (2)	H1Q—C19—C20	110.9 (6)
O16—K1—O15	59.17 (2)	H1R—C19—O13	110.8 (6)
N1—K1—O1	90.40 (2)	H1R—C19—C20	108.4 (6)
N1—K1—O11	62.03 (2)	H1R—C19—H1Q	107.5 (9)
N1—K1—O12	120.45 (2)	C19—C20—O14	109.94 (9)
N1—K1—O13	60.31 (2)	H2A—C20—O14	110.9 (6)
N1—K1—O14	120.38 (2)	H2A—C20—C19	108.6 (6)
N1—K1—O15	59.32 (2)	H2B—C20—O14	109.8 (6)
N1—K1—O16	117.40 (2)	H2B—C20—C19	110.2 (6)
N2—K1—O1	91.99 (2)	H2B—C20—H2A	107.4 (9)
N2—K1—O11	117.24 (2)	C22—C21—O14	109.37 (9)
N2—K1—O12	59.31 (2)	H2C—C21—O14	110.0 (6)
N2—K1—O13	122.30 (2)	H2C—C21—C22	109.0 (6)
N2—K1—O14	61.93 (2)	H2D—C21—O14	110.1 (6)
N2—K1—O15	118.64 (2)	H2D—C21—C22	112.2 (6)
N2—K1—O16	60.21 (2)	H2D—C21—H2C	106.1 (9)
N2—K1—N1	177.10 (3)	C21—C22—N2	113.25 (9)
C1—O1—K1	148.74 (8)	H2E—C22—N2	110.7 (6)
C12—O11—K1	111.70 (6)	H2E—C22—C21	108.8 (6)
C13—O11—K1	113.91 (6)	H2F—C22—N2	110.3 (6)
C13—O11—C12	110.27 (8)	H2F—C22—C21	106.8 (6)
C14—O12—K1	117.52 (6)	H2F—C22—H2E	106.7 (9)
C15—O12—K1	121.04 (6)	C24—C23—N1	113.44 (9)
C15—O12—C14	111.89 (8)	H2G—C23—N1	108.9 (6)
C18—O13—K1	121.06 (6)	H2G—C23—C24	107.0 (6)
C19—O13—K1	113.60 (6)	H2H—C23—N1	112.3 (6)
C19—O13—C18	112.06 (8)	H2H—C23—C24	109.4 (6)
C20—O14—K1	113.71 (6)	H2H—C23—H2G	105.2 (9)
C21—O14—K1	112.06 (6)	C23—C24—O15	108.68 (9)
C21—O14—C20	110.73 (8)	H2I—C24—O15	110.6 (6)
C24—O15—K1	115.62 (6)	H2I—C24—C23	112.1 (6)
C25—O15—K1	117.03 (6)	H2J—C24—O15	109.7 (6)
C25—O15—C24	111.41 (8)	H2J—C24—C23	110.7 (6)
C26—O16—K1	112.75 (6)	H2J—C24—H2I	105.0 (8)
C27—O16—K1	120.07 (6)	C26—C25—O15	109.35 (9)
C27—O16—C26	110.55 (8)	H2K—C25—O15	111.3 (6)
C11—N1—K1	107.25 (6)	H2K—C25—C26	108.7 (6)
C17—N1—K1	107.29 (6)	H2L—C25—O15	110.5 (6)
C17—N1—C11	110.16 (9)	H2L—C25—C26	109.5 (6)
C23—N1—K1	112.10 (6)	H2L—C25—H2K	107.5 (8)
C23—N1—C11	109.37 (9)	C25—C26—O16	109.47 (9)
C23—N1—C17	110.60 (9)	H2M—C26—O16	110.7 (6)
C16—N2—K1	109.79 (6)	H2M—C26—C25	111.1 (6)
C22—N2—K1	107.57 (6)	H2N—C26—O16	111.3 (6)
C22—N2—C16	109.56 (9)	H2N—C26—C25	107.0 (6)
C28—N2—K1	108.73 (6)	H2N—C26—H2M	107.2 (9)
C28—N2—C16	109.89 (9)	C28—C27—O16	110.55 (9)
C28—N2—C22	111.26 (9)	H2O—C27—O16	109.8 (6)
O1—C1—Cr1	177.11 (10)	H2O—C27—C28	110.9 (6)
O2—C2—Cr1	178.69 (10)	H2P—C27—O16	108.0 (6)
O3—C3—Cr1	175.90 (10)	H2P—C27—C28	108.6 (6)
O4—C4—Cr1	177.79 (10)	H2P—C27—H2O	108.9 (9)
O5—C5—Cr1	177.67 (10)	C27—C28—N2	114.20 (9)
O6—C6—Cr2	178.85 (10)	H2Q—C28—N2	112.2 (6)
O7—C7—Cr2	178.54 (10)	H2Q—C28—C27	107.1 (6)
O8—C8—Cr2	174.79 (10)	H2R—C28—N2	107.6 (6)
O9—C9—Cr2	178.57 (10)	H2R—C28—C27	108.9 (6)
O10—C10—Cr2	177.89 (10)	H2R—C28—H2Q	106.6 (9)
C12—C11—N1	114.72 (9)	Cr2—H—Cr1	146.1 (8)
K1—O11—C12—C11	−55.88 (6)	K1—N1—C23—C24	−37.59 (7)
K1—O11—C13—C14	53.09 (6)	K1—N2—C16—C15	−48.45 (7)
K1—O12—C14—C13	42.31 (7)	K1—N2—C22—C21	−39.29 (7)
K1—O12—C15—C16	−41.02 (7)	K1—N2—C28—C27	−48.50 (7)
K1—O13—C18—C17	−40.70 (7)	O11—C12—C11—N1	69.71 (10)
K1—O13—C19—C20	49.25 (7)	O11—C13—C14—O12	−63.33 (9)
K1—O14—C20—C19	47.69 (7)	O12—C15—C16—N2	60.64 (9)
K1—O14—C21—C22	−59.71 (6)	O13—C18—C17—N1	62.37 (10)
K1—O15—C24—C23	−56.08 (7)	O13—C19—C20—O14	−65.86 (10)
K1—O15—C25—C26	37.72 (6)	O14—C21—C22—N2	69.61 (9)
K1—O16—C26—C25	57.35 (6)	O15—C24—C23—N1	63.27 (10)
K1—O16—C27—C28	−39.08 (7)	O15—C25—C26—O16	−63.60 (9)
K1—N1—C11—C12	−41.29 (7)	O16—C27—C28—N2	60.45 (10)
K1—N1—C17—C18	−49.77 (7)

(KCPTCR_standard_HAR)

Crystal data

C28H37Cr2KN2O16	F(000) = 1660.306
Mr = 800.70	Dx = 1.489 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71069 Å
a = 10.458 Å	Cell parameters from 1024 reflections
b = 14.417 Å	θ = 47.5–1.5°
c = 23.882 Å	µ = 0.80 mm^−1
β = 97.26°	T = 28 K
V = 3571.89 Å^3	Ellipsoidal, yellow
Z = 4	0.3 × 0.25 × 0.2 mm

Data collection

SMART CCD diffractometer	5667 reflections with I ≥ 2u(I)
ω scan	Rint = 0.0000
Absorption correction: empirical (using intensity measurements)	θmax = 25.0°, θmin = 2.4°
Tmin = 0.890, Tmax = 0.903	h = −19→20
27917 measured reflections	k = 0→30
5993 independent reflections	l = 0→50

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.014	All H-atom parameters refined
wR(F^2) = 0.032	w = 1/[σ^2(Fo^2) + (0.014P)^2 + 0.3944P] where P = (Fo^2 + 2Fc^2)/3
S = 1.03	(Δ/σ)max = 0.001
5993 reflections	Δρmax = 0.22 e Å^−3
755 parameters	Δρmin = −0.16 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Cr1	0.163858 (13)	0.002352 (9)	0.236365 (6)	0.00553 (4)
Cr2	0.018768 (13)	0.177465 (9)	0.165105 (6)	0.00604 (4)
K1	0.463738 (18)	0.199296 (12)	0.418013 (8)	0.00681 (4)
O1	0.25196 (6)	0.13805 (4)	0.33117 (3)	0.01238 (14)
O2	−0.08338 (6)	−0.04365 (4)	0.28574 (3)	0.01452 (14)
O3	0.10477 (6)	−0.12653 (4)	0.13552 (3)	0.01306 (14)
O4	0.39546 (6)	0.05450 (4)	0.17753 (3)	0.01410 (14)
O5	0.30036 (6)	−0.15025 (4)	0.30578 (3)	0.01295 (14)
O6	−0.25961 (6)	0.12165 (4)	0.17228 (3)	0.01278 (14)
O7	0.01685 (6)	0.05857 (4)	0.05960 (3)	0.01285 (14)
O8	0.28627 (6)	0.25364 (4)	0.15526 (3)	0.01348 (14)
O9	0.02671 (7)	0.26554 (4)	0.28169 (3)	0.01796 (15)
O10	−0.07197 (6)	0.34761 (4)	0.09920 (3)	0.01493 (14)
O11	0.28564 (6)	0.09216 (4)	0.47310 (3)	0.00824 (13)
O12	0.44353 (6)	0.00263 (4)	0.40247 (3)	0.00860 (13)
O13	0.31322 (6)	0.34101 (4)	0.36297 (2)	0.00931 (13)
O14	0.52818 (6)	0.26682 (4)	0.31526 (3)	0.00953 (13)
O15	0.55092 (6)	0.32679 (4)	0.50766 (3)	0.00998 (13)
O16	0.72729 (6)	0.20520 (4)	0.46500 (3)	0.00873 (13)
N1	0.27297 (7)	0.30197 (5)	0.47984 (3)	0.00821 (15)
N2	0.66194 (7)	0.09453 (5)	0.36193 (3)	0.00758 (15)
C1	0.21634 (8)	0.08864 (6)	0.29511 (4)	0.00817 (18)
C2	0.00993 (9)	−0.02695 (6)	0.26776 (4)	0.00896 (18)
C3	0.12291 (8)	−0.07936 (6)	0.17416 (4)	0.00874 (18)
C4	0.30819 (9)	0.03673 (6)	0.19998 (4)	0.00931 (18)
C5	0.25040 (8)	−0.09131 (6)	0.27869 (4)	0.00829 (18)
C6	−0.15481 (9)	0.14175 (6)	0.16988 (4)	0.00877 (18)
C7	0.01883 (8)	0.10392 (6)	0.09904 (4)	0.00851 (18)
C8	0.18842 (9)	0.22120 (6)	0.16008 (4)	0.00933 (18)
C9	0.02386 (9)	0.23378 (6)	0.23786 (4)	0.01109 (19)
C10	−0.03871 (9)	0.28253 (6)	0.12525 (4)	0.00980 (18)
C11	0.20810 (10)	0.23289 (6)	0.51156 (4)	0.00944 (18)
C12	0.17298 (9)	0.14350 (6)	0.47990 (4)	0.00897 (18)
C13	0.25210 (9)	0.00550 (6)	0.44645 (4)	0.00848 (18)
C14	0.37229 (9)	−0.04769 (6)	0.43912 (4)	0.00837 (18)
C15	0.54815 (9)	−0.04993 (6)	0.38670 (4)	0.00822 (18)
C16	0.60997 (9)	0.00370 (6)	0.34260 (4)	0.00852 (18)
C17	0.17921 (9)	0.34657 (7)	0.43700 (4)	0.00992 (19)
C18	0.24066 (10)	0.40154 (6)	0.39329 (4)	0.01010 (19)
C19	0.37487 (10)	0.38868 (7)	0.32183 (4)	0.01137 (19)
C20	0.42824 (10)	0.31891 (7)	0.28400 (4)	0.01106 (19)
C21	0.57230 (10)	0.19493 (6)	0.28137 (4)	0.00986 (19)
C22	0.69044 (9)	0.14952 (7)	0.31301 (4)	0.00930 (18)
C23	0.33599 (9)	0.37150 (7)	0.51920 (4)	0.01069 (19)
C24	0.46525 (9)	0.34029 (7)	0.54883 (4)	0.01081 (19)
C25	0.67992 (9)	0.31751 (7)	0.53312 (4)	0.00893 (18)
C26	0.76446 (10)	0.29309 (6)	0.48872 (4)	0.00950 (18)
C27	0.82386 (9)	0.16968 (7)	0.43399 (4)	0.00943 (18)
C28	0.77739 (9)	0.08198 (6)	0.40284 (4)	0.00857 (18)
H	0.0490 (12)	0.0735 (9)	0.1996 (6)	0.039 (4)
H1A	0.1193 (11)	0.2626 (8)	0.5253 (5)	0.021 (3)
H1B	0.2717 (12)	0.2159 (8)	0.5496 (5)	0.026 (3)
H1C	0.1177 (11)	0.1569 (8)	0.4377 (5)	0.020 (3)
H1D	0.1093 (11)	0.1024 (8)	0.5037 (5)	0.023 (3)
H1E	0.1934 (11)	0.0159 (8)	0.4050 (5)	0.018 (3)
H1F	0.1935 (11)	−0.0359 (8)	0.4718 (5)	0.023 (3)
H1G	0.3435 (10)	−0.1150 (8)	0.4209 (5)	0.018 (3)*
H1H	0.4288 (10)	−0.0592 (7)	0.4805 (5)	0.015 (3)
H1I	0.5130 (11)	−0.1154 (8)	0.3679 (5)	0.023 (3)
H1J	0.6158 (11)	−0.0680 (8)	0.4247 (5)	0.020 (3)
H1K	0.5389 (12)	0.0161 (8)	0.3065 (5)	0.024 (3)*
H1L	0.6862 (11)	−0.0396 (8)	0.3281 (5)	0.023 (3)
H1M	0.1227 (11)	0.2921 (8)	0.4139 (5)	0.023 (3)
H1N	0.1137 (11)	0.3923 (8)	0.4568 (5)	0.022 (3)
H1O	0.1646 (11)	0.4342 (8)	0.3631 (5)	0.026 (3)
H1P	0.3023 (11)	0.4568 (8)	0.4128 (5)	0.025 (3)
H1Q	0.4498 (12)	0.4331 (8)	0.3425 (5)	0.027 (3)
H1R	0.3070 (12)	0.4330 (9)	0.2958 (5)	0.035 (4)
H2A	0.3505 (12)	0.2742 (9)	0.2658 (5)	0.028 (3)
H2B	0.4656 (12)	0.3542 (9)	0.2491 (5)	0.033 (3)
H2C	0.5960 (11)	0.2242 (8)	0.2419 (5)	0.024 (3)*
H2D	0.4956 (12)	0.1454 (8)	0.2696 (5)	0.028 (3)
H2E	0.7371 (11)	0.1055 (8)	0.2829 (5)	0.024 (3)
H2F	0.7577 (11)	0.2052 (8)	0.3270 (5)	0.021 (3)
H2G	0.3535 (11)	0.4330 (8)	0.4958 (5)	0.025 (3)
H2H	0.2738 (11)	0.3931 (9)	0.5512 (5)	0.027 (3)
H2I	0.4574 (11)	0.2757 (8)	0.5743 (5)	0.023 (3)
H2J	0.5042 (12)	0.3926 (9)	0.5793 (5)	0.030 (3)*
H2K	0.7157 (10)	0.3822 (8)	0.5539 (5)	0.020 (3)
H2L	0.6885 (10)	0.2627 (8)	0.5662 (5)	0.021 (3)
H2M	0.7578 (11)	0.3465 (9)	0.4556 (5)	0.028 (3)
H2N	0.8640 (12)	0.2907 (8)	0.5094 (5)	0.029 (3)
H2O	0.8497 (12)	0.2222 (8)	0.4049 (5)	0.027 (3)
H2P	0.9101 (11)	0.1525 (8)	0.4643 (5)	0.023 (3)
H2Q	0.8588 (11)	0.0545 (8)	0.3828 (5)	0.024 (3)
H2R	0.7541 (11)	0.0311 (8)	0.4329 (5)	0.022 (3)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cr1	0.00583 (8)	0.00490 (7)	0.00581 (7)	0.00011 (5)	0.00050 (5)	−0.00016 (5)
Cr2	0.00691 (8)	0.00553 (7)	0.00548 (7)	0.00086 (5)	0.00000 (5)	0.00014 (5)
K1	0.00628 (10)	0.00688 (9)	0.00717 (9)	0.00028 (7)	0.00044 (7)	−0.00005 (7)
O1	0.0156 (4)	0.0097 (3)	0.0107 (3)	−0.0004 (3)	−0.0027 (3)	−0.0020 (3)
O2	0.0110 (4)	0.0166 (3)	0.0172 (3)	0.0000 (3)	0.0067 (3)	0.0014 (3)
O3	0.0155 (4)	0.0131 (3)	0.0107 (3)	−0.0026 (3)	0.0018 (3)	−0.0045 (3)
O4	0.0112 (4)	0.0142 (3)	0.0181 (4)	−0.0011 (3)	0.0066 (3)	−0.0003 (3)
O5	0.0138 (4)	0.0098 (3)	0.0145 (3)	0.0033 (3)	−0.0011 (3)	0.0022 (3)
O6	0.0103 (4)	0.0154 (3)	0.0132 (3)	−0.0012 (3)	0.0033 (3)	0.0004 (3)
O7	0.0172 (4)	0.0125 (3)	0.0090 (3)	−0.0021 (3)	0.0026 (3)	−0.0035 (3)
O8	0.0115 (4)	0.0155 (3)	0.0132 (3)	−0.0051 (3)	0.0009 (3)	0.0011 (3)
O9	0.0260 (4)	0.0176 (3)	0.0094 (4)	0.0094 (3)	−0.0014 (3)	−0.0049 (3)
O10	0.0184 (4)	0.0094 (3)	0.0158 (3)	0.0031 (3)	−0.0022 (3)	0.0044 (3)
O11	0.0066 (3)	0.0082 (3)	0.0097 (3)	−0.0003 (2)	0.0003 (2)	−0.0006 (2)
O12	0.0092 (3)	0.0066 (3)	0.0103 (3)	0.0004 (2)	0.0026 (3)	0.0011 (2)
O13	0.0099 (3)	0.0072 (3)	0.0108 (3)	0.0012 (2)	0.0014 (3)	0.0011 (2)
O14	0.0106 (3)	0.0097 (3)	0.0082 (3)	0.0011 (2)	0.0008 (2)	0.0007 (2)
O15	0.0087 (3)	0.0123 (3)	0.0088 (3)	0.0010 (2)	0.0004 (2)	−0.0019 (3)
O16	0.0063 (3)	0.0092 (3)	0.0106 (3)	−0.0009 (2)	0.0006 (2)	−0.0020 (2)
N1	0.0068 (4)	0.0084 (4)	0.0095 (4)	0.0013 (3)	0.0012 (3)	−0.0006 (3)
N2	0.0077 (4)	0.0074 (3)	0.0079 (4)	0.0002 (3)	0.0020 (3)	−0.0002 (3)
C1	0.0089 (5)	0.0074 (4)	0.0079 (4)	−0.0003 (3)	−0.0002 (4)	−0.0006 (4)
C2	0.0081 (5)	0.0093 (4)	0.0098 (4)	0.0000 (4)	0.0023 (4)	0.0004 (3)
C3	0.0085 (5)	0.0086 (4)	0.0090 (5)	−0.0008 (3)	0.0008 (4)	−0.0020 (4)
C4	0.0081 (5)	0.0090 (4)	0.0110 (4)	−0.0004 (3)	0.0022 (4)	−0.0004 (3)
C5	0.0086 (5)	0.0074 (4)	0.0086 (4)	0.0016 (3)	0.0000 (4)	0.0007 (4)
C6	0.0085 (5)	0.0098 (4)	0.0081 (4)	0.0004 (4)	0.0011 (3)	0.0005 (3)
C7	0.0091 (5)	0.0085 (4)	0.0079 (5)	−0.0004 (3)	0.0007 (3)	−0.0004 (4)
C8	0.0098 (5)	0.0097 (4)	0.0082 (4)	−0.0014 (4)	−0.0002 (4)	−0.0004 (3)
C9	0.0139 (5)	0.0106 (4)	0.0083 (5)	0.0040 (4)	−0.0007 (4)	−0.0011 (4)
C10	0.0112 (5)	0.0075 (4)	0.0103 (4)	0.0018 (4)	−0.0003 (4)	0.0006 (4)
C11	0.0101 (5)	0.0099 (4)	0.0085 (5)	0.0020 (4)	0.0022 (4)	0.0003 (4)
C12	0.0071 (5)	0.0094 (4)	0.0103 (5)	−0.0001 (4)	0.0008 (4)	0.0007 (4)
C13	0.0083 (5)	0.0083 (4)	0.0088 (5)	−0.0022 (4)	0.0010 (4)	−0.0002 (4)
C14	0.0097 (5)	0.0071 (4)	0.0084 (5)	−0.0008 (3)	0.0010 (4)	0.0002 (4)
C15	0.0088 (5)	0.0065 (4)	0.0093 (5)	0.0002 (4)	0.0009 (4)	0.0001 (4)
C16	0.0094 (5)	0.0088 (4)	0.0074 (4)	−0.0002 (4)	0.0012 (4)	−0.0010 (3)
C17	0.0085 (5)	0.0097 (5)	0.0117 (5)	0.0024 (4)	0.0018 (4)	0.0015 (4)
C18	0.0104 (5)	0.0080 (4)	0.0121 (5)	0.0015 (4)	0.0019 (4)	0.0019 (4)
C19	0.0123 (5)	0.0088 (4)	0.0135 (5)	0.0024 (4)	0.0033 (4)	0.0028 (4)
C20	0.0123 (5)	0.0123 (5)	0.0086 (5)	0.0026 (4)	0.0017 (4)	0.0028 (4)
C21	0.0130 (5)	0.0088 (4)	0.0077 (5)	0.0017 (4)	0.0012 (4)	0.0015 (4)
C22	0.0093 (5)	0.0097 (4)	0.0094 (5)	0.0008 (4)	0.0031 (4)	0.0019 (4)
C23	0.0084 (5)	0.0113 (5)	0.0123 (5)	0.0016 (4)	0.0009 (4)	−0.0033 (4)
C24	0.0083 (5)	0.0141 (5)	0.0098 (5)	0.0006 (4)	0.0003 (4)	−0.0030 (4)
C25	0.0079 (5)	0.0095 (5)	0.0089 (5)	−0.0008 (4)	−0.0007 (4)	−0.0024 (4)
C26	0.0087 (5)	0.0097 (4)	0.0101 (5)	−0.0011 (4)	0.0007 (4)	−0.0014 (4)
C27	0.0071 (5)	0.0106 (5)	0.0106 (5)	−0.0013 (4)	0.0009 (4)	−0.0018 (4)
C28	0.0071 (5)	0.0088 (4)	0.0096 (5)	−0.0001 (4)	0.0003 (4)	−0.0012 (4)
H	0.038 (9)	0.024 (8)	0.054 (10)	0.007 (7)	0.001 (8)	0.008 (7)
H1A	0.019 (7)	0.023 (7)	0.024 (7)	0.003 (6)	0.012 (6)	−0.011 (6)
H1B	0.033 (8)	0.022 (7)	0.022 (8)	−0.003 (6)	0.001 (7)	−0.002 (6)
H1C	0.020 (7)	0.027 (7)	0.012 (7)	0.002 (6)	−0.005 (6)	0.001 (6)
H1D	0.028 (8)	0.016 (7)	0.028 (7)	0.009 (6)	0.014 (6)	0.004 (6)
H1E	0.017 (7)	0.023 (7)	0.016 (7)	0.007 (5)	0.003 (6)	−0.003 (6)
H1F	0.028 (8)	0.018 (7)	0.023 (7)	−0.004 (6)	0.006 (6)	0.002 (6)
H1H	0.012 (7)	0.019 (7)	0.016 (7)	0.002 (5)	0.008 (6)	0.005 (5)
H1I	0.018 (7)	0.025 (8)	0.025 (8)	−0.002 (6)	0.000 (6)	0.000 (6)
H1J	0.013 (7)	0.027 (7)	0.020 (7)	−0.009 (6)	0.002 (6)	0.008 (6)
H1L	0.031 (8)	0.020 (7)	0.020 (7)	0.004 (6)	0.008 (6)	−0.003 (6)
H1M	0.020 (7)	0.027 (7)	0.021 (7)	−0.005 (6)	0.003 (6)	−0.004 (6)
H1N	0.018 (7)	0.030 (8)	0.021 (7)	0.007 (6)	0.009 (6)	0.010 (6)
H1O	0.018 (7)	0.031 (8)	0.031 (8)	−0.001 (6)	0.009 (6)	0.014 (7)
H1P	0.030 (8)	0.019 (7)	0.029 (8)	−0.003 (6)	0.011 (6)	−0.012 (6)
H1Q	0.023 (8)	0.017 (7)	0.041 (9)	−0.005 (6)	0.004 (6)	−0.005 (6)
H1R	0.031 (8)	0.036 (8)	0.039 (9)	0.012 (7)	0.012 (7)	0.029 (7)
H2A	0.027 (8)	0.027 (8)	0.025 (8)	0.005 (7)	−0.013 (6)	−0.001 (6)
H2B	0.041 (9)	0.042 (9)	0.017 (7)	0.008 (7)	0.008 (7)	0.016 (7)
H2D	0.030 (8)	0.017 (7)	0.041 (9)	0.004 (6)	0.018 (7)	−0.005 (6)
H2E	0.028 (8)	0.028 (7)	0.018 (7)	0.001 (6)	0.011 (6)	−0.007 (6)
H2F	0.024 (8)	0.017 (7)	0.022 (7)	0.002 (6)	0.005 (6)	−0.006 (6)
H2G	0.017 (7)	0.022 (7)	0.038 (8)	0.004 (6)	0.007 (6)	0.010 (7)
H2H	0.014 (7)	0.040 (9)	0.031 (8)	−0.014 (6)	0.013 (6)	−0.018 (7)
H2I	0.028 (8)	0.020 (7)	0.021 (7)	0.006 (6)	0.002 (6)	0.008 (6)
H2K	0.009 (7)	0.031 (8)	0.018 (7)	0.003 (6)	−0.004 (5)	0.000 (6)
H2L	0.012 (7)	0.032 (8)	0.018 (7)	0.007 (6)	−0.003 (5)	0.012 (7)
H2M	0.021 (8)	0.034 (8)	0.033 (8)	0.013 (6)	0.014 (6)	−0.003 (7)
H2N	0.020 (8)	0.029 (8)	0.036 (8)	−0.005 (6)	0.000 (7)	−0.016 (6)
H2O	0.039 (9)	0.007 (6)	0.033 (8)	0.003 (6)	−0.004 (7)	−0.007 (6)
H2P	0.015 (7)	0.021 (7)	0.032 (8)	−0.002 (6)	−0.002 (6)	−0.015 (6)
H2Q	0.018 (7)	0.025 (7)	0.028 (8)	0.011 (6)	0.006 (6)	−0.006 (6)
H2R	0.034 (8)	0.013 (6)	0.018 (7)	0.001 (6)	0.001 (6)	0.010 (6)

Geometric parameters (Å, º)

Cr1—C1	1.9033 (9)	N2—C22	1.4733 (11)
Cr1—C2	1.9071 (9)	N2—C28	1.4652 (11)
Cr1—C3	1.9018 (9)	C11—C12	1.5157 (13)
Cr1—C4	1.9002 (9)	C11—H1A	1.109 (11)
Cr1—C5	1.8529 (9)	C11—H1B	1.084 (12)
Cr1—H	1.732 (12)	C12—H1C	1.113 (11)
Cr2—C6	1.9041 (9)	C12—H1D	1.102 (11)
Cr2—C7	1.9011 (9)	C13—C14	1.5014 (13)
Cr2—C8	1.9009 (10)	C13—H1E	1.107 (12)
Cr2—C9	1.9126 (9)	C13—H1F	1.092 (11)
Cr2—C10	1.8486 (9)	C14—H1G	1.090 (11)
Cr2—H	1.720 (12)	C14—H1H	1.098 (11)
K1—O1	2.9707 (7)	C15—C16	1.5155 (12)
K1—O11	2.8644 (6)	C15—H1I	1.089 (12)
K1—O12	2.8638 (6)	C15—H1J	1.109 (11)
K1—O13	2.8030 (6)	C16—H1K	1.080 (12)
K1—O14	2.8003 (6)	C16—H1L	1.103 (11)
K1—O15	2.8811 (6)	C17—C18	1.5167 (12)
K1—O16	2.8429 (6)	C17—H1M	1.090 (12)
K1—N1	3.0160 (7)	C17—H1N	1.099 (12)
K1—N2	3.0122 (7)	C18—H1O	1.108 (12)
O1—C1	1.1432 (11)	C18—H1P	1.090 (12)
O2—C2	1.1404 (11)	C19—C20	1.5057 (13)
O3—C3	1.1428 (11)	C19—H1Q	1.082 (12)
O4—C4	1.1444 (11)	C19—H1R	1.090 (12)
O5—C5	1.1524 (11)	C20—H2A	1.085 (13)
O6—C6	1.1420 (11)	C20—H2B	1.091 (12)
O7—C7	1.1445 (11)	C21—C22	1.5133 (13)
O8—C8	1.1441 (11)	C21—H2C	1.091 (12)
O9—C9	1.1394 (11)	C21—H2D	1.084 (13)
O10—C10	1.1547 (11)	C22—H2E	1.116 (11)
O11—C12	1.4180 (11)	C22—H2F	1.092 (12)
O11—C13	1.4258 (10)	C23—C24	1.5129 (13)
O12—C14	1.4185 (10)	C23—H2G	1.077 (12)
O12—C15	1.4204 (10)	C23—H2H	1.109 (11)
O13—C18	1.4145 (11)	C24—H2I	1.120 (11)
O13—C19	1.4190 (11)	C24—H2J	1.090 (13)
O14—C20	1.4201 (11)	C25—C26	1.5057 (12)
O14—C21	1.4271 (10)	C25—H2K	1.099 (12)
O15—C24	1.4248 (11)	C25—H2L	1.113 (11)
O15—C25	1.4143 (11)	C26—H2M	1.100 (13)
O16—C26	1.4218 (10)	C26—H2N	1.095 (12)
O16—C27	1.4212 (11)	C27—C28	1.5155 (12)
N1—C11	1.4683 (11)	C27—H2O	1.086 (13)
N1—C17	1.4724 (12)	C27—H2P	1.111 (12)
N1—C23	1.4718 (11)	C28—H2Q	1.102 (11)
N2—C16	1.4697 (11)	C28—H2R	1.075 (11)
C2—Cr1—C1	91.95 (4)	H1A—C11—N1	110.4 (6)
C3—Cr1—C1	174.94 (4)	H1A—C11—C12	108.4 (6)
C3—Cr1—C2	92.98 (4)	H1B—C11—N1	108.1 (6)
C4—Cr1—C1	89.71 (4)	H1B—C11—C12	108.1 (6)
C4—Cr1—C2	175.09 (4)	H1B—C11—H1A	106.7 (9)
C4—Cr1—C3	85.29 (4)	C11—C12—O11	110.40 (8)
C5—Cr1—C1	89.93 (4)	H1C—C12—O11	109.3 (6)
C5—Cr1—C2	90.14 (4)	H1C—C12—C11	111.7 (6)
C5—Cr1—C3	91.20 (4)	H1D—C12—O11	110.1 (6)
C5—Cr1—C4	94.48 (4)	H1D—C12—C11	108.9 (6)
H—Cr1—C1	95.9 (4)	H1D—C12—H1C	106.4 (9)
H—Cr1—C2	76.4 (4)	C14—C13—O11	109.71 (7)
H—Cr1—C3	84.1 (4)	H1E—C13—O11	110.9 (6)
H—Cr1—C4	98.9 (4)	H1E—C13—C14	110.1 (6)
H—Cr1—C5	165.4 (4)	H1F—C13—O11	110.8 (6)
C7—Cr2—C6	89.96 (4)	H1F—C13—C14	108.8 (6)
C8—Cr2—C6	176.31 (4)	H1F—C13—H1E	106.4 (9)
C8—Cr2—C7	91.97 (4)	C13—C14—O12	108.87 (7)
C9—Cr2—C6	88.72 (4)	H1G—C14—O12	110.4 (6)
C9—Cr2—C7	171.09 (4)	H1G—C14—C13	107.9 (6)
C9—Cr2—C8	89.85 (4)	H1H—C14—O12	111.6 (5)
C10—Cr2—C6	90.12 (4)	H1H—C14—C13	109.6 (5)
C10—Cr2—C7	93.66 (4)	H1H—C14—H1G	108.4 (8)
C10—Cr2—C8	86.62 (4)	C16—C15—O12	108.82 (7)
C10—Cr2—C9	95.16 (4)	H1I—C15—O12	109.9 (6)
H—Cr2—C6	81.6 (4)	H1I—C15—C16	107.9 (6)
H—Cr2—C7	83.8 (5)	H1J—C15—O12	110.0 (6)
H—Cr2—C8	101.7 (4)	H1J—C15—C16	113.9 (5)
H—Cr2—C9	87.3 (5)	H1J—C15—H1I	106.3 (8)
H—Cr2—C10	171.4 (4)	C15—C16—N2	114.18 (7)
O11—K1—O1	71.920 (17)	H1K—C16—N2	107.0 (6)
O12—K1—O1	65.100 (17)	H1K—C16—C15	109.1 (6)
O12—K1—O11	58.939 (17)	H1L—C16—N2	110.5 (6)
O13—K1—O1	64.169 (17)	H1L—C16—C15	108.6 (6)
O13—K1—O11	104.431 (18)	H1L—C16—H1K	107.2 (9)
O13—K1—O12	129.269 (19)	C18—C17—N1	113.80 (8)
O14—K1—O1	74.474 (18)	H1M—C17—N1	108.0 (6)
O14—K1—O11	146.346 (19)	H1M—C17—C18	106.1 (6)
O14—K1—O12	104.630 (18)	H1N—C17—N1	111.1 (6)
O14—K1—O13	61.232 (17)	H1N—C17—C18	108.9 (6)
O15—K1—O1	147.825 (18)	H1N—C17—H1M	108.8 (9)
O15—K1—O11	99.545 (18)	C17—C18—O13	109.35 (7)
O15—K1—O12	137.663 (18)	H1O—C18—O13	108.5 (6)
O15—K1—O13	89.411 (18)	H1O—C18—C17	109.7 (6)
O15—K1—O14	109.926 (18)	H1P—C18—O13	110.0 (6)
O16—K1—O1	152.202 (18)	H1P—C18—C17	111.5 (6)
O16—K1—O11	119.282 (18)	H1P—C18—H1O	107.7 (9)
O16—K1—O12	97.631 (18)	C20—C19—O13	109.10 (8)
O16—K1—O13	128.484 (18)	H1Q—C19—O13	109.7 (6)
O16—K1—O14	90.390 (18)	H1Q—C19—C20	111.5 (6)
O16—K1—O15	59.172 (17)	H1R—C19—O13	111.1 (6)
N1—K1—O1	90.385 (19)	H1R—C19—C20	108.2 (7)
N1—K1—O11	62.033 (18)	H1R—C19—H1Q	107.2 (9)
N1—K1—O12	120.452 (19)	C19—C20—O14	109.99 (8)
N1—K1—O13	60.321 (18)	H2A—C20—O14	111.1 (6)
N1—K1—O14	120.383 (19)	H2A—C20—C19	108.8 (7)
N1—K1—O15	59.326 (18)	H2B—C20—O14	109.8 (7)
N1—K1—O16	117.410 (19)	H2B—C20—C19	110.0 (7)
N2—K1—O1	91.994 (19)	H2B—C20—H2A	107.1 (9)
N2—K1—O11	117.241 (18)	C22—C21—O14	109.46 (8)
N2—K1—O12	59.308 (18)	H2C—C21—O14	109.5 (6)
N2—K1—O13	122.289 (19)	H2C—C21—C22	109.9 (6)
N2—K1—O14	61.923 (18)	H2D—C21—O14	110.1 (6)
N2—K1—O15	118.646 (19)	H2D—C21—C22	112.0 (6)
N2—K1—O16	60.213 (18)	H2D—C21—H2C	105.8 (9)
N2—K1—N1	177.11 (2)	C21—C22—N2	113.24 (8)
C1—O1—K1	148.69 (6)	H2E—C22—N2	110.7 (6)
C12—O11—K1	111.66 (5)	H2E—C22—C21	108.7 (6)
C13—O11—K1	113.90 (5)	H2F—C22—N2	109.8 (6)
C13—O11—C12	110.33 (7)	H2F—C22—C21	106.8 (6)
C14—O12—K1	117.54 (5)	H2F—C22—H2E	107.4 (8)
C15—O12—K1	121.06 (5)	C24—C23—N1	113.43 (7)
C15—O12—C14	111.90 (6)	H2G—C23—N1	108.7 (7)
C18—O13—K1	121.02 (5)	H2G—C23—C24	106.7 (6)
C19—O13—K1	113.60 (5)	H2H—C23—N1	112.1 (6)
C19—O13—C18	112.07 (7)	H2H—C23—C24	109.2 (6)
C20—O14—K1	113.70 (5)	H2H—C23—H2G	106.3 (9)
C21—O14—K1	112.05 (5)	C23—C24—O15	108.69 (7)
C21—O14—C20	110.80 (7)	H2I—C24—O15	110.9 (6)
C24—O15—K1	115.62 (5)	H2I—C24—C23	112.3 (6)
C25—O15—K1	117.02 (5)	H2J—C24—O15	109.9 (6)
C25—O15—C24	111.42 (7)	H2J—C24—C23	110.0 (6)
C26—O16—K1	112.74 (5)	H2J—C24—H2I	105.0 (9)
C27—O16—K1	120.06 (5)	C26—C25—O15	109.42 (8)
C27—O16—C26	110.62 (7)	H2K—C25—O15	111.4 (6)
C11—N1—K1	107.28 (5)	H2K—C25—C26	108.6 (6)
C17—N1—K1	107.32 (5)	H2L—C25—O15	111.1 (6)
C17—N1—C11	110.13 (7)	H2L—C25—C26	109.4 (6)
C23—N1—K1	112.11 (5)	H2L—C25—H2K	106.9 (8)
C23—N1—C11	109.35 (7)	C25—C26—O16	109.49 (8)
C23—N1—C17	110.57 (7)	H2M—C26—O16	110.3 (6)
C16—N2—K1	109.79 (5)	H2M—C26—C25	110.8 (6)
C22—N2—K1	107.59 (5)	H2N—C26—O16	110.4 (6)
C22—N2—C16	109.53 (7)	H2N—C26—C25	107.4 (6)
C28—N2—K1	108.71 (5)	H2N—C26—H2M	108.4 (9)
C28—N2—C16	109.90 (7)	C28—C27—O16	110.58 (7)
C28—N2—C22	111.28 (7)	H2O—C27—O16	109.5 (6)
O1—C1—Cr1	177.17 (7)	H2O—C27—C28	111.0 (6)
O2—C2—Cr1	178.76 (8)	H2P—C27—O16	108.2 (6)
O3—C3—Cr1	175.87 (7)	H2P—C27—C28	108.5 (6)
O4—C4—Cr1	177.77 (7)	H2P—C27—H2O	109.0 (9)
O5—C5—Cr1	177.64 (8)	C27—C28—N2	114.24 (8)
O6—C6—Cr2	178.85 (7)	H2Q—C28—N2	111.8 (6)
O7—C7—Cr2	178.59 (7)	H2Q—C28—C27	107.2 (6)
O8—C8—Cr2	174.72 (8)	H2R—C28—N2	107.0 (6)
O9—C9—Cr2	178.57 (8)	H2R—C28—C27	109.1 (6)
O10—C10—Cr2	177.91 (8)	H2R—C28—H2Q	107.3 (9)
C12—C11—N1	114.70 (8)	Cr2—H—Cr1	146.3 (8)
K1—O11—C12—C11	−55.88 (5)	K1—N1—C23—C24	−37.56 (6)
K1—O11—C13—C14	53.06 (5)	K1—N2—C16—C15	−48.42 (6)
K1—O12—C14—C13	42.25 (5)	K1—N2—C22—C21	−39.23 (5)
K1—O12—C15—C16	−40.94 (5)	K1—N2—C28—C27	−48.50 (5)
K1—O13—C18—C17	−40.72 (6)	O11—C12—C11—N1	69.69 (8)
K1—O13—C19—C20	49.24 (6)	O11—C13—C14—O12	−63.27 (8)
K1—O14—C20—C19	47.67 (5)	O12—C15—C16—N2	60.58 (8)
K1—O14—C21—C22	−59.67 (5)	O13—C18—C17—N1	62.35 (8)
K1—O15—C24—C23	−56.09 (5)	O13—C19—C20—O14	−65.84 (8)
K1—O15—C25—C26	37.71 (5)	O14—C21—C22—N2	69.55 (8)
K1—O16—C26—C25	57.26 (5)	O15—C24—C23—N1	63.25 (8)
K1—O16—C27—C28	−39.01 (5)	O15—C25—C26—O16	−63.57 (8)
K1—N1—C11—C12	−41.25 (5)	O16—C27—C28—N2	60.43 (8)
K1—N1—C17—C18	−49.72 (5)

(KCPTCR_standard_HAR_NoMoRe_1)

Crystal data

C28H37Cr2KN2O16	F(000) = 1660.306
Mr = 800.70	Dx = 1.489 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71069 Å
a = 10.458 Å	Cell parameters from 1024 reflections
b = 14.417 Å	θ = 47.5–1.5°
c = 23.882 Å	µ = 0.80 mm^−1
β = 97.26°	T = 28 K
V = 3571.89 Å^3	Ellipsoidal, yellow
Z = 4	0.3 × 0.25 × 0.2 mm

Data collection

SMART CCD diffractometer	5667 reflections with I ≥ 2u(I)
ω scan	Rint = 0.0000
Absorption correction: empirical (using intensity measurements)	θmax = 25.0°, θmin = 2.4°
Tmin = 0.890, Tmax = 0.903	h = −19→20
27917 measured reflections	k = 0→30
5993 independent reflections	l = 0→50

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.016	Only H-atom coordinates refined
wR(F^2) = 0.055	w = 1/[σ^2(Fo^2) + (0.1P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 0.51	(Δ/σ)max = 0.001
5993 reflections	Δρmax = 0.25 e Å^−3
553 parameters	Δρmin = −0.59 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Cr1	0.163853 (13)	0.002351 (9)	0.236365 (6)	0.00537 (6)
Cr2	0.018773 (14)	0.177459 (10)	0.165113 (6)	0.00586 (6)
K1	0.463767 (17)	0.199315 (13)	0.418021 (8)	0.00665 (6)
O1	0.25195 (6)	0.13804 (4)	0.33118 (3)	0.01200 (14)
O2	−0.08336 (6)	−0.04365 (5)	0.28572 (3)	0.01443 (15)
O3	0.10478 (6)	−0.12655 (5)	0.13550 (3)	0.01289 (15)
O4	0.39544 (6)	0.05442 (5)	0.17752 (3)	0.01370 (15)
O5	0.30034 (6)	−0.15026 (5)	0.30578 (3)	0.01287 (14)
O6	−0.25956 (6)	0.12173 (5)	0.17226 (3)	0.01253 (14)
O7	0.01690 (6)	0.05853 (5)	0.05960 (3)	0.01270 (15)
O8	0.28625 (6)	0.25355 (5)	0.15523 (3)	0.01332 (15)
O9	0.02668 (7)	0.26559 (5)	0.28166 (3)	0.01774 (16)
O10	−0.07195 (7)	0.34760 (5)	0.09920 (3)	0.01480 (15)
O11	0.28561 (6)	0.09220 (4)	0.47309 (3)	0.00804 (13)
O12	0.44349 (6)	0.00266 (4)	0.40251 (3)	0.00827 (14)
O13	0.31320 (6)	0.34098 (4)	0.36298 (3)	0.00894 (14)
O14	0.52812 (6)	0.26682 (4)	0.31527 (3)	0.00933 (13)
O15	0.55081 (6)	0.32675 (4)	0.50763 (3)	0.00975 (14)
O16	0.72733 (6)	0.20518 (4)	0.46503 (3)	0.00874 (13)
N1	0.27295 (7)	0.30199 (5)	0.47983 (3)	0.00808 (16)
N2	0.66197 (7)	0.09450 (5)	0.36198 (3)	0.00745 (16)
C1	0.21632 (9)	0.08869 (6)	0.29519 (4)	0.00824 (18)
C2	0.01009 (9)	−0.02696 (6)	0.26775 (4)	0.00876 (18)
C3	0.12294 (8)	−0.07933 (6)	0.17414 (4)	0.00852 (18)
C4	0.30831 (9)	0.03663 (6)	0.20000 (4)	0.00902 (19)
C5	0.25044 (9)	−0.09127 (6)	0.27869 (4)	0.00829 (18)
C6	−0.15483 (9)	0.14179 (6)	0.16989 (4)	0.00854 (18)
C7	0.01884 (8)	0.10388 (6)	0.09905 (4)	0.00807 (18)
C8	0.18844 (9)	0.22128 (6)	0.16009 (4)	0.00889 (18)
C9	0.02394 (9)	0.23372 (6)	0.23782 (4)	0.01091 (19)
C10	−0.03869 (9)	0.28249 (7)	0.12523 (4)	0.00984 (19)
C11	0.20825 (9)	0.23289 (6)	0.51157 (4)	0.00913 (18)
C12	0.17315 (9)	0.14354 (6)	0.47988 (4)	0.00866 (18)
C13	0.25210 (9)	0.00557 (6)	0.44644 (4)	0.00826 (19)
C14	0.37232 (9)	−0.04767 (6)	0.43914 (4)	0.00811 (18)
C15	0.54807 (9)	−0.04996 (6)	0.38673 (4)	0.00796 (18)
C16	0.60992 (9)	0.00372 (6)	0.34259 (4)	0.00836 (19)
C17	0.17936 (9)	0.34652 (6)	0.43709 (4)	0.00974 (19)
C18	0.24061 (9)	0.40164 (6)	0.39330 (4)	0.00977 (19)
C19	0.37487 (9)	0.38870 (6)	0.32177 (4)	0.01101 (19)
C20	0.42823 (9)	0.31887 (6)	0.28398 (4)	0.01113 (19)
C21	0.57231 (9)	0.19479 (6)	0.28140 (4)	0.00972 (19)
C22	0.69044 (9)	0.14951 (6)	0.31301 (4)	0.00904 (18)
C23	0.33589 (9)	0.37146 (6)	0.51924 (4)	0.01051 (19)
C24	0.46540 (9)	0.34036 (7)	0.54890 (4)	0.01066 (19)
C25	0.68003 (9)	0.31749 (6)	0.53317 (4)	0.00838 (18)
C26	0.76433 (9)	0.29308 (6)	0.48869 (4)	0.00939 (19)
C27	0.82373 (9)	0.16974 (6)	0.43398 (4)	0.00909 (19)
C28	0.77751 (8)	0.08203 (6)	0.40287 (4)	0.00833 (18)
H	0.0496 (13)	0.0750 (10)	0.1992 (6)	0.033652
H1A	0.1194 (13)	0.2617 (9)	0.5254 (6)	0.025013
H1B	0.2728 (13)	0.2170 (9)	0.5497 (6)	0.023076
H1C	0.1188 (13)	0.1562 (9)	0.4379 (6)	0.023746
H1D	0.1087 (12)	0.1019 (9)	0.5035 (6)	0.024598
H1E	0.1943 (13)	0.0151 (9)	0.4053 (6)	0.022215
H1F	0.1941 (13)	−0.0366 (9)	0.4722 (5)	0.023329
H1G	0.3441 (13)	−0.1152 (9)	0.4213 (6)	0.025071
H1H	0.4294 (12)	−0.0582 (9)	0.4801 (5)	0.024233
H1I	0.5125 (12)	−0.1160 (9)	0.3673 (6)	0.022451
H1J	0.6140 (12)	−0.0686 (9)	0.4237 (5)	0.021710
H1K	0.5383 (13)	0.0159 (9)	0.3065 (5)	0.022322
H1L	0.6863 (12)	−0.0393 (9)	0.3283 (5)	0.023001
H1M	0.1245 (13)	0.2932 (9)	0.4142 (6)	0.024511
H1N	0.1147 (13)	0.3933 (10)	0.4567 (6)	0.026678
H1O	0.1636 (13)	0.4350 (9)	0.3626 (6)	0.027525
H1P	0.3031 (13)	0.4574 (9)	0.4132 (6)	0.026323
H1Q	0.4499 (13)	0.4333 (9)	0.3435 (6)	0.027823
H1R	0.3050 (13)	0.4327 (10)	0.2957 (6)	0.029725
H2A	0.3495 (13)	0.2739 (10)	0.2658 (6)	0.026016
H2B	0.4670 (13)	0.3544 (10)	0.2493 (5)	0.028356
H2C	0.5966 (13)	0.2253 (10)	0.2417 (5)	0.025505
H2D	0.4947 (13)	0.1446 (9)	0.2688 (6)	0.024538
H2E	0.7389 (13)	0.1061 (10)	0.2835 (5)	0.025760
H2F	0.7569 (13)	0.2056 (9)	0.3272 (6)	0.024185
H2G	0.3543 (13)	0.4334 (9)	0.4959 (6)	0.025234
H2H	0.2740 (13)	0.3929 (10)	0.5517 (6)	0.026839
H2I	0.4578 (13)	0.2745 (10)	0.5750 (6)	0.026520
H2J	0.5071 (13)	0.3933 (10)	0.5790 (5)	0.027507
H2K	0.7145 (12)	0.3806 (9)	0.5541 (5)	0.024028
H2L	0.6884 (13)	0.2634 (10)	0.5668 (6)	0.023835
H2M	0.7570 (14)	0.3473 (9)	0.4544 (6)	0.025301
H2N	0.8629 (12)	0.2911 (10)	0.5088 (6)	0.026087
H2O	0.8504 (13)	0.2221 (9)	0.4056 (6)	0.025953
H2P	0.9108 (13)	0.1524 (10)	0.4651 (6)	0.027682
H2Q	0.8586 (12)	0.0544 (10)	0.3825 (5)	0.024815
H2R	0.7536 (12)	0.0322 (9)	0.4332 (5)	0.022425

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cr1	0.00570 (9)	0.00479 (9)	0.00556 (9)	0.00015 (5)	0.00041 (6)	−0.00010 (5)
Cr2	0.00675 (9)	0.00544 (9)	0.00519 (9)	0.00085 (5)	−0.00005 (6)	0.00016 (5)
K1	0.00613 (11)	0.00680 (10)	0.00689 (11)	0.00026 (7)	0.00031 (8)	−0.00013 (7)
O1	0.0158 (4)	0.0090 (3)	0.0102 (3)	−0.0003 (3)	−0.0026 (3)	−0.0023 (3)
O2	0.0113 (4)	0.0162 (3)	0.0171 (3)	0.0000 (3)	0.0070 (3)	0.0010 (3)
O3	0.0150 (3)	0.0128 (3)	0.0109 (3)	−0.0024 (3)	0.0017 (3)	−0.0050 (3)
O4	0.0110 (3)	0.0143 (3)	0.0170 (3)	−0.0007 (3)	0.0063 (3)	0.0002 (3)
O5	0.0138 (3)	0.0099 (3)	0.0141 (3)	0.0032 (3)	−0.0010 (3)	0.0022 (3)
O6	0.0097 (4)	0.0151 (3)	0.0133 (3)	−0.0010 (3)	0.0033 (3)	0.0011 (3)
O7	0.0164 (4)	0.0126 (3)	0.0094 (3)	−0.0018 (3)	0.0027 (3)	−0.0036 (3)
O8	0.0110 (4)	0.0158 (3)	0.0131 (3)	−0.0047 (3)	0.0010 (3)	0.0013 (3)
O9	0.0259 (4)	0.0176 (4)	0.0088 (4)	0.0096 (3)	−0.0014 (3)	−0.0050 (3)
O10	0.0184 (4)	0.0092 (3)	0.0156 (3)	0.0028 (3)	−0.0024 (3)	0.0043 (3)
O11	0.0063 (3)	0.0078 (3)	0.0099 (3)	0.0001 (2)	0.0004 (2)	−0.0005 (2)
O12	0.0094 (3)	0.0060 (3)	0.0098 (3)	0.0005 (2)	0.0029 (3)	0.0011 (2)
O13	0.0096 (3)	0.0070 (3)	0.0103 (3)	0.0013 (2)	0.0015 (3)	0.0009 (2)
O14	0.0105 (3)	0.0095 (3)	0.0078 (3)	0.0014 (2)	0.0006 (2)	0.0005 (2)
O15	0.0083 (3)	0.0122 (3)	0.0086 (3)	0.0009 (2)	0.0005 (2)	−0.0019 (2)
O16	0.0059 (3)	0.0093 (3)	0.0108 (3)	−0.0012 (2)	0.0006 (2)	−0.0021 (2)
N1	0.0066 (4)	0.0080 (4)	0.0096 (4)	0.0012 (3)	0.0010 (3)	−0.0008 (3)
N2	0.0073 (4)	0.0073 (3)	0.0080 (4)	0.0000 (3)	0.0017 (3)	0.0001 (3)
C1	0.0085 (4)	0.0067 (4)	0.0093 (4)	0.0002 (3)	0.0000 (3)	−0.0003 (4)
C2	0.0068 (5)	0.0096 (4)	0.0101 (4)	0.0005 (4)	0.0019 (4)	0.0005 (3)
C3	0.0080 (4)	0.0078 (4)	0.0097 (5)	−0.0004 (3)	0.0007 (3)	−0.0019 (4)
C4	0.0077 (5)	0.0087 (4)	0.0109 (4)	−0.0008 (3)	0.0019 (4)	−0.0005 (3)
C5	0.0089 (4)	0.0072 (4)	0.0085 (4)	0.0014 (3)	0.0002 (3)	0.0006 (3)
C6	0.0087 (5)	0.0092 (4)	0.0077 (4)	0.0004 (3)	0.0011 (3)	0.0005 (3)
C7	0.0091 (4)	0.0074 (4)	0.0074 (4)	−0.0002 (3)	0.0001 (3)	−0.0004 (4)
C8	0.0091 (5)	0.0093 (4)	0.0080 (4)	−0.0016 (4)	−0.0001 (3)	−0.0003 (3)
C9	0.0142 (5)	0.0103 (4)	0.0077 (5)	0.0041 (4)	−0.0009 (4)	−0.0009 (4)
C10	0.0111 (4)	0.0074 (4)	0.0106 (4)	0.0013 (3)	0.0000 (4)	0.0005 (4)
C11	0.0101 (4)	0.0097 (4)	0.0079 (4)	0.0024 (4)	0.0020 (3)	0.0001 (3)
C12	0.0065 (4)	0.0093 (4)	0.0100 (4)	0.0002 (3)	0.0006 (3)	0.0009 (3)
C13	0.0082 (5)	0.0082 (4)	0.0085 (4)	−0.0024 (3)	0.0010 (4)	−0.0006 (3)
C14	0.0094 (4)	0.0065 (4)	0.0085 (4)	−0.0006 (3)	0.0013 (3)	0.0007 (3)
C15	0.0080 (4)	0.0072 (4)	0.0086 (4)	0.0006 (3)	0.0009 (4)	0.0006 (3)
C16	0.0097 (5)	0.0087 (4)	0.0067 (4)	−0.0006 (3)	0.0014 (4)	−0.0013 (3)
C17	0.0086 (5)	0.0091 (4)	0.0117 (4)	0.0019 (4)	0.0022 (4)	0.0013 (4)
C18	0.0101 (4)	0.0078 (4)	0.0116 (4)	0.0019 (3)	0.0022 (4)	0.0020 (4)
C19	0.0116 (5)	0.0082 (4)	0.0135 (5)	0.0024 (4)	0.0028 (4)	0.0029 (4)
C20	0.0128 (5)	0.0121 (5)	0.0086 (4)	0.0034 (4)	0.0017 (4)	0.0034 (4)
C21	0.0120 (5)	0.0087 (4)	0.0082 (4)	0.0025 (4)	0.0004 (4)	0.0011 (3)
C22	0.0088 (5)	0.0094 (4)	0.0095 (4)	0.0005 (4)	0.0032 (3)	0.0014 (4)
C23	0.0088 (5)	0.0110 (4)	0.0115 (4)	0.0017 (4)	0.0004 (4)	−0.0037 (4)
C24	0.0078 (5)	0.0145 (5)	0.0093 (4)	0.0005 (4)	−0.0002 (4)	−0.0029 (4)
C25	0.0070 (4)	0.0090 (4)	0.0086 (4)	−0.0005 (3)	−0.0009 (4)	−0.0025 (3)
C26	0.0077 (5)	0.0096 (4)	0.0107 (4)	−0.0015 (3)	0.0005 (4)	−0.0019 (4)
C27	0.0066 (4)	0.0107 (4)	0.0100 (4)	−0.0018 (3)	0.0011 (4)	−0.0023 (4)
C28	0.0065 (4)	0.0087 (4)	0.0097 (4)	0.0000 (3)	0.0008 (3)	−0.0016 (4)
H	0.027000	0.026000	0.046000	0.004000	−0.003000	0.018000
H1A	0.023000	0.023000	0.032000	0.005000	0.015000	−0.000000
H1B	0.028000	0.024000	0.016000	0.000000	−0.002000	0.003000
H1C	0.022000	0.026000	0.021000	0.004000	−0.006000	0.001000
H1D	0.021000	0.022000	0.033000	−0.003000	0.012000	0.003000
H1E	0.022000	0.027000	0.016000	0.000000	−0.004000	−0.001000
H1F	0.026000	0.022000	0.024000	−0.009000	0.011000	−0.000000
H1G	0.033000	0.013000	0.031000	−0.006000	0.011000	−0.005000
H1H	0.026000	0.029000	0.017000	0.005000	0.000000	0.007000
H1I	0.027000	0.013000	0.028000	−0.003000	0.006000	−0.005000
H1J	0.019000	0.026000	0.019000	0.004000	−0.002000	0.006000
H1K	0.025000	0.023000	0.017000	−0.002000	−0.005000	0.001000
H1L	0.024000	0.020000	0.027000	0.004000	0.011000	−0.005000
H1M	0.021000	0.025000	0.026000	−0.006000	−0.003000	0.004000
H1N	0.025000	0.029000	0.028000	0.013000	0.011000	0.005000
H1O	0.025000	0.030000	0.028000	0.013000	0.005000	0.012000
H1P	0.034000	0.017000	0.029000	−0.006000	0.008000	−0.005000
H1Q	0.028000	0.021000	0.036000	−0.009000	0.010000	−0.005000
H1R	0.032000	0.030000	0.028000	0.016000	0.007000	0.014000
H2A	0.021000	0.029000	0.026000	−0.002000	−0.005000	−0.005000
H2B	0.035000	0.032000	0.020000	0.009000	0.011000	0.012000
H2C	0.036000	0.027000	0.015000	0.006000	0.009000	0.006000
H2D	0.024000	0.020000	0.028000	−0.004000	−0.003000	−0.004000
H2E	0.032000	0.026000	0.022000	0.010000	0.014000	0.001000
H2F	0.021000	0.022000	0.029000	−0.007000	0.001000	0.004000
H2G	0.028000	0.016000	0.031000	−0.002000	0.001000	0.003000
H2H	0.024000	0.031000	0.027000	0.003000	0.009000	−0.011000
H2I	0.027000	0.028000	0.025000	0.002000	0.005000	0.010000
H2J	0.026000	0.034000	0.022000	−0.002000	0.001000	−0.014000
H2K	0.025000	0.020000	0.026000	−0.003000	−0.001000	−0.010000
H2L	0.028000	0.024000	0.019000	0.003000	0.001000	0.007000
H2M	0.035000	0.018000	0.024000	−0.002000	0.008000	0.004000
H2N	0.014000	0.031000	0.032000	−0.002000	−0.002000	−0.010000
H2O	0.031000	0.022000	0.027000	−0.007000	0.012000	−0.000000
H2P	0.014000	0.034000	0.033000	0.004000	−0.005000	−0.009000
H2Q	0.017000	0.030000	0.028000	0.006000	0.005000	−0.008000
H2R	0.027000	0.019000	0.020000	−0.002000	−0.002000	0.005000

Geometric parameters (Å, º)

Cr1—C1	1.9051 (9)	N2—C22	1.4741 (11)
Cr1—C2	1.9055 (9)	N2—C28	1.4654 (11)
Cr1—C3	1.9019 (9)	C11—C12	1.5154 (12)
Cr1—C4	1.9005 (9)	C11—H1A	1.105 (13)
Cr1—C5	1.8526 (9)	C11—H1B	1.087 (13)
Cr1—H	1.744 (13)	C12—H1C	1.103 (13)
Cr2—C6	1.9042 (9)	C12—H1D	1.108 (13)
Cr2—C7	1.9013 (9)	C13—C14	1.5019 (13)
Cr2—C8	1.9015 (9)	C13—H1E	1.095 (13)
Cr2—C9	1.9111 (10)	C13—H1F	1.100 (12)
Cr2—C10	1.8483 (10)	C14—H1G	1.088 (13)
Cr2—H	1.698 (13)	C14—H1H	1.090 (12)
K1—O1	2.9711 (7)	C15—C16	1.5168 (12)
K1—O11	2.8645 (6)	C15—H1I	1.104 (13)
K1—O12	2.8637 (6)	C15—H1J	1.083 (12)
K1—O13	2.8028 (6)	C16—H1K	1.083 (12)
K1—O14	2.7999 (6)	C16—H1L	1.099 (12)
K1—O15	2.8795 (6)	C17—C18	1.5182 (12)
K1—O16	2.8431 (6)	C17—H1M	1.067 (13)
K1—N1	3.0161 (8)	C17—H1N	1.102 (13)
K1—N2	3.0121 (8)	C18—H1O	1.126 (13)
O1—C1	1.1413 (11)	C18—H1P	1.105 (13)
O2—C2	1.1415 (12)	C19—C20	1.5057 (13)
O3—C3	1.1432 (11)	C19—H1Q	1.093 (13)
O4—C4	1.1437 (12)	C19—H1R	1.099 (13)
O5—C5	1.1528 (12)	C20—H2A	1.093 (13)
O6—C6	1.1411 (12)	C20—H2B	1.094 (13)
O7—C7	1.1448 (11)	C21—C22	1.5122 (13)
O8—C8	1.1430 (12)	C21—H2C	1.104 (13)
O9—C9	1.1403 (12)	C21—H2D	1.101 (13)
O10—C10	1.1550 (12)	C22—H2E	1.111 (13)
O11—C12	1.4161 (11)	C22—H2F	1.092 (13)
O11—C13	1.4253 (10)	C23—C24	1.5149 (13)
O12—C14	1.4179 (10)	C23—H2G	1.083 (13)
O12—C15	1.4206 (11)	C23—H2H	1.115 (13)
O13—C18	1.4159 (11)	C24—H2I	1.144 (14)
O13—C19	1.4206 (11)	C24—H2J	1.100 (13)
O14—C20	1.4197 (11)	C25—C26	1.5054 (12)
O14—C21	1.4285 (11)	C25—H2K	1.078 (13)
O15—C24	1.4249 (11)	C25—H2L	1.115 (13)
O15—C25	1.4169 (11)	C26—H2M	1.127 (13)
O16—C26	1.4211 (11)	C26—H2N	1.081 (13)
O16—C27	1.4199 (11)	C27—C28	1.5146 (12)
N1—C11	1.4678 (11)	C27—H2O	1.075 (13)
N1—C17	1.4696 (11)	C27—H2P	1.128 (13)
N1—C23	1.4716 (11)	C28—H2Q	1.105 (13)
N2—C16	1.4696 (11)	C28—H2R	1.071 (13)
C2—Cr1—C1	91.92 (4)	H1A—C11—N1	111.0 (7)
C3—Cr1—C1	174.95 (4)	H1A—C11—C12	108.0 (7)
C3—Cr1—C2	93.00 (4)	H1B—C11—N1	107.3 (7)
C4—Cr1—C1	89.75 (4)	H1B—C11—C12	109.0 (7)
C4—Cr1—C2	175.17 (4)	H1B—C11—H1A	106.5 (10)
C4—Cr1—C3	85.26 (4)	C11—C12—O11	110.44 (7)
C5—Cr1—C1	89.90 (4)	H1C—C12—O11	108.8 (7)
C5—Cr1—C2	90.14 (4)	H1C—C12—C11	112.2 (7)
C5—Cr1—C3	91.23 (4)	H1D—C12—O11	110.0 (7)
C5—Cr1—C4	94.40 (4)	H1D—C12—C11	109.3 (7)
H—Cr1—C1	95.6 (5)	H1D—C12—H1C	105.9 (10)
H—Cr1—C2	77.0 (5)	C14—C13—O11	109.72 (7)
H—Cr1—C3	84.4 (5)	H1E—C13—O11	111.6 (7)
H—Cr1—C4	98.3 (5)	H1E—C13—C14	109.6 (7)
H—Cr1—C5	166.2 (5)	H1F—C13—O11	110.9 (7)
C7—Cr2—C6	89.96 (4)	H1F—C13—C14	108.2 (7)
C8—Cr2—C6	176.25 (4)	H1F—C13—H1E	106.8 (10)
C8—Cr2—C7	91.99 (4)	C13—C14—O12	108.81 (7)
C9—Cr2—C6	88.73 (4)	H1G—C14—O12	110.7 (7)
C9—Cr2—C7	171.06 (4)	H1G—C14—C13	108.2 (7)
C9—Cr2—C8	89.82 (4)	H1H—C14—O12	110.7 (7)
C10—Cr2—C6	90.10 (4)	H1H—C14—C13	109.8 (7)
C10—Cr2—C7	93.65 (4)	H1H—C14—H1G	108.5 (10)
C10—Cr2—C8	86.59 (4)	C16—C15—O12	108.79 (7)
C10—Cr2—C9	95.19 (4)	H1I—C15—O12	110.0 (7)
H—Cr2—C6	82.0 (5)	H1I—C15—C16	107.4 (7)
H—Cr2—C7	83.8 (5)	H1J—C15—O12	110.3 (7)
H—Cr2—C8	101.4 (5)	H1J—C15—C16	114.2 (7)
H—Cr2—C9	87.3 (5)	H1J—C15—H1I	106.0 (10)
H—Cr2—C10	171.7 (5)	C15—C16—N2	114.14 (7)
O11—K1—O1	71.901 (18)	H1K—C16—N2	107.4 (7)
O12—K1—O1	65.092 (18)	H1K—C16—C15	108.8 (7)
O12—K1—O11	58.924 (18)	H1L—C16—N2	110.2 (7)
O13—K1—O1	64.160 (18)	H1L—C16—C15	108.6 (7)
O13—K1—O11	104.401 (18)	H1L—C16—H1K	107.5 (10)
O13—K1—O12	129.252 (19)	C18—C17—N1	113.90 (8)
O14—K1—O1	74.465 (19)	H1M—C17—N1	108.0 (7)
O14—K1—O11	146.318 (19)	H1M—C17—C18	105.7 (7)
O14—K1—O12	104.644 (19)	H1N—C17—N1	111.3 (7)
O14—K1—O13	61.228 (18)	H1N—C17—C18	107.9 (7)
O15—K1—O1	147.809 (19)	H1N—C17—H1M	109.9 (10)
O15—K1—O11	99.534 (19)	C17—C18—O13	109.22 (7)
O15—K1—O12	137.657 (19)	H1O—C18—O13	108.4 (7)
O15—K1—O13	89.413 (18)	H1O—C18—C17	110.1 (7)
O15—K1—O14	109.948 (19)	H1P—C18—O13	110.1 (7)
O16—K1—O1	152.203 (19)	H1P—C18—C17	111.2 (7)
O16—K1—O11	119.284 (19)	H1P—C18—H1O	107.8 (10)
O16—K1—O12	97.631 (19)	C20—C19—O13	109.05 (7)
O16—K1—O13	128.515 (19)	H1Q—C19—O13	108.5 (7)
O16—K1—O14	90.419 (19)	H1Q—C19—C20	112.3 (7)
O16—K1—O15	59.194 (17)	H1R—C19—O13	110.1 (7)
N1—K1—O1	90.37 (2)	H1R—C19—C20	108.4 (7)
N1—K1—O11	62.023 (19)	H1R—C19—H1Q	108.4 (11)
N1—K1—O12	120.43 (2)	C19—C20—O14	109.98 (7)
N1—K1—O13	60.310 (19)	H2A—C20—O14	111.3 (7)
N1—K1—O14	120.37 (2)	H2A—C20—C19	108.5 (7)
N1—K1—O15	59.317 (19)	H2B—C20—O14	109.1 (7)
N1—K1—O16	117.42 (2)	H2B—C20—C19	110.0 (7)
N2—K1—O1	92.001 (19)	H2B—C20—H2A	108.0 (10)
N2—K1—O11	117.23 (2)	C22—C21—O14	109.48 (7)
N2—K1—O12	59.315 (19)	H2C—C21—O14	108.8 (7)
N2—K1—O13	122.313 (19)	H2C—C21—C22	109.8 (7)
N2—K1—O14	61.953 (19)	H2D—C21—O14	110.7 (7)
N2—K1—O15	118.66 (2)	H2D—C21—C22	112.4 (7)
N2—K1—O16	60.206 (19)	H2D—C21—H2C	105.6 (10)
N2—K1—N1	177.10 (2)	C21—C22—N2	113.22 (7)
C1—O1—K1	148.72 (6)	H2E—C22—N2	110.7 (7)
C12—O11—K1	111.63 (5)	H2E—C22—C21	109.6 (7)
C13—O11—K1	113.88 (5)	H2F—C22—N2	109.7 (7)
C13—O11—C12	110.38 (7)	H2F—C22—C21	106.4 (7)
C14—O12—K1	117.58 (5)	H2F—C22—H2E	106.9 (10)
C15—O12—K1	121.07 (5)	C24—C23—N1	113.50 (7)
C15—O12—C14	111.85 (7)	H2G—C23—N1	109.0 (7)
C18—O13—K1	121.06 (5)	H2G—C23—C24	106.2 (7)
C19—O13—K1	113.61 (5)	H2H—C23—N1	112.4 (7)
C19—O13—C18	112.01 (7)	H2H—C23—C24	108.7 (7)
C20—O14—K1	113.74 (5)	H2H—C23—H2G	106.6 (10)
C21—O14—K1	111.98 (5)	C23—C24—O15	108.59 (7)
C21—O14—C20	110.82 (7)	H2I—C24—O15	110.8 (7)
C24—O15—K1	115.78 (5)	H2I—C24—C23	112.4 (7)
C25—O15—K1	117.03 (5)	H2J—C24—O15	108.4 (7)
C25—O15—C24	111.25 (7)	H2J—C24—C23	110.9 (7)
C26—O16—K1	112.66 (5)	H2J—C24—H2I	105.6 (10)
C27—O16—K1	120.00 (5)	C26—C25—O15	109.27 (7)
C27—O16—C26	110.67 (7)	H2K—C25—O15	111.4 (7)
C11—N1—K1	107.24 (5)	H2K—C25—C26	109.5 (7)
C17—N1—K1	107.35 (5)	H2L—C25—O15	111.1 (7)
C17—N1—C11	110.19 (7)	H2L—C25—C26	110.2 (7)
C23—N1—K1	112.14 (5)	C25—C26—O16	109.55 (7)
C23—N1—C11	109.27 (7)	H2M—C26—O16	109.9 (7)
C23—N1—C17	110.59 (7)	H2M—C26—C25	110.9 (7)
C16—N2—K1	109.78 (5)	H2N—C26—O16	110.5 (7)
C22—N2—K1	107.57 (5)	H2N—C26—C25	107.7 (7)
C22—N2—C16	109.45 (7)	H2N—C26—H2M	108.3 (11)
C28—N2—K1	108.73 (5)	C28—C27—O16	110.67 (7)
C28—N2—C16	110.01 (7)	H2O—C27—O16	109.6 (7)
C28—N2—C22	111.25 (7)	H2O—C27—C28	111.6 (7)
O1—C1—Cr1	177.15 (8)	H2P—C27—O16	107.7 (7)
O2—C2—Cr1	178.69 (8)	H2P—C27—C28	108.6 (7)
O3—C3—Cr1	175.91 (8)	H2P—C27—H2O	108.6 (10)
O4—C4—Cr1	177.83 (8)	C27—C28—N2	114.19 (7)
O5—C5—Cr1	177.59 (8)	H2Q—C28—N2	111.4 (7)
O6—C6—Cr2	178.85 (8)	H2Q—C28—C27	107.6 (7)
O7—C7—Cr2	178.63 (8)	H2R—C28—N2	106.8 (7)
O8—C8—Cr2	174.82 (8)	H2R—C28—C27	108.4 (7)
O9—C9—Cr2	178.64 (8)	H2R—C28—H2Q	108.3 (10)
O10—C10—Cr2	177.94 (8)	Cr2—H—Cr1	147.4 (9)
C12—C11—N1	114.67 (7)
K1—O11—C12—C11	−55.92 (5)	K1—N1—C23—C24	−37.44 (6)
K1—O11—C13—C14	53.08 (5)	K1—N2—C16—C15	−48.50 (5)
K1—O12—C14—C13	42.27 (5)	K1—N2—C22—C21	−39.26 (5)
K1—O12—C15—C16	−40.93 (6)	K1—N2—C28—C27	−48.40 (5)
K1—O13—C18—C17	−40.69 (6)	O11—C12—C11—N1	69.81 (8)
K1—O13—C19—C20	49.23 (5)	O11—C13—C14—O12	−63.30 (7)
K1—O14—C20—C19	47.71 (5)	O12—C15—C16—N2	60.62 (8)
K1—O14—C21—C22	−59.72 (5)	O13—C18—C17—N1	62.33 (8)
K1—O15—C24—C23	−55.99 (5)	O13—C19—C20—O14	−65.83 (8)
K1—O15—C25—C26	37.71 (5)	O14—C21—C22—N2	69.62 (8)
K1—O16—C26—C25	57.41 (5)	O15—C24—C23—N1	63.02 (8)
K1—O16—C27—C28	−39.14 (5)	O15—C25—C26—O16	−63.68 (7)
K1—N1—C11—C12	−41.32 (5)	O16—C27—C28—N2	60.46 (8)
K1—N1—C17—C18	−49.74 (5)

(KCPTCR_standard_HAR_NoMoRe)

Crystal data

C28H37Cr2KN2O16	F(000) = 1660.306
Mr = 800.70	Dx = 1.489 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71069 Å
a = 10.458 Å	Cell parameters from 1024 reflections
b = 14.417 Å	θ = 47.5–1.5°
c = 23.882 Å	µ = 0.80 mm^−1
β = 97.26°	T = 28 K
V = 3571.89 Å^3	Ellipsoidal, yellow
Z = 4	0.3 × 0.25 × 0.2 mm

Data collection

SMART CCD diffractometer	5667 reflections with I ≥ 2u(I)
ω scan	Rint = 0.0000
Absorption correction: empirical (using intensity measurements)	θmax = 25.0°, θmin = 2.4°
Tmin = 0.890, Tmax = 0.903	h = −19→20
27917 measured reflections	k = 0→30
5993 independent reflections	l = 0→50

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.016	Only H-atom coordinates refined
wR(F^2) = 0.055	w = 1/[σ^2(Fo^2) + (0.1P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 0.51	(Δ/σ)max = 0.001
5993 reflections	Δρmax = 0.25 e Å^−3
553 parameters	Δρmin = −0.59 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Cr1	0.163854 (14)	0.002352 (9)	0.236365 (6)	0.00538 (6)
Cr2	0.018769 (14)	0.177459 (10)	0.165112 (6)	0.00586 (6)
K1	0.463767 (17)	0.199315 (13)	0.418022 (8)	0.00666 (6)
O1	0.25195 (6)	0.13804 (4)	0.33119 (3)	0.01200 (14)
O2	−0.08336 (6)	−0.04365 (5)	0.28572 (3)	0.01444 (15)
O3	0.10478 (6)	−0.12655 (5)	0.13550 (3)	0.01289 (15)
O4	0.39544 (6)	0.05442 (5)	0.17752 (3)	0.01369 (15)
O5	0.30034 (6)	−0.15026 (5)	0.30578 (3)	0.01287 (14)
O6	−0.25956 (6)	0.12173 (5)	0.17225 (3)	0.01252 (14)
O7	0.01690 (6)	0.05854 (5)	0.05960 (3)	0.01271 (15)
O8	0.28626 (6)	0.25355 (5)	0.15523 (3)	0.01332 (15)
O9	0.02668 (7)	0.26559 (5)	0.28166 (3)	0.01775 (16)
O10	−0.07195 (7)	0.34759 (5)	0.09920 (3)	0.01478 (15)
O11	0.28561 (6)	0.09220 (4)	0.47309 (3)	0.00804 (13)
O12	0.44349 (6)	0.00266 (4)	0.40251 (3)	0.00827 (14)
O13	0.31320 (6)	0.34098 (4)	0.36297 (3)	0.00894 (14)
O14	0.52813 (6)	0.26682 (4)	0.31527 (3)	0.00934 (14)
O15	0.55082 (6)	0.32676 (4)	0.50763 (3)	0.00975 (14)
O16	0.72735 (6)	0.20519 (4)	0.46503 (3)	0.00874 (13)
N1	0.27296 (7)	0.30200 (5)	0.47984 (3)	0.00809 (16)
N2	0.66198 (7)	0.09450 (5)	0.36198 (3)	0.00745 (16)
C1	0.21631 (9)	0.08870 (6)	0.29520 (4)	0.00824 (18)
C2	0.01007 (9)	−0.02697 (6)	0.26775 (4)	0.00873 (18)
C3	0.12294 (8)	−0.07933 (6)	0.17415 (4)	0.00853 (18)
C4	0.30829 (9)	0.03662 (6)	0.20000 (4)	0.00903 (19)
C5	0.25044 (9)	−0.09128 (6)	0.27869 (4)	0.00828 (18)
C6	−0.15481 (9)	0.14179 (6)	0.16988 (4)	0.00855 (18)
C7	0.01882 (8)	0.10387 (6)	0.09905 (4)	0.00806 (18)
C8	0.18844 (9)	0.22127 (6)	0.16009 (4)	0.00889 (18)
C9	0.02393 (9)	0.23371 (6)	0.23784 (4)	0.01089 (19)
C10	−0.03869 (9)	0.28246 (7)	0.12524 (4)	0.00986 (19)
C11	0.20826 (9)	0.23290 (6)	0.51157 (4)	0.00913 (18)
C12	0.17316 (9)	0.14355 (6)	0.47988 (4)	0.00867 (18)
C13	0.25209 (9)	0.00558 (6)	0.44644 (4)	0.00827 (19)
C14	0.37230 (9)	−0.04767 (6)	0.43914 (4)	0.00812 (18)
C15	0.54807 (9)	−0.04996 (6)	0.38672 (4)	0.00795 (18)
C16	0.60993 (9)	0.00373 (6)	0.34259 (4)	0.00836 (19)
C17	0.17936 (9)	0.34653 (6)	0.43709 (4)	0.00975 (19)
C18	0.24060 (9)	0.40164 (6)	0.39331 (4)	0.00977 (19)
C19	0.37487 (9)	0.38871 (6)	0.32178 (4)	0.01101 (19)
C20	0.42824 (9)	0.31888 (6)	0.28399 (4)	0.0111 (2)
C21	0.57232 (9)	0.19480 (6)	0.28140 (4)	0.00972 (19)
C22	0.69045 (9)	0.14951 (6)	0.31301 (4)	0.00904 (18)
C23	0.33590 (9)	0.37146 (6)	0.51925 (4)	0.01052 (19)
C24	0.46540 (9)	0.34037 (7)	0.54890 (4)	0.01066 (19)
C25	0.68003 (9)	0.31749 (6)	0.53317 (4)	0.00838 (18)
C26	0.76434 (9)	0.29310 (6)	0.48870 (4)	0.00939 (19)
C27	0.82373 (9)	0.16975 (6)	0.43398 (4)	0.00909 (19)
C28	0.77752 (8)	0.08205 (6)	0.40287 (4)	0.00833 (18)
H	0.0497 (14)	0.0753 (10)	0.1993 (6)	0.034324
H1A	0.1196 (13)	0.2615 (9)	0.5254 (6)	0.025685
H1B	0.2728 (13)	0.2170 (9)	0.5496 (6)	0.023415
H1C	0.1183 (13)	0.1562 (9)	0.4377 (6)	0.023746
H1D	0.1086 (12)	0.1018 (9)	0.5034 (6)	0.025185
H1E	0.1944 (13)	0.0152 (9)	0.4053 (6)	0.022553
H1F	0.1941 (13)	−0.0368 (9)	0.4722 (5)	0.023329
H1G	0.3442 (13)	−0.1154 (9)	0.4213 (6)	0.025162
H1H	0.4297 (12)	−0.0583 (9)	0.4803 (5)	0.023985
H1I	0.5122 (13)	−0.1160 (9)	0.3671 (6)	0.022542
H1J	0.6141 (12)	−0.0684 (9)	0.4239 (5)	0.022049
H1K	0.5380 (13)	0.0156 (9)	0.3063 (5)	0.022322
H1L	0.6860 (13)	−0.0395 (9)	0.3282 (5)	0.023425
H1M	0.1243 (13)	0.2931 (9)	0.4142 (6)	0.024263
H1N	0.1145 (13)	0.3931 (10)	0.4565 (6)	0.026345
H1O	0.1638 (13)	0.4349 (9)	0.3627 (6)	0.027864
H1P	0.3030 (13)	0.4574 (9)	0.4131 (6)	0.026242
H1Q	0.4496 (13)	0.4332 (9)	0.3434 (6)	0.027151
H1R	0.3054 (13)	0.4325 (10)	0.2958 (6)	0.029811
H2A	0.3495 (13)	0.2736 (10)	0.2657 (6)	0.026354
H2B	0.4669 (14)	0.3543 (10)	0.2492 (5)	0.028695
H2C	0.5966 (13)	0.2251 (10)	0.2418 (5)	0.025839
H2D	0.4946 (13)	0.1445 (9)	0.2687 (6)	0.024538
H2E	0.7388 (13)	0.1061 (10)	0.2835 (5)	0.026094
H2F	0.7567 (13)	0.2054 (9)	0.3272 (6)	0.024524
H2G	0.3542 (13)	0.4337 (9)	0.4959 (6)	0.025658
H2H	0.2741 (13)	0.3929 (10)	0.5515 (6)	0.027172
H2I	0.4578 (13)	0.2743 (10)	0.5748 (6)	0.026853
H2J	0.5067 (13)	0.3933 (10)	0.5788 (5)	0.028513
H2K	0.7143 (12)	0.3804 (9)	0.5540 (5)	0.023695
H2L	0.6880 (13)	0.2633 (9)	0.5666 (6)	0.023163
H2M	0.7568 (14)	0.3471 (9)	0.4544 (6)	0.025306
H2N	0.8624 (12)	0.2910 (9)	0.5085 (6)	0.025415
H2O	0.8501 (13)	0.2217 (9)	0.4056 (6)	0.025867
H2P	0.9113 (13)	0.1520 (10)	0.4650 (6)	0.028016
H2Q	0.8586 (12)	0.0543 (10)	0.3825 (6)	0.025573
H2R	0.7534 (12)	0.0319 (9)	0.4334 (5)	0.022425

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cr1	0.00570 (9)	0.00479 (9)	0.00556 (9)	0.00015 (5)	0.00041 (6)	−0.00010 (5)
Cr2	0.00674 (9)	0.00543 (9)	0.00521 (9)	0.00086 (5)	−0.00006 (6)	0.00018 (5)
K1	0.00614 (11)	0.00681 (10)	0.00689 (11)	0.00025 (7)	0.00031 (8)	−0.00014 (7)
O1	0.0157 (4)	0.0090 (3)	0.0102 (3)	−0.0003 (3)	−0.0026 (3)	−0.0023 (3)
O2	0.0114 (4)	0.0162 (3)	0.0171 (3)	0.0000 (3)	0.0069 (3)	0.0010 (3)
O3	0.0151 (3)	0.0127 (3)	0.0109 (3)	−0.0024 (3)	0.0017 (3)	−0.0050 (3)
O4	0.0109 (3)	0.0143 (3)	0.0170 (3)	−0.0007 (3)	0.0063 (3)	0.0002 (3)
O5	0.0139 (3)	0.0099 (3)	0.0141 (3)	0.0032 (3)	−0.0009 (3)	0.0022 (3)
O6	0.0097 (4)	0.0151 (3)	0.0133 (3)	−0.0011 (3)	0.0033 (3)	0.0011 (3)
O7	0.0164 (4)	0.0126 (3)	0.0094 (3)	−0.0018 (3)	0.0027 (3)	−0.0036 (3)
O8	0.0110 (4)	0.0158 (3)	0.0130 (3)	−0.0047 (3)	0.0010 (3)	0.0013 (3)
O9	0.0258 (4)	0.0176 (4)	0.0089 (4)	0.0097 (3)	−0.0014 (3)	−0.0050 (3)
O10	0.0185 (4)	0.0091 (3)	0.0156 (3)	0.0028 (3)	−0.0024 (3)	0.0044 (3)
O11	0.0063 (3)	0.0077 (3)	0.0100 (3)	0.0001 (2)	0.0004 (2)	−0.0005 (2)
O12	0.0095 (3)	0.0060 (3)	0.0098 (3)	0.0005 (2)	0.0029 (3)	0.0011 (2)
O13	0.0096 (3)	0.0070 (3)	0.0103 (3)	0.0013 (2)	0.0015 (3)	0.0009 (2)
O14	0.0105 (3)	0.0095 (3)	0.0079 (3)	0.0014 (2)	0.0006 (2)	0.0005 (2)
O15	0.0084 (3)	0.0121 (3)	0.0086 (3)	0.0009 (2)	0.0005 (3)	−0.0019 (2)
O16	0.0059 (3)	0.0094 (3)	0.0108 (3)	−0.0012 (2)	0.0006 (2)	−0.0021 (2)
N1	0.0066 (4)	0.0080 (4)	0.0097 (4)	0.0012 (3)	0.0010 (3)	−0.0007 (3)
N2	0.0073 (4)	0.0072 (3)	0.0080 (4)	0.0000 (3)	0.0017 (3)	0.0001 (3)
C1	0.0085 (4)	0.0067 (4)	0.0093 (4)	0.0002 (3)	0.0000 (3)	−0.0003 (4)
C2	0.0068 (5)	0.0096 (4)	0.0100 (4)	0.0005 (4)	0.0019 (4)	0.0005 (3)
C3	0.0080 (4)	0.0078 (4)	0.0097 (5)	−0.0004 (3)	0.0007 (3)	−0.0019 (4)
C4	0.0077 (5)	0.0087 (4)	0.0109 (4)	−0.0008 (3)	0.0019 (4)	−0.0004 (3)
C5	0.0089 (4)	0.0072 (4)	0.0085 (4)	0.0014 (3)	0.0002 (3)	0.0006 (3)
C6	0.0087 (5)	0.0092 (4)	0.0078 (4)	0.0004 (3)	0.0012 (3)	0.0005 (3)
C7	0.0092 (4)	0.0074 (4)	0.0074 (4)	−0.0002 (3)	0.0002 (3)	−0.0004 (4)
C8	0.0091 (5)	0.0093 (4)	0.0080 (4)	−0.0015 (4)	−0.0001 (3)	−0.0003 (3)
C9	0.0142 (5)	0.0102 (4)	0.0076 (5)	0.0041 (4)	−0.0009 (4)	−0.0009 (4)
C10	0.0111 (4)	0.0074 (4)	0.0107 (4)	0.0013 (3)	0.0000 (4)	0.0005 (4)
C11	0.0101 (5)	0.0096 (4)	0.0079 (4)	0.0024 (4)	0.0020 (3)	0.0000 (3)
C12	0.0065 (4)	0.0094 (4)	0.0100 (4)	0.0003 (3)	0.0006 (3)	0.0009 (4)
C13	0.0081 (5)	0.0082 (4)	0.0085 (4)	−0.0023 (3)	0.0011 (4)	−0.0006 (3)
C14	0.0094 (4)	0.0065 (4)	0.0085 (4)	−0.0007 (3)	0.0012 (4)	0.0007 (3)
C15	0.0080 (4)	0.0072 (4)	0.0086 (4)	0.0006 (3)	0.0008 (4)	0.0006 (3)
C16	0.0097 (5)	0.0087 (4)	0.0067 (4)	−0.0006 (3)	0.0014 (4)	−0.0012 (3)
C17	0.0086 (5)	0.0091 (4)	0.0117 (4)	0.0018 (4)	0.0022 (4)	0.0012 (4)
C18	0.0101 (5)	0.0078 (4)	0.0116 (4)	0.0019 (3)	0.0022 (4)	0.0019 (4)
C19	0.0117 (5)	0.0082 (4)	0.0135 (5)	0.0024 (4)	0.0029 (4)	0.0029 (4)
C20	0.0128 (5)	0.0121 (5)	0.0086 (4)	0.0033 (4)	0.0016 (4)	0.0034 (4)
C21	0.0120 (5)	0.0087 (4)	0.0082 (4)	0.0024 (4)	0.0003 (4)	0.0011 (3)
C22	0.0089 (5)	0.0094 (4)	0.0094 (4)	0.0006 (4)	0.0033 (3)	0.0014 (4)
C23	0.0089 (5)	0.0109 (4)	0.0115 (4)	0.0016 (4)	0.0003 (4)	−0.0037 (4)
C24	0.0078 (5)	0.0145 (5)	0.0094 (4)	0.0006 (4)	−0.0002 (4)	−0.0028 (4)
C25	0.0069 (4)	0.0091 (4)	0.0087 (4)	−0.0005 (3)	−0.0009 (4)	−0.0024 (3)
C26	0.0078 (5)	0.0095 (4)	0.0107 (4)	−0.0016 (3)	0.0005 (4)	−0.0020 (4)
C27	0.0066 (4)	0.0107 (4)	0.0100 (4)	−0.0018 (3)	0.0010 (4)	−0.0024 (4)
C28	0.0065 (4)	0.0087 (4)	0.0097 (4)	0.0000 (3)	0.0008 (3)	−0.0014 (4)
H	0.028000	0.027000	0.046000	0.004000	−0.003000	0.018000
H1A	0.024000	0.024000	0.032000	0.006000	0.015000	−0.000000
H1B	0.029000	0.024000	0.016000	0.001000	−0.002000	0.003000
H1C	0.022000	0.026000	0.021000	0.004000	−0.006000	0.001000
H1D	0.021000	0.023000	0.034000	−0.003000	0.013000	0.004000
H1E	0.023000	0.027000	0.016000	0.000000	−0.004000	−0.001000
H1F	0.026000	0.022000	0.024000	−0.009000	0.011000	−0.000000
H1G	0.034000	0.012000	0.031000	−0.006000	0.010000	−0.005000
H1H	0.026000	0.028000	0.017000	0.004000	−0.001000	0.006000
H1I	0.028000	0.012000	0.028000	−0.003000	0.005000	−0.005000
H1J	0.020000	0.026000	0.019000	0.004000	−0.002000	0.005000
H1K	0.025000	0.023000	0.017000	−0.002000	−0.005000	0.001000
H1L	0.024000	0.020000	0.028000	0.004000	0.010000	−0.006000
H1M	0.021000	0.024000	0.026000	−0.006000	−0.004000	0.004000
H1N	0.025000	0.028000	0.028000	0.013000	0.011000	0.005000
H1O	0.025000	0.030000	0.029000	0.013000	0.005000	0.012000
H1P	0.034000	0.016000	0.030000	−0.006000	0.009000	−0.005000
H1Q	0.028000	0.020000	0.035000	−0.009000	0.010000	−0.004000
H1R	0.033000	0.030000	0.027000	0.016000	0.006000	0.013000
H2A	0.022000	0.029000	0.026000	−0.001000	−0.005000	−0.006000
H2B	0.036000	0.032000	0.020000	0.009000	0.011000	0.012000
H2C	0.036000	0.028000	0.015000	0.006000	0.009000	0.006000
H2D	0.024000	0.020000	0.028000	−0.004000	−0.003000	−0.004000
H2E	0.032000	0.027000	0.022000	0.009000	0.014000	−0.000000
H2F	0.022000	0.022000	0.029000	−0.007000	0.001000	0.004000
H2G	0.028000	0.016000	0.032000	−0.002000	0.000000	0.003000
H2H	0.023000	0.032000	0.028000	0.004000	0.009000	−0.012000
H2I	0.026000	0.029000	0.026000	0.003000	0.005000	0.010000
H2J	0.026000	0.036000	0.023000	−0.001000	0.001000	−0.015000
H2K	0.025000	0.019000	0.026000	−0.003000	−0.001000	−0.010000
H2L	0.027000	0.023000	0.019000	0.003000	0.001000	0.007000
H2M	0.036000	0.017000	0.024000	−0.003000	0.008000	0.004000
H2N	0.014000	0.030000	0.031000	−0.002000	−0.002000	−0.010000
H2O	0.032000	0.022000	0.026000	−0.008000	0.013000	−0.001000
H2P	0.014000	0.035000	0.033000	0.004000	−0.005000	−0.011000
H2Q	0.018000	0.031000	0.028000	0.007000	0.004000	−0.010000
H2R	0.027000	0.019000	0.020000	−0.001000	−0.002000	0.004000

Geometric parameters (Å, º)

Cr1—C1	1.9053 (9)	N2—C22	1.4741 (11)
Cr1—C2	1.9057 (9)	N2—C28	1.4656 (11)
Cr1—C3	1.9018 (9)	C11—C12	1.5155 (12)
Cr1—C4	1.9004 (9)	C11—H1A	1.104 (13)
Cr1—C5	1.8527 (9)	C11—H1B	1.086 (13)
Cr1—H	1.747 (13)	C12—H1C	1.109 (13)
Cr2—C6	1.9040 (9)	C12—H1D	1.108 (13)
Cr2—C7	1.9014 (9)	C13—C14	1.5018 (13)
Cr2—C8	1.9015 (9)	C13—H1E	1.095 (13)
Cr2—C9	1.9114 (10)	C13—H1F	1.102 (12)
Cr2—C10	1.8480 (10)	C14—H1G	1.090 (13)
Cr2—H	1.695 (14)	C14—H1H	1.096 (12)
K1—O1	2.9711 (7)	C15—C16	1.5168 (12)
K1—O11	2.8645 (6)	C15—H1I	1.105 (13)
K1—O12	2.8636 (6)	C15—H1J	1.087 (12)
K1—O13	2.8029 (6)	C16—H1K	1.087 (13)
K1—O14	2.8000 (6)	C16—H1L	1.100 (12)
K1—O15	2.8796 (6)	C17—C18	1.5180 (12)
K1—O16	2.8432 (6)	C17—H1M	1.070 (13)
K1—N1	3.0162 (8)	C17—H1N	1.098 (13)
K1—N2	3.0121 (8)	C18—H1O	1.123 (13)
O1—C1	1.1412 (11)	C18—H1P	1.103 (13)
O2—C2	1.1413 (12)	C19—C20	1.5057 (13)
O3—C3	1.1432 (12)	C19—H1Q	1.089 (13)
O4—C4	1.1438 (12)	C19—H1R	1.094 (13)
O5—C5	1.1527 (12)	C20—H2A	1.097 (13)
O6—C6	1.1412 (12)	C20—H2B	1.095 (13)
O7—C7	1.1446 (11)	C21—C22	1.5122 (13)
O8—C8	1.1431 (12)	C21—H2C	1.101 (13)
O9—C9	1.1400 (12)	C21—H2D	1.103 (13)
O10—C10	1.1552 (12)	C22—H2E	1.110 (13)
O11—C12	1.4162 (11)	C22—H2F	1.089 (13)
O11—C13	1.4253 (10)	C23—C24	1.5147 (13)
O12—C14	1.4180 (10)	C23—H2G	1.086 (13)
O12—C15	1.4206 (11)	C23—H2H	1.110 (13)
O13—C18	1.4159 (11)	C24—H2I	1.145 (14)
O13—C19	1.4205 (11)	C24—H2J	1.096 (13)
O14—C20	1.4196 (11)	C25—C26	1.5053 (12)
O14—C21	1.4284 (11)	C25—H2K	1.074 (13)
O15—C24	1.4248 (11)	C25—H2L	1.113 (13)
O15—C25	1.4169 (11)	C26—H2M	1.124 (13)
O16—C26	1.4212 (11)	C26—H2N	1.075 (12)
O16—C27	1.4199 (11)	C27—C28	1.5145 (12)
N1—C11	1.4678 (11)	C27—H2O	1.068 (13)
N1—C17	1.4697 (11)	C27—H2P	1.132 (13)
N1—C23	1.4715 (11)	C28—H2Q	1.104 (13)
N2—C16	1.4694 (11)	C28—H2R	1.079 (13)
C2—Cr1—C1	91.92 (4)	H1A—C11—N1	111.2 (7)
C3—Cr1—C1	174.95 (4)	H1A—C11—C12	107.9 (7)
C3—Cr1—C2	93.00 (4)	H1B—C11—N1	107.3 (7)
C4—Cr1—C1	89.75 (4)	H1B—C11—C12	108.9 (7)
C4—Cr1—C2	175.16 (4)	H1B—C11—H1A	106.5 (10)
C4—Cr1—C3	85.26 (4)	C11—C12—O11	110.44 (7)
C5—Cr1—C1	89.90 (4)	H1C—C12—O11	108.9 (7)
C5—Cr1—C2	90.14 (4)	H1C—C12—C11	112.3 (7)
C5—Cr1—C3	91.22 (4)	H1D—C12—O11	110.0 (7)
C5—Cr1—C4	94.40 (4)	H1D—C12—C11	109.4 (7)
H—Cr1—C1	95.5 (5)	H1D—C12—H1C	105.7 (10)
H—Cr1—C2	77.1 (5)	C14—C13—O11	109.72 (7)
H—Cr1—C3	84.5 (5)	H1E—C13—O11	111.5 (7)
H—Cr1—C4	98.3 (5)	H1E—C13—C14	109.6 (7)
H—Cr1—C5	166.2 (5)	H1F—C13—O11	111.0 (7)
C7—Cr2—C6	89.95 (4)	H1F—C13—C14	108.0 (7)
C8—Cr2—C6	176.26 (4)	H1F—C13—H1E	107.0 (10)
C8—Cr2—C7	92.00 (4)	C13—C14—O12	108.81 (7)
C9—Cr2—C6	88.74 (4)	H1G—C14—O12	110.7 (7)
C9—Cr2—C7	171.05 (4)	H1G—C14—C13	108.3 (7)
C9—Cr2—C8	89.83 (4)	H1H—C14—O12	110.7 (7)
C10—Cr2—C6	90.10 (4)	H1H—C14—C13	109.8 (7)
C10—Cr2—C7	93.65 (4)	H1H—C14—H1G	108.4 (10)
C10—Cr2—C8	86.60 (4)	C16—C15—O12	108.79 (7)
C10—Cr2—C9	95.20 (4)	H1I—C15—O12	109.9 (7)
H—Cr2—C6	82.1 (5)	H1I—C15—C16	107.2 (7)
H—Cr2—C7	83.9 (5)	H1J—C15—O12	110.2 (7)
H—Cr2—C8	101.3 (5)	H1J—C15—C16	114.2 (7)
H—Cr2—C9	87.1 (5)	H1J—C15—H1I	106.5 (10)
H—Cr2—C10	171.8 (5)	C15—C16—N2	114.15 (7)
O11—K1—O1	71.900 (18)	H1K—C16—N2	107.6 (7)
O12—K1—O1	65.090 (18)	H1K—C16—C15	108.7 (7)
O12—K1—O11	58.925 (18)	H1L—C16—N2	110.5 (7)
O13—K1—O1	64.161 (18)	H1L—C16—C15	108.5 (7)
O13—K1—O11	104.402 (18)	H1L—C16—H1K	107.1 (10)
O13—K1—O12	129.251 (19)	C18—C17—N1	113.90 (8)
O14—K1—O1	74.468 (19)	H1M—C17—N1	108.0 (7)
O14—K1—O11	146.321 (19)	H1M—C17—C18	105.7 (7)
O14—K1—O12	104.644 (19)	H1N—C17—N1	111.6 (7)
O14—K1—O13	61.228 (18)	H1N—C17—C18	107.9 (7)
O15—K1—O1	147.809 (19)	H1N—C17—H1M	109.5 (10)
O15—K1—O11	99.534 (19)	C17—C18—O13	109.23 (7)
O15—K1—O12	137.659 (19)	H1O—C18—O13	108.4 (7)
O15—K1—O13	89.413 (19)	H1O—C18—C17	110.0 (7)
O15—K1—O14	109.946 (19)	H1P—C18—O13	110.0 (7)
O16—K1—O1	152.205 (19)	H1P—C18—C17	111.3 (7)
O16—K1—O11	119.286 (19)	H1P—C18—H1O	107.7 (10)
O16—K1—O12	97.635 (19)	C20—C19—O13	109.05 (7)
O16—K1—O13	128.511 (19)	H1Q—C19—O13	108.6 (7)
O16—K1—O14	90.416 (19)	H1Q—C19—C20	112.3 (7)
O16—K1—O15	59.192 (17)	H1R—C19—O13	110.2 (7)
N1—K1—O1	90.37 (2)	H1R—C19—C20	108.4 (7)
N1—K1—O11	62.025 (19)	H1R—C19—H1Q	108.4 (11)
N1—K1—O12	120.43 (2)	C19—C20—O14	110.00 (7)
N1—K1—O13	60.311 (19)	H2A—C20—O14	111.1 (7)
N1—K1—O14	120.37 (2)	H2A—C20—C19	108.6 (7)
N1—K1—O15	59.314 (19)	H2B—C20—O14	109.1 (7)
N1—K1—O16	117.42 (2)	H2B—C20—C19	110.1 (7)
N2—K1—O1	92.002 (19)	H2B—C20—H2A	107.8 (10)
N2—K1—O11	117.24 (2)	C22—C21—O14	109.48 (7)
N2—K1—O12	59.317 (19)	H2C—C21—O14	109.0 (7)
N2—K1—O13	122.311 (19)	H2C—C21—C22	109.8 (7)
N2—K1—O14	61.951 (19)	H2D—C21—O14	110.7 (7)
N2—K1—O15	118.66 (2)	H2D—C21—C22	112.3 (7)
N2—K1—O16	60.207 (19)	H2D—C21—H2C	105.5 (10)
N2—K1—N1	177.10 (2)	C21—C22—N2	113.21 (7)
C1—O1—K1	148.72 (6)	H2E—C22—N2	110.7 (7)
C12—O11—K1	111.63 (5)	H2E—C22—C21	109.6 (7)
C13—O11—K1	113.88 (5)	H2F—C22—N2	109.6 (7)
C13—O11—C12	110.38 (7)	H2F—C22—C21	106.5 (7)
C14—O12—K1	117.57 (5)	H2F—C22—H2E	107.0 (10)
C15—O12—K1	121.07 (5)	C24—C23—N1	113.51 (7)
C15—O12—C14	111.86 (7)	H2G—C23—N1	109.1 (7)
C18—O13—K1	121.06 (5)	H2G—C23—C24	106.2 (7)
C19—O13—K1	113.61 (5)	H2H—C23—N1	112.4 (7)
C19—O13—C18	112.01 (7)	H2H—C23—C24	108.8 (7)
C20—O14—K1	113.73 (5)	H2H—C23—H2G	106.4 (10)
C21—O14—K1	111.98 (5)	C23—C24—O15	108.61 (7)
C21—O14—C20	110.83 (7)	H2I—C24—O15	110.6 (7)
C24—O15—K1	115.78 (5)	H2I—C24—C23	112.3 (7)
C25—O15—K1	117.03 (5)	H2J—C24—O15	108.5 (7)
C25—O15—C24	111.25 (7)	H2J—C24—C23	110.8 (7)
C26—O16—K1	112.66 (5)	H2J—C24—H2I	105.9 (10)
C27—O16—K1	119.99 (5)	C26—C25—O15	109.27 (7)
C27—O16—C26	110.67 (7)	H2K—C25—O15	111.3 (7)
C11—N1—K1	107.24 (5)	H2K—C25—C26	109.5 (7)
C17—N1—K1	107.35 (5)	H2L—C25—O15	110.8 (7)
C17—N1—C11	110.19 (7)	H2L—C25—C26	110.2 (7)
C23—N1—K1	112.14 (5)	H2L—C25—H2K	105.7 (10)
C23—N1—C11	109.26 (7)	C25—C26—O16	109.55 (7)
C23—N1—C17	110.60 (7)	H2M—C26—O16	109.7 (7)
C16—N2—K1	109.78 (5)	H2M—C26—C25	111.0 (7)
C22—N2—K1	107.57 (5)	H2N—C26—O16	110.3 (7)
C22—N2—C16	109.46 (7)	H2N—C26—C25	107.9 (7)
C28—N2—K1	108.73 (5)	H2N—C26—H2M	108.4 (10)
C28—N2—C16	110.01 (7)	C28—C27—O16	110.68 (7)
C28—N2—C22	111.24 (7)	H2O—C27—O16	109.6 (7)
O1—C1—Cr1	177.15 (8)	H2O—C27—C28	111.5 (7)
O2—C2—Cr1	178.69 (8)	H2P—C27—O16	107.9 (7)
O3—C3—Cr1	175.92 (8)	H2P—C27—C28	108.3 (7)
O4—C4—Cr1	177.83 (8)	H2P—C27—H2O	108.7 (10)
O5—C5—Cr1	177.59 (8)	C27—C28—N2	114.19 (7)
O6—C6—Cr2	178.85 (8)	H2Q—C28—N2	111.4 (7)
O7—C7—Cr2	178.63 (8)	H2Q—C28—C27	107.7 (7)
O8—C8—Cr2	174.82 (8)	H2R—C28—N2	106.8 (7)
O9—C9—Cr2	178.65 (8)	H2R—C28—C27	108.4 (7)
O10—C10—Cr2	177.95 (8)	H2R—C28—H2Q	108.3 (10)
C12—C11—N1	114.67 (7)	Cr2—H—Cr1	147.6 (9)
K1—O11—C12—C11	−55.91 (5)	K1—N1—C23—C24	−37.42 (6)
K1—O11—C13—C14	53.09 (5)	K1—N2—C16—C15	−48.49 (5)
K1—O12—C14—C13	42.27 (5)	K1—N2—C22—C21	−39.26 (5)
K1—O12—C15—C16	−40.91 (6)	K1—N2—C28—C27	−48.39 (5)
K1—O13—C18—C17	−40.68 (6)	O11—C12—C11—N1	69.81 (8)
K1—O13—C19—C20	49.22 (5)	O11—C13—C14—O12	−63.30 (7)
K1—O14—C20—C19	47.70 (5)	O12—C15—C16—N2	60.60 (8)
K1—O14—C21—C22	−59.72 (5)	O13—C18—C17—N1	62.32 (8)
K1—O15—C24—C23	−55.98 (5)	O13—C19—C20—O14	−65.82 (8)
K1—O15—C25—C26	37.72 (5)	O14—C21—C22—N2	69.62 (8)
K1—O16—C26—C25	57.41 (5)	O15—C24—C23—N1	63.01 (8)
K1—O16—C27—C28	−39.13 (5)	O15—C25—C26—O16	−63.68 (7)
K1—N1—C11—C12	−41.32 (5)	O16—C27—C28—N2	60.45 (8)
K1—N1—C17—C18	−49.74 (5)

(KCPTCR_standard_HAR_SHADE3_1)

Crystal data

C28H37Cr2KN2O16	F(000) = 1660.306
Mr = 800.70	Dx = 1.489 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71069 Å
a = 10.458 Å	Cell parameters from 1024 reflections
b = 14.417 Å	θ = 47.5–1.5°
c = 23.882 Å	µ = 0.80 mm^−1
β = 97.26°	T = 28 K
V = 3571.89 Å^3	Ellipsoidal, yellow
Z = 4	0.3 × 0.25 × 0.2 mm

Data collection

SMART CCD diffractometer	5667 reflections with I ≥ 2u(I)
ω scan	Rint = 0.0000
Absorption correction: empirical (using intensity measurements)	θmax = 25.0°, θmin = 2.4°
Tmin = 0.890, Tmax = 0.903	h = −19→20
27917 measured reflections	k = 0→30
5993 independent reflections	l = 0→50

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.016	Only H-atom coordinates refined
wR(F^2) = 0.056	w = 1/[σ^2(Fo^2) + (0.1P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 0.51	(Δ/σ)max = 0.001
5993 reflections	Δρmax = 0.25 e Å^−3
553 parameters	Δρmin = −0.59 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Cr1	0.163857 (14)	0.002353 (9)	0.236366 (6)	0.00535 (6)
Cr2	0.018773 (14)	0.177459 (10)	0.165113 (6)	0.00584 (6)
K1	0.463767 (17)	0.199316 (13)	0.418020 (8)	0.00663 (6)
O1	0.25195 (6)	0.13804 (4)	0.33118 (3)	0.01197 (15)
O2	−0.08335 (6)	−0.04365 (5)	0.28572 (3)	0.01439 (15)
O3	0.10477 (6)	−0.12655 (5)	0.13550 (3)	0.01288 (15)
O4	0.39544 (6)	0.05442 (5)	0.17753 (3)	0.01369 (15)
O5	0.30033 (6)	−0.15026 (5)	0.30577 (3)	0.01283 (15)
O6	−0.25955 (6)	0.12174 (5)	0.17226 (3)	0.01253 (14)
O7	0.01689 (6)	0.05853 (5)	0.05959 (3)	0.01265 (15)
O8	0.28627 (6)	0.25357 (5)	0.15522 (3)	0.01332 (15)
O9	0.02667 (7)	0.26561 (5)	0.28166 (3)	0.01768 (16)
O10	−0.07195 (7)	0.34760 (5)	0.09921 (3)	0.01480 (15)
O11	0.28561 (6)	0.09220 (4)	0.47310 (3)	0.00803 (13)
O12	0.44349 (6)	0.00265 (4)	0.40251 (3)	0.00826 (14)
O13	0.31320 (6)	0.34098 (4)	0.36297 (3)	0.00891 (14)
O14	0.52813 (6)	0.26682 (4)	0.31526 (3)	0.00929 (14)
O15	0.55082 (6)	0.32675 (4)	0.50763 (3)	0.00971 (14)
O16	0.72734 (6)	0.20519 (4)	0.46503 (3)	0.00873 (14)
N1	0.27295 (7)	0.30200 (5)	0.47983 (3)	0.00807 (16)
N2	0.66199 (7)	0.09449 (5)	0.36198 (3)	0.00740 (16)
C1	0.21632 (9)	0.08869 (6)	0.29519 (4)	0.00826 (18)
C2	0.01007 (9)	−0.02697 (6)	0.26775 (4)	0.00875 (18)
C3	0.12294 (8)	−0.07934 (6)	0.17414 (4)	0.00853 (18)
C4	0.30831 (9)	0.03662 (6)	0.20000 (4)	0.00901 (19)
C5	0.25044 (9)	−0.09128 (6)	0.27870 (4)	0.00825 (18)
C6	−0.15484 (9)	0.14177 (6)	0.16988 (4)	0.00850 (19)
C7	0.01884 (9)	0.10387 (6)	0.09905 (4)	0.00802 (18)
C8	0.18841 (9)	0.22128 (6)	0.16008 (4)	0.00885 (19)
C9	0.02390 (9)	0.23371 (6)	0.23781 (4)	0.01087 (19)
C10	−0.03871 (9)	0.28248 (7)	0.12523 (4)	0.00980 (19)
C11	0.20826 (9)	0.23288 (6)	0.51157 (4)	0.00909 (18)
C12	0.17315 (9)	0.14353 (6)	0.47987 (4)	0.00860 (18)
C13	0.25210 (9)	0.00557 (6)	0.44644 (4)	0.00822 (19)
C14	0.37235 (9)	−0.04766 (6)	0.43914 (4)	0.00808 (18)
C15	0.54807 (9)	−0.04995 (6)	0.38673 (4)	0.00794 (18)
C16	0.60993 (9)	0.00372 (6)	0.34259 (4)	0.00835 (19)
C17	0.17935 (9)	0.34650 (6)	0.43709 (4)	0.00973 (19)
C18	0.24061 (9)	0.40164 (6)	0.39330 (4)	0.00972 (19)
C19	0.37489 (9)	0.38871 (6)	0.32179 (4)	0.01096 (19)
C20	0.42823 (9)	0.31886 (6)	0.28397 (4)	0.0111 (2)
C21	0.57231 (9)	0.19478 (6)	0.28140 (4)	0.00970 (19)
C22	0.69042 (9)	0.14951 (6)	0.31301 (4)	0.00901 (18)
C23	0.33591 (9)	0.37147 (6)	0.51924 (4)	0.01050 (19)
C24	0.46540 (9)	0.34038 (7)	0.54890 (4)	0.01063 (19)
C25	0.68002 (9)	0.31748 (6)	0.53316 (4)	0.00836 (19)
C26	0.76432 (9)	0.29307 (6)	0.48869 (4)	0.00937 (19)
C27	0.82371 (9)	0.16975 (6)	0.43399 (4)	0.00907 (19)
C28	0.77751 (8)	0.08204 (6)	0.40286 (4)	0.00832 (18)
H	0.0497 (13)	0.0751 (10)	0.1992 (6)	0.030761
H1A	0.1193 (13)	0.2615 (9)	0.5255 (6)	0.023889
H1B	0.2728 (12)	0.2169 (10)	0.5499 (6)	0.022725
H1C	0.1187 (12)	0.1563 (9)	0.4379 (5)	0.021236
H1D	0.1090 (12)	0.1021 (9)	0.5033 (5)	0.022704
H1E	0.1943 (13)	0.0149 (9)	0.4055 (6)	0.020886
H1F	0.1943 (12)	−0.0365 (9)	0.4722 (5)	0.022221
H1G	0.3438 (12)	−0.1150 (9)	0.4214 (5)	0.021051
H1H	0.4291 (12)	−0.0584 (9)	0.4802 (5)	0.021280
H1I	0.5124 (12)	−0.1159 (9)	0.3672 (6)	0.022380
H1J	0.6137 (12)	−0.0685 (9)	0.4237 (5)	0.021936
H1K	0.5383 (13)	0.0162 (9)	0.3065 (6)	0.021258
H1L	0.6859 (12)	−0.0393 (9)	0.3284 (5)	0.022910
H1M	0.1244 (13)	0.2929 (9)	0.4141 (5)	0.022307
H1N	0.1145 (12)	0.3930 (10)	0.4568 (5)	0.024103
H1O	0.1637 (13)	0.4349 (9)	0.3624 (6)	0.023539
H1P	0.3033 (12)	0.4574 (9)	0.4133 (5)	0.023299
H1Q	0.4504 (13)	0.4334 (9)	0.3434 (5)	0.022483
H1R	0.3052 (12)	0.4325 (9)	0.2957 (5)	0.022623
H2A	0.3498 (12)	0.2739 (9)	0.2659 (5)	0.020778
H2B	0.4672 (13)	0.3541 (9)	0.2492 (5)	0.022274
H2C	0.5967 (13)	0.2253 (9)	0.2416 (5)	0.022464
H2D	0.4948 (12)	0.1446 (9)	0.2686 (5)	0.020833
H2E	0.7386 (12)	0.1061 (9)	0.2837 (5)	0.022928
H2F	0.7568 (12)	0.2058 (9)	0.3271 (5)	0.022610
H2G	0.3546 (12)	0.4336 (9)	0.4961 (5)	0.023717
H2H	0.2738 (13)	0.3930 (10)	0.5515 (6)	0.024368
H2I	0.4577 (12)	0.2745 (10)	0.5750 (6)	0.022245
H2J	0.5071 (12)	0.3930 (9)	0.5790 (5)	0.023654
H2K	0.7145 (12)	0.3806 (9)	0.5543 (5)	0.022772
H2L	0.6884 (12)	0.2633 (9)	0.5666 (6)	0.022034
H2M	0.7571 (13)	0.3473 (9)	0.4545 (5)	0.022184
H2N	0.8626 (12)	0.2911 (9)	0.5087 (5)	0.022344
H2O	0.8506 (12)	0.2219 (9)	0.4057 (5)	0.022316
H2P	0.9109 (13)	0.1524 (9)	0.4652 (6)	0.022948
H2Q	0.8588 (12)	0.0544 (10)	0.3825 (5)	0.023668
H2R	0.7539 (12)	0.0324 (9)	0.4331 (5)	0.022260

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cr1	0.00568 (9)	0.00476 (9)	0.00553 (9)	0.00014 (5)	0.00040 (6)	−0.00011 (5)
Cr2	0.00673 (9)	0.00541 (9)	0.00517 (9)	0.00084 (5)	−0.00005 (6)	0.00017 (5)
K1	0.00610 (11)	0.00679 (10)	0.00686 (11)	0.00026 (7)	0.00029 (8)	−0.00013 (7)
O1	0.0157 (4)	0.0090 (3)	0.0101 (3)	−0.0003 (3)	−0.0026 (3)	−0.0023 (3)
O2	0.0113 (4)	0.0162 (4)	0.0171 (3)	0.0000 (3)	0.0070 (3)	0.0010 (3)
O3	0.0151 (3)	0.0127 (3)	0.0109 (3)	−0.0024 (3)	0.0017 (3)	−0.0050 (3)
O4	0.0109 (3)	0.0143 (3)	0.0170 (3)	−0.0007 (3)	0.0062 (3)	0.0001 (3)
O5	0.0138 (3)	0.0098 (3)	0.0142 (3)	0.0032 (3)	−0.0010 (3)	0.0021 (3)
O6	0.0097 (4)	0.0150 (3)	0.0133 (3)	−0.0011 (3)	0.0032 (3)	0.0011 (3)
O7	0.0164 (4)	0.0125 (3)	0.0094 (3)	−0.0017 (3)	0.0026 (3)	−0.0036 (3)
O8	0.0110 (4)	0.0157 (3)	0.0131 (3)	−0.0047 (3)	0.0010 (3)	0.0014 (3)
O9	0.0258 (4)	0.0175 (4)	0.0088 (4)	0.0096 (3)	−0.0014 (3)	−0.0050 (3)
O10	0.0183 (4)	0.0092 (3)	0.0157 (3)	0.0027 (3)	−0.0025 (3)	0.0043 (3)
O11	0.0062 (3)	0.0077 (3)	0.0100 (3)	0.0001 (2)	0.0004 (2)	−0.0004 (2)
O12	0.0094 (3)	0.0060 (3)	0.0098 (3)	0.0005 (2)	0.0029 (3)	0.0011 (2)
O13	0.0096 (3)	0.0069 (3)	0.0103 (3)	0.0013 (2)	0.0014 (3)	0.0009 (2)
O14	0.0105 (3)	0.0094 (3)	0.0078 (3)	0.0014 (2)	0.0006 (2)	0.0005 (2)
O15	0.0083 (3)	0.0121 (3)	0.0085 (3)	0.0009 (2)	0.0004 (3)	−0.0019 (2)
O16	0.0059 (3)	0.0093 (3)	0.0108 (3)	−0.0012 (2)	0.0005 (3)	−0.0021 (2)
N1	0.0066 (4)	0.0079 (4)	0.0097 (4)	0.0011 (3)	0.0011 (3)	−0.0008 (3)
N2	0.0073 (4)	0.0072 (4)	0.0079 (4)	−0.0001 (3)	0.0017 (3)	0.0001 (3)
C1	0.0085 (4)	0.0066 (4)	0.0094 (4)	0.0002 (3)	0.0000 (3)	−0.0003 (4)
C2	0.0069 (5)	0.0096 (4)	0.0101 (4)	0.0005 (4)	0.0019 (4)	0.0004 (3)
C3	0.0080 (4)	0.0078 (4)	0.0097 (5)	−0.0004 (3)	0.0007 (3)	−0.0019 (4)
C4	0.0077 (5)	0.0087 (4)	0.0109 (4)	−0.0008 (3)	0.0019 (4)	−0.0003 (3)
C5	0.0089 (4)	0.0072 (4)	0.0085 (4)	0.0014 (3)	0.0003 (3)	0.0006 (3)
C6	0.0087 (5)	0.0092 (4)	0.0077 (4)	0.0004 (3)	0.0011 (3)	0.0005 (3)
C7	0.0091 (4)	0.0074 (4)	0.0074 (5)	−0.0002 (3)	0.0001 (3)	−0.0003 (4)
C8	0.0091 (5)	0.0092 (4)	0.0079 (4)	−0.0016 (4)	−0.0001 (3)	−0.0004 (3)
C9	0.0141 (5)	0.0102 (4)	0.0077 (5)	0.0041 (4)	−0.0009 (4)	−0.0009 (4)
C10	0.0111 (4)	0.0074 (4)	0.0106 (4)	0.0013 (3)	0.0000 (4)	0.0005 (4)
C11	0.0099 (5)	0.0096 (4)	0.0080 (4)	0.0023 (4)	0.0020 (3)	0.0000 (3)
C12	0.0065 (4)	0.0093 (4)	0.0099 (4)	0.0002 (3)	0.0007 (3)	0.0009 (4)
C13	0.0081 (5)	0.0082 (4)	0.0084 (4)	−0.0023 (3)	0.0010 (4)	−0.0006 (3)
C14	0.0093 (4)	0.0064 (4)	0.0086 (4)	−0.0007 (3)	0.0012 (4)	0.0006 (3)
C15	0.0081 (4)	0.0071 (4)	0.0085 (4)	0.0006 (3)	0.0008 (4)	0.0006 (3)
C16	0.0097 (5)	0.0086 (4)	0.0068 (4)	−0.0005 (3)	0.0014 (4)	−0.0013 (3)
C17	0.0088 (5)	0.0091 (4)	0.0116 (4)	0.0019 (4)	0.0022 (4)	0.0012 (4)
C18	0.0100 (5)	0.0079 (4)	0.0114 (4)	0.0019 (3)	0.0021 (4)	0.0019 (4)
C19	0.0116 (5)	0.0082 (4)	0.0134 (5)	0.0025 (4)	0.0026 (4)	0.0029 (4)
C20	0.0128 (5)	0.0119 (5)	0.0088 (4)	0.0032 (4)	0.0019 (4)	0.0034 (4)
C21	0.0120 (5)	0.0086 (4)	0.0083 (4)	0.0024 (4)	0.0005 (4)	0.0012 (3)
C22	0.0089 (5)	0.0093 (4)	0.0094 (4)	0.0006 (4)	0.0032 (4)	0.0013 (4)
C23	0.0089 (5)	0.0110 (4)	0.0114 (5)	0.0017 (4)	0.0004 (4)	−0.0036 (4)
C24	0.0079 (5)	0.0143 (5)	0.0094 (4)	0.0005 (4)	−0.0002 (4)	−0.0029 (4)
C25	0.0070 (4)	0.0089 (4)	0.0087 (4)	−0.0005 (3)	−0.0008 (4)	−0.0024 (3)
C26	0.0076 (5)	0.0096 (4)	0.0107 (4)	−0.0015 (3)	0.0004 (4)	−0.0019 (4)
C27	0.0067 (4)	0.0108 (4)	0.0097 (4)	−0.0018 (3)	0.0011 (4)	−0.0023 (4)
C28	0.0066 (4)	0.0087 (4)	0.0096 (4)	−0.0001 (3)	0.0009 (3)	−0.0015 (4)
H	0.026950	0.024430	0.039490	0.003320	−0.001300	0.012070
H1A	0.018090	0.028260	0.026500	0.003850	0.007420	−0.004510
H1B	0.021280	0.028200	0.017220	−0.000560	−0.003310	0.001250
H1C	0.020130	0.026710	0.015700	0.004190	−0.002280	−0.000760
H1D	0.019670	0.026340	0.023350	−0.003230	0.007580	0.001310
H1E	0.021970	0.022410	0.016650	0.002480	−0.003900	0.000740
H1F	0.021940	0.022690	0.023100	−0.004970	0.007000	0.003170
H1G	0.024800	0.014990	0.023070	−0.002480	0.001880	−0.001150
H1H	0.019270	0.025930	0.017300	−0.000280	−0.002910	0.004600
H1I	0.024420	0.015220	0.027530	−0.001140	0.003400	−0.003790
H1J	0.019190	0.025220	0.020290	0.005240	−0.001820	0.002540
H1K	0.019890	0.022080	0.020200	0.000040	−0.003710	0.001260
H1L	0.019810	0.021530	0.028490	0.004860	0.007340	−0.004180
H1M	0.022560	0.020750	0.022160	−0.002320	−0.002820	−0.003110
H1N	0.023510	0.025820	0.023440	0.009400	0.004760	−0.004390
H1O	0.023760	0.022860	0.022740	0.008020	−0.001960	0.001360
H1P	0.024910	0.018350	0.026090	−0.002380	0.001090	−0.006680
H1Q	0.024760	0.020080	0.021850	−0.007290	−0.000010	−0.002850
H1R	0.024560	0.019300	0.022980	0.004810	−0.001000	0.003950
H2A	0.019310	0.016420	0.025450	−0.003430	−0.001670	−0.002180
H2B	0.026450	0.022100	0.018900	−0.001510	0.005310	0.005020
H2C	0.025730	0.025460	0.017180	0.000170	0.006520	0.003400
H2D	0.017150	0.018990	0.026170	−0.003840	0.002000	−0.004470
H2E	0.023210	0.025770	0.020970	0.004170	0.007330	−0.003740
H2F	0.020550	0.023140	0.023400	−0.007350	−0.000100	−0.000990
H2G	0.027120	0.019370	0.023680	−0.000850	−0.000610	0.001150
H2H	0.020660	0.031140	0.021840	0.003780	0.004770	−0.008290
H2I	0.022570	0.022140	0.022640	0.001760	0.005250	0.003380
H2J	0.022120	0.026260	0.021820	−0.001040	−0.000190	−0.009590
H2K	0.022210	0.021200	0.024270	−0.002930	0.000460	−0.007230
H2L	0.020600	0.024770	0.020640	0.000400	0.002250	0.005730
H2M	0.028640	0.019440	0.018360	−0.002360	0.002530	0.002290
H2N	0.014540	0.027080	0.024570	−0.000960	−0.000810	−0.003010
H2O	0.024090	0.022000	0.021910	−0.002100	0.007000	0.002010
H2P	0.014960	0.030120	0.022740	0.002450	−0.001610	−0.002570
H2Q	0.016710	0.029800	0.025110	0.004240	0.005040	−0.006160
H2R	0.022290	0.022140	0.021870	−0.001610	0.000920	0.004480

Geometric parameters (Å, º)

Cr1—C1	1.9051 (9)	N2—C22	1.4742 (11)
Cr1—C2	1.9057 (9)	N2—C28	1.4652 (11)
Cr1—C3	1.9020 (9)	C11—C12	1.5156 (12)
Cr1—C4	1.9006 (9)	C11—H1A	1.106 (13)
Cr1—C5	1.8528 (9)	C11—H1B	1.090 (13)
Cr1—H	1.744 (13)	C12—H1C	1.104 (12)
Cr2—C6	1.9043 (10)	C12—H1D	1.103 (13)
Cr2—C7	1.9012 (9)	C13—C14	1.5020 (13)
Cr2—C8	1.9012 (9)	C13—H1E	1.091 (13)
Cr2—C9	1.9109 (10)	C13—H1F	1.097 (12)
Cr2—C10	1.8483 (10)	C14—H1G	1.086 (13)
Cr2—H	1.697 (13)	C14—H1H	1.091 (12)
K1—O1	2.9711 (7)	C15—C16	1.5169 (12)
K1—O11	2.8646 (6)	C15—H1I	1.104 (13)
K1—O12	2.8638 (6)	C15—H1J	1.080 (12)
K1—O13	2.8029 (6)	C16—H1K	1.083 (13)
K1—O14	2.8001 (6)	C16—H1L	1.095 (12)
K1—O15	2.8795 (7)	C17—C18	1.5183 (12)
K1—O16	2.8431 (6)	C17—H1M	1.072 (13)
K1—N1	3.0162 (8)	C17—H1N	1.101 (13)
K1—N2	3.0123 (8)	C18—H1O	1.127 (13)
O1—C1	1.1413 (11)	C18—H1P	1.107 (13)
O2—C2	1.1413 (12)	C19—C20	1.5061 (13)
O3—C3	1.1432 (12)	C19—H1Q	1.096 (13)
O4—C4	1.1436 (12)	C19—H1R	1.097 (12)
O5—C5	1.1524 (12)	C20—H2A	1.090 (13)
O6—C6	1.1408 (12)	C20—H2B	1.094 (13)
O7—C7	1.1449 (11)	C21—C22	1.5120 (13)
O8—C8	1.1434 (12)	C21—H2C	1.105 (13)
O9—C9	1.1407 (12)	C21—H2D	1.101 (13)
O10—C10	1.1549 (12)	C22—H2E	1.106 (13)
O11—C12	1.4160 (11)	C22—H2F	1.093 (13)
O11—C13	1.4254 (11)	C23—C24	1.5146 (13)
O12—C14	1.4175 (11)	C23—H2G	1.084 (13)
O12—C15	1.4204 (11)	C23—H2H	1.113 (13)
O13—C18	1.4160 (11)	C24—H2I	1.144 (14)
O13—C19	1.4204 (11)	C24—H2J	1.097 (13)
O14—C20	1.4196 (11)	C25—C26	1.5053 (12)
O14—C21	1.4285 (11)	C25—H2K	1.081 (13)
O15—C24	1.4249 (11)	C25—H2L	1.114 (13)
O15—C25	1.4168 (11)	C26—H2M	1.126 (13)
O16—C26	1.4208 (11)	C26—H2N	1.077 (12)
O16—C27	1.4197 (11)	C27—C28	1.5146 (12)
N1—C11	1.4679 (11)	C27—H2O	1.073 (13)
N1—C17	1.4695 (12)	C27—H2P	1.130 (13)
N1—C23	1.4717 (12)	C28—H2Q	1.105 (13)
N2—C16	1.4696 (11)	C28—H2R	1.067 (13)
C2—Cr1—C1	91.93 (4)	H1A—C11—N1	111.2 (7)
C3—Cr1—C1	174.95 (4)	H1A—C11—C12	107.9 (7)
C3—Cr1—C2	92.99 (4)	H1B—C11—N1	107.5 (7)
C4—Cr1—C1	89.75 (4)	H1B—C11—C12	108.9 (7)
C4—Cr1—C2	175.16 (4)	H1B—C11—H1A	106.4 (10)
C4—Cr1—C3	85.25 (4)	C11—C12—O11	110.42 (7)
C5—Cr1—C1	89.90 (4)	H1C—C12—O11	108.9 (7)
C5—Cr1—C2	90.13 (4)	H1C—C12—C11	112.1 (7)
C5—Cr1—C3	91.23 (4)	H1D—C12—O11	110.0 (7)
C5—Cr1—C4	94.41 (4)	H1D—C12—C11	109.4 (7)
H—Cr1—C1	95.6 (5)	H1D—C12—H1C	105.9 (10)
H—Cr1—C2	77.1 (5)	C14—C13—O11	109.71 (7)
H—Cr1—C3	84.4 (5)	H1E—C13—O11	111.6 (7)
H—Cr1—C4	98.3 (5)	H1E—C13—C14	109.7 (7)
H—Cr1—C5	166.2 (5)	H1F—C13—O11	110.8 (7)
C7—Cr2—C6	89.96 (4)	H1F—C13—C14	108.1 (7)
C8—Cr2—C6	176.26 (4)	H1F—C13—H1E	106.7 (10)
C8—Cr2—C7	91.99 (4)	C13—C14—O12	108.82 (7)
C9—Cr2—C6	88.73 (4)	H1G—C14—O12	110.8 (7)
C9—Cr2—C7	171.06 (4)	H1G—C14—C13	108.0 (7)
C9—Cr2—C8	89.84 (4)	H1H—C14—O12	111.0 (7)
C10—Cr2—C6	90.10 (4)	H1H—C14—C13	109.7 (7)
C10—Cr2—C7	93.65 (4)	H1H—C14—H1G	108.4 (10)
C10—Cr2—C8	86.59 (4)	C16—C15—O12	108.80 (7)
C10—Cr2—C9	95.19 (4)	H1I—C15—O12	110.0 (7)
H—Cr2—C6	82.1 (5)	H1I—C15—C16	107.2 (7)
H—Cr2—C7	83.9 (5)	H1J—C15—O12	110.3 (7)
H—Cr2—C8	101.3 (5)	H1J—C15—C16	114.3 (7)
H—Cr2—C9	87.2 (5)	H1J—C15—H1I	106.2 (10)
H—Cr2—C10	171.8 (5)	C15—C16—N2	114.13 (7)
O11—K1—O1	71.905 (18)	H1K—C16—N2	107.1 (7)
O12—K1—O1	65.093 (18)	H1K—C16—C15	109.0 (7)
O12—K1—O11	58.923 (18)	H1L—C16—N2	110.3 (7)
O13—K1—O1	64.158 (18)	H1L—C16—C15	108.5 (7)
O13—K1—O11	104.404 (18)	H1L—C16—H1K	107.7 (10)
O13—K1—O12	129.251 (19)	C18—C17—N1	113.89 (8)
O14—K1—O1	74.465 (19)	H1M—C17—N1	107.9 (7)
O14—K1—O11	146.322 (19)	H1M—C17—C18	105.7 (7)
O14—K1—O12	104.648 (19)	H1N—C17—N1	111.2 (7)
O14—K1—O13	61.225 (18)	H1N—C17—C18	108.2 (7)
O15—K1—O1	147.810 (19)	H1N—C17—H1M	109.8 (10)
O15—K1—O11	99.532 (19)	C17—C18—O13	109.22 (7)
O15—K1—O12	137.655 (19)	H1O—C18—O13	108.2 (7)
O15—K1—O13	89.416 (19)	H1O—C18—C17	110.2 (7)
O15—K1—O14	109.947 (19)	H1P—C18—O13	110.0 (7)
O16—K1—O1	152.204 (19)	H1P—C18—C17	111.3 (7)
O16—K1—O11	119.282 (19)	H1P—C18—H1O	107.9 (9)
O16—K1—O12	97.632 (19)	C20—C19—O13	109.04 (7)
O16—K1—O13	128.514 (19)	H1Q—C19—O13	108.8 (7)
O16—K1—O14	90.419 (19)	H1Q—C19—C20	112.1 (7)
O16—K1—O15	59.192 (18)	H1R—C19—O13	110.2 (7)
N1—K1—O1	90.38 (2)	H1R—C19—C20	108.3 (7)
N1—K1—O11	62.024 (19)	H1R—C19—H1Q	108.5 (10)
N1—K1—O12	120.43 (2)	C19—C20—O14	109.97 (7)
N1—K1—O13	60.314 (19)	H2A—C20—O14	111.1 (7)
N1—K1—O14	120.37 (2)	H2A—C20—C19	108.5 (7)
N1—K1—O15	59.315 (19)	H2B—C20—O14	109.0 (7)
N1—K1—O16	117.42 (2)	H2B—C20—C19	110.2 (7)
N2—K1—O1	92.003 (19)	H2B—C20—H2A	108.0 (10)
N2—K1—O11	117.23 (2)	C22—C21—O14	109.47 (7)
N2—K1—O12	59.316 (19)	H2C—C21—O14	108.9 (7)
N2—K1—O13	122.31 (2)	H2C—C21—C22	109.8 (7)
N2—K1—O14	61.956 (19)	H2D—C21—O14	110.8 (7)
N2—K1—O15	118.66 (2)	H2D—C21—C22	112.4 (7)
N2—K1—O16	60.204 (19)	H2D—C21—H2C	105.4 (10)
N2—K1—N1	177.10 (2)	C21—C22—N2	113.23 (7)
C1—O1—K1	148.71 (6)	H2E—C22—N2	110.5 (7)
C12—O11—K1	111.63 (5)	H2E—C22—C21	109.7 (7)
C13—O11—K1	113.88 (5)	H2F—C22—N2	109.8 (7)
C13—O11—C12	110.37 (7)	H2F—C22—C21	106.2 (7)
C14—O12—K1	117.57 (5)	H2F—C22—H2E	107.0 (10)
C15—O12—K1	121.06 (5)	C24—C23—N1	113.51 (7)
C15—O12—C14	111.86 (7)	H2G—C23—N1	109.3 (7)
C18—O13—K1	121.05 (5)	H2G—C23—C24	106.0 (7)
C19—O13—K1	113.60 (5)	H2H—C23—N1	112.3 (7)
C19—O13—C18	112.01 (7)	H2H—C23—C24	108.9 (7)
C20—O14—K1	113.74 (5)	H2H—C23—H2G	106.3 (10)
C21—O14—K1	111.98 (5)	C23—C24—O15	108.60 (7)
C21—O14—C20	110.82 (7)	H2I—C24—O15	110.8 (7)
C24—O15—K1	115.79 (5)	H2I—C24—C23	112.3 (7)
C25—O15—K1	117.03 (5)	H2J—C24—O15	108.5 (7)
C25—O15—C24	111.25 (7)	H2J—C24—C23	111.1 (7)
C26—O16—K1	112.66 (5)	H2J—C24—H2I	105.4 (9)
C27—O16—K1	119.99 (5)	C26—C25—O15	109.28 (7)
C27—O16—C26	110.67 (7)	H2K—C25—O15	111.4 (7)
C11—N1—K1	107.23 (5)	H2K—C25—C26	109.7 (7)
C17—N1—K1	107.34 (5)	H2L—C25—O15	111.1 (7)
C17—N1—C11	110.19 (7)	H2L—C25—C26	110.0 (7)
C23—N1—K1	112.14 (5)	H2L—C25—H2K	105.3 (10)
C23—N1—C11	109.26 (7)	C25—C26—O16	109.56 (7)
C23—N1—C17	110.61 (7)	H2M—C26—O16	110.0 (7)
C16—N2—K1	109.78 (5)	H2M—C26—C25	110.9 (7)
C22—N2—K1	107.55 (5)	H2N—C26—O16	110.4 (7)
C22—N2—C16	109.45 (7)	H2N—C26—C25	107.7 (7)
C28—N2—K1	108.74 (5)	H2N—C26—H2M	108.2 (10)
C28—N2—C16	110.02 (7)	C28—C27—O16	110.69 (7)
C28—N2—C22	111.25 (7)	H2O—C27—O16	109.7 (7)
O1—C1—Cr1	177.16 (8)	H2O—C27—C28	111.6 (7)
O2—C2—Cr1	178.70 (8)	H2P—C27—O16	107.6 (7)
O3—C3—Cr1	175.92 (8)	H2P—C27—C28	108.6 (7)
O4—C4—Cr1	177.84 (8)	H2P—C27—H2O	108.4 (10)
O5—C5—Cr1	177.60 (8)	C27—C28—N2	114.19 (7)
O6—C6—Cr2	178.83 (8)	H2Q—C28—N2	111.5 (7)
O7—C7—Cr2	178.63 (8)	H2Q—C28—C27	107.5 (7)
O8—C8—Cr2	174.82 (8)	H2R—C28—N2	106.9 (7)
O9—C9—Cr2	178.65 (8)	H2R—C28—C27	108.3 (7)
O10—C10—Cr2	177.95 (8)	H2R—C28—H2Q	108.2 (10)
C12—C11—N1	114.67 (7)	Cr2—H—Cr1	147.5 (9)
K1—O11—C12—C11	−55.94 (5)	K1—N1—C23—C24	−37.43 (6)
K1—O11—C13—C14	53.08 (5)	K1—N2—C16—C15	−48.50 (5)
K1—O12—C14—C13	42.28 (5)	K1—N2—C22—C21	−39.26 (5)
K1—O12—C15—C16	−40.93 (6)	K1—N2—C28—C27	−48.38 (5)
K1—O13—C18—C17	−40.69 (6)	O11—C12—C11—N1	69.84 (8)
K1—O13—C19—C20	49.26 (5)	O11—C13—C14—O12	−63.31 (7)
K1—O14—C20—C19	47.72 (5)	O12—C15—C16—N2	60.62 (8)
K1—O14—C21—C22	−59.73 (5)	O13—C18—C17—N1	62.36 (8)
K1—O15—C24—C23	−55.98 (5)	O13—C19—C20—O14	−65.86 (8)
K1—O15—C25—C26	37.70 (5)	O14—C21—C22—N2	69.64 (8)
K1—O16—C26—C25	57.41 (5)	O15—C24—C23—N1	63.00 (8)
K1—O16—C27—C28	−39.14 (5)	O15—C25—C26—O16	−63.67 (7)
K1—N1—C11—C12	−41.33 (5)	O16—C27—C28—N2	60.45 (8)
K1—N1—C17—C18	−49.77 (5)

(KCPTCR_standard_HAR_SHADE3)

Crystal data

C28H37Cr2KN2O16	F(000) = 1660.306
Mr = 800.70	Dx = 1.489 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71069 Å
a = 10.458 Å	Cell parameters from 1024 reflections
b = 14.417 Å	θ = 47.5–1.5°
c = 23.882 Å	µ = 0.80 mm^−1
β = 97.26°	T = 28 K
V = 3571.89 Å^3	Ellipsoidal, yellow
Z = 4	0.3 × 0.25 × 0.2 mm

Data collection

SMART CCD diffractometer	5667 reflections with I ≥ 2u(I)
ω scan	Rint = 0.0000
Absorption correction: empirical (using intensity measurements)	θmax = 25.0°, θmin = 2.4°
Tmin = 0.890, Tmax = 0.903	h = −19→20
27917 measured reflections	k = 0→30
5993 independent reflections	l = 0→50

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.016	Only H-atom coordinates refined
wR(F^2) = 0.056	w = 1/[σ^2(Fo^2) + (0.1P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 0.51	(Δ/σ)max = 0.0003
5993 reflections	Δρmax = 0.25 e Å^−3
553 parameters	Δρmin = −0.59 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Cr1	0.163857 (14)	0.002354 (9)	0.236365 (6)	0.00535 (6)
Cr2	0.018770 (14)	0.177459 (10)	0.165111 (6)	0.00584 (6)
K1	0.463767 (17)	0.199315 (13)	0.418020 (8)	0.00663 (6)
O1	0.25195 (6)	0.13804 (4)	0.33118 (3)	0.01198 (15)
O2	−0.08335 (6)	−0.04365 (5)	0.28572 (3)	0.01439 (15)
O3	0.10476 (6)	−0.12655 (5)	0.13550 (3)	0.01288 (15)
O4	0.39544 (6)	0.05442 (5)	0.17753 (3)	0.01367 (15)
O5	0.30034 (6)	−0.15026 (5)	0.30578 (3)	0.01284 (15)
O6	−0.25954 (6)	0.12173 (5)	0.17226 (3)	0.01252 (14)
O7	0.01688 (6)	0.05854 (5)	0.05959 (3)	0.01266 (15)
O8	0.28627 (6)	0.25357 (5)	0.15522 (3)	0.01333 (15)
O9	0.02667 (7)	0.26560 (5)	0.28166 (3)	0.01770 (16)
O10	−0.07195 (7)	0.34759 (5)	0.09921 (3)	0.01478 (15)
O11	0.28561 (6)	0.09221 (4)	0.47310 (3)	0.00803 (13)
O12	0.44348 (6)	0.00266 (4)	0.40251 (3)	0.00826 (14)
O13	0.31320 (6)	0.34098 (4)	0.36297 (3)	0.00891 (14)
O14	0.52814 (6)	0.26683 (4)	0.31526 (3)	0.00930 (14)
O15	0.55082 (6)	0.32676 (4)	0.50763 (3)	0.00971 (14)
O16	0.72735 (6)	0.20520 (4)	0.46503 (3)	0.00872 (14)
N1	0.27296 (7)	0.30201 (5)	0.47984 (3)	0.00808 (16)
N2	0.66199 (7)	0.09450 (5)	0.36198 (3)	0.00740 (16)
C1	0.21632 (9)	0.08870 (6)	0.29520 (4)	0.00825 (18)
C2	0.01006 (9)	−0.02698 (6)	0.26775 (4)	0.00874 (18)
C3	0.12295 (8)	−0.07934 (6)	0.17414 (4)	0.00854 (18)
C4	0.30830 (9)	0.03662 (6)	0.20000 (4)	0.00902 (19)
C5	0.25044 (9)	−0.09129 (6)	0.27870 (4)	0.00825 (18)
C6	−0.15482 (9)	0.14177 (6)	0.16988 (4)	0.00850 (19)
C7	0.01883 (9)	0.10387 (6)	0.09905 (4)	0.00801 (18)
C8	0.18842 (9)	0.22127 (6)	0.16008 (4)	0.00885 (19)
C9	0.02390 (9)	0.23370 (6)	0.23782 (4)	0.01084 (19)
C10	−0.03871 (9)	0.28246 (7)	0.12523 (4)	0.00981 (19)
C11	0.20826 (9)	0.23289 (6)	0.51158 (4)	0.00908 (18)
C12	0.17315 (9)	0.14354 (6)	0.47988 (4)	0.00860 (18)
C13	0.25209 (9)	0.00557 (6)	0.44644 (4)	0.00823 (19)
C14	0.37233 (9)	−0.04765 (6)	0.43914 (4)	0.00809 (18)
C15	0.54807 (9)	−0.04995 (6)	0.38673 (4)	0.00793 (18)
C16	0.60994 (9)	0.00372 (6)	0.34259 (4)	0.00835 (19)
C17	0.17935 (9)	0.34651 (6)	0.43709 (4)	0.00974 (19)
C18	0.24060 (9)	0.40164 (6)	0.39330 (4)	0.00971 (19)
C19	0.37489 (9)	0.38872 (6)	0.32179 (4)	0.01096 (19)
C20	0.42824 (9)	0.31887 (6)	0.28398 (4)	0.0111 (2)
C21	0.57231 (9)	0.19479 (6)	0.28140 (4)	0.00969 (19)
C22	0.69043 (9)	0.14952 (6)	0.31301 (4)	0.00900 (18)
C23	0.33591 (9)	0.37147 (6)	0.51925 (4)	0.01049 (19)
C24	0.46540 (9)	0.34038 (7)	0.54890 (4)	0.01063 (19)
C25	0.68003 (9)	0.31749 (6)	0.53316 (4)	0.00836 (19)
C26	0.76434 (9)	0.29308 (6)	0.48870 (4)	0.00938 (19)
C27	0.82372 (9)	0.16976 (6)	0.43399 (4)	0.00907 (19)
C28	0.77753 (8)	0.08205 (6)	0.40286 (4)	0.00832 (18)
H	0.0498 (13)	0.0755 (10)	0.1993 (6)	0.030527
H1A	0.1194 (13)	0.2614 (9)	0.5255 (6)	0.024289
H1B	0.2727 (12)	0.2168 (10)	0.5498 (6)	0.022751
H1C	0.1183 (13)	0.1562 (9)	0.4377 (5)	0.021028
H1D	0.1091 (12)	0.1020 (9)	0.5033 (5)	0.022939
H1E	0.1944 (13)	0.0151 (9)	0.4055 (5)	0.020573
H1F	0.1943 (12)	−0.0367 (9)	0.4722 (5)	0.022397
H1G	0.3439 (12)	−0.1152 (9)	0.4214 (5)	0.021019
H1H	0.4294 (12)	−0.0585 (9)	0.4804 (5)	0.021119
H1I	0.5121 (12)	−0.1158 (9)	0.3670 (6)	0.022303
H1J	0.6138 (12)	−0.0683 (9)	0.4239 (5)	0.021728
H1K	0.5381 (13)	0.0160 (9)	0.3063 (6)	0.020906
H1L	0.6856 (12)	−0.0395 (9)	0.3283 (5)	0.023003
H1M	0.1242 (13)	0.2928 (9)	0.4141 (6)	0.022053
H1N	0.1143 (12)	0.3928 (10)	0.4566 (5)	0.024473
H1O	0.1639 (13)	0.4348 (9)	0.3625 (6)	0.023631
H1P	0.3032 (12)	0.4574 (9)	0.4132 (5)	0.023421
H1Q	0.4501 (13)	0.4332 (9)	0.3433 (5)	0.022510
H1R	0.3055 (12)	0.4323 (9)	0.2958 (5)	0.022657
H2A	0.3498 (12)	0.2737 (9)	0.2659 (5)	0.020374
H2B	0.4671 (13)	0.3540 (9)	0.2491 (5)	0.022422
H2C	0.5967 (12)	0.2251 (10)	0.2417 (5)	0.022614
H2D	0.4947 (12)	0.1445 (9)	0.2686 (6)	0.020467
H2E	0.7385 (12)	0.1061 (9)	0.2838 (5)	0.023148
H2F	0.7566 (12)	0.2056 (9)	0.3271 (5)	0.022658
H2G	0.3545 (13)	0.4339 (9)	0.4961 (5)	0.023863
H2H	0.2739 (13)	0.3930 (10)	0.5513 (6)	0.024830
H2I	0.4576 (13)	0.2743 (10)	0.5748 (6)	0.022146
H2J	0.5069 (12)	0.3929 (9)	0.5789 (5)	0.023871
H2K	0.7142 (12)	0.3804 (9)	0.5542 (5)	0.022828
H2L	0.6879 (12)	0.2631 (9)	0.5665 (6)	0.021779
H2M	0.7570 (13)	0.3471 (9)	0.4545 (5)	0.022142
H2N	0.8621 (12)	0.2910 (9)	0.5085 (5)	0.022271
H2O	0.8503 (12)	0.2214 (9)	0.4057 (5)	0.022294
H2P	0.9114 (13)	0.1520 (9)	0.4652 (6)	0.022884
H2Q	0.8588 (12)	0.0544 (10)	0.3826 (5)	0.023803
H2R	0.7537 (12)	0.0321 (9)	0.4333 (5)	0.021898

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cr1	0.00568 (9)	0.00476 (9)	0.00553 (9)	0.00015 (5)	0.00040 (6)	−0.00011 (5)
Cr2	0.00672 (9)	0.00541 (9)	0.00518 (9)	0.00084 (5)	−0.00006 (6)	0.00019 (5)
K1	0.00610 (11)	0.00679 (10)	0.00686 (11)	0.00026 (7)	0.00029 (8)	−0.00014 (7)
O1	0.0157 (4)	0.0090 (3)	0.0101 (3)	−0.0003 (3)	−0.0026 (3)	−0.0023 (3)
O2	0.0113 (4)	0.0162 (4)	0.0170 (3)	0.0000 (3)	0.0070 (3)	0.0010 (3)
O3	0.0151 (3)	0.0127 (3)	0.0109 (3)	−0.0024 (3)	0.0017 (3)	−0.0050 (3)
O4	0.0109 (3)	0.0143 (3)	0.0170 (3)	−0.0008 (3)	0.0063 (3)	0.0001 (3)
O5	0.0138 (3)	0.0098 (3)	0.0142 (3)	0.0032 (3)	−0.0009 (3)	0.0021 (3)
O6	0.0097 (4)	0.0151 (3)	0.0133 (3)	−0.0011 (3)	0.0032 (3)	0.0011 (3)
O7	0.0164 (4)	0.0125 (3)	0.0094 (3)	−0.0017 (3)	0.0027 (3)	−0.0036 (3)
O8	0.0110 (4)	0.0157 (3)	0.0131 (3)	−0.0047 (3)	0.0010 (3)	0.0014 (3)
O9	0.0258 (4)	0.0175 (4)	0.0089 (4)	0.0096 (3)	−0.0014 (3)	−0.0050 (3)
O10	0.0184 (4)	0.0091 (3)	0.0157 (3)	0.0027 (3)	−0.0025 (3)	0.0044 (3)
O11	0.0063 (3)	0.0077 (3)	0.0100 (3)	0.0001 (2)	0.0004 (2)	−0.0004 (2)
O12	0.0094 (3)	0.0060 (3)	0.0098 (3)	0.0005 (2)	0.0029 (3)	0.0011 (2)
O13	0.0096 (3)	0.0069 (3)	0.0103 (3)	0.0013 (2)	0.0014 (3)	0.0009 (2)
O14	0.0105 (3)	0.0094 (3)	0.0078 (3)	0.0014 (2)	0.0006 (2)	0.0005 (2)
O15	0.0083 (3)	0.0121 (3)	0.0085 (3)	0.0009 (2)	0.0005 (3)	−0.0019 (2)
O16	0.0058 (3)	0.0094 (3)	0.0108 (3)	−0.0012 (2)	0.0005 (3)	−0.0020 (3)
N1	0.0066 (4)	0.0080 (4)	0.0097 (4)	0.0011 (3)	0.0011 (3)	−0.0008 (3)
N2	0.0073 (4)	0.0071 (4)	0.0080 (4)	−0.0001 (3)	0.0017 (3)	0.0000 (3)
C1	0.0085 (4)	0.0066 (4)	0.0094 (4)	0.0002 (3)	0.0001 (3)	−0.0003 (4)
C2	0.0069 (5)	0.0095 (4)	0.0100 (4)	0.0005 (4)	0.0019 (4)	0.0004 (3)
C3	0.0080 (4)	0.0078 (4)	0.0097 (5)	−0.0004 (3)	0.0007 (3)	−0.0019 (4)
C4	0.0077 (5)	0.0087 (4)	0.0109 (4)	−0.0008 (3)	0.0019 (4)	−0.0003 (3)
C5	0.0089 (4)	0.0072 (4)	0.0085 (4)	0.0014 (3)	0.0003 (3)	0.0006 (4)
C6	0.0087 (5)	0.0092 (4)	0.0077 (4)	0.0004 (3)	0.0012 (3)	0.0004 (3)
C7	0.0092 (4)	0.0073 (4)	0.0073 (5)	−0.0002 (3)	0.0002 (3)	−0.0004 (4)
C8	0.0091 (5)	0.0092 (4)	0.0079 (4)	−0.0015 (4)	−0.0001 (3)	−0.0004 (3)
C9	0.0141 (5)	0.0102 (4)	0.0077 (5)	0.0041 (4)	−0.0010 (4)	−0.0009 (4)
C10	0.0111 (4)	0.0073 (4)	0.0106 (4)	0.0013 (3)	0.0000 (4)	0.0005 (4)
C11	0.0100 (5)	0.0095 (4)	0.0080 (4)	0.0023 (4)	0.0020 (3)	−0.0001 (4)
C12	0.0064 (4)	0.0094 (4)	0.0099 (4)	0.0002 (3)	0.0007 (3)	0.0009 (4)
C13	0.0080 (5)	0.0083 (4)	0.0084 (4)	−0.0023 (3)	0.0011 (4)	−0.0006 (3)
C14	0.0093 (4)	0.0064 (4)	0.0085 (4)	−0.0007 (3)	0.0011 (4)	0.0006 (3)
C15	0.0080 (4)	0.0071 (4)	0.0085 (4)	0.0006 (3)	0.0008 (4)	0.0006 (3)
C16	0.0097 (5)	0.0086 (4)	0.0068 (4)	−0.0005 (3)	0.0014 (4)	−0.0012 (3)
C17	0.0088 (5)	0.0091 (4)	0.0116 (4)	0.0019 (4)	0.0022 (4)	0.0012 (4)
C18	0.0100 (5)	0.0079 (4)	0.0114 (4)	0.0019 (3)	0.0021 (4)	0.0019 (4)
C19	0.0116 (5)	0.0082 (4)	0.0134 (5)	0.0025 (4)	0.0027 (4)	0.0029 (4)
C20	0.0128 (5)	0.0119 (5)	0.0088 (4)	0.0031 (4)	0.0018 (4)	0.0034 (4)
C21	0.0119 (5)	0.0086 (4)	0.0083 (4)	0.0023 (4)	0.0004 (4)	0.0012 (3)
C22	0.0089 (5)	0.0093 (4)	0.0093 (4)	0.0006 (4)	0.0033 (4)	0.0014 (4)
C23	0.0089 (5)	0.0109 (4)	0.0114 (5)	0.0017 (4)	0.0003 (4)	−0.0036 (4)
C24	0.0079 (5)	0.0143 (5)	0.0094 (4)	0.0005 (4)	−0.0002 (4)	−0.0028 (4)
C25	0.0069 (4)	0.0090 (4)	0.0087 (4)	−0.0005 (3)	−0.0009 (4)	−0.0024 (4)
C26	0.0077 (5)	0.0095 (4)	0.0108 (5)	−0.0016 (3)	0.0004 (4)	−0.0020 (4)
C27	0.0067 (4)	0.0107 (4)	0.0098 (4)	−0.0018 (3)	0.0010 (4)	−0.0023 (4)
C28	0.0066 (4)	0.0087 (4)	0.0096 (4)	−0.0001 (3)	0.0009 (3)	−0.0014 (4)
H	0.026530	0.024200	0.039420	0.003300	−0.001400	0.011960
H1A	0.018270	0.029330	0.026570	0.004120	0.007910	−0.004980
H1B	0.021540	0.028380	0.016960	−0.000530	−0.002910	0.001140
H1C	0.019820	0.026620	0.015600	0.004020	−0.001830	−0.000840
H1D	0.019820	0.027100	0.023320	−0.003700	0.008270	0.001420
H1E	0.021780	0.021930	0.016470	0.002090	−0.003580	0.000800
H1F	0.022380	0.022850	0.023110	−0.005780	0.007350	0.003540
H1G	0.025360	0.014280	0.023080	−0.002870	0.001750	−0.001010
H1H	0.019700	0.025300	0.017020	−0.000610	−0.002880	0.004800
H1I	0.024800	0.014670	0.027390	−0.000930	0.003110	−0.003990
H1J	0.019390	0.024650	0.019980	0.005400	−0.002040	0.002520
H1K	0.019500	0.022030	0.019620	0.000230	−0.003630	0.001260
H1L	0.019700	0.022100	0.028290	0.005480	0.007240	−0.004460
H1M	0.022110	0.020540	0.022110	−0.002280	−0.002650	−0.003250
H1N	0.023680	0.026200	0.023940	0.010010	0.004570	−0.005080
H1O	0.023820	0.022390	0.023260	0.008270	−0.002560	0.001270
H1P	0.025160	0.017720	0.026640	−0.002260	0.000380	−0.006720
H1Q	0.024690	0.019650	0.022270	−0.007680	−0.000620	−0.002250
H1R	0.024530	0.018860	0.023380	0.004630	−0.001650	0.004470
H2A	0.018630	0.016200	0.025140	−0.003530	−0.001720	−0.001730
H2B	0.026250	0.022620	0.018970	−0.002130	0.005090	0.005990
H2C	0.025280	0.026650	0.016940	−0.000110	0.006670	0.004150
H2D	0.016510	0.019080	0.025670	−0.003720	0.002120	−0.004140
H2E	0.022660	0.027250	0.020760	0.004440	0.007520	−0.003490
H2F	0.019980	0.023970	0.023310	−0.007610	−0.000040	−0.000320
H2G	0.027620	0.018710	0.024110	−0.000500	−0.001200	0.000910
H2H	0.021240	0.031620	0.022100	0.004500	0.004570	−0.008990
H2I	0.022880	0.021860	0.022310	0.001970	0.005240	0.003330
H2J	0.022880	0.025750	0.022060	−0.000620	−0.000750	−0.009920
H2K	0.022670	0.020310	0.024650	−0.002880	−0.000330	−0.007100
H2L	0.020780	0.023920	0.020450	0.000530	0.001880	0.005890
H2M	0.028630	0.018820	0.018720	−0.002770	0.002000	0.002940
H2N	0.014380	0.026590	0.024860	−0.001130	−0.001350	−0.002540
H2O	0.023620	0.022300	0.021990	−0.002410	0.006890	0.002620
H2P	0.014580	0.030160	0.022820	0.002540	−0.001890	−0.002250
H2Q	0.016290	0.030690	0.025050	0.004600	0.005030	−0.006170
H2R	0.022120	0.021570	0.021490	−0.001400	0.000760	0.004650

Geometric parameters (Å, º)

Cr1—C1	1.9053 (9)	N2—C22	1.4742 (11)
Cr1—C2	1.9059 (9)	N2—C28	1.4653 (11)
Cr1—C3	1.9020 (9)	C11—C12	1.5157 (13)
Cr1—C4	1.9004 (9)	C11—H1A	1.105 (13)
Cr1—C5	1.8529 (9)	C11—H1B	1.089 (13)
Cr1—H	1.747 (13)	C12—H1C	1.109 (13)
Cr2—C6	1.9041 (10)	C12—H1D	1.102 (13)
Cr2—C7	1.9013 (9)	C13—C14	1.5020 (13)
Cr2—C8	1.9013 (9)	C13—H1E	1.091 (13)
Cr2—C9	1.9111 (10)	C13—H1F	1.099 (12)
Cr2—C10	1.8480 (10)	C14—H1G	1.088 (13)
Cr2—H	1.694 (13)	C14—H1H	1.096 (12)
K1—O1	2.9711 (7)	C15—C16	1.5169 (12)
K1—O11	2.8645 (6)	C15—H1I	1.105 (13)
K1—O12	2.8637 (6)	C15—H1J	1.084 (12)
K1—O13	2.8029 (6)	C16—H1K	1.087 (13)
K1—O14	2.8001 (6)	C16—H1L	1.096 (12)
K1—O15	2.8796 (7)	C17—C18	1.5181 (12)
K1—O16	2.8432 (6)	C17—H1M	1.074 (13)
K1—N1	3.0163 (8)	C17—H1N	1.097 (13)
K1—N2	3.0122 (8)	C18—H1O	1.124 (13)
O1—C1	1.1413 (11)	C18—H1P	1.106 (13)
O2—C2	1.1412 (12)	C19—C20	1.5061 (13)
O3—C3	1.1433 (12)	C19—H1Q	1.092 (12)
O4—C4	1.1437 (12)	C19—H1R	1.092 (12)
O5—C5	1.1524 (12)	C20—H2A	1.093 (13)
O6—C6	1.1410 (12)	C20—H2B	1.096 (13)
O7—C7	1.1448 (11)	C21—C22	1.5120 (13)
O8—C8	1.1435 (12)	C21—H2C	1.103 (13)
O9—C9	1.1405 (12)	C21—H2D	1.103 (13)
O10—C10	1.1551 (12)	C22—H2E	1.105 (13)
O11—C12	1.4161 (11)	C22—H2F	1.090 (13)
O11—C13	1.4254 (11)	C23—C24	1.5145 (13)
O12—C14	1.4176 (11)	C23—H2G	1.087 (13)
O12—C15	1.4205 (11)	C23—H2H	1.109 (13)
O13—C18	1.4160 (11)	C24—H2I	1.146 (14)
O13—C19	1.4203 (11)	C24—H2J	1.094 (13)
O14—C20	1.4195 (11)	C25—C26	1.5052 (12)
O14—C21	1.4284 (11)	C25—H2K	1.076 (13)
O15—C24	1.4248 (11)	C25—H2L	1.112 (13)
O15—C25	1.4168 (11)	C26—H2M	1.123 (13)
O16—C26	1.4210 (11)	C26—H2N	1.071 (12)
O16—C27	1.4196 (11)	C27—C28	1.5146 (12)
N1—C11	1.4680 (11)	C27—H2O	1.066 (13)
N1—C17	1.4696 (12)	C27—H2P	1.135 (13)
N1—C23	1.4716 (12)	C28—H2Q	1.105 (13)
N2—C16	1.4695 (11)	C28—H2R	1.075 (13)
C2—Cr1—C1	91.93 (4)	H1A—C11—N1	111.3 (7)
C3—Cr1—C1	174.95 (4)	H1A—C11—C12	107.9 (7)
C3—Cr1—C2	92.99 (4)	H1B—C11—N1	107.5 (7)
C4—Cr1—C1	89.76 (4)	H1B—C11—C12	108.9 (7)
C4—Cr1—C2	175.16 (4)	H1B—C11—H1A	106.4 (10)
C4—Cr1—C3	85.25 (4)	C11—C12—O11	110.42 (7)
C5—Cr1—C1	89.90 (4)	H1C—C12—O11	108.9 (7)
C5—Cr1—C2	90.13 (4)	H1C—C12—C11	112.3 (7)
C5—Cr1—C3	91.22 (4)	H1D—C12—O11	109.9 (7)
C5—Cr1—C4	94.41 (4)	H1D—C12—C11	109.4 (7)
H—Cr1—C1	95.4 (5)	H1D—C12—H1C	105.8 (10)
H—Cr1—C2	77.1 (5)	C14—C13—O11	109.71 (7)
H—Cr1—C3	84.6 (5)	H1E—C13—O11	111.6 (7)
H—Cr1—C4	98.2 (5)	H1E—C13—C14	109.6 (7)
H—Cr1—C5	166.3 (5)	H1F—C13—O11	110.9 (7)
C7—Cr2—C6	89.95 (4)	H1F—C13—C14	108.0 (7)
C8—Cr2—C6	176.26 (4)	H1F—C13—H1E	106.9 (10)
C8—Cr2—C7	91.99 (4)	C13—C14—O12	108.83 (7)
C9—Cr2—C6	88.73 (4)	H1G—C14—O12	110.9 (7)
C9—Cr2—C7	171.05 (4)	H1G—C14—C13	108.1 (7)
C9—Cr2—C8	89.84 (4)	H1H—C14—O12	111.0 (7)
C10—Cr2—C6	90.10 (4)	H1H—C14—C13	109.7 (7)
C10—Cr2—C7	93.65 (4)	H1H—C14—H1G	108.2 (10)
C10—Cr2—C8	86.60 (4)	C16—C15—O12	108.81 (7)
C10—Cr2—C9	95.20 (4)	H1I—C15—O12	109.9 (7)
H—Cr2—C6	82.1 (5)	H1I—C15—C16	107.1 (7)
H—Cr2—C7	84.0 (5)	H1J—C15—O12	110.1 (7)
H—Cr2—C8	101.3 (5)	H1J—C15—C16	114.3 (7)
H—Cr2—C9	87.0 (5)	H1J—C15—H1I	106.6 (10)
H—Cr2—C10	171.8 (5)	C15—C16—N2	114.14 (7)
O11—K1—O1	71.904 (18)	H1K—C16—N2	107.3 (7)
O12—K1—O1	65.092 (18)	H1K—C16—C15	108.9 (7)
O12—K1—O11	58.924 (18)	H1L—C16—N2	110.6 (7)
O13—K1—O1	64.159 (18)	H1L—C16—C15	108.4 (7)
O13—K1—O11	104.404 (18)	H1L—C16—H1K	107.3 (10)
O13—K1—O12	129.251 (19)	C18—C17—N1	113.90 (8)
O14—K1—O1	74.468 (19)	H1M—C17—N1	108.0 (7)
O14—K1—O11	146.325 (19)	H1M—C17—C18	105.7 (7)
O14—K1—O12	104.649 (19)	H1N—C17—N1	111.4 (7)
O14—K1—O13	61.224 (18)	H1N—C17—C18	108.1 (7)
O15—K1—O1	147.809 (19)	H1N—C17—H1M	109.5 (10)
O15—K1—O11	99.530 (19)	C17—C18—O13	109.22 (7)
O15—K1—O12	137.655 (19)	H1O—C18—O13	108.2 (7)
O15—K1—O13	89.415 (19)	H1O—C18—C17	110.2 (7)
O15—K1—O14	109.945 (19)	H1P—C18—O13	110.0 (7)
O16—K1—O1	152.206 (19)	H1P—C18—C17	111.3 (7)
O16—K1—O11	119.284 (19)	H1P—C18—H1O	107.9 (9)
O16—K1—O12	97.636 (19)	C20—C19—O13	109.03 (7)
O16—K1—O13	128.510 (19)	H1Q—C19—O13	108.8 (7)
O16—K1—O14	90.416 (19)	H1Q—C19—C20	112.1 (7)
O16—K1—O15	59.190 (18)	H1R—C19—O13	110.2 (7)
N1—K1—O1	90.38 (2)	H1R—C19—C20	108.3 (7)
N1—K1—O11	62.025 (19)	H1R—C19—H1Q	108.4 (10)
N1—K1—O12	120.43 (2)	C19—C20—O14	109.98 (7)
N1—K1—O13	60.314 (19)	H2A—C20—O14	111.0 (7)
N1—K1—O14	120.37 (2)	H2A—C20—C19	108.6 (7)
N1—K1—O15	59.312 (19)	H2B—C20—O14	109.0 (7)
N1—K1—O16	117.41 (2)	H2B—C20—C19	110.3 (7)
N2—K1—O1	92.004 (19)	H2B—C20—H2A	107.9 (10)
N2—K1—O11	117.24 (2)	C22—C21—O14	109.48 (7)
N2—K1—O12	59.319 (19)	H2C—C21—O14	109.0 (7)
N2—K1—O13	122.31 (2)	H2C—C21—C22	109.7 (7)
N2—K1—O14	61.954 (19)	H2D—C21—O14	110.8 (7)
N2—K1—O15	118.66 (2)	H2D—C21—C22	112.4 (7)
N2—K1—O16	60.206 (19)	H2D—C21—H2C	105.4 (10)
N2—K1—N1	177.10 (2)	C21—C22—N2	113.23 (7)
C1—O1—K1	148.72 (6)	H2E—C22—N2	110.5 (7)
C12—O11—K1	111.63 (5)	H2E—C22—C21	109.7 (7)
C13—O11—K1	113.88 (5)	H2F—C22—N2	109.8 (7)
C13—O11—C12	110.37 (7)	H2F—C22—C21	106.3 (7)
C14—O12—K1	117.57 (5)	H2F—C22—H2E	107.1 (10)
C15—O12—K1	121.06 (5)	C24—C23—N1	113.51 (7)
C15—O12—C14	111.86 (7)	H2G—C23—N1	109.4 (7)
C18—O13—K1	121.05 (5)	H2G—C23—C24	106.0 (7)
C19—O13—K1	113.61 (5)	H2H—C23—N1	112.3 (7)
C19—O13—C18	112.01 (7)	H2H—C23—C24	109.1 (7)
C20—O14—K1	113.73 (5)	H2H—C23—H2G	106.1 (10)
C21—O14—K1	111.98 (5)	C23—C24—O15	108.61 (7)
C21—O14—C20	110.82 (7)	H2I—C24—O15	110.7 (7)
C24—O15—K1	115.79 (5)	H2I—C24—C23	112.2 (7)
C25—O15—K1	117.03 (5)	H2J—C24—O15	108.5 (7)
C25—O15—C24	111.26 (7)	H2J—C24—C23	111.0 (7)
C26—O16—K1	112.66 (5)	H2J—C24—H2I	105.8 (9)
C27—O16—K1	119.99 (5)	C26—C25—O15	109.28 (7)
C27—O16—C26	110.67 (7)	H2K—C25—O15	111.4 (7)
C11—N1—K1	107.23 (5)	H2K—C25—C26	109.7 (7)
C17—N1—K1	107.34 (5)	H2L—C25—O15	110.8 (7)
C17—N1—C11	110.19 (7)	H2L—C25—C26	110.0 (7)
C23—N1—K1	112.14 (5)	H2L—C25—H2K	105.7 (10)
C23—N1—C11	109.25 (7)	C25—C26—O16	109.56 (7)
C23—N1—C17	110.62 (7)	H2M—C26—O16	109.8 (7)
C16—N2—K1	109.78 (5)	H2M—C26—C25	111.0 (7)
C22—N2—K1	107.56 (5)	H2N—C26—O16	110.3 (7)
C22—N2—C16	109.46 (7)	H2N—C26—C25	107.9 (7)
C28—N2—K1	108.73 (5)	H2N—C26—H2M	108.3 (10)
C28—N2—C16	110.02 (7)	C28—C27—O16	110.69 (7)
C28—N2—C22	111.25 (7)	H2O—C27—O16	109.8 (7)
O1—C1—Cr1	177.15 (8)	H2O—C27—C28	111.4 (7)
O2—C2—Cr1	178.70 (8)	H2P—C27—O16	107.9 (7)
O3—C3—Cr1	175.92 (8)	H2P—C27—C28	108.4 (7)
O4—C4—Cr1	177.84 (8)	H2P—C27—H2O	108.6 (10)
O5—C5—Cr1	177.60 (8)	C27—C28—N2	114.20 (7)
O6—C6—Cr2	178.83 (8)	H2Q—C28—N2	111.5 (7)
O7—C7—Cr2	178.63 (8)	H2Q—C28—C27	107.6 (7)
O8—C8—Cr2	174.82 (8)	H2R—C28—N2	106.9 (7)
O9—C9—Cr2	178.67 (8)	H2R—C28—C27	108.3 (7)
O10—C10—Cr2	177.95 (8)	H2R—C28—H2Q	108.2 (10)
C12—C11—N1	114.67 (7)	Cr2—H—Cr1	147.7 (9)
K1—O11—C12—C11	−55.93 (5)	K1—N1—C23—C24	−37.41 (6)
K1—O11—C13—C14	53.08 (5)	K1—N2—C16—C15	−48.49 (5)
K1—O12—C14—C13	42.28 (5)	K1—N2—C22—C21	−39.26 (5)
K1—O12—C15—C16	−40.92 (6)	K1—N2—C28—C27	−48.38 (5)
K1—O13—C18—C17	−40.68 (6)	O11—C12—C11—N1	69.83 (8)
K1—O13—C19—C20	49.26 (5)	O11—C13—C14—O12	−63.31 (7)
K1—O14—C20—C19	47.72 (5)	O12—C15—C16—N2	60.61 (8)
K1—O14—C21—C22	−59.72 (5)	O13—C18—C17—N1	62.35 (8)
K1—O15—C24—C23	−55.98 (5)	O13—C19—C20—O14	−65.86 (8)
K1—O15—C25—C26	37.71 (5)	O14—C21—C22—N2	69.63 (8)
K1—O16—C26—C25	57.40 (5)	O15—C24—C23—N1	62.99 (8)
K1—O16—C27—C28	−39.13 (5)	O15—C25—C26—O16	−63.67 (7)
K1—N1—C11—C12	−41.33 (5)	O16—C27—C28—N2	60.44 (8)
K1—N1—C17—C18	−49.77 (5)

(KCPTCR_standard_IAM_0_HADPs)

Crystal data

C28H37Cr2KN2O16	F(000) = 1660.538
Mr = 800.70	Dx = 1.489 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71069 Å
a = 10.458 Å	Cell parameters from 1024 reflections
b = 14.417 Å	θ = 47.5–1.5°
c = 23.882 Å	µ = 0.80 mm^−1
β = 97.26°	T = 28 K
V = 3571.89 Å^3	Ellipsoidal, yellow
Z = 4	0.3 × 0.25 × 0.2 mm

Data collection

SMART CCD diffractometer	5667 reflections with I ≥ 2u(I)
ω scan	Rint = 0.0000
Absorption correction: empirical (using intensity measurements)	θmax = 25.0°, θmin = 2.4°
Tmin = 0.890, Tmax = 0.903	h = −19→20
27917 measured reflections	k = 0→30
5993 independent reflections	l = 0→50

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.023	Only H-atom coordinates refined
wR(F^2) = 0.058	w = 1/[σ^2(Fo^2) + (0.0255P)^2 + 2.6258P] where P = (Fo^2 + 2Fc^2)/3
S = 1.07	(Δ/σ)max = −0.0004
5993 reflections	Δρmax = 0.29 e Å^−3
553 parameters	Δρmin = −0.42 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Cr1	0.16383 (2)	0.002378 (16)	0.236355 (10)	0.00593 (7)
Cr2	0.01878 (2)	0.177442 (16)	0.165112 (10)	0.00645 (7)
K1	0.46375 (3)	0.19929 (2)	0.418013 (13)	0.00710 (8)
O1	0.25196 (11)	0.13802 (7)	0.33118 (5)	0.0122 (2)
O2	−0.08332 (11)	−0.04365 (8)	0.28576 (5)	0.0142 (2)
O3	0.10480 (11)	−0.12659 (8)	0.13552 (5)	0.0127 (2)
O4	0.39525 (11)	0.05451 (8)	0.17752 (5)	0.0138 (2)
O5	0.30030 (11)	−0.15024 (8)	0.30579 (5)	0.0126 (2)
O6	−0.25961 (11)	0.12158 (8)	0.17225 (5)	0.0125 (2)
O7	0.01680 (11)	0.05859 (8)	0.05960 (4)	0.0125 (2)
O8	0.28634 (11)	0.25366 (8)	0.15525 (5)	0.0132 (2)
O9	0.02667 (12)	0.26551 (8)	0.28166 (5)	0.0174 (3)
O10	−0.07189 (11)	0.34756 (8)	0.09920 (5)	0.0146 (2)
O11	0.28611 (10)	0.09228 (7)	0.47319 (4)	0.0084 (2)
O12	0.44336 (10)	0.00296 (7)	0.40241 (5)	0.0088 (2)
O13	0.31323 (10)	0.34068 (7)	0.36303 (4)	0.0093 (2)
O14	0.52836 (10)	0.26690 (7)	0.31550 (4)	0.0096 (2)
O15	0.55084 (10)	0.32678 (7)	0.50742 (4)	0.0101 (2)
O16	0.72689 (10)	0.20500 (7)	0.46502 (4)	0.0088 (2)
N1	0.27338 (12)	0.30189 (9)	0.47976 (5)	0.0085 (3)
N2	0.66152 (12)	0.09473 (9)	0.36203 (5)	0.0081 (3)
C1	0.21620 (14)	0.08848 (10)	0.29503 (6)	0.0087 (3)
C2	0.01015 (15)	−0.02691 (10)	0.26768 (6)	0.0094 (3)
C3	0.12291 (14)	−0.07916 (11)	0.17424 (7)	0.0092 (3)
C4	0.30799 (15)	0.03674 (10)	0.19998 (6)	0.0097 (3)
C5	0.25009 (15)	−0.09109 (11)	0.27864 (6)	0.0087 (3)
C6	−0.15442 (16)	0.14187 (10)	0.16986 (6)	0.0094 (3)
C7	0.01875 (14)	0.10408 (10)	0.09911 (7)	0.0089 (3)
C8	0.18801 (16)	0.22114 (10)	0.16010 (6)	0.0099 (3)
C9	0.02388 (15)	0.23368 (11)	0.23779 (7)	0.0117 (3)
C10	−0.03865 (15)	0.28238 (11)	0.12531 (7)	0.0102 (3)
C11	0.20805 (15)	0.23278 (11)	0.51155 (7)	0.0097 (3)
C12	0.17287 (15)	0.14371 (11)	0.47994 (7)	0.0093 (3)
C13	0.25210 (15)	0.00532 (10)	0.44638 (7)	0.0089 (3)
C14	0.37204 (15)	−0.04775 (10)	0.43920 (7)	0.0088 (3)
C15	0.54846 (15)	−0.05003 (11)	0.38668 (7)	0.0085 (3)
C16	0.60995 (16)	0.00358 (11)	0.34264 (7)	0.0089 (3)
C17	0.17912 (15)	0.34655 (11)	0.43692 (7)	0.0102 (3)
C18	0.24061 (16)	0.40169 (11)	0.39338 (7)	0.0104 (3)
C19	0.37513 (16)	0.38878 (11)	0.32174 (7)	0.0115 (3)
C20	0.42789 (16)	0.31899 (11)	0.28397 (7)	0.0113 (3)
C21	0.57251 (16)	0.19473 (11)	0.28131 (7)	0.0100 (3)
C22	0.69032 (15)	0.14961 (11)	0.31295 (7)	0.0097 (3)
C23	0.33616 (15)	0.37150 (11)	0.51920 (7)	0.0111 (3)
C24	0.46484 (15)	0.34036 (11)	0.54887 (7)	0.0110 (3)
C25	0.68027 (15)	0.31743 (11)	0.53316 (7)	0.0090 (3)
C26	0.76444 (15)	0.29331 (11)	0.48877 (7)	0.0097 (3)
C27	0.82398 (15)	0.16960 (11)	0.43392 (7)	0.0095 (3)
C28	0.77738 (15)	0.08199 (11)	0.40286 (7)	0.0087 (3)
H	0.0517 (15)	0.0755 (11)	0.2001 (7)	0.000000
H11a	0.1282 (16)	0.2597 (11)	0.5232 (7)	0.000000
H11b	0.2631 (16)	0.2186 (11)	0.5452 (7)	0.000000
H12a	0.1254 (16)	0.1556 (11)	0.4423 (7)	0.000000
H12b	0.1155 (16)	0.1072 (11)	0.5018 (7)	0.000000
H13a	0.2013 (16)	0.0150 (11)	0.4099 (7)	0.000000
H13b	0.2008 (16)	−0.0306 (11)	0.4687 (7)	0.000000
H14a	0.3453 (15)	−0.1074 (12)	0.4229 (7)	0.000000
H14b	0.4219 (15)	−0.0567 (11)	0.4761 (7)	0.000000
H15a	0.5171 (15)	−0.1073 (12)	0.3704 (7)	0.000000
H15b	0.6084 (16)	−0.0653 (11)	0.4195 (7)	0.000000
H16a	0.5463 (16)	0.0132 (11)	0.3112 (7)	0.000000
H16b	0.6764 (16)	−0.0340 (11)	0.3298 (7)	0.000000
H17a	0.1290 (16)	0.2986 (12)	0.4169 (7)	0.000000
H17b	0.1222 (16)	0.3858 (11)	0.4543 (7)	0.000000
H18a	0.1730 (16)	0.4298 (11)	0.3673 (7)	0.000000
H18b	0.2972 (16)	0.4499 (12)	0.4115 (7)	0.000000
H19a	0.4423 (16)	0.4274 (12)	0.3400 (7)	0.000000
H19b	0.3138 (16)	0.4270 (11)	0.2984 (7)	0.000000
H20a	0.3594 (16)	0.2787 (12)	0.2685 (7)	0.000000
H20b	0.4602 (15)	0.3498 (11)	0.2544 (7)	0.000000
H21a	0.5936 (15)	0.2209 (11)	0.2457 (7)	0.000000
H21b	0.5068 (16)	0.1519 (12)	0.2718 (7)	0.000000
H22a	0.7302 (15)	0.1095 (11)	0.2859 (7)	0.000000
H22b	0.7486 (16)	0.1983 (12)	0.3254 (7)	0.000000
H23a	0.3487 (15)	0.4265 (12)	0.4977 (7)	0.000000
H23b	0.2812 (16)	0.3898 (11)	0.5470 (7)	0.000000
H24a	0.4602 (15)	0.2824 (12)	0.5713 (7)	0.000000
H24b	0.4981 (15)	0.3860 (12)	0.5751 (7)	0.000000
H25a	0.7111 (15)	0.3742 (12)	0.5510 (7)	0.000000
H25b	0.6866 (15)	0.2688 (12)	0.5622 (7)	0.000000
H26a	0.7598 (15)	0.3379 (12)	0.4598 (7)	0.000000
H26b	0.8519 (17)	0.2920 (11)	0.5070 (7)	0.000000
H27a	0.8471 (15)	0.2145 (12)	0.4087 (7)	0.000000
H27b	0.9012 (16)	0.1542 (11)	0.4611 (7)	0.000000
H28a	0.8467 (16)	0.0562 (11)	0.3853 (7)	0.000000
H28b	0.7606 (15)	0.0371 (12)	0.4290 (7)	0.000000

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cr1	0.00628 (13)	0.00529 (12)	0.00618 (12)	−0.00001 (9)	0.00058 (9)	−0.00023 (9)
Cr2	0.00742 (13)	0.00596 (12)	0.00581 (12)	0.00071 (9)	0.00014 (9)	0.00003 (9)
K1	0.00662 (16)	0.00719 (15)	0.00738 (16)	0.00028 (12)	0.00039 (12)	−0.00007 (12)
O1	0.0148 (6)	0.0097 (5)	0.0110 (6)	0.0001 (4)	−0.0024 (5)	−0.0012 (5)
O2	0.0113 (6)	0.0157 (6)	0.0166 (6)	0.0004 (5)	0.0055 (5)	0.0010 (5)
O3	0.0141 (6)	0.0128 (6)	0.0113 (6)	−0.0023 (5)	0.0018 (4)	−0.0038 (5)
O4	0.0116 (6)	0.0133 (6)	0.0173 (6)	−0.0007 (5)	0.0056 (5)	−0.0006 (5)
O5	0.0132 (6)	0.0100 (5)	0.0142 (6)	0.0027 (5)	−0.0006 (5)	0.0014 (5)
O6	0.0111 (6)	0.0146 (6)	0.0124 (6)	−0.0009 (5)	0.0033 (4)	0.0006 (4)
O7	0.0160 (6)	0.0124 (5)	0.0091 (6)	−0.0020 (5)	0.0023 (4)	−0.0025 (5)
O8	0.0122 (6)	0.0151 (6)	0.0120 (6)	−0.0039 (5)	0.0006 (4)	0.0009 (5)
O9	0.0248 (7)	0.0168 (6)	0.0096 (6)	0.0094 (5)	−0.0016 (5)	−0.0043 (5)
O10	0.0179 (6)	0.0098 (6)	0.0151 (6)	0.0027 (5)	−0.0018 (5)	0.0036 (5)
O11	0.0059 (5)	0.0072 (5)	0.0119 (5)	0.0003 (4)	0.0004 (4)	−0.0019 (4)
O12	0.0089 (5)	0.0070 (5)	0.0112 (5)	0.0011 (4)	0.0046 (4)	0.0018 (4)
O13	0.0106 (6)	0.0075 (5)	0.0106 (5)	0.0016 (4)	0.0036 (4)	0.0011 (4)
O14	0.0109 (5)	0.0095 (5)	0.0082 (5)	0.0030 (4)	0.0001 (4)	0.0001 (4)
O15	0.0070 (5)	0.0147 (6)	0.0084 (5)	0.0011 (4)	0.0006 (4)	−0.0020 (4)
O16	0.0064 (5)	0.0086 (5)	0.0116 (5)	−0.0009 (4)	0.0016 (4)	−0.0040 (4)
N1	0.0073 (6)	0.0085 (6)	0.0093 (6)	0.0003 (5)	−0.0003 (5)	0.0001 (5)
N2	0.0085 (6)	0.0078 (6)	0.0081 (6)	−0.0010 (5)	0.0008 (5)	0.0006 (5)
C1	0.0070 (7)	0.0080 (7)	0.0112 (8)	0.0024 (6)	0.0020 (6)	0.0046 (6)
C2	0.0131 (8)	0.0066 (7)	0.0077 (7)	0.0020 (6)	−0.0020 (6)	−0.0007 (6)
C3	0.0052 (7)	0.0092 (7)	0.0134 (8)	0.0009 (6)	0.0022 (6)	0.0037 (6)
C4	0.0117 (8)	0.0064 (7)	0.0099 (7)	0.0016 (6)	−0.0026 (6)	−0.0016 (6)
C5	0.0076 (7)	0.0102 (7)	0.0088 (7)	−0.0028 (6)	0.0028 (6)	−0.0045 (6)
C6	0.0160 (9)	0.0073 (7)	0.0045 (7)	0.0035 (6)	0.0003 (6)	0.0006 (6)
C7	0.0055 (7)	0.0089 (7)	0.0121 (8)	−0.0006 (6)	0.0007 (6)	0.0054 (6)
C8	0.0158 (9)	0.0083 (7)	0.0050 (7)	0.0027 (6)	−0.0015 (6)	−0.0012 (6)
C9	0.0104 (8)	0.0091 (7)	0.0149 (9)	0.0040 (6)	−0.0010 (6)	0.0035 (6)
C10	0.0088 (8)	0.0118 (8)	0.0099 (7)	−0.0011 (6)	0.0012 (6)	−0.0045 (6)
C11	0.0092 (8)	0.0115 (8)	0.0085 (8)	0.0029 (6)	0.0022 (6)	0.0015 (6)
C12	0.0063 (7)	0.0109 (8)	0.0109 (8)	0.0016 (6)	0.0012 (6)	0.0017 (6)
C13	0.0103 (8)	0.0078 (7)	0.0085 (8)	−0.0036 (6)	0.0006 (6)	−0.0006 (6)
C14	0.0107 (8)	0.0075 (7)	0.0083 (8)	−0.0023 (6)	0.0014 (6)	0.0010 (6)
C15	0.0079 (8)	0.0069 (7)	0.0104 (8)	0.0020 (6)	0.0000 (6)	−0.0009 (6)
C16	0.0097 (8)	0.0088 (7)	0.0079 (7)	0.0007 (6)	0.0003 (6)	−0.0022 (6)
C17	0.0081 (8)	0.0094 (7)	0.0131 (8)	0.0030 (6)	0.0016 (6)	0.0007 (6)
C18	0.0105 (8)	0.0081 (7)	0.0125 (8)	0.0029 (6)	0.0011 (6)	0.0006 (6)
C19	0.0124 (8)	0.0094 (8)	0.0130 (8)	0.0014 (7)	0.0026 (7)	0.0048 (6)
C20	0.0117 (8)	0.0131 (8)	0.0090 (8)	0.0025 (7)	0.0009 (6)	0.0051 (6)
C21	0.0141 (8)	0.0079 (7)	0.0081 (8)	0.0013 (6)	0.0021 (6)	−0.0001 (6)
C22	0.0104 (8)	0.0100 (7)	0.0095 (8)	−0.0006 (6)	0.0040 (6)	0.0009 (6)
C23	0.0098 (8)	0.0112 (8)	0.0125 (8)	0.0011 (6)	0.0026 (6)	−0.0042 (6)
C24	0.0098 (8)	0.0142 (8)	0.0094 (8)	0.0000 (6)	0.0026 (6)	−0.0037 (7)
C25	0.0071 (8)	0.0091 (7)	0.0101 (7)	−0.0007 (6)	−0.0022 (6)	−0.0019 (6)
C26	0.0088 (8)	0.0086 (7)	0.0112 (8)	−0.0022 (6)	−0.0006 (6)	−0.0012 (6)
C27	0.0062 (8)	0.0120 (8)	0.0106 (8)	−0.0004 (6)	0.0021 (6)	−0.0012 (6)
C28	0.0062 (8)	0.0101 (7)	0.0097 (7)	0.0010 (6)	0.0013 (6)	−0.0004 (6)
H	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H11a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H11b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H12a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H12b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H13a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H13b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H14a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H14b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H15a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H15b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H16a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H16b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H17a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H17b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H18a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H18b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H19a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H19b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H20a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H20b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H21a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H21b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H22a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H22b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H23a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H23b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H24a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H24b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H25a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H25b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H26a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H26b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H27a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H27b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H28a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H28b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000

Geometric parameters (Å, º)

Cr1—C1	1.9001 (16)	N2—C22	1.4763 (19)
Cr1—C2	1.9040 (16)	N2—C28	1.468 (2)
Cr1—C3	1.8987 (16)	C11—C12	1.511 (2)
Cr1—C4	1.8983 (16)	C11—H11a	0.992 (17)
Cr1—C5	1.8491 (16)	C11—H11b	0.950 (17)
Cr1—H	1.726 (16)	C12—H12a	0.986 (17)
Cr2—C6	1.8997 (17)	C12—H12b	0.994 (17)
Cr2—C7	1.8981 (16)	C13—C14	1.497 (2)
Cr2—C8	1.8965 (17)	C13—H13a	0.971 (17)
Cr2—C9	1.9104 (17)	C13—H13b	0.956 (17)
Cr2—C10	1.8463 (16)	C14—H14a	0.970 (17)
Cr2—H	1.704 (16)	C14—H14b	0.974 (17)
K1—O1	2.9708 (11)	C15—C16	1.513 (2)
K1—O11	2.8612 (11)	C15—H15a	0.952 (17)
K1—O12	2.8594 (11)	C15—H15b	0.964 (17)
K1—O13	2.7991 (11)	C16—H16a	0.948 (17)
K1—O14	2.7961 (11)	C16—H16b	0.962 (17)
K1—O15	2.8766 (11)	C17—C18	1.515 (2)
K1—O16	2.8388 (11)	C17—H17a	0.959 (17)
K1—N1	3.0113 (13)	C17—H17b	0.954 (17)
K1—N2	3.0061 (13)	C18—H18a	0.970 (17)
O1—C1	1.1462 (19)	C18—H18b	0.977 (17)
O2—C2	1.143 (2)	C19—C20	1.502 (2)
O3—C3	1.1465 (19)	C19—H19a	0.957 (17)
O4—C4	1.144 (2)	C19—H19b	0.967 (17)
O5—C5	1.1564 (19)	C20—H20a	0.959 (17)
O6—C6	1.147 (2)	C20—H20b	0.933 (17)
O7—C7	1.1472 (19)	C21—C22	1.509 (2)
O8—C8	1.149 (2)	C21—H21a	0.981 (17)
O9—C9	1.141 (2)	C21—H21b	0.930 (17)
O10—C10	1.157 (2)	C22—H22a	0.997 (17)
O11—C12	1.4236 (18)	C22—H22b	0.952 (17)
O11—C13	1.4320 (18)	C23—C24	1.508 (2)
O12—C14	1.4243 (18)	C23—H23a	0.963 (17)
O12—C15	1.4274 (18)	C23—H23b	0.967 (17)
O13—C18	1.4196 (18)	C24—H24a	0.997 (17)
O13—C19	1.4261 (19)	C24—H24b	0.944 (17)
O14—C20	1.4265 (19)	C25—C26	1.502 (2)
O14—C21	1.4345 (18)	C25—H25a	0.960 (17)
O15—C24	1.4327 (18)	C25—H25b	0.982 (17)
O15—C25	1.4206 (19)	C26—H26a	0.941 (17)
O16—C26	1.4285 (18)	C26—H26b	0.962 (17)
O16—C27	1.4261 (18)	C27—C28	1.514 (2)
N1—C11	1.472 (2)	C27—H27a	0.938 (17)
N1—C17	1.476 (2)	C27—H27b	0.995 (17)
N1—C23	1.473 (2)	C28—H28a	0.958 (17)
N2—C16	1.4728 (19)	C28—H28b	0.931 (17)
C2—Cr1—C1	91.95 (6)	H11a—C11—N1	109.9 (9)
C3—Cr1—C1	174.96 (6)	H11a—C11—C12	108.2 (9)
C3—Cr1—C2	92.96 (6)	H11b—C11—N1	108.1 (10)
C4—Cr1—C1	89.74 (6)	H11b—C11—C12	108.8 (10)
C4—Cr1—C2	175.07 (6)	H11b—C11—H11a	106.8 (13)
C4—Cr1—C3	85.28 (6)	C11—C12—O11	110.22 (12)
C5—Cr1—C1	89.89 (6)	H12a—C12—O11	108.5 (9)
C5—Cr1—C2	90.09 (6)	H12a—C12—C11	111.8 (9)
C5—Cr1—C3	91.24 (6)	H12b—C12—O11	110.4 (9)
C5—Cr1—C4	94.54 (6)	H12b—C12—C11	108.3 (9)
H—Cr1—C1	94.9 (5)	H12b—C12—H12a	107.6 (13)
H—Cr1—C2	77.2 (5)	C14—C13—O11	109.52 (12)
H—Cr1—C3	85.1 (5)	H13a—C13—O11	110.6 (10)
H—Cr1—C4	98.0 (5)	H13a—C13—C14	110.0 (10)
H—Cr1—C5	166.6 (5)	H13b—C13—O11	110.5 (10)
C7—Cr2—C6	89.95 (6)	H13b—C13—C14	108.9 (10)
C8—Cr2—C6	176.25 (7)	H13b—C13—H13a	107.2 (13)
C8—Cr2—C7	92.00 (6)	C13—C14—O12	108.66 (12)
C9—Cr2—C6	88.72 (7)	H14a—C14—O12	110.8 (9)
C9—Cr2—C7	171.12 (6)	H14a—C14—C13	107.2 (9)
C9—Cr2—C8	89.84 (7)	H14b—C14—O12	111.3 (9)
C10—Cr2—C6	90.08 (7)	H14b—C14—C13	109.0 (9)
C10—Cr2—C7	93.62 (7)	H14b—C14—H14a	109.9 (13)
C10—Cr2—C8	86.61 (7)	C16—C15—O12	108.58 (12)
C10—Cr2—C9	95.16 (7)	H15a—C15—O12	109.5 (10)
H—Cr2—C6	82.7 (5)	H15a—C15—C16	108.3 (10)
H—Cr2—C7	84.6 (5)	H15b—C15—O12	110.6 (10)
H—Cr2—C8	100.7 (5)	H15b—C15—C16	113.1 (10)
H—Cr2—C9	86.6 (5)	H15b—C15—H15a	106.7 (14)
H—Cr2—C10	172.6 (5)	C15—C16—N2	114.11 (12)
O11—K1—O1	72.00 (3)	H16a—C16—N2	108.1 (10)
O12—K1—O1	65.04 (3)	H16a—C16—C15	107.9 (10)
O12—K1—O11	58.95 (3)	H16b—C16—N2	110.6 (10)
O13—K1—O1	64.12 (3)	H16b—C16—C15	108.7 (10)
O13—K1—O11	104.44 (3)	H16b—C16—H16a	107.1 (14)
O13—K1—O12	129.16 (3)	C18—C17—N1	113.60 (13)
O14—K1—O1	74.56 (3)	H17a—C17—N1	107.8 (10)
O14—K1—O11	146.51 (3)	H17a—C17—C18	106.8 (10)
O14—K1—O12	104.67 (3)	H17b—C17—N1	110.8 (10)
O14—K1—O13	61.26 (3)	H17b—C17—C18	109.3 (10)
O15—K1—O1	147.81 (3)	H17b—C17—H17a	108.3 (13)
O15—K1—O11	99.54 (3)	C17—C18—O13	109.04 (12)
O15—K1—O12	137.79 (3)	H18a—C18—O13	108.9 (9)
O15—K1—O13	89.39 (3)	H18a—C18—C17	108.8 (9)
O15—K1—O14	109.77 (3)	H18b—C18—O13	109.5 (9)
O16—K1—O1	152.20 (3)	H18b—C18—C17	110.8 (9)
O16—K1—O11	119.14 (3)	H18b—C18—H18a	109.8 (13)
O16—K1—O12	97.63 (3)	C20—C19—O13	108.83 (13)
O16—K1—O13	128.61 (3)	H19a—C19—O13	109.8 (10)
O16—K1—O14	90.39 (3)	H19a—C19—C20	111.0 (10)
O16—K1—O15	59.19 (3)	H19b—C19—O13	110.4 (9)
N1—K1—O1	90.41 (3)	H19b—C19—C20	107.7 (9)
N1—K1—O11	62.06 (3)	H19b—C19—H19a	109.0 (14)
N1—K1—O12	120.47 (3)	C19—C20—O14	109.73 (13)
N1—K1—O13	60.30 (3)	H20a—C20—O14	110.4 (10)
N1—K1—O14	120.36 (3)	H20a—C20—C19	108.9 (10)
N1—K1—O15	59.31 (3)	H20b—C20—O14	109.7 (10)
N1—K1—O16	117.38 (3)	H20b—C20—C19	109.3 (10)
N2—K1—O1	91.98 (3)	H20b—C20—H20a	108.7 (14)
N2—K1—O11	117.24 (3)	C22—C21—O14	109.20 (12)
N2—K1—O12	59.32 (3)	H21a—C21—O14	109.8 (9)
N2—K1—O13	122.29 (3)	H21a—C21—C22	110.0 (9)
N2—K1—O14	61.93 (3)	H21b—C21—O14	109.9 (10)
N2—K1—O15	118.65 (3)	H21b—C21—C22	111.6 (10)
N2—K1—O16	60.23 (3)	H21b—C21—H21a	106.4 (13)
N2—K1—N1	177.11 (4)	C21—C22—N2	113.14 (13)
C1—O1—K1	148.72 (10)	H22a—C22—N2	110.4 (9)
C12—O11—K1	111.67 (8)	H22a—C22—C21	107.9 (9)
C13—O11—K1	113.90 (8)	H22b—C22—N2	109.5 (10)
C13—O11—C12	110.08 (11)	H22b—C22—C21	106.8 (10)
C14—O12—K1	117.64 (8)	H22b—C22—H22a	109.0 (13)
C15—O12—K1	121.13 (8)	C24—C23—N1	113.39 (13)
C15—O12—C14	111.61 (11)	H23a—C23—N1	107.4 (10)
C18—O13—K1	121.14 (9)	H23a—C23—C24	108.8 (10)
C19—O13—K1	113.64 (9)	H23b—C23—N1	111.7 (10)
C19—O13—C18	111.76 (11)	H23b—C23—C24	109.3 (9)
C20—O14—K1	113.72 (9)	H23b—C23—H23a	105.9 (13)
C21—O14—K1	112.10 (8)	C23—C24—O15	108.48 (13)
C21—O14—C20	110.49 (12)	H24a—C24—O15	109.6 (9)
C24—O15—K1	115.63 (9)	H24a—C24—C23	113.6 (9)
C25—O15—K1	117.10 (8)	H24b—C24—O15	110.0 (10)
C25—O15—C24	111.16 (11)	H24b—C24—C23	109.7 (10)
C26—O16—K1	112.77 (8)	H24b—C24—H24a	105.4 (13)
C27—O16—K1	120.14 (8)	C26—C25—O15	109.14 (12)
C27—O16—C26	110.34 (11)	H25a—C25—O15	111.1 (10)
C11—N1—K1	107.38 (9)	H25a—C25—C26	108.5 (9)
C17—N1—K1	107.45 (9)	H25b—C25—O15	110.4 (9)
C17—N1—C11	109.87 (12)	H25b—C25—C26	109.8 (9)
C23—N1—K1	112.27 (9)	H25b—C25—H25a	107.9 (13)
C23—N1—C11	109.25 (12)	C25—C26—O16	109.29 (12)
C23—N1—C17	110.54 (12)	H26a—C26—O16	109.3 (10)
C16—N2—K1	110.00 (9)	H26a—C26—C25	112.3 (10)
C22—N2—K1	107.77 (9)	H26b—C26—O16	111.1 (10)
C22—N2—C16	109.40 (12)	H26b—C26—C25	107.1 (10)
C28—N2—K1	108.90 (9)	H26b—C26—H26a	107.6 (14)
C28—N2—C16	109.63 (12)	C28—C27—O16	110.34 (12)
C28—N2—C22	111.12 (12)	H27a—C27—O16	110.2 (10)
O1—C1—Cr1	177.16 (13)	H27a—C27—C28	110.8 (10)
O2—C2—Cr1	178.81 (13)	H27b—C27—O16	108.2 (9)
O3—C3—Cr1	175.88 (13)	H27b—C27—C28	108.5 (9)
O4—C4—Cr1	177.77 (13)	H27b—C27—H27a	108.7 (13)
O5—C5—Cr1	177.74 (13)	C27—C28—N2	114.13 (13)
O6—C6—Cr2	178.94 (13)	H28a—C28—N2	111.4 (10)
O7—C7—Cr2	178.58 (13)	H28a—C28—C27	108.9 (10)
O8—C8—Cr2	174.78 (13)	H28b—C28—N2	108.8 (10)
O9—C9—Cr2	178.60 (14)	H28b—C28—C27	109.2 (10)
O10—C10—Cr2	177.85 (13)	H28b—C28—H28a	104.0 (14)
C12—C11—N1	114.65 (13)	Cr2—H—Cr1	148.8 (10)
K1—O11—C12—C11	−56.06 (9)	K1—N1—C23—C24	−37.64 (10)
K1—O11—C13—C14	53.32 (9)	K1—N2—C16—C15	−48.39 (9)
K1—O12—C14—C13	42.44 (9)	K1—N2—C22—C21	−39.32 (9)
K1—O12—C15—C16	−41.13 (9)	K1—N2—C28—C27	−48.53 (9)
K1—O13—C18—C17	−41.02 (9)	O11—C12—C11—N1	69.62 (13)
K1—O13—C19—C20	49.50 (9)	O11—C13—C14—O12	−63.36 (12)
K1—O14—C20—C19	48.07 (9)	O12—C15—C16—N2	60.44 (13)
K1—O14—C21—C22	−59.80 (9)	O13—C18—C17—N1	62.46 (13)
K1—O15—C24—C23	−56.20 (9)	O13—C19—C20—O14	−66.06 (13)
K1—O15—C25—C26	38.04 (9)	O14—C21—C22—N2	69.44 (13)
K1—O16—C26—C25	57.52 (9)	O15—C24—C23—N1	63.18 (13)
K1—O16—C27—C28	−39.20 (9)	O15—C25—C26—O16	−63.73 (13)
K1—N1—C11—C12	−41.24 (9)	O16—C27—C28—N2	60.36 (13)
K1—N1—C17—C18	−49.95 (9)

(KCPTCR_standard_IAM)

Crystal data

C28H37Cr2KN2O16	F(000) = 1660.538
Mr = 800.70	Dx = 1.489 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71069 Å
a = 10.458 Å	Cell parameters from 1024 reflections
b = 14.417 Å	θ = 47.5–1.5°
c = 23.882 Å	µ = 0.80 mm^−1
β = 97.26°	T = 28 K
V = 3571.89 Å^3	Ellipsoidal, yellow
Z = 4	0.3 × 0.25 × 0.2 mm

Data collection

SMART CCD diffractometer	5667 reflections with I ≥ 2u(I)
ω scan	Rint = 0.0000
Absorption correction: empirical (using intensity measurements)	θmax = 25.0°, θmin = 2.4°
Tmin = 0.890, Tmax = 0.903	h = −19→20
27917 measured reflections	k = 0→30
5993 independent reflections	l = 0→50

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.022	All H-atom parameters refined
wR(F^2) = 0.057	w = 1/[σ^2(Fo^2) + (0.0257P)^2 + 2.5203P] where P = (Fo^2 + 2Fc^2)/3
S = 1.06	(Δ/σ)max = −0.001
5993 reflections	Δρmax = 0.30 e Å^−3
590 parameters	Δρmin = −0.36 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Cr1	0.16384 (2)	0.002378 (16)	0.236356 (10)	0.00599 (6)
Cr2	0.01879 (2)	0.177442 (16)	0.165112 (10)	0.00652 (7)
K1	0.46375 (3)	0.19929 (2)	0.418014 (13)	0.00714 (7)
O1	0.25195 (11)	0.13804 (7)	0.33117 (4)	0.0122 (2)
O2	−0.08330 (10)	−0.04365 (8)	0.28577 (5)	0.0143 (2)
O3	0.10481 (11)	−0.12657 (8)	0.13552 (5)	0.0128 (2)
O4	0.39526 (10)	0.05452 (8)	0.17752 (5)	0.0138 (2)
O5	0.30030 (10)	−0.15023 (7)	0.30578 (5)	0.0127 (2)
O6	−0.25961 (11)	0.12159 (8)	0.17225 (5)	0.0126 (2)
O7	0.01682 (10)	0.05859 (7)	0.05961 (4)	0.0126 (2)
O8	0.28633 (11)	0.25366 (8)	0.15525 (5)	0.0133 (2)
O9	0.02666 (12)	0.26550 (8)	0.28167 (5)	0.0175 (3)
O10	−0.07189 (11)	0.34755 (8)	0.09920 (5)	0.0146 (2)
O11	0.28611 (10)	0.09227 (7)	0.47319 (4)	0.0085 (2)
O12	0.44336 (10)	0.00298 (7)	0.40241 (4)	0.0088 (2)
O13	0.31324 (10)	0.34067 (7)	0.36303 (4)	0.0094 (2)
O14	0.52834 (10)	0.26690 (7)	0.31550 (4)	0.0097 (2)
O15	0.55083 (10)	0.32677 (7)	0.50741 (4)	0.0101 (2)
O16	0.72689 (10)	0.20501 (7)	0.46502 (4)	0.0089 (2)
N1	0.27339 (12)	0.30188 (9)	0.47975 (5)	0.0085 (3)
N2	0.66152 (12)	0.09474 (9)	0.36202 (5)	0.0081 (3)
C1	0.21619 (14)	0.08849 (10)	0.29504 (6)	0.0087 (3)
C2	0.01018 (15)	−0.02689 (10)	0.26768 (6)	0.0094 (3)
C3	0.12290 (14)	−0.07916 (10)	0.17424 (6)	0.0093 (3)
C4	0.30799 (15)	0.03673 (10)	0.19998 (6)	0.0097 (3)
C5	0.25013 (14)	−0.09112 (10)	0.27864 (6)	0.0088 (3)
C6	−0.15440 (15)	0.14188 (10)	0.16987 (6)	0.0094 (3)
C7	0.01874 (14)	0.10408 (10)	0.09912 (6)	0.0090 (3)
C8	0.18803 (15)	0.22113 (10)	0.16010 (6)	0.0100 (3)
C9	0.02390 (15)	0.23366 (10)	0.23779 (7)	0.0118 (3)
C10	−0.03866 (15)	0.28241 (11)	0.12530 (6)	0.0103 (3)
C11	0.20809 (15)	0.23277 (11)	0.51155 (6)	0.0098 (3)
C12	0.17289 (15)	0.14373 (11)	0.47994 (7)	0.0095 (3)
C13	0.25214 (15)	0.00532 (10)	0.44638 (7)	0.0090 (3)
C14	0.37204 (15)	−0.04774 (10)	0.43920 (6)	0.0089 (3)
C15	0.54841 (15)	−0.05002 (10)	0.38667 (6)	0.0086 (3)
C16	0.60993 (15)	0.00361 (10)	0.34263 (6)	0.0089 (3)
C17	0.17912 (15)	0.34653 (11)	0.43692 (7)	0.0103 (3)
C18	0.24064 (15)	0.40167 (11)	0.39339 (7)	0.0106 (3)
C19	0.37514 (16)	0.38876 (11)	0.32173 (7)	0.0117 (3)
C20	0.42786 (16)	0.31898 (11)	0.28398 (7)	0.0114 (3)
C21	0.57252 (16)	0.19470 (11)	0.28133 (6)	0.0100 (3)
C22	0.69030 (15)	0.14961 (11)	0.31296 (6)	0.0099 (3)
C23	0.33617 (15)	0.37146 (11)	0.51920 (7)	0.0112 (3)
C24	0.46483 (15)	0.34035 (11)	0.54886 (7)	0.0112 (3)
C25	0.68024 (14)	0.31744 (11)	0.53316 (6)	0.0091 (3)
C26	0.76442 (15)	0.29330 (11)	0.48877 (7)	0.0098 (3)
C27	0.82397 (15)	0.16958 (11)	0.43392 (7)	0.0097 (3)
C28	0.77736 (14)	0.08200 (11)	0.40287 (6)	0.0088 (3)
H	0.052 (2)	0.0759 (16)	0.2000 (9)	0.033 (6)*
H1A	0.1277 (18)	0.2598 (12)	0.5231 (7)	0.009 (4)*
H1B	0.2633 (17)	0.2184 (12)	0.5453 (8)	0.008 (4)*
H1C	0.1254 (16)	0.1555 (12)	0.4423 (7)	0.006 (4)*
H1D	0.1151 (17)	0.1071 (12)	0.5019 (7)	0.009 (4)*
H1E	0.2012 (16)	0.0147 (12)	0.4098 (8)	0.006 (4)*
H1F	0.2004 (17)	−0.0307 (12)	0.4687 (7)	0.007 (4)*
H1G	0.3450 (16)	−0.1076 (12)	0.4228 (7)	0.006 (4)*
H1H	0.4222 (15)	−0.0567 (11)	0.4761 (7)	0.000 (4)*
H1I	0.5172 (16)	−0.1074 (13)	0.3703 (7)	0.007 (4)*
H1J	0.6085 (17)	−0.0655 (12)	0.4197 (7)	0.006 (4)*
H1K	0.5462 (17)	0.0132 (11)	0.3111 (7)	0.005 (4)*
H1L	0.6765 (17)	−0.0339 (12)	0.3298 (7)	0.008 (4)*
H1M	0.1288 (16)	0.2985 (12)	0.4169 (7)	0.003 (4)*
H1N	0.1218 (17)	0.3858 (12)	0.4544 (7)	0.009 (4)*
H1O	0.1733 (18)	0.4297 (13)	0.3675 (8)	0.012 (4)*
H1P	0.2974 (16)	0.4501 (12)	0.4117 (7)	0.005 (4)*
H1Q	0.4424 (17)	0.4274 (12)	0.3401 (7)	0.006 (4)*
H1R	0.3131 (19)	0.4272 (14)	0.2981 (8)	0.020 (5)*
H2A	0.3592 (18)	0.2786 (13)	0.2683 (7)	0.008 (4)*
H2B	0.4605 (18)	0.3502 (14)	0.2543 (8)	0.017 (5)*
H2C	0.5929 (17)	0.2211 (12)	0.2456 (8)	0.010 (4)*
H2D	0.5067 (17)	0.1517 (12)	0.2717 (7)	0.007 (4)*
H2E	0.7300 (17)	0.1094 (13)	0.2857 (8)	0.013 (4)*
H2F	0.7489 (17)	0.1984 (13)	0.3255 (7)	0.010 (4)*
H2G	0.3487 (16)	0.4267 (13)	0.4975 (7)	0.008 (4)*
H2H	0.2808 (18)	0.3897 (13)	0.5473 (8)	0.016 (5)*
H2I	0.4605 (17)	0.2827 (13)	0.5714 (8)	0.011 (4)*
H2J	0.4975 (18)	0.3865 (14)	0.5751 (8)	0.016 (5)*
H2K	0.7111 (16)	0.3743 (12)	0.5510 (7)	0.005 (4)*
H2L	0.6869 (16)	0.2689 (12)	0.5623 (7)	0.007 (4)*
H2M	0.7596 (17)	0.3382 (13)	0.4597 (8)	0.010 (4)*
H2N	0.8525 (18)	0.2916 (12)	0.5070 (8)	0.010 (4)*
H2O	0.8472 (17)	0.2147 (13)	0.4085 (8)	0.009 (4)*
H2P	0.9014 (17)	0.1541 (12)	0.4612 (7)	0.008 (4)*
H2Q	0.8467 (18)	0.0560 (12)	0.3851 (8)	0.011 (4)*
H2R	0.7606 (15)	0.0369 (12)	0.4290 (7)	0.001 (4)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cr1	0.00634 (12)	0.00536 (12)	0.00623 (12)	−0.00003 (8)	0.00060 (9)	−0.00025 (9)
Cr2	0.00746 (13)	0.00604 (12)	0.00588 (12)	0.00071 (9)	0.00016 (9)	0.00002 (9)
K1	0.00667 (16)	0.00723 (15)	0.00741 (15)	0.00029 (12)	0.00041 (12)	−0.00006 (12)
O1	0.0149 (6)	0.0097 (5)	0.0110 (5)	0.0002 (4)	−0.0024 (4)	−0.0012 (5)
O2	0.0114 (6)	0.0158 (6)	0.0167 (6)	0.0005 (4)	0.0055 (5)	0.0010 (5)
O3	0.0142 (6)	0.0129 (5)	0.0113 (6)	−0.0023 (4)	0.0018 (4)	−0.0038 (5)
O4	0.0117 (6)	0.0134 (6)	0.0174 (6)	−0.0007 (4)	0.0056 (5)	−0.0006 (5)
O5	0.0133 (6)	0.0101 (5)	0.0141 (5)	0.0027 (4)	−0.0006 (4)	0.0015 (5)
O6	0.0113 (6)	0.0147 (5)	0.0124 (5)	−0.0008 (4)	0.0034 (4)	0.0005 (4)
O7	0.0161 (6)	0.0126 (5)	0.0092 (6)	−0.0021 (4)	0.0022 (4)	−0.0025 (5)
O8	0.0122 (6)	0.0151 (6)	0.0122 (5)	−0.0039 (5)	0.0005 (4)	0.0010 (4)
O9	0.0250 (7)	0.0169 (6)	0.0097 (6)	0.0094 (5)	−0.0016 (5)	−0.0042 (5)
O10	0.0179 (6)	0.0098 (5)	0.0152 (6)	0.0027 (5)	−0.0018 (5)	0.0037 (5)
O11	0.0060 (5)	0.0073 (5)	0.0119 (5)	0.0003 (4)	0.0004 (4)	−0.0019 (4)
O12	0.0089 (5)	0.0070 (5)	0.0113 (5)	0.0011 (4)	0.0046 (4)	0.0019 (4)
O13	0.0106 (5)	0.0075 (5)	0.0107 (5)	0.0016 (4)	0.0036 (4)	0.0012 (4)
O14	0.0109 (5)	0.0096 (5)	0.0083 (5)	0.0030 (4)	0.0002 (4)	0.0001 (4)
O15	0.0071 (5)	0.0148 (5)	0.0084 (5)	0.0011 (4)	0.0006 (4)	−0.0020 (4)
O16	0.0064 (5)	0.0087 (5)	0.0117 (5)	−0.0010 (4)	0.0016 (4)	−0.0040 (4)
N1	0.0074 (6)	0.0084 (6)	0.0094 (6)	0.0003 (5)	−0.0002 (5)	0.0000 (5)
N2	0.0085 (6)	0.0078 (6)	0.0080 (6)	−0.0010 (5)	0.0007 (5)	0.0005 (5)
C1	0.0071 (7)	0.0082 (7)	0.0111 (7)	0.0023 (6)	0.0021 (6)	0.0046 (6)
C2	0.0131 (8)	0.0066 (7)	0.0077 (7)	0.0020 (6)	−0.0019 (6)	−0.0006 (6)
C3	0.0052 (7)	0.0093 (7)	0.0135 (8)	0.0008 (6)	0.0022 (6)	0.0038 (6)
C4	0.0117 (8)	0.0065 (7)	0.0099 (7)	0.0017 (6)	−0.0025 (6)	−0.0016 (6)
C5	0.0076 (7)	0.0103 (7)	0.0088 (7)	−0.0027 (6)	0.0027 (6)	−0.0044 (6)
C6	0.0160 (9)	0.0074 (7)	0.0046 (7)	0.0034 (6)	0.0002 (6)	0.0005 (6)
C7	0.0056 (7)	0.0089 (7)	0.0123 (8)	−0.0005 (6)	0.0008 (6)	0.0054 (6)
C8	0.0158 (9)	0.0083 (7)	0.0051 (7)	0.0026 (6)	−0.0016 (6)	−0.0011 (6)
C9	0.0105 (8)	0.0093 (7)	0.0148 (8)	0.0041 (6)	−0.0010 (6)	0.0035 (6)
C10	0.0089 (7)	0.0119 (8)	0.0101 (7)	−0.0011 (6)	0.0012 (6)	−0.0046 (6)
C11	0.0095 (8)	0.0117 (7)	0.0086 (7)	0.0028 (6)	0.0023 (6)	0.0015 (6)
C12	0.0064 (7)	0.0110 (7)	0.0110 (8)	0.0016 (6)	0.0012 (6)	0.0016 (6)
C13	0.0104 (8)	0.0079 (7)	0.0088 (7)	−0.0035 (6)	0.0006 (6)	−0.0007 (6)
C14	0.0107 (8)	0.0077 (7)	0.0083 (7)	−0.0022 (6)	0.0015 (6)	0.0011 (6)
C15	0.0081 (7)	0.0070 (7)	0.0105 (8)	0.0021 (6)	0.0003 (6)	−0.0009 (6)
C16	0.0097 (8)	0.0089 (7)	0.0079 (7)	0.0007 (6)	0.0005 (6)	−0.0021 (6)
C17	0.0083 (8)	0.0096 (7)	0.0131 (8)	0.0030 (6)	0.0015 (6)	0.0007 (6)
C18	0.0107 (8)	0.0083 (7)	0.0128 (8)	0.0029 (6)	0.0014 (6)	0.0006 (6)
C19	0.0126 (8)	0.0096 (7)	0.0132 (8)	0.0013 (6)	0.0029 (6)	0.0046 (6)
C20	0.0118 (8)	0.0132 (8)	0.0093 (7)	0.0027 (6)	0.0009 (6)	0.0049 (6)
C21	0.0142 (8)	0.0081 (7)	0.0080 (7)	0.0014 (6)	0.0021 (6)	−0.0002 (6)
C22	0.0106 (8)	0.0102 (7)	0.0096 (7)	−0.0005 (6)	0.0041 (6)	0.0010 (6)
C23	0.0100 (8)	0.0113 (8)	0.0126 (8)	0.0010 (6)	0.0025 (6)	−0.0042 (6)
C24	0.0099 (8)	0.0144 (8)	0.0096 (7)	0.0002 (6)	0.0027 (6)	−0.0035 (7)
C25	0.0071 (7)	0.0092 (7)	0.0101 (7)	−0.0006 (6)	−0.0021 (6)	−0.0019 (6)
C26	0.0090 (8)	0.0087 (7)	0.0113 (7)	−0.0022 (6)	−0.0004 (6)	−0.0013 (6)
C27	0.0063 (7)	0.0123 (8)	0.0107 (7)	−0.0004 (6)	0.0022 (6)	−0.0013 (6)
C28	0.0064 (7)	0.0101 (7)	0.0099 (7)	0.0010 (6)	0.0012 (6)	−0.0004 (6)

Geometric parameters (Å, º)

Cr1—C1	1.9003 (16)	N2—C22	1.4760 (19)
Cr1—C2	1.9037 (16)	N2—C28	1.4677 (19)
Cr1—C3	1.8987 (16)	C11—C12	1.511 (2)
Cr1—C4	1.8982 (16)	C11—H1A	0.997 (18)
Cr1—C5	1.8495 (16)	C11—H1B	0.954 (18)
Cr1—H	1.73 (2)	C12—H1C	0.986 (18)
Cr2—C6	1.8995 (16)	C12—H1D	1.000 (18)
Cr2—C7	1.8980 (16)	C13—C14	1.497 (2)
Cr2—C8	1.8966 (16)	C13—H1E	0.973 (18)
Cr2—C9	1.9101 (16)	C13—H1F	0.960 (18)
Cr2—C10	1.8468 (16)	C14—H1G	0.975 (18)
Cr2—H	1.70 (2)	C14—H1H	0.976 (17)
K1—O1	2.9710 (11)	C15—C16	1.513 (2)
K1—O11	2.8613 (11)	C15—H1I	0.955 (18)
K1—O12	2.8592 (10)	C15—H1J	0.970 (18)
K1—O13	2.7990 (11)	C16—H1K	0.950 (18)
K1—O14	2.7960 (11)	C16—H1L	0.962 (18)
K1—O15	2.8763 (11)	C17—C18	1.515 (2)
K1—O16	2.8388 (11)	C17—H1M	0.960 (17)
K1—N1	3.0111 (13)	C17—H1N	0.957 (19)
K1—N2	3.0061 (13)	C18—H1O	0.965 (19)
O1—C1	1.1460 (19)	C18—H1P	0.983 (18)
O2—C2	1.1434 (19)	C19—C20	1.501 (2)
O3—C3	1.1464 (19)	C19—H1Q	0.959 (18)
O4—C4	1.1447 (19)	C19—H1R	0.98 (2)
O5—C5	1.1557 (19)	C20—H2A	0.963 (19)
O6—C6	1.1468 (19)	C20—H2B	0.94 (2)
O7—C7	1.1472 (19)	C21—C22	1.508 (2)
O8—C8	1.1491 (19)	C21—H2C	0.982 (19)
O9—C9	1.141 (2)	C21—H2D	0.934 (18)
O10—C10	1.1560 (19)	C22—H2E	1.001 (19)
O11—C12	1.4235 (18)	C22—H2F	0.956 (19)
O11—C13	1.4319 (18)	C23—C24	1.507 (2)
O12—C14	1.4242 (18)	C23—H2G	0.967 (18)
O12—C15	1.4270 (18)	C23—H2H	0.98 (2)
O13—C18	1.4194 (18)	C24—H2I	0.994 (19)
O13—C19	1.4260 (18)	C24—H2J	0.95 (2)
O14—C20	1.4265 (18)	C25—C26	1.502 (2)
O14—C21	1.4346 (18)	C25—H2K	0.961 (18)
O15—C24	1.4326 (18)	C25—H2L	0.983 (18)
O15—C25	1.4204 (18)	C26—H2M	0.946 (19)
O16—C26	1.4282 (18)	C26—H2N	0.968 (19)
O16—C27	1.4261 (18)	C27—C28	1.513 (2)
N1—C11	1.4720 (19)	C27—H2O	0.942 (19)
N1—C17	1.476 (2)	C27—H2P	0.999 (18)
N1—C23	1.4726 (19)	C28—H2Q	0.961 (19)
N2—C16	1.4726 (19)	C28—H2R	0.933 (17)
C2—Cr1—C1	91.94 (6)	H1A—C11—N1	109.9 (10)
C3—Cr1—C1	174.97 (6)	H1A—C11—C12	108.1 (10)
C3—Cr1—C2	92.96 (6)	H1B—C11—N1	108.2 (11)
C4—Cr1—C1	89.75 (6)	H1B—C11—C12	108.8 (11)
C4—Cr1—C2	175.07 (6)	H1B—C11—H1A	107.0 (14)
C4—Cr1—C3	85.28 (6)	C11—C12—O11	110.23 (12)
C5—Cr1—C1	89.90 (6)	H1C—C12—O11	108.5 (10)
C5—Cr1—C2	90.10 (6)	H1C—C12—C11	111.9 (10)
C5—Cr1—C3	91.24 (6)	H1D—C12—O11	110.5 (10)
C5—Cr1—C4	94.54 (6)	H1D—C12—C11	108.2 (10)
H—Cr1—C1	94.8 (7)	H1D—C12—H1C	107.5 (14)
H—Cr1—C2	77.3 (7)	C14—C13—O11	109.54 (12)
H—Cr1—C3	85.1 (7)	H1E—C13—O11	110.9 (10)
H—Cr1—C4	97.9 (7)	H1E—C13—C14	109.8 (10)
H—Cr1—C5	166.7 (7)	H1F—C13—O11	110.5 (10)
C7—Cr2—C6	89.95 (6)	H1F—C13—C14	109.1 (10)
C8—Cr2—C6	176.25 (6)	H1F—C13—H1E	106.9 (14)
C8—Cr2—C7	92.00 (6)	C13—C14—O12	108.65 (12)
C9—Cr2—C6	88.72 (6)	H1G—C14—O12	110.8 (10)
C9—Cr2—C7	171.11 (6)	H1G—C14—C13	107.1 (10)
C9—Cr2—C8	89.84 (6)	H1H—C14—O12	111.2 (9)
C10—Cr2—C6	90.08 (6)	H1H—C14—C13	109.0 (9)
C10—Cr2—C7	93.62 (6)	H1H—C14—H1G	109.9 (14)
C10—Cr2—C8	86.61 (6)	C16—C15—O12	108.58 (12)
C10—Cr2—C9	95.17 (6)	H1I—C15—O12	109.7 (10)
H—Cr2—C6	82.7 (7)	H1I—C15—C16	108.2 (10)
H—Cr2—C7	84.6 (7)	H1J—C15—O12	110.5 (10)
H—Cr2—C8	100.6 (7)	H1J—C15—C16	113.2 (10)
H—Cr2—C9	86.5 (7)	H1J—C15—H1I	106.6 (14)
H—Cr2—C10	172.6 (7)	C15—C16—N2	114.10 (12)
O11—K1—O1	72.00 (3)	H1K—C16—N2	108.2 (10)
O12—K1—O1	65.04 (3)	H1K—C16—C15	107.9 (10)
O12—K1—O11	58.95 (3)	H1L—C16—N2	110.5 (10)
O13—K1—O1	64.12 (3)	H1L—C16—C15	108.8 (10)
O13—K1—O11	104.44 (3)	H1L—C16—H1K	107.1 (14)
O13—K1—O12	129.16 (3)	C18—C17—N1	113.58 (13)
O14—K1—O1	74.55 (3)	H1M—C17—N1	107.8 (10)
O14—K1—O11	146.51 (3)	H1M—C17—C18	106.9 (10)
O14—K1—O12	104.67 (3)	H1N—C17—N1	110.9 (10)
O14—K1—O13	61.26 (3)	H1N—C17—C18	109.4 (10)
O15—K1—O1	147.80 (3)	H1N—C17—H1M	108.1 (14)
O15—K1—O11	99.55 (3)	C17—C18—O13	109.05 (12)
O15—K1—O12	137.79 (3)	H1O—C18—O13	109.0 (11)
O15—K1—O13	89.40 (3)	H1O—C18—C17	108.7 (11)
O15—K1—O14	109.77 (3)	H1P—C18—O13	109.6 (10)
O16—K1—O1	152.21 (3)	H1P—C18—C17	110.6 (10)
O16—K1—O11	119.14 (3)	H1P—C18—H1O	109.8 (14)
O16—K1—O12	97.64 (3)	C20—C19—O13	108.83 (12)
O16—K1—O13	128.61 (3)	H1Q—C19—O13	109.7 (10)
O16—K1—O14	90.39 (3)	H1Q—C19—C20	111.2 (10)
O16—K1—O15	59.19 (3)	H1R—C19—O13	110.5 (11)
N1—K1—O1	90.41 (3)	H1R—C19—C20	107.5 (12)
N1—K1—O11	62.06 (3)	H1R—C19—H1Q	109.2 (15)
N1—K1—O12	120.46 (3)	C19—C20—O14	109.74 (13)
N1—K1—O13	60.31 (3)	H2A—C20—O14	110.5 (10)
N1—K1—O14	120.36 (3)	H2A—C20—C19	109.1 (10)
N1—K1—O15	59.31 (3)	H2B—C20—O14	109.7 (12)
N1—K1—O16	117.39 (3)	H2B—C20—C19	109.2 (12)
N2—K1—O1	91.98 (3)	H2B—C20—H2A	108.7 (15)
N2—K1—O11	117.24 (3)	C22—C21—O14	109.21 (12)
N2—K1—O12	59.32 (3)	H2C—C21—O14	109.5 (10)
N2—K1—O13	122.29 (3)	H2C—C21—C22	110.4 (10)
N2—K1—O14	61.93 (3)	H2D—C21—O14	110.0 (11)
N2—K1—O15	118.65 (3)	H2D—C21—C22	111.5 (11)
N2—K1—O16	60.23 (3)	H2D—C21—H2C	106.1 (14)
N2—K1—N1	177.12 (3)	C21—C22—N2	113.14 (13)
C1—O1—K1	148.71 (10)	H2E—C22—N2	110.4 (10)
C12—O11—K1	111.65 (8)	H2E—C22—C21	107.6 (10)
C13—O11—K1	113.89 (8)	H2F—C22—N2	109.5 (11)
C13—O11—C12	110.12 (11)	H2F—C22—C21	106.9 (10)
C14—O12—K1	117.65 (8)	H2F—C22—H2E	109.1 (15)
C15—O12—K1	121.14 (8)	C24—C23—N1	113.41 (13)
C15—O12—C14	111.60 (11)	H2G—C23—N1	107.3 (10)
C18—O13—K1	121.12 (8)	H2G—C23—C24	108.8 (10)
C19—O13—K1	113.64 (8)	H2H—C23—N1	111.6 (11)
C19—O13—C18	111.78 (11)	H2H—C23—C24	109.2 (11)
C20—O14—K1	113.71 (8)	H2H—C23—H2G	106.2 (15)
C21—O14—K1	112.09 (8)	C23—C24—O15	108.48 (12)
C21—O14—C20	110.51 (11)	H2I—C24—O15	109.6 (10)
C24—O15—K1	115.64 (8)	H2I—C24—C23	113.8 (10)
C25—O15—K1	117.11 (8)	H2J—C24—O15	110.3 (11)
C25—O15—C24	111.15 (11)	H2J—C24—C23	109.2 (11)
C26—O16—K1	112.77 (8)	H2J—C24—H2I	105.4 (15)
C27—O16—K1	120.13 (8)	C26—C25—O15	109.14 (12)
C27—O16—C26	110.36 (11)	H2K—C25—O15	111.1 (10)
C11—N1—K1	107.38 (8)	H2K—C25—C26	108.5 (10)
C17—N1—K1	107.46 (9)	H2L—C25—O15	110.6 (10)
C17—N1—C11	109.88 (12)	H2L—C25—C26	109.9 (10)
C23—N1—K1	112.27 (9)	H2L—C25—H2K	107.6 (14)
C23—N1—C11	109.23 (12)	C25—C26—O16	109.30 (12)
C23—N1—C17	110.55 (12)	H2M—C26—O16	109.3 (11)
C16—N2—K1	110.00 (9)	H2M—C26—C25	112.3 (11)
C22—N2—K1	107.76 (9)	H2N—C26—O16	110.8 (11)
C22—N2—C16	109.38 (12)	H2N—C26—C25	107.3 (10)
C28—N2—K1	108.88 (8)	H2N—C26—H2M	107.8 (15)
C28—N2—C16	109.65 (12)	C28—C27—O16	110.34 (12)
C28—N2—C22	111.14 (12)	H2O—C27—O16	110.3 (11)
O1—C1—Cr1	177.16 (13)	H2O—C27—C28	110.7 (11)
O2—C2—Cr1	178.84 (13)	H2P—C27—O16	108.2 (10)
O3—C3—Cr1	175.86 (13)	H2P—C27—C28	108.5 (10)
O4—C4—Cr1	177.78 (13)	H2P—C27—H2O	108.7 (14)
O5—C5—Cr1	177.73 (13)	C27—C28—N2	114.14 (12)
O6—C6—Cr2	178.94 (13)	H2Q—C28—N2	111.1 (11)
O7—C7—Cr2	178.60 (13)	H2Q—C28—C27	109.1 (11)
O8—C8—Cr2	174.78 (13)	H2R—C28—N2	108.9 (10)
O9—C9—Cr2	178.60 (13)	H2R—C28—C27	109.2 (10)
O10—C10—Cr2	177.86 (13)	H2R—C28—H2Q	103.8 (14)
C12—C11—N1	114.64 (12)	Cr2—H—Cr1	148.9 (14)
K1—O11—C12—C11	−56.05 (8)	K1—N1—C23—C24	−37.62 (9)
K1—O11—C13—C14	53.32 (9)	K1—N2—C16—C15	−48.40 (9)
K1—O12—C14—C13	42.44 (9)	K1—N2—C22—C21	−39.32 (9)
K1—O12—C15—C16	−41.11 (9)	K1—N2—C28—C27	−48.55 (9)
K1—O13—C18—C17	−41.04 (9)	O11—C12—C11—N1	69.64 (13)
K1—O13—C19—C20	49.50 (9)	O11—C13—C14—O12	−63.37 (12)
K1—O14—C20—C19	48.08 (9)	O12—C15—C16—N2	60.44 (13)
K1—O14—C21—C22	−59.80 (9)	O13—C18—C17—N1	62.47 (13)
K1—O15—C24—C23	−56.18 (9)	O13—C19—C20—O14	−66.07 (13)
K1—O15—C25—C26	38.02 (9)	O14—C21—C22—N2	69.46 (13)
K1—O16—C26—C25	57.51 (9)	O15—C24—C23—N1	63.16 (13)
K1—O16—C27—C28	−39.19 (9)	O15—C25—C26—O16	−63.71 (12)
K1—N1—C11—C12	−41.26 (9)	O16—C27—C28—N2	60.37 (13)
K1—N1—C17—C18	−49.94 (9)

(KCPTCR_standard_IAM_NoMoRe)

Crystal data

C28H37Cr2KN2O16	F(000) = 1660.538
Mr = 800.70	Dx = 1.489 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71069 Å
a = 10.458 Å	Cell parameters from 1024 reflections
b = 14.417 Å	θ = 47.5–1.5°
c = 23.882 Å	µ = 0.80 mm^−1
β = 97.26°	T = 28 K
V = 3571.89 Å^3	Ellipsoidal, yellow
Z = 4	0.3 × 0.25 × 0.2 mm

Data collection

SMART CCD diffractometer	5667 reflections with I ≥ 2u(I)
ω scan	Rint = 0.0000
Absorption correction: empirical (using intensity measurements)	θmax = 25.0°, θmin = 2.4°
Tmin = 0.890, Tmax = 0.903	h = −19→20
27917 measured reflections	k = 0→30
5993 independent reflections	l = 0→50

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.023	Only H-atom coordinates refined
wR(F^2) = 0.059	w = 1/[σ^2(Fo^2) + (0.0272P)^2 + 2.8766P] where P = (Fo^2 + 2Fc^2)/3
S = 1.05	(Δ/σ)max = 0.001
5993 reflections	Δρmax = 0.30 e Å^−3
553 parameters	Δρmin = −0.39 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Cr1	0.16384 (2)	0.002377 (16)	0.236357 (10)	0.00608 (7)
Cr2	0.01879 (2)	0.177439 (17)	0.165112 (10)	0.00660 (7)
K1	0.46375 (3)	0.19929 (2)	0.418017 (13)	0.00722 (8)
O1	0.25191 (11)	0.13806 (8)	0.33116 (5)	0.0123 (2)
O2	−0.08331 (11)	−0.04366 (8)	0.28579 (5)	0.0144 (3)
O3	0.10484 (11)	−0.12657 (8)	0.13552 (5)	0.0129 (2)
O4	0.39527 (11)	0.05452 (8)	0.17751 (5)	0.0139 (2)
O5	0.30030 (11)	−0.15022 (8)	0.30578 (5)	0.0128 (2)
O6	−0.25963 (11)	0.12160 (8)	0.17226 (5)	0.0127 (2)
O7	0.01683 (11)	0.05861 (8)	0.05960 (5)	0.0127 (2)
O8	0.28633 (11)	0.25365 (8)	0.15524 (5)	0.0134 (2)
O9	0.02666 (12)	0.26549 (8)	0.28167 (5)	0.0177 (3)
O10	−0.07190 (11)	0.34753 (8)	0.09920 (5)	0.0147 (3)
O11	0.28613 (10)	0.09227 (7)	0.47318 (5)	0.0086 (2)
O12	0.44335 (10)	0.00301 (7)	0.40241 (5)	0.0089 (2)
O13	0.31323 (10)	0.34066 (7)	0.36302 (5)	0.0095 (2)
O14	0.52834 (11)	0.26689 (7)	0.31550 (5)	0.0098 (2)
O15	0.55079 (10)	0.32677 (8)	0.50740 (5)	0.0103 (2)
O16	0.72690 (10)	0.20500 (7)	0.46503 (5)	0.0090 (2)
N1	0.27341 (12)	0.30187 (9)	0.47975 (5)	0.0086 (3)
N2	0.66148 (12)	0.09476 (9)	0.36202 (5)	0.0082 (3)
C1	0.21619 (15)	0.08851 (11)	0.29503 (7)	0.0088 (3)
C2	0.01022 (16)	−0.02688 (11)	0.26769 (6)	0.0094 (3)
C3	0.12291 (15)	−0.07915 (11)	0.17424 (7)	0.0094 (3)
C4	0.30799 (15)	0.03673 (11)	0.20000 (7)	0.0098 (3)
C5	0.25013 (15)	−0.09112 (11)	0.27864 (6)	0.0088 (3)
C6	−0.15439 (16)	0.14191 (11)	0.16988 (6)	0.0095 (3)
C7	0.01874 (15)	0.10408 (11)	0.09912 (7)	0.0090 (3)
C8	0.18804 (16)	0.22111 (11)	0.16009 (6)	0.0101 (3)
C9	0.02395 (16)	0.23364 (11)	0.23779 (7)	0.0119 (3)
C10	−0.03868 (15)	0.28243 (11)	0.12528 (7)	0.0103 (3)
C11	0.20808 (16)	0.23279 (11)	0.51156 (7)	0.0100 (3)
C12	0.17289 (15)	0.14373 (11)	0.47995 (7)	0.0096 (3)
C13	0.25211 (16)	0.00531 (11)	0.44637 (7)	0.0092 (3)
C14	0.37204 (15)	−0.04779 (11)	0.43918 (7)	0.0091 (3)
C15	0.54835 (15)	−0.05003 (11)	0.38666 (7)	0.0088 (3)
C16	0.60993 (16)	0.00362 (11)	0.34261 (7)	0.0090 (3)
C17	0.17911 (16)	0.34654 (11)	0.43694 (7)	0.0105 (3)
C18	0.24062 (16)	0.40169 (11)	0.39337 (7)	0.0108 (3)
C19	0.37510 (16)	0.38878 (11)	0.32172 (7)	0.0119 (3)
C20	0.42783 (16)	0.31899 (12)	0.28397 (7)	0.0116 (3)
C21	0.57248 (16)	0.19470 (11)	0.28131 (7)	0.0102 (3)
C22	0.69034 (16)	0.14960 (11)	0.31296 (7)	0.0100 (3)
C23	0.33614 (16)	0.37143 (11)	0.51922 (7)	0.0113 (3)
C24	0.46486 (16)	0.34036 (12)	0.54889 (7)	0.0114 (3)
C25	0.68023 (15)	0.31745 (11)	0.53318 (7)	0.0093 (3)
C26	0.76444 (16)	0.29331 (11)	0.48875 (7)	0.0099 (3)
C27	0.82399 (15)	0.16959 (11)	0.43393 (7)	0.0098 (3)
C28	0.77739 (15)	0.08200 (11)	0.40286 (7)	0.0089 (3)
H	0.052 (2)	0.0762 (16)	0.1999 (10)	0.033652
H1A	0.127 (2)	0.2600 (15)	0.5230 (9)	0.025013
H1B	0.263 (2)	0.2186 (15)	0.5456 (9)	0.023076
H1C	0.125 (2)	0.1554 (15)	0.4421 (9)	0.023746
H1D	0.114 (2)	0.1069 (15)	0.5022 (9)	0.024598
H1E	0.201 (2)	0.0143 (15)	0.4093 (9)	0.022215
H1F	0.200 (2)	−0.0309 (15)	0.4688 (9)	0.023329
H1G	0.344 (2)	−0.1086 (15)	0.4227 (9)	0.025071
H1H	0.423 (2)	−0.0564 (15)	0.4767 (9)	0.024233
H1I	0.517 (2)	−0.1079 (15)	0.3703 (9)	0.022451
H1J	0.609 (2)	−0.0658 (15)	0.4202 (9)	0.021710
H1K	0.546 (2)	0.0131 (14)	0.3108 (9)	0.022322
H1L	0.677 (2)	−0.0343 (15)	0.3295 (9)	0.023001
H1M	0.128 (2)	0.2980 (16)	0.4167 (9)	0.024511
H1N	0.121 (2)	0.3860 (16)	0.4543 (9)	0.026678
H1O	0.173 (2)	0.4296 (16)	0.3674 (9)	0.027525
H1P	0.298 (2)	0.4507 (15)	0.4121 (9)	0.026323
H1Q	0.442 (2)	0.4276 (16)	0.3403 (10)	0.027823
H1R	0.312 (2)	0.4275 (16)	0.2977 (9)	0.029725
H2A	0.359 (2)	0.2783 (16)	0.2681 (9)	0.026016
H2B	0.461 (2)	0.3509 (16)	0.2541 (9)	0.028356
H2C	0.593 (2)	0.2213 (15)	0.2452 (9)	0.025505
H2D	0.506 (2)	0.1513 (15)	0.2716 (9)	0.024538
H2E	0.730 (2)	0.1091 (15)	0.2855 (9)	0.025760
H2F	0.749 (2)	0.1987 (15)	0.3256 (9)	0.024185
H2G	0.349 (2)	0.4270 (15)	0.4973 (9)	0.025234
H2H	0.281 (2)	0.3895 (15)	0.5478 (9)	0.026839
H2I	0.461 (2)	0.2826 (16)	0.5716 (9)	0.026520
H2J	0.497 (2)	0.3875 (16)	0.5756 (9)	0.027507
H2K	0.711 (2)	0.3747 (15)	0.5511 (9)	0.024028
H2L	0.687 (2)	0.2688 (15)	0.5626 (9)	0.023835
H2M	0.760 (2)	0.3387 (15)	0.4593 (9)	0.025301
H2N	0.854 (2)	0.2913 (16)	0.5072 (9)	0.026087
H2O	0.848 (2)	0.2153 (16)	0.4082 (9)	0.025953
H2P	0.902 (2)	0.1537 (16)	0.4613 (10)	0.027682
H2Q	0.847 (2)	0.0557 (15)	0.3850 (9)	0.024815
H2R	0.760 (2)	0.0363 (15)	0.4293 (9)	0.022425

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cr1	0.00645 (13)	0.00545 (12)	0.00629 (13)	−0.00004 (9)	0.00061 (9)	−0.00025 (9)
Cr2	0.00752 (13)	0.00614 (12)	0.00596 (13)	0.00072 (9)	0.00016 (9)	0.00003 (9)
K1	0.00675 (16)	0.00730 (16)	0.00749 (16)	0.00030 (12)	0.00044 (12)	−0.00006 (12)
O1	0.0150 (6)	0.0099 (5)	0.0111 (6)	0.0001 (5)	−0.0024 (5)	−0.0012 (5)
O2	0.0115 (6)	0.0159 (6)	0.0168 (6)	0.0005 (5)	0.0054 (5)	0.0010 (5)
O3	0.0143 (6)	0.0130 (6)	0.0114 (6)	−0.0022 (5)	0.0017 (5)	−0.0039 (5)
O4	0.0118 (6)	0.0135 (6)	0.0175 (6)	−0.0006 (5)	0.0056 (5)	−0.0004 (5)
O5	0.0136 (6)	0.0103 (6)	0.0141 (6)	0.0027 (5)	−0.0005 (5)	0.0015 (5)
O6	0.0114 (6)	0.0149 (6)	0.0124 (6)	−0.0007 (5)	0.0034 (5)	0.0006 (5)
O7	0.0162 (6)	0.0127 (6)	0.0094 (6)	−0.0021 (5)	0.0022 (5)	−0.0025 (5)
O8	0.0123 (6)	0.0153 (6)	0.0123 (6)	−0.0039 (5)	0.0005 (5)	0.0010 (5)
O9	0.0251 (7)	0.0173 (6)	0.0098 (6)	0.0094 (5)	−0.0016 (5)	−0.0043 (5)
O10	0.0179 (6)	0.0099 (6)	0.0154 (6)	0.0027 (5)	−0.0017 (5)	0.0036 (5)
O11	0.0061 (5)	0.0074 (5)	0.0120 (5)	0.0003 (4)	0.0004 (4)	−0.0020 (4)
O12	0.0091 (5)	0.0071 (5)	0.0114 (5)	0.0011 (4)	0.0047 (4)	0.0019 (4)
O13	0.0107 (6)	0.0074 (5)	0.0109 (5)	0.0014 (4)	0.0036 (4)	0.0011 (4)
O14	0.0110 (6)	0.0097 (5)	0.0084 (5)	0.0031 (4)	0.0002 (4)	0.0000 (4)
O15	0.0073 (6)	0.0148 (6)	0.0086 (5)	0.0011 (4)	0.0007 (4)	−0.0020 (4)
O16	0.0065 (5)	0.0089 (5)	0.0118 (5)	−0.0011 (4)	0.0017 (4)	−0.0040 (4)
N1	0.0076 (6)	0.0084 (6)	0.0095 (6)	0.0003 (5)	−0.0003 (5)	−0.0001 (5)
N2	0.0087 (7)	0.0078 (6)	0.0081 (6)	−0.0010 (5)	0.0007 (5)	0.0005 (5)
C1	0.0071 (7)	0.0085 (7)	0.0111 (8)	0.0023 (6)	0.0022 (6)	0.0045 (6)
C2	0.0130 (8)	0.0067 (7)	0.0078 (7)	0.0021 (6)	−0.0018 (6)	−0.0005 (6)
C3	0.0053 (7)	0.0094 (7)	0.0136 (8)	0.0008 (6)	0.0021 (6)	0.0038 (7)
C4	0.0118 (8)	0.0066 (7)	0.0100 (8)	0.0017 (6)	−0.0026 (6)	−0.0017 (6)
C5	0.0077 (7)	0.0104 (8)	0.0088 (7)	−0.0026 (6)	0.0025 (6)	−0.0043 (6)
C6	0.0160 (9)	0.0075 (7)	0.0047 (7)	0.0035 (6)	0.0002 (6)	0.0004 (6)
C7	0.0056 (7)	0.0091 (7)	0.0124 (8)	−0.0004 (6)	0.0008 (6)	0.0053 (7)
C8	0.0158 (9)	0.0084 (7)	0.0053 (7)	0.0025 (7)	−0.0016 (6)	−0.0010 (6)
C9	0.0108 (8)	0.0095 (8)	0.0146 (9)	0.0041 (6)	−0.0009 (6)	0.0035 (7)
C10	0.0090 (8)	0.0117 (8)	0.0102 (8)	−0.0011 (6)	0.0011 (6)	−0.0045 (6)
C11	0.0101 (8)	0.0115 (8)	0.0088 (8)	0.0025 (6)	0.0025 (6)	0.0013 (6)
C12	0.0064 (8)	0.0110 (8)	0.0115 (8)	0.0017 (6)	0.0012 (6)	0.0013 (6)
C13	0.0103 (8)	0.0077 (7)	0.0094 (8)	−0.0034 (6)	0.0007 (6)	−0.0010 (6)
C14	0.0107 (8)	0.0078 (8)	0.0088 (8)	−0.0019 (6)	0.0019 (6)	0.0014 (6)
C15	0.0083 (8)	0.0071 (7)	0.0108 (8)	0.0023 (6)	0.0008 (6)	−0.0007 (6)
C16	0.0101 (8)	0.0089 (7)	0.0080 (8)	0.0002 (6)	0.0009 (6)	−0.0020 (6)
C17	0.0085 (8)	0.0099 (8)	0.0132 (8)	0.0031 (6)	0.0015 (6)	0.0013 (6)
C18	0.0112 (8)	0.0082 (7)	0.0133 (8)	0.0030 (6)	0.0021 (7)	0.0008 (6)
C19	0.0131 (8)	0.0094 (8)	0.0135 (8)	0.0013 (7)	0.0035 (7)	0.0045 (7)
C20	0.0121 (8)	0.0135 (8)	0.0090 (8)	0.0032 (7)	0.0006 (6)	0.0048 (6)
C21	0.0145 (8)	0.0082 (8)	0.0081 (8)	0.0019 (6)	0.0020 (6)	−0.0003 (6)
C22	0.0103 (8)	0.0106 (8)	0.0098 (8)	−0.0003 (7)	0.0040 (6)	0.0012 (6)
C23	0.0100 (8)	0.0113 (8)	0.0128 (8)	0.0011 (6)	0.0022 (6)	−0.0043 (7)
C24	0.0097 (8)	0.0153 (8)	0.0096 (8)	0.0004 (6)	0.0026 (6)	−0.0033 (7)
C25	0.0070 (8)	0.0099 (8)	0.0101 (8)	−0.0004 (6)	−0.0019 (6)	−0.0019 (6)
C26	0.0093 (8)	0.0087 (8)	0.0114 (8)	−0.0023 (6)	0.0001 (6)	−0.0017 (6)
C27	0.0063 (8)	0.0124 (8)	0.0111 (8)	−0.0006 (6)	0.0024 (6)	−0.0017 (6)
C28	0.0063 (8)	0.0102 (8)	0.0103 (8)	0.0011 (6)	0.0008 (6)	−0.0006 (6)
H	0.027000	0.026000	0.046000	0.004000	−0.003000	0.018000
H1A	0.023000	0.023000	0.032000	0.005000	0.015000	−0.000000
H1B	0.028000	0.024000	0.016000	0.000000	−0.002000	0.003000
H1C	0.022000	0.026000	0.021000	0.004000	−0.006000	0.001000
H1D	0.021000	0.022000	0.033000	−0.003000	0.012000	0.003000
H1E	0.022000	0.027000	0.016000	0.000000	−0.004000	−0.001000
H1F	0.026000	0.022000	0.024000	−0.009000	0.011000	−0.000000
H1G	0.033000	0.013000	0.031000	−0.006000	0.011000	−0.005000
H1H	0.026000	0.029000	0.017000	0.005000	0.000000	0.007000
H1I	0.027000	0.013000	0.028000	−0.003000	0.006000	−0.005000
H1J	0.019000	0.026000	0.019000	0.004000	−0.002000	0.006000
H1K	0.025000	0.023000	0.017000	−0.002000	−0.005000	0.001000
H1L	0.024000	0.020000	0.027000	0.004000	0.011000	−0.005000
H1M	0.021000	0.025000	0.026000	−0.006000	−0.003000	0.004000
H1N	0.025000	0.029000	0.028000	0.013000	0.011000	0.005000
H1O	0.025000	0.030000	0.028000	0.013000	0.005000	0.012000
H1P	0.034000	0.017000	0.029000	−0.006000	0.008000	−0.005000
H1Q	0.028000	0.021000	0.036000	−0.009000	0.010000	−0.005000
H1R	0.032000	0.030000	0.028000	0.016000	0.007000	0.014000
H2A	0.021000	0.029000	0.026000	−0.002000	−0.005000	−0.005000
H2B	0.035000	0.032000	0.020000	0.009000	0.011000	0.012000
H2C	0.036000	0.027000	0.015000	0.006000	0.009000	0.006000
H2D	0.024000	0.020000	0.028000	−0.004000	−0.003000	−0.004000
H2E	0.032000	0.026000	0.022000	0.010000	0.014000	0.001000
H2F	0.021000	0.022000	0.029000	−0.007000	0.001000	0.004000
H2G	0.028000	0.016000	0.031000	−0.002000	0.001000	0.003000
H2H	0.024000	0.031000	0.027000	0.003000	0.009000	−0.011000
H2I	0.027000	0.028000	0.025000	0.002000	0.005000	0.010000
H2J	0.026000	0.034000	0.022000	−0.002000	0.001000	−0.014000
H2K	0.025000	0.020000	0.026000	−0.003000	−0.001000	−0.010000
H2L	0.028000	0.024000	0.019000	0.003000	0.001000	0.007000
H2M	0.035000	0.018000	0.024000	−0.002000	0.008000	0.004000
H2N	0.014000	0.031000	0.032000	−0.002000	−0.002000	−0.010000
H2O	0.031000	0.022000	0.027000	−0.007000	0.012000	−0.000000
H2P	0.014000	0.034000	0.033000	0.004000	−0.005000	−0.009000
H2Q	0.017000	0.030000	0.028000	0.006000	0.005000	−0.008000
H2R	0.027000	0.019000	0.020000	−0.002000	−0.002000	0.005000

Geometric parameters (Å, º)

Cr1—C1	1.9004 (16)	N2—C22	1.476 (2)
Cr1—C2	1.9033 (17)	N2—C28	1.468 (2)
Cr1—C3	1.8987 (17)	C11—C12	1.511 (2)
Cr1—C4	1.8982 (17)	C11—H1A	1.00 (2)
Cr1—C5	1.8495 (16)	C11—H1B	0.96 (2)
Cr1—H	1.73 (2)	C12—H1C	0.99 (2)
Cr2—C6	1.8994 (17)	C12—H1D	1.01 (2)
Cr2—C7	1.8979 (17)	C13—C14	1.498 (2)
Cr2—C8	1.8967 (17)	C13—H1E	0.98 (2)
Cr2—C9	1.9100 (17)	C13—H1F	0.97 (2)
Cr2—C10	1.8474 (17)	C14—H1G	0.99 (2)
Cr2—H	1.69 (2)	C14—H1H	0.99 (2)
K1—O1	2.9713 (12)	C15—C16	1.514 (2)
K1—O11	2.8610 (11)	C15—H1I	0.96 (2)
K1—O12	2.8587 (11)	C15—H1J	0.98 (2)
K1—O13	2.7990 (11)	C16—H1K	0.96 (2)
K1—O14	2.7960 (11)	C16—H1L	0.97 (2)
K1—O15	2.8761 (11)	C17—C18	1.516 (2)
K1—O16	2.8390 (11)	C17—H1M	0.97 (2)
K1—N1	3.0108 (13)	C17—H1N	0.96 (2)
K1—N2	3.0058 (13)	C18—H1O	0.97 (2)
O1—C1	1.146 (2)	C18—H1P	1.00 (2)
O2—C2	1.144 (2)	C19—C20	1.502 (2)
O3—C3	1.146 (2)	C19—H1Q	0.96 (2)
O4—C4	1.145 (2)	C19—H1R	0.99 (2)
O5—C5	1.156 (2)	C20—H2A	0.97 (2)
O6—C6	1.147 (2)	C20—H2B	0.95 (2)
O7—C7	1.147 (2)	C21—C22	1.509 (2)
O8—C8	1.149 (2)	C21—H2C	0.99 (2)
O9—C9	1.141 (2)	C21—H2D	0.94 (2)
O10—C10	1.155 (2)	C22—H2E	1.01 (2)
O11—C12	1.4239 (19)	C22—H2F	0.96 (2)
O11—C13	1.4320 (19)	C23—C24	1.508 (2)
O12—C14	1.4244 (18)	C23—H2G	0.98 (2)
O12—C15	1.4270 (19)	C23—H2H	0.99 (2)
O13—C18	1.4196 (19)	C24—H2I	1.00 (2)
O13—C19	1.4262 (19)	C24—H2J	0.96 (2)
O14—C20	1.4270 (19)	C25—C26	1.503 (2)
O14—C21	1.4347 (19)	C25—H2K	0.97 (2)
O15—C24	1.4328 (19)	C25—H2L	0.99 (2)
O15—C25	1.4208 (19)	C26—H2M	0.96 (2)
O16—C26	1.4281 (19)	C26—H2N	0.98 (2)
O16—C27	1.4262 (19)	C27—C28	1.514 (2)
N1—C11	1.472 (2)	C27—H2O	0.96 (2)
N1—C17	1.476 (2)	C27—H2P	1.01 (2)
N1—C23	1.472 (2)	C28—H2Q	0.96 (2)
N2—C16	1.473 (2)	C28—H2R	0.94 (2)
C2—Cr1—C1	91.94 (7)	H1A—C11—N1	109.9 (12)
C3—Cr1—C1	174.96 (7)	H1A—C11—C12	107.8 (13)
C3—Cr1—C2	92.97 (7)	H1B—C11—N1	108.4 (13)
C4—Cr1—C1	89.74 (6)	H1B—C11—C12	109.0 (13)
C4—Cr1—C2	175.08 (7)	H1B—C11—H1A	106.9 (18)
C4—Cr1—C3	85.28 (6)	C11—C12—O11	110.24 (13)
C5—Cr1—C1	89.91 (7)	H1C—C12—O11	108.3 (13)
C5—Cr1—C2	90.10 (7)	H1C—C12—C11	112.0 (13)
C5—Cr1—C3	91.24 (7)	H1D—C12—O11	110.8 (12)
C5—Cr1—C4	94.53 (7)	H1D—C12—C11	108.0 (12)
H—Cr1—C1	94.7 (8)	H1D—C12—H1C	107.5 (18)
H—Cr1—C2	77.6 (8)	C14—C13—O11	109.54 (13)
H—Cr1—C3	85.2 (8)	H1E—C13—O11	111.3 (13)
H—Cr1—C4	97.6 (8)	H1E—C13—C14	109.5 (12)
H—Cr1—C5	167.0 (7)	H1F—C13—O11	110.5 (13)
C7—Cr2—C6	89.96 (6)	H1F—C13—C14	109.3 (13)
C8—Cr2—C6	176.25 (7)	H1F—C13—H1E	106.6 (18)
C8—Cr2—C7	91.99 (7)	C13—C14—O12	108.61 (12)
C9—Cr2—C6	88.72 (7)	H1G—C14—O12	111.1 (12)
C9—Cr2—C7	171.10 (7)	H1G—C14—C13	106.9 (13)
C9—Cr2—C8	89.84 (7)	H1H—C14—O12	111.1 (12)
C10—Cr2—C6	90.07 (7)	H1H—C14—C13	108.8 (12)
C10—Cr2—C7	93.61 (7)	H1H—C14—H1G	110.3 (18)
C10—Cr2—C8	86.62 (7)	C16—C15—O12	108.57 (12)
C10—Cr2—C9	95.18 (7)	H1I—C15—O12	109.8 (13)
H—Cr2—C6	83.0 (8)	H1I—C15—C16	108.3 (13)
H—Cr2—C7	84.6 (8)	H1J—C15—O12	110.4 (12)
H—Cr2—C8	100.4 (8)	H1J—C15—C16	113.4 (12)
H—Cr2—C9	86.5 (8)	H1J—C15—H1I	106.3 (18)
H—Cr2—C10	172.8 (8)	C15—C16—N2	114.09 (13)
O11—K1—O1	72.00 (3)	H1K—C16—N2	108.3 (13)
O12—K1—O1	65.05 (3)	H1K—C16—C15	107.8 (13)
O12—K1—O11	58.94 (3)	H1L—C16—N2	110.7 (13)
O13—K1—O1	64.10 (3)	H1L—C16—C15	108.9 (13)
O13—K1—O11	104.44 (3)	H1L—C16—H1K	106.7 (18)
O13—K1—O12	129.15 (3)	C18—C17—N1	113.58 (13)
O14—K1—O1	74.55 (3)	H1M—C17—N1	107.9 (13)
O14—K1—O11	146.50 (3)	H1M—C17—C18	106.9 (13)
O14—K1—O12	104.66 (3)	H1N—C17—N1	111.3 (13)
O14—K1—O13	61.26 (3)	H1N—C17—C18	109.3 (13)
O15—K1—O1	147.79 (3)	H1N—C17—H1M	107.7 (19)
O15—K1—O11	99.55 (3)	C17—C18—O13	109.04 (13)
O15—K1—O12	137.79 (3)	H1O—C18—O13	108.9 (13)
O15—K1—O13	89.40 (3)	H1O—C18—C17	108.7 (13)
O15—K1—O14	109.78 (3)	H1P—C18—O13	109.6 (13)
O16—K1—O1	152.21 (3)	H1P—C18—C17	110.4 (13)
O16—K1—O11	119.13 (3)	H1P—C18—H1O	110.1 (19)
O16—K1—O12	97.64 (3)	C20—C19—O13	108.81 (13)
O16—K1—O13	128.61 (3)	H1Q—C19—O13	109.4 (13)
O16—K1—O14	90.39 (3)	H1Q—C19—C20	111.4 (13)
O16—K1—O15	59.19 (3)	H1R—C19—O13	110.3 (13)
N1—K1—O1	90.40 (3)	H1R—C19—C20	107.4 (13)
N1—K1—O11	62.06 (3)	H1R—C19—H1Q	109.5 (19)
N1—K1—O12	120.46 (3)	C19—C20—O14	109.74 (13)
N1—K1—O13	60.31 (3)	H2A—C20—O14	110.5 (13)
N1—K1—O14	120.36 (3)	H2A—C20—C19	109.3 (13)
N1—K1—O15	59.30 (3)	H2B—C20—O14	109.7 (13)
N1—K1—O16	117.38 (3)	H2B—C20—C19	108.9 (14)
N2—K1—O1	91.98 (3)	H2B—C20—H2A	108.8 (19)
N2—K1—O11	117.24 (3)	C22—C21—O14	109.18 (13)
N2—K1—O12	59.33 (3)	H2C—C21—O14	109.5 (13)
N2—K1—O13	122.28 (3)	H2C—C21—C22	110.7 (13)
N2—K1—O14	61.92 (3)	H2D—C21—O14	110.1 (13)
N2—K1—O15	118.66 (3)	H2D—C21—C22	111.5 (13)
N2—K1—O16	60.23 (3)	H2D—C21—H2C	105.9 (18)
N2—K1—N1	177.12 (4)	C21—C22—N2	113.10 (13)
C1—O1—K1	148.68 (11)	H2E—C22—N2	110.5 (12)
C12—O11—K1	111.65 (8)	H2E—C22—C21	107.7 (12)
C13—O11—K1	113.91 (8)	H2F—C22—N2	109.4 (13)
C13—O11—C12	110.11 (12)	H2F—C22—C21	106.9 (13)
C14—O12—K1	117.70 (8)	H2F—C22—H2E	109.2 (18)
C15—O12—K1	121.17 (9)	C24—C23—N1	113.43 (13)
C15—O12—C14	111.54 (11)	H2G—C23—N1	107.2 (13)
C18—O13—K1	121.14 (9)	H2G—C23—C24	108.7 (13)
C19—O13—K1	113.66 (9)	H2H—C23—N1	111.7 (13)
C19—O13—C18	111.74 (12)	H2H—C23—C24	108.8 (13)
C20—O14—K1	113.72 (9)	H2H—C23—H2G	106.7 (18)
C21—O14—K1	112.11 (9)	C23—C24—O15	108.44 (13)
C21—O14—C20	110.48 (12)	H2I—C24—O15	109.5 (13)
C24—O15—K1	115.68 (9)	H2I—C24—C23	114.1 (13)
C25—O15—K1	117.13 (9)	H2J—C24—O15	110.7 (13)
C25—O15—C24	111.09 (12)	H2J—C24—C23	108.8 (13)
C26—O16—K1	112.76 (9)	H2J—C24—H2I	105.3 (18)
C27—O16—K1	120.13 (9)	C26—C25—O15	109.10 (13)
C27—O16—C26	110.34 (12)	H2K—C25—O15	111.0 (13)
C11—N1—K1	107.40 (9)	H2K—C25—C26	108.5 (13)
C17—N1—K1	107.48 (9)	H2L—C25—O15	111.0 (13)
C17—N1—C11	109.85 (12)	H2L—C25—C26	109.8 (13)
C23—N1—K1	112.29 (9)	H2L—C25—H2K	107.4 (18)
C23—N1—C11	109.20 (12)	C25—C26—O16	109.29 (13)
C23—N1—C17	110.55 (12)	H2M—C26—O16	109.3 (13)
C16—N2—K1	110.02 (9)	H2M—C26—C25	112.4 (13)
C22—N2—K1	107.81 (9)	H2N—C26—O16	110.5 (13)
C22—N2—C16	109.37 (12)	H2N—C26—C25	107.4 (13)
C28—N2—K1	108.90 (9)	H2N—C26—H2M	107.9 (19)
C28—N2—C16	109.63 (12)	C28—C27—O16	110.34 (13)
C28—N2—C22	111.10 (12)	H2O—C27—O16	110.4 (13)
O1—C1—Cr1	177.18 (13)	H2O—C27—C28	110.7 (13)
O2—C2—Cr1	178.83 (14)	H2P—C27—O16	108.4 (13)
O3—C3—Cr1	175.87 (13)	H2P—C27—C28	108.3 (13)
O4—C4—Cr1	177.78 (13)	H2P—C27—H2O	108.6 (19)
O5—C5—Cr1	177.73 (13)	C27—C28—N2	114.12 (13)
O6—C6—Cr2	178.94 (13)	H2Q—C28—N2	111.0 (13)
O7—C7—Cr2	178.61 (13)	H2Q—C28—C27	109.4 (13)
O8—C8—Cr2	174.75 (14)	H2R—C28—N2	108.8 (13)
O9—C9—Cr2	178.60 (14)	H2R—C28—C27	109.3 (13)
O10—C10—Cr2	177.87 (14)	H2R—C28—H2Q	103.7 (18)
C12—C11—N1	114.63 (13)	Cr2—H—Cr1	149.5 (14)
K1—O11—C12—C11	−56.04 (9)	K1—N1—C23—C24	−37.59 (10)
K1—O11—C13—C14	53.33 (9)	K1—N2—C16—C15	−48.37 (9)
K1—O12—C14—C13	42.42 (9)	K1—N2—C22—C21	−39.33 (9)
K1—O12—C15—C16	−41.08 (10)	K1—N2—C28—C27	−48.53 (9)
K1—O13—C18—C17	−41.03 (10)	O11—C12—C11—N1	69.61 (13)
K1—O13—C19—C20	49.51 (9)	O11—C13—C14—O12	−63.32 (13)
K1—O14—C20—C19	48.08 (9)	O12—C15—C16—N2	60.37 (13)
K1—O14—C21—C22	−59.81 (9)	O13—C18—C17—N1	62.44 (14)
K1—O15—C24—C23	−56.16 (9)	O13—C19—C20—O14	−66.05 (13)
K1—O15—C25—C26	38.02 (9)	O14—C21—C22—N2	69.45 (13)
K1—O16—C26—C25	57.54 (9)	O15—C24—C23—N1	63.09 (14)
K1—O16—C27—C28	−39.19 (9)	O15—C25—C26—O16	−63.73 (13)
K1—N1—C11—C12	−41.24 (9)	O16—C27—C28—N2	60.35 (14)
K1—N1—C17—C18	−49.92 (9)

(KCPTCR_standard_IAM_SHADE3)

Crystal data

C28H37Cr2KN2O16	F(000) = 1660.538
Mr = 800.70	Dx = 1.489 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71069 Å
a = 10.458 Å	Cell parameters from 1024 reflections
b = 14.417 Å	θ = 47.5–1.5°
c = 23.882 Å	µ = 0.80 mm^−1
β = 97.26°	T = 28 K
V = 3571.89 Å^3	Ellipsoidal, yellow
Z = 4	0.3 × 0.25 × 0.2 mm

Data collection

SMART CCD diffractometer	5667 reflections with I ≥ 2u(I)
ω scan	Rint = 0.0000
Absorption correction: empirical (using intensity measurements)	θmax = 25.0°, θmin = 2.4°
Tmin = 0.890, Tmax = 0.903	h = −19→20
27917 measured reflections	k = 0→30
5993 independent reflections	l = 0→50

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.023	Only H-atom coordinates refined
wR(F^2) = 0.059	w = 1/[σ^2(Fo^2) + (0.0269P)^2 + 2.8087P] where P = (Fo^2 + 2Fc^2)/3
S = 1.05	(Δ/σ)max = 0.001
5993 reflections	Δρmax = 0.30 e Å^−3
553 parameters	Δρmin = −0.38 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Cr1	0.16384 (2)	0.002378 (16)	0.236357 (10)	0.00606 (7)
Cr2	0.01879 (2)	0.177440 (16)	0.165112 (10)	0.00659 (7)
K1	0.46375 (3)	0.19929 (2)	0.418016 (13)	0.00720 (8)
O1	0.25192 (11)	0.13806 (8)	0.33116 (5)	0.0123 (2)
O2	−0.08331 (11)	−0.04366 (8)	0.28578 (5)	0.0144 (2)
O3	0.10483 (11)	−0.12657 (8)	0.13552 (5)	0.0129 (2)
O4	0.39527 (11)	0.05452 (8)	0.17751 (5)	0.0139 (2)
O5	0.30031 (11)	−0.15023 (8)	0.30577 (5)	0.0128 (2)
O6	−0.25963 (11)	0.12159 (8)	0.17226 (5)	0.0127 (2)
O7	0.01683 (11)	0.05860 (8)	0.05960 (5)	0.0127 (2)
O8	0.28633 (11)	0.25365 (8)	0.15525 (5)	0.0134 (2)
O9	0.02666 (12)	0.26549 (8)	0.28167 (5)	0.0177 (3)
O10	−0.07190 (11)	0.34753 (8)	0.09920 (5)	0.0147 (2)
O11	0.28612 (10)	0.09228 (7)	0.47318 (4)	0.0086 (2)
O12	0.44336 (10)	0.00301 (7)	0.40241 (5)	0.0089 (2)
O13	0.31323 (10)	0.34067 (7)	0.36302 (4)	0.0095 (2)
O14	0.52834 (10)	0.26689 (7)	0.31550 (4)	0.0098 (2)
O15	0.55080 (10)	0.32677 (8)	0.50740 (4)	0.0102 (2)
O16	0.72690 (10)	0.20501 (7)	0.46503 (4)	0.0090 (2)
N1	0.27340 (12)	0.30187 (9)	0.47975 (5)	0.0086 (3)
N2	0.66149 (12)	0.09476 (9)	0.36202 (5)	0.0082 (3)
C1	0.21619 (15)	0.08850 (11)	0.29503 (7)	0.0088 (3)
C2	0.01020 (15)	−0.02688 (10)	0.26768 (6)	0.0095 (3)
C3	0.12291 (14)	−0.07915 (11)	0.17424 (7)	0.0094 (3)
C4	0.30799 (15)	0.03673 (10)	0.20000 (7)	0.0098 (3)
C5	0.25012 (15)	−0.09112 (11)	0.27864 (6)	0.0088 (3)
C6	−0.15439 (16)	0.14190 (10)	0.16988 (6)	0.0095 (3)
C7	0.01874 (14)	0.10408 (11)	0.09912 (7)	0.0090 (3)
C8	0.18803 (16)	0.22111 (11)	0.16009 (6)	0.0100 (3)
C9	0.02394 (15)	0.23365 (11)	0.23779 (7)	0.0118 (3)
C10	−0.03867 (15)	0.28243 (11)	0.12528 (7)	0.0103 (3)
C11	0.20808 (16)	0.23278 (11)	0.51156 (7)	0.0100 (3)
C12	0.17289 (15)	0.14374 (11)	0.47995 (7)	0.0096 (3)
C13	0.25212 (16)	0.00532 (11)	0.44637 (7)	0.0092 (3)
C14	0.37205 (15)	−0.04777 (11)	0.43919 (7)	0.0090 (3)
C15	0.54836 (15)	−0.05003 (11)	0.38667 (7)	0.0088 (3)
C16	0.60994 (16)	0.00361 (11)	0.34261 (7)	0.0090 (3)
C17	0.17908 (15)	0.34653 (11)	0.43694 (7)	0.0105 (3)
C18	0.24063 (16)	0.40169 (11)	0.39338 (7)	0.0108 (3)
C19	0.37514 (16)	0.38878 (11)	0.32172 (7)	0.0118 (3)
C20	0.42782 (16)	0.31898 (12)	0.28397 (7)	0.0115 (3)
C21	0.57248 (16)	0.19470 (11)	0.28131 (7)	0.0102 (3)
C22	0.69033 (16)	0.14962 (11)	0.31296 (7)	0.0100 (3)
C23	0.33615 (15)	0.37142 (11)	0.51923 (7)	0.0113 (3)
C24	0.46485 (16)	0.34037 (12)	0.54888 (7)	0.0114 (3)
C25	0.68023 (15)	0.31745 (11)	0.53317 (7)	0.0092 (3)
C26	0.76443 (16)	0.29330 (11)	0.48876 (7)	0.0099 (3)
C27	0.82399 (15)	0.16959 (11)	0.43393 (7)	0.0098 (3)
C28	0.77739 (15)	0.08201 (11)	0.40285 (7)	0.0089 (3)
H	0.052 (2)	0.0761 (15)	0.1999 (10)	0.030761
H1A	0.127 (2)	0.2600 (15)	0.5230 (9)	0.023889
H1B	0.263 (2)	0.2185 (15)	0.5457 (9)	0.022725
H1C	0.125 (2)	0.1555 (15)	0.4422 (9)	0.021236
H1D	0.114 (2)	0.1071 (15)	0.5021 (9)	0.022704
H1E	0.201 (2)	0.0143 (14)	0.4094 (9)	0.020886
H1F	0.200 (2)	−0.0308 (15)	0.4689 (9)	0.022221
H1G	0.344 (2)	−0.1083 (15)	0.4227 (9)	0.021051
H1H	0.4226 (19)	−0.0565 (15)	0.4767 (9)	0.021280
H1I	0.517 (2)	−0.1078 (15)	0.3703 (9)	0.022380
H1J	0.609 (2)	−0.0658 (15)	0.4201 (9)	0.021936
H1K	0.546 (2)	0.0132 (14)	0.3109 (9)	0.021258
H1L	0.677 (2)	−0.0343 (15)	0.3295 (9)	0.022910
H1M	0.128 (2)	0.2980 (15)	0.4167 (9)	0.022307
H1N	0.121 (2)	0.3860 (15)	0.4543 (9)	0.024103
H1O	0.173 (2)	0.4295 (15)	0.3675 (9)	0.023539
H1P	0.298 (2)	0.4507 (15)	0.4121 (9)	0.023299
H1Q	0.442 (2)	0.4277 (15)	0.3403 (9)	0.022483
H1R	0.313 (2)	0.4272 (15)	0.2980 (9)	0.022622
H2A	0.359 (2)	0.2784 (15)	0.2681 (9)	0.020778
H2B	0.461 (2)	0.3506 (15)	0.2541 (9)	0.022274
H2C	0.593 (2)	0.2211 (15)	0.2454 (9)	0.022464
H2D	0.506 (2)	0.1514 (15)	0.2716 (9)	0.020833
H2E	0.730 (2)	0.1093 (15)	0.2856 (9)	0.022929
H2F	0.749 (2)	0.1988 (15)	0.3257 (9)	0.022610
H2G	0.349 (2)	0.4270 (15)	0.4974 (9)	0.023717
H2H	0.281 (2)	0.3896 (15)	0.5477 (9)	0.024368
H2I	0.461 (2)	0.2828 (15)	0.5715 (9)	0.022245
H2J	0.497 (2)	0.3873 (15)	0.5755 (9)	0.023654
H2K	0.711 (2)	0.3747 (15)	0.5511 (9)	0.022769
H2L	0.687 (2)	0.2688 (15)	0.5625 (9)	0.022034
H2M	0.760 (2)	0.3386 (15)	0.4594 (9)	0.022184
H2N	0.853 (2)	0.2914 (15)	0.5071 (9)	0.022344
H2O	0.848 (2)	0.2152 (15)	0.4082 (9)	0.022316
H2P	0.902 (2)	0.1538 (15)	0.4613 (9)	0.022948
H2Q	0.847 (2)	0.0557 (15)	0.3850 (9)	0.023665
H2R	0.760 (2)	0.0364 (15)	0.4292 (9)	0.022260

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cr1	0.00643 (13)	0.00543 (12)	0.00628 (12)	−0.00004 (9)	0.00061 (9)	−0.00025 (9)
Cr2	0.00752 (13)	0.00612 (12)	0.00595 (12)	0.00072 (9)	0.00016 (9)	0.00003 (9)
K1	0.00673 (16)	0.00728 (15)	0.00748 (16)	0.00030 (12)	0.00043 (12)	−0.00006 (12)
O1	0.0150 (6)	0.0098 (5)	0.0110 (6)	0.0001 (5)	−0.0024 (5)	−0.0011 (5)
O2	0.0115 (6)	0.0158 (6)	0.0168 (6)	0.0005 (5)	0.0055 (5)	0.0010 (5)
O3	0.0144 (6)	0.0130 (6)	0.0113 (6)	−0.0022 (5)	0.0017 (5)	−0.0039 (5)
O4	0.0118 (6)	0.0135 (6)	0.0174 (6)	−0.0006 (5)	0.0056 (5)	−0.0004 (5)
O5	0.0135 (6)	0.0103 (5)	0.0141 (6)	0.0027 (5)	−0.0005 (5)	0.0015 (5)
O6	0.0114 (6)	0.0148 (6)	0.0124 (6)	−0.0007 (5)	0.0034 (4)	0.0006 (5)
O7	0.0162 (6)	0.0126 (6)	0.0093 (6)	−0.0021 (5)	0.0022 (5)	−0.0025 (5)
O8	0.0123 (6)	0.0153 (6)	0.0123 (6)	−0.0039 (5)	0.0005 (5)	0.0010 (5)
O9	0.0251 (7)	0.0172 (6)	0.0098 (6)	0.0094 (5)	−0.0016 (5)	−0.0043 (5)
O10	0.0179 (6)	0.0099 (6)	0.0154 (6)	0.0027 (5)	−0.0017 (5)	0.0036 (5)
O11	0.0061 (5)	0.0074 (5)	0.0120 (5)	0.0003 (4)	0.0004 (4)	−0.0020 (4)
O12	0.0091 (5)	0.0071 (5)	0.0114 (5)	0.0011 (4)	0.0047 (4)	0.0019 (4)
O13	0.0107 (6)	0.0074 (5)	0.0108 (5)	0.0015 (4)	0.0036 (4)	0.0012 (4)
O14	0.0110 (6)	0.0097 (5)	0.0084 (5)	0.0031 (4)	0.0002 (4)	0.0000 (4)
O15	0.0072 (5)	0.0148 (6)	0.0086 (5)	0.0011 (4)	0.0007 (4)	−0.0020 (4)
O16	0.0064 (5)	0.0089 (5)	0.0118 (5)	−0.0011 (4)	0.0016 (4)	−0.0040 (4)
N1	0.0076 (6)	0.0084 (6)	0.0095 (6)	0.0003 (5)	−0.0003 (5)	−0.0001 (5)
N2	0.0087 (6)	0.0078 (6)	0.0081 (6)	−0.0010 (5)	0.0007 (5)	0.0005 (5)
C1	0.0071 (7)	0.0084 (7)	0.0111 (8)	0.0023 (6)	0.0022 (6)	0.0046 (6)
C2	0.0130 (8)	0.0067 (7)	0.0078 (7)	0.0021 (6)	−0.0018 (6)	−0.0005 (6)
C3	0.0053 (7)	0.0094 (7)	0.0136 (8)	0.0008 (6)	0.0021 (6)	0.0038 (7)
C4	0.0118 (8)	0.0065 (7)	0.0100 (7)	0.0016 (6)	−0.0025 (6)	−0.0017 (6)
C5	0.0077 (7)	0.0104 (7)	0.0088 (7)	−0.0027 (6)	0.0025 (6)	−0.0043 (6)
C6	0.0159 (9)	0.0075 (7)	0.0047 (7)	0.0034 (6)	0.0002 (6)	0.0004 (6)
C7	0.0055 (7)	0.0090 (7)	0.0124 (8)	−0.0005 (6)	0.0008 (6)	0.0053 (7)
C8	0.0158 (9)	0.0084 (7)	0.0052 (7)	0.0025 (6)	−0.0016 (6)	−0.0010 (6)
C9	0.0107 (8)	0.0095 (7)	0.0147 (9)	0.0041 (6)	−0.0010 (6)	0.0036 (7)
C10	0.0090 (8)	0.0117 (8)	0.0102 (7)	−0.0011 (6)	0.0011 (6)	−0.0045 (6)
C11	0.0099 (8)	0.0115 (8)	0.0089 (8)	0.0025 (6)	0.0025 (6)	0.0012 (6)
C12	0.0065 (7)	0.0110 (8)	0.0113 (8)	0.0016 (6)	0.0013 (6)	0.0013 (6)
C13	0.0103 (8)	0.0077 (7)	0.0093 (8)	−0.0034 (6)	0.0007 (6)	−0.0009 (6)
C14	0.0107 (8)	0.0078 (7)	0.0088 (8)	−0.0020 (6)	0.0018 (6)	0.0012 (6)
C15	0.0083 (8)	0.0071 (7)	0.0107 (8)	0.0022 (6)	0.0008 (6)	−0.0007 (6)
C16	0.0100 (8)	0.0089 (7)	0.0081 (7)	0.0003 (6)	0.0008 (6)	−0.0020 (6)
C17	0.0086 (8)	0.0098 (8)	0.0130 (8)	0.0031 (6)	0.0015 (6)	0.0012 (6)
C18	0.0110 (8)	0.0084 (7)	0.0131 (8)	0.0030 (6)	0.0019 (6)	0.0008 (6)
C19	0.0130 (8)	0.0095 (8)	0.0133 (8)	0.0015 (7)	0.0032 (7)	0.0046 (6)
C20	0.0121 (8)	0.0133 (8)	0.0092 (8)	0.0030 (7)	0.0008 (6)	0.0049 (6)
C21	0.0144 (8)	0.0082 (7)	0.0081 (8)	0.0018 (6)	0.0021 (6)	−0.0002 (6)
C22	0.0104 (8)	0.0106 (8)	0.0097 (8)	−0.0002 (6)	0.0040 (6)	0.0011 (6)
C23	0.0101 (8)	0.0114 (8)	0.0127 (8)	0.0011 (6)	0.0023 (6)	−0.0042 (6)
C24	0.0098 (8)	0.0150 (8)	0.0097 (8)	0.0003 (6)	0.0026 (6)	−0.0033 (7)
C25	0.0070 (8)	0.0098 (8)	0.0101 (8)	−0.0005 (6)	−0.0019 (6)	−0.0019 (6)
C26	0.0093 (8)	0.0088 (7)	0.0113 (8)	−0.0022 (6)	−0.0001 (6)	−0.0016 (6)
C27	0.0064 (8)	0.0124 (8)	0.0109 (8)	−0.0005 (6)	0.0024 (6)	−0.0016 (6)
C28	0.0063 (8)	0.0102 (7)	0.0102 (8)	0.0010 (6)	0.0009 (6)	−0.0006 (6)
H	0.026950	0.024430	0.039490	0.003320	−0.001300	0.012070
H1A	0.018090	0.028260	0.026500	0.003850	0.007420	−0.004510
H1B	0.021280	0.028200	0.017220	−0.000560	−0.003310	0.001250
H1C	0.020130	0.026710	0.015700	0.004180	−0.002280	−0.000760
H1D	0.019670	0.026340	0.023350	−0.003230	0.007580	0.001310
H1E	0.021970	0.022410	0.016650	0.002480	−0.003900	0.000740
H1F	0.021940	0.022690	0.023100	−0.004970	0.007000	0.003170
H1G	0.024800	0.014990	0.023070	−0.002480	0.001880	−0.001150
H1H	0.019270	0.025930	0.017300	−0.000280	−0.002910	0.004600
H1I	0.024420	0.015220	0.027530	−0.001140	0.003400	−0.003790
H1J	0.019190	0.025220	0.020290	0.005240	−0.001820	0.002540
H1K	0.019890	0.022080	0.020200	0.000040	−0.003710	0.001260
H1L	0.019810	0.021530	0.028490	0.004860	0.007340	−0.004180
H1M	0.022560	0.020750	0.022160	−0.002320	−0.002820	−0.003110
H1N	0.023510	0.025820	0.023440	0.009390	0.004760	−0.004390
H1O	0.023760	0.022860	0.022740	0.008020	−0.001960	0.001360
H1P	0.024910	0.018350	0.026090	−0.002380	0.001090	−0.006680
H1Q	0.024760	0.020080	0.021850	−0.007290	−0.000010	−0.002850
H1R	0.024560	0.019300	0.022980	0.004810	−0.000990	0.003950
H2A	0.019310	0.016420	0.025450	−0.003430	−0.001670	−0.002180
H2B	0.026450	0.022100	0.018900	−0.001510	0.005310	0.005020
H2C	0.025730	0.025460	0.017180	0.000170	0.006520	0.003400
H2D	0.017150	0.018990	0.026170	−0.003840	0.002000	−0.004460
H2E	0.023210	0.025770	0.020970	0.004170	0.007320	−0.003740
H2F	0.020550	0.023140	0.023400	−0.007350	−0.000100	−0.000990
H2G	0.027120	0.019370	0.023680	−0.000850	−0.000610	0.001150
H2H	0.020660	0.031140	0.021840	0.003780	0.004770	−0.008290
H2I	0.022570	0.022140	0.022640	0.001760	0.005250	0.003380
H2J	0.022120	0.026260	0.021820	−0.001040	−0.000190	−0.009590
H2K	0.022210	0.021200	0.024260	−0.002930	0.000460	−0.007230
H2L	0.020600	0.024770	0.020640	0.000400	0.002250	0.005730
H2M	0.028640	0.019440	0.018360	−0.002360	0.002530	0.002290
H2N	0.014540	0.027080	0.024570	−0.000960	−0.000810	−0.003010
H2O	0.024090	0.022000	0.021910	−0.002100	0.007000	0.002010
H2P	0.014960	0.030120	0.022740	0.002450	−0.001610	−0.002570
H2Q	0.016710	0.029800	0.025100	0.004240	0.005040	−0.006160
H2R	0.022290	0.022140	0.021870	−0.001610	0.000920	0.004480

Geometric parameters (Å, º)

Cr1—C1	1.9003 (16)	N2—C22	1.4758 (19)
Cr1—C2	1.9034 (16)	N2—C28	1.468 (2)
Cr1—C3	1.8987 (16)	C11—C12	1.511 (2)
Cr1—C4	1.8982 (16)	C11—H1A	1.00 (2)
Cr1—C5	1.8495 (16)	C11—H1B	0.96 (2)
Cr1—H	1.73 (2)	C12—H1C	0.99 (2)
Cr2—C6	1.8994 (17)	C12—H1D	1.01 (2)
Cr2—C7	1.8979 (16)	C13—C14	1.498 (2)
Cr2—C8	1.8966 (17)	C13—H1E	0.98 (2)
Cr2—C9	1.9101 (17)	C13—H1F	0.97 (2)
Cr2—C10	1.8473 (17)	C14—H1G	0.99 (2)
Cr2—H	1.69 (2)	C14—H1H	0.99 (2)
K1—O1	2.9713 (12)	C15—C16	1.514 (2)
K1—O11	2.8611 (11)	C15—H1I	0.96 (2)
K1—O12	2.8587 (11)	C15—H1J	0.98 (2)
K1—O13	2.7990 (11)	C16—H1K	0.96 (2)
K1—O14	2.7961 (11)	C16—H1L	0.97 (2)
K1—O15	2.8761 (11)	C17—C18	1.516 (2)
K1—O16	2.8390 (11)	C17—H1M	0.97 (2)
K1—N1	3.0109 (13)	C17—H1N	0.96 (2)
K1—N2	3.0059 (13)	C18—H1O	0.96 (2)
O1—C1	1.1459 (19)	C18—H1P	1.00 (2)
O2—C2	1.144 (2)	C19—C20	1.502 (2)
O3—C3	1.146 (2)	C19—H1Q	0.96 (2)
O4—C4	1.145 (2)	C19—H1R	0.98 (2)
O5—C5	1.156 (2)	C20—H2A	0.97 (2)
O6—C6	1.147 (2)	C20—H2B	0.95 (2)
O7—C7	1.147 (2)	C21—C22	1.509 (2)
O8—C8	1.149 (2)	C21—H2C	0.99 (2)
O9—C9	1.141 (2)	C21—H2D	0.94 (2)
O10—C10	1.155 (2)	C22—H2E	1.00 (2)
O11—C12	1.4238 (19)	C22—H2F	0.96 (2)
O11—C13	1.4320 (18)	C23—C24	1.508 (2)
O12—C14	1.4244 (18)	C23—H2G	0.98 (2)
O12—C15	1.4270 (18)	C23—H2H	0.98 (2)
O13—C18	1.4196 (19)	C24—H2I	0.99 (2)
O13—C19	1.4264 (19)	C24—H2J	0.96 (2)
O14—C20	1.4270 (19)	C25—C26	1.503 (2)
O14—C21	1.4347 (19)	C25—H2K	0.97 (2)
O15—C24	1.4327 (19)	C25—H2L	0.99 (2)
O15—C25	1.4207 (19)	C26—H2M	0.95 (2)
O16—C26	1.4281 (19)	C26—H2N	0.98 (2)
O16—C27	1.4262 (19)	C27—C28	1.514 (2)
N1—C11	1.472 (2)	C27—H2O	0.95 (2)
N1—C17	1.476 (2)	C27—H2P	1.00 (2)
N1—C23	1.473 (2)	C28—H2Q	0.96 (2)
N2—C16	1.473 (2)	C28—H2R	0.94 (2)
C2—Cr1—C1	91.94 (6)	H1A—C11—N1	109.8 (12)
C3—Cr1—C1	174.96 (6)	H1A—C11—C12	107.9 (12)
C3—Cr1—C2	92.97 (6)	H1B—C11—N1	108.5 (13)
C4—Cr1—C1	89.74 (6)	H1B—C11—C12	108.9 (13)
C4—Cr1—C2	175.08 (7)	H1B—C11—H1A	106.8 (17)
C4—Cr1—C3	85.28 (6)	C11—C12—O11	110.23 (13)
C5—Cr1—C1	89.90 (6)	H1C—C12—O11	108.4 (12)
C5—Cr1—C2	90.10 (7)	H1C—C12—C11	111.9 (12)
C5—Cr1—C3	91.24 (7)	H1D—C12—O11	110.8 (12)
C5—Cr1—C4	94.53 (7)	H1D—C12—C11	108.0 (12)
H—Cr1—C1	94.8 (8)	H1D—C12—H1C	107.5 (17)
H—Cr1—C2	77.6 (7)	C14—C13—O11	109.54 (13)
H—Cr1—C3	85.2 (8)	H1E—C13—O11	111.3 (12)
H—Cr1—C4	97.7 (7)	H1E—C13—C14	109.6 (12)
H—Cr1—C5	166.9 (7)	H1F—C13—O11	110.5 (13)
C7—Cr2—C6	89.96 (6)	H1F—C13—C14	109.2 (13)
C8—Cr2—C6	176.25 (7)	H1F—C13—H1E	106.7 (17)
C8—Cr2—C7	91.99 (6)	C13—C14—O12	108.61 (12)
C9—Cr2—C6	88.72 (7)	H1G—C14—O12	111.1 (12)
C9—Cr2—C7	171.11 (7)	H1G—C14—C13	106.8 (12)
C9—Cr2—C8	89.84 (7)	H1H—C14—O12	111.2 (12)
C10—Cr2—C6	90.07 (7)	H1H—C14—C13	108.7 (12)
C10—Cr2—C7	93.61 (7)	H1H—C14—H1G	110.2 (17)
C10—Cr2—C8	86.61 (7)	C16—C15—O12	108.58 (12)
C10—Cr2—C9	95.18 (7)	H1I—C15—O12	109.8 (12)
H—Cr2—C6	83.0 (7)	H1I—C15—C16	108.3 (13)
H—Cr2—C7	84.5 (8)	H1J—C15—O12	110.4 (12)
H—Cr2—C8	100.4 (7)	H1J—C15—C16	113.4 (12)
H—Cr2—C9	86.6 (8)	H1J—C15—H1I	106.4 (17)
H—Cr2—C10	172.8 (7)	C15—C16—N2	114.09 (13)
O11—K1—O1	72.00 (3)	H1K—C16—N2	108.2 (12)
O12—K1—O1	65.05 (3)	H1K—C16—C15	107.8 (13)
O12—K1—O11	58.94 (3)	H1L—C16—N2	110.7 (12)
O13—K1—O1	64.11 (3)	H1L—C16—C15	108.9 (13)
O13—K1—O11	104.44 (3)	H1L—C16—H1K	106.8 (18)
O13—K1—O12	129.15 (3)	C18—C17—N1	113.56 (13)
O14—K1—O1	74.55 (3)	H1M—C17—N1	107.9 (12)
O14—K1—O11	146.50 (3)	H1M—C17—C18	106.9 (13)
O14—K1—O12	104.66 (3)	H1N—C17—N1	111.2 (13)
O14—K1—O13	61.26 (3)	H1N—C17—C18	109.3 (13)
O15—K1—O1	147.79 (3)	H1N—C17—H1M	107.7 (18)
O15—K1—O11	99.55 (3)	C17—C18—O13	109.03 (12)
O15—K1—O12	137.79 (3)	H1O—C18—O13	108.9 (12)
O15—K1—O13	89.40 (3)	H1O—C18—C17	108.6 (13)
O15—K1—O14	109.78 (3)	H1P—C18—O13	109.7 (12)
O16—K1—O1	152.21 (3)	H1P—C18—C17	110.4 (12)
O16—K1—O11	119.14 (3)	H1P—C18—H1O	110.2 (17)
O16—K1—O12	97.64 (3)	C20—C19—O13	108.81 (13)
O16—K1—O13	128.61 (3)	H1Q—C19—O13	109.6 (12)
O16—K1—O14	90.39 (3)	H1Q—C19—C20	111.3 (13)
O16—K1—O15	59.19 (3)	H1R—C19—O13	110.3 (12)
N1—K1—O1	90.40 (3)	H1R—C19—C20	107.4 (12)
N1—K1—O11	62.06 (3)	H1R—C19—H1Q	109.4 (18)
N1—K1—O12	120.46 (3)	C19—C20—O14	109.72 (13)
N1—K1—O13	60.31 (3)	H2A—C20—O14	110.5 (12)
N1—K1—O14	120.36 (3)	H2A—C20—C19	109.3 (12)
N1—K1—O15	59.31 (3)	H2B—C20—O14	109.7 (13)
N1—K1—O16	117.38 (3)	H2B—C20—C19	109.0 (13)
N2—K1—O1	91.98 (3)	H2B—C20—H2A	108.6 (18)
N2—K1—O11	117.24 (3)	C22—C21—O14	109.18 (13)
N2—K1—O12	59.33 (3)	H2C—C21—O14	109.6 (12)
N2—K1—O13	122.28 (3)	H2C—C21—C22	110.6 (12)
N2—K1—O14	61.92 (3)	H2D—C21—O14	110.1 (13)
N2—K1—O15	118.66 (3)	H2D—C21—C22	111.5 (13)
N2—K1—O16	60.23 (3)	H2D—C21—H2C	105.9 (17)
N2—K1—N1	177.12 (4)	C21—C22—N2	113.11 (13)
C1—O1—K1	148.68 (11)	H2E—C22—N2	110.5 (12)
C12—O11—K1	111.65 (8)	H2E—C22—C21	107.8 (12)
C13—O11—K1	113.90 (8)	H2F—C22—N2	109.4 (12)
C13—O11—C12	110.11 (11)	H2F—C22—C21	106.9 (13)
C14—O12—K1	117.69 (8)	H2F—C22—H2E	109.1 (17)
C15—O12—K1	121.17 (9)	C24—C23—N1	113.44 (13)
C15—O12—C14	111.55 (11)	H2G—C23—N1	107.3 (12)
C18—O13—K1	121.13 (9)	H2G—C23—C24	108.7 (12)
C19—O13—K1	113.64 (9)	H2H—C23—N1	111.7 (12)
C19—O13—C18	111.75 (12)	H2H—C23—C24	108.9 (12)
C20—O14—K1	113.71 (9)	H2H—C23—H2G	106.5 (18)
C21—O14—K1	112.10 (8)	C23—C24—O15	108.46 (13)
C21—O14—C20	110.49 (12)	H2I—C24—O15	109.5 (12)
C24—O15—K1	115.68 (9)	H2I—C24—C23	114.0 (12)
C25—O15—K1	117.13 (8)	H2J—C24—O15	110.7 (13)
C25—O15—C24	111.10 (12)	H2J—C24—C23	108.9 (13)
C26—O16—K1	112.76 (9)	H2J—C24—H2I	105.4 (17)
C27—O16—K1	120.13 (9)	C26—C25—O15	109.11 (13)
C27—O16—C26	110.35 (11)	H2K—C25—O15	111.0 (12)
C11—N1—K1	107.40 (9)	H2K—C25—C26	108.5 (12)
C17—N1—K1	107.48 (9)	H2L—C25—O15	110.9 (12)
C17—N1—C11	109.86 (12)	H2L—C25—C26	109.8 (12)
C23—N1—K1	112.28 (9)	H2L—C25—H2K	107.4 (17)
C23—N1—C11	109.19 (12)	C25—C26—O16	109.29 (13)
C23—N1—C17	110.57 (12)	H2M—C26—O16	109.4 (12)
C16—N2—K1	110.02 (9)	H2M—C26—C25	112.3 (13)
C22—N2—K1	107.79 (9)	H2N—C26—O16	110.5 (13)
C22—N2—C16	109.38 (12)	H2N—C26—C25	107.4 (12)
C28—N2—K1	108.90 (9)	H2N—C26—H2M	107.8 (18)
C28—N2—C16	109.63 (12)	C28—C27—O16	110.35 (12)
C28—N2—C22	111.10 (12)	H2O—C27—O16	110.4 (13)
O1—C1—Cr1	177.18 (13)	H2O—C27—C28	110.7 (13)
O2—C2—Cr1	178.84 (13)	H2P—C27—O16	108.3 (12)
O3—C3—Cr1	175.87 (13)	H2P—C27—C28	108.3 (12)
O4—C4—Cr1	177.78 (13)	H2P—C27—H2O	108.7 (17)
O5—C5—Cr1	177.74 (13)	C27—C28—N2	114.13 (13)
O6—C6—Cr2	178.95 (13)	H2Q—C28—N2	111.1 (12)
O7—C7—Cr2	178.60 (13)	H2Q—C28—C27	109.3 (13)
O8—C8—Cr2	174.76 (14)	H2R—C28—N2	108.8 (12)
O9—C9—Cr2	178.60 (14)	H2R—C28—C27	109.3 (13)
O10—C10—Cr2	177.87 (14)	H2R—C28—H2Q	103.7 (18)
C12—C11—N1	114.62 (13)	Cr2—H—Cr1	149.4 (14)
K1—O11—C12—C11	−56.06 (9)	K1—N1—C23—C24	−37.57 (10)
K1—O11—C13—C14	53.33 (9)	K1—N2—C16—C15	−48.37 (9)
K1—O12—C14—C13	42.43 (9)	K1—N2—C22—C21	−39.35 (9)
K1—O12—C15—C16	−41.08 (10)	K1—N2—C28—C27	−48.52 (9)
K1—O13—C18—C17	−41.05 (10)	O11—C12—C11—N1	69.63 (13)
K1—O13—C19—C20	49.54 (9)	O11—C13—C14—O12	−63.34 (13)
K1—O14—C20—C19	48.10 (9)	O12—C15—C16—N2	60.38 (13)
K1—O14—C21—C22	−59.82 (9)	O13—C18—C17—N1	62.46 (14)
K1—O15—C24—C23	−56.15 (9)	O13—C19—C20—O14	−66.09 (13)
K1—O15—C25—C26	38.02 (9)	O14—C21—C22—N2	69.47 (13)
K1—O16—C26—C25	57.53 (9)	O15—C24—C23—N1	63.08 (14)
K1—O16—C27—C28	−39.18 (9)	O15—C25—C26—O16	−63.72 (13)
K1—N1—C11—C12	−41.26 (9)	O16—C27—C28—N2	60.34 (14)
K1—N1—C17—C18	−49.94 (9)

 

Dicarbonyl-cis-dihydrido-trans-bis(triphenylphosphite)iron(II) (QOSZON_HAR_0_HADPs)

Crystal data

C38H32FeO8P2	Z = 2
Mr = 734.47	F(000) = 761.455
Triclinic, P1	Dx = 1.431 Mg m^−3
a = 9.6397 (12) Å	Mo Kα radiation, λ = 0.71073 Å
b = 10.4410 (13) Å	Cell parameters from 5000 reflections
c = 18.381 (2) Å	θ = 3.3–52.1°
α = 102.148 (15)°	µ = 0.59 mm^−1
β = 94.667 (15)°	T = 293 K
γ = 107.402 (14)°	Parallelepiped, colourless
V = 1705.0 (4) Å^3	0.5 × 0.25 × 0.1 mm

Data collection

STOE diffractometer	Rint = 0.034
Detector resolution: 1.60 pixels mm^-1	θmax = 26.1°, θmin = 2.1°
rotation en phi scans	h = −11→11
16806 measured reflections	k = −12→12
6202 independent reflections	l = −22→22
5084 reflections with I ≥ 2u(I)

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.032	Only H-atom coordinates refined
wR(F^2) = 0.102	w = 1/[σ^2(Fo^2) + (0.1P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 0.80	(Δ/σ)max = 0.001
6202 reflections	Δρmax = 0.30 e Å^−3
538 parameters	Δρmin = −0.62 e Å^−3

Special details

Experimental. The crystal was pasted on a glass fiber, by using an oil-coated shock-cooled crystal.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Fe1	0.53170 (3)	0.83647 (3)	0.270663 (14)	0.01826 (10)
P1	0.35098 (5)	0.72591 (5)	0.18540 (3)	0.01817 (13)
P2	0.72504 (5)	1.00381 (5)	0.32211 (3)	0.01814 (13)
O1	0.30699 (16)	0.79741 (15)	0.12202 (8)	0.0248 (3)
O2	0.37066 (15)	0.59229 (15)	0.13044 (8)	0.0225 (3)
O3	0.18552 (14)	0.66713 (15)	0.20476 (8)	0.0238 (3)
O4	0.71945 (16)	1.12338 (16)	0.39188 (7)	0.0246 (3)
O5	0.84519 (14)	0.95236 (15)	0.36186 (8)	0.0234 (3)
O6	0.82093 (15)	1.10476 (15)	0.27657 (7)	0.0249 (3)
O7	0.4086 (2)	0.8190 (2)	0.41020 (10)	0.0550 (6)
O8	0.67935 (19)	0.6270 (2)	0.25563 (11)	0.0418 (4)
C1	0.3279 (2)	0.9370 (2)	0.13019 (10)	0.0193 (4)
C2	0.2243 (2)	0.9926 (2)	0.15933 (11)	0.0266 (4)
C3	0.2382 (3)	1.1293 (3)	0.16007 (13)	0.0352 (5)
C4	0.3544 (3)	1.2087 (2)	0.13205 (14)	0.0355 (5)
C5	0.4581 (2)	1.1518 (2)	0.10370 (14)	0.0331 (5)
C6	0.4457 (2)	1.0149 (2)	0.10267 (12)	0.0259 (4)
C7	0.2935 (2)	0.5320 (2)	0.05758 (11)	0.0212 (4)
C8	0.3631 (2)	0.5679 (2)	−0.00192 (12)	0.0305 (5)
C9	0.2894 (3)	0.5057 (3)	−0.07511 (13)	0.0366 (5)
C10	0.1483 (3)	0.4095 (3)	−0.08806 (13)	0.0358 (5)
C11	0.0815 (2)	0.3756 (3)	−0.02752 (13)	0.0350 (5)
C12	0.1547 (2)	0.4360 (2)	0.04595 (12)	0.0286 (5)
C13	0.1487 (2)	0.5890 (2)	0.25694 (11)	0.0215 (4)
C14	0.0356 (2)	0.6071 (3)	0.29576 (13)	0.0305 (5)
C15	−0.0109 (3)	0.5284 (3)	0.34682 (14)	0.0373 (6)
C16	0.0556 (3)	0.4317 (3)	0.35967 (13)	0.0350 (5)
C17	0.1685 (2)	0.4153 (2)	0.32059 (13)	0.0324 (5)
C18	0.2154 (2)	0.4926 (2)	0.26883 (12)	0.0266 (5)
C19	0.6711 (2)	1.2346 (2)	0.38990 (11)	0.0215 (4)
C20	0.7001 (2)	1.3327 (2)	0.45794 (11)	0.0263 (5)
C21	0.6533 (3)	1.4475 (3)	0.46202 (13)	0.0327 (5)
C22	0.5791 (3)	1.4643 (3)	0.39836 (14)	0.0328 (5)
C23	0.5525 (2)	1.3660 (2)	0.33054 (13)	0.0299 (5)
C24	0.5985 (2)	1.2505 (2)	0.32548 (11)	0.0255 (4)
C25	0.9896 (2)	1.0352 (2)	0.39223 (11)	0.0234 (4)
C26	1.0997 (2)	1.0143 (3)	0.35234 (14)	0.0343 (5)
C27	1.2459 (3)	1.0862 (3)	0.38411 (18)	0.0462 (7)
C28	1.2801 (3)	1.1769 (3)	0.45547 (17)	0.0440 (7)
C29	1.1671 (3)	1.1960 (3)	0.49418 (14)	0.0383 (6)
C30	1.0205 (2)	1.1257 (2)	0.46302 (12)	0.0285 (5)
C31	0.8280 (2)	1.0854 (2)	0.20076 (11)	0.0202 (4)
C32	0.8358 (2)	0.9624 (2)	0.15663 (11)	0.0244 (4)
C33	0.8455 (2)	0.9526 (3)	0.08083 (12)	0.0307 (5)
C34	0.8500 (2)	1.0633 (3)	0.04955 (12)	0.0324 (5)
C35	0.8441 (2)	1.1862 (3)	0.09481 (12)	0.0297 (5)
C36	0.8334 (2)	1.1978 (2)	0.17086 (12)	0.0246 (4)
C37	0.4561 (2)	0.8229 (3)	0.35579 (12)	0.0312 (5)
C38	0.6196 (2)	0.7076 (2)	0.26262 (11)	0.0259 (5)
H1	0.468 (2)	0.952 (2)	0.2700 (11)	0.000000
H2	0.587 (2)	0.872 (2)	0.2013 (10)	0.000000
H3	0.1347 (19)	0.9311 (19)	0.1791 (10)	0.000000
H4	0.1504 (19)	1.171 (2)	0.1796 (10)	0.000000
H5	0.3641 (18)	1.309 (2)	0.1308 (10)	0.000000
H6	0.5495 (19)	1.2121 (19)	0.0796 (10)	0.000000
H7	0.5250 (19)	0.969 (2)	0.0788 (10)	0.000000
H8	0.4752 (19)	0.647 (2)	0.0107 (10)	0.000000
H9	0.3474 (19)	0.5273 (19)	−0.1218 (10)	0.000000
H10	0.0889 (19)	0.359 (2)	−0.1464 (10)	0.000000
H11	−0.0332 (19)	0.298 (2)	−0.0357 (10)	0.000000
H12	0.1045 (19)	0.4113 (19)	0.0924 (10)	0.000000
H13	−0.0139 (19)	0.681 (2)	0.2836 (10)	0.000000
H14	−0.1020 (19)	0.5346 (19)	0.3745 (10)	0.000000
H15	0.0095 (19)	0.367 (2)	0.3993 (10)	0.000000
H16	0.2172 (19)	0.339 (2)	0.3301 (10)	0.000000
H17	0.3027 (19)	0.478 (2)	0.2381 (10)	0.000000
H18	0.7598 (19)	1.3167 (19)	0.5057 (10)	0.000000
H19	0.6836 (18)	1.5182 (19)	0.5148 (10)	0.000000
H20	0.5483 (18)	1.552 (2)	0.4036 (9)	0.000000
H21	0.4947 (19)	1.380 (2)	0.2793 (10)	0.000000
H22	0.5747 (19)	1.173 (2)	0.2690 (10)	0.000000
H23	1.0631 (19)	0.942 (2)	0.2930 (10)	0.000000
H24	1.3347 (19)	1.069 (2)	0.3524 (10)	0.000000
H25	1.3979 (19)	1.234 (2)	0.4796 (10)	0.000000
H26	1.1951 (19)	1.2666 (19)	0.5486 (10)	0.000000
H27	0.9308 (19)	1.141 (2)	0.4928 (10)	0.000000
H28	0.8373 (19)	0.876 (2)	0.1821 (10)	0.000000
H29	0.8505 (19)	0.859 (2)	0.0472 (10)	0.000000
H30	0.8446 (19)	1.0461 (19)	−0.0112 (10)	0.000000
H31	0.8416 (19)	1.2661 (19)	0.0686 (10)	0.000000
H32	0.8322 (19)	1.297 (2)	0.2077 (10)	0.000000

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Fe1	0.01675 (15)	0.01909 (17)	0.01688 (15)	0.00247 (11)	0.00080 (10)	0.00563 (11)
P1	0.0170 (2)	0.0169 (3)	0.0190 (2)	0.00277 (19)	0.00010 (17)	0.00616 (19)
P2	0.0184 (2)	0.0181 (3)	0.0157 (2)	0.00301 (19)	0.00127 (17)	0.00428 (19)
O1	0.0297 (7)	0.0187 (7)	0.0222 (7)	0.0038 (6)	−0.0044 (6)	0.0065 (6)
O2	0.0222 (7)	0.0202 (8)	0.0233 (7)	0.0062 (6)	−0.0006 (5)	0.0039 (6)
O3	0.0168 (6)	0.0259 (8)	0.0297 (7)	0.0050 (6)	0.0026 (5)	0.0122 (6)
O4	0.0302 (7)	0.0253 (8)	0.0180 (6)	0.0108 (6)	0.0015 (5)	0.0032 (6)
O5	0.0197 (6)	0.0214 (8)	0.0260 (7)	0.0037 (6)	−0.0027 (5)	0.0059 (6)
O6	0.0277 (7)	0.0221 (8)	0.0189 (6)	−0.0001 (6)	0.0034 (5)	0.0047 (6)
O7	0.0520 (11)	0.0763 (15)	0.0282 (9)	0.0024 (10)	0.0165 (8)	0.0176 (9)
O8	0.0426 (10)	0.0340 (11)	0.0527 (10)	0.0212 (8)	0.0029 (8)	0.0078 (8)
C1	0.0199 (9)	0.0195 (10)	0.0192 (8)	0.0065 (8)	0.0026 (7)	0.0063 (8)
C2	0.0258 (10)	0.0300 (12)	0.0264 (10)	0.0117 (9)	0.0084 (8)	0.0066 (9)
C3	0.0390 (13)	0.0325 (14)	0.0360 (12)	0.0191 (11)	0.0039 (9)	0.0024 (10)
C4	0.0406 (13)	0.0205 (13)	0.0447 (13)	0.0116 (10)	−0.0046 (10)	0.0084 (10)
C5	0.0290 (11)	0.0247 (12)	0.0470 (13)	0.0051 (9)	0.0032 (9)	0.0179 (10)
C6	0.0220 (10)	0.0259 (12)	0.0338 (10)	0.0078 (8)	0.0079 (8)	0.0143 (9)
C7	0.0215 (9)	0.0182 (10)	0.0225 (9)	0.0063 (8)	0.0010 (7)	0.0030 (8)
C8	0.0333 (11)	0.0285 (12)	0.0260 (11)	0.0047 (10)	0.0044 (9)	0.0070 (9)
C9	0.0497 (14)	0.0320 (14)	0.0237 (11)	0.0097 (11)	0.0032 (10)	0.0037 (10)
C10	0.0459 (14)	0.0300 (13)	0.0263 (11)	0.0130 (11)	−0.0062 (10)	−0.0008 (10)
C11	0.0295 (11)	0.0305 (13)	0.0340 (12)	0.0046 (10)	−0.0071 (9)	−0.0031 (10)
C12	0.0240 (10)	0.0244 (12)	0.0293 (11)	0.0010 (9)	−0.0001 (8)	0.0010 (9)
C13	0.0162 (9)	0.0211 (11)	0.0262 (9)	0.0031 (7)	0.0028 (7)	0.0081 (8)
C14	0.0271 (10)	0.0320 (13)	0.0355 (11)	0.0106 (9)	0.0111 (9)	0.0110 (10)
C15	0.0309 (12)	0.0472 (16)	0.0368 (12)	0.0100 (11)	0.0164 (10)	0.0162 (11)
C16	0.0332 (11)	0.0369 (14)	0.0317 (11)	0.0023 (10)	0.0069 (9)	0.0139 (10)
C17	0.0344 (12)	0.0292 (13)	0.0355 (12)	0.0077 (10)	0.0044 (9)	0.0160 (10)
C18	0.0247 (10)	0.0259 (12)	0.0336 (11)	0.0088 (8)	0.0078 (8)	0.0143 (9)
C19	0.0228 (9)	0.0195 (11)	0.0198 (9)	0.0050 (8)	0.0031 (7)	0.0029 (8)
C20	0.0314 (10)	0.0211 (11)	0.0209 (9)	0.0040 (9)	0.0050 (8)	0.0000 (8)
C21	0.0380 (12)	0.0260 (13)	0.0284 (11)	0.0065 (10)	0.0089 (9)	−0.0011 (9)
C22	0.0389 (12)	0.0225 (13)	0.0388 (12)	0.0143 (10)	0.0091 (10)	0.0038 (10)
C23	0.0313 (11)	0.0226 (12)	0.0338 (12)	0.0093 (9)	−0.0005 (9)	0.0038 (9)
C24	0.0259 (10)	0.0252 (12)	0.0226 (10)	0.0071 (8)	−0.0007 (8)	0.0038 (9)
C25	0.0205 (9)	0.0211 (11)	0.0251 (10)	0.0029 (8)	−0.0005 (7)	0.0056 (8)
C26	0.0235 (11)	0.0373 (14)	0.0401 (13)	0.0071 (10)	0.0070 (9)	0.0088 (11)
C27	0.0216 (11)	0.0467 (17)	0.0681 (18)	0.0055 (11)	0.0088 (11)	0.0169 (14)
C28	0.0223 (11)	0.0373 (15)	0.0651 (17)	−0.0015 (10)	−0.0051 (11)	0.0174 (13)
C29	0.0339 (12)	0.0268 (13)	0.0413 (13)	−0.0025 (10)	−0.0127 (10)	0.0060 (11)
C30	0.0257 (11)	0.0262 (12)	0.0279 (10)	0.0034 (9)	−0.0027 (8)	0.0047 (9)
C31	0.0182 (8)	0.0215 (11)	0.0195 (9)	0.0046 (7)	0.0020 (7)	0.0054 (8)
C32	0.0264 (10)	0.0250 (12)	0.0237 (10)	0.0098 (8)	0.0077 (8)	0.0064 (9)
C33	0.0338 (11)	0.0334 (14)	0.0249 (10)	0.0135 (10)	0.0074 (8)	0.0024 (10)
C34	0.0299 (11)	0.0469 (15)	0.0204 (10)	0.0105 (10)	0.0046 (8)	0.0110 (10)
C35	0.0288 (10)	0.0375 (14)	0.0287 (11)	0.0105 (9)	0.0075 (8)	0.0195 (10)
C36	0.0254 (10)	0.0232 (12)	0.0264 (10)	0.0062 (8)	0.0055 (8)	0.0107 (9)
C37	0.0287 (10)	0.0384 (13)	0.0232 (11)	0.0036 (9)	0.0041 (8)	0.0112 (9)
C38	0.0239 (10)	0.0235 (12)	0.0290 (10)	0.0067 (9)	0.0002 (8)	0.0066 (9)
H1	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H3	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H4	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H5	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H6	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H7	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H8	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H9	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H10	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H11	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H12	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H13	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H14	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H15	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H16	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H17	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H18	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H19	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H20	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H21	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H22	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H23	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H24	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H25	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H26	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H27	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H28	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H29	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H30	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H31	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H32	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000

Geometric parameters (Å, º)

Fe1—P1	2.1012 (7)	C13—C18	1.389 (3)
Fe1—P2	2.1191 (7)	C14—C15	1.389 (3)
Fe1—C37	1.793 (2)	C14—H13	1.071 (19)
Fe1—C38	1.781 (2)	C15—C16	1.396 (4)
Fe1—H1	1.514 (19)	C15—H14	1.062 (18)
Fe1—H2	1.499 (18)	C16—C17	1.385 (4)
P1—O1	1.6030 (14)	C16—H15	1.123 (18)
P1—O2	1.6122 (16)	C17—C18	1.391 (3)
P1—O3	1.6266 (14)	C17—H16	1.075 (19)
P2—O4	1.6073 (15)	C18—H17	1.081 (18)
P2—O5	1.6011 (14)	C19—C20	1.387 (3)
P2—O6	1.6064 (14)	C19—C24	1.392 (3)
O1—C1	1.384 (2)	C20—C21	1.392 (3)
O2—C7	1.395 (2)	C20—H18	1.080 (17)
O3—C13	1.387 (2)	C21—C22	1.392 (3)
O4—C19	1.380 (3)	C21—H19	1.046 (18)
O5—C25	1.395 (2)	C22—C23	1.388 (3)
O6—C31	1.376 (2)	C22—H20	1.035 (19)
O7—C37	1.137 (3)	C23—C24	1.393 (3)
O8—C38	1.145 (3)	C23—H21	1.112 (17)
C1—C2	1.387 (3)	C24—H22	1.132 (19)
C1—C6	1.386 (3)	C25—C26	1.382 (3)
C2—C3	1.390 (3)	C25—C30	1.388 (3)
C2—H3	1.052 (18)	C26—C27	1.392 (3)
C3—C4	1.388 (4)	C26—H23	1.146 (18)
C3—H4	1.114 (19)	C27—C28	1.395 (4)
C4—C5	1.390 (4)	C27—H24	1.110 (18)
C4—H5	1.024 (19)	C28—C29	1.389 (4)
C5—C6	1.394 (3)	C28—H25	1.115 (17)
C5—H6	1.105 (18)	C29—C30	1.391 (3)
C6—H7	1.091 (19)	C29—H26	1.069 (18)
C7—C8	1.388 (3)	C30—H27	1.093 (18)
C7—C12	1.379 (3)	C31—C32	1.393 (3)
C8—C9	1.392 (3)	C31—C36	1.386 (3)
C8—H8	1.119 (18)	C32—C33	1.388 (3)
C9—C10	1.394 (4)	C32—H28	1.105 (19)
C9—H9	1.088 (18)	C33—C34	1.387 (3)
C10—C11	1.387 (4)	C33—H29	1.06 (2)
C10—H10	1.112 (17)	C34—C35	1.394 (4)
C11—C12	1.393 (3)	C34—H30	1.088 (17)
C11—H11	1.134 (18)	C35—C36	1.393 (3)
C12—H12	1.057 (18)	C35—H31	1.052 (18)
C13—C14	1.388 (3)	C36—H32	1.11 (2)
P2—Fe1—P1	154.36 (2)	C15—C14—C13	119.7 (2)
C37—Fe1—P1	103.54 (7)	H13—C14—C13	117.5 (10)
C37—Fe1—P2	95.95 (7)	H13—C14—C15	122.8 (10)
C38—Fe1—P1	97.56 (7)	C16—C15—C14	120.6 (2)
C38—Fe1—P2	94.95 (7)	H14—C15—C14	121.6 (10)
C38—Fe1—C37	100.73 (11)	H14—C15—C16	117.7 (10)
H1—Fe1—P1	82.3 (7)	C17—C16—C15	118.9 (2)
H1—Fe1—P2	82.5 (7)	H15—C16—C15	117.4 (10)
H1—Fe1—C37	86.3 (7)	H15—C16—C17	123.6 (10)
H1—Fe1—C38	172.7 (7)	C18—C17—C16	121.1 (2)
H2—Fe1—P1	76.9 (7)	H16—C17—C16	118.2 (10)
H2—Fe1—P2	80.8 (7)	H16—C17—C18	120.7 (10)
H2—Fe1—C37	169.2 (8)	C17—C18—C13	119.3 (2)
H2—Fe1—C38	89.9 (8)	H17—C18—C13	120.1 (10)
H2—Fe1—H1	83.0 (11)	H17—C18—C17	120.6 (10)
O1—P1—Fe1	120.10 (6)	C20—C19—O4	115.05 (17)
O2—P1—Fe1	113.99 (5)	C24—C19—O4	123.92 (18)
O2—P1—O1	98.11 (8)	C24—C19—C20	121.0 (2)
O3—P1—Fe1	121.58 (6)	C21—C20—C19	119.4 (2)
O3—P1—O1	95.79 (7)	H18—C20—C19	117.9 (10)
O3—P1—O2	103.21 (8)	H18—C20—C21	122.8 (10)
O4—P2—Fe1	120.25 (6)	C22—C21—C20	120.4 (2)
O5—P2—Fe1	111.50 (6)	H19—C21—C20	114.2 (10)
O5—P2—O4	98.98 (8)	H19—C21—C22	125.4 (10)
O6—P2—Fe1	123.04 (5)	C23—C22—C21	119.5 (2)
O6—P2—O4	96.68 (8)	H20—C22—C21	117.8 (9)
O6—P2—O5	102.49 (8)	H20—C22—C23	122.6 (9)
C1—O1—P1	126.70 (12)	C24—C23—C22	120.8 (2)
C7—O2—P1	123.71 (13)	H21—C23—C22	119.8 (10)
C13—O3—P1	124.36 (12)	H21—C23—C24	119.4 (10)
C19—O4—P2	127.98 (12)	C23—C24—C19	118.86 (19)
C25—O5—P2	124.78 (13)	H22—C24—C19	122.8 (10)
C31—O6—P2	130.45 (13)	H22—C24—C23	118.4 (10)
C2—C1—O1	119.53 (18)	C26—C25—O5	117.50 (19)
C6—C1—O1	118.60 (18)	C30—C25—O5	120.36 (19)
C6—C1—C2	121.61 (19)	C30—C25—C26	121.90 (19)
C3—C2—C1	119.1 (2)	C27—C26—C25	119.0 (2)
H3—C2—C1	120.4 (10)	H23—C26—C25	116.7 (9)
H3—C2—C3	120.5 (10)	H23—C26—C27	124.2 (9)
C4—C3—C2	120.3 (2)	C28—C27—C26	120.2 (2)
H4—C3—C2	118.9 (10)	H24—C27—C26	119.2 (10)
H4—C3—C4	120.7 (10)	H24—C27—C28	120.5 (9)
C5—C4—C3	119.9 (2)	C29—C28—C27	119.4 (2)
H5—C4—C3	121.0 (10)	H25—C28—C27	118.9 (10)
H5—C4—C5	119.1 (10)	H25—C28—C29	121.6 (10)
C6—C5—C4	120.5 (2)	C30—C29—C28	121.0 (2)
H6—C5—C4	121.1 (10)	H26—C29—C28	118.5 (10)
H6—C5—C6	118.4 (10)	H26—C29—C30	120.5 (10)
C5—C6—C1	118.6 (2)	C29—C30—C25	118.3 (2)
H7—C6—C1	120.8 (10)	H27—C30—C25	120.1 (9)
H7—C6—C5	120.6 (10)	H27—C30—C29	121.5 (9)
C8—C7—O2	117.94 (17)	C32—C31—O6	122.42 (18)
C12—C7—O2	120.20 (18)	C36—C31—O6	116.18 (19)
C12—C7—C8	121.81 (19)	C36—C31—C32	121.35 (19)
C9—C8—C7	118.7 (2)	C33—C32—C31	118.7 (2)
H8—C8—C7	118.9 (9)	H28—C32—C31	120.3 (10)
H8—C8—C9	122.4 (9)	H28—C32—C33	121.0 (10)
C10—C9—C8	120.4 (2)	C34—C33—C32	121.0 (2)
H9—C9—C8	118.6 (9)	H29—C33—C32	118.7 (10)
H9—C9—C10	120.8 (9)	H29—C33—C34	120.3 (9)
C11—C10—C9	119.7 (2)	C35—C34—C33	119.6 (2)
H10—C10—C9	120.7 (9)	H30—C34—C33	117.8 (10)
H10—C10—C11	119.6 (9)	H30—C34—C35	122.2 (10)
C12—C11—C10	120.5 (2)	C36—C35—C34	120.3 (2)
H11—C11—C10	121.8 (9)	H31—C35—C34	117.6 (10)
H11—C11—C12	117.7 (9)	H31—C35—C36	122.0 (10)
C11—C12—C7	118.9 (2)	C35—C36—C31	119.1 (2)
H12—C12—C7	120.0 (9)	H32—C36—C31	120.1 (9)
H12—C12—C11	121.0 (9)	H32—C36—C35	120.7 (9)
C14—C13—O3	116.57 (19)	O7—C37—Fe1	177.7 (2)
C18—C13—O3	123.01 (18)	O8—C38—Fe1	177.38 (19)
C18—C13—C14	120.37 (19)
Fe1—P1—O1—C1	−29.95 (11)	O5—C25—C30—C29	173.7 (2)
Fe1—P1—O2—C7	−157.44 (12)	O6—C31—C32—C33	−178.77 (19)
Fe1—P1—O3—C13	−50.70 (12)	O6—C31—C36—C35	178.52 (17)
Fe1—P2—O4—C19	−79.55 (11)	C1—C2—C3—C4	−0.1 (2)
Fe1—P2—O5—C25	171.72 (12)	C1—C6—C5—C4	0.2 (2)
Fe1—P2—O6—C31	−20.70 (12)	C2—C3—C4—C5	−0.5 (3)
P1—O1—C1—C2	−84.68 (17)	C3—C4—C5—C6	0.5 (3)
P1—O1—C1—C6	100.97 (17)	C7—C8—C9—C10	0.2 (3)
P1—O2—C7—C8	97.52 (17)	C7—C12—C11—C10	1.2 (3)
P1—O2—C7—C12	−84.84 (17)	C8—C9—C10—C11	−0.2 (3)
P1—O3—C13—C14	147.05 (17)	C9—C10—C11—C12	−0.6 (3)
P1—O3—C13—C18	−35.52 (18)	C13—C14—C15—C16	0.3 (3)
P2—O4—C19—C20	−170.49 (17)	C13—C18—C17—C16	0.8 (2)
P2—O4—C19—C24	9.41 (19)	C14—C15—C16—C17	−0.1 (3)
P2—O5—C25—C26	−105.51 (18)	C15—C16—C17—C18	−0.4 (3)
P2—O5—C25—C30	80.10 (17)	C19—C20—C21—C22	−0.5 (2)
P2—O6—C31—C32	−44.15 (19)	C19—C24—C23—C22	0.4 (2)
P2—O6—C31—C36	138.57 (18)	C20—C21—C22—C23	−0.3 (3)
O1—C1—C2—C3	−173.39 (17)	C21—C22—C23—C24	0.3 (3)
O1—C1—C6—C5	173.35 (18)	C25—C26—C27—C28	0.6 (3)
O2—C7—C8—C9	178.1 (2)	C25—C30—C29—C28	0.3 (3)
O2—C7—C12—C11	−178.8 (2)	C26—C27—C28—C29	−0.7 (3)
O3—C13—C14—C15	177.55 (19)	C27—C28—C29—C30	0.3 (3)
O3—C13—C18—C17	−177.91 (19)	C31—C32—C33—C34	1.1 (2)
O4—C19—C20—C21	−178.86 (17)	C31—C36—C35—C34	−0.3 (2)
O4—C19—C24—C23	178.9 (2)	C32—C33—C34—C35	−0.2 (2)
O5—C25—C26—C27	−174.3 (2)	C33—C34—C35—C36	−0.2 (2)

Dicarbonyl-cis-dihydrido-trans-bis(triphenylphosphite)iron(II) (QOSZON_HAR)

Crystal data

C38H32FeO8P2	Z = 2
Mr = 734.47	F(000) = 761.455
Triclinic, P1	Dx = 1.431 Mg m^−3
a = 9.6397 (12) Å	Mo Kα radiation, λ = 0.71073 Å
b = 10.4410 (13) Å	Cell parameters from 5000 reflections
c = 18.381 (2) Å	θ = 3.3–52.1°
α = 102.148 (15)°	µ = 0.59 mm^−1
β = 94.667 (15)°	T = 293 K
γ = 107.402 (14)°	Parallelepiped, colourless
V = 1705.0 (4) Å^3	0.5 × 0.25 × 0.1 mm

Data collection

STOE diffractometer	Rint = 0.034
Detector resolution: 1.60 pixels mm^-1	θmax = 26.1°, θmin = 2.1°
rotation en phi scans	h = −11→11
16806 measured reflections	k = −12→12
6202 independent reflections	l = −22→22
5084 reflections with I ≥ 2u(I)

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.019	All H-atom parameters refined
wR(F^2) = 0.049	w = 1/[σ^2(Fo^2) + (0.0387P)^2 + 0.3279P] where P = (Fo^2 + 2Fc^2)/3
S = 0.71	(Δ/σ)max = 0.0003
6202 reflections	Δρmax = 0.21 e Å^−3
720 parameters	Δρmin = −0.25 e Å^−3

Special details

Experimental. The crystal was pasted on a glass fiber, by using an oil-coated shock-cooled crystal.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Fe1	0.531700 (18)	0.836461 (19)	0.270676 (9)	0.01857 (5)
P1	0.35097 (3)	0.72595 (3)	0.185420 (17)	0.01849 (7)
P2	0.72500 (3)	1.00382 (3)	0.322139 (16)	0.01843 (7)
O1	0.30695 (9)	0.79743 (9)	0.12205 (5)	0.0249 (2)
O2	0.37093 (9)	0.59221 (9)	0.13042 (5)	0.02306 (19)
O3	0.18561 (9)	0.66714 (9)	0.20473 (5)	0.02385 (19)
O4	0.71935 (9)	1.12333 (9)	0.39185 (4)	0.02491 (19)
O5	0.84519 (9)	0.95249 (9)	0.36180 (5)	0.02383 (19)
O6	0.82086 (9)	1.10483 (9)	0.27664 (4)	0.0251 (2)
O7	0.40859 (13)	0.81930 (15)	0.41022 (6)	0.0555 (3)
O8	0.67923 (12)	0.62711 (12)	0.25559 (6)	0.0420 (3)
C1	0.32776 (12)	0.93697 (13)	0.13014 (6)	0.0199 (2)
C2	0.22444 (15)	0.99258 (15)	0.15932 (7)	0.0273 (3)
C3	0.23790 (17)	1.12932 (17)	0.15992 (8)	0.0354 (3)
C4	0.35461 (17)	1.20907 (17)	0.13207 (9)	0.0360 (3)
C5	0.45835 (16)	1.15169 (15)	0.10376 (8)	0.0332 (3)
C6	0.44562 (14)	1.01497 (15)	0.10274 (8)	0.0262 (3)
C7	0.29354 (13)	0.53190 (13)	0.05766 (7)	0.0216 (3)
C8	0.36313 (16)	0.56782 (16)	−0.00193 (8)	0.0310 (3)
C9	0.28950 (18)	0.50550 (16)	−0.07511 (8)	0.0373 (3)
C10	0.14816 (17)	0.40975 (16)	−0.08811 (8)	0.0358 (3)
C11	0.08159 (16)	0.37553 (16)	−0.02757 (8)	0.0355 (3)
C12	0.15454 (15)	0.43570 (15)	0.04597 (8)	0.0292 (3)
C13	0.14880 (12)	0.58912 (13)	0.25703 (7)	0.0215 (3)
C14	0.03546 (14)	0.60736 (17)	0.29570 (8)	0.0303 (3)
C15	−0.01101 (16)	0.52836 (18)	0.34676 (8)	0.0372 (3)
C16	0.05554 (16)	0.43227 (17)	0.35968 (8)	0.0349 (3)
C17	0.16844 (15)	0.41499 (16)	0.32058 (8)	0.0324 (3)
C18	0.21571 (14)	0.49274 (15)	0.26873 (8)	0.0270 (3)
C19	0.67137 (12)	1.23480 (13)	0.38984 (7)	0.0214 (3)
C20	0.70011 (14)	1.33291 (14)	0.45794 (7)	0.0264 (3)
C21	0.65349 (16)	1.44771 (16)	0.46203 (8)	0.0323 (3)
C22	0.57917 (16)	1.46453 (17)	0.39845 (8)	0.0337 (3)
C23	0.55266 (15)	1.36615 (15)	0.33055 (8)	0.0303 (3)
C24	0.59872 (14)	1.25051 (15)	0.32544 (7)	0.0259 (3)
C25	0.98949 (13)	1.03523 (13)	0.39226 (7)	0.0233 (3)
C26	1.09982 (15)	1.01457 (17)	0.35244 (9)	0.0343 (3)
C27	1.24576 (17)	1.08623 (19)	0.38418 (11)	0.0459 (4)
C28	1.27969 (16)	1.17640 (17)	0.45518 (10)	0.0442 (4)
C29	1.16712 (16)	1.19615 (16)	0.49417 (9)	0.0380 (4)
C30	1.02041 (16)	1.12556 (15)	0.46288 (8)	0.0286 (3)
C31	0.82803 (12)	1.08540 (13)	0.20076 (6)	0.0203 (3)
C32	0.83575 (13)	0.96238 (15)	0.15671 (7)	0.0246 (3)
C33	0.84568 (14)	0.95245 (17)	0.08078 (8)	0.0307 (3)
C34	0.84995 (14)	1.06359 (17)	0.04960 (8)	0.0321 (3)
C35	0.84397 (14)	1.18623 (16)	0.09476 (8)	0.0296 (3)
C36	0.83327 (13)	1.19797 (16)	0.17087 (8)	0.0253 (3)
C37	0.45601 (14)	0.82302 (15)	0.35562 (7)	0.0314 (3)
C38	0.61936 (14)	0.70733 (14)	0.26258 (7)	0.0264 (3)
H1	0.4673 (18)	0.9519 (18)	0.2688 (9)	0.040 (5)*
H2	0.5855 (18)	0.8741 (18)	0.2010 (9)	0.040 (5)*
H3	0.134 (2)	0.928 (2)	0.1806 (12)	0.060 (6)
H4	0.153 (2)	1.174 (2)	0.1811 (12)	0.066 (6)
H5	0.364 (2)	1.316 (2)	0.1313 (13)	0.068 (7)
H6	0.550 (2)	1.215 (2)	0.0813 (13)	0.071 (7)
H7	0.527 (2)	0.970 (2)	0.0792 (12)	0.060 (6)
H8	0.475 (2)	0.644 (2)	0.0110 (10)	0.059 (6)
H9	0.343 (3)	0.529 (2)	−0.1232 (11)	0.083 (8)
H10	0.094 (2)	0.364 (2)	−0.1458 (9)	0.064 (6)
H11	−0.030 (2)	0.301 (3)	−0.0379 (11)	0.082 (8)
H12	0.104 (2)	0.407 (2)	0.0925 (11)	0.057 (6)
H13	−0.012 (2)	0.685 (2)	0.2856 (12)	0.064 (6)
H14	−0.101 (2)	0.540 (2)	0.3762 (12)	0.068 (6)
H15	0.016 (2)	0.370 (2)	0.4000 (13)	0.071 (7)
H16	0.220 (2)	0.338 (2)	0.3295 (12)	0.062 (6)
H17	0.3003 (19)	0.477 (2)	0.2355 (11)	0.051 (5)
H18	0.7612 (19)	1.3172 (19)	0.5068 (9)	0.043 (5)
H19	0.677 (2)	1.521 (2)	0.5153 (10)	0.068 (6)
H20	0.545 (2)	1.555 (2)	0.4028 (11)	0.064 (6)
H21	0.494 (2)	1.3784 (19)	0.2807 (10)	0.050 (5)
H22	0.574 (2)	1.1757 (19)	0.2703 (9)	0.051 (5)
H23	1.069 (2)	0.941 (2)	0.2966 (11)	0.063 (6)
H24	1.331 (2)	1.069 (3)	0.3519 (16)	0.092 (9)
H25	1.397 (2)	1.231 (2)	0.4810 (13)	0.075 (7)
H26	1.194 (2)	1.267 (2)	0.5506 (11)	0.065 (6)
H27	0.9331 (19)	1.142 (2)	0.4932 (10)	0.048 (5)
H28	0.832 (2)	0.8719 (19)	0.1806 (11)	0.051 (5)
H29	0.849 (2)	0.855 (2)	0.0460 (11)	0.066 (6)
H30	0.856 (2)	1.055 (2)	−0.0095 (10)	0.064 (6)
H31	0.847 (2)	1.273 (2)	0.0708 (11)	0.061 (6)
H32	0.828 (2)	1.2954 (19)	0.2062 (10)	0.045 (5)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Fe1	0.01700 (9)	0.01950 (10)	0.01715 (8)	0.00251 (7)	0.00086 (6)	0.00583 (7)
P1	0.01706 (14)	0.01744 (17)	0.01934 (14)	0.00281 (12)	0.00015 (11)	0.00615 (12)
P2	0.01853 (14)	0.01844 (17)	0.01605 (14)	0.00314 (12)	0.00126 (11)	0.00411 (12)
O1	0.0296 (5)	0.0192 (5)	0.0221 (4)	0.0037 (4)	−0.0044 (3)	0.0066 (4)
O2	0.0226 (4)	0.0213 (5)	0.0238 (4)	0.0070 (4)	−0.0004 (3)	0.0041 (4)
O3	0.0175 (4)	0.0258 (5)	0.0295 (4)	0.0054 (3)	0.0031 (3)	0.0121 (4)
O4	0.0306 (5)	0.0258 (5)	0.0181 (4)	0.0107 (4)	0.0020 (3)	0.0034 (4)
O5	0.0203 (4)	0.0219 (5)	0.0261 (4)	0.0036 (3)	−0.0024 (3)	0.0061 (4)
O6	0.0278 (4)	0.0226 (5)	0.0191 (4)	−0.0003 (4)	0.0036 (3)	0.0050 (4)
O7	0.0532 (7)	0.0766 (9)	0.0289 (6)	0.0029 (6)	0.0173 (5)	0.0186 (6)
O8	0.0430 (6)	0.0343 (6)	0.0522 (6)	0.0210 (5)	0.0021 (5)	0.0081 (5)
C1	0.0204 (6)	0.0203 (7)	0.0197 (5)	0.0064 (5)	0.0026 (4)	0.0071 (5)
C2	0.0266 (7)	0.0312 (8)	0.0263 (6)	0.0115 (6)	0.0075 (5)	0.0071 (6)
C3	0.0392 (8)	0.0337 (9)	0.0357 (7)	0.0197 (7)	0.0045 (6)	0.0025 (7)
C4	0.0410 (8)	0.0232 (8)	0.0437 (8)	0.0121 (7)	−0.0039 (6)	0.0092 (7)
C5	0.0292 (7)	0.0249 (8)	0.0467 (8)	0.0046 (6)	0.0031 (6)	0.0181 (7)
C6	0.0225 (6)	0.0256 (8)	0.0339 (7)	0.0075 (5)	0.0071 (5)	0.0142 (6)
C7	0.0205 (6)	0.0188 (7)	0.0238 (6)	0.0053 (5)	0.0007 (5)	0.0038 (5)
C8	0.0345 (8)	0.0286 (8)	0.0255 (7)	0.0043 (6)	0.0046 (6)	0.0063 (6)
C9	0.0520 (9)	0.0323 (9)	0.0231 (7)	0.0095 (7)	0.0028 (6)	0.0040 (6)
C10	0.0459 (8)	0.0294 (8)	0.0265 (7)	0.0127 (7)	−0.0065 (6)	−0.0009 (6)
C11	0.0299 (7)	0.0313 (8)	0.0337 (7)	0.0038 (6)	−0.0070 (6)	−0.0032 (6)
C12	0.0239 (7)	0.0254 (8)	0.0302 (7)	0.0008 (6)	0.0004 (6)	0.0013 (6)
C13	0.0167 (5)	0.0205 (7)	0.0263 (6)	0.0036 (5)	0.0034 (4)	0.0072 (5)
C14	0.0258 (7)	0.0331 (9)	0.0352 (7)	0.0104 (6)	0.0107 (5)	0.0115 (6)
C15	0.0315 (7)	0.0447 (10)	0.0382 (8)	0.0095 (7)	0.0166 (6)	0.0160 (7)
C16	0.0333 (7)	0.0360 (9)	0.0323 (7)	0.0021 (6)	0.0074 (6)	0.0141 (7)
C17	0.0338 (7)	0.0296 (8)	0.0355 (7)	0.0076 (6)	0.0052 (6)	0.0160 (6)
C18	0.0260 (6)	0.0254 (8)	0.0339 (7)	0.0092 (5)	0.0080 (5)	0.0140 (6)
C19	0.0220 (6)	0.0204 (7)	0.0193 (6)	0.0046 (5)	0.0029 (4)	0.0029 (5)
C20	0.0308 (7)	0.0223 (7)	0.0215 (6)	0.0042 (5)	0.0056 (5)	0.0014 (5)
C21	0.0394 (7)	0.0242 (8)	0.0294 (7)	0.0079 (6)	0.0099 (6)	0.0000 (6)
C22	0.0382 (8)	0.0244 (8)	0.0386 (8)	0.0126 (6)	0.0089 (6)	0.0034 (7)
C23	0.0317 (7)	0.0229 (7)	0.0347 (7)	0.0094 (6)	−0.0007 (6)	0.0052 (6)
C24	0.0271 (6)	0.0244 (8)	0.0236 (6)	0.0075 (5)	−0.0016 (5)	0.0035 (6)
C25	0.0203 (6)	0.0215 (7)	0.0251 (6)	0.0033 (5)	−0.0001 (5)	0.0059 (5)
C26	0.0242 (7)	0.0369 (9)	0.0400 (8)	0.0082 (6)	0.0074 (6)	0.0074 (7)
C27	0.0218 (7)	0.0458 (11)	0.0684 (11)	0.0065 (7)	0.0087 (7)	0.0167 (9)
C28	0.0219 (7)	0.0372 (9)	0.0653 (11)	−0.0021 (7)	−0.0058 (7)	0.0171 (8)
C29	0.0320 (8)	0.0283 (8)	0.0410 (8)	−0.0023 (6)	−0.0122 (7)	0.0062 (7)
C30	0.0261 (7)	0.0258 (8)	0.0279 (7)	0.0031 (6)	−0.0029 (6)	0.0042 (6)
C31	0.0188 (5)	0.0210 (7)	0.0200 (5)	0.0046 (5)	0.0022 (4)	0.0060 (5)
C32	0.0269 (6)	0.0254 (8)	0.0230 (6)	0.0101 (5)	0.0074 (5)	0.0059 (6)
C33	0.0331 (7)	0.0358 (9)	0.0239 (7)	0.0132 (6)	0.0075 (5)	0.0048 (6)
C34	0.0309 (7)	0.0459 (10)	0.0207 (7)	0.0115 (6)	0.0059 (5)	0.0114 (6)
C35	0.0287 (6)	0.0368 (9)	0.0285 (7)	0.0103 (6)	0.0068 (5)	0.0184 (7)
C36	0.0263 (6)	0.0241 (8)	0.0268 (6)	0.0058 (5)	0.0056 (5)	0.0117 (6)
C37	0.0286 (6)	0.0386 (8)	0.0234 (7)	0.0035 (6)	0.0042 (5)	0.0108 (6)
C38	0.0248 (6)	0.0236 (8)	0.0299 (6)	0.0070 (6)	0.0008 (5)	0.0071 (6)
H3	0.051 (12)	0.055 (15)	0.074 (15)	0.012 (11)	0.028 (11)	0.016 (12)
H4	0.065 (15)	0.063 (17)	0.074 (15)	0.032 (13)	0.024 (12)	0.004 (12)
H5	0.057 (13)	0.035 (13)	0.109 (18)	0.008 (11)	−0.005 (12)	0.029 (13)
H6	0.051 (13)	0.052 (14)	0.114 (19)	−0.003 (11)	0.021 (12)	0.055 (14)
H7	0.068 (14)	0.068 (17)	0.072 (15)	0.044 (13)	0.035 (12)	0.038 (13)
H8	0.043 (12)	0.054 (14)	0.054 (12)	−0.008 (11)	0.019 (10)	−0.009 (10)
H9	0.13 (2)	0.080 (18)	0.027 (11)	0.026 (16)	0.017 (13)	0.002 (11)
H10	0.089 (15)	0.071 (15)	0.020 (10)	0.033 (13)	−0.021 (10)	−0.012 (10)
H11	0.043 (13)	0.10 (2)	0.058 (14)	−0.012 (13)	−0.010 (11)	−0.009 (13)
H12	0.044 (12)	0.070 (16)	0.047 (12)	0.002 (10)	0.014 (10)	0.010 (11)
H13	0.075 (15)	0.063 (16)	0.077 (15)	0.046 (13)	0.021 (12)	0.026 (13)
H14	0.064 (14)	0.082 (18)	0.075 (15)	0.031 (13)	0.043 (12)	0.033 (13)
H15	0.076 (16)	0.071 (17)	0.085 (16)	0.027 (13)	0.030 (13)	0.047 (14)
H16	0.078 (15)	0.054 (15)	0.077 (15)	0.042 (12)	0.013 (12)	0.036 (13)
H17	0.042 (11)	0.056 (14)	0.066 (13)	0.022 (10)	0.027 (10)	0.022 (11)
H18	0.054 (12)	0.040 (12)	0.027 (10)	0.015 (10)	−0.008 (9)	−0.005 (9)
H19	0.102 (17)	0.051 (14)	0.038 (11)	0.028 (13)	0.005 (11)	−0.016 (10)
H20	0.083 (16)	0.047 (15)	0.069 (14)	0.047 (13)	0.000 (11)	−0.006 (12)
H21	0.063 (13)	0.040 (12)	0.050 (11)	0.026 (10)	−0.014 (10)	0.016 (10)
H22	0.081 (15)	0.033 (12)	0.029 (10)	0.009 (11)	−0.007 (10)	0.000 (9)
H23	0.067 (14)	0.065 (16)	0.047 (13)	0.014 (12)	0.022 (11)	−0.002 (11)
H24	0.026 (12)	0.10 (2)	0.15 (2)	0.023 (12)	0.024 (14)	0.024 (18)
H25	0.025 (11)	0.083 (18)	0.104 (18)	−0.001 (11)	−0.005 (11)	0.032 (15)
H26	0.066 (14)	0.057 (15)	0.053 (13)	0.011 (12)	−0.017 (11)	−0.004 (12)
H27	0.042 (11)	0.059 (15)	0.043 (11)	0.010 (10)	0.014 (9)	0.015 (10)
H28	0.059 (13)	0.038 (12)	0.073 (14)	0.022 (10)	0.026 (11)	0.033 (11)
H29	0.109 (19)	0.041 (14)	0.049 (12)	0.037 (13)	0.025 (12)	−0.010 (11)
H30	0.078 (15)	0.098 (19)	0.034 (11)	0.045 (13)	0.026 (10)	0.022 (11)
H31	0.086 (16)	0.060 (14)	0.067 (14)	0.038 (12)	0.025 (12)	0.048 (12)
H32	0.062 (13)	0.023 (11)	0.042 (11)	0.016 (10)	0.006 (9)	−0.012 (9)

Geometric parameters (Å, º)

Fe1—P1	2.1011 (6)	C13—C18	1.3899 (18)
Fe1—P2	2.1190 (6)	C14—C15	1.391 (2)
Fe1—C37	1.7906 (14)	C14—H13	1.08 (2)
Fe1—C38	1.7808 (15)	C15—C16	1.391 (2)
Fe1—H1	1.517 (17)	C15—H14	1.080 (19)
Fe1—H2	1.503 (16)	C16—C17	1.387 (2)
P1—O1	1.6027 (8)	C16—H15	1.11 (2)
P1—O2	1.6147 (10)	C17—C18	1.3964 (19)
P1—O3	1.6255 (9)	C17—H16	1.091 (18)
P2—O4	1.6066 (10)	C18—H17	1.088 (17)
P2—O5	1.5997 (9)	C19—C20	1.3882 (18)
P2—O6	1.6061 (9)	C19—C24	1.3908 (17)
O1—C1	1.3835 (15)	C20—C21	1.391 (2)
O2—C7	1.3943 (14)	C20—H18	1.102 (16)
O3—C13	1.3878 (14)	C21—C22	1.391 (2)
O4—C19	1.3810 (16)	C21—H19	1.070 (18)
O5—C25	1.3949 (14)	C22—C23	1.389 (2)
O6—C31	1.3770 (14)	C22—H20	1.08 (2)
O7—C37	1.1393 (17)	C23—C24	1.394 (2)
O8—C38	1.1433 (17)	C23—H21	1.089 (16)
C1—C2	1.3851 (18)	C24—H22	1.100 (17)
C1—C6	1.3857 (17)	C25—C26	1.382 (2)
C2—C3	1.392 (2)	C25—C30	1.3846 (19)
C2—H3	1.091 (19)	C26—C27	1.390 (2)
C3—C4	1.391 (2)	C26—H23	1.102 (19)
C3—H4	1.11 (2)	C27—C28	1.388 (3)
C4—C5	1.393 (2)	C27—H24	1.09 (2)
C4—H5	1.095 (19)	C28—C29	1.390 (2)
C5—C6	1.392 (2)	C28—H25	1.114 (18)
C5—H6	1.101 (18)	C29—C30	1.3928 (19)
C6—H7	1.098 (19)	C29—H26	1.099 (19)
C7—C8	1.3900 (18)	C30—H27	1.082 (18)
C7—C12	1.3813 (18)	C31—C32	1.393 (2)
C8—C9	1.392 (2)	C31—C36	1.3881 (18)
C8—H8	1.104 (17)	C32—C33	1.3909 (18)
C9—C10	1.394 (2)	C32—H28	1.114 (17)
C9—H9	1.10 (2)	C33—C34	1.390 (2)
C10—C11	1.387 (2)	C33—H29	1.09 (2)
C10—H10	1.084 (15)	C34—C35	1.392 (2)
C11—C12	1.3928 (19)	C34—H30	1.078 (17)
C11—H11	1.10 (2)	C35—C36	1.3935 (19)
C12—H12	1.072 (19)	C35—H31	1.078 (17)
C13—C14	1.3889 (18)	C36—H32	1.103 (18)
P2—Fe1—P1	154.359 (15)	C15—C14—C13	119.47 (14)
C37—Fe1—P1	103.49 (4)	H13—C14—C13	118.2 (11)
C37—Fe1—P2	95.98 (4)	H13—C14—C15	122.3 (11)
C38—Fe1—P1	97.50 (4)	C16—C15—C14	120.64 (14)
C38—Fe1—P2	95.04 (4)	H14—C15—C14	120.4 (11)
C38—Fe1—C37	100.77 (6)	H14—C15—C16	119.0 (11)
H1—Fe1—P1	81.6 (6)	C17—C16—C15	119.27 (14)
H1—Fe1—P2	82.9 (6)	H15—C16—C15	119.5 (11)
H1—Fe1—C37	86.9 (6)	H15—C16—C17	121.2 (11)
H1—Fe1—C38	172.2 (6)	C18—C17—C16	120.82 (15)
H2—Fe1—P1	76.5 (6)	H16—C17—C16	119.9 (11)
H2—Fe1—P2	81.0 (6)	H16—C17—C18	119.3 (11)
H2—Fe1—C37	168.1 (7)	C17—C18—C13	119.10 (13)
H2—Fe1—C38	91.0 (7)	H17—C18—C13	118.9 (10)
H2—Fe1—H1	81.3 (9)	H17—C18—C17	122.0 (10)
O1—P1—Fe1	120.12 (3)	C20—C19—O4	115.07 (11)
O2—P1—Fe1	113.90 (3)	C24—C19—O4	123.84 (11)
O2—P1—O1	98.15 (5)	C24—C19—C20	121.09 (13)
O3—P1—Fe1	121.61 (3)	C21—C20—C19	119.41 (13)
O3—P1—O1	95.78 (4)	H18—C20—C19	118.2 (9)
O3—P1—O2	103.25 (5)	H18—C20—C21	122.4 (9)
O4—P2—Fe1	120.24 (4)	C22—C21—C20	120.39 (14)
O5—P2—Fe1	111.53 (4)	H19—C21—C20	117.9 (12)
O5—P2—O4	99.03 (5)	H19—C21—C22	121.8 (12)
O6—P2—Fe1	123.05 (3)	C23—C22—C21	119.48 (15)
O6—P2—O4	96.64 (5)	H20—C22—C21	119.2 (10)
O6—P2—O5	102.44 (5)	H20—C22—C23	121.3 (10)
C1—O1—P1	126.76 (7)	C24—C23—C22	120.88 (13)
C7—O2—P1	123.58 (8)	H21—C23—C22	119.8 (10)
C13—O3—P1	124.37 (7)	H21—C23—C24	119.3 (10)
C19—O4—P2	127.99 (7)	C23—C24—C19	118.75 (13)
C25—O5—P2	124.87 (8)	H22—C24—C19	123.7 (10)
C31—O6—P2	130.42 (8)	H22—C24—C23	117.5 (10)
C2—C1—O1	119.57 (11)	C26—C25—O5	117.53 (12)
C6—C1—O1	118.65 (11)	C30—C25—O5	120.46 (12)
C6—C1—C2	121.55 (12)	C30—C25—C26	121.77 (12)
C3—C2—C1	119.22 (13)	C27—C26—C25	119.14 (15)
H3—C2—C1	119.2 (11)	H23—C26—C25	118.5 (10)
H3—C2—C3	121.6 (11)	H23—C26—C27	122.3 (10)
C4—C3—C2	120.17 (15)	C28—C27—C26	120.20 (16)
H4—C3—C2	120.0 (12)	H24—C27—C26	118.2 (13)
H4—C3—C4	119.8 (12)	H24—C27—C28	121.6 (13)
C5—C4—C3	119.73 (14)	C29—C28—C27	119.76 (14)
H5—C4—C3	120.2 (12)	H25—C28—C27	119.8 (13)
H5—C4—C5	120.0 (12)	H25—C28—C29	120.4 (13)
C6—C5—C4	120.53 (14)	C30—C29—C28	120.63 (15)
H6—C5—C4	119.5 (12)	H26—C29—C28	119.9 (11)
H6—C5—C6	120.0 (12)	H26—C29—C30	119.5 (11)
C5—C6—C1	118.80 (13)	C29—C30—C25	118.49 (15)
H7—C6—C1	121.3 (11)	H27—C30—C25	121.1 (9)
H7—C6—C5	119.9 (11)	H27—C30—C29	120.4 (9)
C8—C7—O2	117.85 (11)	C32—C31—O6	122.40 (11)
C12—C7—O2	120.34 (11)	C36—C31—O6	116.08 (12)
C12—C7—C8	121.76 (12)	C36—C31—C32	121.47 (12)
C9—C8—C7	118.72 (13)	C33—C32—C31	118.67 (13)
H8—C8—C7	118.4 (10)	H28—C32—C31	121.6 (11)
H8—C8—C9	122.9 (10)	H28—C32—C33	119.7 (11)
C10—C9—C8	120.44 (14)	C34—C33—C32	120.77 (15)
H9—C9—C8	120.2 (12)	H29—C33—C32	118.6 (11)
H9—C9—C10	119.3 (12)	H29—C33—C34	120.6 (11)
C11—C10—C9	119.59 (13)	C35—C34—C33	119.70 (13)
H10—C10—C9	118.4 (12)	H30—C34—C33	120.5 (12)
H10—C10—C11	122.0 (12)	H30—C34—C35	119.8 (12)
C12—C11—C10	120.67 (14)	C36—C35—C34	120.38 (14)
H11—C11—C10	119.5 (11)	H31—C35—C34	120.0 (11)
H11—C11—C12	119.9 (11)	H31—C35—C36	119.6 (11)
C11—C12—C7	118.81 (14)	C35—C36—C31	119.00 (14)
H12—C12—C7	120.7 (10)	H32—C36—C31	121.1 (9)
H12—C12—C11	120.5 (10)	H32—C36—C35	119.9 (9)
C14—C13—O3	116.47 (12)	O7—C37—Fe1	177.61 (15)
C18—C13—O3	122.78 (11)	O8—C38—Fe1	177.23 (12)
C18—C13—C14	120.69 (12)
Fe1—P1—O1—C1	−29.97 (7)	O5—C25—C30—C29	173.82 (12)
Fe1—P1—O2—C7	−157.60 (7)	O6—C31—C32—C33	−178.72 (11)
Fe1—P1—O3—C13	−50.55 (7)	O6—C31—C36—C35	178.57 (10)
Fe1—P2—O4—C19	−79.77 (7)	C1—C2—C3—C4	−0.54 (14)
Fe1—P2—O5—C25	171.81 (8)	C1—C6—C5—C4	0.21 (15)
Fe1—P2—O6—C31	−20.81 (7)	C2—C3—C4—C5	−0.20 (16)
P1—O1—C1—C2	−84.58 (10)	C3—C4—C5—C6	0.37 (16)
P1—O1—C1—C6	100.85 (10)	C7—C8—C9—C10	0.50 (17)
P1—O2—C7—C8	97.71 (11)	C7—C12—C11—C10	1.07 (17)
P1—O2—C7—C12	−84.75 (11)	C8—C9—C10—C11	−0.72 (19)
P1—O3—C13—C14	147.08 (11)	C9—C10—C11—C12	−0.07 (18)
P1—O3—C13—C18	−35.69 (11)	C13—C14—C15—C16	0.42 (16)
P2—O4—C19—C20	−170.54 (10)	C13—C18—C17—C16	0.51 (15)
P2—O4—C19—C24	9.75 (11)	C14—C15—C16—C17	−0.52 (17)
P2—O5—C25—C26	−105.56 (11)	C15—C16—C17—C18	0.05 (17)
P2—O5—C25—C30	79.95 (11)	C19—C20—C21—C22	−0.22 (15)
P2—O6—C31—C32	−43.98 (12)	C19—C24—C23—C22	0.32 (15)
P2—O6—C31—C36	138.57 (11)	C20—C21—C22—C23	−0.46 (16)
O1—C1—C2—C3	−173.26 (11)	C21—C22—C23—C24	0.41 (16)
O1—C1—C6—C5	173.48 (11)	C25—C26—C27—C28	0.50 (18)
O2—C7—C8—C9	178.04 (13)	C25—C30—C29—C28	0.15 (16)
O2—C7—C12—C11	−178.75 (13)	C26—C27—C28—C29	−0.8 (2)
O3—C13—C14—C15	177.45 (12)	C27—C28—C29—C30	0.43 (19)
O3—C13—C18—C17	−177.73 (12)	C31—C32—C33—C34	0.90 (14)
O4—C19—C20—C21	−178.75 (11)	C31—C36—C35—C34	−0.28 (14)
O4—C19—C24—C23	178.68 (12)	C32—C33—C34—C35	−0.11 (15)
O5—C25—C26—C27	−174.31 (13)	C33—C34—C35—C36	−0.20 (15)

(QOSZON_HAR_NoMoRe_1)

Crystal data

C38H32FeO8P2	Z = 2
Mr = 734.47	F(000) = 761.455
Triclinic, P1	Dx = 1.431 Mg m^−3
a = 9.6397 (12) Å	Mo Kα radiation, λ = 0.71073 Å
b = 10.4410 (13) Å	Cell parameters from 5000 reflections
c = 18.381 (2) Å	θ = 3.3–52.1°
α = 102.148 (15)°	µ = 0.59 mm^−1
β = 94.667 (15)°	T = 293 K
γ = 107.402 (14)°	Parallelepiped, colourless
V = 1705.0 (4) Å^3	0.5 × 0.25 × 0.1 mm

Data collection

STOE diffractometer	Rint = 0.034
rotation en phi scans	θmax = 26.1°, θmin = 2.1°
16806 measured reflections	h = −11→11
6202 independent reflections	k = −12→12
5084 reflections with I ≥ 2u(I)	l = −22→22

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.019	Only H-atom coordinates refined
wR(F^2) = 0.049	w = 1/[σ^2(Fo^2) + (0.0387P)^2 + 0.3279P] where P = (Fo^2 + 2Fc^2)/3
S = 0.71	(Δ/σ)max = 0.0004
6202 reflections	Δρmax = 0.21 e Å^−3
538 parameters	Δρmin = −0.25 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Fe1	0.531702 (17)	0.836466 (18)	0.270676 (9)	0.01852 (5)
P1	0.35096 (3)	0.72595 (3)	0.185419 (16)	0.01844 (7)
P2	0.72501 (3)	1.00381 (3)	0.322137 (16)	0.01839 (7)
O1	0.30698 (9)	0.79743 (9)	0.12204 (5)	0.02483 (19)
O2	0.37091 (9)	0.59219 (9)	0.13042 (5)	0.02300 (19)
O3	0.18561 (8)	0.66712 (9)	0.20472 (5)	0.02381 (19)
O4	0.71936 (9)	1.12334 (9)	0.39186 (4)	0.02485 (19)
O5	0.84517 (9)	0.95249 (9)	0.36179 (5)	0.02381 (19)
O6	0.82086 (9)	1.10483 (9)	0.27663 (4)	0.0251 (2)
O7	0.40859 (13)	0.81929 (14)	0.41022 (6)	0.0554 (3)
O8	0.67921 (11)	0.62709 (12)	0.25559 (6)	0.0419 (3)
C1	0.32777 (12)	0.93698 (13)	0.13015 (6)	0.0199 (2)
C2	0.22442 (14)	0.99258 (15)	0.15930 (7)	0.0273 (3)
C3	0.23792 (16)	1.12921 (16)	0.15991 (8)	0.0354 (3)
C4	0.35456 (16)	1.20904 (15)	0.13208 (8)	0.0360 (3)
C5	0.45825 (15)	1.15169 (15)	0.10377 (8)	0.0332 (3)
C6	0.44561 (13)	1.01497 (14)	0.10272 (7)	0.0262 (3)
C7	0.29356 (13)	0.53190 (13)	0.05765 (7)	0.0216 (3)
C8	0.36308 (15)	0.56781 (15)	−0.00193 (7)	0.0310 (3)
C9	0.28941 (17)	0.50547 (16)	−0.07511 (8)	0.0372 (3)
C10	0.14820 (17)	0.40980 (15)	−0.08809 (8)	0.0357 (3)
C11	0.08163 (15)	0.37552 (16)	−0.02756 (8)	0.0354 (3)
C12	0.15460 (14)	0.43573 (14)	0.04596 (8)	0.0291 (3)
C13	0.14880 (12)	0.58912 (13)	0.25702 (7)	0.0214 (3)
C14	0.03549 (14)	0.60726 (16)	0.29569 (8)	0.0303 (3)
C15	−0.01099 (15)	0.52833 (17)	0.34674 (8)	0.0372 (3)
C16	0.05555 (15)	0.43223 (16)	0.35968 (8)	0.0348 (3)
C17	0.16841 (15)	0.41507 (15)	0.32055 (8)	0.0324 (3)
C18	0.21564 (14)	0.49275 (14)	0.26876 (7)	0.0270 (3)
C19	0.67137 (12)	1.23481 (13)	0.38984 (6)	0.0214 (3)
C20	0.70012 (14)	1.33293 (14)	0.45796 (7)	0.0264 (3)
C21	0.65345 (15)	1.44764 (15)	0.46201 (8)	0.0323 (3)
C22	0.57915 (15)	1.46445 (16)	0.39845 (8)	0.0337 (3)
C23	0.55264 (14)	1.36611 (15)	0.33055 (8)	0.0303 (3)
C24	0.59872 (13)	1.25051 (14)	0.32545 (7)	0.0259 (3)
C25	0.98949 (13)	1.03524 (13)	0.39225 (7)	0.0233 (3)
C26	1.09981 (15)	1.01461 (16)	0.35244 (8)	0.0342 (3)
C27	1.24576 (16)	1.08632 (19)	0.38423 (11)	0.0457 (4)
C28	1.27967 (15)	1.17640 (17)	0.45518 (10)	0.0441 (4)
C29	1.16708 (16)	1.19615 (15)	0.49416 (9)	0.0379 (4)
C30	1.02043 (15)	1.12551 (14)	0.46285 (7)	0.0286 (3)
C31	0.82804 (12)	1.08538 (13)	0.20077 (6)	0.0203 (2)
C32	0.83574 (13)	0.96241 (14)	0.15670 (7)	0.0245 (3)
C33	0.84571 (14)	0.95257 (16)	0.08083 (7)	0.0307 (3)
C34	0.84995 (14)	1.06358 (17)	0.04960 (7)	0.0320 (3)
C35	0.84395 (14)	1.18618 (16)	0.09477 (7)	0.0296 (3)
C36	0.83326 (13)	1.19783 (14)	0.17083 (7)	0.0253 (3)
C37	0.45604 (14)	0.82302 (15)	0.35563 (7)	0.0314 (3)
C38	0.61937 (13)	0.70735 (14)	0.26257 (7)	0.0264 (3)
H1	0.4679 (19)	0.9516 (18)	0.2688 (10)	0.045061
H2	0.5857 (18)	0.874 (2)	0.2013 (9)	0.045787
H3	0.134 (2)	0.928 (2)	0.1807 (10)	0.053059
H4	0.153 (2)	1.174 (2)	0.1813 (11)	0.061152
H5	0.364 (2)	1.3154 (19)	0.1309 (11)	0.058949
H6	0.5501 (19)	1.214 (2)	0.0810 (12)	0.061456
H7	0.5269 (19)	0.971 (2)	0.0793 (11)	0.052226
H8	0.4750 (18)	0.644 (2)	0.0108 (10)	0.046232
H9	0.343 (2)	0.528 (2)	−0.1232 (10)	0.059017
H10	0.092 (2)	0.364 (2)	−0.1456 (10)	0.067339
H11	−0.031 (2)	0.300 (2)	−0.0379 (11)	0.065807
H12	0.1047 (18)	0.407 (2)	0.0927 (10)	0.053730
H13	−0.011 (2)	0.685 (2)	0.2857 (11)	0.052450
H14	−0.100 (2)	0.539 (2)	0.3763 (11)	0.063191
H15	0.015 (2)	0.369 (2)	0.4002 (11)	0.062925
H16	0.219 (2)	0.338 (2)	0.3295 (11)	0.057289
H17	0.2998 (19)	0.477 (2)	0.2356 (10)	0.049260
H18	0.761 (2)	1.3172 (19)	0.5068 (9)	0.048171
H19	0.677 (2)	1.522 (2)	0.5153 (10)	0.055836
H20	0.545 (2)	1.555 (2)	0.4026 (11)	0.056627
H21	0.494 (2)	1.379 (2)	0.2807 (10)	0.058423
H22	0.573 (2)	1.1758 (19)	0.2702 (10)	0.051213
H23	1.069 (2)	0.941 (2)	0.2968 (11)	0.062344
H24	1.332 (2)	1.069 (2)	0.3520 (14)	0.078902
H25	1.397 (2)	1.231 (2)	0.4811 (13)	0.073811
H26	1.193 (2)	1.266 (2)	0.5506 (11)	0.062575
H27	0.9336 (19)	1.1418 (19)	0.4933 (9)	0.045956
H28	0.8319 (19)	0.8730 (18)	0.1806 (10)	0.046353
H29	0.850 (2)	0.855 (2)	0.0461 (10)	0.057435
H30	0.855 (2)	1.054 (2)	−0.0098 (9)	0.059463
H31	0.846 (2)	1.272 (2)	0.0704 (10)	0.054601
H32	0.829 (2)	1.2949 (19)	0.2061 (10)	0.048066

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Fe1	0.01693 (8)	0.01946 (10)	0.01711 (8)	0.00248 (7)	0.00084 (6)	0.00581 (7)
P1	0.01703 (14)	0.01740 (16)	0.01928 (14)	0.00281 (12)	0.00016 (11)	0.00614 (12)
P2	0.01851 (14)	0.01839 (17)	0.01599 (14)	0.00315 (12)	0.00128 (11)	0.00409 (12)
O1	0.0296 (5)	0.0191 (5)	0.0221 (4)	0.0037 (4)	−0.0044 (3)	0.0066 (4)
O2	0.0225 (4)	0.0212 (5)	0.0238 (4)	0.0070 (4)	−0.0005 (3)	0.0041 (4)
O3	0.0174 (4)	0.0258 (5)	0.0295 (4)	0.0054 (3)	0.0031 (3)	0.0120 (4)
O4	0.0305 (5)	0.0257 (5)	0.0181 (4)	0.0107 (4)	0.0020 (3)	0.0033 (4)
O5	0.0202 (4)	0.0219 (5)	0.0261 (4)	0.0035 (3)	−0.0024 (3)	0.0061 (4)
O6	0.0277 (4)	0.0226 (5)	0.0191 (4)	−0.0003 (4)	0.0036 (3)	0.0050 (4)
O7	0.0531 (7)	0.0766 (9)	0.0288 (5)	0.0028 (6)	0.0173 (5)	0.0186 (6)
O8	0.0429 (6)	0.0343 (6)	0.0522 (6)	0.0209 (5)	0.0021 (5)	0.0081 (5)
C1	0.0204 (6)	0.0204 (6)	0.0196 (5)	0.0064 (5)	0.0025 (4)	0.0071 (5)
C2	0.0265 (6)	0.0312 (8)	0.0262 (6)	0.0116 (6)	0.0076 (5)	0.0070 (6)
C3	0.0393 (8)	0.0336 (9)	0.0357 (7)	0.0200 (7)	0.0046 (6)	0.0023 (6)
C4	0.0408 (8)	0.0230 (8)	0.0439 (8)	0.0119 (6)	−0.0040 (6)	0.0094 (6)
C5	0.0289 (7)	0.0251 (8)	0.0467 (8)	0.0046 (6)	0.0033 (6)	0.0182 (7)
C6	0.0223 (6)	0.0257 (7)	0.0341 (6)	0.0075 (5)	0.0071 (5)	0.0144 (6)
C7	0.0205 (6)	0.0187 (7)	0.0238 (6)	0.0054 (5)	0.0008 (5)	0.0039 (5)
C8	0.0341 (7)	0.0287 (8)	0.0257 (6)	0.0041 (6)	0.0046 (5)	0.0063 (6)
C9	0.0517 (9)	0.0321 (8)	0.0233 (7)	0.0094 (7)	0.0031 (6)	0.0042 (6)
C10	0.0460 (8)	0.0294 (8)	0.0262 (7)	0.0129 (7)	−0.0068 (6)	−0.0012 (6)
C11	0.0297 (7)	0.0313 (8)	0.0337 (7)	0.0036 (6)	−0.0068 (6)	−0.0031 (6)
C12	0.0239 (6)	0.0251 (7)	0.0301 (7)	0.0008 (5)	0.0004 (5)	0.0011 (6)
C13	0.0166 (5)	0.0205 (7)	0.0262 (6)	0.0035 (5)	0.0033 (4)	0.0071 (5)
C14	0.0259 (6)	0.0328 (8)	0.0354 (7)	0.0106 (6)	0.0107 (5)	0.0115 (6)
C15	0.0315 (7)	0.0450 (10)	0.0381 (7)	0.0098 (6)	0.0168 (6)	0.0160 (7)
C16	0.0331 (7)	0.0363 (9)	0.0322 (7)	0.0023 (6)	0.0076 (6)	0.0142 (6)
C17	0.0342 (7)	0.0294 (8)	0.0357 (7)	0.0078 (6)	0.0052 (6)	0.0162 (6)
C18	0.0259 (6)	0.0255 (7)	0.0337 (7)	0.0092 (5)	0.0080 (5)	0.0139 (6)
C19	0.0220 (6)	0.0204 (7)	0.0193 (6)	0.0046 (5)	0.0029 (4)	0.0029 (5)
C20	0.0309 (6)	0.0222 (7)	0.0215 (6)	0.0042 (5)	0.0056 (5)	0.0015 (5)
C21	0.0393 (7)	0.0242 (8)	0.0291 (7)	0.0078 (6)	0.0097 (6)	−0.0005 (6)
C22	0.0385 (7)	0.0240 (8)	0.0388 (8)	0.0125 (6)	0.0088 (6)	0.0037 (6)
C23	0.0318 (7)	0.0230 (7)	0.0345 (7)	0.0094 (6)	−0.0007 (5)	0.0052 (6)
C24	0.0271 (6)	0.0244 (7)	0.0235 (6)	0.0074 (5)	−0.0015 (5)	0.0035 (5)
C25	0.0203 (6)	0.0214 (7)	0.0251 (6)	0.0033 (5)	−0.0002 (5)	0.0058 (5)
C26	0.0242 (7)	0.0366 (9)	0.0401 (8)	0.0080 (6)	0.0074 (6)	0.0074 (7)
C27	0.0221 (7)	0.0459 (10)	0.0678 (11)	0.0069 (7)	0.0090 (7)	0.0165 (9)
C28	0.0217 (7)	0.0373 (9)	0.0653 (10)	−0.0021 (6)	−0.0060 (7)	0.0172 (8)
C29	0.0322 (7)	0.0282 (8)	0.0408 (8)	−0.0023 (6)	−0.0123 (6)	0.0061 (7)
C30	0.0262 (7)	0.0258 (7)	0.0279 (6)	0.0035 (6)	−0.0028 (5)	0.0041 (6)
C31	0.0188 (5)	0.0210 (7)	0.0201 (5)	0.0046 (5)	0.0022 (4)	0.0060 (5)
C32	0.0268 (6)	0.0254 (7)	0.0232 (6)	0.0100 (5)	0.0075 (5)	0.0062 (5)
C33	0.0333 (7)	0.0354 (9)	0.0239 (6)	0.0131 (6)	0.0075 (5)	0.0043 (6)
C34	0.0308 (7)	0.0459 (9)	0.0206 (6)	0.0115 (6)	0.0058 (5)	0.0113 (6)
C35	0.0289 (6)	0.0367 (9)	0.0284 (7)	0.0102 (6)	0.0069 (5)	0.0186 (6)
C36	0.0264 (6)	0.0236 (7)	0.0268 (6)	0.0058 (5)	0.0055 (5)	0.0114 (6)
C37	0.0285 (6)	0.0385 (8)	0.0234 (7)	0.0034 (6)	0.0042 (5)	0.0107 (6)
C38	0.0248 (6)	0.0236 (7)	0.0298 (6)	0.0070 (5)	0.0008 (5)	0.0070 (6)
H1	0.051000	0.034000	0.051000	0.016000	0.000000	0.012000
H2	0.040000	0.064000	0.032000	0.012000	0.011000	0.014000
H3	0.051000	0.053000	0.058000	0.015000	0.028000	0.015000
H4	0.080000	0.044000	0.067000	0.032000	0.023000	0.008000
H5	0.065000	0.031000	0.076000	0.006000	0.000000	0.021000
H6	0.035000	0.058000	0.099000	0.008000	0.018000	0.043000
H7	0.042000	0.048000	0.080000	0.024000	0.021000	0.026000
H8	0.033000	0.052000	0.049000	0.007000	0.010000	0.011000
H9	0.077000	0.065000	0.034000	0.018000	0.020000	0.013000
H10	0.081000	0.071000	0.034000	0.015000	−0.020000	0.004000
H11	0.033000	0.080000	0.064000	0.002000	−0.013000	0.006000
H12	0.037000	0.070000	0.045000	0.004000	0.012000	0.012000
H13	0.063000	0.044000	0.060000	0.026000	0.022000	0.016000
H14	0.064000	0.071000	0.060000	0.024000	0.035000	0.015000
H15	0.063000	0.072000	0.053000	0.006000	0.022000	0.032000
H16	0.065000	0.052000	0.066000	0.020000	0.012000	0.036000
H17	0.049000	0.051000	0.063000	0.027000	0.021000	0.026000
H18	0.066000	0.045000	0.030000	0.015000	0.000000	0.009000
H19	0.081000	0.035000	0.039000	0.009000	0.009000	−0.003000
H20	0.076000	0.030000	0.064000	0.018000	0.010000	0.011000
H21	0.078000	0.046000	0.051000	0.022000	−0.012000	0.017000
H22	0.074000	0.037000	0.034000	0.017000	−0.013000	0.000000
H23	0.054000	0.064000	0.057000	0.020000	0.009000	−0.012000
H24	0.044000	0.076000	0.121000	0.031000	0.025000	0.012000
H25	0.030000	0.078000	0.107000	0.008000	−0.013000	0.032000
H26	0.054000	0.063000	0.048000	−0.004000	−0.016000	0.008000
H27	0.046000	0.050000	0.038000	0.014000	0.009000	0.004000
H28	0.061000	0.032000	0.048000	0.012000	0.015000	0.016000
H29	0.072000	0.047000	0.044000	0.018000	0.010000	−0.007000
H30	0.072000	0.086000	0.027000	0.031000	0.016000	0.017000
H31	0.064000	0.061000	0.053000	0.021000	0.020000	0.039000
H32	0.063000	0.031000	0.047000	0.009000	0.011000	0.011000

Geometric parameters (Å, º)

Fe1—P1	2.1012 (6)	C13—C18	1.3895 (18)
Fe1—P2	2.1190 (6)	C14—C15	1.390 (2)
Fe1—C37	1.7907 (14)	C14—H13	1.075 (19)
Fe1—C38	1.7808 (15)	C15—C16	1.391 (2)
Fe1—H1	1.511 (17)	C15—H14	1.077 (18)
Fe1—H2	1.499 (16)	C16—C17	1.387 (2)
P1—O1	1.6028 (8)	C16—H15	1.114 (18)
P1—O2	1.6147 (10)	C17—C18	1.3951 (18)
P1—O3	1.6254 (9)	C17—H16	1.087 (19)
P2—O4	1.6067 (10)	C18—H17	1.083 (18)
P2—O5	1.5995 (9)	C19—C20	1.3885 (17)
P2—O6	1.6062 (9)	C19—C24	1.3905 (17)
O1—C1	1.3836 (15)	C20—C21	1.390 (2)
O2—C7	1.3941 (14)	C20—H18	1.099 (17)
O3—C13	1.3877 (14)	C21—C22	1.391 (2)
O4—C19	1.3811 (16)	C21—H19	1.073 (18)
O5—C25	1.3950 (14)	C22—C23	1.389 (2)
O6—C31	1.3767 (14)	C22—H20	1.086 (19)
O7—C37	1.1393 (17)	C23—C24	1.394 (2)
O8—C38	1.1434 (17)	C23—H21	1.090 (17)
C1—C2	1.3851 (18)	C24—H22	1.100 (17)
C1—C6	1.3857 (17)	C25—C26	1.3820 (19)
C2—C3	1.391 (2)	C25—C30	1.3839 (19)
C2—H3	1.089 (18)	C26—C27	1.390 (2)
C3—C4	1.390 (2)	C26—H23	1.100 (19)
C3—H4	1.11 (2)	C27—C28	1.387 (3)
C4—C5	1.393 (2)	C27—H24	1.09 (2)
C4—H5	1.092 (18)	C28—C29	1.390 (2)
C5—C6	1.3917 (19)	C28—H25	1.114 (18)
C5—H6	1.103 (18)	C29—C30	1.3924 (18)
C6—H7	1.097 (18)	C29—H26	1.096 (19)
C7—C8	1.3897 (18)	C30—H27	1.079 (17)
C7—C12	1.3808 (17)	C31—C32	1.3926 (19)
C8—C9	1.3916 (19)	C31—C36	1.3874 (18)
C8—H8	1.103 (17)	C32—C33	1.3899 (18)
C9—C10	1.393 (2)	C32—H28	1.105 (17)
C9—H9	1.094 (17)	C33—C34	1.389 (2)
C10—C11	1.387 (2)	C33—H29	1.10 (2)
C10—H10	1.085 (17)	C34—C35	1.391 (2)
C11—C12	1.3925 (18)	C34—H30	1.081 (16)
C11—H11	1.106 (18)	C35—C36	1.3925 (18)
C12—H12	1.072 (18)	C35—H31	1.077 (17)
C13—C14	1.3884 (18)	C36—H32	1.098 (19)
P2—Fe1—P1	154.361 (14)	C15—C14—C13	119.54 (14)
C37—Fe1—P1	103.49 (4)	H13—C14—C13	118.0 (10)
C37—Fe1—P2	95.97 (4)	H13—C14—C15	122.4 (10)
C38—Fe1—P1	97.50 (4)	C16—C15—C14	120.63 (13)
C38—Fe1—P2	95.04 (4)	H14—C15—C14	120.7 (11)
C38—Fe1—C37	100.77 (6)	H14—C15—C16	118.7 (11)
H1—Fe1—P1	81.7 (6)	C17—C16—C15	119.20 (13)
H1—Fe1—P2	82.8 (6)	H15—C16—C15	119.2 (11)
H1—Fe1—C37	87.0 (7)	H15—C16—C17	121.6 (11)
H1—Fe1—C38	172.1 (7)	C18—C17—C16	120.88 (14)
H2—Fe1—P1	76.6 (6)	H16—C17—C16	119.4 (10)
H2—Fe1—P2	80.9 (7)	H16—C17—C18	119.7 (10)
H2—Fe1—C37	168.2 (7)	C17—C18—C13	119.14 (13)
H2—Fe1—C38	90.9 (7)	H17—C18—C13	118.8 (9)
H2—Fe1—H1	81.3 (10)	H17—C18—C17	122.0 (9)
O1—P1—Fe1	120.12 (3)	C20—C19—O4	115.06 (10)
O2—P1—Fe1	113.90 (3)	C24—C19—O4	123.85 (11)
O2—P1—O1	98.14 (5)	C24—C19—C20	121.09 (12)
O3—P1—Fe1	121.62 (3)	C21—C20—C19	119.37 (12)
O3—P1—O1	95.80 (4)	H18—C20—C19	118.3 (10)
O3—P1—O2	103.23 (5)	H18—C20—C21	122.4 (10)
O4—P2—Fe1	120.24 (3)	C22—C21—C20	120.42 (13)
O5—P2—Fe1	111.53 (3)	H19—C21—C20	118.0 (11)
O5—P2—O4	99.02 (5)	H19—C21—C22	121.5 (11)
O6—P2—Fe1	123.05 (3)	C23—C22—C21	119.49 (14)
O6—P2—O4	96.64 (5)	H20—C22—C21	119.3 (10)
O6—P2—O5	102.45 (5)	H20—C22—C23	121.2 (10)
C1—O1—P1	126.75 (7)	C24—C23—C22	120.86 (13)
C7—O2—P1	123.59 (8)	H21—C23—C22	119.7 (11)
C13—O3—P1	124.37 (7)	H21—C23—C24	119.5 (10)
C19—O4—P2	127.98 (7)	C23—C24—C19	118.76 (12)
C25—O5—P2	124.87 (8)	H22—C24—C19	123.9 (9)
C31—O6—P2	130.41 (8)	H22—C24—C23	117.3 (9)
C2—C1—O1	119.58 (11)	C26—C25—O5	117.54 (12)
C6—C1—O1	118.63 (11)	C30—C25—O5	120.47 (11)
C6—C1—C2	121.55 (12)	C30—C25—C26	121.75 (12)
C3—C2—C1	119.21 (13)	C27—C26—C25	119.11 (14)
H3—C2—C1	119.5 (10)	H23—C26—C25	118.6 (10)
H3—C2—C3	121.2 (10)	H23—C26—C27	122.3 (10)
C4—C3—C2	120.23 (14)	C28—C27—C26	120.25 (15)
H4—C3—C2	119.9 (11)	H24—C27—C26	118.2 (12)
H4—C3—C4	119.9 (11)	H24—C27—C28	121.6 (12)
C5—C4—C3	119.69 (13)	C29—C28—C27	119.75 (13)
H5—C4—C3	120.6 (11)	H25—C28—C27	119.9 (13)
H5—C4—C5	119.7 (11)	H25—C28—C29	120.4 (13)
C6—C5—C4	120.56 (13)	C30—C29—C28	120.60 (14)
H6—C5—C4	119.8 (11)	H26—C29—C28	120.0 (10)
H6—C5—C6	119.6 (11)	H26—C29—C30	119.4 (10)
C5—C6—C1	118.75 (13)	C29—C30—C25	118.54 (13)
H7—C6—C1	121.4 (10)	H27—C30—C25	121.3 (9)
H7—C6—C5	119.8 (10)	H27—C30—C29	120.2 (9)
C8—C7—O2	117.88 (10)	C32—C31—O6	122.43 (11)
C12—C7—O2	120.34 (11)	C36—C31—O6	116.12 (12)
C12—C7—C8	121.73 (11)	C36—C31—C32	121.39 (11)
C9—C8—C7	118.72 (13)	C33—C32—C31	118.66 (13)
H8—C8—C7	118.5 (9)	H28—C32—C31	121.3 (10)
H8—C8—C9	122.8 (9)	H28—C32—C33	120.0 (10)
C10—C9—C8	120.45 (13)	C34—C33—C32	120.85 (14)
H9—C9—C8	120.4 (10)	H29—C33—C32	118.5 (10)
H9—C9—C10	119.1 (10)	H29—C33—C34	120.6 (10)
C11—C10—C9	119.60 (12)	C35—C34—C33	119.63 (12)
H10—C10—C9	119.0 (11)	H30—C34—C33	120.2 (11)
H10—C10—C11	121.4 (11)	H30—C34—C35	120.2 (11)
C12—C11—C10	120.64 (13)	C36—C35—C34	120.37 (13)
H11—C11—C10	119.6 (10)	H31—C35—C34	119.6 (11)
H11—C11—C12	119.8 (10)	H31—C35—C36	120.0 (11)
C11—C12—C7	118.84 (13)	C35—C36—C31	119.08 (13)
H12—C12—C7	120.5 (9)	H32—C36—C31	121.0 (9)
H12—C12—C11	120.7 (9)	H32—C36—C35	119.9 (9)
C14—C13—O3	116.52 (11)	O7—C37—Fe1	177.61 (15)
C18—C13—O3	122.81 (11)	O8—C38—Fe1	177.26 (12)
C18—C13—C14	120.61 (12)
Fe1—P1—O1—C1	−30.00 (7)	O5—C25—C30—C29	173.84 (12)
Fe1—P1—O2—C7	−157.59 (7)	O6—C31—C32—C33	−178.70 (11)
Fe1—P1—O3—C13	−50.54 (7)	O6—C31—C36—C35	178.58 (10)
Fe1—P2—O4—C19	−79.76 (7)	C1—C2—C3—C4	−0.50 (14)
Fe1—P2—O5—C25	171.81 (7)	C1—C6—C5—C4	0.19 (14)
Fe1—P2—O6—C31	−20.83 (7)	C2—C3—C4—C5	−0.21 (16)
P1—O1—C1—C2	−84.58 (10)	C3—C4—C5—C6	0.37 (16)
P1—O1—C1—C6	100.90 (10)	C7—C8—C9—C10	0.53 (17)
P1—O2—C7—C8	97.67 (10)	C7—C12—C11—C10	1.01 (16)
P1—O2—C7—C12	−84.75 (10)	C8—C9—C10—C11	−0.76 (19)
P1—O3—C13—C14	147.08 (10)	C9—C10—C11—C12	−0.02 (18)
P1—O3—C13—C18	−35.70 (11)	C13—C14—C15—C16	0.40 (15)
P2—O4—C19—C20	−170.55 (10)	C13—C18—C17—C16	0.50 (15)
P2—O4—C19—C24	9.75 (11)	C14—C15—C16—C17	−0.51 (17)
P2—O5—C25—C26	−105.55 (11)	C15—C16—C17—C18	0.06 (16)
P2—O5—C25—C30	79.97 (11)	C19—C20—C21—C22	−0.24 (15)
P2—O6—C31—C32	−43.96 (12)	C19—C24—C23—C22	0.32 (15)
P2—O6—C31—C36	138.58 (11)	C20—C21—C22—C23	−0.44 (16)
O1—C1—C2—C3	−173.27 (11)	C21—C22—C23—C24	0.40 (16)
O1—C1—C6—C5	173.48 (11)	C25—C26—C27—C28	0.49 (17)
O2—C7—C8—C9	178.04 (13)	C25—C30—C29—C28	0.12 (16)
O2—C7—C12—C11	−178.74 (13)	C26—C27—C28—C29	−0.77 (19)
O3—C13—C14—C15	177.45 (11)	C27—C28—C29—C30	0.46 (18)
O3—C13—C18—C17	−177.72 (11)	C31—C32—C33—C34	0.87 (14)
O4—C19—C20—C21	−178.73 (10)	C31—C36—C35—C34	−0.28 (14)
O4—C19—C24—C23	178.67 (12)	C32—C33—C34—C35	−0.09 (15)
O5—C25—C26—C27	−174.30 (13)	C33—C34—C35—C36	−0.21 (15)

(QOSZON_HAR_NoMoRe)

Crystal data

C38H32FeO8P2	Z = 2
Mr = 734.47	F(000) = 761.455
Triclinic, P1	Dx = 1.431 Mg m^−3
a = 9.6397 (12) Å	Mo Kα radiation, λ = 0.71073 Å
b = 10.4410 (13) Å	Cell parameters from 5000 reflections
c = 18.381 (2) Å	θ = 3.3–52.1°
α = 102.148 (15)°	µ = 0.59 mm^−1
β = 94.667 (15)°	T = 293 K
γ = 107.402 (14)°	Parallelepiped, colourless
V = 1705.0 (4) Å^3	0.5 × 0.25 × 0.1 mm

Data collection

STOE diffractometer	Rint = 0.034
rotation en phi scans	θmax = 26.1°, θmin = 2.1°
16806 measured reflections	h = −11→11
6202 independent reflections	k = −12→12
5084 reflections with I ≥ 2u(I)	l = −22→22

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.020	Only H-atom coordinates refined
wR(F^2) = 0.070	w = 1/[σ^2(Fo^2) + (0.1P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 0.55	(Δ/σ)max = 0.001
6202 reflections	Δρmax = 0.21 e Å^−3
538 parameters	Δρmin = −0.28 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Fe1	0.531699 (19)	0.83646 (2)	0.270659 (10)	0.01889 (7)
P1	0.35099 (3)	0.72595 (4)	0.185422 (18)	0.01878 (9)
P2	0.72498 (3)	1.00381 (4)	0.322124 (17)	0.01876 (9)
O1	0.30700 (11)	0.79744 (10)	0.12205 (5)	0.0253 (2)
O2	0.37086 (10)	0.59223 (10)	0.13043 (5)	0.0233 (2)
O3	0.18551 (10)	0.66713 (10)	0.20472 (5)	0.0243 (2)
O4	0.71936 (11)	1.12331 (11)	0.39187 (5)	0.0252 (2)
O5	0.84522 (10)	0.95244 (10)	0.36185 (5)	0.0242 (2)
O6	0.82084 (10)	1.10478 (10)	0.27664 (5)	0.0255 (2)
O7	0.40859 (15)	0.81931 (17)	0.41020 (7)	0.0556 (4)
O8	0.67923 (13)	0.62706 (13)	0.25560 (7)	0.0423 (3)
C1	0.32775 (14)	0.93701 (14)	0.13015 (7)	0.0203 (3)
C2	0.22437 (15)	0.99247 (17)	0.15926 (8)	0.0276 (3)
C3	0.23793 (18)	1.12913 (19)	0.15990 (9)	0.0359 (4)
C4	0.35439 (18)	1.20894 (17)	0.13210 (9)	0.0363 (4)
C5	0.45821 (17)	1.15178 (17)	0.10376 (10)	0.0337 (4)
C6	0.44563 (15)	1.01496 (16)	0.10277 (8)	0.0266 (3)
C7	0.29353 (14)	0.53188 (15)	0.05763 (7)	0.0220 (3)
C8	0.36301 (17)	0.56780 (17)	−0.00191 (8)	0.0315 (3)
C9	0.2894 (2)	0.50561 (18)	−0.07514 (9)	0.0378 (4)
C10	0.14827 (19)	0.40983 (18)	−0.08804 (9)	0.0363 (4)
C11	0.08166 (17)	0.37549 (18)	−0.02759 (9)	0.0356 (4)
C12	0.15461 (16)	0.43578 (16)	0.04600 (9)	0.0297 (3)
C13	0.14876 (14)	0.58909 (15)	0.25699 (7)	0.0220 (3)
C14	0.03545 (16)	0.60725 (17)	0.29568 (9)	0.0309 (3)
C15	−0.01100 (17)	0.52826 (19)	0.34675 (9)	0.0376 (4)
C16	0.05557 (17)	0.43220 (18)	0.35974 (9)	0.0353 (4)
C17	0.16838 (17)	0.41516 (17)	0.32053 (9)	0.0327 (3)
C18	0.21553 (15)	0.49271 (16)	0.26879 (8)	0.0271 (3)
C19	0.67130 (14)	1.23477 (15)	0.38993 (7)	0.0218 (3)
C20	0.69999 (16)	1.33283 (16)	0.45792 (8)	0.0269 (3)
C21	0.65346 (17)	1.44754 (17)	0.46198 (9)	0.0329 (3)
C22	0.57909 (18)	1.46433 (18)	0.39836 (9)	0.0339 (3)
C23	0.55270 (16)	1.36613 (16)	0.33048 (9)	0.0309 (3)
C24	0.59870 (15)	1.25046 (16)	0.32544 (8)	0.0261 (3)
C25	0.98948 (14)	1.03526 (15)	0.39228 (8)	0.0236 (3)
C26	1.09971 (17)	1.01445 (18)	0.35242 (10)	0.0344 (4)
C27	1.24588 (18)	1.0864 (2)	0.38416 (12)	0.0462 (5)
C28	1.27960 (17)	1.17647 (19)	0.45524 (12)	0.0444 (4)
C29	1.16711 (18)	1.19610 (17)	0.49414 (10)	0.0388 (4)
C30	1.02048 (17)	1.12559 (16)	0.46288 (8)	0.0292 (3)
C31	0.82808 (13)	1.08543 (15)	0.20079 (7)	0.0206 (3)
C32	0.83576 (15)	0.96249 (16)	0.15665 (8)	0.0250 (3)
C33	0.84554 (16)	0.95235 (18)	0.08076 (8)	0.0311 (3)
C34	0.84990 (16)	1.06361 (19)	0.04962 (8)	0.0325 (4)
C35	0.84393 (15)	1.18616 (17)	0.09478 (8)	0.0299 (3)
C36	0.83327 (15)	1.19777 (16)	0.17082 (8)	0.0254 (3)
C37	0.45593 (16)	0.82299 (17)	0.35569 (8)	0.0318 (3)
C38	0.61952 (15)	0.70738 (16)	0.26260 (8)	0.0266 (3)
H1	0.468 (2)	0.951 (2)	0.2694 (12)	0.045279
H2	0.585 (2)	0.872 (2)	0.2010 (11)	0.046552
H3	0.134 (2)	0.929 (2)	0.1809 (12)	0.053768
H4	0.151 (3)	1.173 (3)	0.1804 (14)	0.062774
H5	0.364 (3)	1.316 (2)	0.1313 (14)	0.060579
H6	0.548 (2)	1.213 (2)	0.0803 (14)	0.061802
H7	0.528 (2)	0.971 (2)	0.0794 (14)	0.053335
H8	0.474 (2)	0.643 (2)	0.0108 (11)	0.046997
H9	0.347 (3)	0.529 (3)	−0.1227 (12)	0.059466
H10	0.093 (3)	0.363 (3)	−0.1459 (12)	0.067875
H11	−0.032 (2)	0.300 (3)	−0.0367 (13)	0.067476
H12	0.103 (2)	0.406 (2)	0.0921 (12)	0.054537
H13	−0.010 (2)	0.686 (2)	0.2858 (13)	0.052667
H14	−0.101 (3)	0.539 (3)	0.3763 (13)	0.064154
H15	0.013 (3)	0.369 (3)	0.4001 (13)	0.063392
H16	0.218 (3)	0.337 (2)	0.3296 (13)	0.057538
H17	0.300 (2)	0.479 (2)	0.2356 (12)	0.049435
H18	0.761 (2)	1.317 (2)	0.5067 (11)	0.048171
H19	0.677 (3)	1.521 (2)	0.5151 (11)	0.055163
H20	0.545 (3)	1.555 (2)	0.4025 (13)	0.056252
H21	0.494 (3)	1.379 (2)	0.2809 (12)	0.059027
H22	0.574 (2)	1.177 (2)	0.2691 (11)	0.051588
H23	1.067 (2)	0.942 (3)	0.2960 (13)	0.062788
H24	1.332 (3)	1.067 (3)	0.3513 (17)	0.079389
H25	1.398 (2)	1.232 (3)	0.4808 (16)	0.075312
H26	1.194 (2)	1.267 (3)	0.5501 (13)	0.062820
H27	0.934 (2)	1.140 (2)	0.4927 (11)	0.045799
H28	0.832 (2)	0.874 (2)	0.1808 (11)	0.046499
H29	0.850 (3)	0.856 (2)	0.0461 (12)	0.057435
H30	0.855 (3)	1.054 (3)	−0.0096 (11)	0.059692
H31	0.846 (2)	1.271 (2)	0.0705 (12)	0.054612
H32	0.830 (2)	1.295 (2)	0.2062 (12)	0.048223

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Fe1	0.01738 (10)	0.01978 (12)	0.01746 (10)	0.00265 (7)	0.00094 (7)	0.00588 (8)
P1	0.01745 (16)	0.01769 (18)	0.01962 (16)	0.00296 (13)	0.00012 (12)	0.00624 (13)
P2	0.01895 (16)	0.01868 (19)	0.01641 (16)	0.00326 (13)	0.00137 (12)	0.00423 (13)
O1	0.0303 (5)	0.0194 (5)	0.0224 (5)	0.0041 (4)	−0.0043 (4)	0.0064 (4)
O2	0.0229 (5)	0.0211 (5)	0.0243 (5)	0.0067 (4)	−0.0003 (4)	0.0042 (4)
O3	0.0177 (4)	0.0262 (6)	0.0301 (5)	0.0056 (4)	0.0031 (4)	0.0123 (4)
O4	0.0304 (5)	0.0260 (6)	0.0187 (4)	0.0106 (4)	0.0017 (4)	0.0034 (4)
O5	0.0206 (4)	0.0223 (5)	0.0266 (5)	0.0036 (4)	−0.0025 (4)	0.0064 (4)
O6	0.0280 (5)	0.0229 (5)	0.0198 (4)	0.0001 (4)	0.0037 (4)	0.0051 (4)
O7	0.0535 (8)	0.0763 (10)	0.0288 (6)	0.0027 (7)	0.0167 (5)	0.0178 (6)
O8	0.0431 (7)	0.0347 (7)	0.0528 (7)	0.0212 (6)	0.0023 (5)	0.0082 (6)
C1	0.0214 (6)	0.0207 (7)	0.0196 (6)	0.0068 (5)	0.0026 (5)	0.0070 (5)
C2	0.0264 (7)	0.0315 (9)	0.0267 (7)	0.0117 (6)	0.0076 (5)	0.0067 (6)
C3	0.0397 (9)	0.0340 (10)	0.0365 (8)	0.0202 (7)	0.0045 (6)	0.0024 (7)
C4	0.0414 (9)	0.0231 (9)	0.0440 (9)	0.0122 (7)	−0.0044 (7)	0.0088 (7)
C5	0.0294 (7)	0.0255 (8)	0.0470 (9)	0.0043 (6)	0.0032 (6)	0.0183 (7)
C6	0.0229 (7)	0.0262 (8)	0.0340 (7)	0.0076 (6)	0.0069 (5)	0.0143 (6)
C7	0.0213 (6)	0.0195 (7)	0.0240 (6)	0.0063 (5)	0.0009 (5)	0.0041 (5)
C8	0.0348 (8)	0.0293 (8)	0.0262 (7)	0.0044 (7)	0.0048 (6)	0.0069 (6)
C9	0.0523 (10)	0.0320 (9)	0.0243 (7)	0.0098 (8)	0.0026 (7)	0.0037 (7)
C10	0.0467 (9)	0.0305 (9)	0.0266 (8)	0.0138 (7)	−0.0064 (7)	−0.0008 (7)
C11	0.0297 (8)	0.0315 (9)	0.0341 (8)	0.0038 (7)	−0.0067 (6)	−0.0033 (7)
C12	0.0247 (7)	0.0256 (8)	0.0308 (8)	0.0012 (6)	0.0004 (6)	0.0013 (6)
C13	0.0171 (6)	0.0210 (7)	0.0268 (6)	0.0036 (5)	0.0035 (5)	0.0074 (5)
C14	0.0271 (7)	0.0331 (9)	0.0357 (8)	0.0109 (6)	0.0113 (6)	0.0114 (7)
C15	0.0323 (8)	0.0453 (11)	0.0382 (8)	0.0103 (7)	0.0167 (7)	0.0162 (7)
C16	0.0333 (8)	0.0367 (9)	0.0327 (8)	0.0021 (7)	0.0075 (6)	0.0143 (7)
C17	0.0337 (8)	0.0299 (9)	0.0361 (8)	0.0075 (6)	0.0045 (6)	0.0159 (7)
C18	0.0256 (7)	0.0258 (8)	0.0341 (7)	0.0090 (6)	0.0079 (6)	0.0138 (6)
C19	0.0224 (6)	0.0208 (7)	0.0199 (6)	0.0049 (5)	0.0032 (5)	0.0032 (5)
C20	0.0317 (7)	0.0224 (8)	0.0217 (6)	0.0044 (6)	0.0060 (5)	0.0011 (6)
C21	0.0394 (8)	0.0247 (8)	0.0301 (8)	0.0077 (6)	0.0097 (6)	−0.0003 (6)
C22	0.0390 (8)	0.0249 (9)	0.0385 (8)	0.0134 (7)	0.0091 (7)	0.0038 (7)
C23	0.0326 (7)	0.0238 (8)	0.0345 (8)	0.0097 (6)	−0.0007 (6)	0.0049 (6)
C24	0.0276 (7)	0.0252 (8)	0.0232 (7)	0.0079 (6)	−0.0008 (5)	0.0037 (6)
C25	0.0213 (6)	0.0218 (7)	0.0250 (7)	0.0037 (5)	0.0003 (5)	0.0060 (6)
C26	0.0241 (7)	0.0364 (10)	0.0411 (9)	0.0080 (7)	0.0075 (6)	0.0077 (7)
C27	0.0227 (8)	0.0463 (11)	0.0683 (12)	0.0073 (7)	0.0090 (8)	0.0165 (10)
C28	0.0223 (8)	0.0375 (10)	0.0652 (12)	−0.0022 (7)	−0.0056 (7)	0.0173 (9)
C29	0.0333 (8)	0.0281 (9)	0.0421 (9)	−0.0018 (7)	−0.0126 (7)	0.0059 (7)
C30	0.0267 (7)	0.0264 (8)	0.0288 (7)	0.0037 (6)	−0.0023 (6)	0.0045 (6)
C31	0.0186 (6)	0.0215 (7)	0.0207 (6)	0.0048 (5)	0.0021 (5)	0.0059 (5)
C32	0.0273 (7)	0.0256 (8)	0.0237 (7)	0.0101 (6)	0.0076 (5)	0.0061 (6)
C33	0.0338 (7)	0.0357 (10)	0.0244 (7)	0.0136 (7)	0.0071 (6)	0.0043 (7)
C34	0.0310 (7)	0.0460 (10)	0.0214 (7)	0.0112 (7)	0.0061 (5)	0.0112 (7)
C35	0.0293 (7)	0.0369 (9)	0.0289 (7)	0.0107 (6)	0.0072 (6)	0.0188 (7)
C36	0.0264 (7)	0.0241 (8)	0.0270 (7)	0.0062 (6)	0.0055 (5)	0.0112 (6)
C37	0.0296 (7)	0.0391 (9)	0.0232 (7)	0.0035 (6)	0.0045 (6)	0.0112 (6)
C38	0.0248 (7)	0.0239 (8)	0.0297 (7)	0.0068 (6)	0.0004 (5)	0.0065 (6)
H1	0.052000	0.034000	0.051000	0.016000	0.000000	0.013000
H2	0.041000	0.065000	0.032000	0.012000	0.011000	0.014000
H3	0.052000	0.055000	0.058000	0.016000	0.029000	0.016000
H4	0.084000	0.046000	0.066000	0.034000	0.023000	0.007000
H5	0.068000	0.031000	0.076000	0.005000	−0.002000	0.020000
H6	0.034000	0.059000	0.100000	0.007000	0.017000	0.045000
H7	0.042000	0.050000	0.082000	0.025000	0.021000	0.027000
H8	0.034000	0.053000	0.049000	0.007000	0.010000	0.011000
H9	0.077000	0.066000	0.034000	0.018000	0.019000	0.013000
H10	0.082000	0.072000	0.034000	0.016000	−0.020000	0.004000
H11	0.034000	0.082000	0.065000	0.002000	−0.013000	0.005000
H12	0.037000	0.071000	0.046000	0.004000	0.011000	0.012000
H13	0.063000	0.044000	0.060000	0.026000	0.021000	0.015000
H14	0.064000	0.072000	0.061000	0.024000	0.034000	0.014000
H15	0.064000	0.073000	0.052000	0.006000	0.021000	0.032000
H16	0.065000	0.053000	0.065000	0.020000	0.011000	0.035000
H17	0.050000	0.051000	0.062000	0.027000	0.021000	0.025000
H18	0.066000	0.045000	0.030000	0.015000	0.000000	0.009000
H19	0.080000	0.035000	0.038000	0.009000	0.008000	−0.003000
H20	0.075000	0.030000	0.064000	0.018000	0.010000	0.011000
H21	0.079000	0.046000	0.051000	0.021000	−0.012000	0.017000
H22	0.075000	0.037000	0.034000	0.017000	−0.013000	0.000000
H23	0.055000	0.064000	0.058000	0.021000	0.010000	−0.012000
H24	0.045000	0.076000	0.123000	0.032000	0.026000	0.014000
H25	0.030000	0.078000	0.111000	0.007000	−0.013000	0.033000
H26	0.055000	0.062000	0.049000	−0.004000	−0.017000	0.009000
H27	0.046000	0.050000	0.038000	0.014000	0.009000	0.005000
H28	0.062000	0.032000	0.048000	0.013000	0.015000	0.016000
H29	0.072000	0.047000	0.044000	0.018000	0.010000	−0.007000
H30	0.072000	0.086000	0.027000	0.030000	0.016000	0.017000
H31	0.063000	0.061000	0.053000	0.020000	0.020000	0.038000
H32	0.063000	0.031000	0.047000	0.009000	0.011000	0.010000

Geometric parameters (Å, º)

Fe1—P1	2.1008 (6)	C13—C18	1.389 (2)
Fe1—P2	2.1189 (6)	C14—C15	1.391 (2)
Fe1—C37	1.7924 (16)	C14—H13	1.08 (2)
Fe1—C38	1.7815 (16)	C15—C16	1.391 (3)
Fe1—H1	1.50 (2)	C15—H14	1.08 (2)
Fe1—H2	1.494 (19)	C16—C17	1.387 (2)
P1—O1	1.6028 (9)	C16—H15	1.12 (2)
P1—O2	1.6140 (11)	C17—C18	1.393 (2)
P1—O3	1.6265 (10)	C17—H16	1.09 (2)
P2—O4	1.6068 (11)	C18—H17	1.08 (2)
P2—O5	1.6010 (10)	C19—C20	1.3864 (19)
P2—O6	1.6057 (10)	C19—C24	1.3919 (19)
O1—C1	1.3839 (17)	C20—C21	1.389 (2)
O2—C7	1.3948 (16)	C20—H18	1.10 (2)
O3—C13	1.3873 (16)	C21—C22	1.392 (2)
O4—C19	1.3810 (18)	C21—H19	1.07 (2)
O5—C25	1.3946 (16)	C22—C23	1.388 (2)
O6—C31	1.3767 (16)	C22—H20	1.08 (2)
O7—C37	1.138 (2)	C23—C24	1.394 (2)
O8—C38	1.1430 (19)	C23—H21	1.09 (2)
C1—C2	1.384 (2)	C24—H22	1.11 (2)
C1—C6	1.3853 (19)	C25—C26	1.382 (2)
C2—C3	1.391 (2)	C25—C30	1.384 (2)
C2—H3	1.09 (2)	C26—C27	1.392 (2)
C3—C4	1.389 (2)	C26—H23	1.11 (2)
C3—H4	1.12 (2)	C27—C28	1.388 (3)
C4—C5	1.393 (2)	C27—H24	1.10 (2)
C4—H5	1.10 (2)	C28—C29	1.388 (3)
C5—C6	1.393 (2)	C28—H25	1.12 (2)
C5—H6	1.09 (2)	C29—C30	1.392 (2)
C6—H7	1.10 (2)	C29—H26	1.09 (2)
C7—C8	1.389 (2)	C30—H27	1.07 (2)
C7—C12	1.380 (2)	C31—C32	1.393 (2)
C8—C9	1.392 (2)	C31—C36	1.3868 (19)
C8—H8	1.09 (2)	C32—C33	1.390 (2)
C9—C10	1.393 (2)	C32—H28	1.10 (2)
C9—H9	1.11 (2)	C33—C34	1.391 (2)
C10—C11	1.386 (2)	C33—H29	1.09 (2)
C10—H10	1.09 (2)	C34—C35	1.391 (2)
C11—C12	1.394 (2)	C34—H30	1.078 (19)
C11—H11	1.12 (2)	C35—C36	1.392 (2)
C12—H12	1.07 (2)	C35—H31	1.07 (2)
C13—C14	1.389 (2)	C36—H32	1.09 (2)
P2—Fe1—P1	154.367 (16)	C15—C14—C13	119.51 (15)
C37—Fe1—P1	103.48 (5)	H13—C14—C13	117.7 (12)
C37—Fe1—P2	95.98 (5)	H13—C14—C15	122.8 (12)
C38—Fe1—P1	97.54 (4)	C16—C15—C14	120.66 (15)
C38—Fe1—P2	95.00 (4)	H14—C15—C14	120.5 (14)
C38—Fe1—C37	100.77 (7)	H14—C15—C16	118.9 (14)
H1—Fe1—P1	81.9 (8)	C17—C16—C15	119.09 (14)
H1—Fe1—P2	82.7 (8)	H15—C16—C15	118.6 (14)
H1—Fe1—C37	86.6 (8)	H15—C16—C17	122.3 (14)
H1—Fe1—C38	172.5 (8)	C18—C17—C16	120.98 (15)
H2—Fe1—P1	76.1 (8)	H16—C17—C16	118.8 (12)
H2—Fe1—P2	81.5 (8)	H16—C17—C18	120.2 (12)
H2—Fe1—C37	168.5 (9)	C17—C18—C13	119.19 (14)
H2—Fe1—C38	90.6 (9)	H17—C18—C13	117.8 (11)
H2—Fe1—H1	82.0 (12)	H17—C18—C17	123.0 (11)
O1—P1—Fe1	120.11 (4)	C20—C19—O4	115.16 (12)
O2—P1—Fe1	113.93 (4)	C24—C19—O4	123.76 (12)
O2—P1—O1	98.13 (5)	C24—C19—C20	121.08 (14)
O3—P1—Fe1	121.63 (4)	C21—C20—C19	119.44 (14)
O3—P1—O1	95.77 (5)	H18—C20—C19	118.1 (11)
O3—P1—O2	103.23 (5)	H18—C20—C21	122.4 (11)
O4—P2—Fe1	120.25 (4)	C22—C21—C20	120.38 (14)
O5—P2—Fe1	111.52 (4)	H19—C21—C20	117.5 (13)
O5—P2—O4	98.99 (5)	H19—C21—C22	122.1 (13)
O6—P2—Fe1	123.05 (4)	C23—C22—C21	119.52 (15)
O6—P2—O4	96.66 (5)	H20—C22—C21	119.3 (12)
O6—P2—O5	102.45 (5)	H20—C22—C23	121.2 (12)
C1—O1—P1	126.76 (8)	C24—C23—C22	120.81 (14)
C7—O2—P1	123.63 (9)	H21—C23—C22	119.3 (13)
C13—O3—P1	124.32 (8)	H21—C23—C24	119.9 (13)
C19—O4—P2	128.02 (8)	C23—C24—C19	118.75 (13)
C25—O5—P2	124.81 (9)	H22—C24—C19	124.7 (11)
C31—O6—P2	130.45 (9)	H22—C24—C23	116.5 (11)
C2—C1—O1	119.55 (12)	C26—C25—O5	117.45 (13)
C6—C1—O1	118.60 (12)	C30—C25—O5	120.51 (13)
C6—C1—C2	121.62 (13)	C30—C25—C26	121.79 (13)
C3—C2—C1	119.15 (14)	C27—C26—C25	119.07 (16)
H3—C2—C1	119.7 (12)	H23—C26—C25	117.8 (12)
H3—C2—C3	121.2 (12)	H23—C26—C27	123.1 (12)
C4—C3—C2	120.28 (15)	C28—C27—C26	120.13 (17)
H4—C3—C2	119.4 (13)	H24—C27—C26	117.7 (15)
H4—C3—C4	120.2 (13)	H24—C27—C28	122.2 (14)
C5—C4—C3	119.74 (15)	C29—C28—C27	119.81 (14)
H5—C4—C3	120.4 (14)	H25—C28—C27	119.6 (15)
H5—C4—C5	119.8 (14)	H25—C28—C29	120.6 (15)
C6—C5—C4	120.47 (15)	C30—C29—C28	120.68 (16)
H6—C5—C4	120.0 (12)	H26—C29—C28	119.6 (13)
H6—C5—C6	119.5 (13)	H26—C29—C30	119.7 (13)
C5—C6—C1	118.73 (14)	C29—C30—C25	118.51 (15)
H7—C6—C1	122.0 (12)	H27—C30—C25	120.5 (10)
H7—C6—C5	119.3 (12)	H27—C30—C29	121.0 (11)
C8—C7—O2	117.88 (12)	C32—C31—O6	122.45 (12)
C12—C7—O2	120.28 (13)	C36—C31—O6	116.19 (13)
C12—C7—C8	121.80 (13)	C36—C31—C32	121.31 (13)
C9—C8—C7	118.77 (14)	C33—C32—C31	118.82 (14)
H8—C8—C7	118.3 (11)	H28—C32—C31	121.1 (11)
H8—C8—C9	122.9 (11)	H28—C32—C33	120.1 (11)
C10—C9—C8	120.33 (15)	C34—C33—C32	120.67 (16)
H9—C9—C8	118.7 (12)	H29—C33—C32	118.8 (12)
H9—C9—C10	120.9 (12)	H29—C33—C34	120.5 (12)
C11—C10—C9	119.71 (14)	C35—C34—C33	119.70 (14)
H10—C10—C9	118.7 (14)	H30—C34—C33	120.0 (13)
H10—C10—C11	121.6 (14)	H30—C34—C35	120.3 (13)
C12—C11—C10	120.62 (14)	C36—C35—C34	120.36 (14)
H11—C11—C10	120.8 (12)	H31—C35—C34	119.6 (13)
H11—C11—C12	118.6 (13)	H31—C35—C36	120.1 (13)
C11—C12—C7	118.76 (15)	C35—C36—C31	119.13 (15)
H12—C12—C7	121.4 (11)	H32—C36—C31	120.8 (11)
H12—C12—C11	119.8 (11)	H32—C36—C35	120.1 (11)
C14—C13—O3	116.49 (13)	O7—C37—Fe1	177.59 (17)
C18—C13—O3	122.91 (12)	O8—C38—Fe1	177.30 (13)
C18—C13—C14	120.55 (13)

Dicarbonyl-cis-dihydrido-trans-bis(triphenylphosphite)iron(II) (QOSZON_HAR_SHADE3_1)

Crystal data

C38H32FeO8P2	Z = 2
Mr = 734.47	F(000) = 761.455
Triclinic, P1	Dx = 1.431 Mg m^−3
a = 9.6397 (12) Å	Mo Kα radiation, λ = 0.71073 Å
b = 10.4410 (13) Å	Cell parameters from 5000 reflections
c = 18.381 (2) Å	θ = 3.3–52.1°
α = 102.148 (15)°	µ = 0.59 mm^−1
β = 94.667 (15)°	T = 293 K
γ = 107.402 (14)°	Parallelepiped, colourless
V = 1705.0 (4) Å^3	0.5 × 0.25 × 0.1 mm

Data collection

STOE diffractometer	Rint = 0.034
Detector resolution: 1.60 pixels mm^-1	θmax = 26.1°, θmin = 2.1°
rotation en phi scans	h = −11→11
16806 measured reflections	k = −12→12
6202 independent reflections	l = −22→22
5084 reflections with I ≥ 2u(I)

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.020	Only H-atom coordinates refined
wR(F^2) = 0.051	w = 1/[σ^2(Fo^2) + (0.0387P)^2 + 0.3279P] where P = (Fo^2 + 2Fc^2)/3
S = 0.73	(Δ/σ)max = 0.001
6202 reflections	Δρmax = 0.22 e Å^−3
538 parameters	Δρmin = −0.25 e Å^−3

Special details

Experimental. The crystal was pasted on a glass fiber, by using an oil-coated shock-cooled crystal.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Fe1	0.531702 (18)	0.836466 (19)	0.270676 (9)	0.01845 (5)
P1	0.35096 (3)	0.72595 (3)	0.185417 (17)	0.01838 (7)
P2	0.72501 (3)	1.00381 (3)	0.322138 (16)	0.01833 (7)
O1	0.30696 (10)	0.79744 (9)	0.12204 (5)	0.0248 (2)
O2	0.37089 (9)	0.59222 (9)	0.13041 (5)	0.02289 (19)
O3	0.18561 (9)	0.66713 (9)	0.20473 (5)	0.0237 (2)
O4	0.71938 (10)	1.12336 (10)	0.39185 (5)	0.0248 (2)
O5	0.84516 (9)	0.95249 (9)	0.36179 (5)	0.0237 (2)
O6	0.82088 (9)	1.10485 (9)	0.27663 (5)	0.0250 (2)
O7	0.40856 (13)	0.81929 (15)	0.41022 (6)	0.0553 (3)
O8	0.67923 (12)	0.62712 (12)	0.25560 (6)	0.0419 (3)
C1	0.32779 (13)	0.93698 (13)	0.13016 (6)	0.0198 (3)
C2	0.22445 (14)	0.99263 (15)	0.15932 (7)	0.0271 (3)
C3	0.23801 (17)	1.12922 (17)	0.15994 (8)	0.0353 (3)
C4	0.35455 (17)	1.20898 (16)	0.13207 (9)	0.0359 (3)
C5	0.45817 (15)	1.15165 (16)	0.10380 (9)	0.0331 (3)
C6	0.44558 (14)	1.01500 (15)	0.10274 (7)	0.0260 (3)
C7	0.29358 (13)	0.53191 (13)	0.05767 (7)	0.0215 (3)
C8	0.36304 (16)	0.56778 (15)	−0.00196 (8)	0.0309 (3)
C9	0.28935 (18)	0.50545 (16)	−0.07506 (8)	0.0371 (4)
C10	0.14822 (17)	0.40978 (16)	−0.08809 (8)	0.0356 (3)
C11	0.08168 (16)	0.37556 (16)	−0.02754 (8)	0.0353 (3)
C12	0.15462 (14)	0.43583 (15)	0.04590 (8)	0.0291 (3)
C13	0.14880 (13)	0.58909 (13)	0.25701 (7)	0.0214 (3)
C14	0.03556 (14)	0.60727 (16)	0.29573 (8)	0.0302 (3)
C15	−0.01089 (16)	0.52839 (18)	0.34674 (8)	0.0372 (4)
C16	0.05554 (16)	0.43227 (16)	0.35970 (8)	0.0348 (3)
C17	0.16836 (16)	0.41513 (16)	0.32056 (8)	0.0324 (3)
C18	0.21556 (14)	0.49273 (15)	0.26878 (8)	0.0269 (3)
C19	0.67136 (13)	1.23479 (13)	0.38984 (7)	0.0214 (3)
C20	0.70012 (14)	1.33292 (14)	0.45794 (7)	0.0263 (3)
C21	0.65343 (16)	1.44762 (16)	0.46200 (8)	0.0322 (3)
C22	0.57914 (16)	1.46441 (16)	0.39842 (8)	0.0337 (3)
C23	0.55272 (15)	1.36613 (15)	0.33060 (8)	0.0302 (3)
C24	0.59870 (14)	1.25055 (14)	0.32547 (7)	0.0258 (3)
C25	0.98952 (13)	1.03521 (14)	0.39225 (7)	0.0232 (3)
C26	1.09989 (15)	1.01461 (17)	0.35247 (9)	0.0343 (3)
C27	1.24564 (17)	1.08633 (19)	0.38429 (11)	0.0458 (4)
C28	1.27969 (16)	1.17643 (18)	0.45518 (10)	0.0441 (4)
C29	1.16706 (16)	1.19611 (16)	0.49416 (9)	0.0380 (4)
C30	1.02049 (15)	1.12553 (15)	0.46285 (8)	0.0286 (3)
C31	0.82802 (12)	1.08537 (14)	0.20077 (7)	0.0202 (3)
C32	0.83573 (14)	0.96245 (15)	0.15667 (7)	0.0245 (3)
C33	0.84569 (15)	0.95265 (17)	0.08086 (8)	0.0306 (3)
C34	0.84993 (15)	1.06353 (17)	0.04961 (7)	0.0320 (3)
C35	0.84394 (14)	1.18615 (16)	0.09480 (8)	0.0296 (3)
C36	0.83330 (14)	1.19779 (15)	0.17081 (7)	0.0252 (3)
C37	0.45608 (15)	0.82301 (16)	0.35564 (8)	0.0313 (3)
C38	0.61941 (14)	0.70737 (15)	0.26258 (7)	0.0263 (3)
H1	0.4683 (19)	0.9517 (18)	0.2688 (10)	0.043455
H2	0.5857 (18)	0.8740 (19)	0.2012 (9)	0.041723
H3	0.1338 (18)	0.9291 (18)	0.1804 (10)	0.040070
H4	0.1532 (19)	1.1731 (19)	0.1807 (11)	0.044504
H5	0.3637 (19)	1.3145 (19)	0.1310 (11)	0.046276
H6	0.5491 (18)	1.2142 (19)	0.0809 (10)	0.040968
H7	0.5258 (19)	0.9704 (18)	0.0791 (9)	0.038043
H8	0.4747 (18)	0.644 (2)	0.0107 (9)	0.041945
H9	0.343 (2)	0.528 (2)	−0.1227 (10)	0.050025
H10	0.092 (2)	0.363 (2)	−0.1458 (10)	0.053748
H11	−0.0302 (19)	0.3004 (19)	−0.0376 (10)	0.046007
H12	0.1058 (18)	0.4076 (19)	0.0922 (10)	0.040938
H13	−0.0113 (19)	0.684 (2)	0.2855 (10)	0.045308
H14	−0.101 (2)	0.539 (2)	0.3762 (11)	0.054197
H15	0.014 (2)	0.368 (2)	0.3999 (11)	0.056417
H16	0.218 (2)	0.338 (2)	0.3292 (10)	0.047594
H17	0.2996 (18)	0.4777 (18)	0.2361 (10)	0.039425
H18	0.760 (2)	1.3168 (19)	0.5067 (10)	0.045409
H19	0.677 (2)	1.522 (2)	0.5152 (10)	0.050087
H20	0.545 (2)	1.555 (2)	0.4028 (10)	0.050415
H21	0.4949 (19)	1.3788 (18)	0.2804 (10)	0.041360
H22	0.5740 (18)	1.1754 (18)	0.2700 (9)	0.035962
H23	1.0679 (18)	0.9412 (19)	0.2967 (10)	0.043708
H24	1.3312 (19)	1.070 (2)	0.3523 (11)	0.050678
H25	1.3963 (19)	1.231 (2)	0.4812 (11)	0.055228
H26	1.1936 (19)	1.266 (2)	0.5502 (10)	0.050032
H27	0.9339 (19)	1.142 (2)	0.4933 (10)	0.044477
H28	0.8320 (18)	0.8735 (18)	0.1806 (9)	0.037841
H29	0.8503 (19)	0.856 (2)	0.0461 (10)	0.043471
H30	0.854 (2)	1.053 (2)	−0.0097 (9)	0.049309
H31	0.8457 (19)	1.2714 (19)	0.0703 (10)	0.044595
H32	0.8288 (18)	1.2951 (19)	0.2060 (9)	0.038536

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Fe1	0.01685 (9)	0.01939 (10)	0.01704 (9)	0.00245 (7)	0.00081 (6)	0.00579 (7)
P1	0.01698 (14)	0.01733 (17)	0.01922 (14)	0.00280 (12)	0.00016 (11)	0.00613 (13)
P2	0.01848 (15)	0.01833 (17)	0.01595 (14)	0.00314 (12)	0.00128 (11)	0.00412 (12)
O1	0.0295 (5)	0.0190 (5)	0.0220 (4)	0.0037 (4)	−0.0045 (3)	0.0065 (4)
O2	0.0224 (4)	0.0211 (5)	0.0237 (4)	0.0069 (4)	−0.0004 (3)	0.0041 (4)
O3	0.0173 (4)	0.0257 (5)	0.0293 (4)	0.0054 (4)	0.0030 (3)	0.0120 (4)
O4	0.0305 (5)	0.0256 (5)	0.0180 (4)	0.0107 (4)	0.0020 (3)	0.0033 (4)
O5	0.0201 (4)	0.0217 (5)	0.0260 (4)	0.0034 (4)	−0.0024 (3)	0.0061 (4)
O6	0.0276 (5)	0.0225 (5)	0.0189 (4)	−0.0004 (4)	0.0035 (3)	0.0049 (4)
O7	0.0529 (7)	0.0764 (10)	0.0287 (6)	0.0028 (6)	0.0172 (5)	0.0186 (6)
O8	0.0428 (6)	0.0343 (7)	0.0522 (6)	0.0209 (5)	0.0021 (5)	0.0081 (5)
C1	0.0202 (6)	0.0202 (7)	0.0196 (5)	0.0064 (5)	0.0024 (4)	0.0070 (5)
C2	0.0262 (7)	0.0308 (8)	0.0262 (6)	0.0112 (6)	0.0077 (5)	0.0070 (6)
C3	0.0388 (8)	0.0337 (9)	0.0358 (7)	0.0199 (7)	0.0045 (6)	0.0025 (7)
C4	0.0408 (8)	0.0226 (8)	0.0441 (8)	0.0120 (6)	−0.0041 (6)	0.0094 (7)
C5	0.0288 (7)	0.0250 (8)	0.0467 (8)	0.0046 (6)	0.0037 (6)	0.0185 (7)
C6	0.0224 (6)	0.0254 (8)	0.0339 (7)	0.0077 (5)	0.0075 (5)	0.0140 (6)
C7	0.0206 (6)	0.0186 (7)	0.0237 (6)	0.0056 (5)	0.0008 (5)	0.0038 (5)
C8	0.0339 (7)	0.0286 (8)	0.0257 (7)	0.0039 (6)	0.0044 (6)	0.0062 (6)
C9	0.0516 (9)	0.0325 (9)	0.0229 (7)	0.0095 (7)	0.0036 (6)	0.0045 (6)
C10	0.0458 (9)	0.0292 (8)	0.0261 (7)	0.0127 (7)	−0.0069 (6)	−0.0014 (6)
C11	0.0294 (7)	0.0310 (8)	0.0339 (8)	0.0032 (6)	−0.0068 (6)	−0.0031 (6)
C12	0.0242 (7)	0.0252 (8)	0.0296 (7)	0.0008 (6)	0.0006 (5)	0.0014 (6)
C13	0.0164 (6)	0.0205 (7)	0.0261 (6)	0.0034 (5)	0.0032 (5)	0.0071 (5)
C14	0.0260 (7)	0.0327 (8)	0.0354 (7)	0.0107 (6)	0.0106 (6)	0.0114 (6)
C15	0.0311 (7)	0.0454 (10)	0.0382 (8)	0.0096 (7)	0.0169 (6)	0.0163 (7)
C16	0.0329 (7)	0.0362 (9)	0.0323 (7)	0.0022 (6)	0.0075 (6)	0.0143 (7)
C17	0.0346 (7)	0.0290 (8)	0.0356 (7)	0.0080 (6)	0.0052 (6)	0.0161 (6)
C18	0.0257 (6)	0.0258 (8)	0.0338 (7)	0.0093 (6)	0.0084 (5)	0.0141 (6)
C19	0.0221 (6)	0.0203 (7)	0.0192 (6)	0.0046 (5)	0.0029 (5)	0.0029 (5)
C20	0.0309 (7)	0.0222 (7)	0.0214 (6)	0.0042 (6)	0.0054 (5)	0.0014 (5)
C21	0.0392 (8)	0.0242 (8)	0.0289 (7)	0.0077 (6)	0.0097 (6)	−0.0004 (6)
C22	0.0385 (8)	0.0240 (8)	0.0389 (8)	0.0128 (6)	0.0089 (6)	0.0036 (6)
C23	0.0318 (7)	0.0230 (8)	0.0343 (7)	0.0094 (6)	−0.0008 (6)	0.0051 (6)
C24	0.0271 (6)	0.0242 (8)	0.0234 (6)	0.0074 (5)	−0.0014 (5)	0.0033 (6)
C25	0.0202 (6)	0.0213 (7)	0.0250 (6)	0.0032 (5)	−0.0003 (5)	0.0057 (5)
C26	0.0242 (7)	0.0368 (9)	0.0396 (8)	0.0077 (6)	0.0069 (6)	0.0072 (7)
C27	0.0216 (7)	0.0464 (11)	0.0684 (11)	0.0069 (7)	0.0097 (7)	0.0168 (9)
C28	0.0217 (7)	0.0372 (10)	0.0649 (11)	−0.0021 (7)	−0.0064 (7)	0.0169 (8)
C29	0.0323 (8)	0.0281 (8)	0.0408 (8)	−0.0024 (6)	−0.0123 (6)	0.0060 (7)
C30	0.0261 (7)	0.0258 (8)	0.0280 (7)	0.0035 (6)	−0.0027 (5)	0.0042 (6)
C31	0.0187 (5)	0.0210 (7)	0.0200 (5)	0.0046 (5)	0.0023 (4)	0.0061 (5)
C32	0.0269 (6)	0.0251 (8)	0.0232 (6)	0.0100 (5)	0.0075 (5)	0.0063 (6)
C33	0.0333 (7)	0.0348 (9)	0.0241 (7)	0.0132 (6)	0.0076 (5)	0.0040 (6)
C34	0.0307 (7)	0.0460 (10)	0.0203 (6)	0.0115 (6)	0.0058 (5)	0.0113 (6)
C35	0.0290 (7)	0.0366 (9)	0.0284 (7)	0.0102 (6)	0.0071 (5)	0.0189 (7)
C36	0.0265 (6)	0.0234 (8)	0.0267 (6)	0.0059 (5)	0.0056 (5)	0.0112 (6)
C37	0.0283 (7)	0.0384 (9)	0.0235 (7)	0.0033 (6)	0.0041 (5)	0.0108 (6)
C38	0.0247 (6)	0.0234 (8)	0.0297 (6)	0.0070 (6)	0.0008 (5)	0.0070 (6)
H1	0.050510	0.032410	0.049170	0.015320	0.004270	0.012320
H2	0.040840	0.054000	0.031110	0.012410	0.011750	0.014150
H3	0.029570	0.036170	0.053700	0.008420	0.008820	0.011830
H4	0.037090	0.034310	0.063650	0.016170	0.005150	0.009680
H5	0.045040	0.030390	0.064070	0.010400	0.002900	0.017860
H6	0.039860	0.039070	0.044520	0.007970	0.007450	0.018170
H7	0.040470	0.035630	0.039100	0.013300	0.008560	0.009200
H8	0.035360	0.048250	0.035060	0.007910	0.001630	0.004760
H9	0.055510	0.055620	0.030390	0.011780	0.004500	0.002380
H10	0.056270	0.056240	0.033390	0.009180	−0.011030	−0.001470
H11	0.036780	0.042480	0.047540	0.005620	−0.009850	0.004050
H12	0.035920	0.043170	0.039320	0.008010	0.000650	0.009820
H13	0.041720	0.040340	0.055190	0.010950	0.013240	0.015870
H14	0.044400	0.056150	0.059690	0.006290	0.021880	0.018660
H15	0.053340	0.054650	0.058130	−0.000640	0.015760	0.031010
H16	0.048430	0.038050	0.055400	0.005360	0.002170	0.024470
H17	0.038430	0.036760	0.044340	0.011080	0.007170	0.014010
H18	0.053460	0.044100	0.031480	0.008800	0.001330	0.006300
H19	0.055730	0.040600	0.040720	0.009330	0.004740	−0.007790
H20	0.055010	0.031800	0.058700	0.015450	0.004010	−0.001170
H21	0.044070	0.034280	0.044280	0.013200	0.000460	0.008330
H22	0.041680	0.030530	0.031060	0.009560	0.000930	0.002730
H23	0.033000	0.042030	0.047940	0.008270	−0.003160	0.003060
H24	0.031280	0.047950	0.068200	0.012080	−0.001150	0.009050
H25	0.033410	0.052790	0.067140	0.005850	−0.016370	0.009610
H26	0.046520	0.046180	0.042100	0.002280	−0.013880	0.004880
H27	0.040690	0.047330	0.037650	0.007660	−0.001290	0.006450
H28	0.040980	0.034490	0.038560	0.010080	0.009560	0.011950
H29	0.047310	0.040640	0.038280	0.010790	0.013710	0.003240
H30	0.059070	0.054130	0.031630	0.009370	0.018290	0.012840
H31	0.051540	0.041160	0.040170	0.005260	0.011780	0.020560
H32	0.044260	0.030860	0.036560	0.006870	0.005910	0.007860

Geometric parameters (Å, º)

Fe1—P1	2.1012 (6)	C13—C18	1.3891 (19)
Fe1—P2	2.1190 (6)	C14—C15	1.389 (2)
Fe1—C37	1.7907 (14)	C14—H13	1.067 (19)
Fe1—C38	1.7809 (15)	C15—C16	1.391 (2)
Fe1—H1	1.508 (17)	C15—H14	1.078 (19)
Fe1—H2	1.500 (16)	C16—C17	1.386 (2)
P1—O1	1.6029 (9)	C16—H15	1.116 (18)
P1—O2	1.6145 (10)	C17—C18	1.3943 (19)
P1—O3	1.6254 (9)	C17—H16	1.086 (19)
P2—O4	1.6067 (10)	C18—H17	1.075 (17)
P2—O5	1.5994 (9)	C19—C20	1.3883 (18)
P2—O6	1.6064 (9)	C19—C24	1.3906 (17)
O1—C1	1.3834 (15)	C20—C21	1.390 (2)
O2—C7	1.3937 (14)	C20—H18	1.096 (17)
O3—C13	1.3876 (15)	C21—C22	1.391 (2)
O4—C19	1.3808 (16)	C21—H19	1.073 (18)
O5—C25	1.3952 (14)	C22—C23	1.388 (2)
O6—C31	1.3766 (14)	C22—H20	1.084 (19)
O7—C37	1.1395 (18)	C23—C24	1.393 (2)
O8—C38	1.1432 (17)	C23—H21	1.091 (16)
C1—C2	1.3854 (18)	C24—H22	1.106 (16)
C1—C6	1.3855 (17)	C25—C26	1.382 (2)
C2—C3	1.390 (2)	C25—C30	1.3841 (19)
C2—H3	1.082 (17)	C26—C27	1.389 (2)
C3—C4	1.390 (2)	C26—H23	1.100 (18)
C3—H4	1.107 (18)	C27—C28	1.386 (3)
C4—C5	1.392 (2)	C27—H24	1.085 (19)
C4—H5	1.083 (18)	C28—C29	1.390 (2)
C5—C6	1.391 (2)	C28—H25	1.110 (17)
C5—H6	1.097 (17)	C29—C30	1.3918 (19)
C6—H7	1.090 (18)	C29—H26	1.092 (18)
C7—C8	1.3899 (19)	C30—H27	1.078 (19)
C7—C12	1.3802 (18)	C31—C32	1.392 (2)
C8—C9	1.391 (2)	C31—C36	1.3872 (18)
C8—H8	1.103 (17)	C32—C33	1.3888 (18)
C9—C10	1.393 (2)	C32—H28	1.101 (17)
C9—H9	1.084 (18)	C33—C34	1.388 (2)
C10—C11	1.387 (2)	C33—H29	1.093 (19)
C10—H10	1.090 (16)	C34—C35	1.392 (2)
C11—C12	1.3914 (19)	C34—H30	1.077 (16)
C11—H11	1.102 (17)	C35—C36	1.3916 (19)
C12—H12	1.059 (18)	C35—H31	1.075 (17)
C13—C14	1.3884 (19)	C36—H32	1.098 (19)
P2—Fe1—P1	154.362 (15)	C15—C14—C13	119.55 (14)
C37—Fe1—P1	103.51 (4)	H13—C14—C13	117.9 (10)
C37—Fe1—P2	95.96 (4)	H13—C14—C15	122.5 (10)
C38—Fe1—P1	97.51 (4)	C16—C15—C14	120.67 (14)
C38—Fe1—P2	95.03 (4)	H14—C15—C14	120.8 (11)
C38—Fe1—C37	100.76 (7)	H14—C15—C16	118.5 (11)
H1—Fe1—P1	81.8 (7)	C17—C16—C15	119.14 (13)
H1—Fe1—P2	82.7 (7)	H15—C16—C15	119.3 (11)
H1—Fe1—C37	87.0 (7)	H15—C16—C17	121.5 (11)
H1—Fe1—C38	172.1 (7)	C18—C17—C16	120.92 (14)
H2—Fe1—P1	76.6 (6)	H16—C17—C16	119.5 (10)
H2—Fe1—P2	80.9 (7)	H16—C17—C18	119.6 (10)
H2—Fe1—C37	168.1 (7)	C17—C18—C13	119.16 (13)
H2—Fe1—C38	90.9 (7)	H17—C18—C13	118.8 (9)
H2—Fe1—H1	81.2 (10)	H17—C18—C17	122.0 (9)
O1—P1—Fe1	120.12 (3)	C20—C19—O4	115.07 (11)
O2—P1—Fe1	113.91 (3)	C24—C19—O4	123.87 (11)
O2—P1—O1	98.13 (5)	C24—C19—C20	121.06 (13)
O3—P1—Fe1	121.61 (3)	C21—C20—C19	119.38 (12)
O3—P1—O1	95.80 (5)	H18—C20—C19	118.2 (10)
O3—P1—O2	103.24 (5)	H18—C20—C21	122.4 (10)
O4—P2—Fe1	120.24 (4)	C22—C21—C20	120.40 (13)
O5—P2—Fe1	111.53 (4)	H19—C21—C20	117.9 (11)
O5—P2—O4	99.03 (5)	H19—C21—C22	121.7 (11)
O6—P2—Fe1	123.05 (3)	C23—C22—C21	119.48 (14)
O6—P2—O4	96.63 (5)	H20—C22—C21	119.0 (10)
O6—P2—O5	102.46 (5)	H20—C22—C23	121.5 (10)
C1—O1—P1	126.74 (7)	C24—C23—C22	120.92 (13)
C7—O2—P1	123.61 (8)	H21—C23—C22	119.9 (9)
C13—O3—P1	124.37 (7)	H21—C23—C24	119.2 (9)
C19—O4—P2	128.00 (8)	C23—C24—C19	118.75 (12)
C25—O5—P2	124.88 (8)	H22—C24—C19	123.5 (9)
C31—O6—P2	130.40 (8)	H22—C24—C23	117.7 (9)
C2—C1—O1	119.59 (11)	C26—C25—O5	117.58 (12)
C6—C1—O1	118.66 (11)	C30—C25—O5	120.47 (12)
C6—C1—C2	121.51 (12)	C30—C25—C26	121.71 (12)
C3—C2—C1	119.21 (13)	C27—C26—C25	119.08 (15)
H3—C2—C1	119.8 (9)	H23—C26—C25	118.1 (9)
H3—C2—C3	121.0 (9)	H23—C26—C27	122.8 (9)
C4—C3—C2	120.23 (14)	C28—C27—C26	120.37 (16)
H4—C3—C2	119.7 (10)	H24—C27—C26	118.3 (10)
H4—C3—C4	120.0 (10)	H24—C27—C28	121.3 (10)
C5—C4—C3	119.69 (14)	C29—C28—C27	119.67 (13)
H5—C4—C3	120.4 (10)	H25—C28—C27	120.2 (11)
H5—C4—C5	119.9 (10)	H25—C28—C29	120.1 (11)
C6—C5—C4	120.59 (13)	C30—C29—C28	120.62 (15)
H6—C5—C4	119.6 (10)	H26—C29—C28	119.8 (10)
H6—C5—C6	119.8 (10)	H26—C29—C30	119.6 (10)
C5—C6—C1	118.77 (13)	C29—C30—C25	118.55 (14)
H7—C6—C1	121.3 (9)	H27—C30—C25	121.4 (9)
H7—C6—C5	119.9 (9)	H27—C30—C29	120.1 (9)
C8—C7—O2	117.91 (11)	C32—C31—O6	122.47 (11)
C12—C7—O2	120.40 (11)	C36—C31—O6	116.14 (12)
C12—C7—C8	121.65 (12)	C36—C31—C32	121.33 (12)
C9—C8—C7	118.72 (13)	C33—C32—C31	118.68 (13)
H8—C8—C7	118.6 (9)	H28—C32—C31	121.2 (9)
H8—C8—C9	122.7 (9)	H28—C32—C33	120.1 (9)
C10—C9—C8	120.53 (14)	C34—C33—C32	120.89 (15)
H9—C9—C8	120.2 (9)	H29—C33—C32	118.7 (9)
H9—C9—C10	119.2 (9)	H29—C33—C34	120.4 (9)
C11—C10—C9	119.54 (12)	C35—C34—C33	119.59 (13)
H10—C10—C9	119.3 (10)	H30—C34—C33	119.8 (11)
H10—C10—C11	121.1 (10)	H30—C34—C35	120.6 (11)
C12—C11—C10	120.63 (13)	C36—C35—C34	120.37 (13)
H11—C11—C10	119.8 (9)	H31—C35—C34	119.5 (10)
H11—C11—C12	119.6 (9)	H31—C35—C36	120.2 (10)
C11—C12—C7	118.93 (13)	C35—C36—C31	119.12 (14)
H12—C12—C7	120.1 (9)	H32—C36—C31	121.1 (9)
H12—C12—C11	120.9 (9)	H32—C36—C35	119.8 (9)
C14—C13—O3	116.52 (12)	O7—C37—Fe1	177.59 (15)
C18—C13—O3	122.86 (11)	O8—C38—Fe1	177.26 (12)
C18—C13—C14	120.56 (12)
Fe1—P1—O1—C1	−29.98 (7)	O5—C25—C30—C29	173.84 (12)
Fe1—P1—O2—C7	−157.59 (7)	O6—C31—C32—C33	−178.69 (12)
Fe1—P1—O3—C13	−50.57 (7)	O6—C31—C36—C35	178.58 (10)
Fe1—P2—O4—C19	−79.73 (7)	C1—C2—C3—C4	−0.43 (14)
Fe1—P2—O5—C25	171.80 (8)	C1—C6—C5—C4	0.17 (15)
Fe1—P2—O6—C31	−20.82 (7)	C2—C3—C4—C5	−0.29 (16)
P1—O1—C1—C2	−84.60 (10)	C3—C4—C5—C6	0.42 (16)
P1—O1—C1—C6	100.91 (10)	C7—C8—C9—C10	0.50 (17)
P1—O2—C7—C8	97.67 (11)	C7—C12—C11—C10	0.95 (17)
P1—O2—C7—C12	−84.70 (11)	C8—C9—C10—C11	−0.71 (19)
P1—O3—C13—C14	147.06 (11)	C9—C10—C11—C12	−0.03 (18)
P1—O3—C13—C18	−35.67 (11)	C13—C14—C15—C16	0.42 (16)
P2—O4—C19—C20	−170.55 (11)	C13—C18—C17—C16	0.51 (16)
P2—O4—C19—C24	9.72 (12)	C14—C15—C16—C17	−0.49 (18)
P2—O5—C25—C26	−105.54 (11)	C15—C16—C17—C18	0.02 (17)
P2—O5—C25—C30	79.96 (11)	C19—C20—C21—C22	−0.27 (15)
P2—O6—C31—C32	−43.98 (12)	C19—C24—C23—C22	0.29 (15)
P2—O6—C31—C36	138.61 (11)	C20—C21—C22—C23	−0.43 (16)
O1—C1—C2—C3	−173.28 (11)	C21—C22—C23—C24	0.42 (16)
O1—C1—C6—C5	173.46 (11)	C25—C26—C27—C28	0.48 (18)
O2—C7—C8—C9	178.06 (13)	C25—C30—C29—C28	0.17 (16)
O2—C7—C12—C11	−178.72 (13)	C26—C27—C28—C29	−0.7 (2)
O3—C13—C14—C15	177.46 (12)	C27—C28—C29—C30	0.41 (19)
O3—C13—C18—C17	−177.75 (12)	C31—C32—C33—C34	0.87 (14)
O4—C19—C20—C21	−178.74 (11)	C31—C36—C35—C34	−0.32 (14)
O4—C19—C24—C23	178.71 (12)	C32—C33—C34—C35	−0.08 (15)
O5—C25—C26—C27	−174.32 (13)	C33—C34—C35—C36	−0.20 (15)

(QOSZON_HAR_SHADE3)

Crystal data

C38H32FeO8P2	Z = 2
Mr = 734.47	F(000) = 761.455
Triclinic, P1	Dx = 1.431 Mg m^−3
a = 9.6397 (12) Å	Mo Kα radiation, λ = 0.71073 Å
b = 10.4410 (13) Å	Cell parameters from 5000 reflections
c = 18.381 (2) Å	θ = 3.3–52.1°
α = 102.148 (15)°	µ = 0.59 mm^−1
β = 94.667 (15)°	T = 293 K
γ = 107.402 (14)°	Parallelepiped, colourless
V = 1705.0 (4) Å^3	0.5 × 0.25 × 0.1 mm

Data collection

STOE diffractometer	Rint = 0.034
rotation en phi scans	θmax = 26.1°, θmin = 2.1°
16806 measured reflections	h = −11→11
6202 independent reflections	k = −12→12
5084 reflections with I ≥ 2u(I)	l = −22→22

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.020	Only H-atom coordinates refined
wR(F^2) = 0.050	w = 1/[σ^2(Fo^2) + (0.0364P)^2 + 0.4163P] where P = (Fo^2 + 2Fc^2)/3
S = 0.73	(Δ/σ)max = 0.001
6202 reflections	Δρmax = 0.22 e Å^−3
538 parameters	Δρmin = −0.24 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Fe1	0.531703 (18)	0.836466 (19)	0.270677 (9)	0.01844 (5)
P1	0.35096 (3)	0.72595 (3)	0.185418 (17)	0.01837 (7)
P2	0.72502 (3)	1.00382 (3)	0.322138 (16)	0.01832 (7)
O1	0.30696 (9)	0.79744 (9)	0.12204 (5)	0.0247 (2)
O2	0.37090 (9)	0.59222 (9)	0.13041 (5)	0.02288 (19)
O3	0.18562 (9)	0.66713 (9)	0.20473 (5)	0.0237 (2)
O4	0.71938 (10)	1.12336 (10)	0.39185 (5)	0.0247 (2)
O5	0.84516 (9)	0.95249 (9)	0.36179 (5)	0.0237 (2)
O6	0.82088 (9)	1.10485 (9)	0.27663 (5)	0.0250 (2)
O7	0.40856 (13)	0.81929 (15)	0.41022 (6)	0.0553 (3)
O8	0.67923 (12)	0.62712 (12)	0.25560 (6)	0.0419 (3)
C1	0.32780 (13)	0.93698 (13)	0.13016 (6)	0.0198 (3)
C2	0.22446 (14)	0.99264 (15)	0.15931 (7)	0.0271 (3)
C3	0.23800 (17)	1.12923 (17)	0.15995 (8)	0.0352 (3)
C4	0.35456 (17)	1.20899 (16)	0.13207 (9)	0.0359 (3)
C5	0.45818 (15)	1.15164 (15)	0.10380 (9)	0.0331 (3)
C6	0.44557 (14)	1.01501 (15)	0.10274 (7)	0.0260 (3)
C7	0.29358 (13)	0.53191 (13)	0.05767 (7)	0.0215 (3)
C8	0.36305 (16)	0.56779 (15)	−0.00196 (8)	0.0309 (3)
C9	0.28936 (18)	0.50544 (16)	−0.07506 (8)	0.0371 (4)
C10	0.14821 (17)	0.40978 (16)	−0.08810 (8)	0.0356 (3)
C11	0.08166 (16)	0.37555 (16)	−0.02754 (8)	0.0353 (3)
C12	0.15462 (14)	0.43583 (15)	0.04591 (8)	0.0290 (3)
C13	0.14881 (13)	0.58909 (13)	0.25701 (7)	0.0214 (3)
C14	0.03556 (14)	0.60728 (16)	0.29573 (8)	0.0302 (3)
C15	−0.01091 (16)	0.52840 (18)	0.34675 (8)	0.0372 (4)
C16	0.05554 (16)	0.43226 (16)	0.35971 (8)	0.0348 (3)
C17	0.16837 (16)	0.41513 (16)	0.32056 (8)	0.0324 (3)
C18	0.21558 (14)	0.49272 (15)	0.26877 (8)	0.0269 (3)
C19	0.67137 (13)	1.23479 (13)	0.38983 (7)	0.0214 (3)
C20	0.70012 (14)	1.33293 (14)	0.45794 (7)	0.0263 (3)
C21	0.65345 (16)	1.44764 (16)	0.46201 (8)	0.0322 (3)
C22	0.57913 (16)	1.46444 (16)	0.39843 (8)	0.0336 (3)
C23	0.55271 (15)	1.36613 (15)	0.33061 (8)	0.0302 (3)
C24	0.59870 (14)	1.25055 (14)	0.32546 (7)	0.0258 (3)
C25	0.98952 (13)	1.03521 (14)	0.39225 (7)	0.0232 (3)
C26	1.09989 (15)	1.01463 (17)	0.35247 (9)	0.0342 (3)
C27	1.24564 (17)	1.08631 (19)	0.38428 (11)	0.0458 (4)
C28	1.27971 (16)	1.17642 (18)	0.45518 (10)	0.0440 (4)
C29	1.16707 (16)	1.19613 (16)	0.49417 (9)	0.0379 (4)
C30	1.02047 (15)	1.12552 (15)	0.46285 (8)	0.0285 (3)
C31	0.82801 (12)	1.08536 (14)	0.20077 (7)	0.0202 (3)
C32	0.83573 (13)	0.96245 (15)	0.15667 (7)	0.0244 (3)
C33	0.84570 (15)	0.95265 (17)	0.08086 (8)	0.0305 (3)
C34	0.84994 (15)	1.06354 (17)	0.04961 (7)	0.0319 (3)
C35	0.84394 (14)	1.18617 (16)	0.09480 (8)	0.0296 (3)
C36	0.83330 (14)	1.19780 (15)	0.17081 (7)	0.0251 (3)
C37	0.45608 (15)	0.82301 (16)	0.35564 (8)	0.0313 (3)
C38	0.61939 (14)	0.70737 (15)	0.26258 (7)	0.0263 (3)
H1	0.4683 (19)	0.9516 (18)	0.2688 (10)	0.042674
H2	0.5857 (18)	0.8740 (19)	0.2012 (9)	0.040747
H3	0.1339 (18)	0.9291 (18)	0.1804 (10)	0.040445
H4	0.1532 (19)	1.173 (2)	0.1808 (11)	0.046108
H5	0.3638 (19)	1.3146 (19)	0.1310 (11)	0.047921
H6	0.5491 (19)	1.2142 (19)	0.0810 (10)	0.041837
H7	0.5257 (18)	0.9703 (18)	0.0791 (9)	0.037568
H8	0.4748 (18)	0.6440 (19)	0.0107 (9)	0.041184
H9	0.343 (2)	0.528 (2)	−0.1228 (9)	0.050987
H10	0.092 (2)	0.363 (2)	−0.1458 (10)	0.056375
H11	−0.0304 (19)	0.3005 (19)	−0.0377 (10)	0.048036
H12	0.1058 (18)	0.4075 (18)	0.0923 (10)	0.041209
H13	−0.0113 (19)	0.684 (2)	0.2856 (10)	0.045348
H14	−0.101 (2)	0.539 (2)	0.3763 (11)	0.054846
H15	0.015 (2)	0.368 (2)	0.4000 (11)	0.057414
H16	0.218 (2)	0.3381 (19)	0.3292 (11)	0.047662
H17	0.2997 (18)	0.4777 (18)	0.2361 (9)	0.038539
H18	0.760 (2)	1.3169 (19)	0.5067 (10)	0.046180
H19	0.677 (2)	1.522 (2)	0.5153 (10)	0.052179
H20	0.545 (2)	1.555 (2)	0.4028 (11)	0.052679
H21	0.4949 (19)	1.3787 (18)	0.2804 (10)	0.042111
H22	0.5740 (18)	1.1754 (18)	0.2701 (9)	0.035412
H23	1.0680 (18)	0.9411 (19)	0.2968 (10)	0.043023
H24	1.3312 (19)	1.070 (2)	0.3523 (11)	0.051716
H25	1.3965 (19)	1.231 (2)	0.4812 (11)	0.057758
H26	1.1936 (19)	1.266 (2)	0.5503 (10)	0.052335
H27	0.9338 (19)	1.142 (2)	0.4934 (9)	0.044864
H28	0.8320 (18)	0.8734 (18)	0.1805 (9)	0.036685
H29	0.8502 (19)	0.8556 (19)	0.0460 (10)	0.042916
H30	0.854 (2)	1.053 (2)	−0.0098 (9)	0.049437
H31	0.8457 (19)	1.2715 (19)	0.0704 (10)	0.045130
H32	0.8287 (18)	1.2950 (19)	0.2060 (9)	0.038560

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Fe1	0.01684 (9)	0.01938 (10)	0.01703 (9)	0.00244 (7)	0.00081 (6)	0.00579 (7)
P1	0.01697 (14)	0.01731 (17)	0.01921 (14)	0.00279 (12)	0.00016 (11)	0.00612 (13)
P2	0.01846 (15)	0.01832 (17)	0.01593 (14)	0.00313 (12)	0.00128 (11)	0.00412 (12)
O1	0.0295 (5)	0.0190 (5)	0.0220 (4)	0.0037 (4)	−0.0044 (3)	0.0065 (4)
O2	0.0224 (4)	0.0211 (5)	0.0237 (4)	0.0069 (4)	−0.0004 (3)	0.0041 (4)
O3	0.0173 (4)	0.0257 (5)	0.0293 (4)	0.0054 (4)	0.0030 (3)	0.0120 (4)
O4	0.0305 (5)	0.0256 (5)	0.0180 (4)	0.0107 (4)	0.0020 (3)	0.0033 (4)
O5	0.0201 (4)	0.0217 (5)	0.0260 (4)	0.0034 (4)	−0.0024 (3)	0.0060 (4)
O6	0.0276 (5)	0.0225 (5)	0.0189 (4)	−0.0004 (4)	0.0035 (3)	0.0049 (4)
O7	0.0529 (7)	0.0764 (10)	0.0287 (6)	0.0028 (6)	0.0172 (5)	0.0186 (6)
O8	0.0428 (6)	0.0343 (7)	0.0521 (6)	0.0209 (5)	0.0021 (5)	0.0081 (5)
C1	0.0202 (6)	0.0202 (7)	0.0195 (5)	0.0064 (5)	0.0024 (4)	0.0070 (5)
C2	0.0262 (7)	0.0308 (8)	0.0262 (6)	0.0112 (6)	0.0077 (5)	0.0071 (6)
C3	0.0388 (8)	0.0336 (9)	0.0358 (7)	0.0199 (7)	0.0045 (6)	0.0026 (7)
C4	0.0407 (8)	0.0226 (8)	0.0441 (8)	0.0120 (6)	−0.0041 (6)	0.0094 (7)
C5	0.0289 (7)	0.0249 (8)	0.0467 (8)	0.0046 (6)	0.0037 (6)	0.0185 (7)
C6	0.0224 (6)	0.0254 (8)	0.0338 (7)	0.0077 (5)	0.0075 (5)	0.0140 (6)
C7	0.0206 (6)	0.0186 (7)	0.0237 (6)	0.0055 (5)	0.0008 (5)	0.0038 (5)
C8	0.0339 (7)	0.0286 (8)	0.0257 (7)	0.0039 (6)	0.0044 (6)	0.0062 (6)
C9	0.0516 (9)	0.0325 (9)	0.0229 (7)	0.0095 (7)	0.0036 (6)	0.0045 (6)
C10	0.0457 (9)	0.0291 (8)	0.0262 (7)	0.0126 (7)	−0.0069 (6)	−0.0014 (6)
C11	0.0294 (7)	0.0309 (8)	0.0338 (8)	0.0033 (6)	−0.0068 (6)	−0.0031 (6)
C12	0.0242 (7)	0.0251 (8)	0.0296 (7)	0.0007 (6)	0.0005 (5)	0.0014 (6)
C13	0.0165 (6)	0.0205 (7)	0.0261 (6)	0.0035 (5)	0.0032 (5)	0.0071 (5)
C14	0.0259 (7)	0.0327 (8)	0.0353 (7)	0.0107 (6)	0.0106 (6)	0.0114 (6)
C15	0.0311 (7)	0.0453 (10)	0.0382 (8)	0.0096 (7)	0.0168 (6)	0.0163 (7)
C16	0.0329 (7)	0.0361 (9)	0.0323 (7)	0.0022 (6)	0.0075 (6)	0.0142 (7)
C17	0.0346 (7)	0.0290 (8)	0.0356 (7)	0.0080 (6)	0.0052 (6)	0.0161 (6)
C18	0.0257 (6)	0.0258 (8)	0.0338 (7)	0.0093 (6)	0.0084 (5)	0.0141 (6)
C19	0.0221 (6)	0.0203 (7)	0.0192 (6)	0.0046 (5)	0.0028 (5)	0.0029 (5)
C20	0.0308 (7)	0.0222 (7)	0.0213 (6)	0.0042 (6)	0.0054 (5)	0.0014 (5)
C21	0.0393 (8)	0.0242 (8)	0.0289 (7)	0.0078 (6)	0.0097 (6)	−0.0004 (6)
C22	0.0384 (8)	0.0240 (8)	0.0388 (8)	0.0127 (6)	0.0088 (6)	0.0036 (6)
C23	0.0317 (7)	0.0230 (8)	0.0343 (7)	0.0094 (6)	−0.0008 (6)	0.0051 (6)
C24	0.0271 (6)	0.0242 (8)	0.0234 (6)	0.0074 (5)	−0.0014 (5)	0.0033 (6)
C25	0.0201 (6)	0.0214 (7)	0.0250 (6)	0.0032 (5)	−0.0003 (5)	0.0058 (5)
C26	0.0241 (7)	0.0368 (9)	0.0396 (8)	0.0076 (6)	0.0068 (6)	0.0072 (7)
C27	0.0215 (7)	0.0464 (11)	0.0684 (11)	0.0069 (7)	0.0097 (7)	0.0168 (9)
C28	0.0218 (7)	0.0372 (9)	0.0649 (11)	−0.0021 (7)	−0.0064 (7)	0.0169 (8)
C29	0.0322 (8)	0.0281 (8)	0.0407 (8)	−0.0024 (6)	−0.0122 (6)	0.0061 (7)
C30	0.0262 (7)	0.0257 (8)	0.0279 (7)	0.0035 (6)	−0.0028 (5)	0.0041 (6)
C31	0.0187 (5)	0.0209 (7)	0.0200 (5)	0.0046 (5)	0.0023 (4)	0.0061 (5)
C32	0.0269 (6)	0.0251 (8)	0.0232 (6)	0.0100 (5)	0.0075 (5)	0.0064 (6)
C33	0.0333 (7)	0.0348 (9)	0.0240 (7)	0.0132 (6)	0.0076 (5)	0.0040 (6)
C34	0.0307 (7)	0.0460 (10)	0.0204 (6)	0.0115 (6)	0.0058 (5)	0.0113 (6)
C35	0.0290 (7)	0.0366 (9)	0.0284 (7)	0.0101 (6)	0.0070 (5)	0.0188 (7)
C36	0.0265 (6)	0.0234 (8)	0.0267 (7)	0.0059 (5)	0.0056 (5)	0.0112 (6)
C37	0.0282 (7)	0.0384 (9)	0.0235 (7)	0.0033 (6)	0.0041 (5)	0.0107 (6)
C38	0.0247 (6)	0.0234 (8)	0.0297 (6)	0.0070 (6)	0.0008 (5)	0.0070 (6)
H1	0.050060	0.031780	0.048300	0.015700	0.004090	0.012190
H2	0.040090	0.052700	0.030120	0.011990	0.011640	0.013750
H3	0.029610	0.038100	0.053790	0.009660	0.008700	0.012770
H4	0.039490	0.037220	0.065320	0.019270	0.005670	0.011510
H5	0.049110	0.031970	0.065410	0.013150	0.003830	0.019720
H6	0.043000	0.039230	0.044480	0.008720	0.008130	0.019090
H7	0.040840	0.034830	0.037940	0.012950	0.008720	0.008930
H8	0.034580	0.046860	0.034060	0.006160	0.002040	0.004410
H9	0.056480	0.056210	0.029560	0.009410	0.004720	0.001510
H10	0.057540	0.059050	0.033690	0.006160	−0.011710	−0.002850
H11	0.036320	0.044790	0.048970	0.002750	−0.009870	0.003210
H12	0.034680	0.043620	0.039920	0.006290	0.001440	0.009820
H13	0.040630	0.041970	0.055870	0.012240	0.013600	0.016590
H14	0.043860	0.058420	0.061580	0.007930	0.023820	0.020050
H15	0.053920	0.056520	0.060680	0.000850	0.018990	0.033100
H16	0.048400	0.038100	0.057230	0.006380	0.004640	0.025830
H17	0.037220	0.035960	0.044240	0.011130	0.008370	0.014020
H18	0.055240	0.045050	0.030660	0.009630	0.000930	0.005080
H19	0.060240	0.041350	0.041490	0.010890	0.005770	−0.009390
H20	0.060260	0.031870	0.061420	0.018100	0.005810	−0.001230
H21	0.047190	0.034200	0.044900	0.015140	0.001310	0.009060
H22	0.042300	0.029640	0.030190	0.010190	0.000880	0.002620
H23	0.031790	0.041580	0.047290	0.007980	−0.002560	0.002130
H24	0.030040	0.049840	0.069600	0.011690	−0.000720	0.007760
H25	0.033060	0.057160	0.068510	0.005500	−0.017520	0.007580
H26	0.047470	0.050340	0.041960	0.002520	−0.015210	0.002650
H27	0.041010	0.049050	0.036310	0.008400	−0.001550	0.004990
H28	0.039940	0.032210	0.037910	0.009060	0.009360	0.011250
H29	0.047510	0.038140	0.037900	0.009310	0.014260	0.002130
H30	0.061200	0.052000	0.031160	0.008100	0.019000	0.012330
H31	0.054540	0.039120	0.040510	0.004820	0.012590	0.020360
H32	0.045840	0.028650	0.036750	0.006520	0.006170	0.006840

Geometric parameters (Å, º)

Fe1—P1	2.1012 (6)	C13—C18	1.3891 (19)
Fe1—P2	2.1190 (6)	C14—C15	1.390 (2)
Fe1—C37	1.7906 (14)	C14—H13	1.068 (19)
Fe1—C38	1.7808 (15)	C15—C16	1.391 (2)
Fe1—H1	1.508 (17)	C15—H14	1.078 (19)
Fe1—H2	1.501 (15)	C16—C17	1.386 (2)
P1—O1	1.6029 (9)	C16—H15	1.116 (18)
P1—O2	1.6146 (10)	C17—C18	1.3944 (19)
P1—O3	1.6253 (9)	C17—H16	1.085 (19)
P2—O4	1.6067 (10)	C18—H17	1.076 (17)
P2—O5	1.5993 (9)	C19—C20	1.3884 (18)
P2—O6	1.6064 (9)	C19—C24	1.3906 (17)
O1—C1	1.3834 (15)	C20—C21	1.390 (2)
O2—C7	1.3937 (14)	C20—H18	1.096 (17)
O3—C13	1.3877 (15)	C21—C22	1.391 (2)
O4—C19	1.3808 (16)	C21—H19	1.074 (18)
O5—C25	1.3952 (14)	C22—C23	1.388 (2)
O6—C31	1.3766 (14)	C22—H20	1.085 (19)
O7—C37	1.1396 (18)	C23—C24	1.393 (2)
O8—C38	1.1433 (17)	C23—H21	1.090 (16)
C1—C2	1.3854 (18)	C24—H22	1.105 (16)
C1—C6	1.3854 (17)	C25—C26	1.382 (2)
C2—C3	1.390 (2)	C25—C30	1.3841 (19)
C2—H3	1.082 (17)	C26—C27	1.389 (2)
C3—C4	1.390 (2)	C26—H23	1.099 (18)
C3—H4	1.107 (18)	C27—C28	1.386 (3)
C4—C5	1.392 (2)	C27—H24	1.085 (19)
C4—H5	1.083 (18)	C28—C29	1.390 (2)
C5—C6	1.391 (2)	C28—H25	1.111 (17)
C5—H6	1.097 (17)	C29—C30	1.3920 (19)
C6—H7	1.090 (17)	C29—H26	1.093 (18)
C7—C8	1.3901 (19)	C30—H27	1.079 (18)
C7—C12	1.3803 (18)	C31—C32	1.392 (2)
C8—C9	1.391 (2)	C31—C36	1.3874 (18)
C8—H8	1.103 (17)	C32—C33	1.3889 (18)
C9—C10	1.393 (2)	C32—H28	1.101 (17)
C9—H9	1.085 (18)	C33—C34	1.388 (2)
C10—C11	1.387 (2)	C33—H29	1.094 (19)
C10—H10	1.089 (16)	C34—C35	1.392 (2)
C11—C12	1.3917 (19)	C34—H30	1.078 (16)
C11—H11	1.102 (17)	C35—C36	1.3917 (19)
C12—H12	1.060 (17)	C35—H31	1.076 (17)
C13—C14	1.3884 (18)	C36—H32	1.098 (18)
P2—Fe1—P1	154.362 (15)	C15—C14—C13	119.55 (14)
C37—Fe1—P1	103.50 (4)	H13—C14—C13	118.0 (9)
C37—Fe1—P2	95.97 (4)	H13—C14—C15	122.5 (10)
C38—Fe1—P1	97.51 (4)	C16—C15—C14	120.66 (14)
C38—Fe1—P2	95.03 (4)	H14—C15—C14	120.8 (11)
C38—Fe1—C37	100.76 (7)	H14—C15—C16	118.6 (11)
H1—Fe1—P1	81.8 (7)	C17—C16—C15	119.14 (13)
H1—Fe1—P2	82.7 (7)	H15—C16—C15	119.3 (11)
H1—Fe1—C37	87.1 (7)	H15—C16—C17	121.5 (11)
H1—Fe1—C38	172.1 (7)	C18—C17—C16	120.92 (14)
H2—Fe1—P1	76.6 (6)	H16—C17—C16	119.5 (10)
H2—Fe1—P2	80.9 (6)	H16—C17—C18	119.6 (10)
H2—Fe1—C37	168.1 (7)	C17—C18—C13	119.15 (13)
H2—Fe1—C38	90.9 (7)	H17—C18—C13	118.9 (9)
H2—Fe1—H1	81.2 (10)	H17—C18—C17	121.9 (9)
O1—P1—Fe1	120.12 (3)	C20—C19—O4	115.07 (11)
O2—P1—Fe1	113.91 (3)	C24—C19—O4	123.88 (11)
O2—P1—O1	98.13 (5)	C24—C19—C20	121.06 (13)
O3—P1—Fe1	121.61 (3)	C21—C20—C19	119.39 (12)
O3—P1—O1	95.80 (5)	H18—C20—C19	118.2 (10)
O3—P1—O2	103.24 (5)	H18—C20—C21	122.4 (10)
O4—P2—Fe1	120.24 (4)	C22—C21—C20	120.40 (13)
O5—P2—Fe1	111.53 (4)	H19—C21—C20	118.0 (11)
O5—P2—O4	99.03 (5)	H19—C21—C22	121.6 (11)
O6—P2—Fe1	123.05 (3)	C23—C22—C21	119.46 (14)
O6—P2—O4	96.63 (5)	H20—C22—C21	119.1 (10)
O6—P2—O5	102.46 (5)	H20—C22—C23	121.4 (10)
C1—O1—P1	126.74 (7)	C24—C23—C22	120.93 (13)
C7—O2—P1	123.61 (8)	H21—C23—C22	120.0 (9)
C13—O3—P1	124.38 (7)	H21—C23—C24	119.1 (9)
C19—O4—P2	127.99 (8)	C23—C24—C19	118.75 (12)
C25—O5—P2	124.88 (8)	H22—C24—C19	123.5 (9)
C31—O6—P2	130.39 (8)	H22—C24—C23	117.7 (9)
C2—C1—O1	119.60 (11)	C26—C25—O5	117.58 (12)
C6—C1—O1	118.67 (11)	C30—C25—O5	120.47 (12)
C6—C1—C2	121.49 (12)	C30—C25—C26	121.71 (12)
C3—C2—C1	119.22 (13)	C27—C26—C25	119.09 (15)
H3—C2—C1	119.7 (9)	H23—C26—C25	118.1 (9)
H3—C2—C3	121.1 (9)	H23—C26—C27	122.8 (9)
C4—C3—C2	120.23 (14)	C28—C27—C26	120.36 (16)
H4—C3—C2	119.7 (10)	H24—C27—C26	118.3 (10)
H4—C3—C4	120.0 (10)	H24—C27—C28	121.3 (10)
C5—C4—C3	119.68 (14)	C29—C28—C27	119.67 (13)
H5—C4—C3	120.4 (10)	H25—C28—C27	120.1 (11)
H5—C4—C5	119.9 (10)	H25—C28—C29	120.2 (11)
C6—C5—C4	120.59 (13)	C30—C29—C28	120.61 (15)
H6—C5—C4	119.6 (10)	H26—C29—C28	119.8 (10)
H6—C5—C6	119.8 (10)	H26—C29—C30	119.5 (10)
C5—C6—C1	118.78 (13)	C29—C30—C25	118.55 (14)
H7—C6—C1	121.2 (9)	H27—C30—C25	121.4 (9)
H7—C6—C5	120.0 (9)	H27—C30—C29	120.1 (9)
C8—C7—O2	117.90 (11)	C32—C31—O6	122.48 (11)
C12—C7—O2	120.40 (11)	C36—C31—O6	116.13 (12)
C12—C7—C8	121.66 (12)	C36—C31—C32	121.34 (12)
C9—C8—C7	118.72 (13)	C33—C32—C31	118.68 (13)
H8—C8—C7	118.6 (9)	H28—C32—C31	121.3 (9)
H8—C8—C9	122.7 (9)	H28—C32—C33	120.0 (9)
C10—C9—C8	120.53 (14)	C34—C33—C32	120.90 (15)
H9—C9—C8	120.3 (9)	H29—C33—C32	118.7 (9)
H9—C9—C10	119.1 (9)	H29—C33—C34	120.4 (9)
C11—C10—C9	119.54 (12)	C35—C34—C33	119.59 (13)
H10—C10—C9	119.3 (10)	H30—C34—C33	119.8 (11)
H10—C10—C11	121.1 (10)	H30—C34—C35	120.5 (11)
C12—C11—C10	120.62 (13)	C36—C35—C34	120.37 (13)
H11—C11—C10	119.7 (9)	H31—C35—C34	119.5 (10)
H11—C11—C12	119.7 (9)	H31—C35—C36	120.1 (10)
C11—C12—C7	118.92 (13)	C35—C36—C31	119.11 (14)
H12—C12—C7	120.1 (9)	H32—C36—C31	121.1 (9)
H12—C12—C11	121.0 (9)	H32—C36—C35	119.8 (9)
C14—C13—O3	116.52 (12)	O7—C37—Fe1	177.59 (15)
C18—C13—O3	122.85 (11)	O8—C38—Fe1	177.26 (12)
C18—C13—C14	120.58 (12)
Fe1—P1—O1—C1	−29.98 (7)	O5—C25—C30—C29	173.85 (12)
Fe1—P1—O2—C7	−157.59 (7)	O6—C31—C32—C33	−178.68 (12)
Fe1—P1—O3—C13	−50.56 (7)	O6—C31—C36—C35	178.58 (10)
Fe1—P2—O4—C19	−79.74 (7)	C1—C2—C3—C4	−0.43 (14)
Fe1—P2—O5—C25	171.80 (8)	C1—C6—C5—C4	0.16 (15)
Fe1—P2—O6—C31	−20.83 (7)	C2—C3—C4—C5	−0.29 (16)
P1—O1—C1—C2	−84.61 (10)	C3—C4—C5—C6	0.43 (16)
P1—O1—C1—C6	100.91 (10)	C7—C8—C9—C10	0.52 (17)
P1—O2—C7—C8	97.67 (11)	C7—C12—C11—C10	0.96 (17)
P1—O2—C7—C12	−84.70 (11)	C8—C9—C10—C11	−0.73 (19)
P1—O3—C13—C14	147.06 (11)	C9—C10—C11—C12	−0.02 (18)
P1—O3—C13—C18	−35.68 (11)	C13—C14—C15—C16	0.43 (16)
P2—O4—C19—C20	−170.55 (11)	C13—C18—C17—C16	0.52 (16)
P2—O4—C19—C24	9.73 (12)	C14—C15—C16—C17	−0.50 (18)
P2—O5—C25—C26	−105.54 (11)	C15—C16—C17—C18	0.03 (17)
P2—O5—C25—C30	79.96 (11)	C19—C20—C21—C22	−0.26 (15)
P2—O6—C31—C32	−43.98 (12)	C19—C24—C23—C22	0.29 (15)
P2—O6—C31—C36	138.61 (11)	C20—C21—C22—C23	−0.43 (16)
O1—C1—C2—C3	−173.28 (11)	C21—C22—C23—C24	0.42 (16)
O1—C1—C6—C5	173.47 (11)	C25—C26—C27—C28	0.47 (18)
O2—C7—C8—C9	178.05 (13)	C25—C30—C29—C28	0.16 (16)
O2—C7—C12—C11	−178.72 (13)	C26—C27—C28—C29	−0.7 (2)
O3—C13—C14—C15	177.46 (12)	C27—C28—C29—C30	0.42 (19)
O3—C13—C18—C17	−177.75 (12)	C31—C32—C33—C34	0.86 (14)
O4—C19—C20—C21	−178.73 (11)	C31—C36—C35—C34	−0.32 (14)
O4—C19—C24—C23	178.70 (12)	C32—C33—C34—C35	−0.07 (15)
O5—C25—C26—C27	−174.32 (13)	C33—C34—C35—C36	−0.20 (15)

Dicarbonyl-cis-dihydrido-trans-bis(triphenylphosphite)iron(II) (QOSZON_IAM_0_HADPs)

Crystal data

C38H32FeO8P2	Z = 2
Mr = 734.47	F(000) = 761.550
Triclinic, P1	Dx = 1.431 Mg m^−3
a = 9.6397 (12) Å	Mo Kα radiation, λ = 0.71073 Å
b = 10.4410 (13) Å	Cell parameters from 5000 reflections
c = 18.381 (2) Å	θ = 3.3–52.1°
α = 102.148 (15)°	µ = 0.59 mm^−1
β = 94.667 (15)°	T = 293 K
γ = 107.402 (14)°	Parallelepiped, colourless
V = 1705.0 (4) Å^3	0.5 × 0.25 × 0.1 mm

Data collection

STOE diffractometer	Rint = 0.034
Detector resolution: (1.60 pixels mm^-1	θmax = 26.1°, θmin = 2.1°
rotation en phi scans	h = −11→11
16806 measured reflections	k = −12→12
6202 independent reflections	l = −22→22
5084 reflections with I ≥ 2u(I)

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.033	Only H-atom coordinates refined
wR(F^2) = 0.083	w = 1/[σ^2(Fo^2) + (0.0391P)^2 + 1.1381P] where P = (Fo^2 + 2Fc^2)/3
S = 1.01	(Δ/σ)max = −0.001
6202 reflections	Δρmax = 0.36 e Å^−3
538 parameters	Δρmin = −0.47 e Å^−3

Special details

Experimental. The crystal was pasted on a glass fiber, by using an oil-coated shock-cooled crystal.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Fe1	0.53171 (3)	0.83646 (3)	0.270680 (16)	0.01936 (9)
P1	0.35102 (5)	0.72598 (6)	0.18546 (3)	0.01903 (12)
P2	0.72491 (5)	1.00378 (6)	0.32210 (3)	0.01900 (12)
O1	0.30701 (16)	0.79721 (15)	0.12199 (8)	0.0246 (3)
O2	0.37117 (15)	0.59236 (15)	0.13057 (8)	0.0225 (3)
O3	0.18553 (15)	0.66731 (16)	0.20456 (8)	0.0238 (3)
O4	0.71956 (16)	1.12311 (16)	0.39192 (8)	0.0245 (3)
O5	0.84479 (15)	0.95206 (15)	0.36170 (8)	0.0234 (3)
O6	0.82087 (16)	1.10524 (16)	0.27688 (8)	0.0248 (3)
O7	0.4085 (2)	0.8192 (2)	0.41016 (10)	0.0547 (6)
O8	0.6792 (2)	0.6270 (2)	0.25557 (11)	0.0413 (4)
C1	0.3280 (2)	0.9378 (2)	0.13025 (11)	0.0201 (4)
C2	0.2250 (2)	0.9929 (3)	0.15915 (12)	0.0267 (5)
C3	0.2391 (3)	1.1291 (3)	0.15970 (14)	0.0352 (6)
C4	0.3545 (3)	1.2081 (3)	0.13212 (15)	0.0361 (6)
C5	0.4574 (3)	1.1512 (3)	0.10394 (14)	0.0324 (5)
C6	0.4453 (2)	1.0154 (2)	0.10283 (13)	0.0260 (5)
C7	0.2932 (2)	0.5315 (2)	0.05719 (11)	0.0218 (4)
C8	0.3624 (3)	0.5674 (3)	−0.00199 (13)	0.0306 (5)
C9	0.2890 (3)	0.5050 (3)	−0.07494 (14)	0.0371 (6)
C10	0.1485 (3)	0.4099 (3)	−0.08772 (13)	0.0352 (6)
C11	0.0823 (3)	0.3759 (3)	−0.02770 (14)	0.0351 (6)
C12	0.1547 (2)	0.4358 (2)	0.04566 (13)	0.0285 (5)
C13	0.1486 (2)	0.5884 (2)	0.25720 (11)	0.0218 (4)
C14	0.0359 (2)	0.6067 (3)	0.29573 (13)	0.0300 (5)
C15	−0.0105 (3)	0.5279 (3)	0.34651 (14)	0.0376 (6)
C16	0.0557 (3)	0.4326 (3)	0.35943 (13)	0.0348 (6)
C17	0.1679 (3)	0.4158 (3)	0.32066 (14)	0.0322 (5)
C18	0.2152 (2)	0.4927 (2)	0.26888 (13)	0.0270 (5)
C19	0.6711 (2)	1.2353 (2)	0.38981 (12)	0.0218 (4)
C20	0.6998 (2)	1.3331 (2)	0.45770 (12)	0.0257 (5)
C21	0.6531 (3)	1.4469 (3)	0.46157 (14)	0.0328 (5)
C22	0.5795 (3)	1.4636 (3)	0.39837 (15)	0.0332 (5)
C23	0.5528 (2)	1.3657 (2)	0.33076 (13)	0.0298 (5)
C24	0.5987 (2)	1.2511 (2)	0.32575 (12)	0.0259 (5)
C25	0.9905 (2)	1.0358 (2)	0.39248 (12)	0.0236 (5)
C26	1.0999 (3)	1.0150 (3)	0.35267 (14)	0.0340 (5)
C27	1.2454 (3)	1.0866 (3)	0.38454 (19)	0.0463 (7)
C28	1.2789 (3)	1.1761 (3)	0.45505 (17)	0.0437 (7)
C29	1.1674 (3)	1.1957 (3)	0.49380 (15)	0.0378 (6)
C30	1.0207 (3)	1.1255 (2)	0.46275 (13)	0.0287 (5)
C31	0.8280 (2)	1.0848 (2)	0.20018 (11)	0.0205 (4)
C32	0.8357 (2)	0.9632 (2)	0.15682 (12)	0.0249 (5)
C33	0.8456 (2)	0.9534 (3)	0.08094 (13)	0.0301 (5)
C34	0.8500 (2)	1.0636 (3)	0.05001 (13)	0.0319 (6)
C35	0.8441 (2)	1.1853 (3)	0.09470 (13)	0.0296 (5)
C36	0.8333 (2)	1.1973 (3)	0.17062 (13)	0.0246 (5)
C37	0.4560 (2)	0.8230 (3)	0.35556 (13)	0.0315 (5)
C38	0.6192 (2)	0.7078 (2)	0.26269 (12)	0.0264 (5)
H	0.4714 (19)	0.9467 (19)	0.2686 (10)	0.000000
Ha	0.5799 (19)	0.8724 (19)	0.2040 (10)	0.000000
H2	0.149 (2)	0.938 (2)	0.1766 (10)	0.000000
H3	0.167 (2)	1.162 (2)	0.1770 (10)	0.000000
H4	0.3636 (19)	1.299 (2)	0.1320 (10)	0.000000
H5	0.532 (2)	1.202 (2)	0.0860 (10)	0.000000
H6	0.511 (2)	0.975 (2)	0.0818 (10)	0.000000
H8	0.458 (2)	0.634 (2)	0.0079 (10)	0.000000
H9	0.3336 (19)	0.526 (2)	−0.1157 (11)	0.000000
H10	0.1010 (19)	0.372 (2)	−0.1382 (11)	0.000000
H11	−0.016 (2)	0.310 (2)	−0.0351 (10)	0.000000
H12	0.113 (2)	0.413 (2)	0.0855 (11)	0.000000
H14	−0.004 (2)	0.671 (2)	0.2861 (10)	0.000000
H15	−0.090 (2)	0.539 (2)	0.3723 (10)	0.000000
H16	0.0229 (19)	0.378 (2)	0.3942 (10)	0.000000
H17	0.209 (2)	0.351 (2)	0.3275 (10)	0.000000
H18	0.288 (2)	0.478 (2)	0.2407 (10)	0.000000
H20	0.7501 (19)	1.3186 (19)	0.4991 (11)	0.000000
H21	0.6732 (19)	1.507 (2)	0.5048 (11)	0.000000
H22	0.550 (2)	1.535 (2)	0.4029 (10)	0.000000
H23	0.5015 (19)	1.3779 (19)	0.2853 (10)	0.000000
H24	0.5821 (19)	1.188 (2)	0.2781 (11)	0.000000
H26	1.0722 (19)	0.952 (2)	0.3056 (11)	0.000000
H27	1.319 (2)	1.072 (2)	0.3589 (10)	0.000000
H28	1.382 (2)	1.224 (2)	0.4776 (10)	0.000000
H29	1.188 (2)	1.257 (2)	0.5416 (11)	0.000000
H30	0.943 (2)	1.137 (2)	0.4883 (10)	0.000000
H32	0.8345 (19)	0.886 (2)	0.1767 (10)	0.000000
H33	0.8520 (19)	0.877 (2)	0.0544 (11)	0.000000
H34	0.8517 (19)	1.0523 (19)	−0.0007 (11)	0.000000
H35	0.8479 (19)	1.262 (2)	0.0755 (10)	0.000000
H36	0.8307 (19)	1.280 (2)	0.2003 (10)	0.000000

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Fe1	0.01774 (15)	0.02026 (17)	0.01795 (14)	0.00270 (11)	0.00091 (10)	0.00595 (12)
P1	0.0177 (2)	0.0180 (3)	0.0200 (2)	0.0032 (2)	0.00059 (19)	0.0067 (2)
P2	0.0193 (2)	0.0193 (3)	0.0165 (2)	0.0035 (2)	0.00158 (18)	0.0048 (2)
O1	0.0298 (8)	0.0179 (8)	0.0223 (7)	0.0033 (6)	−0.0048 (6)	0.0064 (6)
O2	0.0224 (7)	0.0213 (8)	0.0221 (7)	0.0072 (6)	−0.0011 (6)	0.0033 (6)
O3	0.0174 (7)	0.0260 (8)	0.0292 (8)	0.0047 (6)	0.0032 (6)	0.0128 (7)
O4	0.0306 (8)	0.0244 (8)	0.0184 (7)	0.0108 (6)	0.0016 (6)	0.0032 (6)
O5	0.0187 (7)	0.0211 (8)	0.0264 (7)	0.0026 (6)	−0.0032 (6)	0.0054 (6)
O6	0.0278 (8)	0.0224 (8)	0.0177 (7)	−0.0011 (6)	0.0032 (6)	0.0044 (6)
O7	0.0514 (12)	0.0753 (16)	0.0295 (9)	0.0029 (10)	0.0159 (8)	0.0179 (10)
O8	0.0411 (10)	0.0344 (11)	0.0512 (11)	0.0192 (9)	0.0014 (8)	0.0084 (9)
C1	0.0228 (10)	0.0190 (11)	0.0175 (9)	0.0059 (8)	−0.0018 (7)	0.0054 (8)
C2	0.0250 (11)	0.0318 (13)	0.0235 (10)	0.0091 (10)	0.0060 (9)	0.0067 (10)
C3	0.0378 (13)	0.0385 (16)	0.0316 (12)	0.0218 (12)	0.0028 (10)	0.0011 (11)
C4	0.0438 (14)	0.0198 (13)	0.0426 (14)	0.0116 (11)	−0.0087 (11)	0.0072 (11)
C5	0.0267 (11)	0.0261 (13)	0.0438 (13)	0.0022 (10)	0.0017 (10)	0.0181 (11)
C6	0.0214 (10)	0.0294 (13)	0.0302 (11)	0.0092 (9)	0.0053 (9)	0.0120 (10)
C7	0.0236 (10)	0.0173 (11)	0.0235 (10)	0.0090 (8)	−0.0014 (8)	0.0015 (8)
C8	0.0331 (12)	0.0248 (13)	0.0304 (11)	0.0054 (10)	0.0039 (9)	0.0058 (10)
C9	0.0544 (16)	0.0326 (15)	0.0251 (11)	0.0143 (12)	0.0078 (11)	0.0079 (10)
C10	0.0475 (14)	0.0274 (14)	0.0261 (12)	0.0160 (11)	−0.0086 (10)	−0.0031 (10)
C11	0.0279 (12)	0.0277 (14)	0.0401 (13)	0.0054 (10)	−0.0063 (10)	−0.0024 (11)
C12	0.0268 (11)	0.0242 (13)	0.0304 (12)	0.0049 (9)	0.0041 (9)	0.0031 (10)
C13	0.0176 (9)	0.0203 (11)	0.0231 (10)	−0.0004 (8)	0.0003 (8)	0.0065 (9)
C14	0.0261 (11)	0.0296 (14)	0.0356 (12)	0.0104 (10)	0.0066 (9)	0.0085 (11)
C15	0.0283 (12)	0.0471 (17)	0.0359 (13)	0.0064 (11)	0.0144 (10)	0.0122 (12)
C16	0.0336 (12)	0.0347 (14)	0.0293 (12)	−0.0018 (10)	0.0041 (10)	0.0129 (11)
C17	0.0345 (12)	0.0264 (13)	0.0356 (12)	0.0069 (10)	0.0003 (10)	0.0135 (11)
C18	0.0230 (10)	0.0273 (13)	0.0319 (11)	0.0074 (9)	0.0064 (9)	0.0103 (10)
C19	0.0199 (10)	0.0192 (11)	0.0254 (10)	0.0044 (8)	0.0056 (8)	0.0059 (9)
C20	0.0285 (11)	0.0228 (12)	0.0212 (10)	0.0027 (9)	0.0053 (9)	0.0033 (9)
C21	0.0372 (13)	0.0256 (14)	0.0283 (12)	0.0036 (10)	0.0116 (10)	−0.0021 (10)
C22	0.0361 (13)	0.0215 (13)	0.0453 (14)	0.0141 (11)	0.0120 (11)	0.0061 (11)
C23	0.0283 (11)	0.0243 (13)	0.0350 (12)	0.0075 (9)	0.0005 (9)	0.0068 (10)
C24	0.0241 (11)	0.0256 (13)	0.0227 (10)	0.0039 (9)	0.0003 (8)	0.0020 (9)
C25	0.0192 (10)	0.0205 (11)	0.0281 (11)	0.0016 (8)	−0.0022 (8)	0.0087 (9)
C26	0.0294 (12)	0.0339 (15)	0.0364 (13)	0.0080 (10)	0.0052 (10)	0.0068 (11)
C27	0.0230 (12)	0.0478 (18)	0.0716 (19)	0.0094 (12)	0.0140 (13)	0.0231 (16)
C28	0.0223 (12)	0.0355 (15)	0.0656 (18)	−0.0023 (11)	−0.0080 (12)	0.0189 (14)
C29	0.0383 (14)	0.0251 (13)	0.0378 (14)	−0.0022 (11)	−0.0127 (11)	0.0072 (11)
C30	0.0274 (11)	0.0266 (13)	0.0303 (11)	0.0060 (10)	0.0001 (9)	0.0090 (10)
C31	0.0157 (9)	0.0249 (12)	0.0181 (9)	0.0032 (8)	0.0010 (7)	0.0053 (8)
C32	0.0225 (10)	0.0264 (13)	0.0282 (11)	0.0086 (9)	0.0065 (8)	0.0098 (10)
C33	0.0299 (12)	0.0315 (14)	0.0268 (11)	0.0122 (10)	0.0066 (9)	−0.0012 (10)
C34	0.0265 (11)	0.0495 (17)	0.0199 (11)	0.0106 (10)	0.0045 (8)	0.0112 (11)
C35	0.0246 (11)	0.0377 (15)	0.0317 (12)	0.0086 (10)	0.0058 (9)	0.0210 (11)
C36	0.0230 (10)	0.0212 (12)	0.0292 (11)	0.0054 (9)	0.0047 (8)	0.0075 (10)
C37	0.0254 (11)	0.0344 (14)	0.0290 (12)	0.0016 (10)	−0.0013 (9)	0.0099 (10)
C38	0.0235 (10)	0.0252 (13)	0.0255 (11)	0.0016 (9)	−0.0006 (8)	0.0065 (9)
H	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
Ha	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H3	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H4	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H5	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H6	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H8	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H9	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H10	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H11	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H12	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H14	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H15	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H16	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H17	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H18	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H20	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H21	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H22	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H23	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H24	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H26	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H27	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H28	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H29	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H30	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H32	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H33	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H34	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H35	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H36	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000

Geometric parameters (Å, º)

Fe1—P1	2.1004 (7)	C13—C18	1.381 (3)
Fe1—P2	2.1181 (8)	C14—C15	1.386 (4)
Fe1—C37	1.789 (2)	C14—H14	0.91 (2)
Fe1—C38	1.776 (3)	C15—C16	1.380 (4)
Fe1—H	1.442 (18)	C15—H15	0.954 (19)
Fe1—Ha	1.428 (17)	C16—C17	1.377 (4)
P1—O1	1.6024 (14)	C16—H16	0.953 (19)
P1—O2	1.6135 (17)	C17—C18	1.390 (3)
P1—O3	1.6251 (15)	C17—H17	0.90 (2)
P2—O4	1.6058 (16)	C18—H18	0.930 (19)
P2—O5	1.5996 (15)	C19—C20	1.384 (3)
P2—O6	1.6056 (15)	C19—C24	1.385 (3)
O1—C1	1.394 (3)	C20—C21	1.381 (4)
O2—C7	1.406 (2)	C20—H20	0.933 (18)
O3—C13	1.399 (2)	C21—C22	1.382 (4)
O4—C19	1.391 (3)	C21—H21	0.87 (2)
O5—C25	1.409 (2)	C22—C23	1.382 (4)
O6—C31	1.391 (2)	C22—H22	0.86 (2)
O7—C37	1.140 (3)	C23—C24	1.383 (3)
O8—C38	1.149 (3)	C23—H23	0.987 (18)
C1—C2	1.378 (3)	C24—H24	0.950 (19)
C1—C6	1.381 (3)	C25—C26	1.375 (3)
C2—C3	1.386 (4)	C25—C30	1.377 (3)
C2—H2	0.914 (19)	C26—C27	1.387 (4)
C3—C4	1.376 (4)	C26—H26	0.93 (2)
C3—H3	0.92 (2)	C27—C28	1.378 (4)
C4—C5	1.384 (4)	C27—H27	0.915 (19)
C4—H4	0.92 (2)	C28—C29	1.379 (4)
C5—C6	1.383 (3)	C28—H28	0.982 (18)
C5—H5	0.891 (19)	C29—C30	1.391 (3)
C6—H6	0.92 (2)	C29—H29	0.936 (19)
C7—C8	1.382 (3)	C30—H30	0.937 (19)
C7—C12	1.375 (3)	C31—C32	1.376 (3)
C8—C9	1.388 (3)	C31—C36	1.384 (3)
C8—H8	0.947 (18)	C32—C33	1.390 (3)
C9—C10	1.386 (4)	C32—H32	0.952 (19)
C9—H9	0.928 (19)	C33—C34	1.379 (4)
C10—C11	1.376 (4)	C33—H33	0.87 (2)
C10—H10	0.947 (18)	C34—C35	1.380 (4)
C11—C12	1.388 (3)	C34—H34	0.916 (19)
C11—H11	0.974 (18)	C35—C36	1.390 (3)
C12—H12	0.905 (19)	C35—H35	0.93 (2)
C13—C14	1.382 (3)	C36—H36	0.93 (2)
P2—Fe1—P1	154.35 (2)	C15—C14—C13	119.4 (2)
C37—Fe1—P1	103.47 (7)	H14—C14—C13	117.2 (12)
C37—Fe1—P2	96.00 (7)	H14—C14—C15	123.4 (12)
C38—Fe1—P1	97.54 (7)	C16—C15—C14	120.7 (2)
C38—Fe1—P2	95.01 (7)	H15—C15—C14	119.5 (12)
C38—Fe1—C37	100.74 (11)	H15—C15—C16	119.8 (11)
H—Fe1—P1	81.7 (7)	C17—C16—C15	119.2 (2)
H—Fe1—P2	82.7 (7)	H16—C16—C15	120.3 (11)
H—Fe1—C37	87.3 (7)	H16—C16—C17	120.5 (11)
H—Fe1—C38	171.8 (7)	C18—C17—C16	121.2 (2)
Ha—Fe1—P1	75.6 (7)	H17—C17—C16	119.6 (12)
Ha—Fe1—P2	81.7 (7)	H17—C17—C18	119.2 (12)
Ha—Fe1—C37	167.3 (7)	C17—C18—C13	118.8 (2)
Ha—Fe1—C38	91.9 (7)	H18—C18—C13	119.8 (12)
Ha—Fe1—H	80.0 (10)	H18—C18—C17	121.3 (12)
O1—P1—Fe1	120.18 (6)	C20—C19—O4	114.98 (18)
O2—P1—Fe1	113.82 (5)	C24—C19—O4	123.99 (19)
O2—P1—O1	98.09 (8)	C24—C19—C20	121.0 (2)
O3—P1—Fe1	121.74 (6)	C21—C20—C19	119.2 (2)
O3—P1—O1	95.64 (8)	H20—C20—C19	117.9 (12)
O3—P1—O2	103.30 (8)	H20—C20—C21	122.9 (12)
O4—P2—Fe1	120.31 (6)	C22—C21—C20	120.5 (2)
O5—P2—Fe1	111.37 (6)	H21—C21—C20	117.1 (13)
O5—P2—O4	98.95 (8)	H21—C21—C22	122.3 (13)
O6—P2—Fe1	123.24 (6)	C23—C22—C21	119.6 (2)
O6—P2—O4	96.49 (8)	H22—C22—C21	118.2 (12)
O6—P2—O5	102.55 (8)	H22—C22—C23	122.2 (12)
C1—O1—P1	126.59 (12)	C24—C23—C22	120.7 (2)
C7—O2—P1	123.56 (13)	H23—C23—C22	119.9 (11)
C13—O3—P1	124.12 (12)	H23—C23—C24	119.4 (11)
C19—O4—P2	127.76 (13)	C23—C24—C19	118.9 (2)
C25—O5—P2	124.65 (13)	H24—C24—C19	122.4 (12)
C31—O6—P2	129.94 (13)	H24—C24—C23	118.7 (11)
C2—C1—O1	119.53 (19)	C26—C25—O5	117.3 (2)
C6—C1—O1	118.57 (19)	C30—C25—O5	120.3 (2)
C6—C1—C2	121.6 (2)	C30—C25—C26	122.2 (2)
C3—C2—C1	118.9 (2)	C27—C26—C25	118.8 (2)
H2—C2—C1	118.7 (12)	H26—C26—C25	118.0 (11)
H2—C2—C3	122.4 (12)	H26—C26—C27	123.2 (11)
C4—C3—C2	120.5 (2)	C28—C27—C26	120.3 (3)
H3—C3—C2	117.1 (12)	H27—C27—C26	119.4 (12)
H3—C3—C4	122.4 (12)	H27—C27—C28	120.2 (12)
C5—C4—C3	119.7 (2)	C29—C28—C27	119.9 (2)
H4—C4—C3	120.7 (12)	H28—C28—C27	119.4 (11)
H4—C4—C5	119.6 (12)	H28—C28—C29	120.7 (11)
C6—C5—C4	120.7 (2)	C30—C29—C28	120.8 (2)
H5—C5—C4	119.9 (12)	H29—C29—C28	121.3 (11)
H5—C5—C6	119.4 (13)	H29—C29—C30	117.9 (11)
C5—C6—C1	118.5 (2)	C29—C30—C25	118.1 (2)
H6—C6—C1	120.1 (12)	H30—C30—C25	119.9 (11)
H6—C6—C5	121.3 (12)	H30—C30—C29	122.0 (11)
C8—C7—O2	117.80 (18)	C32—C31—O6	122.58 (19)
C12—C7—O2	120.26 (19)	C36—C31—O6	115.6 (2)
C12—C7—C8	121.9 (2)	C36—C31—C32	121.8 (2)
C9—C8—C7	118.6 (2)	C33—C32—C31	118.5 (2)
H8—C8—C7	119.7 (11)	H32—C32—C31	122.7 (12)
H8—C8—C9	121.7 (11)	H32—C32—C33	118.9 (12)
C10—C9—C8	120.4 (2)	C34—C33—C32	120.8 (2)
H9—C9—C8	120.3 (11)	H33—C33—C32	117.5 (12)
H9—C9—C10	119.3 (11)	H33—C33—C34	121.6 (12)
C11—C10—C9	119.7 (2)	C35—C34—C33	119.8 (2)
H10—C10—C9	117.8 (11)	H34—C34—C33	118.6 (12)
H10—C10—C11	122.4 (11)	H34—C34—C35	121.5 (12)
C12—C11—C10	120.7 (2)	C36—C35—C34	120.4 (2)
H11—C11—C10	121.4 (10)	H35—C35—C34	121.7 (12)
H11—C11—C12	117.9 (11)	H35—C35—C36	117.9 (12)
C11—C12—C7	118.6 (2)	C35—C36—C31	118.7 (2)
H12—C12—C7	119.8 (11)	H36—C36—C31	121.5 (11)
H12—C12—C11	121.6 (11)	H36—C36—C35	119.9 (11)
C14—C13—O3	116.3 (2)	O7—C37—Fe1	177.6 (3)
C18—C13—O3	122.91 (19)	O8—C38—Fe1	177.2 (2)
C18—C13—C14	120.8 (2)
Fe1—P1—O1—C1	−30.08 (12)	O5—C25—C30—C29	173.7 (2)
Fe1—P1—O2—C7	−157.61 (12)	O6—C31—C32—C33	−178.66 (19)
Fe1—P1—O3—C13	−50.76 (12)	O6—C31—C36—C35	178.46 (17)
Fe1—P2—O4—C19	−79.80 (11)	C1—C2—C3—C4	−0.3 (2)
Fe1—P2—O5—C25	171.86 (13)	C1—C6—C5—C4	0.2 (2)
Fe1—P2—O6—C31	−21.16 (12)	C2—C3—C4—C5	−0.3 (3)
P1—O1—C1—C2	−84.67 (18)	C3—C4—C5—C6	0.3 (3)
P1—O1—C1—C6	101.06 (17)	C7—C8—C9—C10	0.8 (3)
P1—O2—C7—C8	97.58 (18)	C7—C12—C11—C10	1.0 (3)
P1—O2—C7—C12	−84.61 (18)	C8—C9—C10—C11	−0.8 (3)
P1—O3—C13—C14	147.02 (18)	C9—C10—C11—C12	−0.1 (3)
P1—O3—C13—C18	−35.51 (19)	C13—C14—C15—C16	0.7 (3)
P2—O4—C19—C20	−170.58 (18)	C13—C18—C17—C16	0.6 (3)
P2—O4—C19—C24	9.69 (19)	C14—C15—C16—C17	−0.6 (3)
P2—O5—C25—C26	−105.59 (19)	C15—C16—C17—C18	−0.1 (3)
P2—O5—C25—C30	79.95 (18)	C19—C20—C21—C22	−0.5 (3)
P2—O6—C31—C32	−43.8 (2)	C19—C24—C23—C22	0.4 (3)
P2—O6—C31—C36	138.84 (19)	C20—C21—C22—C23	−0.2 (3)
O1—C1—C2—C3	−173.28 (18)	C21—C22—C23—C24	0.2 (3)
O1—C1—C6—C5	173.38 (18)	C25—C26—C27—C28	0.5 (3)
O2—C7—C8—C9	178.0 (2)	C25—C30—C29—C28	0.2 (3)
O2—C7—C12—C11	−178.8 (2)	C26—C27—C28—C29	−0.7 (3)
O3—C13—C14—C15	177.42 (19)	C27—C28—C29—C30	0.3 (3)
O3—C13—C18—C17	−177.9 (2)	C31—C32—C33—C34	1.0 (2)
O4—C19—C20—C21	−178.65 (18)	C31—C36—C35—C34	−0.2 (2)
O4—C19—C24—C23	178.7 (2)	C32—C33—C34—C35	−0.2 (3)
O5—C25—C26—C27	−174.2 (2)	C33—C34—C35—C36	−0.3 (3)

(QOSZON_IAM_NoMoRe)

Crystal data

C38H32FeO8P2	Z = 2
Mr = 734.47	F(000) = 761.455
Triclinic, P1	Dx = 1.431 Mg m^−3
a = 9.6397 (12) Å	Mo Kα radiation, λ = 0.71073 Å
b = 10.4410 (13) Å	Cell parameters from 5000 reflections
c = 18.381 (2) Å	θ = 3.3–52.1°
α = 102.148 (15)°	µ = 0.59 mm^−1
β = 94.667 (15)°	T = 293 K
γ = 107.402 (14)°	Parallelepiped, colourless
V = 1705.0 (4) Å^3	0.5 × 0.25 × 0.1 mm

Data collection

STOE diffractometer	Rint = 0.034
rotation en phi scans	θmax = 26.1°, θmin = 2.1°
16806 measured reflections	h = −11→11
6202 independent reflections	k = −12→12
5084 reflections with I ≥ 2u(I)	l = −22→22

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.027	Only H-atom coordinates refined
wR(F^2) = 0.071	w = 1/[σ^2(Fo^2) + (0.0387P)^2 + 0.3279P] where P = (Fo^2 + 2Fc^2)/3
S = 1.01	(Δ/σ)max = 0.001
6202 reflections	Δρmax = 0.35 e Å^−3
538 parameters	Δρmin = −0.35 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Fe1	0.53170 (3)	0.83647 (3)	0.270683 (13)	0.01977 (8)
P1	0.35104 (4)	0.72598 (5)	0.18545 (2)	0.01946 (10)
P2	0.72486 (4)	1.00381 (5)	0.32211 (2)	0.01934 (10)
O1	0.30700 (13)	0.79717 (13)	0.12198 (7)	0.0249 (3)
O2	0.37128 (13)	0.59228 (13)	0.13061 (6)	0.0230 (3)
O3	0.18561 (12)	0.66731 (13)	0.20456 (7)	0.0242 (3)
O4	0.71942 (13)	1.12304 (14)	0.39192 (6)	0.0250 (3)
O5	0.84476 (13)	0.95203 (13)	0.36170 (7)	0.0240 (3)
O6	0.82076 (13)	1.10512 (13)	0.27691 (6)	0.0250 (3)
O7	0.40858 (18)	0.8193 (2)	0.41021 (8)	0.0552 (5)
O8	0.67906 (16)	0.62690 (17)	0.25554 (9)	0.0417 (4)
C1	0.32784 (18)	0.93779 (18)	0.13018 (9)	0.0207 (4)
C2	0.2250 (2)	0.9926 (2)	0.15919 (10)	0.0277 (4)
C3	0.2386 (2)	1.1292 (2)	0.15974 (11)	0.0360 (5)
C4	0.3546 (2)	1.2085 (2)	0.13217 (12)	0.0366 (5)
C5	0.4577 (2)	1.1513 (2)	0.10379 (12)	0.0331 (5)
C6	0.4454 (2)	1.0153 (2)	0.10286 (10)	0.0267 (4)
C7	0.29318 (18)	0.53138 (19)	0.05713 (10)	0.0221 (4)
C8	0.3626 (2)	0.5674 (2)	−0.00199 (11)	0.0313 (4)
C9	0.2891 (3)	0.5052 (2)	−0.07506 (11)	0.0380 (5)
C10	0.1484 (2)	0.4100 (2)	−0.08774 (11)	0.0357 (5)
C11	0.0822 (2)	0.3758 (2)	−0.02778 (12)	0.0356 (5)
C12	0.1547 (2)	0.4355 (2)	0.04583 (11)	0.0293 (4)
C13	0.14860 (18)	0.58850 (19)	0.25725 (9)	0.0220 (4)
C14	0.0355 (2)	0.6067 (2)	0.29558 (11)	0.0305 (4)
C15	−0.0107 (2)	0.5279 (2)	0.34652 (12)	0.0376 (5)
C16	0.0558 (2)	0.4327 (2)	0.35948 (11)	0.0350 (5)
C17	0.1681 (2)	0.4154 (2)	0.32056 (11)	0.0327 (5)
C18	0.2154 (2)	0.4929 (2)	0.26887 (11)	0.0275 (4)
C19	0.67118 (18)	1.23530 (19)	0.38982 (10)	0.0220 (4)
C20	0.6997 (2)	1.3332 (2)	0.45776 (10)	0.0264 (4)
C21	0.6533 (2)	1.4471 (2)	0.46172 (11)	0.0329 (4)
C22	0.5794 (2)	1.4640 (2)	0.39847 (12)	0.0340 (4)
C23	0.5528 (2)	1.3657 (2)	0.33071 (11)	0.0307 (4)
C24	0.59880 (19)	1.2510 (2)	0.32567 (10)	0.0262 (4)
C25	0.99051 (18)	1.03597 (19)	0.39252 (10)	0.0239 (4)
C26	1.0998 (2)	1.0149 (2)	0.35257 (12)	0.0342 (5)
C27	1.2456 (2)	1.0866 (3)	0.38449 (15)	0.0460 (6)
C28	1.2787 (2)	1.1761 (2)	0.45511 (15)	0.0440 (6)
C29	1.1674 (2)	1.1959 (2)	0.49395 (13)	0.0381 (5)
C30	1.0206 (2)	1.1253 (2)	0.46261 (11)	0.0292 (4)
C31	0.82817 (17)	1.08486 (19)	0.20017 (9)	0.0208 (4)
C32	0.83570 (19)	0.9631 (2)	0.15686 (10)	0.0253 (4)
C33	0.8458 (2)	0.9529 (2)	0.08080 (11)	0.0306 (4)
C34	0.8499 (2)	1.0638 (2)	0.05000 (11)	0.0323 (5)
C35	0.8441 (2)	1.1855 (2)	0.09464 (11)	0.0300 (4)
C36	0.83314 (19)	1.1977 (2)	0.17078 (10)	0.0256 (4)
C37	0.4560 (2)	0.8231 (2)	0.35548 (11)	0.0318 (5)
C38	0.61911 (19)	0.7077 (2)	0.26265 (10)	0.0269 (4)
H1	0.471 (3)	0.946 (2)	0.2678 (13)	0.045061
H2	0.578 (2)	0.871 (3)	0.2038 (12)	0.045787
H3	0.144 (3)	0.933 (3)	0.1776 (14)	0.053059
H4	0.163 (3)	1.166 (3)	0.1787 (15)	0.061152
H5	0.364 (3)	1.305 (3)	0.1321 (16)	0.058949
H6	0.538 (3)	1.205 (3)	0.0863 (17)	0.061456
H7	0.513 (3)	0.973 (3)	0.0799 (16)	0.052226
H8	0.461 (3)	0.633 (3)	0.0081 (13)	0.046232
H9	0.337 (3)	0.528 (3)	−0.1188 (14)	0.059017
H10	0.101 (3)	0.374 (3)	−0.1379 (15)	0.067339
H11	−0.019 (3)	0.308 (3)	−0.0357 (15)	0.065807
H12	0.110 (3)	0.409 (3)	0.0875 (14)	0.053730
H13	−0.005 (3)	0.676 (3)	0.2865 (15)	0.052450
H14	−0.091 (3)	0.541 (3)	0.3736 (15)	0.063191
H15	0.025 (3)	0.378 (3)	0.3952 (15)	0.062925
H16	0.213 (3)	0.349 (3)	0.3285 (15)	0.057289
H17	0.289 (3)	0.476 (3)	0.2395 (15)	0.049260
H18	0.754 (3)	1.319 (3)	0.5008 (13)	0.048171
H19	0.673 (3)	1.511 (3)	0.5084 (14)	0.055836
H20	0.548 (3)	1.539 (3)	0.4020 (15)	0.056627
H21	0.498 (3)	1.376 (3)	0.2850 (15)	0.058423
H22	0.582 (3)	1.187 (3)	0.2773 (14)	0.051213
H23	1.074 (3)	0.950 (3)	0.3052 (16)	0.062344
H24	1.322 (3)	1.069 (3)	0.3572 (19)	0.078902
H25	1.386 (3)	1.227 (3)	0.4791 (18)	0.073811
H26	1.188 (3)	1.258 (3)	0.5435 (15)	0.062575
H27	0.942 (3)	1.136 (3)	0.4888 (13)	0.045956
H28	0.835 (3)	0.882 (3)	0.1783 (14)	0.046353
H29	0.851 (3)	0.869 (3)	0.0527 (14)	0.057435
H30	0.856 (3)	1.054 (3)	−0.0029 (14)	0.059463
H31	0.850 (3)	1.267 (3)	0.0759 (14)	0.054601
H32	0.829 (3)	1.283 (3)	0.2011 (14)	0.048066

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Fe1	0.01818 (12)	0.02069 (14)	0.01835 (12)	0.00283 (9)	0.00105 (9)	0.00613 (10)
P1	0.0180 (2)	0.0184 (2)	0.0206 (2)	0.00321 (17)	0.00067 (16)	0.00674 (18)
P2	0.0196 (2)	0.0196 (2)	0.0168 (2)	0.00361 (17)	0.00163 (15)	0.00471 (17)
O1	0.0300 (6)	0.0185 (7)	0.0224 (6)	0.0036 (5)	−0.0048 (5)	0.0064 (5)
O2	0.0232 (6)	0.0217 (7)	0.0224 (6)	0.0074 (5)	−0.0013 (5)	0.0034 (5)
O3	0.0178 (6)	0.0265 (7)	0.0297 (6)	0.0050 (5)	0.0034 (5)	0.0131 (6)
O4	0.0311 (7)	0.0253 (7)	0.0187 (6)	0.0110 (5)	0.0017 (5)	0.0035 (5)
O5	0.0194 (6)	0.0217 (7)	0.0268 (6)	0.0027 (5)	−0.0031 (5)	0.0058 (5)
O6	0.0277 (6)	0.0231 (7)	0.0181 (6)	−0.0005 (5)	0.0033 (5)	0.0046 (5)
O7	0.0521 (10)	0.0759 (13)	0.0296 (8)	0.0028 (9)	0.0161 (7)	0.0182 (8)
O8	0.0424 (8)	0.0346 (9)	0.0506 (9)	0.0193 (7)	0.0013 (7)	0.0086 (7)
C1	0.0234 (8)	0.0201 (9)	0.0180 (7)	0.0062 (7)	−0.0013 (6)	0.0062 (7)
C2	0.0264 (9)	0.0335 (11)	0.0233 (9)	0.0100 (8)	0.0048 (7)	0.0061 (8)
C3	0.0398 (11)	0.0383 (13)	0.0314 (10)	0.0213 (10)	0.0015 (8)	0.0009 (9)
C4	0.0435 (12)	0.0235 (11)	0.0409 (11)	0.0120 (9)	−0.0082 (9)	0.0075 (9)
C5	0.0278 (9)	0.0269 (11)	0.0434 (11)	0.0026 (8)	0.0005 (8)	0.0171 (9)
C6	0.0227 (9)	0.0295 (11)	0.0303 (9)	0.0086 (8)	0.0039 (7)	0.0124 (8)
C7	0.0226 (8)	0.0184 (9)	0.0243 (8)	0.0085 (7)	−0.0014 (7)	0.0020 (7)
C8	0.0351 (10)	0.0258 (11)	0.0299 (9)	0.0064 (9)	0.0043 (8)	0.0060 (8)
C9	0.0553 (13)	0.0324 (12)	0.0265 (10)	0.0149 (10)	0.0059 (9)	0.0067 (9)
C10	0.0478 (12)	0.0280 (11)	0.0272 (10)	0.0163 (9)	−0.0081 (9)	−0.0027 (9)
C11	0.0296 (10)	0.0287 (12)	0.0392 (11)	0.0061 (9)	−0.0066 (8)	−0.0023 (9)
C12	0.0270 (9)	0.0242 (11)	0.0323 (10)	0.0053 (8)	0.0033 (8)	0.0024 (8)
C13	0.0181 (8)	0.0198 (9)	0.0240 (8)	0.0000 (7)	0.0010 (6)	0.0063 (7)
C14	0.0257 (9)	0.0316 (12)	0.0346 (10)	0.0094 (8)	0.0064 (8)	0.0083 (9)
C15	0.0301 (10)	0.0448 (14)	0.0367 (11)	0.0070 (9)	0.0140 (8)	0.0119 (10)
C16	0.0334 (10)	0.0348 (12)	0.0301 (10)	−0.0012 (9)	0.0042 (8)	0.0118 (9)
C17	0.0334 (10)	0.0280 (11)	0.0357 (10)	0.0057 (8)	0.0009 (8)	0.0134 (9)
C18	0.0242 (9)	0.0266 (11)	0.0326 (9)	0.0072 (8)	0.0057 (7)	0.0101 (8)
C19	0.0198 (8)	0.0201 (10)	0.0254 (8)	0.0042 (7)	0.0061 (6)	0.0060 (7)
C20	0.0281 (9)	0.0235 (10)	0.0229 (8)	0.0023 (8)	0.0065 (7)	0.0039 (7)
C21	0.0367 (10)	0.0254 (11)	0.0308 (10)	0.0046 (8)	0.0118 (8)	−0.0001 (8)
C22	0.0359 (11)	0.0236 (11)	0.0437 (11)	0.0115 (9)	0.0117 (9)	0.0060 (9)
C23	0.0288 (9)	0.0251 (11)	0.0364 (10)	0.0072 (8)	0.0008 (8)	0.0078 (9)
C24	0.0246 (9)	0.0254 (11)	0.0241 (9)	0.0044 (8)	0.0003 (7)	0.0029 (8)
C25	0.0198 (8)	0.0212 (10)	0.0280 (9)	0.0018 (7)	−0.0017 (7)	0.0092 (8)
C26	0.0286 (10)	0.0337 (12)	0.0395 (11)	0.0094 (9)	0.0064 (8)	0.0079 (9)
C27	0.0250 (10)	0.0454 (15)	0.0706 (16)	0.0096 (10)	0.0119 (10)	0.0215 (13)
C28	0.0235 (10)	0.0351 (13)	0.0665 (15)	−0.0018 (9)	−0.0071 (10)	0.0194 (12)
C29	0.0364 (11)	0.0267 (11)	0.0398 (11)	−0.0017 (9)	−0.0125 (9)	0.0082 (9)
C30	0.0284 (9)	0.0256 (11)	0.0309 (9)	0.0054 (8)	−0.0008 (8)	0.0085 (8)
C31	0.0157 (7)	0.0254 (10)	0.0188 (8)	0.0035 (7)	0.0011 (6)	0.0055 (7)
C32	0.0228 (9)	0.0278 (11)	0.0270 (9)	0.0090 (7)	0.0061 (7)	0.0084 (8)
C33	0.0288 (10)	0.0352 (12)	0.0264 (9)	0.0114 (8)	0.0060 (7)	0.0022 (9)
C34	0.0268 (9)	0.0490 (14)	0.0219 (9)	0.0111 (9)	0.0050 (7)	0.0112 (9)
C35	0.0244 (9)	0.0384 (12)	0.0318 (10)	0.0088 (8)	0.0056 (7)	0.0199 (9)
C36	0.0226 (8)	0.0242 (10)	0.0292 (9)	0.0043 (7)	0.0042 (7)	0.0098 (8)
C37	0.0263 (9)	0.0348 (12)	0.0286 (10)	0.0018 (8)	−0.0010 (8)	0.0093 (9)
C38	0.0243 (9)	0.0257 (11)	0.0257 (9)	0.0019 (8)	−0.0007 (7)	0.0065 (8)
H1	0.051000	0.034000	0.051000	0.016000	0.000000	0.012000
H2	0.040000	0.064000	0.032000	0.012000	0.011000	0.014000
H3	0.051000	0.053000	0.058000	0.015000	0.028000	0.015000
H4	0.080000	0.044000	0.067000	0.032000	0.023000	0.008000
H5	0.065000	0.031000	0.076000	0.006000	0.000000	0.021000
H6	0.035000	0.058000	0.099000	0.008000	0.018000	0.043000
H7	0.042000	0.048000	0.080000	0.024000	0.021000	0.026000
H8	0.033000	0.052000	0.049000	0.007000	0.010000	0.011000
H9	0.077000	0.065000	0.034000	0.018000	0.020000	0.013000
H10	0.081000	0.071000	0.034000	0.015000	−0.020000	0.004000
H11	0.033000	0.080000	0.064000	0.002000	−0.013000	0.006000
H12	0.037000	0.070000	0.045000	0.004000	0.012000	0.012000
H13	0.063000	0.044000	0.060000	0.026000	0.022000	0.016000
H14	0.064000	0.071000	0.060000	0.024000	0.035000	0.015000
H15	0.063000	0.072000	0.053000	0.006000	0.022000	0.032000
H16	0.065000	0.052000	0.066000	0.020000	0.012000	0.036000
H17	0.049000	0.051000	0.063000	0.027000	0.021000	0.026000
H18	0.066000	0.045000	0.030000	0.015000	0.000000	0.009000
H19	0.081000	0.035000	0.039000	0.009000	0.009000	−0.003000
H20	0.076000	0.030000	0.064000	0.018000	0.010000	0.011000
H21	0.078000	0.046000	0.051000	0.022000	−0.012000	0.017000
H22	0.074000	0.037000	0.034000	0.017000	−0.013000	0.000000
H23	0.054000	0.064000	0.057000	0.020000	0.009000	−0.012000
H24	0.044000	0.076000	0.121000	0.031000	0.025000	0.012000
H25	0.030000	0.078000	0.107000	0.008000	−0.013000	0.032000
H26	0.054000	0.063000	0.048000	−0.004000	−0.016000	0.008000
H27	0.046000	0.050000	0.038000	0.014000	0.009000	0.004000
H28	0.061000	0.032000	0.048000	0.012000	0.015000	0.016000
H29	0.072000	0.047000	0.044000	0.018000	0.010000	−0.007000
H30	0.072000	0.086000	0.027000	0.031000	0.016000	0.017000
H31	0.064000	0.061000	0.053000	0.021000	0.020000	0.039000
H32	0.063000	0.031000	0.047000	0.009000	0.011000	0.011000

Geometric parameters (Å, º)

Fe1—P1	2.1004 (7)	C13—C18	1.382 (3)
Fe1—P2	2.1180 (7)	C14—C15	1.388 (3)
Fe1—C37	1.788 (2)	C14—H13	0.96 (3)
Fe1—C38	1.776 (2)	C15—C16	1.382 (3)
Fe1—H1	1.44 (2)	C15—H14	0.98 (3)
Fe1—H2	1.42 (2)	C16—C17	1.381 (3)
P1—O1	1.6022 (12)	C16—H15	0.97 (3)
P1—O2	1.6141 (14)	C17—C18	1.393 (3)
P1—O3	1.6245 (12)	C17—H16	0.95 (3)
P2—O4	1.6053 (14)	C18—H17	0.96 (3)
P2—O5	1.6001 (13)	C19—C20	1.385 (3)
P2—O6	1.6044 (12)	C19—C24	1.386 (2)
O1—C1	1.394 (2)	C20—C21	1.382 (3)
O2—C7	1.408 (2)	C20—H18	0.97 (2)
O3—C13	1.399 (2)	C21—C22	1.384 (3)
O4—C19	1.391 (2)	C21—H19	0.93 (3)
O5—C25	1.410 (2)	C22—C23	1.387 (3)
O6—C31	1.393 (2)	C22—H20	0.92 (3)
O7—C37	1.142 (2)	C23—C24	1.385 (3)
O8—C38	1.149 (2)	C23—H21	1.00 (2)
C1—C2	1.376 (3)	C24—H22	0.96 (2)
C1—C6	1.381 (2)	C25—C26	1.376 (3)
C2—C3	1.390 (3)	C25—C30	1.373 (3)
C2—H3	0.98 (3)	C26—C27	1.390 (3)
C3—C4	1.382 (3)	C26—H23	0.95 (3)
C3—H4	0.97 (3)	C27—C28	1.379 (4)
C4—C5	1.388 (3)	C27—H24	0.96 (3)
C4—H5	0.99 (3)	C28—C29	1.378 (4)
C5—C6	1.386 (3)	C28—H25	1.02 (2)
C5—H6	0.93 (3)	C29—C30	1.394 (3)
C6—H7	0.97 (3)	C29—H26	0.97 (3)
C7—C8	1.382 (3)	C30—H27	0.95 (2)
C7—C12	1.377 (3)	C31—C32	1.376 (3)
C8—C9	1.389 (3)	C31—C36	1.386 (3)
C8—H8	0.97 (2)	C32—C33	1.393 (3)
C9—C10	1.388 (3)	C32—H28	1.00 (2)
C9—H9	1.00 (3)	C33—C34	1.385 (3)
C10—C11	1.376 (3)	C33—H29	0.94 (3)
C10—H10	0.94 (2)	C34—C35	1.379 (3)
C11—C12	1.392 (3)	C34—H30	0.96 (2)
C11—H11	0.99 (3)	C35—C36	1.394 (3)
C12—H12	0.96 (3)	C35—H31	0.97 (3)
C13—C14	1.383 (3)	C36—H32	0.96 (3)
P2—Fe1—P1	154.35 (2)	C15—C14—C13	119.3 (2)
C37—Fe1—P1	103.46 (6)	H13—C14—C13	117.7 (16)
C37—Fe1—P2	96.00 (6)	H13—C14—C15	123.0 (16)
C38—Fe1—P1	97.51 (6)	C16—C15—C14	120.7 (2)
C38—Fe1—P2	95.06 (6)	H14—C15—C14	119.3 (18)
C38—Fe1—C37	100.79 (9)	H14—C15—C16	120.1 (17)
H1—Fe1—P1	81.2 (9)	C17—C16—C15	119.37 (19)
H1—Fe1—P2	83.1 (9)	H15—C16—C15	121.3 (18)
H1—Fe1—C37	87.6 (10)	H15—C16—C17	119.3 (18)
H1—Fe1—C38	171.6 (10)	C18—C17—C16	120.8 (2)
H2—Fe1—P1	75.0 (9)	H16—C17—C16	120.0 (16)
H2—Fe1—P2	82.4 (9)	H16—C17—C18	119.2 (16)
H2—Fe1—C37	167.3 (10)	C17—C18—C13	118.94 (18)
H2—Fe1—C38	91.9 (10)	H17—C18—C13	120.3 (15)
H2—Fe1—H1	79.7 (14)	H17—C18—C17	120.7 (15)
O1—P1—Fe1	120.20 (5)	C20—C19—O4	115.05 (15)
O2—P1—Fe1	113.78 (5)	C24—C19—O4	123.90 (16)
O2—P1—O1	98.15 (7)	C24—C19—C20	121.05 (18)
O3—P1—Fe1	121.72 (5)	C21—C20—C19	119.35 (17)
O3—P1—O1	95.64 (6)	H18—C20—C19	118.1 (15)
O3—P1—O2	103.30 (7)	H18—C20—C21	122.6 (15)
O4—P2—Fe1	120.29 (5)	C22—C21—C20	120.51 (19)
O5—P2—Fe1	111.34 (5)	H19—C21—C20	117.6 (18)
O5—P2—O4	98.98 (7)	H19—C21—C22	121.9 (18)
O6—P2—Fe1	123.22 (5)	C23—C22—C21	119.4 (2)
O6—P2—O4	96.54 (7)	H20—C22—C21	119.7 (17)
O6—P2—O5	102.54 (7)	H20—C22—C23	120.9 (17)
C1—O1—P1	126.64 (10)	C24—C23—C22	120.83 (18)
C7—O2—P1	123.47 (11)	H21—C23—C22	120.0 (16)
C13—O3—P1	124.17 (10)	H21—C23—C24	119.2 (16)
C19—O4—P2	127.78 (11)	C23—C24—C19	118.81 (18)
C25—O5—P2	124.58 (11)	H22—C24—C19	122.6 (15)
C31—O6—P2	130.07 (11)	H22—C24—C23	118.6 (15)
C2—C1—O1	119.47 (16)	C26—C25—O5	117.14 (17)
C6—C1—O1	118.44 (16)	C30—C25—O5	120.32 (17)
C6—C1—C2	121.86 (17)	C30—C25—C26	122.29 (17)
C3—C2—C1	118.99 (18)	C27—C26—C25	118.7 (2)
H3—C2—C1	118.5 (16)	H23—C26—C25	119.6 (16)
H3—C2—C3	122.5 (16)	H23—C26—C27	121.6 (16)
C4—C3—C2	120.3 (2)	C28—C27—C26	120.1 (2)
H4—C3—C2	118.3 (17)	H24—C27—C26	118.4 (19)
H4—C3—C4	121.4 (17)	H24—C27—C28	121.5 (19)
C5—C4—C3	119.72 (19)	C29—C28—C27	120.20 (19)
H5—C4—C3	120.7 (17)	H25—C28—C27	120.0 (19)
H5—C4—C5	119.6 (17)	H25—C28—C29	119.8 (19)
C6—C5—C4	120.60 (19)	C30—C29—C28	120.4 (2)
H6—C5—C4	120.4 (18)	H26—C29—C28	121.8 (16)
H6—C5—C6	118.9 (18)	H26—C29—C30	117.7 (17)
C5—C6—C1	118.56 (18)	C29—C30—C25	118.3 (2)
H7—C6—C1	120.5 (15)	H27—C30—C25	120.0 (14)
H7—C6—C5	120.8 (15)	H27—C30—C29	121.7 (14)
C8—C7—O2	117.72 (15)	C32—C31—O6	122.46 (16)
C12—C7—O2	120.07 (16)	C36—C31—O6	115.42 (17)
C12—C7—C8	122.17 (17)	C36—C31—C32	122.07 (17)
C9—C8—C7	118.58 (18)	C33—C32—C31	118.58 (18)
H8—C8—C7	119.8 (14)	H28—C32—C31	122.2 (15)
H8—C8—C9	121.6 (14)	H28—C32—C33	119.3 (15)
C10—C9—C8	120.2 (2)	C34—C33—C32	120.4 (2)
H9—C9—C8	120.2 (16)	H29—C33—C32	116.8 (17)
H9—C9—C10	119.6 (15)	H29—C33—C34	122.8 (17)
C11—C10—C9	119.89 (18)	C35—C34—C33	120.02 (18)
H10—C10—C9	117.2 (18)	H30—C34—C33	119.2 (18)
H10—C10—C11	122.9 (18)	H30—C34—C35	120.8 (18)
C12—C11—C10	120.82 (19)	C36—C35—C34	120.50 (19)
H11—C11—C10	121.1 (16)	H31—C35—C34	122.9 (16)
H11—C11—C12	118.1 (16)	H31—C35—C36	116.6 (17)
C11—C12—C7	118.30 (19)	C35—C36—C31	118.4 (2)
H12—C12—C7	120.8 (15)	H32—C36—C31	122.2 (14)
H12—C12—C11	120.9 (15)	H32—C36—C35	119.4 (14)
C14—C13—O3	116.24 (16)	O7—C37—Fe1	177.6 (2)
C18—C13—O3	122.76 (16)	O8—C38—Fe1	177.26 (17)
C18—C13—C14	120.94 (17)
Fe1—P1—O1—C1	−30.10 (10)	O5—C25—C30—C29	173.67 (17)
Fe1—P1—O2—C7	−157.61 (10)	O6—C31—C32—C33	−178.74 (16)
Fe1—P1—O3—C13	−50.68 (10)	O6—C31—C36—C35	178.55 (14)
Fe1—P2—O4—C19	−79.92 (9)	C1—C2—C3—C4	−0.6 (2)
Fe1—P2—O5—C25	171.90 (11)	C1—C6—C5—C4	0.5 (2)
Fe1—P2—O6—C31	−21.17 (10)	C2—C3—C4—C5	0.1 (2)
P1—O1—C1—C2	−84.50 (15)	C3—C4—C5—C6	0.0 (2)
P1—O1—C1—C6	100.90 (15)	C7—C8—C9—C10	0.6 (2)
P1—O2—C7—C8	97.62 (15)	C7—C12—C11—C10	1.1 (2)
P1—O2—C7—C12	−84.76 (15)	C8—C9—C10—C11	−0.8 (3)
P1—O3—C13—C14	147.17 (15)	C9—C10—C11—C12	0.0 (3)
P1—O3—C13—C18	−35.55 (16)	C13—C14—C15—C16	0.5 (2)
P2—O4—C19—C20	−170.58 (15)	C13—C18—C17—C16	0.3 (2)
P2—O4—C19—C24	9.80 (16)	C14—C15—C16—C17	−0.7 (2)
P2—O5—C25—C26	−105.64 (16)	C15—C16—C17—C18	0.3 (2)
P2—O5—C25—C30	79.99 (15)	C19—C20—C21—C22	−0.3 (2)
P2—O6—C31—C32	−43.67 (16)	C19—C24—C23—C22	0.5 (2)
P2—O6—C31—C36	138.69 (16)	C20—C21—C22—C23	−0.3 (2)
O1—C1—C2—C3	−173.25 (15)	C21—C22—C23—C24	0.2 (2)
O1—C1—C6—C5	173.36 (15)	C25—C26—C27—C28	0.5 (2)
O2—C7—C8—C9	178.05 (18)	C25—C30—C29—C28	0.1 (2)
O2—C7—C12—C11	−178.84 (18)	C26—C27—C28—C29	−0.7 (3)
O3—C13—C14—C15	177.51 (16)	C27—C28—C29—C30	0.5 (3)
O3—C13—C18—C17	−177.71 (16)	C31—C32—C33—C34	0.8 (2)
O4—C19—C20—C21	−178.66 (15)	C31—C36—C35—C34	−0.1 (2)
O4—C19—C24—C23	178.53 (17)	C32—C33—C34—C35	0.0 (2)
O5—C25—C26—C27	−174.13 (18)	C33—C34—C35—C36	−0.4 (2)

Dicarbonyl-cis-dihydrido-trans-bis(triphenylphosphite)iron(II) (QOSZON_IAM_SHADE3)

Crystal data

C38H32FeO8P2	Z = 2
Mr = 734.47	F(000) = 761.455
Triclinic, P1	Dx = 1.431 Mg m^−3
a = 9.6397 (12) Å	Mo Kα radiation, λ = 0.71073 Å
b = 10.4410 (13) Å	Cell parameters from 5000 reflections
c = 18.381 (2) Å	θ = 3.3–52.1°
α = 102.148 (15)°	µ = 0.59 mm^−1
β = 94.667 (15)°	T = 293 K
γ = 107.402 (14)°	Parallelepiped, colourless
V = 1705.0 (4) Å^3	0.5 × 0.25 × 0.1 mm

Data collection

STOE diffractometer	Rint = 0.034
Detector resolution: 1.60 pixels mm^-1	θmax = 26.1°, θmin = 2.1°
rotation en phi scans	h = −11→11
16806 measured reflections	k = −12→12
6202 independent reflections	l = −22→22
5084 reflections with I ≥ 2u(I)

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.027	Only H-atom coordinates refined
wR(F^2) = 0.069	w = 1/[σ^2(Fo^2) + (0.0365P)^2 + 0.4167P] where P = (Fo^2 + 2Fc^2)/3
S = 0.99	(Δ/σ)max = 0.001
6202 reflections	Δρmax = 0.34 e Å^−3
538 parameters	Δρmin = −0.33 e Å^−3

Special details

Experimental. The crystal was pasted on a glass fiber, by using an oil-coated shock-cooled crystal.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Fe1	0.53170 (2)	0.83647 (3)	0.270682 (13)	0.01970 (7)
P1	0.35103 (4)	0.72598 (5)	0.18545 (2)	0.01938 (10)
P2	0.72487 (4)	1.00380 (5)	0.32211 (2)	0.01928 (10)
O1	0.30698 (13)	0.79719 (12)	0.12198 (6)	0.0249 (3)
O2	0.37125 (12)	0.59230 (13)	0.13060 (6)	0.0229 (3)
O3	0.18561 (12)	0.66732 (13)	0.20457 (7)	0.0241 (3)
O4	0.71943 (13)	1.12305 (13)	0.39192 (6)	0.0249 (3)
O5	0.84475 (12)	0.95202 (13)	0.36170 (7)	0.0238 (3)
O6	0.82079 (13)	1.10514 (13)	0.27691 (6)	0.0250 (3)
O7	0.40855 (18)	0.8193 (2)	0.41021 (8)	0.0551 (5)
O8	0.67910 (16)	0.62695 (17)	0.25555 (9)	0.0416 (4)
C1	0.32786 (18)	0.93778 (18)	0.13020 (9)	0.0206 (4)
C2	0.2250 (2)	0.9927 (2)	0.15919 (10)	0.0275 (4)
C3	0.2387 (2)	1.1292 (2)	0.15977 (11)	0.0358 (5)
C4	0.3546 (2)	1.2085 (2)	0.13216 (12)	0.0365 (5)
C5	0.4576 (2)	1.1513 (2)	0.10384 (12)	0.0330 (5)
C6	0.44539 (19)	1.0153 (2)	0.10289 (10)	0.0265 (4)
C7	0.29318 (18)	0.53138 (18)	0.05715 (9)	0.0220 (4)
C8	0.3625 (2)	0.5674 (2)	−0.00202 (11)	0.0312 (4)
C9	0.2890 (3)	0.5052 (2)	−0.07501 (11)	0.0379 (5)
C10	0.1484 (2)	0.4100 (2)	−0.08773 (11)	0.0356 (5)
C11	0.0823 (2)	0.3759 (2)	−0.02776 (12)	0.0355 (5)
C12	0.1547 (2)	0.4356 (2)	0.04576 (11)	0.0292 (4)
C13	0.14860 (17)	0.58848 (18)	0.25724 (9)	0.0220 (4)
C14	0.0356 (2)	0.6068 (2)	0.29563 (11)	0.0304 (4)
C15	−0.0105 (2)	0.5280 (2)	0.34652 (12)	0.0376 (5)
C16	0.0557 (2)	0.4328 (2)	0.35949 (11)	0.0350 (5)
C17	0.1681 (2)	0.4154 (2)	0.32057 (11)	0.0327 (4)
C18	0.2154 (2)	0.4929 (2)	0.26890 (11)	0.0275 (4)
C19	0.67117 (17)	1.23530 (18)	0.38982 (9)	0.0220 (4)
C20	0.6997 (2)	1.3332 (2)	0.45773 (10)	0.0263 (4)
C21	0.6533 (2)	1.4471 (2)	0.46172 (11)	0.0328 (4)
C22	0.5795 (2)	1.4639 (2)	0.39843 (12)	0.0339 (4)
C23	0.5529 (2)	1.3657 (2)	0.33077 (11)	0.0305 (4)
C24	0.59877 (19)	1.2510 (2)	0.32570 (10)	0.0261 (4)
C25	0.99053 (18)	1.03593 (19)	0.39252 (10)	0.0238 (4)
C26	1.1000 (2)	1.0150 (2)	0.35265 (12)	0.0343 (4)
C27	1.2454 (2)	1.0867 (3)	0.38458 (15)	0.0462 (6)
C28	1.2787 (2)	1.1761 (2)	0.45509 (14)	0.0439 (6)
C29	1.1674 (2)	1.1959 (2)	0.49394 (12)	0.0380 (5)
C30	1.0207 (2)	1.1254 (2)	0.46261 (11)	0.0291 (4)
C31	0.82814 (17)	1.08485 (19)	0.20017 (9)	0.0207 (4)
C32	0.83568 (19)	0.9631 (2)	0.15682 (10)	0.0252 (4)
C33	0.8457 (2)	0.9530 (2)	0.08084 (11)	0.0306 (4)
C34	0.8499 (2)	1.0638 (2)	0.05002 (10)	0.0322 (5)
C35	0.84404 (19)	1.1854 (2)	0.09468 (11)	0.0299 (4)
C36	0.83318 (19)	1.1976 (2)	0.17074 (10)	0.0255 (4)
C37	0.4560 (2)	0.8231 (2)	0.35549 (11)	0.0317 (4)
C38	0.61914 (19)	0.7077 (2)	0.26266 (10)	0.0267 (4)
H1	0.471 (2)	0.946 (2)	0.2680 (13)	0.043455
H2	0.578 (2)	0.871 (3)	0.2038 (12)	0.041723
H3	0.145 (2)	0.934 (2)	0.1773 (13)	0.040070
H4	0.164 (3)	1.165 (3)	0.1783 (14)	0.044504
H5	0.364 (3)	1.304 (3)	0.1321 (14)	0.046276
H6	0.536 (3)	1.203 (3)	0.0863 (13)	0.040968
H7	0.512 (2)	0.973 (2)	0.0802 (13)	0.038042
H8	0.461 (2)	0.633 (3)	0.0079 (12)	0.041945
H9	0.336 (3)	0.528 (3)	−0.1180 (13)	0.050025
H10	0.101 (3)	0.373 (3)	−0.1379 (14)	0.053748
H11	−0.017 (3)	0.309 (3)	−0.0355 (13)	0.046007
H12	0.111 (2)	0.410 (2)	0.0867 (13)	0.040938
H13	−0.005 (3)	0.675 (3)	0.2865 (14)	0.045308
H14	−0.090 (3)	0.541 (3)	0.3734 (15)	0.054197
H15	0.024 (3)	0.378 (3)	0.3952 (15)	0.056417
H16	0.213 (3)	0.349 (3)	0.3282 (14)	0.047598
H17	0.289 (2)	0.477 (2)	0.2400 (13)	0.039425
H18	0.753 (3)	1.319 (3)	0.5006 (13)	0.045409
H19	0.673 (3)	1.511 (3)	0.5082 (14)	0.050087
H20	0.549 (3)	1.539 (3)	0.4020 (14)	0.050419
H21	0.499 (2)	1.377 (2)	0.2854 (13)	0.041360
H22	0.582 (2)	1.187 (2)	0.2777 (13)	0.035962
H23	1.074 (2)	0.950 (3)	0.3054 (14)	0.043708
H24	1.319 (3)	1.070 (3)	0.3581 (15)	0.050678
H25	1.385 (3)	1.226 (3)	0.4784 (14)	0.055228
H26	1.188 (3)	1.258 (3)	0.5430 (14)	0.050032
H27	0.943 (3)	1.137 (3)	0.4888 (13)	0.044477
H28	0.834 (2)	0.883 (2)	0.1778 (12)	0.037841
H29	0.851 (3)	0.870 (3)	0.0528 (13)	0.043471
H30	0.855 (3)	1.054 (3)	−0.0024 (13)	0.049313
H31	0.849 (3)	1.266 (3)	0.0758 (13)	0.044591
H32	0.829 (2)	1.283 (3)	0.2010 (13)	0.038536

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Fe1	0.01810 (12)	0.02061 (14)	0.01828 (12)	0.00280 (9)	0.00102 (9)	0.00610 (10)
P1	0.0180 (2)	0.0184 (2)	0.0205 (2)	0.00321 (16)	0.00067 (15)	0.00673 (17)
P2	0.0195 (2)	0.0196 (2)	0.01679 (19)	0.00361 (17)	0.00163 (15)	0.00474 (17)
O1	0.0299 (6)	0.0183 (7)	0.0224 (6)	0.0035 (5)	−0.0048 (5)	0.0063 (5)
O2	0.0230 (6)	0.0217 (7)	0.0224 (6)	0.0074 (5)	−0.0013 (5)	0.0033 (5)
O3	0.0177 (6)	0.0263 (7)	0.0296 (6)	0.0049 (5)	0.0033 (5)	0.0130 (5)
O4	0.0310 (6)	0.0251 (7)	0.0186 (6)	0.0110 (5)	0.0017 (5)	0.0034 (5)
O5	0.0192 (6)	0.0215 (7)	0.0267 (6)	0.0026 (5)	−0.0031 (5)	0.0058 (5)
O6	0.0276 (6)	0.0229 (7)	0.0180 (5)	−0.0006 (5)	0.0033 (5)	0.0045 (5)
O7	0.0520 (10)	0.0757 (13)	0.0295 (8)	0.0029 (9)	0.0161 (7)	0.0182 (8)
O8	0.0422 (8)	0.0346 (9)	0.0506 (9)	0.0192 (7)	0.0014 (7)	0.0085 (7)
C1	0.0233 (8)	0.0199 (9)	0.0179 (7)	0.0062 (7)	−0.0014 (6)	0.0061 (7)
C2	0.0260 (9)	0.0329 (11)	0.0234 (8)	0.0095 (8)	0.0049 (7)	0.0061 (8)
C3	0.0391 (11)	0.0385 (13)	0.0316 (10)	0.0213 (10)	0.0014 (8)	0.0012 (9)
C4	0.0435 (12)	0.0229 (11)	0.0412 (11)	0.0121 (9)	−0.0082 (9)	0.0074 (9)
C5	0.0277 (9)	0.0267 (11)	0.0436 (11)	0.0024 (8)	0.0010 (8)	0.0175 (9)
C6	0.0227 (9)	0.0292 (11)	0.0301 (9)	0.0088 (8)	0.0044 (7)	0.0120 (8)
C7	0.0227 (8)	0.0182 (9)	0.0242 (8)	0.0086 (7)	−0.0014 (7)	0.0019 (7)
C8	0.0348 (10)	0.0256 (11)	0.0300 (9)	0.0061 (8)	0.0040 (8)	0.0058 (8)
C9	0.0552 (13)	0.0328 (12)	0.0262 (9)	0.0150 (10)	0.0064 (9)	0.0070 (9)
C10	0.0475 (12)	0.0277 (11)	0.0270 (10)	0.0161 (9)	−0.0082 (9)	−0.0029 (8)
C11	0.0292 (10)	0.0282 (11)	0.0394 (11)	0.0056 (9)	−0.0066 (8)	−0.0024 (9)
C12	0.0272 (9)	0.0243 (11)	0.0318 (10)	0.0052 (8)	0.0034 (8)	0.0027 (8)
C13	0.0179 (8)	0.0199 (9)	0.0239 (8)	0.0000 (7)	0.0008 (6)	0.0063 (7)
C14	0.0258 (9)	0.0313 (11)	0.0345 (10)	0.0096 (8)	0.0063 (8)	0.0082 (9)
C15	0.0296 (10)	0.0453 (14)	0.0369 (10)	0.0067 (9)	0.0141 (8)	0.0122 (10)
C16	0.0333 (10)	0.0346 (12)	0.0303 (10)	−0.0012 (9)	0.0041 (8)	0.0119 (9)
C17	0.0338 (10)	0.0276 (11)	0.0356 (10)	0.0059 (8)	0.0009 (8)	0.0134 (9)
C18	0.0240 (9)	0.0269 (11)	0.0325 (9)	0.0073 (8)	0.0061 (7)	0.0103 (8)
C19	0.0197 (8)	0.0200 (9)	0.0254 (8)	0.0042 (7)	0.0060 (6)	0.0060 (7)
C20	0.0280 (9)	0.0236 (10)	0.0228 (8)	0.0023 (8)	0.0063 (7)	0.0039 (7)
C21	0.0367 (10)	0.0253 (11)	0.0304 (10)	0.0045 (8)	0.0117 (8)	−0.0001 (8)
C22	0.0357 (10)	0.0237 (11)	0.0438 (11)	0.0118 (9)	0.0118 (9)	0.0061 (9)
C23	0.0285 (9)	0.0252 (11)	0.0362 (10)	0.0072 (8)	0.0006 (8)	0.0077 (8)
C24	0.0246 (9)	0.0252 (10)	0.0238 (8)	0.0044 (7)	0.0004 (7)	0.0026 (8)
C25	0.0196 (8)	0.0211 (9)	0.0279 (9)	0.0018 (7)	−0.0018 (7)	0.0091 (7)
C26	0.0288 (10)	0.0337 (12)	0.0388 (11)	0.0090 (9)	0.0058 (8)	0.0074 (9)
C27	0.0244 (10)	0.0461 (15)	0.0715 (16)	0.0099 (10)	0.0129 (10)	0.0220 (13)
C28	0.0235 (10)	0.0349 (13)	0.0659 (15)	−0.0019 (9)	−0.0076 (10)	0.0190 (11)
C29	0.0365 (11)	0.0265 (11)	0.0396 (11)	−0.0018 (9)	−0.0123 (9)	0.0081 (9)
C30	0.0284 (9)	0.0256 (10)	0.0309 (9)	0.0053 (8)	−0.0007 (8)	0.0086 (8)
C31	0.0157 (7)	0.0254 (10)	0.0187 (7)	0.0034 (7)	0.0012 (6)	0.0056 (7)
C32	0.0229 (8)	0.0274 (11)	0.0271 (9)	0.0090 (7)	0.0061 (7)	0.0086 (8)
C33	0.0289 (9)	0.0346 (12)	0.0266 (9)	0.0116 (8)	0.0062 (7)	0.0018 (8)
C34	0.0267 (9)	0.0490 (14)	0.0215 (9)	0.0112 (9)	0.0050 (7)	0.0113 (9)
C35	0.0244 (9)	0.0382 (12)	0.0319 (9)	0.0087 (8)	0.0058 (7)	0.0201 (9)
C36	0.0227 (8)	0.0238 (10)	0.0292 (9)	0.0045 (7)	0.0043 (7)	0.0094 (8)
C37	0.0260 (9)	0.0346 (12)	0.0288 (10)	0.0017 (8)	−0.0011 (7)	0.0094 (8)
C38	0.0242 (9)	0.0255 (11)	0.0256 (9)	0.0019 (8)	−0.0006 (7)	0.0066 (8)
H1	0.050510	0.032410	0.049170	0.015320	0.004270	0.012320
H2	0.040840	0.054000	0.031110	0.012410	0.011750	0.014150
H3	0.029570	0.036170	0.053700	0.008420	0.008820	0.011830
H4	0.037090	0.034310	0.063650	0.016170	0.005150	0.009680
H5	0.045040	0.030390	0.064070	0.010400	0.002900	0.017860
H6	0.039860	0.039070	0.044520	0.007970	0.007450	0.018170
H7	0.040470	0.035630	0.039100	0.013300	0.008570	0.009200
H8	0.035360	0.048250	0.035060	0.007910	0.001630	0.004760
H9	0.055510	0.055620	0.030390	0.011780	0.004500	0.002380
H10	0.056270	0.056240	0.033390	0.009180	−0.011030	−0.001470
H11	0.036780	0.042480	0.047540	0.005620	−0.009850	0.004050
H12	0.035920	0.043170	0.039320	0.008010	0.000650	0.009820
H13	0.041720	0.040340	0.055190	0.010950	0.013240	0.015870
H14	0.044400	0.056150	0.059690	0.006290	0.021880	0.018660
H15	0.053340	0.054650	0.058130	−0.000640	0.015760	0.031010
H16	0.048430	0.038060	0.055400	0.005360	0.002170	0.024470
H17	0.038430	0.036760	0.044340	0.011080	0.007170	0.014010
H18	0.053460	0.044100	0.031480	0.008800	0.001330	0.006300
H19	0.055730	0.040600	0.040720	0.009330	0.004740	−0.007790
H20	0.055010	0.031810	0.058700	0.015450	0.004010	−0.001170
H21	0.044070	0.034280	0.044280	0.013200	0.000460	0.008330
H22	0.041680	0.030530	0.031060	0.009560	0.000930	0.002730
H23	0.033000	0.042030	0.047940	0.008270	−0.003160	0.003060
H24	0.031280	0.047950	0.068200	0.012080	−0.001150	0.009050
H25	0.033410	0.052790	0.067140	0.005850	−0.016370	0.009610
H26	0.046520	0.046180	0.042100	0.002280	−0.013880	0.004880
H27	0.040690	0.047330	0.037650	0.007660	−0.001290	0.006450
H28	0.040980	0.034490	0.038560	0.010080	0.009560	0.011950
H29	0.047310	0.040640	0.038280	0.010790	0.013710	0.003240
H30	0.059070	0.054140	0.031630	0.009370	0.018290	0.012840
H31	0.051530	0.041160	0.040170	0.005260	0.011780	0.020560
H32	0.044260	0.030860	0.036560	0.006870	0.005910	0.007860

Geometric parameters (Å, º)

Fe1—P1	2.1004 (7)	C13—C18	1.381 (3)
Fe1—P2	2.1180 (7)	C14—C15	1.386 (3)
Fe1—C37	1.788 (2)	C14—H13	0.95 (3)
Fe1—C38	1.776 (2)	C15—C16	1.381 (3)
Fe1—H1	1.44 (2)	C15—H14	0.97 (3)
Fe1—H2	1.42 (2)	C16—C17	1.380 (3)
P1—O1	1.6023 (12)	C16—H15	0.97 (2)
P1—O2	1.6140 (14)	C17—C18	1.392 (3)
P1—O3	1.6245 (12)	C17—H16	0.95 (3)
P2—O4	1.6052 (13)	C18—H17	0.95 (2)
P2—O5	1.5999 (12)	C19—C20	1.385 (3)
P2—O6	1.6046 (12)	C19—C24	1.385 (2)
O1—C1	1.394 (2)	C20—C21	1.381 (3)
O2—C7	1.407 (2)	C20—H18	0.97 (2)
O3—C13	1.399 (2)	C21—C22	1.384 (3)
O4—C19	1.391 (2)	C21—H19	0.93 (2)
O5—C25	1.410 (2)	C22—C23	1.385 (3)
O6—C31	1.392 (2)	C22—H20	0.91 (3)
O7—C37	1.142 (2)	C23—C24	1.384 (3)
O8—C38	1.149 (2)	C23—H21	0.99 (2)
C1—C2	1.376 (3)	C24—H22	0.96 (2)
C1—C6	1.381 (2)	C25—C26	1.376 (3)
C2—C3	1.389 (3)	C25—C30	1.374 (3)
C2—H3	0.96 (2)	C26—C27	1.387 (3)
C3—C4	1.381 (3)	C26—H23	0.94 (2)
C3—H4	0.96 (2)	C27—C28	1.378 (4)
C4—C5	1.386 (3)	C27—H24	0.93 (3)
C4—H5	0.97 (2)	C28—C29	1.378 (3)
C5—C6	1.385 (3)	C28—H25	1.01 (2)
C5—H6	0.92 (2)	C29—C30	1.393 (3)
C6—H7	0.95 (2)	C29—H26	0.96 (3)
C7—C8	1.382 (3)	C30—H27	0.95 (3)
C7—C12	1.376 (3)	C31—C32	1.376 (3)
C8—C9	1.388 (3)	C31—C36	1.385 (3)
C8—H8	0.96 (2)	C32—C33	1.392 (3)
C9—C10	1.387 (3)	C32—H28	0.99 (2)
C9—H9	0.98 (2)	C33—C34	1.383 (3)
C10—C11	1.376 (3)	C33—H29	0.93 (3)
C10—H10	0.94 (2)	C34—C35	1.379 (3)
C11—C12	1.390 (3)	C34—H30	0.95 (2)
C11—H11	0.98 (2)	C35—C36	1.393 (3)
C12—H12	0.94 (2)	C35—H31	0.96 (2)
C13—C14	1.383 (3)	C36—H32	0.96 (2)
P2—Fe1—P1	154.35 (2)	C15—C14—C13	119.30 (19)
C37—Fe1—P1	103.47 (6)	H13—C14—C13	117.6 (15)
C37—Fe1—P2	95.99 (6)	H13—C14—C15	123.1 (15)
C38—Fe1—P1	97.52 (6)	C16—C15—C14	120.72 (19)
C38—Fe1—P2	95.05 (6)	H14—C15—C14	119.3 (16)
C38—Fe1—C37	100.77 (9)	H14—C15—C16	120.0 (16)
H1—Fe1—P1	81.4 (9)	C17—C16—C15	119.30 (18)
H1—Fe1—P2	82.9 (9)	H15—C16—C15	121.2 (17)
H1—Fe1—C37	87.6 (9)	H15—C16—C17	119.5 (17)
H1—Fe1—C38	171.6 (9)	C18—C17—C16	120.9 (2)
H2—Fe1—P1	75.0 (9)	H16—C17—C16	120.0 (15)
H2—Fe1—P2	82.3 (9)	H16—C17—C18	119.2 (15)
H2—Fe1—C37	167.3 (10)	C17—C18—C13	118.96 (18)
H2—Fe1—C38	91.9 (10)	H17—C18—C13	120.3 (14)
H2—Fe1—H1	79.7 (13)	H17—C18—C17	120.7 (14)
O1—P1—Fe1	120.20 (5)	C20—C19—O4	115.07 (15)
O2—P1—Fe1	113.79 (4)	C24—C19—O4	123.93 (16)
O2—P1—O1	98.14 (6)	C24—C19—C20	121.00 (17)
O3—P1—Fe1	121.72 (5)	C21—C20—C19	119.38 (17)
O3—P1—O1	95.65 (6)	H18—C20—C19	118.0 (15)
O3—P1—O2	103.30 (7)	H18—C20—C21	122.6 (15)
O4—P2—Fe1	120.29 (5)	C22—C21—C20	120.47 (18)
O5—P2—Fe1	111.34 (5)	H19—C21—C20	117.6 (17)
O5—P2—O4	98.99 (6)	H19—C21—C22	122.0 (17)
O6—P2—Fe1	123.22 (5)	C23—C22—C21	119.4 (2)
O6—P2—O4	96.53 (7)	H20—C22—C21	119.5 (16)
O6—P2—O5	102.54 (7)	H20—C22—C23	121.0 (16)
C1—O1—P1	126.63 (10)	C24—C23—C22	120.90 (18)
C7—O2—P1	123.49 (11)	H21—C23—C22	119.8 (14)
C13—O3—P1	124.18 (10)	H21—C23—C24	119.3 (14)
C19—O4—P2	127.79 (10)	C23—C24—C19	118.81 (17)
C25—O5—P2	124.59 (11)	H22—C24—C19	122.5 (14)
C31—O6—P2	130.04 (11)	H22—C24—C23	118.7 (14)
C2—C1—O1	119.50 (15)	C26—C25—O5	117.22 (17)
C6—C1—O1	118.51 (16)	C30—C25—O5	120.33 (16)
C6—C1—C2	121.77 (17)	C30—C25—C26	122.20 (17)
C3—C2—C1	119.01 (18)	C27—C26—C25	118.7 (2)
H3—C2—C1	118.8 (14)	H23—C26—C25	119.3 (14)
H3—C2—C3	122.2 (14)	H23—C26—C27	121.9 (14)
C4—C3—C2	120.3 (2)	C28—C27—C26	120.3 (2)
H4—C3—C2	118.1 (15)	H24—C27—C26	118.6 (15)
H4—C3—C4	121.6 (15)	H24—C27—C28	121.1 (15)
C5—C4—C3	119.69 (19)	C29—C28—C27	120.09 (18)
H5—C4—C3	120.6 (15)	H25—C28—C27	119.5 (16)
H5—C4—C5	119.7 (15)	H25—C28—C29	120.4 (16)
C6—C5—C4	120.67 (19)	C30—C29—C28	120.4 (2)
H6—C5—C4	120.3 (15)	H26—C29—C28	121.6 (15)
H6—C5—C6	119.0 (15)	H26—C29—C30	118.0 (15)
C5—C6—C1	118.58 (18)	C29—C30—C25	118.3 (2)
H7—C6—C1	120.2 (14)	H27—C30—C25	120.1 (14)
H7—C6—C5	121.0 (14)	H27—C30—C29	121.5 (14)
C8—C7—O2	117.75 (15)	C32—C31—O6	122.51 (16)
C12—C7—O2	120.15 (16)	C36—C31—O6	115.46 (16)
C12—C7—C8	122.06 (16)	C36—C31—C32	121.99 (16)
C9—C8—C7	118.59 (18)	C33—C32—C31	118.59 (18)
H8—C8—C7	120.0 (13)	H28—C32—C31	122.2 (14)
H8—C8—C9	121.4 (13)	H28—C32—C33	119.2 (14)
C10—C9—C8	120.3 (2)	C34—C33—C32	120.5 (2)
H9—C9—C8	120.2 (14)	H29—C33—C32	117.1 (15)
H9—C9—C10	119.5 (14)	H29—C33—C34	122.4 (15)
C11—C10—C9	119.82 (18)	C35—C34—C33	119.97 (18)
H10—C10—C9	117.5 (16)	H30—C34—C33	119.0 (16)
H10—C10—C11	122.6 (16)	H30—C34—C35	121.0 (16)
C12—C11—C10	120.82 (18)	C36—C35—C34	120.49 (18)
H11—C11—C10	121.1 (14)	H31—C35—C34	122.7 (15)
H11—C11—C12	118.1 (14)	H31—C35—C36	116.8 (15)
C11—C12—C7	118.39 (19)	C35—C36—C31	118.45 (19)
H12—C12—C7	120.5 (13)	H32—C36—C31	122.2 (13)
H12—C12—C11	121.1 (13)	H32—C36—C35	119.4 (13)
C14—C13—O3	116.27 (16)	O7—C37—Fe1	177.6 (2)
C18—C13—O3	122.81 (16)	O8—C38—Fe1	177.25 (17)
C18—C13—C14	120.86 (17)

 

(SITKUB_HAR_0_HADPs)

Crystal data

C24H47BClO2P2Rh	F(000) = 1213.334
Mr = 578.77	Dx = 1.348 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
a = 11.228 (3) Å	Cell parameters from 925 reflections
b = 11.101 (3) Å	θ = 12.0–24.6°
c = 23.414 (7) Å	µ = 0.82 mm^−1
β = 102.28 (4)°	T = 120 K
V = 2851.6 (14) Å^3	Fragment, colourless
Z = 4	0.6 × 0.4 × 0.2 mm

Data collection

SMART 1K CCD area detector diffractometer	7021 reflections with I ≥ 2u(I)
Radiation source: fine-focus sealed tube	Rint = 0.029
Graphite monochromator	θmax = 29.1°, θmin = 1.8°
ω scans	h = −15→15
33082 measured reflections	k = −15→15
7624 independent reflections	l = −31→31

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.034	Only H-atom coordinates refined
wR(F^2) = 0.125	w = 1/[σ^2(Fo^2) + (0.1P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 1.08	(Δ/σ)max = 0.001
7624 reflections	Δρmax = 0.56 e Å^−3
421 parameters	Δρmin = −0.87 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Rh	0.311338 (12)	0.814873 (12)	0.861869 (6)	0.01603 (8)
H	0.3434 (19)	0.7723 (19)	0.9227 (9)	0.000000
Cl	0.32707 (5)	0.93363 (5)	0.77702 (2)	0.02754 (12)
B	0.2123 (2)	0.68038 (19)	0.88061 (10)	0.0192 (4)
P1	0.17687 (4)	0.96110 (4)	0.88295 (2)	0.01929 (11)
P2	0.46544 (5)	0.68311 (4)	0.84844 (2)	0.01814 (12)
O1	0.10472 (13)	0.64522 (13)	0.84059 (6)	0.0206 (3)
O2	0.22703 (13)	0.60328 (14)	0.93007 (6)	0.0235 (3)
C1	0.05439 (18)	0.55196 (17)	0.86606 (8)	0.0197 (4)
C2	0.12868 (18)	0.52631 (18)	0.91998 (9)	0.0215 (4)
C3	0.0992 (2)	0.4377 (2)	0.95623 (11)	0.0321 (5)
H3	0.1608 (19)	0.4143 (19)	0.9988 (9)	0.000000
C4	−0.0095 (2)	0.3744 (2)	0.93512 (12)	0.0341 (5)
H4	−0.034 (2)	0.3013 (18)	0.9669 (10)	0.000000
C5	−0.0840 (2)	0.4000 (2)	0.88072 (10)	0.0278 (4)
H5	−0.1722 (19)	0.348 (2)	0.8684 (9)	0.000000
C6	−0.05300 (18)	0.49057 (19)	0.84502 (9)	0.0226 (4)
H6	−0.1131 (19)	0.4999 (19)	0.8002 (9)	0.000000
C7	0.09960 (19)	0.9378 (2)	0.94522 (9)	0.0238 (4)
H7	0.0615 (18)	1.0262 (18)	0.9523 (9)	0.000000
C8	0.0002 (2)	0.8410 (2)	0.93431 (10)	0.0275 (4)
H8A	0.0344 (18)	0.7643 (18)	0.9246 (8)	0.000000
H8B	−0.0736 (19)	0.868 (2)	0.8900 (9)	0.000000
H8C	−0.0497 (18)	0.841 (2)	0.9665 (9)	0.000000
C9	0.1914 (2)	0.9114 (2)	1.00212 (10)	0.0326 (5)
H9A	0.1414 (19)	0.9044 (19)	1.0403 (9)	0.000000
H9B	0.2531 (18)	0.9775 (18)	1.0145 (8)	0.000000
H9C	0.2367 (19)	0.8339 (19)	0.9946 (9)	0.000000
C10	0.05464 (18)	1.00398 (19)	0.81998 (9)	0.0237 (4)
H10	0.1175 (19)	1.0588 (19)	0.7962 (9)	0.000000
C11	−0.0435 (2)	1.0868 (2)	0.83484 (12)	0.0352 (5)
H11A	−0.0946 (19)	1.1286 (19)	0.7933 (9)	0.000000
H11B	−0.0107 (18)	1.1539 (19)	0.8646 (9)	0.000000
H11C	−0.1164 (18)	1.0374 (19)	0.8515 (9)	0.000000
C12	−0.00192 (19)	0.8938 (2)	0.78408 (9)	0.0256 (4)
H12A	−0.043 (2)	0.8283 (18)	0.8072 (10)	0.000000
H12B	0.073 (2)	0.838 (2)	0.7714 (9)	0.000000
H12C	−0.0566 (19)	0.9384 (18)	0.7454 (9)	0.000000
C13	0.2597 (2)	1.10605 (19)	0.90651 (11)	0.0300 (5)
H13	0.2165 (18)	1.1444 (19)	0.9392 (8)	0.000000
C14	0.2507 (3)	1.2024 (2)	0.85859 (15)	0.0451 (7)
H14A	0.2999 (18)	1.282 (2)	0.8726 (9)	0.000000
H14B	0.1554 (19)	1.2316 (19)	0.8409 (9)	0.000000
H14C	0.288 (2)	1.1741 (17)	0.8228 (9)	0.000000
C15	0.3941 (2)	1.0819 (2)	0.93309 (14)	0.0419 (6)
H15A	0.4303 (18)	1.0510 (18)	0.9023 (9)	0.000000
H15B	0.4023 (18)	1.0119 (18)	0.9650 (9)	0.000000
H15C	0.4386 (19)	1.163 (2)	0.9571 (9)	0.000000
C16	0.43424 (19)	0.5852 (2)	0.78290 (10)	0.0247 (4)
H16	0.5106 (18)	0.5270 (18)	0.7812 (9)	0.000000
C17	0.3295 (2)	0.4988 (2)	0.78519 (12)	0.0373 (6)
H17A	0.2429 (19)	0.5471 (19)	0.7896 (9)	0.000000
H17B	0.3383 (18)	0.4436 (18)	0.8201 (9)	0.000000
H17C	0.3107 (18)	0.4415 (18)	0.7505 (9)	0.000000
C18	0.4074 (3)	0.6567 (3)	0.72577 (11)	0.0375 (5)
H18A	0.3882 (19)	0.5987 (19)	0.6862 (9)	0.000000
H18B	0.4832 (19)	0.7108 (19)	0.7203 (9)	0.000000
H18C	0.318 (2)	0.7028 (18)	0.7256 (10)	0.000000
C19	0.5141 (2)	0.5733 (2)	0.90887 (10)	0.0266 (4)
H19	0.4276 (18)	0.5419 (18)	0.9111 (8)	0.000000
C20	0.5639 (3)	0.6346 (3)	0.96760 (11)	0.0400 (6)
H20A	0.565 (2)	0.5660 (19)	1.0071 (10)	0.000000
H20B	0.494 (2)	0.6971 (18)	0.9820 (10)	0.000000
H20C	0.6523 (19)	0.6685 (18)	0.9647 (9)	0.000000
C21	0.6008 (3)	0.4724 (3)	0.89894 (14)	0.0452 (7)
H21A	0.6869 (18)	0.5040 (19)	0.8955 (9)	0.000000
H21B	0.5697 (17)	0.4299 (17)	0.8646 (9)	0.000000
H21C	0.6089 (19)	0.4163 (19)	0.9409 (9)	0.000000
C22	0.59689 (17)	0.77505 (19)	0.83757 (9)	0.0219 (4)
H22	0.553 (2)	0.8235 (16)	0.8026 (9)	0.000000
C23	0.6395 (2)	0.8672 (2)	0.88652 (11)	0.0313 (5)
H23A	0.686 (2)	0.8219 (17)	0.9242 (10)	0.000000
H23B	0.5629 (18)	0.9186 (19)	0.8911 (9)	0.000000
H23C	0.7019 (19)	0.9417 (19)	0.8746 (9)	0.000000
C24	0.7061 (2)	0.7058 (2)	0.82474 (13)	0.0335 (5)
H24A	0.7706 (19)	0.7628 (19)	0.8039 (9)	0.000000
H24B	0.6912 (18)	0.6477 (19)	0.7924 (9)	0.000000
H24C	0.760 (2)	0.665 (2)	0.8680 (9)	0.000000

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Rh	0.01390 (11)	0.01691 (11)	0.01760 (11)	0.00037 (4)	0.00405 (7)	0.00055 (4)
H	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
Cl	0.0233 (2)	0.0310 (3)	0.0306 (2)	0.00458 (18)	0.01086 (19)	0.01196 (19)
B	0.0168 (10)	0.0198 (10)	0.0220 (10)	−0.0004 (7)	0.0064 (8)	0.0001 (7)
P1	0.0176 (2)	0.0190 (2)	0.0216 (2)	0.00190 (17)	0.00470 (18)	−0.00068 (17)
P2	0.0150 (2)	0.0191 (2)	0.0208 (2)	0.00077 (15)	0.00468 (19)	−0.00013 (15)
O1	0.0194 (6)	0.0231 (7)	0.0190 (6)	−0.0018 (5)	0.0032 (5)	0.0009 (5)
O2	0.0203 (7)	0.0260 (7)	0.0230 (7)	−0.0019 (5)	0.0017 (5)	0.0056 (5)
C1	0.0202 (9)	0.0183 (8)	0.0216 (9)	−0.0012 (7)	0.0067 (7)	−0.0027 (6)
C2	0.0209 (9)	0.0199 (9)	0.0236 (9)	−0.0012 (7)	0.0047 (7)	0.0035 (7)
C3	0.0311 (11)	0.0295 (11)	0.0349 (12)	−0.0028 (9)	0.0057 (9)	0.0110 (9)
H3	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C4	0.0343 (12)	0.0264 (10)	0.0429 (13)	−0.0063 (9)	0.0113 (10)	0.0100 (9)
H4	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C5	0.0258 (10)	0.0222 (9)	0.0370 (11)	−0.0042 (8)	0.0103 (9)	−0.0022 (8)
H5	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C6	0.0193 (9)	0.0226 (9)	0.0265 (9)	−0.0012 (7)	0.0059 (7)	−0.0033 (7)
H6	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C7	0.0236 (9)	0.0275 (10)	0.0217 (9)	0.0030 (8)	0.0075 (7)	−0.0037 (7)
H7	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C8	0.0286 (11)	0.0293 (10)	0.0276 (10)	0.0014 (9)	0.0128 (8)	−0.0018 (8)
H8A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H8B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H8C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C9	0.0344 (12)	0.0404 (13)	0.0228 (10)	0.0018 (10)	0.0055 (9)	−0.0053 (9)
H9A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H9B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H9C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C10	0.0208 (9)	0.0239 (9)	0.0254 (9)	0.0052 (7)	0.0028 (7)	0.0047 (7)
H10	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C11	0.0290 (11)	0.0355 (12)	0.0409 (13)	0.0166 (10)	0.0070 (10)	0.0014 (10)
H11A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H11B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H11C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C12	0.0207 (9)	0.0312 (11)	0.0236 (9)	0.0004 (8)	0.0017 (7)	0.0027 (8)
H12A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H12B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H12C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C13	0.0273 (10)	0.0200 (9)	0.0422 (12)	0.0001 (8)	0.0063 (9)	−0.0063 (8)
H13	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C14	0.0521 (17)	0.0250 (11)	0.0599 (18)	−0.0091 (11)	0.0155 (15)	0.0026 (11)
H14A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H14B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H14C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C15	0.0298 (12)	0.0328 (12)	0.0591 (17)	−0.0048 (10)	0.0005 (12)	−0.0141 (12)
H15A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H15B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H15C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C16	0.0197 (9)	0.0251 (9)	0.0307 (10)	−0.0022 (7)	0.0084 (8)	−0.0074 (8)
H16	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C17	0.0321 (12)	0.0353 (13)	0.0476 (14)	−0.0125 (10)	0.0155 (11)	−0.0182 (11)
H17A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H17B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H17C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C18	0.0429 (14)	0.0409 (13)	0.0275 (11)	−0.0033 (12)	0.0046 (10)	−0.0078 (10)
H18A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H18B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H18C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C19	0.0237 (10)	0.0265 (10)	0.0309 (10)	0.0069 (8)	0.0087 (8)	0.0078 (8)
H19	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C20	0.0440 (14)	0.0435 (14)	0.0281 (11)	0.0056 (12)	−0.0022 (10)	0.0078 (10)
H20A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H20B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H20C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C21	0.0482 (16)	0.0406 (15)	0.0502 (17)	0.0235 (13)	0.0180 (14)	0.0136 (12)
H21A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H21B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H21C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C22	0.0141 (8)	0.0244 (9)	0.0272 (9)	−0.0026 (7)	0.0045 (7)	0.0001 (8)
H22	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C23	0.0243 (10)	0.0294 (11)	0.0393 (12)	−0.0042 (8)	0.0048 (9)	−0.0078 (9)
H23A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H23B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H23C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C24	0.0207 (10)	0.0331 (11)	0.0490 (14)	−0.0053 (9)	0.0128 (10)	−0.0130 (11)
H24A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H24B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H24C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000

Geometric parameters (Å, º)

Rh—H	1.471 (19)	C12—H12a	1.07 (2)
Rh—Cl	2.4217 (7)	C12—H12b	1.13 (2)
Rh—B	1.966 (2)	C12—H12c	1.10 (2)
Rh—P1	2.3399 (7)	C13—H13	1.08 (2)
Rh—P2	2.3375 (7)	C13—C14	1.538 (4)
B—O1	1.417 (3)	C13—C15	1.529 (3)
B—O2	1.421 (3)	C14—H14a	1.06 (2)
P1—C7	1.866 (2)	C14—H14b	1.11 (2)
P1—C10	1.850 (2)	C14—H14c	1.06 (2)
P1—C13	1.882 (2)	C15—H15a	0.963 (19)
P2—C16	1.852 (2)	C15—H15b	1.07 (2)
P2—C19	1.859 (2)	C15—H15c	1.12 (2)
P2—C22	1.856 (2)	C16—H16	1.08 (2)
O1—C1	1.375 (2)	C16—C17	1.527 (3)
O2—C2	1.376 (2)	C16—C18	1.529 (4)
C1—C2	1.387 (3)	C17—H17a	1.13 (2)
C1—C6	1.381 (3)	C17—H17b	1.01 (2)
C2—C3	1.385 (3)	C17—H17c	1.019 (19)
C3—H3	1.12 (2)	C18—H18a	1.11 (2)
C3—C4	1.404 (3)	C18—H18b	1.07 (2)
C4—H4	1.17 (2)	C18—H18c	1.13 (2)
C4—C5	1.396 (4)	C19—H19	1.043 (19)
C5—H5	1.13 (2)	C19—C20	1.529 (4)
C5—C6	1.398 (3)	C19—C21	1.534 (3)
C6—H6	1.12 (2)	C20—H20a	1.20 (2)
C7—H7	1.10 (2)	C20—H20b	1.15 (2)
C7—C8	1.531 (3)	C20—H20c	1.08 (2)
C7—C9	1.529 (3)	C21—H21a	1.05 (2)
C8—H8a	0.98 (2)	C21—H21b	0.933 (19)
C8—H8b	1.22 (2)	C21—H21c	1.15 (2)
C8—H8c	1.03 (2)	C22—H22	1.01 (2)
C9—H9a	1.15 (2)	C22—C23	1.535 (3)
C9—H9b	1.008 (19)	C22—C24	1.531 (3)
C9—H9c	1.03 (2)	C23—H23a	1.05 (2)
C10—H10	1.16 (2)	C23—H23b	1.06 (2)
C10—C11	1.531 (3)	C23—H23c	1.16 (2)
C10—C12	1.542 (3)	C24—H24a	1.15 (2)
C11—H11a	1.12 (2)	C24—H24b	0.98 (2)
C11—H11b	1.03 (2)	C24—H24c	1.16 (2)
C11—H11c	1.12 (2)
Cl—Rh—H	157.5 (8)	H12b—C12—H12a	100.4 (16)
B—Rh—H	64.8 (8)	H12c—C12—C10	100.6 (11)
B—Rh—Cl	137.72 (7)	H12c—C12—H12a	119.8 (16)
P1—Rh—H	93.1 (8)	H12c—C12—H12b	110.4 (15)
P1—Rh—Cl	87.608 (18)	H13—C13—P1	106.1 (11)
P1—Rh—B	93.36 (7)	C14—C13—P1	115.41 (18)
P2—Rh—H	83.9 (8)	C14—C13—H13	105.9 (11)
P2—Rh—Cl	92.582 (18)	C15—C13—P1	110.69 (16)
P2—Rh—B	91.43 (6)	C15—C13—H13	109.5 (11)
P2—Rh—P1	172.661 (19)	C15—C13—C14	109.0 (2)
O1—B—Rh	120.31 (15)	H14a—C14—C13	114.0 (11)
O2—B—Rh	131.74 (17)	H14b—C14—C13	112.6 (11)
O2—B—O1	107.95 (17)	H14b—C14—H14a	105.6 (16)
C7—P1—Rh	119.78 (7)	H14c—C14—C13	113.3 (11)
C10—P1—Rh	114.39 (7)	H14c—C14—H14a	103.0 (16)
C10—P1—C7	105.60 (10)	H14c—C14—H14b	107.6 (16)
C13—P1—Rh	110.75 (7)	H15a—C15—C13	107.2 (12)
C13—P1—C7	99.92 (11)	H15b—C15—C13	110.0 (11)
C13—P1—C10	104.49 (10)	H15b—C15—H15a	106.0 (16)
C16—P2—Rh	117.62 (7)	H15c—C15—C13	111.0 (11)
C19—P2—Rh	114.44 (7)	H15c—C15—H15a	116.6 (16)
C19—P2—C16	102.66 (11)	H15c—C15—H15b	105.8 (16)
C22—P2—Rh	107.90 (7)	H16—C16—P2	111.7 (11)
C22—P2—C16	103.00 (9)	C17—C16—P2	110.53 (15)
C22—P2—C19	110.58 (10)	C17—C16—H16	104.4 (11)
C1—O1—B	106.96 (15)	C18—C16—P2	112.82 (16)
C2—O2—B	106.48 (16)	C18—C16—H16	106.7 (11)
C2—C1—O1	109.05 (16)	C18—C16—C17	110.3 (2)
C6—C1—O1	128.67 (18)	H17a—C17—C16	112.8 (11)
C6—C1—C2	122.27 (18)	H17b—C17—C16	117.7 (12)
C1—C2—O2	109.52 (16)	H17b—C17—H17a	98.7 (16)
C3—C2—O2	128.58 (19)	H17c—C17—C16	113.2 (11)
C3—C2—C1	121.86 (19)	H17c—C17—H17a	109.4 (15)
H3—C3—C2	121.9 (11)	H17c—C17—H17b	103.6 (16)
C4—C3—C2	116.3 (2)	H18a—C18—C16	113.3 (11)
C4—C3—H3	121.7 (11)	H18b—C18—C16	112.5 (11)
H4—C4—C3	115.1 (12)	H18b—C18—H18a	104.1 (16)
C5—C4—C3	121.8 (2)	H18c—C18—C16	104.4 (11)
C5—C4—H4	123.1 (12)	H18c—C18—H18a	104.2 (15)
H5—C5—C4	116.9 (11)	H18c—C18—H18b	118.4 (16)
C6—C5—C4	121.0 (2)	H19—C19—P2	97.6 (11)
C6—C5—H5	122.0 (11)	C20—C19—P2	112.61 (17)
C5—C6—C1	116.8 (2)	C20—C19—H19	105.6 (11)
H6—C6—C1	126.3 (11)	C21—C19—P2	117.15 (17)
H6—C6—C5	116.6 (11)	C21—C19—H19	113.0 (11)
H7—C7—P1	104.8 (11)	C21—C19—C20	109.8 (2)
C8—C7—P1	114.22 (14)	H20a—C20—C19	110.7 (11)
C8—C7—H7	111.1 (11)	H20b—C20—C19	112.9 (12)
C9—C7—P1	111.60 (16)	H20b—C20—H20a	93.0 (15)
C9—C7—H7	104.6 (10)	H20c—C20—C19	105.4 (11)
C9—C7—C8	110.06 (19)	H20c—C20—H20a	114.4 (15)
H8a—C8—C7	110.0 (12)	H20c—C20—H20b	120.2 (15)
H8b—C8—C7	108.0 (10)	H21a—C21—C19	113.2 (12)
H8b—C8—H8a	104.2 (15)	H21b—C21—C19	111.5 (12)
H8c—C8—C7	111.5 (12)	H21b—C21—H21a	106.6 (16)
H8c—C8—H8a	118.2 (17)	H21c—C21—C19	101.7 (11)
H8c—C8—H8b	104.1 (15)	H21c—C21—H21a	109.9 (15)
H9a—C9—C7	109.8 (10)	H21c—C21—H21b	114.1 (17)
H9b—C9—C7	113.9 (11)	H22—C22—P2	98.1 (12)
H9b—C9—H9a	104.1 (15)	C23—C22—P2	113.24 (15)
H9c—C9—C7	106.0 (11)	C23—C22—H22	105.6 (11)
H9c—C9—H9a	114.4 (16)	C24—C22—P2	116.39 (15)
H9c—C9—H9b	108.7 (16)	C24—C22—H22	112.2 (12)
H10—C10—P1	95.4 (11)	C24—C22—C23	110.25 (17)
C11—C10—P1	114.92 (16)	H23a—C23—C22	109.1 (11)
C11—C10—H10	109.6 (10)	H23b—C23—C22	107.7 (11)
C12—C10—P1	112.33 (14)	H23b—C23—H23a	116.1 (16)
C12—C10—H10	112.1 (10)	H23c—C23—C22	113.9 (11)
C12—C10—C11	111.54 (18)	H23c—C23—H23a	109.2 (15)
H11a—C11—C10	108.2 (11)	H23c—C23—H23b	100.8 (16)
H11b—C11—C10	114.5 (11)	H24a—C24—C22	114.3 (11)
H11b—C11—H11a	109.4 (16)	H24b—C24—C22	118.0 (12)
H11c—C11—C10	113.5 (11)	H24b—C24—H24a	93.2 (16)
H11c—C11—H11a	103.2 (15)	H24c—C24—C22	108.6 (12)
H11c—C11—H11b	107.5 (15)	H24c—C24—H24a	109.2 (16)
H12a—C12—C10	115.9 (12)	H24c—C24—H24b	112.7 (17)
H12b—C12—C10	109.8 (11)

(SITKUB_HAR)

Crystal data

C24H47BClO2P2Rh	F(000) = 1213.334
Mr = 578.77	Dx = 1.348 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
a = 11.228 (3) Å	Cell parameters from 925 reflections
b = 11.101 (3) Å	θ = 12.0–24.6°
c = 23.414 (7) Å	µ = 0.82 mm^−1
β = 102.28 (4)°	T = 120 K
V = 2851.6 (14) Å^3	Fragment, colourless
Z = 4	0.6 × 0.4 × 0.2 mm

Data collection

SMART 1K CCD area detector diffractometer	7021 reflections with I ≥ 2u(I)
Radiation source: fine-focus sealed tube	Rint = 0.029
Graphite monochromator	θmax = 29.1°, θmin = 1.8°
ω scans	h = −15→15
33082 measured reflections	k = −15→15
7624 independent reflections	l = −31→31

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.023	All H-atom parameters refined
wR(F^2) = 0.047	w = 1/[σ^2(Fo^2) + (0.0158P)^2 + 1.5535P] where P = (Fo^2 + 2Fc^2)/3
S = 1.06	(Δ/σ)max = 0.001
7624 reflections	Δρmax = 0.44 e Å^−3
688 parameters	Δρmin = −0.73 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Rh	0.311323 (9)	0.814891 (9)	0.861855 (4)	0.01631 (3)
H	0.3464 (18)	0.7839 (19)	0.9268 (8)	0.036 (5)*
Cl	0.32707 (3)	0.93355 (3)	0.776999 (16)	0.02808 (7)
B	0.21251 (13)	0.68029 (14)	0.88083 (6)	0.0197 (3)
P1	0.17685 (3)	0.96113 (3)	0.882947 (15)	0.01980 (7)
P2	0.46546 (3)	0.68313 (3)	0.848425 (15)	0.01864 (7)
O1	0.10459 (8)	0.64532 (9)	0.84072 (4)	0.02144 (19)
O2	0.22706 (9)	0.60330 (9)	0.93007 (4)	0.0241 (2)
C1	0.05451 (12)	0.55188 (12)	0.86615 (6)	0.0204 (2)
C2	0.12875 (12)	0.52619 (13)	0.92016 (6)	0.0228 (3)
C3	0.09920 (15)	0.43759 (15)	0.95640 (7)	0.0325 (3)
H3	0.158 (2)	0.421 (2)	1.0006 (9)	0.056 (7)
C4	−0.00953 (15)	0.37435 (15)	0.93523 (8)	0.0342 (3)
H4	−0.038 (3)	0.308 (2)	0.9627 (11)	0.074 (9)
C5	−0.08365 (14)	0.40012 (14)	0.88094 (7)	0.0286 (3)
H5	−0.1681 (17)	0.351 (2)	0.8679 (11)	0.053 (7)
C6	−0.05324 (13)	0.49071 (13)	0.84511 (7)	0.0241 (3)
H6	−0.1132 (17)	0.508 (2)	0.8019 (8)	0.036 (6)
C7	0.09985 (13)	0.93783 (14)	0.94521 (6)	0.0243 (3)
H7	0.0574 (18)	1.0270 (19)	0.9508 (9)	0.042 (6)
C8	0.00049 (14)	0.84075 (15)	0.93440 (7)	0.0284 (3)
H8A	0.038 (2)	0.753 (2)	0.9318 (13)	0.071 (9)
H8B	−0.070 (2)	0.858 (2)	0.8924 (9)	0.056 (8)
H8C	−0.0443 (19)	0.841 (2)	0.9711 (10)	0.052 (6)
C9	0.19144 (16)	0.91170 (18)	1.00213 (7)	0.0335 (3)
H9A	0.144 (2)	0.902 (2)	1.0392 (10)	0.049 (6)*
H9B	0.259 (2)	0.981 (3)	1.0153 (11)	0.066 (8)
H9C	0.240 (2)	0.830 (2)	0.9986 (10)	0.055 (7)
C10	0.05439 (13)	1.00360 (13)	0.81982 (6)	0.0240 (3)
H10	0.1079 (18)	1.055 (2)	0.7927 (9)	0.040 (6)
C11	−0.04338 (16)	1.08692 (17)	0.83513 (9)	0.0352 (4)
H11A	−0.095 (2)	1.127 (2)	0.7950 (10)	0.068 (8)
H11B	−0.004 (2)	1.159 (2)	0.8651 (13)	0.069 (8)
H11C	−0.108 (2)	1.036 (2)	0.8557 (11)	0.062 (8)
C12	−0.00193 (14)	0.89405 (15)	0.78406 (7)	0.0260 (3)
H12A	−0.045 (2)	0.833 (2)	0.8105 (10)	0.054 (7)
H12B	0.0682 (17)	0.8418 (19)	0.7695 (8)	0.033 (5)
H12C	−0.0687 (19)	0.921 (2)	0.7449 (10)	0.048 (6)
C13	0.25942 (14)	1.10616 (14)	0.90632 (8)	0.0304 (3)
H13	0.2183 (19)	1.1470 (19)	0.9407 (9)	0.045 (6)
C14	0.2507 (2)	1.20167 (18)	0.85833 (10)	0.0450 (4)
H14A	0.306 (2)	1.279 (2)	0.8752 (13)	0.083 (10)
H14B	0.157 (2)	1.232 (2)	0.8390 (13)	0.083 (10)
H14C	0.288 (2)	1.168 (2)	0.8220 (12)	0.065 (8)
C15	0.39403 (17)	1.08185 (18)	0.93308 (11)	0.0432 (4)
H15A	0.440 (2)	1.054 (3)	0.8977 (12)	0.068 (8)
H15B	0.407 (2)	1.011 (2)	0.9650 (10)	0.061 (8)
H15C	0.440 (3)	1.166 (2)	0.9526 (14)	0.098 (12)
C16	0.43398 (13)	0.58553 (14)	0.78281 (7)	0.0254 (3)
H16	0.5158 (17)	0.5300 (18)	0.7824 (9)	0.035 (5)
C17	0.32943 (16)	0.49897 (17)	0.78546 (9)	0.0376 (4)
H17A	0.2419 (18)	0.546 (2)	0.7840 (13)	0.080 (11)
H17B	0.340 (2)	0.442 (3)	0.8245 (11)	0.071 (9)
H17C	0.307 (2)	0.444 (2)	0.7458 (11)	0.063 (7)*
C18	0.40739 (19)	0.65671 (19)	0.72552 (7)	0.0378 (4)
H18A	0.392 (2)	0.595 (2)	0.6885 (9)	0.059 (7)
H18B	0.483 (3)	0.716 (2)	0.7209 (10)	0.070 (9)
H18C	0.325 (2)	0.710 (2)	0.7225 (10)	0.062 (8)
C19	0.51421 (14)	0.57327 (14)	0.90883 (7)	0.0272 (3)
H19	0.4282 (18)	0.532 (2)	0.9106 (10)	0.049 (6)
C20	0.5634 (2)	0.63479 (19)	0.96757 (8)	0.0405 (4)
H20A	0.580 (2)	0.570 (3)	1.0034 (10)	0.076 (9)
H20B	0.499 (3)	0.705 (3)	0.9779 (11)	0.081 (10)
H20C	0.652 (3)	0.674 (3)	0.9651 (12)	0.078 (9)
C21	0.6008 (2)	0.4726 (2)	0.89877 (10)	0.0468 (5)
H21A	0.690 (3)	0.507 (3)	0.8959 (14)	0.089 (12)
H21B	0.564 (3)	0.424 (3)	0.8594 (14)	0.094 (11)
H21C	0.614 (3)	0.408 (2)	0.9353 (11)	0.071 (9)
C22	0.59711 (12)	0.77490 (13)	0.83775 (6)	0.0225 (3)
H22	0.5536 (19)	0.826 (2)	0.7991 (9)	0.043 (6)
C23	0.63907 (15)	0.86717 (16)	0.88637 (8)	0.0317 (3)
H23A	0.694 (3)	0.826 (2)	0.9248 (10)	0.069 (8)
H23B	0.564 (2)	0.911 (3)	0.8984 (15)	0.097 (12)
H23C	0.697 (2)	0.934 (2)	0.8720 (11)	0.058 (7)
C24	0.70610 (14)	0.70566 (16)	0.82477 (9)	0.0332 (3)
H24A	0.768 (2)	0.770 (2)	0.8089 (11)	0.060 (7)
H24B	0.678 (2)	0.640 (3)	0.7904 (12)	0.071 (9)
H24C	0.760 (2)	0.663 (2)	0.8642 (12)	0.060 (7)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Rh	0.01393 (5)	0.01725 (5)	0.01802 (5)	0.00038 (3)	0.00400 (3)	0.00054 (4)
Cl	0.02373 (15)	0.03189 (18)	0.03092 (17)	0.00469 (13)	0.01099 (13)	0.01214 (14)
B	0.0167 (6)	0.0212 (7)	0.0220 (6)	−0.0003 (5)	0.0056 (5)	0.0009 (6)
P1	0.01786 (15)	0.01941 (15)	0.02244 (16)	0.00194 (12)	0.00496 (12)	−0.00074 (12)
P2	0.01514 (14)	0.01966 (15)	0.02151 (15)	0.00071 (12)	0.00476 (12)	−0.00030 (12)
O1	0.0196 (4)	0.0243 (5)	0.0200 (4)	−0.0018 (4)	0.0035 (4)	0.0014 (4)
O2	0.0210 (5)	0.0264 (5)	0.0236 (5)	−0.0021 (4)	0.0018 (4)	0.0052 (4)
C1	0.0195 (6)	0.0200 (6)	0.0226 (6)	−0.0003 (5)	0.0063 (5)	−0.0014 (5)
C2	0.0216 (6)	0.0220 (6)	0.0251 (7)	−0.0008 (5)	0.0053 (5)	0.0040 (5)
C3	0.0314 (8)	0.0306 (8)	0.0349 (8)	−0.0040 (6)	0.0056 (7)	0.0113 (7)
H3	0.065 (17)	0.057 (17)	0.037 (14)	−0.006 (14)	−0.006 (12)	0.032 (13)
C4	0.0320 (8)	0.0277 (8)	0.0436 (9)	−0.0060 (6)	0.0099 (7)	0.0097 (7)
H4	0.10 (2)	0.055 (17)	0.077 (19)	−0.023 (16)	0.042 (17)	0.035 (15)
C5	0.0244 (7)	0.0236 (7)	0.0397 (8)	−0.0042 (6)	0.0108 (6)	−0.0027 (6)
H5	0.009 (10)	0.056 (16)	0.09 (2)	−0.015 (11)	0.006 (11)	0.014 (14)
C6	0.0198 (6)	0.0242 (7)	0.0289 (7)	−0.0016 (5)	0.0067 (6)	−0.0033 (6)
H6	0.016 (11)	0.059 (16)	0.027 (12)	0.015 (10)	−0.006 (9)	0.002 (11)
C7	0.0241 (7)	0.0269 (7)	0.0232 (6)	0.0030 (6)	0.0077 (5)	−0.0037 (5)
H7	0.043 (14)	0.038 (13)	0.049 (14)	0.026 (11)	0.021 (11)	0.011 (11)
C8	0.0272 (7)	0.0327 (8)	0.0281 (7)	0.0000 (6)	0.0121 (6)	−0.0012 (6)
H8A	0.074 (19)	0.030 (14)	0.13 (3)	−0.012 (13)	0.068 (18)	−0.041 (15)
H8B	0.050 (15)	0.10 (2)	0.013 (11)	−0.036 (15)	−0.006 (11)	0.008 (12)
H8C	0.040 (14)	0.072 (18)	0.052 (15)	0.005 (13)	0.029 (12)	0.002 (13)
C9	0.0338 (8)	0.0435 (10)	0.0229 (7)	0.0035 (8)	0.0051 (6)	−0.0045 (7)
H9B	0.041 (15)	0.09 (2)	0.060 (18)	−0.021 (15)	−0.004 (13)	−0.023 (16)
H9C	0.056 (16)	0.063 (17)	0.040 (15)	0.034 (14)	−0.001 (12)	0.002 (13)
C10	0.0210 (6)	0.0253 (7)	0.0255 (7)	0.0055 (5)	0.0041 (5)	0.0041 (5)
H10	0.037 (13)	0.052 (15)	0.033 (12)	−0.004 (11)	0.011 (10)	0.017 (11)
C11	0.0298 (8)	0.0355 (9)	0.0397 (9)	0.0151 (7)	0.0063 (7)	0.0011 (8)
H11A	0.073 (19)	0.08 (2)	0.041 (15)	0.031 (16)	−0.013 (14)	0.005 (14)
H11B	0.051 (17)	0.044 (16)	0.11 (2)	0.008 (14)	0.004 (16)	−0.030 (16)
H11C	0.053 (16)	0.061 (18)	0.09 (2)	0.025 (14)	0.050 (15)	0.032 (15)
C12	0.0206 (7)	0.0318 (8)	0.0244 (7)	0.0008 (6)	0.0023 (6)	0.0024 (6)
H12A	0.072 (18)	0.041 (15)	0.058 (16)	0.009 (13)	0.035 (14)	0.010 (12)
H12B	0.030 (11)	0.047 (13)	0.030 (12)	0.005 (10)	0.022 (10)	−0.008 (10)
H12C	0.037 (13)	0.045 (15)	0.054 (15)	0.011 (12)	−0.006 (12)	0.004 (12)
C13	0.0286 (7)	0.0218 (7)	0.0409 (9)	−0.0008 (6)	0.0075 (7)	−0.0056 (6)
H13	0.043 (13)	0.046 (14)	0.056 (15)	−0.007 (11)	0.029 (12)	−0.035 (12)
C14	0.0515 (12)	0.0264 (9)	0.0588 (12)	−0.0084 (8)	0.0155 (10)	0.0029 (8)
H14A	0.08 (2)	0.036 (16)	0.12 (3)	−0.031 (16)	−0.006 (19)	0.020 (16)
H14B	0.031 (15)	0.06 (2)	0.13 (3)	0.014 (14)	−0.029 (16)	0.021 (18)
H14C	0.08 (2)	0.037 (16)	0.09 (2)	−0.010 (14)	0.039 (17)	−0.029 (15)
C15	0.0289 (8)	0.0341 (9)	0.0619 (13)	−0.0053 (7)	−0.0008 (8)	−0.0153 (9)
H15A	0.040 (15)	0.08 (2)	0.09 (2)	0.004 (15)	0.031 (15)	−0.003 (18)
H15B	0.074 (19)	0.045 (16)	0.053 (17)	0.014 (14)	−0.010 (14)	0.020 (13)
H15C	0.08 (2)	0.047 (18)	0.14 (3)	−0.008 (16)	−0.04 (2)	−0.049 (19)
C16	0.0207 (6)	0.0262 (7)	0.0306 (7)	−0.0022 (5)	0.0085 (6)	−0.0077 (6)
H16	0.025 (11)	0.026 (12)	0.058 (15)	0.007 (9)	0.013 (10)	−0.001 (10)
C17	0.0309 (8)	0.0359 (9)	0.0491 (10)	−0.0136 (7)	0.0156 (8)	−0.0194 (8)
H17A	0.013 (12)	0.09 (2)	0.14 (3)	0.002 (13)	0.007 (14)	−0.08 (2)
H17B	0.09 (2)	0.08 (2)	0.046 (16)	−0.019 (17)	0.021 (15)	0.031 (15)
C18	0.0429 (10)	0.0428 (10)	0.0260 (8)	−0.0040 (8)	0.0037 (7)	−0.0077 (7)
H18A	0.09 (2)	0.054 (16)	0.031 (13)	−0.018 (15)	0.009 (13)	−0.025 (12)
H18B	0.09 (2)	0.063 (18)	0.052 (17)	−0.042 (17)	0.000 (15)	0.019 (14)
H18C	0.046 (16)	0.08 (2)	0.054 (17)	0.020 (15)	−0.014 (13)	0.023 (14)
C19	0.0239 (7)	0.0273 (7)	0.0314 (7)	0.0068 (6)	0.0078 (6)	0.0076 (6)
H19	0.028 (12)	0.053 (16)	0.069 (17)	−0.005 (11)	0.016 (11)	0.015 (13)
C20	0.0441 (10)	0.0429 (10)	0.0298 (8)	0.0058 (9)	−0.0030 (8)	0.0092 (8)
H20A	0.07 (2)	0.12 (3)	0.037 (15)	0.017 (18)	0.003 (14)	0.037 (17)
H20B	0.09 (2)	0.09 (2)	0.059 (19)	0.072 (19)	−0.001 (16)	0.021 (16)
H20C	0.09 (2)	0.07 (2)	0.07 (2)	−0.014 (18)	−0.006 (17)	0.023 (16)
C21	0.0480 (12)	0.0429 (11)	0.0537 (12)	0.0255 (9)	0.0200 (10)	0.0160 (10)
H21A	0.061 (19)	0.08 (2)	0.15 (3)	0.053 (17)	0.07 (2)	0.07 (2)
H21B	0.11 (3)	0.09 (3)	0.08 (2)	0.04 (2)	0.02 (2)	−0.04 (2)
H21C	0.12 (2)	0.031 (14)	0.063 (18)	0.046 (16)	0.029 (17)	0.033 (13)
C22	0.0159 (6)	0.0242 (6)	0.0275 (7)	−0.0016 (5)	0.0050 (5)	−0.0003 (5)
H22	0.040 (13)	0.057 (16)	0.033 (12)	0.009 (11)	0.013 (10)	0.030 (11)
C23	0.0241 (7)	0.0293 (8)	0.0417 (9)	−0.0054 (6)	0.0068 (7)	−0.0096 (7)
H23A	0.09 (2)	0.062 (19)	0.040 (15)	0.000 (16)	−0.016 (15)	0.013 (13)
H23B	0.039 (15)	0.07 (2)	0.19 (3)	0.005 (15)	0.037 (19)	−0.07 (2)
H23C	0.039 (14)	0.060 (17)	0.070 (18)	−0.029 (13)	0.002 (13)	0.006 (14)
C24	0.0194 (7)	0.0343 (9)	0.0483 (10)	−0.0032 (6)	0.0125 (7)	−0.0105 (8)
H24A	0.034 (14)	0.053 (16)	0.10 (2)	−0.028 (13)	0.031 (14)	−0.006 (15)
H24B	0.061 (18)	0.08 (2)	0.09 (2)	−0.002 (16)	0.053 (16)	−0.043 (17)
H24C	0.051 (16)	0.047 (17)	0.08 (2)	0.007 (13)	0.009 (15)	0.024 (15)

Geometric parameters (Å, º)

Rh—H	1.526 (19)	C12—H12a	1.10 (2)
Rh—Cl	2.4214 (6)	C12—H12b	1.089 (18)
Rh—B	1.9673 (16)	C12—H12c	1.10 (2)
Rh—P1	2.3401 (6)	C13—H13	1.107 (18)
Rh—P2	2.3377 (6)	C13—C14	1.533 (3)
B—O1	1.4202 (18)	C13—C15	1.532 (2)
B—O2	1.4165 (18)	C14—H14a	1.08 (2)
P1—C7	1.8643 (16)	C14—H14b	1.11 (2)
P1—C10	1.8528 (16)	C14—H14c	1.09 (2)
P1—C13	1.8803 (16)	C15—H15a	1.11 (3)
P2—C16	1.8516 (15)	C15—H15b	1.08 (2)
P2—C19	1.8596 (16)	C15—H15c	1.11 (2)
P2—C22	1.8554 (14)	C16—H16	1.108 (18)
O1—C1	1.3744 (16)	C16—C17	1.528 (2)
O2—C2	1.3770 (17)	C16—C18	1.530 (2)
C1—C2	1.388 (2)	C17—H17a	1.10 (2)
C1—C6	1.3834 (19)	C17—H17b	1.10 (2)
C2—C3	1.385 (2)	C17—H17c	1.10 (3)
C3—H3	1.12 (2)	C18—H18a	1.09 (2)
C3—C4	1.404 (2)	C18—H18b	1.10 (2)
C4—H4	1.08 (2)	C18—H18c	1.09 (2)
C4—C5	1.393 (2)	C19—H19	1.08 (2)
C5—H5	1.082 (19)	C19—C20	1.530 (3)
C5—C6	1.398 (2)	C19—C21	1.532 (2)
C6—H6	1.107 (18)	C20—H20a	1.09 (2)
C7—H7	1.119 (19)	C20—H20b	1.12 (3)
C7—C8	1.533 (2)	C20—H20c	1.10 (3)
C7—C9	1.528 (2)	C21—H21a	1.08 (3)
C8—H8a	1.07 (2)	C21—H21b	1.07 (3)
C8—H8b	1.14 (2)	C21—H21c	1.10 (2)
C8—H8c	1.09 (2)	C22—H22	1.093 (19)
C9—H9a	1.12 (2)	C22—C23	1.529 (2)
C9—H9b	1.08 (2)	C22—C24	1.529 (2)
C9—H9c	1.07 (2)	C23—H23a	1.08 (2)
C10—H10	1.119 (19)	C23—H23b	1.06 (2)
C10—C11	1.535 (2)	C23—H23c	1.08 (2)
C10—C12	1.535 (2)	C24—H24a	1.11 (2)
C11—H11a	1.09 (2)	C24—H24b	1.08 (3)
C11—H11b	1.10 (2)	C24—H24c	1.10 (2)
C11—H11c	1.11 (2)
Cl—Rh—H	153.0 (8)	H12b—C12—H12a	106.5 (16)
B—Rh—H	69.1 (8)	H12c—C12—C10	111.5 (12)
B—Rh—Cl	137.86 (4)	H12c—C12—H12a	109.6 (17)
P1—Rh—H	89.3 (8)	H12c—C12—H12b	107.3 (15)
P1—Rh—Cl	87.637 (12)	H13—C13—P1	107.8 (11)
P1—Rh—B	93.39 (4)	C14—C13—P1	115.35 (13)
P2—Rh—H	87.2 (8)	C14—C13—H13	106.2 (12)
P2—Rh—Cl	92.559 (12)	C15—C13—P1	110.53 (11)
P2—Rh—B	91.39 (4)	C15—C13—H13	107.6 (12)
P2—Rh—P1	172.650 (13)	C15—C13—C14	108.98 (16)
O1—B—Rh	120.08 (10)	H14a—C14—C13	109.7 (15)
O2—B—Rh	132.00 (10)	H14b—C14—C13	114.5 (16)
O2—B—O1	107.92 (11)	H14b—C14—H14a	109 (2)
C7—P1—Rh	119.74 (5)	H14c—C14—C13	111.0 (14)
C10—P1—Rh	114.26 (5)	H14c—C14—H14a	106 (2)
C10—P1—C7	105.68 (6)	H14c—C14—H14b	106 (2)
C13—P1—Rh	110.80 (5)	H15a—C15—C13	108.8 (14)
C13—P1—C7	99.97 (7)	H15b—C15—C13	112.7 (14)
C13—P1—C10	104.52 (7)	H15b—C15—H15a	107 (2)
C16—P2—Rh	117.49 (5)	H15c—C15—C13	110.5 (15)
C19—P2—Rh	114.50 (5)	H15c—C15—H15a	107 (2)
C19—P2—C16	102.75 (7)	H15c—C15—H15b	110 (2)
C22—P2—Rh	107.96 (5)	H16—C16—P2	108.6 (11)
C22—P2—C16	103.09 (6)	C17—C16—P2	110.30 (10)
C22—P2—C19	110.40 (7)	C17—C16—H16	107.2 (10)
C1—O1—B	106.86 (10)	C18—C16—P2	113.10 (11)
C2—O2—B	106.76 (10)	C18—C16—H16	106.7 (11)
C2—C1—O1	109.15 (11)	C18—C16—C17	110.60 (14)
C6—C1—O1	128.57 (13)	H17a—C17—C16	112.9 (15)
C6—C1—C2	122.26 (13)	H17b—C17—C16	116.5 (14)
C1—C2—O2	109.29 (11)	H17b—C17—H17a	104 (2)
C3—C2—O2	128.77 (13)	H17c—C17—C16	110.9 (13)
C3—C2—C1	121.91 (13)	H17c—C17—H17a	101.2 (17)
H3—C3—C2	120.8 (12)	H17c—C17—H17b	110 (2)
C4—C3—C2	116.26 (15)	H18a—C18—C16	110.0 (13)
C4—C3—H3	122.9 (12)	H18b—C18—C16	112.6 (13)
H4—C4—C3	118.8 (15)	H18b—C18—H18a	107.3 (19)
C5—C4—C3	121.69 (14)	H18c—C18—C16	110.1 (13)
C5—C4—H4	119.4 (15)	H18c—C18—H18a	107.3 (19)
H5—C5—C4	118.0 (12)	H18c—C18—H18b	109 (2)
C6—C5—C4	121.38 (14)	H19—C19—P2	100.8 (12)
C6—C5—H5	120.5 (12)	C20—C19—P2	112.50 (12)
C5—C6—C1	116.50 (14)	C20—C19—H19	108.2 (13)
H6—C6—C1	123.9 (11)	C21—C19—P2	117.08 (12)
H6—C6—C5	119.5 (11)	C21—C19—H19	107.3 (12)
H7—C7—P1	104.4 (10)	C21—C19—C20	110.14 (16)
C8—C7—P1	114.24 (10)	H20a—C20—C19	111.4 (16)
C8—C7—H7	109.2 (11)	H20b—C20—C19	112.3 (14)
C9—C7—P1	111.74 (10)	H20b—C20—H20a	108.0 (19)
C9—C7—H7	106.9 (11)	H20c—C20—C19	106.8 (15)
C9—C7—C8	109.98 (13)	H20c—C20—H20a	107.0 (19)
H8a—C8—C7	111.5 (13)	H20c—C20—H20b	111 (2)
H8b—C8—C7	111.8 (12)	H21a—C21—C19	112.2 (15)
H8b—C8—H8a	108 (2)	H21b—C21—C19	111.1 (16)
H8c—C8—C7	108.2 (13)	H21b—C21—H21a	108 (2)
H8c—C8—H8a	107.6 (19)	H21c—C21—C19	110.3 (13)
H8c—C8—H8b	109.2 (16)	H21c—C21—H21a	107 (2)
H9a—C9—C7	110.8 (12)	H21c—C21—H21b	108 (2)
H9b—C9—C7	114.5 (14)	H22—C22—P2	99.8 (11)
H9b—C9—H9a	105.6 (18)	C23—C22—P2	113.29 (10)
H9c—C9—C7	110.6 (12)	C23—C22—H22	106.2 (12)
H9c—C9—H9a	108.0 (17)	C24—C22—P2	116.42 (11)
H9c—C9—H9b	107.0 (19)	C24—C22—H22	109.5 (11)
H10—C10—P1	100.7 (10)	C24—C22—C23	110.59 (12)
C11—C10—P1	114.41 (11)	H23a—C23—C22	111.8 (14)
C11—C10—H10	108.9 (11)	H23b—C23—C22	111.8 (14)
C12—C10—P1	112.55 (10)	H23b—C23—H23a	109 (2)
C12—C10—H10	107.6 (11)	H23c—C23—C22	109.5 (13)
C12—C10—C11	111.89 (13)	H23c—C23—H23a	105.6 (18)
H11a—C11—C10	108.8 (14)	H23c—C23—H23b	109 (2)
H11b—C11—C10	112.5 (13)	H24a—C24—C22	109.2 (13)
H11b—C11—H11a	109 (2)	H24b—C24—C22	111.3 (13)
H11c—C11—C10	111.2 (12)	H24b—C24—H24a	106.7 (18)
H11c—C11—H11a	107.6 (19)	H24c—C24—C22	111.9 (14)
H11c—C11—H11b	108 (2)	H24c—C24—H24a	106.6 (18)
H12a—C12—C10	111.2 (13)	H24c—C24—H24b	111 (2)
H12b—C12—C10	110.6 (11)

(SITKUB_HAR_NoMoRe_1)

Crystal data

C24H47BClO2P2Rh	F(000) = 1213.281
Mr = 578.77	Dx = 1.348 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
a = 11.228 (3) Å	Cell parameters from 925 reflections
b = 11.101 (3) Å	θ = 12.0–24.6°
c = 23.414 (7) Å	µ = 0.82 mm^−1
β = 102.28 (4)°	T = 120 K
V = 2851.6 (14) Å^3	Fragment, colourless
Z = 4	0.6 × 0.4 × 0.2 mm

Data collection

SMART 1K CCD area detector diffractometer	7021 reflections with I ≥ 2u(I)
Radiation source: fine-focus sealed tube	Rint = 0.029
Graphite monochromator	θmax = 29.1°, θmin = 1.8°
ω scans	h = −15→15
33082 measured reflections	k = −15→15
7624 independent reflections	l = −31→31

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.026	Only H-atom coordinates refined
wR(F^2) = 0.096	w = 1/[σ^2(Fo^2) + (0.1P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 0.83	(Δ/σ)max = 0.001
7624 reflections	Δρmax = 0.42 e Å^−3
421 parameters	Δρmin = −0.74 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Rh	0.311338 (9)	0.814889 (9)	0.861862 (5)	0.01651 (6)
H	0.344 (2)	0.776 (2)	0.9248 (10)	0.033687
Cl	0.32708 (4)	0.93356 (4)	0.777009 (18)	0.02814 (9)
B	0.21232 (17)	0.68036 (14)	0.88076 (8)	0.0197 (3)
P1	0.17683 (3)	0.96115 (3)	0.882931 (17)	0.01977 (9)
P2	0.46543 (4)	0.68313 (3)	0.848421 (18)	0.01857 (9)
O1	0.10463 (10)	0.64528 (10)	0.84065 (5)	0.0214 (2)
O2	0.22699 (10)	0.60328 (10)	0.93011 (5)	0.0240 (2)
C1	0.05450 (14)	0.55179 (13)	0.86612 (7)	0.0204 (3)
C2	0.12879 (14)	0.52622 (14)	0.91998 (7)	0.0225 (3)
C3	0.09894 (17)	0.43779 (17)	0.95634 (8)	0.0324 (4)
H3	0.157 (3)	0.423 (3)	0.9999 (13)	0.055786
C4	−0.00943 (18)	0.37431 (16)	0.93528 (9)	0.0344 (4)
H4	−0.042 (3)	0.308 (3)	0.9667 (16)	0.058138
C5	−0.08388 (16)	0.40011 (15)	0.88090 (8)	0.0284 (3)
H5	−0.169 (3)	0.344 (3)	0.8703 (13)	0.048448
C6	−0.05313 (14)	0.49067 (15)	0.84514 (7)	0.0237 (3)
H6	−0.112 (2)	0.504 (3)	0.8028 (12)	0.043466
C7	0.09980 (15)	0.93787 (15)	0.94527 (7)	0.0247 (3)
H7	0.054 (3)	1.025 (2)	0.9504 (12)	0.041514
C8	0.00023 (16)	0.84086 (17)	0.93431 (8)	0.0283 (3)
H8A	0.038 (3)	0.758 (3)	0.9306 (14)	0.052999
H8B	−0.073 (3)	0.863 (3)	0.8911 (14)	0.055194
H8C	−0.044 (3)	0.843 (3)	0.9716 (13)	0.050208
C9	0.19109 (18)	0.91160 (19)	1.00211 (8)	0.0335 (4)
H9A	0.145 (3)	0.904 (3)	1.0424 (13)	0.058991
H9B	0.254 (3)	0.982 (3)	1.0164 (13)	0.061030
H9C	0.238 (3)	0.834 (3)	0.9961 (13)	0.056017
C10	0.05454 (14)	1.00379 (15)	0.81984 (7)	0.0239 (3)
H10	0.113 (2)	1.056 (2)	0.7933 (12)	0.037249
C11	−0.04329 (17)	1.08685 (18)	0.83497 (9)	0.0349 (4)
H11A	−0.099 (3)	1.126 (3)	0.7945 (13)	0.057304
H11B	−0.006 (3)	1.160 (3)	0.8659 (15)	0.054709
H11C	−0.111 (3)	1.034 (3)	0.8520 (15)	0.057309
C12	−0.00191 (14)	0.89383 (16)	0.78404 (7)	0.0260 (3)
H12A	−0.041 (3)	0.834 (3)	0.8101 (14)	0.053644
H12B	0.070 (3)	0.844 (3)	0.7692 (14)	0.049628
H12C	−0.061 (3)	0.926 (3)	0.7453 (13)	0.050188
C13	0.25947 (16)	1.10631 (15)	0.90638 (8)	0.0303 (3)
H13	0.219 (3)	1.143 (3)	0.9390 (13)	0.047655
C14	0.2508 (2)	1.20198 (19)	0.85841 (12)	0.0456 (5)
H14A	0.305 (3)	1.275 (3)	0.8738 (15)	0.072451
H14B	0.156 (3)	1.232 (3)	0.8388 (17)	0.068641
H14C	0.289 (3)	1.170 (3)	0.8237 (16)	0.065301
C15	0.39402 (19)	1.0820 (2)	0.93305 (12)	0.0431 (5)
H15A	0.441 (3)	1.046 (3)	0.9001 (15)	0.056581
H15B	0.403 (3)	1.012 (3)	0.9656 (14)	0.057565
H15C	0.442 (3)	1.168 (3)	0.9552 (17)	0.071268
C16	0.43415 (15)	0.58540 (15)	0.78284 (7)	0.0255 (3)
H16	0.513 (2)	0.531 (2)	0.7804 (12)	0.044142
C17	0.32951 (18)	0.49883 (19)	0.78538 (10)	0.0375 (4)
H17A	0.242 (3)	0.541 (3)	0.7882 (14)	0.051834
H17B	0.338 (3)	0.443 (3)	0.8230 (16)	0.073388
H17C	0.311 (3)	0.446 (3)	0.7465 (17)	0.071258
C18	0.4075 (2)	0.6567 (2)	0.72563 (8)	0.0375 (4)
H18A	0.388 (3)	0.597 (3)	0.6862 (13)	0.066228
H18B	0.488 (3)	0.718 (3)	0.7231 (14)	0.064530
H18C	0.322 (3)	0.707 (3)	0.7263 (14)	0.058895
C19	0.51406 (15)	0.57333 (15)	0.90890 (8)	0.0269 (3)
H19	0.425 (2)	0.535 (2)	0.9106 (12)	0.042480
C20	0.5636 (2)	0.6348 (2)	0.96769 (9)	0.0399 (4)
H20A	0.579 (3)	0.566 (3)	1.0036 (14)	0.069096
H20B	0.500 (4)	0.704 (3)	0.9806 (16)	0.074535
H20C	0.647 (3)	0.675 (3)	0.9618 (16)	0.071186
C21	0.6008 (2)	0.4725 (2)	0.89879 (11)	0.0468 (5)
H21A	0.684 (3)	0.500 (3)	0.8941 (18)	0.080510
H21B	0.560 (4)	0.426 (3)	0.8607 (18)	0.089113
H21C	0.610 (3)	0.405 (3)	0.9356 (17)	0.070545
C22	0.59697 (13)	0.77488 (15)	0.83774 (7)	0.0222 (3)
H22	0.555 (3)	0.825 (2)	0.8004 (12)	0.037850
C23	0.63924 (16)	0.86735 (17)	0.88638 (9)	0.0316 (4)
H23A	0.692 (3)	0.829 (3)	0.9265 (14)	0.053459
H23B	0.559 (3)	0.910 (3)	0.8953 (15)	0.059590
H23C	0.698 (3)	0.933 (3)	0.8740 (13)	0.052620
C24	0.70616 (17)	0.70578 (18)	0.82479 (10)	0.0334 (4)
H24A	0.765 (3)	0.765 (3)	0.8046 (15)	0.056677
H24B	0.682 (3)	0.648 (3)	0.7922 (14)	0.055202
H24C	0.763 (3)	0.665 (3)	0.8657 (15)	0.053350

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Rh	0.01433 (8)	0.01740 (8)	0.01809 (8)	0.00040 (3)	0.00412 (5)	0.00055 (3)
H	0.035000	0.040000	0.025000	0.003000	0.004000	0.001000
Cl	0.02401 (18)	0.0319 (2)	0.03085 (19)	0.00456 (14)	0.01096 (15)	0.01201 (15)
B	0.0177 (8)	0.0210 (8)	0.0215 (8)	−0.0001 (5)	0.0067 (6)	0.0006 (5)
P1	0.01814 (17)	0.01924 (17)	0.02226 (18)	0.00199 (13)	0.00503 (14)	−0.00065 (13)
P2	0.01541 (19)	0.01951 (19)	0.02116 (19)	0.00088 (11)	0.00476 (15)	−0.00025 (12)
O1	0.0201 (5)	0.0242 (5)	0.0194 (5)	−0.0016 (4)	0.0033 (4)	0.0012 (4)
O2	0.0210 (5)	0.0264 (5)	0.0231 (5)	−0.0021 (4)	0.0016 (4)	0.0050 (4)
C1	0.0203 (7)	0.0197 (6)	0.0221 (7)	−0.0006 (5)	0.0062 (5)	−0.0018 (5)
C2	0.0216 (7)	0.0213 (7)	0.0246 (7)	−0.0018 (5)	0.0051 (6)	0.0038 (5)
C3	0.0312 (9)	0.0308 (9)	0.0345 (9)	−0.0030 (7)	0.0052 (7)	0.0106 (7)
H3	0.049000	0.071000	0.043000	−0.015000	0.000000	0.025000
C4	0.0330 (9)	0.0275 (8)	0.0438 (10)	−0.0057 (7)	0.0107 (8)	0.0105 (7)
H4	0.056000	0.059000	0.061000	−0.022000	0.016000	0.021000
C5	0.0257 (7)	0.0233 (7)	0.0382 (9)	−0.0047 (6)	0.0114 (7)	−0.0026 (6)
H5	0.039000	0.047000	0.060000	−0.021000	0.012000	−0.005000
C6	0.0199 (7)	0.0247 (7)	0.0270 (7)	−0.0010 (6)	0.0058 (6)	−0.0029 (6)
H6	0.038000	0.052000	0.036000	−0.011000	−0.002000	−0.001000
C7	0.0247 (7)	0.0275 (8)	0.0233 (7)	0.0033 (6)	0.0085 (6)	−0.0039 (6)
H7	0.047000	0.035000	0.047000	0.008000	0.020000	−0.005000
C8	0.0283 (8)	0.0311 (8)	0.0284 (8)	0.0005 (7)	0.0128 (7)	−0.0009 (7)
H8A	0.055000	0.035000	0.077000	−0.001000	0.032000	−0.009000
H8B	0.037000	0.077000	0.048000	−0.011000	0.001000	0.011000
H8C	0.056000	0.057000	0.047000	−0.003000	0.032000	−0.002000
C9	0.0352 (9)	0.0417 (10)	0.0232 (7)	0.0035 (8)	0.0056 (7)	−0.0044 (7)
H9A	0.065000	0.084000	0.031000	0.007000	0.017000	−0.001000
H9B	0.054000	0.080000	0.044000	−0.016000	−0.001000	−0.011000
H9C	0.060000	0.063000	0.042000	0.025000	0.004000	0.002000
C10	0.0210 (7)	0.0249 (7)	0.0252 (7)	0.0054 (6)	0.0033 (6)	0.0044 (6)
H10	0.039000	0.036000	0.038000	−0.000000	0.011000	0.008000
C11	0.0286 (8)	0.0349 (9)	0.0407 (10)	0.0152 (7)	0.0064 (7)	0.0017 (8)
H11A	0.052000	0.060000	0.054000	0.028000	−0.002000	0.006000
H11B	0.052000	0.048000	0.061000	0.015000	0.005000	−0.016000
H11C	0.043000	0.065000	0.071000	0.013000	0.028000	0.004000
C12	0.0210 (7)	0.0314 (8)	0.0245 (7)	0.0010 (6)	0.0021 (6)	0.0027 (6)
H12A	0.060000	0.059000	0.042000	−0.025000	0.011000	0.004000
H12B	0.039000	0.048000	0.062000	0.005000	0.011000	−0.018000
H12C	0.046000	0.052000	0.043000	0.006000	−0.012000	0.004000
C13	0.0284 (8)	0.0213 (7)	0.0415 (9)	0.0004 (6)	0.0077 (7)	−0.0057 (6)
H13	0.052000	0.038000	0.058000	−0.002000	0.023000	−0.016000
C14	0.0516 (13)	0.0261 (9)	0.0612 (14)	−0.0084 (9)	0.0168 (12)	0.0019 (9)
H14A	0.083000	0.037000	0.096000	−0.022000	0.016000	0.003000
H14B	0.062000	0.044000	0.096000	0.008000	0.008000	0.020000
H14C	0.082000	0.058000	0.062000	−0.010000	0.029000	0.008000
C15	0.0297 (9)	0.0341 (10)	0.0614 (13)	−0.0057 (8)	0.0002 (9)	−0.0144 (9)
H15A	0.040000	0.057000	0.077000	−0.003000	0.022000	−0.011000
H15B	0.046000	0.059000	0.060000	0.000000	−0.006000	0.001000
H15C	0.054000	0.054000	0.099000	−0.017000	0.001000	−0.034000
C16	0.0204 (7)	0.0256 (7)	0.0317 (8)	−0.0024 (6)	0.0085 (6)	−0.0074 (6)
H16	0.034000	0.045000	0.055000	0.008000	0.013000	−0.014000
C17	0.0308 (9)	0.0363 (10)	0.0483 (11)	−0.0127 (7)	0.0146 (8)	−0.0177 (8)
H17A	0.031000	0.057000	0.069000	−0.005000	0.014000	−0.020000
H17B	0.076000	0.059000	0.080000	−0.029000	0.005000	0.018000
H17C	0.061000	0.066000	0.092000	−0.022000	0.028000	−0.053000
C18	0.0426 (11)	0.0417 (10)	0.0266 (8)	−0.0036 (9)	0.0038 (7)	−0.0080 (7)
H18A	0.087000	0.074000	0.038000	−0.008000	0.014000	−0.025000
H18B	0.068000	0.087000	0.041000	−0.030000	0.017000	0.001000
H18C	0.063000	0.067000	0.043000	0.014000	0.003000	0.004000
C19	0.0244 (7)	0.0270 (8)	0.0305 (8)	0.0065 (6)	0.0083 (6)	0.0077 (6)
H19	0.031000	0.043000	0.056000	0.001000	0.015000	0.016000
C20	0.0440 (11)	0.0425 (11)	0.0288 (8)	0.0062 (9)	−0.0024 (8)	0.0080 (8)
H20A	0.080000	0.081000	0.041000	0.004000	0.001000	0.027000
H20B	0.102000	0.071000	0.042000	0.031000	−0.004000	−0.011000
H20C	0.054000	0.077000	0.070000	−0.016000	−0.015000	0.020000
C21	0.0483 (12)	0.0413 (11)	0.0547 (13)	0.0238 (10)	0.0199 (11)	0.0167 (10)
H21A	0.063000	0.079000	0.116000	0.038000	0.056000	0.040000
H21B	0.122000	0.052000	0.087000	0.037000	0.008000	−0.014000
H21C	0.080000	0.058000	0.082000	0.036000	0.036000	0.038000
C22	0.0157 (6)	0.0246 (7)	0.0265 (7)	−0.0027 (5)	0.0044 (5)	0.0009 (6)
H22	0.033000	0.045000	0.035000	−0.001000	0.006000	0.012000
C23	0.0242 (8)	0.0299 (9)	0.0401 (9)	−0.0050 (6)	0.0056 (7)	−0.0086 (7)
H23A	0.057000	0.057000	0.040000	−0.009000	−0.004000	−0.003000
H23B	0.045000	0.056000	0.082000	−0.000000	0.023000	−0.030000
H23C	0.049000	0.042000	0.068000	−0.018000	0.015000	−0.003000
C24	0.0206 (8)	0.0338 (9)	0.0483 (11)	−0.0047 (7)	0.0128 (7)	−0.0118 (8)
H24A	0.037000	0.058000	0.084000	−0.008000	0.033000	−0.004000
H24B	0.040000	0.062000	0.067000	−0.004000	0.019000	−0.032000
H24C	0.037000	0.055000	0.065000	0.014000	0.004000	0.002000

Geometric parameters (Å, º)

Rh—H	1.51 (2)	C12—H12A	1.06 (3)
Rh—Cl	2.4214 (7)	C12—H12B	1.09 (3)
Rh—B	1.9676 (17)	C12—H12C	1.07 (3)
Rh—P1	2.3404 (6)	C13—H13	1.05 (3)
Rh—P2	2.3374 (6)	C13—C14	1.534 (3)
B—O1	1.419 (2)	C13—C15	1.531 (3)
B—O2	1.419 (2)	C14—H14A	1.03 (3)
P1—C7	1.8661 (18)	C14—H14B	1.12 (3)
P1—C10	1.8517 (18)	C14—H14C	1.06 (4)
P1—C13	1.8822 (18)	C15—H15A	1.10 (3)
P2—C16	1.8517 (17)	C15—H15B	1.08 (3)
P2—C19	1.8601 (17)	C15—H15C	1.16 (3)
P2—C22	1.8543 (16)	C16—H16	1.08 (2)
O1—C1	1.3756 (18)	C16—C17	1.529 (2)
O2—C2	1.3757 (18)	C16—C18	1.530 (3)
C1—C2	1.385 (2)	C17—H17A	1.11 (3)
C1—C6	1.382 (2)	C17—H17B	1.07 (3)
C2—C3	1.386 (2)	C17—H17C	1.06 (3)
C3—H3	1.10 (3)	C18—H18A	1.12 (3)
C3—C4	1.402 (3)	C18—H18B	1.14 (3)
C4—H4	1.15 (3)	C18—H18C	1.11 (3)
C4—C5	1.396 (3)	C19—H19	1.10 (2)
C5—H5	1.13 (3)	C19—C20	1.531 (3)
C5—C6	1.398 (2)	C19—C21	1.534 (3)
C6—H6	1.08 (3)	C20—H20A	1.12 (3)
C7—H7	1.11 (3)	C20—H20B	1.13 (3)
C7—C8	1.534 (3)	C20—H20C	1.07 (3)
C7—C9	1.525 (3)	C21—H21A	1.01 (3)
C8—H8A	1.03 (3)	C21—H21B	1.05 (4)
C8—H8B	1.19 (3)	C21—H21C	1.13 (3)
C8—H8C	1.10 (3)	C22—H22	1.06 (3)
C9—H9A	1.17 (3)	C22—C23	1.532 (2)
C9—H9B	1.06 (3)	C22—C24	1.530 (2)
C9—H9C	1.04 (3)	C23—H23A	1.08 (3)
C10—H10	1.15 (3)	C23—H23B	1.08 (3)
C10—C11	1.532 (2)	C23—H23C	1.06 (3)
C10—C12	1.539 (2)	C24—H24A	1.11 (3)
C11—H11A	1.11 (3)	C24—H24B	0.99 (3)
C11—H11B	1.11 (3)	C24—H24C	1.13 (3)
C11—H11C	1.10 (3)
Cl—Rh—H	156.3 (10)	H12B—C12—H12A	107 (3)
B—Rh—H	65.9 (10)	H12C—C12—C10	107.8 (16)
B—Rh—Cl	137.80 (6)	H12C—C12—H12A	117 (2)
P1—Rh—H	91.6 (10)	H12C—C12—H12B	105 (2)
P1—Rh—Cl	87.620 (14)	H13—C13—P1	106.0 (15)
P1—Rh—B	93.34 (5)	C14—C13—P1	115.39 (14)
P2—Rh—H	85.3 (10)	C14—C13—H13	107.2 (17)
P2—Rh—Cl	92.562 (14)	C15—C13—P1	110.51 (12)
P2—Rh—B	91.44 (5)	C15—C13—H13	108.5 (16)
P2—Rh—P1	172.668 (15)	C15—C13—C14	108.90 (18)
O1—B—Rh	120.14 (12)	H14A—C14—C13	110 (2)
O2—B—Rh	131.88 (13)	H14B—C14—C13	114.6 (18)
O2—B—O1	107.97 (13)	H14B—C14—H14A	111 (3)
C7—P1—Rh	119.74 (5)	H14C—C14—C13	110.7 (18)
C10—P1—Rh	114.29 (5)	H14C—C14—H14A	103 (3)
C10—P1—C7	105.73 (7)	H14C—C14—H14B	107 (3)
C13—P1—Rh	110.81 (6)	H15A—C15—C13	111.0 (17)
C13—P1—C7	99.91 (8)	H15B—C15—C13	110.3 (16)
C13—P1—C10	104.47 (8)	H15B—C15—H15A	104 (3)
C16—P2—Rh	117.58 (6)	H15C—C15—C13	111.0 (18)
C19—P2—Rh	114.42 (5)	H15C—C15—H15A	112 (2)
C19—P2—C16	102.74 (8)	H15C—C15—H15B	108 (3)
C22—P2—Rh	107.94 (5)	H16—C16—P2	111.0 (14)
C22—P2—C16	103.06 (7)	C17—C16—P2	110.36 (12)
C22—P2—C19	110.45 (8)	C17—C16—H16	107.2 (15)
C1—O1—B	106.84 (12)	C18—C16—P2	112.96 (13)
C2—O2—B	106.53 (12)	C18—C16—H16	104.5 (16)
C2—C1—O1	109.06 (13)	C18—C16—C17	110.52 (15)
C6—C1—O1	128.59 (14)	H17A—C17—C16	115.8 (16)
C6—C1—C2	122.33 (14)	H17B—C17—C16	117.5 (18)
C1—C2—O2	109.57 (13)	H17B—C17—H17A	97 (3)
C3—C2—O2	128.60 (15)	H17C—C17—C16	108.9 (19)
C3—C2—C1	121.78 (15)	H17C—C17—H17A	106 (2)
H3—C3—C2	120.1 (15)	H17C—C17—H17B	111 (3)
C4—C3—C2	116.43 (17)	H18A—C18—C16	112.5 (19)
C4—C3—H3	123.5 (15)	H18B—C18—C16	110.3 (17)
H4—C4—C3	117.6 (18)	H18B—C18—H18A	109 (3)
C5—C4—C3	121.61 (16)	H18C—C18—C16	104.9 (17)
C5—C4—H4	120.3 (18)	H18C—C18—H18A	107 (2)
H5—C5—C4	113.9 (16)	H18C—C18—H18B	113 (3)
C6—C5—C4	121.17 (15)	H19—C19—P2	99.1 (14)
C6—C5—H5	124.9 (17)	C20—C19—P2	112.59 (13)
C5—C6—C1	116.67 (15)	C20—C19—H19	107.5 (15)
H6—C6—C1	125.4 (15)	C21—C19—P2	116.98 (13)
H6—C6—C5	117.8 (15)	C21—C19—H19	109.8 (15)
H7—C7—P1	105.3 (14)	C21—C19—C20	110.05 (17)
C8—C7—P1	114.13 (11)	H20A—C20—C19	110 (2)
C8—C7—H7	107.0 (15)	H20B—C20—C19	114.3 (18)
C9—C7—P1	111.82 (12)	H20B—C20—H20A	106 (3)
C9—C7—H7	108.2 (14)	H20C—C20—C19	103 (2)
C9—C7—C8	110.02 (15)	H20C—C20—H20A	112 (2)
H8A—C8—C7	110.4 (17)	H20C—C20—H20B	112 (3)
H8B—C8—C7	110.4 (16)	H21A—C21—C19	115 (2)
H8B—C8—H8A	110 (3)	H21B—C21—C19	108 (2)
H8C—C8—C7	106.9 (17)	H21B—C21—H21A	108 (3)
H8C—C8—H8A	111 (2)	H21C—C21—C19	108.8 (17)
H8C—C8—H8B	109 (2)	H21C—C21—H21A	111 (3)
H9A—C9—C7	112.7 (16)	H21C—C21—H21B	106 (3)
H9B—C9—C7	114.3 (18)	H22—C22—P2	99.9 (15)
H9B—C9—H9A	100 (2)	C23—C22—P2	113.42 (11)
H9C—C9—C7	107.9 (17)	C23—C22—H22	106.0 (15)
H9C—C9—H9A	112 (2)	C24—C22—P2	116.49 (12)
H9C—C9—H9B	110 (3)	C24—C22—H22	109.6 (15)
H10—C10—P1	98.6 (14)	C24—C22—C23	110.40 (13)
C11—C10—P1	114.56 (12)	H23A—C23—C22	114.1 (16)
C11—C10—H10	109.9 (13)	H23B—C23—C22	107.2 (16)
C12—C10—P1	112.42 (11)	H23B—C23—H23A	109 (3)
C12—C10—H10	108.8 (14)	H23C—C23—C22	111.6 (16)
C12—C10—C11	111.76 (14)	H23C—C23—H23A	105 (2)
H11A—C11—C10	109.9 (16)	H23C—C23—H23B	110 (2)
H11B—C11—C10	113.4 (16)	H24A—C24—C22	111.5 (17)
H11B—C11—H11A	110 (2)	H24B—C24—C22	112.5 (16)
H11C—C11—C10	110.3 (16)	H24B—C24—H24A	98 (3)
H11C—C11—H11A	102 (2)	H24C—C24—C22	111.6 (17)
H11C—C11—H11B	111 (2)	H24C—C24—H24A	108 (2)
H12A—C12—C10	111.0 (17)	H24C—C24—H24B	114 (3)
H12B—C12—C10	109.4 (16)
Rh—B—O1—C1	−178.84 (12)	O1—C1—C6—C5	−178.68 (17)
Rh—B—O2—C2	179.19 (15)	O2—C2—C1—C6	−178.08 (12)
B—O1—C1—C2	−1.27 (13)	O2—C2—C3—C4	178.2 (2)
B—O1—C1—C6	177.17 (12)	C1—C2—C3—C4	1.01 (19)
B—O2—C2—C1	0.53 (13)	C1—C6—C5—C4	0.61 (18)
B—O2—C2—C3	−176.95 (14)	C2—C3—C4—C5	−0.8 (2)
O1—C1—C2—O2	0.47 (13)	C3—C4—C5—C6	0.0 (2)
O1—C1—C2—C3	178.15 (13)

(SITKUB_HAR_NoMoRe)

Crystal data

C24H47BClO2P2Rh	F(000) = 1213.281
Mr = 578.77	Dx = 1.348 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
a = 11.228 (3) Å	Cell parameters from 925 reflections
b = 11.101 (3) Å	θ = 12.0–24.6°
c = 23.414 (7) Å	µ = 0.82 mm^−1
β = 102.28 (4)°	T = 120 K
V = 2851.6 (14) Å^3	Fragment, colourless
Z = 4	0.6 × 0.4 × 0.2 mm

Data collection

SMART 1K CCD area detector diffractometer	7021 reflections with I ≥ 2u(I)
Radiation source: fine-focus sealed tube	Rint = 0.029
Graphite monochromator	θmax = 29.1°, θmin = 1.8°
ω scans	h = −15→15
33082 measured reflections	k = −15→15
7624 independent reflections	l = −31→31

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.026	Only H-atom coordinates refined
wR(F^2) = 0.096	w = 1/[σ^2(Fo^2) + (0.1P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 0.83	(Δ/σ)max = 0.001
7624 reflections	Δρmax = 0.42 e Å^−3
421 parameters	Δρmin = −0.74 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Rh	0.311338 (9)	0.814888 (9)	0.861862 (5)	0.01650 (6)
H	0.344 (2)	0.776 (2)	0.9248 (10)	0.033153
Cl	0.32708 (4)	0.93356 (4)	0.777010 (18)	0.02814 (9)
B	0.21232 (17)	0.68036 (14)	0.88076 (8)	0.0197 (3)
P1	0.17683 (3)	0.96115 (3)	0.882932 (17)	0.01977 (9)
P2	0.46543 (4)	0.68313 (3)	0.848421 (18)	0.01857 (9)
O1	0.10463 (10)	0.64528 (10)	0.84065 (5)	0.0214 (2)
O2	0.22699 (10)	0.60328 (10)	0.93011 (5)	0.0240 (2)
C1	0.05450 (14)	0.55179 (13)	0.86612 (7)	0.0204 (3)
C2	0.12880 (14)	0.52621 (14)	0.91998 (7)	0.0225 (3)
C3	0.09894 (17)	0.43779 (17)	0.95634 (8)	0.0324 (4)
H3	0.157 (3)	0.423 (3)	0.9998 (13)	0.054124
C4	−0.00943 (18)	0.37430 (16)	0.93528 (9)	0.0344 (4)
H4	−0.042 (3)	0.308 (3)	0.9666 (16)	0.056825
C5	−0.08387 (16)	0.40011 (15)	0.88090 (8)	0.0284 (3)
H5	−0.169 (3)	0.344 (3)	0.8704 (14)	0.048998
C6	−0.05313 (14)	0.49066 (15)	0.84514 (7)	0.0237 (3)
H6	−0.112 (2)	0.504 (3)	0.8028 (12)	0.043482
C7	0.09980 (15)	0.93787 (15)	0.94527 (7)	0.0247 (3)
H7	0.054 (2)	1.025 (2)	0.9504 (12)	0.041514
C8	0.00023 (16)	0.84086 (17)	0.93431 (8)	0.0283 (3)
H8A	0.038 (3)	0.758 (3)	0.9307 (14)	0.052650
H8B	−0.073 (3)	0.863 (3)	0.8911 (14)	0.054728
H8C	−0.044 (3)	0.843 (3)	0.9716 (13)	0.050408
C9	0.19109 (18)	0.91161 (19)	1.00210 (8)	0.0334 (4)
H9A	0.145 (3)	0.905 (3)	1.0424 (13)	0.059875
H9B	0.254 (3)	0.982 (3)	1.0164 (13)	0.061045
H9C	0.238 (3)	0.834 (3)	0.9961 (13)	0.055334
C10	0.05454 (14)	1.00379 (15)	0.81984 (7)	0.0239 (3)
H10	0.113 (2)	1.056 (2)	0.7934 (12)	0.037249
C11	−0.04330 (17)	1.08685 (18)	0.83497 (9)	0.0349 (4)
H11A	−0.099 (3)	1.126 (3)	0.7944 (13)	0.057320
H11B	−0.006 (3)	1.160 (3)	0.8659 (15)	0.054227
H11C	−0.111 (3)	1.034 (3)	0.8520 (15)	0.056975
C12	−0.00190 (14)	0.89383 (16)	0.78404 (7)	0.0260 (3)
H12A	−0.041 (3)	0.834 (3)	0.8101 (13)	0.052962
H12B	0.070 (3)	0.844 (3)	0.7692 (14)	0.049279
H12C	−0.061 (3)	0.926 (3)	0.7453 (13)	0.050336
C13	0.25947 (16)	1.10631 (15)	0.90638 (8)	0.0303 (3)
H13	0.218 (2)	1.143 (3)	0.9389 (13)	0.046756
C14	0.2508 (2)	1.20197 (19)	0.85841 (12)	0.0456 (5)
H14A	0.305 (3)	1.275 (3)	0.8738 (15)	0.071403
H14B	0.156 (3)	1.232 (3)	0.8389 (16)	0.066413
H14C	0.289 (3)	1.169 (3)	0.8238 (16)	0.063772
C15	0.39403 (19)	1.0820 (2)	0.93305 (12)	0.0431 (5)
H15A	0.441 (3)	1.046 (3)	0.9002 (15)	0.054999
H15B	0.403 (3)	1.012 (3)	0.9656 (14)	0.056867
H15C	0.442 (3)	1.168 (3)	0.9552 (17)	0.070072
C16	0.43415 (15)	0.58540 (15)	0.78284 (7)	0.0255 (3)
H16	0.513 (2)	0.531 (2)	0.7803 (12)	0.044142
C17	0.32951 (18)	0.49882 (19)	0.78538 (10)	0.0375 (4)
H17A	0.242 (3)	0.541 (3)	0.7882 (14)	0.051685
H17B	0.338 (3)	0.443 (3)	0.8229 (17)	0.074086
H17C	0.311 (3)	0.446 (3)	0.7466 (17)	0.071792
C18	0.4075 (2)	0.6567 (2)	0.72563 (8)	0.0375 (4)
H18A	0.389 (3)	0.597 (3)	0.6861 (13)	0.066064
H18B	0.488 (3)	0.718 (3)	0.7231 (14)	0.065197
H18C	0.322 (3)	0.707 (3)	0.7263 (14)	0.058398
C19	0.51406 (15)	0.57333 (15)	0.90889 (8)	0.0269 (3)
H19	0.425 (2)	0.535 (2)	0.9106 (12)	0.042131
C20	0.5636 (2)	0.6348 (2)	0.96769 (9)	0.0399 (4)
H20A	0.579 (3)	0.566 (3)	1.0036 (14)	0.068747
H20B	0.500 (4)	0.704 (3)	0.9806 (15)	0.073154
H20C	0.647 (3)	0.674 (3)	0.9619 (16)	0.070688
C21	0.6008 (2)	0.4725 (2)	0.89879 (11)	0.0468 (5)
H21A	0.684 (3)	0.500 (3)	0.8940 (18)	0.081229
H21B	0.560 (4)	0.426 (3)	0.8607 (18)	0.090710
H21C	0.610 (3)	0.405 (3)	0.9357 (17)	0.070248
C22	0.59697 (13)	0.77488 (15)	0.83774 (7)	0.0222 (3)
H22	0.555 (3)	0.825 (2)	0.8003 (12)	0.038050
C23	0.63925 (16)	0.86735 (17)	0.88638 (9)	0.0316 (4)
H23A	0.692 (3)	0.829 (3)	0.9265 (14)	0.052644
H23B	0.559 (3)	0.910 (3)	0.8952 (15)	0.059325
H23C	0.698 (3)	0.933 (3)	0.8740 (13)	0.052487
C24	0.70616 (17)	0.70578 (18)	0.82479 (10)	0.0334 (4)
H24A	0.765 (3)	0.765 (3)	0.8045 (15)	0.056328
H24B	0.683 (3)	0.648 (3)	0.7922 (14)	0.054652
H24C	0.763 (3)	0.665 (3)	0.8656 (15)	0.052800

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Rh	0.01433 (8)	0.01739 (8)	0.01809 (8)	0.00040 (3)	0.00412 (5)	0.00055 (3)
H	0.034000	0.039000	0.025000	0.002000	0.003000	0.001000
Cl	0.02401 (18)	0.0319 (2)	0.03085 (19)	0.00457 (14)	0.01096 (15)	0.01201 (15)
B	0.0177 (8)	0.0210 (8)	0.0215 (8)	−0.0001 (5)	0.0066 (6)	0.0006 (5)
P1	0.01814 (17)	0.01924 (17)	0.02226 (18)	0.00199 (13)	0.00503 (14)	−0.00065 (13)
P2	0.01542 (19)	0.01951 (19)	0.02116 (19)	0.00088 (11)	0.00476 (15)	−0.00025 (12)
O1	0.0201 (5)	0.0242 (5)	0.0194 (5)	−0.0016 (4)	0.0033 (4)	0.0012 (4)
O2	0.0210 (5)	0.0264 (5)	0.0231 (5)	−0.0021 (4)	0.0016 (4)	0.0050 (4)
C1	0.0203 (7)	0.0197 (6)	0.0221 (7)	−0.0006 (5)	0.0062 (5)	−0.0018 (5)
C2	0.0216 (7)	0.0213 (7)	0.0246 (7)	−0.0018 (5)	0.0051 (6)	0.0038 (5)
C3	0.0312 (9)	0.0308 (9)	0.0345 (9)	−0.0030 (7)	0.0052 (7)	0.0106 (7)
H3	0.047000	0.069000	0.043000	−0.012000	0.002000	0.024000
C4	0.0330 (9)	0.0275 (8)	0.0438 (10)	−0.0057 (7)	0.0107 (8)	0.0105 (7)
H4	0.055000	0.057000	0.061000	−0.020000	0.018000	0.021000
C5	0.0257 (7)	0.0233 (7)	0.0382 (9)	−0.0047 (6)	0.0114 (7)	−0.0026 (6)
H5	0.039000	0.047000	0.062000	−0.021000	0.013000	−0.006000
C6	0.0199 (7)	0.0247 (7)	0.0270 (7)	−0.0010 (6)	0.0058 (6)	−0.0030 (6)
H6	0.038000	0.051000	0.037000	−0.012000	−0.002000	−0.002000
C7	0.0247 (7)	0.0274 (8)	0.0233 (7)	0.0033 (6)	0.0085 (6)	−0.0039 (6)
H7	0.047000	0.035000	0.047000	0.008000	0.020000	−0.006000
C8	0.0283 (8)	0.0311 (8)	0.0284 (8)	0.0005 (7)	0.0128 (7)	−0.0009 (7)
H8A	0.054000	0.035000	0.077000	−0.001000	0.032000	−0.008000
H8B	0.037000	0.075000	0.049000	−0.011000	0.002000	0.011000
H8C	0.056000	0.057000	0.048000	−0.003000	0.033000	−0.001000
C9	0.0352 (9)	0.0417 (10)	0.0232 (7)	0.0035 (8)	0.0056 (7)	−0.0044 (7)
H9A	0.067000	0.085000	0.031000	0.007000	0.018000	−0.001000
H9B	0.055000	0.079000	0.044000	−0.016000	−0.001000	−0.011000
H9C	0.060000	0.062000	0.041000	0.023000	0.004000	0.002000
C10	0.0210 (7)	0.0248 (7)	0.0252 (7)	0.0054 (6)	0.0033 (6)	0.0045 (6)
H10	0.039000	0.036000	0.038000	−0.000000	0.011000	0.008000
C11	0.0286 (8)	0.0349 (9)	0.0407 (10)	0.0152 (7)	0.0064 (7)	0.0016 (8)
H11A	0.052000	0.059000	0.055000	0.028000	−0.002000	0.006000
H11B	0.051000	0.047000	0.062000	0.014000	0.006000	−0.016000
H11C	0.042000	0.064000	0.072000	0.012000	0.028000	0.003000
C12	0.0209 (7)	0.0313 (8)	0.0245 (7)	0.0010 (6)	0.0021 (6)	0.0027 (6)
H12A	0.059000	0.058000	0.042000	−0.025000	0.011000	0.004000
H12B	0.039000	0.048000	0.061000	0.005000	0.011000	−0.018000
H12C	0.046000	0.052000	0.043000	0.006000	−0.013000	0.004000
C13	0.0284 (8)	0.0213 (7)	0.0415 (9)	0.0004 (6)	0.0077 (7)	−0.0057 (6)
H13	0.051000	0.038000	0.056000	−0.002000	0.022000	−0.016000
C14	0.0516 (13)	0.0260 (9)	0.0613 (14)	−0.0084 (9)	0.0168 (12)	0.0018 (9)
H14A	0.081000	0.037000	0.095000	−0.021000	0.016000	0.002000
H14B	0.060000	0.043000	0.093000	0.008000	0.009000	0.020000
H14C	0.079000	0.057000	0.062000	−0.008000	0.030000	0.008000
C15	0.0297 (9)	0.0342 (10)	0.0614 (13)	−0.0057 (8)	0.0003 (9)	−0.0144 (9)
H15A	0.039000	0.056000	0.074000	−0.003000	0.021000	−0.011000
H15B	0.045000	0.059000	0.059000	0.000000	−0.006000	0.001000
H15C	0.052000	0.054000	0.098000	−0.017000	0.002000	−0.035000
C16	0.0204 (7)	0.0256 (7)	0.0317 (8)	−0.0024 (6)	0.0085 (6)	−0.0074 (6)
H16	0.035000	0.045000	0.054000	0.009000	0.013000	−0.014000
C17	0.0308 (9)	0.0363 (10)	0.0483 (11)	−0.0127 (7)	0.0146 (8)	−0.0177 (8)
H17A	0.032000	0.057000	0.068000	−0.005000	0.015000	−0.021000
H17B	0.078000	0.059000	0.080000	−0.030000	0.005000	0.018000
H17C	0.062000	0.067000	0.092000	−0.022000	0.029000	−0.054000
C18	0.0426 (11)	0.0417 (10)	0.0266 (8)	−0.0036 (9)	0.0038 (7)	−0.0080 (7)
H18A	0.086000	0.075000	0.038000	−0.006000	0.015000	−0.024000
H18B	0.067000	0.089000	0.042000	−0.030000	0.017000	0.002000
H18C	0.062000	0.067000	0.043000	0.014000	0.004000	0.004000
C19	0.0244 (7)	0.0270 (8)	0.0305 (8)	0.0065 (6)	0.0083 (6)	0.0077 (6)
H19	0.030000	0.043000	0.056000	0.001000	0.015000	0.016000
C20	0.0440 (11)	0.0425 (11)	0.0288 (8)	0.0062 (9)	−0.0024 (8)	0.0080 (8)
H20A	0.079000	0.081000	0.041000	0.002000	0.001000	0.028000
H20B	0.099000	0.070000	0.042000	0.029000	−0.004000	−0.010000
H20C	0.052000	0.077000	0.071000	−0.017000	−0.014000	0.022000
C21	0.0483 (12)	0.0413 (11)	0.0547 (13)	0.0238 (10)	0.0199 (11)	0.0167 (10)
H21A	0.065000	0.081000	0.115000	0.040000	0.058000	0.043000
H21B	0.126000	0.052000	0.088000	0.039000	0.009000	−0.013000
H21C	0.080000	0.058000	0.082000	0.037000	0.038000	0.039000
C22	0.0157 (6)	0.0245 (7)	0.0265 (7)	−0.0027 (5)	0.0044 (5)	0.0009 (6)
H22	0.033000	0.045000	0.036000	−0.000000	0.007000	0.013000
C23	0.0242 (8)	0.0299 (9)	0.0401 (9)	−0.0050 (6)	0.0056 (7)	−0.0086 (7)
H23A	0.057000	0.055000	0.040000	−0.009000	−0.003000	−0.004000
H23B	0.045000	0.054000	0.084000	−0.000000	0.025000	−0.029000
H23C	0.049000	0.041000	0.069000	−0.018000	0.016000	−0.002000
C24	0.0206 (8)	0.0338 (9)	0.0483 (11)	−0.0047 (7)	0.0128 (7)	−0.0118 (8)
H24A	0.037000	0.058000	0.083000	−0.008000	0.033000	−0.004000
H24B	0.040000	0.062000	0.065000	−0.004000	0.018000	−0.031000
H24C	0.037000	0.055000	0.063000	0.015000	0.003000	0.002000

Geometric parameters (Å, º)

Rh—H	1.51 (2)	C12—H12A	1.06 (3)
Rh—Cl	2.4214 (7)	C12—H12B	1.09 (3)
Rh—B	1.9676 (17)	C12—H12C	1.07 (3)
Rh—P1	2.3404 (6)	C13—H13	1.05 (3)
Rh—P2	2.3374 (6)	C13—C14	1.534 (3)
B—O1	1.419 (2)	C13—C15	1.531 (3)
B—O2	1.419 (2)	C14—H14A	1.03 (3)
P1—C7	1.8660 (18)	C14—H14B	1.12 (3)
P1—C10	1.8517 (18)	C14—H14C	1.06 (4)
P1—C13	1.8821 (18)	C15—H15A	1.10 (3)
P2—C16	1.8517 (17)	C15—H15B	1.08 (3)
P2—C19	1.8601 (17)	C15—H15C	1.16 (3)
P2—C22	1.8543 (16)	C16—H16	1.08 (2)
O1—C1	1.3756 (18)	C16—C17	1.529 (2)
O2—C2	1.3757 (18)	C16—C18	1.530 (3)
C1—C2	1.385 (2)	C17—H17A	1.11 (3)
C1—C6	1.382 (2)	C17—H17B	1.07 (3)
C2—C3	1.386 (2)	C17—H17C	1.06 (3)
C3—H3	1.10 (3)	C18—H18A	1.12 (3)
C3—C4	1.402 (3)	C18—H18B	1.14 (3)
C4—H4	1.15 (3)	C18—H18C	1.11 (3)
C4—C5	1.396 (3)	C19—H19	1.10 (2)
C5—H5	1.13 (3)	C19—C20	1.531 (3)
C5—C6	1.398 (2)	C19—C21	1.534 (3)
C6—H6	1.08 (3)	C20—H20A	1.12 (3)
C7—H7	1.11 (3)	C20—H20B	1.13 (3)
C7—C8	1.534 (3)	C20—H20C	1.07 (3)
C7—C9	1.525 (3)	C21—H21A	1.01 (3)
C8—H8A	1.03 (3)	C21—H21B	1.05 (4)
C8—H8B	1.19 (3)	C21—H21C	1.13 (3)
C8—H8C	1.10 (3)	C22—H22	1.06 (3)
C9—H9A	1.17 (3)	C22—C23	1.532 (2)
C9—H9B	1.06 (3)	C22—C24	1.530 (2)
C9—H9C	1.04 (3)	C23—H23A	1.08 (3)
C10—H10	1.15 (3)	C23—H23B	1.08 (3)
C10—C11	1.532 (2)	C23—H23C	1.06 (3)
C10—C12	1.539 (2)	C24—H24A	1.11 (3)
C11—H11A	1.11 (3)	C24—H24B	0.99 (3)
C11—H11B	1.11 (3)	C24—H24C	1.13 (3)
C11—H11C	1.10 (3)
Cl—Rh—H	156.3 (10)	H12B—C12—H12A	106 (3)
B—Rh—H	65.9 (10)	H12C—C12—C10	107.7 (16)
B—Rh—Cl	137.80 (6)	H12C—C12—H12A	117 (2)
P1—Rh—H	91.6 (10)	H12C—C12—H12B	105 (2)
P1—Rh—Cl	87.620 (14)	H13—C13—P1	106.0 (15)
P1—Rh—B	93.34 (5)	C14—C13—P1	115.39 (14)
P2—Rh—H	85.3 (10)	C14—C13—H13	107.2 (17)
P2—Rh—Cl	92.562 (14)	C15—C13—P1	110.51 (12)
P2—Rh—B	91.44 (5)	C15—C13—H13	108.6 (16)
P2—Rh—P1	172.668 (15)	C15—C13—C14	108.90 (18)
O1—B—Rh	120.15 (12)	H14A—C14—C13	110.3 (19)
O2—B—Rh	131.88 (13)	H14B—C14—C13	114.5 (18)
O2—B—O1	107.97 (13)	H14B—C14—H14A	111 (3)
C7—P1—Rh	119.74 (5)	H14C—C14—C13	110.6 (18)
C10—P1—Rh	114.29 (5)	H14C—C14—H14A	103 (3)
C10—P1—C7	105.72 (7)	H14C—C14—H14B	107 (3)
C13—P1—Rh	110.81 (6)	H15A—C15—C13	111.0 (17)
C13—P1—C7	99.91 (8)	H15B—C15—C13	110.3 (16)
C13—P1—C10	104.46 (8)	H15B—C15—H15A	104 (3)
C16—P2—Rh	117.58 (6)	H15C—C15—C13	111.0 (18)
C19—P2—Rh	114.42 (5)	H15C—C15—H15A	112 (2)
C19—P2—C16	102.74 (8)	H15C—C15—H15B	108 (3)
C22—P2—Rh	107.94 (5)	H16—C16—P2	111.0 (14)
C22—P2—C16	103.06 (7)	C17—C16—P2	110.36 (12)
C22—P2—C19	110.45 (8)	C17—C16—H16	107.2 (15)
C1—O1—B	106.84 (12)	C18—C16—P2	112.96 (13)
C2—O2—B	106.54 (12)	C18—C16—H16	104.5 (16)
C2—C1—O1	109.06 (13)	C18—C16—C17	110.52 (15)
C6—C1—O1	128.60 (14)	H17A—C17—C16	115.9 (16)
C6—C1—C2	122.32 (14)	H17B—C17—C16	117.6 (18)
C1—C2—O2	109.56 (13)	H17B—C17—H17A	97 (3)
C3—C2—O2	128.61 (15)	H17C—C17—C16	108.9 (19)
C3—C2—C1	121.78 (15)	H17C—C17—H17A	106 (2)
H3—C3—C2	120.1 (15)	H17C—C17—H17B	111 (3)
C4—C3—C2	116.43 (17)	H18A—C18—C16	112.5 (19)
C4—C3—H3	123.5 (15)	H18B—C18—C16	110.3 (17)
H4—C4—C3	117.7 (18)	H18B—C18—H18A	109 (3)
C5—C4—C3	121.61 (16)	H18C—C18—C16	104.9 (17)
C5—C4—H4	120.3 (18)	H18C—C18—H18A	107 (2)
H5—C5—C4	113.8 (17)	H18C—C18—H18B	113 (3)
C6—C5—C4	121.18 (15)	H19—C19—P2	99.0 (14)
C6—C5—H5	125.0 (17)	C20—C19—P2	112.59 (13)
C5—C6—C1	116.67 (15)	C20—C19—H19	107.4 (15)
H6—C6—C1	125.4 (15)	C21—C19—P2	116.99 (13)
H6—C6—C5	117.9 (15)	C21—C19—H19	109.9 (15)
H7—C7—P1	105.3 (14)	C21—C19—C20	110.04 (17)
C8—C7—P1	114.14 (11)	H20A—C20—C19	110 (2)
C8—C7—H7	107.1 (15)	H20B—C20—C19	114.3 (18)
C9—C7—P1	111.82 (12)	H20B—C20—H20A	106 (3)
C9—C7—H7	108.1 (14)	H20C—C20—C19	103 (2)
C9—C7—C8	110.02 (15)	H20C—C20—H20A	112 (2)
H8A—C8—C7	110.4 (16)	H20C—C20—H20B	112 (3)
H8B—C8—C7	110.4 (16)	H21A—C21—C19	115 (2)
H8B—C8—H8A	110 (3)	H21B—C21—C19	108 (2)
H8C—C8—C7	106.9 (17)	H21B—C21—H21A	108 (3)
H8C—C8—H8A	111 (2)	H21C—C21—C19	108.7 (17)
H8C—C8—H8B	109 (2)	H21C—C21—H21A	111 (3)
H9A—C9—C7	112.7 (16)	H21C—C21—H21B	106 (3)
H9B—C9—C7	114.4 (18)	H22—C22—P2	99.9 (15)
H9B—C9—H9A	100 (2)	C23—C22—P2	113.42 (11)
H9C—C9—C7	107.9 (17)	C23—C22—H22	106.0 (15)
H9C—C9—H9A	112 (2)	C24—C22—P2	116.49 (12)
H9C—C9—H9B	110 (3)	C24—C22—H22	109.6 (15)
H10—C10—P1	98.5 (14)	C24—C22—C23	110.40 (13)
C11—C10—P1	114.57 (12)	H23A—C23—C22	114.0 (15)
C11—C10—H10	109.9 (13)	H23B—C23—C22	107.2 (16)
C12—C10—P1	112.42 (11)	H23B—C23—H23A	109 (2)
C12—C10—H10	108.8 (14)	H23C—C23—C22	111.6 (16)
C12—C10—C11	111.76 (14)	H23C—C23—H23A	105 (2)
H11A—C11—C10	109.8 (16)	H23C—C23—H23B	110 (2)
H11B—C11—C10	113.4 (16)	H24A—C24—C22	111.4 (17)
H11B—C11—H11A	110 (2)	H24B—C24—C22	112.6 (16)
H11C—C11—C10	110.2 (16)	H24B—C24—H24A	98 (3)
H11C—C11—H11A	102 (2)	H24C—C24—C22	111.6 (17)
H11C—C11—H11B	111 (2)	H24C—C24—H24A	108 (2)
H12A—C12—C10	111.0 (17)	H24C—C24—H24B	114 (3)
H12B—C12—C10	109.4 (16)

(SITKUB_HAR_SHADE3_1)

Crystal data

C24H47BClO2P2Rh	F(000) = 1213.326
Mr = 578.77	Dx = 1.348 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
a = 11.228 (3) Å	Cell parameters from 925 reflections
b = 11.101 (3) Å	θ = 12.0–24.6°
c = 23.414 (7) Å	µ = 0.82 mm^−1
β = 102.28 (4)°	T = 120 K
V = 2851.6 (14) Å^3	Fragment, colourless
Z = 4	0.6 × 0.4 × 0.2 mm

Data collection

SMART 1K CCD area detector diffractometer	7021 reflections with I ≥ 2u(I)
Radiation source: fine-focus sealed tube	Rint = 0.029
Graphite monochromator	θmax = 29.1°, θmin = 1.8°
ω scans	h = −15→15
33082 measured reflections	k = −15→15
7624 independent reflections	l = −31→31

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.024	Only H-atom coordinates refined
wR(F^2) = 0.054	w = 1/[σ^2(Fo^2) + (0.0238P)^2 + 1.9702P] where P = (Fo^2 + 2Fc^2)/3
S = 0.98	(Δ/σ)max = 0.001
7624 reflections	Δρmax = 0.45 e Å^−3
421 parameters	Δρmin = −0.72 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Rh	0.311324 (9)	0.814890 (9)	0.861855 (4)	0.01630 (3)
H	0.3469 (19)	0.783 (2)	0.9265 (8)	0.032322
Cl	0.32708 (3)	0.93355 (4)	0.777003 (17)	0.02803 (8)
B	0.21250 (14)	0.68030 (14)	0.88081 (7)	0.0196 (3)
P1	0.17685 (3)	0.96113 (3)	0.882947 (16)	0.01975 (7)
P2	0.46545 (3)	0.68313 (3)	0.848428 (15)	0.01859 (7)
O1	0.10456 (9)	0.64530 (9)	0.84069 (4)	0.02136 (19)
O2	0.22706 (9)	0.60331 (10)	0.93007 (5)	0.0240 (2)
C1	0.05453 (13)	0.55187 (13)	0.86616 (6)	0.0204 (3)
C2	0.12874 (13)	0.52617 (13)	0.92014 (6)	0.0228 (3)
C3	0.09915 (16)	0.43764 (16)	0.95638 (8)	0.0324 (3)
H3	0.157 (2)	0.420 (2)	1.0001 (10)	0.047342
C4	−0.00953 (16)	0.37443 (15)	0.93523 (8)	0.0341 (4)
H4	−0.040 (2)	0.307 (2)	0.9627 (12)	0.056272
C5	−0.08365 (14)	0.40015 (14)	0.88093 (8)	0.0285 (3)
H5	−0.169 (2)	0.350 (2)	0.8684 (11)	0.051690
C6	−0.05319 (13)	0.49075 (14)	0.84512 (7)	0.0240 (3)
H6	−0.114 (2)	0.507 (2)	0.8023 (10)	0.040352
C7	0.09985 (13)	0.93777 (14)	0.94524 (6)	0.0242 (3)
H7	0.0578 (19)	1.0272 (19)	0.9511 (9)	0.036782
C8	0.00040 (15)	0.84081 (16)	0.93438 (7)	0.0283 (3)
H8A	0.0368 (18)	0.7549 (19)	0.9318 (9)	0.035709
H8B	−0.0693 (19)	0.858 (2)	0.8925 (9)	0.035402
H8C	−0.044 (2)	0.842 (2)	0.9710 (9)	0.041290
C9	0.19136 (16)	0.91165 (18)	1.00216 (7)	0.0335 (4)
H9A	0.144 (2)	0.903 (2)	1.0396 (9)	0.046040
H9B	0.258 (2)	0.979 (2)	1.0155 (10)	0.044959
H9C	0.240 (2)	0.831 (2)	0.9983 (9)	0.039648
C10	0.05440 (13)	1.00357 (14)	0.81985 (7)	0.0240 (3)
H10	0.108 (2)	1.056 (2)	0.7930 (10)	0.039751
C11	−0.04331 (16)	1.08686 (17)	0.83512 (8)	0.0350 (4)
H11A	−0.096 (2)	1.127 (2)	0.7949 (11)	0.052415
H11B	−0.005 (2)	1.159 (2)	0.8655 (12)	0.051254
H11C	−0.109 (2)	1.036 (2)	0.8551 (10)	0.045697
C12	−0.00194 (14)	0.89405 (15)	0.78408 (7)	0.0259 (3)
H12A	−0.0453 (19)	0.834 (2)	0.8103 (9)	0.036839
H12B	0.0681 (19)	0.842 (2)	0.7692 (9)	0.037748
H12C	−0.068 (2)	0.921 (2)	0.7448 (10)	0.045717
C13	0.25948 (15)	1.10611 (14)	0.90632 (8)	0.0304 (3)
H13	0.218 (2)	1.147 (2)	0.9407 (11)	0.044050
C14	0.2507 (2)	1.20161 (17)	0.85839 (10)	0.0451 (5)
H14A	0.307 (2)	1.280 (2)	0.8752 (13)	0.062542
H14B	0.156 (2)	1.233 (2)	0.8395 (12)	0.056505
H14C	0.288 (2)	1.169 (2)	0.8221 (12)	0.054006
C15	0.39408 (17)	1.08196 (18)	0.93301 (10)	0.0430 (5)
H15A	0.441 (2)	1.052 (2)	0.8977 (11)	0.045943
H15B	0.405 (2)	1.012 (2)	0.9652 (10)	0.043998
H15C	0.441 (2)	1.166 (2)	0.9534 (12)	0.054350
C16	0.43400 (13)	0.58549 (14)	0.78283 (7)	0.0253 (3)
H16	0.5152 (18)	0.530 (2)	0.7828 (10)	0.038502
C17	0.32942 (16)	0.49897 (17)	0.78534 (9)	0.0373 (4)
H17A	0.2413 (19)	0.547 (2)	0.7844 (10)	0.039737
H17B	0.340 (2)	0.442 (2)	0.8245 (10)	0.040400
H17C	0.307 (2)	0.444 (2)	0.7460 (10)	0.047522
C18	0.40729 (18)	0.65675 (19)	0.72553 (8)	0.0377 (4)
H18A	0.391 (2)	0.596 (2)	0.6880 (10)	0.051773
H18B	0.483 (2)	0.717 (2)	0.7206 (10)	0.046636
H18C	0.324 (2)	0.710 (2)	0.7228 (10)	0.044260
C19	0.51423 (14)	0.57327 (14)	0.90885 (7)	0.0270 (3)
H19	0.4275 (18)	0.5340 (19)	0.9111 (9)	0.033482
C20	0.56346 (19)	0.63483 (19)	0.96753 (8)	0.0405 (4)
H20A	0.580 (2)	0.568 (2)	1.0032 (10)	0.046909
H20B	0.500 (2)	0.704 (2)	0.9778 (10)	0.039361
H20C	0.6509 (19)	0.675 (2)	0.9657 (10)	0.045138
C21	0.6009 (2)	0.4727 (2)	0.89880 (10)	0.0464 (5)
H21A	0.691 (2)	0.505 (2)	0.8957 (11)	0.049716
H21B	0.565 (2)	0.425 (2)	0.8601 (11)	0.048187
H21C	0.613 (2)	0.406 (2)	0.9352 (11)	0.051882
C22	0.59710 (12)	0.77490 (14)	0.83774 (7)	0.0224 (3)
H22	0.5531 (19)	0.827 (2)	0.7996 (10)	0.037401
C23	0.63915 (15)	0.86720 (16)	0.88635 (8)	0.0316 (3)
H23A	0.693 (2)	0.827 (2)	0.9249 (11)	0.046500
H23B	0.5633 (19)	0.913 (2)	0.8978 (10)	0.041464
H23C	0.698 (2)	0.934 (2)	0.8727 (11)	0.049436
C24	0.70611 (14)	0.70563 (17)	0.82477 (9)	0.0332 (4)
H24A	0.767 (2)	0.769 (2)	0.8088 (11)	0.051887
H24B	0.678 (2)	0.640 (2)	0.7907 (11)	0.046883
H24C	0.762 (2)	0.664 (2)	0.8647 (11)	0.048432

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Rh	0.01393 (5)	0.01723 (5)	0.01800 (5)	0.00039 (4)	0.00400 (4)	0.00055 (4)
H	0.032680	0.038910	0.023480	0.001840	0.001720	0.000740
Cl	0.02371 (16)	0.03180 (18)	0.03087 (18)	0.00467 (14)	0.01098 (14)	0.01211 (14)
B	0.0166 (6)	0.0210 (7)	0.0219 (7)	−0.0004 (5)	0.0056 (5)	0.0009 (6)
P1	0.01782 (15)	0.01936 (16)	0.02237 (16)	0.00193 (12)	0.00495 (13)	−0.00073 (13)
P2	0.01510 (15)	0.01961 (16)	0.02142 (16)	0.00074 (12)	0.00471 (12)	−0.00030 (13)
O1	0.0197 (5)	0.0242 (5)	0.0199 (5)	−0.0018 (4)	0.0035 (4)	0.0013 (4)
O2	0.0209 (5)	0.0264 (5)	0.0235 (5)	−0.0021 (4)	0.0018 (4)	0.0052 (4)
C1	0.0196 (6)	0.0198 (6)	0.0225 (6)	−0.0004 (5)	0.0063 (5)	−0.0014 (5)
C2	0.0215 (6)	0.0219 (7)	0.0250 (7)	−0.0008 (5)	0.0052 (5)	0.0039 (5)
C3	0.0309 (8)	0.0306 (8)	0.0349 (8)	−0.0039 (7)	0.0054 (7)	0.0113 (7)
H3	0.044560	0.049990	0.047290	−0.000690	0.009350	0.021180
C4	0.0322 (8)	0.0274 (8)	0.0435 (10)	−0.0062 (6)	0.0101 (7)	0.0099 (7)
H4	0.051820	0.044950	0.076950	−0.010800	0.024700	0.020040
C5	0.0245 (7)	0.0233 (7)	0.0396 (9)	−0.0044 (6)	0.0108 (6)	−0.0028 (6)
H5	0.037310	0.045470	0.074300	−0.018570	0.016380	−0.005920
C6	0.0197 (6)	0.0244 (7)	0.0284 (7)	−0.0015 (5)	0.0062 (6)	−0.0033 (6)
H6	0.030580	0.049060	0.039730	−0.008160	0.003690	−0.008700
C7	0.0240 (7)	0.0267 (7)	0.0232 (7)	0.0030 (6)	0.0078 (5)	−0.0039 (6)
H7	0.033690	0.034200	0.042930	0.005330	0.009210	−0.010490
C8	0.0271 (7)	0.0321 (8)	0.0283 (7)	0.0006 (6)	0.0119 (6)	−0.0008 (6)
H8A	0.030720	0.031730	0.044630	0.003940	0.007910	−0.002830
H8B	0.028400	0.043500	0.030660	0.002420	−0.001900	0.000740
H8C	0.039250	0.059320	0.029480	−0.007170	0.016690	−0.009640
C9	0.0342 (9)	0.0427 (10)	0.0231 (7)	0.0032 (7)	0.0051 (6)	−0.0048 (7)
H9A	0.038160	0.073290	0.028080	0.003260	0.010210	−0.009470
H9B	0.035710	0.048960	0.046550	−0.008900	0.000540	−0.013840
H9C	0.039690	0.041970	0.034190	0.008400	0.000910	−0.009450
C10	0.0209 (6)	0.0252 (7)	0.0257 (7)	0.0053 (5)	0.0043 (5)	0.0043 (6)
H10	0.037220	0.038570	0.046210	0.006370	0.015040	0.015080
C11	0.0297 (8)	0.0351 (9)	0.0398 (9)	0.0149 (7)	0.0062 (7)	0.0012 (7)
H11A	0.046520	0.055230	0.055160	0.024310	0.010060	0.017860
H11B	0.043670	0.038430	0.071720	0.006480	0.012400	−0.008410
H11C	0.040100	0.042870	0.059520	0.007420	0.022710	0.006680
C12	0.0205 (7)	0.0319 (8)	0.0244 (7)	0.0010 (6)	0.0023 (5)	0.0025 (6)
H12A	0.036650	0.044710	0.031710	−0.003110	0.013000	0.002330
H12B	0.031590	0.046320	0.038210	0.006920	0.013880	−0.001390
H12C	0.038680	0.057200	0.035400	0.011960	−0.005300	0.010060
C13	0.0287 (8)	0.0216 (7)	0.0410 (9)	−0.0005 (6)	0.0077 (7)	−0.0058 (6)
H13	0.038780	0.034260	0.061280	0.001180	0.015510	−0.013290
C14	0.0510 (12)	0.0265 (9)	0.0598 (13)	−0.0082 (8)	0.0158 (10)	0.0027 (8)
H14A	0.058430	0.028570	0.101870	−0.007630	0.019840	0.000620
H14B	0.041800	0.041110	0.089010	0.011490	0.019310	0.015560
H14C	0.058840	0.036690	0.073060	0.009560	0.028780	0.010100
C15	0.0295 (9)	0.0334 (9)	0.0615 (13)	−0.0056 (7)	−0.0008 (8)	−0.0146 (9)
H15A	0.036700	0.047240	0.056780	0.000310	0.016430	−0.007020
H15B	0.036480	0.039000	0.055290	−0.001010	0.007010	−0.002640
H15C	0.041110	0.034690	0.085850	−0.008890	0.010360	−0.023270
C16	0.0206 (6)	0.0261 (7)	0.0307 (7)	−0.0022 (5)	0.0085 (6)	−0.0075 (6)
H16	0.027780	0.041750	0.048330	0.005960	0.013380	−0.007270
C17	0.0310 (8)	0.0354 (9)	0.0487 (11)	−0.0130 (7)	0.0153 (8)	−0.0185 (8)
H17A	0.026390	0.038490	0.055320	0.004920	0.010910	−0.004880
H17B	0.037050	0.038640	0.046360	−0.000630	0.010780	−0.000010
H17C	0.044640	0.051450	0.049850	−0.008040	0.017620	−0.026300
C18	0.0425 (10)	0.0433 (10)	0.0261 (8)	−0.0042 (8)	0.0042 (7)	−0.0083 (7)
H18A	0.056330	0.066270	0.036100	0.000480	0.017420	−0.015170
H18B	0.033860	0.063660	0.045950	−0.005190	0.016480	0.004430
H18C	0.033620	0.063630	0.039260	0.013520	0.016120	0.005930
C19	0.0237 (7)	0.0271 (7)	0.0313 (8)	0.0066 (6)	0.0079 (6)	0.0077 (6)
H19	0.025170	0.032970	0.042320	0.001500	0.007210	0.003850
C20	0.0438 (10)	0.0431 (10)	0.0297 (8)	0.0065 (8)	−0.0027 (8)	0.0091 (8)
H20A	0.046030	0.050480	0.039790	0.004140	−0.000810	0.012750
H20B	0.031870	0.041560	0.041690	0.008440	0.001170	−0.003700
H20C	0.023320	0.060530	0.050010	−0.003370	0.004310	−0.004540
C21	0.0474 (11)	0.0422 (11)	0.0532 (12)	0.0245 (9)	0.0186 (10)	0.0153 (9)
H21A	0.028340	0.044670	0.079120	0.003210	0.018120	−0.000460
H21B	0.037700	0.041360	0.063070	0.006610	0.005260	−0.012330
H21C	0.049120	0.044000	0.062800	0.018180	0.012520	0.015150
C22	0.0159 (6)	0.0242 (7)	0.0274 (7)	−0.0017 (5)	0.0050 (5)	0.0001 (6)
H22	0.030800	0.041020	0.042390	0.001040	0.012290	0.006040
C23	0.0236 (7)	0.0294 (8)	0.0414 (9)	−0.0050 (6)	0.0064 (7)	−0.0092 (7)
H23A	0.037660	0.045230	0.051230	0.003680	−0.002620	−0.002220
H23B	0.026730	0.042840	0.056060	0.001720	0.011580	−0.008560
H23C	0.039090	0.045530	0.067760	−0.016160	0.020500	−0.004160
C24	0.0192 (7)	0.0346 (9)	0.0481 (10)	−0.0037 (6)	0.0123 (7)	−0.0106 (8)
H24A	0.033170	0.052090	0.077500	−0.003190	0.027700	0.002660
H24B	0.035300	0.051060	0.056000	0.002260	0.013550	−0.013210
H24C	0.035030	0.057520	0.052510	0.012270	0.008780	0.003260

Geometric parameters (Å, º)

Rh—H	1.522 (19)	C11—H11c	1.11 (2)
Rh—Cl	2.4214 (7)	C12—H12a	1.09 (2)
Rh—B	1.9672 (16)	C12—H12b	1.09 (2)
Rh—P1	2.3401 (6)	C12—H12c	1.09 (2)
Rh—P2	2.3376 (6)	C13—H13	1.11 (2)
H—B	2.01 (2)	C13—C14	1.532 (3)
B—O1	1.4205 (19)	C13—C15	1.531 (3)
B—O2	1.4167 (19)	C14—H14a	1.10 (3)
P1—C7	1.8650 (16)	C14—H14b	1.11 (2)
P1—C10	1.8522 (17)	C14—H14c	1.09 (3)
P1—C13	1.8801 (17)	C15—H15a	1.12 (2)
P2—C16	1.8515 (16)	C15—H15b	1.07 (2)
P2—C19	1.8599 (16)	C15—H15c	1.13 (2)
P2—C22	1.8554 (15)	C16—H16	1.10 (2)
O1—C1	1.3744 (17)	C16—C17	1.528 (2)
O2—C2	1.3772 (17)	C16—C18	1.531 (3)
C1—C2	1.387 (2)	C17—H17a	1.12 (2)
C1—C6	1.383 (2)	C17—H17b	1.10 (2)
C2—C3	1.384 (2)	C17—H17c	1.09 (2)
C3—H3	1.11 (2)	C18—H18a	1.09 (2)
C3—C4	1.403 (2)	C18—H18b	1.11 (2)
C4—H4	1.08 (2)	C18—H18c	1.10 (2)
C4—C5	1.393 (3)	C19—H19	1.08 (2)
C5—H5	1.09 (2)	C19—C20	1.529 (3)
C5—C6	1.398 (2)	C19—C21	1.531 (2)
C6—H6	1.10 (2)	C20—H20a	1.10 (2)
C7—H7	1.12 (2)	C20—H20b	1.11 (2)
C7—C8	1.533 (2)	C20—H20c	1.09 (2)
C7—C9	1.528 (2)	C21—H21a	1.09 (2)
C8—H8a	1.04 (2)	C21—H21b	1.05 (2)
C8—H8b	1.13 (2)	C21—H21c	1.11 (2)
C8—H8c	1.08 (2)	C22—H22	1.09 (2)
C9—H9a	1.12 (2)	C22—C23	1.530 (2)
C9—H9b	1.06 (2)	C22—C24	1.530 (2)
C9—H9c	1.06 (2)	C23—H23a	1.07 (2)
C10—H10	1.12 (2)	C23—H23b	1.07 (2)
C10—C11	1.534 (2)	C23—H23c	1.09 (2)
C10—C12	1.534 (2)	C24—H24a	1.10 (2)
C11—H11a	1.09 (2)	C24—H24b	1.08 (2)
C11—H11b	1.10 (2)	C24—H24c	1.11 (2)
Cl—Rh—H	153.2 (8)	H12a—C12—C10	110.9 (12)
B—Rh—H	68.9 (8)	H12b—C12—C10	110.5 (12)
B—Rh—Cl	137.85 (5)	H12b—C12—H12a	107.4 (17)
P1—Rh—H	89.9 (8)	H12c—C12—C10	111.8 (13)
P1—Rh—Cl	87.637 (13)	H12c—C12—H12a	109.8 (17)
P1—Rh—B	93.39 (5)	H12c—C12—H12b	106.2 (17)
P2—Rh—H	86.7 (8)	H13—C13—P1	107.7 (12)
P2—Rh—Cl	92.561 (13)	C14—C13—P1	115.38 (13)
P2—Rh—B	91.39 (5)	C14—C13—H13	106.2 (13)
P2—Rh—P1	172.650 (13)	C15—C13—P1	110.61 (12)
B—H—Rh	66.1 (7)	C15—C13—H13	107.7 (12)
H—B—Rh	45.0 (6)	C15—C13—C14	108.91 (16)
O1—B—Rh	120.09 (10)	H14a—C14—C13	110.0 (15)
O1—B—H	161.1 (6)	H14b—C14—C13	114.6 (13)
O2—B—Rh	131.98 (11)	H14b—C14—H14a	108.9 (19)
O2—B—H	88.0 (6)	H14c—C14—C13	111.6 (13)
O2—B—O1	107.92 (12)	H14c—C14—H14a	105 (2)
C7—P1—Rh	119.72 (5)	H14c—C14—H14b	107 (2)
C10—P1—Rh	114.26 (5)	H15a—C15—C13	109.2 (12)
C10—P1—C7	105.68 (7)	H15b—C15—C13	111.5 (12)
C13—P1—Rh	110.77 (5)	H15b—C15—H15a	107.6 (18)
C13—P1—C7	100.00 (7)	H15c—C15—C13	111.0 (13)
C13—P1—C10	104.54 (7)	H15c—C15—H15a	108.0 (18)
C16—P2—Rh	117.50 (5)	H15c—C15—H15b	109.5 (18)
C19—P2—Rh	114.50 (5)	H16—C16—P2	108.4 (11)
C19—P2—C16	102.74 (7)	C17—C16—P2	110.41 (11)
C22—P2—Rh	107.96 (5)	C17—C16—H16	107.1 (12)
C22—P2—C16	103.08 (7)	C18—C16—P2	113.06 (12)
C22—P2—C19	110.39 (7)	C18—C16—H16	107.2 (12)
C1—O1—B	106.83 (11)	C18—C16—C17	110.46 (14)
C2—O2—B	106.75 (11)	H17a—C17—C16	112.7 (12)
C2—C1—O1	109.19 (12)	H17b—C17—C16	116.3 (12)
C6—C1—O1	128.53 (13)	H17b—C17—H17a	103.3 (16)
C6—C1—C2	122.26 (13)	H17c—C17—C16	111.2 (12)
C1—C2—O2	109.29 (12)	H17c—C17—H17a	101.8 (16)
C3—C2—O2	128.77 (14)	H17c—C17—H17b	110.4 (18)
C3—C2—C1	121.91 (14)	H18a—C18—C16	110.7 (14)
H3—C3—C2	121.3 (12)	H18b—C18—C16	113.2 (12)
C4—C3—C2	116.27 (15)	H18b—C18—H18a	106.9 (18)
C4—C3—H3	122.4 (12)	H18c—C18—C16	109.6 (12)
H4—C4—C3	119.4 (14)	H18c—C18—H18a	107.2 (18)
C5—C4—C3	121.70 (15)	H18c—C18—H18b	109.1 (19)
C5—C4—H4	118.8 (14)	H19—C19—P2	100.3 (11)
H5—C5—C4	117.4 (14)	C20—C19—P2	112.47 (12)
C6—C5—C4	121.34 (14)	C20—C19—H19	107.2 (11)
C6—C5—H5	121.2 (14)	C21—C19—P2	117.06 (12)
C5—C6—C1	116.52 (14)	C21—C19—H19	108.8 (11)
H6—C6—C1	124.5 (12)	C21—C19—C20	110.11 (15)
H6—C6—C5	119.0 (12)	H20a—C20—C19	110.6 (13)
H7—C7—P1	104.5 (11)	H20b—C20—C19	112.3 (11)
C8—C7—P1	114.24 (10)	H20b—C20—H20a	108.5 (17)
C8—C7—H7	109.4 (11)	H20c—C20—C19	107.7 (12)
C9—C7—P1	111.78 (11)	H20c—C20—H20a	106.9 (17)
C9—C7—H7	106.5 (11)	H20c—C20—H20b	110.7 (17)
C9—C7—C8	110.03 (14)	H21a—C21—C19	113.4 (13)
H8a—C8—C7	111.7 (11)	H21b—C21—C19	110.9 (12)
H8b—C8—C7	111.7 (12)	H21b—C21—H21a	107.6 (19)
H8b—C8—H8a	108.1 (16)	H21c—C21—C19	110.2 (13)
H8c—C8—C7	107.9 (12)	H21c—C21—H21a	107.7 (18)
H8c—C8—H8a	107.9 (17)	H21c—C21—H21b	107 (2)
H8c—C8—H8b	109.4 (16)	H22—C22—P2	99.6 (11)
H9a—C9—C7	111.0 (12)	C23—C22—P2	113.33 (11)
H9b—C9—C7	115.0 (13)	C23—C22—H22	105.5 (12)
H9b—C9—H9a	104.5 (17)	C24—C22—P2	116.41 (11)
H9c—C9—C7	110.5 (11)	C24—C22—H22	110.3 (11)
H9c—C9—H9a	109.3 (18)	C24—C22—C23	110.55 (13)
H9c—C9—H9b	106.3 (17)	H23a—C23—C22	112.1 (13)
H10—C10—P1	100.5 (11)	H23b—C23—C22	111.4 (12)
C11—C10—P1	114.44 (11)	H23b—C23—H23a	108.6 (18)
C11—C10—H10	108.4 (11)	H23c—C23—C22	110.6 (13)
C12—C10—P1	112.57 (10)	H23c—C23—H23a	105.6 (18)
C12—C10—H10	108.2 (12)	H23c—C23—H23b	108.3 (18)
C12—C10—C11	111.87 (13)	H24a—C24—C22	109.0 (13)
H11a—C11—C10	109.0 (13)	H24b—C24—C22	111.4 (12)
H11b—C11—C10	113.3 (13)	H24b—C24—H24a	106.7 (18)
H11b—C11—H11a	108.7 (19)	H24c—C24—C22	112.1 (12)
H11c—C11—C10	111.6 (12)	H24c—C24—H24a	105.9 (18)
H11c—C11—H11a	106.6 (18)	H24c—C24—H24b	111.4 (19)
H11c—C11—H11b	107.4 (18)
Rh—B—O1—C1	−178.79 (11)	O1—C1—C6—C5	−178.74 (15)
Rh—B—O2—C2	179.01 (14)	O2—C2—C1—C6	−178.21 (11)
B—O1—C1—C2	−1.11 (12)	O2—C2—C3—C4	178.27 (18)
B—O1—C1—C6	177.28 (11)	C1—C2—C3—C4	0.63 (17)
B—O2—C2—C1	0.65 (12)	C1—C6—C5—C4	0.76 (17)
B—O2—C2—C3	−177.23 (13)	C2—C3—C4—C5	−0.4 (2)
O1—C1—C2—O2	0.29 (12)	C3—C4—C5—C6	−0.3 (2)
O1—C1—C2—C3	178.35 (12)

(SITKUB_HAR_SHADE3)

Crystal data

C24H47BClO2P2Rh	F(000) = 1213.326
Mr = 578.77	Dx = 1.348 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
a = 11.228 (3) Å	Cell parameters from 925 reflections
b = 11.101 (3) Å	θ = 12.0–24.6°
c = 23.414 (7) Å	µ = 0.82 mm^−1
β = 102.28 (4)°	T = 120 K
V = 2851.6 (14) Å^3	Fragment, colourless
Z = 4	0.6 × 0.4 × 0.2 mm

Data collection

SMART 1K CCD area detector diffractometer	7021 reflections with I ≥ 2u(I)
Radiation source: fine-focus sealed tube	Rint = 0.029
Graphite monochromator	θmax = 29.1°, θmin = 1.8°
ω scans	h = −15→15
33082 measured reflections	k = −15→15
7624 independent reflections	l = −31→31

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.024	Only H-atom coordinates refined
wR(F^2) = 0.053	w = 1/[σ^2(Fo^2) + (0.0238P)^2 + 1.9702P] where P = (Fo^2 + 2Fc^2)/3
S = 0.97	(Δ/σ)max = 0.001
7624 reflections	Δρmax = 0.45 e Å^−3
421 parameters	Δρmin = −0.72 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Rh	0.311324 (9)	0.814890 (9)	0.861855 (4)	0.01630 (3)
H	0.3470 (19)	0.783 (2)	0.9265 (8)	0.033143
Cl	0.32708 (3)	0.93355 (4)	0.777002 (17)	0.02803 (8)
B	0.21250 (14)	0.68030 (14)	0.88081 (7)	0.0196 (3)
P1	0.17685 (3)	0.96113 (3)	0.882946 (16)	0.01975 (7)
P2	0.46545 (3)	0.68313 (3)	0.848428 (15)	0.01859 (7)
O1	0.10456 (9)	0.64530 (9)	0.84069 (4)	0.02137 (19)
O2	0.22705 (9)	0.60331 (10)	0.93007 (4)	0.0240 (2)
C1	0.05453 (12)	0.55187 (13)	0.86616 (6)	0.0204 (3)
C2	0.12874 (13)	0.52617 (13)	0.92014 (6)	0.0228 (3)
C3	0.09915 (16)	0.43764 (16)	0.95639 (8)	0.0324 (3)
H3	0.157 (2)	0.420 (2)	1.0001 (10)	0.049694
C4	−0.00953 (16)	0.37443 (15)	0.93523 (8)	0.0341 (4)
H4	−0.040 (2)	0.307 (2)	0.9627 (12)	0.059733
C5	−0.08365 (14)	0.40015 (14)	0.88093 (8)	0.0285 (3)
H5	−0.169 (2)	0.350 (2)	0.8684 (11)	0.054976
C6	−0.05319 (13)	0.49075 (14)	0.84512 (7)	0.0240 (3)
H6	−0.114 (2)	0.508 (2)	0.8023 (10)	0.042523
C7	0.09985 (13)	0.93777 (14)	0.94524 (6)	0.0242 (3)
H7	0.0578 (19)	1.027 (2)	0.9512 (10)	0.039134
C8	0.00040 (15)	0.84082 (16)	0.93438 (7)	0.0283 (3)
H8A	0.0369 (19)	0.7549 (19)	0.9318 (9)	0.036911
H8B	−0.0692 (19)	0.858 (2)	0.8925 (9)	0.037011
H8C	−0.044 (2)	0.842 (2)	0.9711 (9)	0.043692
C9	0.19136 (16)	0.91165 (18)	1.00216 (7)	0.0335 (4)
H9A	0.144 (2)	0.903 (2)	1.0397 (9)	0.048811
H9B	0.258 (2)	0.979 (2)	1.0155 (10)	0.047297
H9C	0.240 (2)	0.831 (2)	0.9984 (9)	0.040708
C10	0.05440 (13)	1.00357 (14)	0.81985 (7)	0.0240 (3)
H10	0.108 (2)	1.056 (2)	0.7930 (10)	0.041258
C11	−0.04331 (16)	1.08686 (17)	0.83512 (8)	0.0350 (4)
H11A	−0.096 (2)	1.127 (2)	0.7949 (11)	0.055186
H11B	−0.005 (2)	1.159 (2)	0.8655 (12)	0.053816
H11C	−0.109 (2)	1.036 (2)	0.8551 (11)	0.047531
C12	−0.00194 (14)	0.89406 (15)	0.78407 (7)	0.0259 (3)
H12A	−0.045 (2)	0.834 (2)	0.8102 (9)	0.037667
H12B	0.0682 (19)	0.842 (2)	0.7693 (9)	0.038593
H12C	−0.068 (2)	0.921 (2)	0.7448 (10)	0.047893
C13	0.25948 (15)	1.10612 (14)	0.90632 (8)	0.0304 (3)
H13	0.218 (2)	1.147 (2)	0.9406 (11)	0.046273
C14	0.2507 (2)	1.20161 (17)	0.85839 (10)	0.0452 (5)
H14A	0.307 (2)	1.280 (2)	0.8752 (13)	0.065562
H14B	0.156 (2)	1.233 (2)	0.8395 (13)	0.059315
H14C	0.288 (2)	1.169 (2)	0.8221 (12)	0.055846
C15	0.39409 (17)	1.08196 (18)	0.93301 (10)	0.0430 (5)
H15A	0.441 (2)	1.052 (2)	0.8977 (11)	0.046929
H15B	0.405 (2)	1.012 (2)	0.9652 (10)	0.045218
H15C	0.441 (2)	1.166 (2)	0.9534 (12)	0.057460
C16	0.43400 (13)	0.58549 (14)	0.78283 (7)	0.0253 (3)
H16	0.5151 (19)	0.530 (2)	0.7828 (10)	0.040502
C17	0.32942 (16)	0.49897 (17)	0.78534 (9)	0.0373 (4)
H17A	0.2414 (19)	0.547 (2)	0.7844 (10)	0.040510
H17B	0.340 (2)	0.442 (2)	0.8245 (10)	0.041726
H17C	0.307 (2)	0.444 (2)	0.7460 (10)	0.049566
C18	0.40729 (18)	0.65675 (19)	0.72553 (8)	0.0377 (4)
H18A	0.391 (2)	0.596 (2)	0.6880 (10)	0.054372
H18B	0.483 (2)	0.717 (2)	0.7206 (10)	0.049065
H18C	0.324 (2)	0.710 (2)	0.7228 (10)	0.045377
C19	0.51424 (14)	0.57327 (14)	0.90885 (7)	0.0270 (3)
H19	0.4276 (18)	0.5340 (19)	0.9111 (9)	0.033962
C20	0.56346 (19)	0.63483 (19)	0.96754 (8)	0.0405 (4)
H20A	0.581 (2)	0.568 (2)	1.0032 (10)	0.049112
H20B	0.500 (2)	0.704 (2)	0.9778 (10)	0.040337
H20C	0.651 (2)	0.675 (2)	0.9657 (10)	0.046864
C21	0.6009 (2)	0.4727 (2)	0.89879 (10)	0.0464 (5)
H21A	0.691 (2)	0.505 (2)	0.8958 (11)	0.052040
H21B	0.565 (2)	0.425 (2)	0.8601 (11)	0.050134
H21C	0.613 (2)	0.406 (2)	0.9351 (12)	0.054350
C22	0.59710 (12)	0.77490 (14)	0.83774 (7)	0.0224 (3)
H22	0.5531 (19)	0.827 (2)	0.7996 (10)	0.038561
C23	0.63915 (15)	0.86720 (16)	0.88635 (8)	0.0316 (3)
H23A	0.693 (2)	0.827 (2)	0.9249 (11)	0.048518
H23B	0.5633 (19)	0.913 (2)	0.8979 (10)	0.042690
H23C	0.698 (2)	0.934 (2)	0.8727 (11)	0.052174
C24	0.70611 (14)	0.70563 (16)	0.82477 (9)	0.0332 (4)
H24A	0.767 (2)	0.769 (2)	0.8087 (12)	0.055059
H24B	0.678 (2)	0.640 (2)	0.7907 (11)	0.049444
H24C	0.762 (2)	0.664 (2)	0.8647 (11)	0.051101

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Rh	0.01394 (5)	0.01724 (5)	0.01800 (5)	0.00039 (4)	0.00400 (4)	0.00055 (4)
H	0.033540	0.039930	0.023880	0.001860	0.001440	0.000600
Cl	0.02371 (16)	0.03181 (18)	0.03088 (18)	0.00467 (14)	0.01098 (14)	0.01211 (14)
B	0.0166 (6)	0.0210 (7)	0.0219 (7)	−0.0004 (5)	0.0056 (5)	0.0009 (6)
P1	0.01782 (15)	0.01937 (16)	0.02237 (16)	0.00193 (12)	0.00495 (13)	−0.00073 (13)
P2	0.01510 (15)	0.01962 (16)	0.02142 (16)	0.00074 (12)	0.00471 (12)	−0.00030 (13)
O1	0.0197 (5)	0.0242 (5)	0.0199 (5)	−0.0018 (4)	0.0035 (4)	0.0013 (4)
O2	0.0209 (5)	0.0264 (5)	0.0235 (5)	−0.0021 (4)	0.0018 (4)	0.0052 (4)
C1	0.0196 (6)	0.0199 (6)	0.0225 (6)	−0.0004 (5)	0.0063 (5)	−0.0014 (5)
C2	0.0215 (6)	0.0219 (7)	0.0250 (7)	−0.0008 (5)	0.0053 (5)	0.0039 (5)
C3	0.0310 (8)	0.0306 (8)	0.0349 (8)	−0.0038 (7)	0.0054 (7)	0.0113 (7)
H3	0.047490	0.053170	0.047840	−0.001170	0.008830	0.022880
C4	0.0321 (8)	0.0274 (8)	0.0435 (9)	−0.0061 (6)	0.0101 (7)	0.0099 (7)
H4	0.055340	0.048760	0.079790	−0.012620	0.024900	0.022390
C5	0.0245 (7)	0.0233 (7)	0.0396 (9)	−0.0044 (6)	0.0108 (6)	−0.0028 (6)
H5	0.039660	0.048880	0.078000	−0.020740	0.016130	−0.004990
C6	0.0197 (6)	0.0244 (7)	0.0284 (7)	−0.0015 (5)	0.0063 (6)	−0.0033 (6)
H6	0.031860	0.052160	0.041350	−0.009170	0.002850	−0.009040
C7	0.0240 (7)	0.0267 (7)	0.0233 (7)	0.0030 (6)	0.0078 (5)	−0.0039 (6)
H7	0.035810	0.036050	0.046230	0.006050	0.010270	−0.011390
C8	0.0271 (7)	0.0321 (8)	0.0283 (7)	0.0006 (6)	0.0119 (6)	−0.0008 (6)
H8A	0.031800	0.033530	0.045480	0.003700	0.008390	−0.002550
H8B	0.029150	0.045940	0.032420	0.002790	−0.001360	0.001050
H8C	0.041220	0.063200	0.031220	−0.006990	0.017950	−0.010020
C9	0.0342 (8)	0.0427 (10)	0.0231 (7)	0.0032 (7)	0.0051 (6)	−0.0048 (7)
H9A	0.041250	0.077780	0.029050	0.003560	0.011170	−0.010440
H9B	0.038170	0.051680	0.048250	−0.008850	0.000680	−0.015420
H9C	0.041140	0.043210	0.034620	0.008400	0.000980	−0.009440
C10	0.0209 (6)	0.0252 (7)	0.0257 (7)	0.0053 (5)	0.0043 (5)	0.0043 (6)
H10	0.038650	0.039130	0.048810	0.006430	0.015620	0.015760
C11	0.0297 (8)	0.0351 (9)	0.0398 (9)	0.0150 (7)	0.0062 (7)	0.0012 (7)
H11A	0.048380	0.057810	0.058900	0.025700	0.010360	0.019270
H11B	0.045700	0.039780	0.076070	0.007280	0.013180	−0.009460
H11C	0.040900	0.045570	0.061560	0.008210	0.023100	0.006460
C12	0.0206 (7)	0.0318 (8)	0.0244 (7)	0.0010 (6)	0.0023 (5)	0.0025 (6)
H12A	0.036990	0.045900	0.032600	−0.003410	0.012990	0.002160
H12B	0.032400	0.047560	0.038650	0.006770	0.013910	−0.001260
H12C	0.040020	0.060540	0.036990	0.012600	−0.005570	0.011130
C13	0.0287 (8)	0.0216 (7)	0.0410 (9)	−0.0005 (6)	0.0076 (7)	−0.0057 (6)
H13	0.041040	0.035620	0.064250	0.001670	0.015890	−0.014600
C14	0.0511 (12)	0.0265 (9)	0.0597 (13)	−0.0082 (8)	0.0159 (10)	0.0027 (8)
H14A	0.061180	0.029140	0.107430	−0.007930	0.020320	0.000240
H14B	0.044450	0.042350	0.093480	0.012660	0.019910	0.016940
H14C	0.060580	0.037790	0.075750	0.009600	0.029270	0.011280
C15	0.0295 (9)	0.0334 (9)	0.0615 (13)	−0.0056 (7)	−0.0008 (8)	−0.0146 (9)
H15A	0.037590	0.047730	0.058310	0.000230	0.016580	−0.006350
H15B	0.037720	0.040240	0.056160	−0.001050	0.006540	−0.003350
H15C	0.043720	0.035700	0.091300	−0.009500	0.010630	−0.024630
C16	0.0206 (6)	0.0261 (7)	0.0307 (7)	−0.0022 (5)	0.0085 (6)	−0.0075 (6)
H16	0.029630	0.043650	0.050660	0.006760	0.014000	−0.008070
C17	0.0309 (8)	0.0354 (9)	0.0487 (11)	−0.0130 (7)	0.0153 (8)	−0.0185 (8)
H17A	0.027640	0.039480	0.055140	0.004820	0.010440	−0.005070
H17B	0.038960	0.038820	0.047920	−0.000590	0.010410	−0.000120
H17C	0.047220	0.054080	0.050540	−0.007860	0.017450	−0.027750
C18	0.0425 (10)	0.0433 (10)	0.0260 (8)	−0.0042 (8)	0.0042 (7)	−0.0082 (7)
H18A	0.059320	0.070150	0.037250	0.001060	0.018360	−0.016210
H18B	0.036150	0.067190	0.047940	−0.004750	0.018110	0.005030
H18C	0.035180	0.065260	0.039440	0.013810	0.016350	0.006260
C19	0.0237 (7)	0.0271 (7)	0.0313 (8)	0.0066 (6)	0.0079 (6)	0.0077 (6)
H19	0.026130	0.033110	0.042420	0.001270	0.006780	0.003340
C20	0.0438 (10)	0.0431 (10)	0.0297 (8)	0.0065 (8)	−0.0028 (8)	0.0091 (8)
H20A	0.048060	0.052520	0.041660	0.004610	−0.001900	0.013300
H20B	0.033000	0.042600	0.042090	0.008120	0.000530	−0.004440
H20C	0.024120	0.061810	0.052690	−0.003310	0.003740	−0.005070
C21	0.0474 (11)	0.0422 (11)	0.0532 (12)	0.0245 (9)	0.0186 (10)	0.0153 (9)
H21A	0.029580	0.046670	0.082580	0.004070	0.018010	−0.001170
H21B	0.039640	0.042450	0.065640	0.007330	0.005200	−0.013230
H21C	0.051400	0.045390	0.065880	0.019150	0.011620	0.015610
C22	0.0159 (6)	0.0242 (7)	0.0274 (7)	−0.0017 (5)	0.0050 (5)	0.0000 (6)
H22	0.031860	0.042470	0.043550	0.001230	0.012950	0.006500
C23	0.0236 (7)	0.0294 (8)	0.0414 (9)	−0.0049 (6)	0.0064 (7)	−0.0093 (7)
H23A	0.038300	0.047260	0.054200	0.003580	−0.003170	−0.002740
H23B	0.027620	0.043430	0.058130	0.001470	0.011610	−0.008790
H23C	0.040180	0.047770	0.072750	−0.016810	0.021390	−0.004030
C24	0.0192 (7)	0.0346 (9)	0.0482 (10)	−0.0037 (6)	0.0123 (7)	−0.0106 (7)
H24A	0.034550	0.055890	0.082350	−0.003150	0.029520	0.002980
H24B	0.037040	0.054440	0.058990	0.003070	0.015010	−0.013850
H24C	0.035790	0.060350	0.056760	0.012960	0.008940	0.002910

Geometric parameters (Å, º)

Rh—H	1.523 (19)	C11—H11c	1.11 (2)
Rh—Cl	2.4214 (7)	C12—H12a	1.09 (2)
Rh—B	1.9673 (16)	C12—H12b	1.09 (2)
Rh—P1	2.3401 (6)	C12—H12c	1.09 (2)
Rh—P2	2.3376 (6)	C13—H13	1.10 (2)
H—B	2.01 (2)	C13—C14	1.532 (3)
B—O1	1.4205 (19)	C13—C15	1.531 (3)
B—O2	1.4167 (19)	C14—H14a	1.10 (3)
P1—C7	1.8650 (16)	C14—H14b	1.11 (2)
P1—C10	1.8523 (17)	C14—H14c	1.09 (3)
P1—C13	1.8801 (17)	C15—H15a	1.12 (2)
P2—C16	1.8515 (16)	C15—H15b	1.07 (2)
P2—C19	1.8599 (16)	C15—H15c	1.13 (2)
P2—C22	1.8554 (15)	C16—H16	1.10 (2)
O1—C1	1.3745 (17)	C16—C17	1.528 (2)
O2—C2	1.3772 (17)	C16—C18	1.531 (2)
C1—C2	1.387 (2)	C17—H17a	1.12 (2)
C1—C6	1.383 (2)	C17—H17b	1.10 (2)
C2—C3	1.384 (2)	C17—H17c	1.09 (2)
C3—H3	1.11 (2)	C18—H18a	1.09 (2)
C3—C4	1.404 (2)	C18—H18b	1.11 (2)
C4—H4	1.08 (2)	C18—H18c	1.10 (2)
C4—C5	1.393 (3)	C19—H19	1.08 (2)
C5—H5	1.09 (2)	C19—C20	1.529 (3)
C5—C6	1.398 (2)	C19—C21	1.531 (2)
C6—H6	1.10 (2)	C20—H20a	1.10 (2)
C7—H7	1.12 (2)	C20—H20b	1.10 (2)
C7—C8	1.533 (2)	C20—H20c	1.09 (2)
C7—C9	1.528 (2)	C21—H21a	1.09 (2)
C8—H8a	1.05 (2)	C21—H21b	1.05 (2)
C8—H8b	1.13 (2)	C21—H21c	1.11 (2)
C8—H8c	1.08 (2)	C22—H22	1.09 (2)
C9—H9a	1.12 (2)	C22—C23	1.530 (2)
C9—H9b	1.06 (2)	C22—C24	1.530 (2)
C9—H9c	1.06 (2)	C23—H23a	1.07 (2)
C10—H10	1.12 (2)	C23—H23b	1.07 (2)
C10—C11	1.534 (2)	C23—H23c	1.08 (2)
C10—C12	1.534 (2)	C24—H24a	1.10 (2)
C11—H11a	1.09 (2)	C24—H24b	1.08 (2)
C11—H11b	1.10 (3)	C24—H24c	1.11 (2)
Cl—Rh—H	153.2 (8)	H12a—C12—C10	111.0 (12)
B—Rh—H	68.9 (8)	H12b—C12—C10	110.5 (12)
B—Rh—Cl	137.85 (5)	H12b—C12—H12a	107.4 (17)
P1—Rh—H	89.8 (8)	H12c—C12—C10	111.8 (14)
P1—Rh—Cl	87.637 (13)	H12c—C12—H12a	109.7 (17)
P1—Rh—B	93.39 (5)	H12c—C12—H12b	106.2 (17)
P2—Rh—H	86.7 (8)	H13—C13—P1	107.8 (12)
P2—Rh—Cl	92.561 (13)	C14—C13—P1	115.37 (13)
P2—Rh—B	91.39 (5)	C14—C13—H13	106.2 (13)
P2—Rh—P1	172.651 (13)	C15—C13—P1	110.61 (12)
B—H—Rh	66.1 (7)	C15—C13—H13	107.6 (12)
H—B—Rh	45.0 (6)	C15—C13—C14	108.91 (16)
O1—B—Rh	120.09 (10)	H14a—C14—C13	110.0 (15)
O1—B—H	161.1 (6)	H14b—C14—C13	114.6 (14)
O2—B—Rh	131.98 (11)	H14b—C14—H14a	108.9 (19)
O2—B—H	88.0 (6)	H14c—C14—C13	111.6 (13)
O2—B—O1	107.93 (12)	H14c—C14—H14a	105 (2)
C7—P1—Rh	119.72 (5)	H14c—C14—H14b	107 (2)
C10—P1—Rh	114.26 (5)	H15a—C15—C13	109.1 (12)
C10—P1—C7	105.68 (7)	H15b—C15—C13	111.5 (12)
C13—P1—Rh	110.77 (5)	H15b—C15—H15a	107.6 (18)
C13—P1—C7	99.99 (7)	H15c—C15—C13	111.0 (13)
C13—P1—C10	104.54 (7)	H15c—C15—H15a	108.0 (18)
C16—P2—Rh	117.50 (5)	H15c—C15—H15b	109.5 (19)
C19—P2—Rh	114.50 (5)	H16—C16—P2	108.4 (12)
C19—P2—C16	102.74 (7)	C17—C16—P2	110.40 (11)
C22—P2—Rh	107.96 (5)	C17—C16—H16	107.0 (12)
C22—P2—C16	103.08 (7)	C18—C16—P2	113.06 (12)
C22—P2—C19	110.39 (7)	C18—C16—H16	107.2 (12)
C1—O1—B	106.83 (11)	C18—C16—C17	110.46 (14)
C2—O2—B	106.74 (11)	H17a—C17—C16	112.7 (12)
C2—C1—O1	109.18 (12)	H17b—C17—C16	116.3 (12)
C6—C1—O1	128.53 (13)	H17b—C17—H17a	103.3 (16)
C6—C1—C2	122.27 (13)	H17c—C17—C16	111.2 (13)
C1—C2—O2	109.30 (12)	H17c—C17—H17a	101.8 (17)
C3—C2—O2	128.76 (14)	H17c—C17—H17b	110.5 (18)
C3—C2—C1	121.90 (14)	H18a—C18—C16	110.6 (14)
H3—C3—C2	121.3 (12)	H18b—C18—C16	113.2 (13)
C4—C3—C2	116.27 (15)	H18b—C18—H18a	106.9 (18)
C4—C3—H3	122.5 (12)	H18c—C18—C16	109.7 (12)
H4—C4—C3	119.5 (15)	H18c—C18—H18a	107.1 (18)
C5—C4—C3	121.70 (15)	H18c—C18—H18b	109.1 (19)
C5—C4—H4	118.7 (14)	H19—C19—P2	100.3 (11)
H5—C5—C4	117.5 (14)	C20—C19—P2	112.47 (12)
C6—C5—C4	121.34 (14)	C20—C19—H19	107.2 (11)
C6—C5—H5	121.1 (14)	C21—C19—P2	117.06 (12)
C5—C6—C1	116.51 (14)	C21—C19—H19	108.8 (11)
H6—C6—C1	124.5 (12)	C21—C19—C20	110.12 (15)
H6—C6—C5	119.0 (12)	H20a—C20—C19	110.6 (13)
H7—C7—P1	104.5 (12)	H20b—C20—C19	112.3 (12)
C8—C7—P1	114.24 (10)	H20b—C20—H20a	108.5 (17)
C8—C7—H7	109.3 (11)	H20c—C20—C19	107.6 (13)
C9—C7—P1	111.78 (11)	H20c—C20—H20a	106.8 (17)
C9—C7—H7	106.5 (11)	H20c—C20—H20b	110.8 (17)
C9—C7—C8	110.03 (14)	H21a—C21—C19	113.3 (13)
H8a—C8—C7	111.7 (11)	H21b—C21—C19	110.8 (13)
H8b—C8—C7	111.7 (12)	H21b—C21—H21a	107.6 (19)
H8b—C8—H8a	108.1 (16)	H21c—C21—C19	110.2 (13)
H8c—C8—C7	107.9 (12)	H21c—C21—H21a	107.7 (18)
H8c—C8—H8a	107.8 (18)	H21c—C21—H21b	107 (2)
H8c—C8—H8b	109.5 (16)	H22—C22—P2	99.6 (11)
H9a—C9—C7	111.0 (12)	C23—C22—P2	113.33 (11)
H9b—C9—C7	115.0 (13)	C23—C22—H22	105.5 (12)
H9b—C9—H9a	104.4 (18)	C24—C22—P2	116.41 (11)
H9c—C9—C7	110.5 (12)	C24—C22—H22	110.3 (11)
H9c—C9—H9a	109.3 (18)	C24—C22—C23	110.55 (13)
H9c—C9—H9b	106.2 (17)	H23a—C23—C22	112.1 (13)
H10—C10—P1	100.5 (11)	H23b—C23—C22	111.5 (12)
C11—C10—P1	114.44 (11)	H23b—C23—H23a	108.6 (18)
C11—C10—H10	108.4 (11)	H23c—C23—C22	110.5 (13)
C12—C10—P1	112.57 (10)	H23c—C23—H23a	105.5 (18)
C12—C10—H10	108.2 (12)	H23c—C23—H23b	108.4 (18)
C12—C10—C11	111.87 (13)	H24a—C24—C22	109.0 (13)
H11a—C11—C10	109.0 (13)	H24b—C24—C22	111.3 (12)
H11b—C11—C10	113.2 (13)	H24b—C24—H24a	106.7 (19)
H11b—C11—H11a	109 (2)	H24c—C24—C22	112.1 (13)
H11c—C11—C10	111.6 (12)	H24c—C24—H24a	105.9 (19)
H11c—C11—H11a	106.7 (18)	H24c—C24—H24b	111.5 (19)
H11c—C11—H11b	107.4 (18)
Rh—B—O1—C1	−178.79 (11)	O1—C1—C6—C5	−178.74 (15)
Rh—B—O2—C2	179.01 (14)	O2—C2—C1—C6	−178.21 (11)
B—O1—C1—C2	−1.11 (12)	O2—C2—C3—C4	178.28 (18)
B—O1—C1—C6	177.27 (11)	C1—C2—C3—C4	0.63 (17)
B—O2—C2—C1	0.65 (12)	C1—C6—C5—C4	0.76 (17)
B—O2—C2—C3	−177.23 (13)	C2—C3—C4—C5	−0.4 (2)
O1—C1—C2—O2	0.29 (12)	C3—C4—C5—C6	−0.3 (2)
O1—C1—C2—C3	178.35 (12)

(SITKUB_IAM_0_HADPs)

Crystal data

C24H47BClO2P2Rh	F(000) = 1213.437
Mr = 578.77	Dx = 1.348 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
a = 11.228 (3) Å	Cell parameters from 925 reflections
b = 11.101 (3) Å	θ = 12.0–24.6°
c = 23.414 (7) Å	µ = 0.82 mm^−1
β = 102.28 (4)°	T = 120 K
V = 2851.6 (14) Å^3	Fragment, colourless
Z = 4	0.6 × 0.4 × 0.2 mm

Data collection

SMART 1K CCD area detector diffractometer	7021 reflections with I ≥ 2u(I)
Radiation source: fine-focus sealed tube	Rint = 0.029
Graphite monochromator	θmax = 29.1°, θmin = 1.8°
ω scans	h = −15→15
33082 measured reflections	k = −15→15
7624 independent reflections	l = −31→31

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.031	Only H-atom coordinates refined
wR(F^2) = 0.071	w = 1/[σ^2(Fo^2) + (0.027P)^2 + 3.773P] where P = (Fo^2 + 2Fc^2)/3
S = 1.07	(Δ/σ)max = 0.001
7624 reflections	Δρmax = 0.51 e Å^−3
421 parameters	Δρmin = −0.77 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Rh	0.311323 (12)	0.814898 (13)	0.861849 (6)	0.01565 (4)
H	0.3434 (17)	0.7914 (17)	0.9219 (8)	0.000000
Cl	0.32708 (4)	0.93356 (5)	0.77699 (2)	0.02676 (10)
B	0.21275 (19)	0.68056 (19)	0.88084 (9)	0.0184 (4)
P1	0.17689 (4)	0.96109 (4)	0.88294 (2)	0.01850 (9)
P2	0.46544 (4)	0.68315 (4)	0.84843 (2)	0.01733 (9)
O1	0.10454 (12)	0.64545 (13)	0.84060 (6)	0.0197 (3)
O2	0.22743 (12)	0.60352 (13)	0.93015 (6)	0.0224 (3)
C1	0.05457 (17)	0.55162 (17)	0.86629 (8)	0.0193 (3)
C2	0.12846 (17)	0.52587 (18)	0.92002 (9)	0.0214 (4)
C3	0.0989 (2)	0.4377 (2)	0.95630 (10)	0.0309 (5)
H3	0.1501 (17)	0.4187 (17)	0.9931 (8)	0.000000
C4	−0.0097 (2)	0.3748 (2)	0.93500 (11)	0.0328 (5)
H4	−0.0313 (17)	0.3171 (17)	0.9584 (8)	0.000000
C5	−0.08335 (19)	0.40030 (19)	0.88101 (10)	0.0272 (4)
H5	−0.1533 (18)	0.3582 (18)	0.8704 (8)	0.000000
C6	−0.05308 (18)	0.49057 (19)	0.84519 (9)	0.0227 (4)
H6	−0.1021 (17)	0.5072 (17)	0.8089 (8)	0.000000
C7	0.09986 (18)	0.93774 (19)	0.94527 (9)	0.0228 (4)
H7	0.0628 (17)	1.0168 (17)	0.9491 (8)	0.000000
C8	0.0006 (2)	0.8408 (2)	0.93442 (10)	0.0268 (4)
H8a	0.0341 (17)	0.7652 (18)	0.9325 (8)	0.000000
H8b	−0.0607 (17)	0.8564 (17)	0.8988 (8)	0.000000
H8c	−0.0391 (17)	0.8437 (17)	0.9666 (8)	0.000000
C9	0.1913 (2)	0.9116 (2)	1.00217 (10)	0.0315 (5)
H9a	0.1487 (17)	0.9047 (17)	1.0342 (8)	0.000000
H9b	0.2488 (18)	0.9701 (18)	1.0132 (8)	0.000000
H9c	0.2311 (17)	0.8427 (18)	0.9988 (8)	0.000000
C10	0.05444 (18)	1.00348 (19)	0.81987 (9)	0.0229 (4)
H10	0.1007 (17)	1.0471 (17)	0.7967 (8)	0.000000
C11	−0.0433 (2)	1.0868 (2)	0.83509 (11)	0.0330 (5)
H11a	−0.0876 (17)	1.1196 (17)	0.8004 (8)	0.000000
H11b	−0.0106 (17)	1.1491 (18)	0.8598 (8)	0.000000
H11c	−0.0988 (17)	1.0412 (17)	0.8533 (8)	0.000000
C12	−0.00182 (18)	0.8941 (2)	0.78416 (9)	0.0243 (4)
H12a	−0.0376 (17)	0.8414 (18)	0.8063 (8)	0.000000
H12b	0.0589 (17)	0.8483 (18)	0.7713 (8)	0.000000
H12c	−0.0564 (17)	0.9196 (17)	0.7514 (8)	0.000000
C13	0.2594 (2)	1.10601 (19)	0.90618 (11)	0.0288 (4)
H13	0.2208 (17)	1.1415 (17)	0.9368 (8)	0.000000
C14	0.2507 (3)	1.2016 (2)	0.85841 (14)	0.0426 (6)
H14a	0.2999 (17)	1.2694 (18)	0.8758 (8)	0.000000
H14b	0.1697 (18)	1.2269 (18)	0.8426 (8)	0.000000
H14c	0.2841 (17)	1.1737 (17)	0.8262 (9)	0.000000
C15	0.3938 (2)	1.0819 (2)	0.93301 (14)	0.0401 (6)
H15a	0.4324 (17)	1.0597 (18)	0.9038 (8)	0.000000
H15b	0.4033 (17)	1.0201 (18)	0.9620 (8)	0.000000
H15c	0.4352 (17)	1.1532 (18)	0.9522 (8)	0.000000
C16	0.43394 (18)	0.58560 (19)	0.78281 (9)	0.0240 (4)
H16	0.5025 (17)	0.5396 (17)	0.7834 (8)	0.000000
C17	0.3294 (2)	0.4988 (2)	0.78533 (12)	0.0352 (5)
H17a	0.2525 (17)	0.5407 (17)	0.7832 (8)	0.000000
H17b	0.3408 (17)	0.4502 (18)	0.8193 (9)	0.000000
H17c	0.3129 (17)	0.4481 (18)	0.7520 (8)	0.000000
C18	0.4074 (2)	0.6566 (3)	0.72559 (10)	0.0359 (5)
H18a	0.3931 (17)	0.6030 (17)	0.6930 (8)	0.000000
H18b	0.4701 (18)	0.7082 (18)	0.7223 (8)	0.000000
H18c	0.3348 (18)	0.7024 (17)	0.7236 (8)	0.000000
C19	0.51447 (19)	0.57323 (19)	0.90887 (9)	0.0255 (4)
H19	0.4430 (18)	0.5392 (17)	0.9110 (8)	0.000000
C20	0.5633 (3)	0.6348 (3)	0.96749 (11)	0.0386 (6)
H20a	0.5749 (17)	0.5745 (17)	0.9985 (8)	0.000000
H20b	0.5104 (18)	0.6942 (18)	0.9770 (8)	0.000000
H20c	0.6352 (18)	0.6688 (18)	0.9669 (8)	0.000000
C21	0.6009 (3)	0.4729 (3)	0.89898 (14)	0.0437 (6)
H21a	0.6832 (18)	0.5067 (17)	0.8987 (8)	0.000000
H21b	0.5743 (18)	0.4339 (18)	0.8683 (9)	0.000000
H21c	0.6121 (17)	0.4133 (17)	0.9324 (8)	0.000000
C22	0.59708 (17)	0.77491 (18)	0.83770 (9)	0.0210 (4)
H22	0.5610 (17)	0.8203 (17)	0.8042 (8)	0.000000
C23	0.6392 (2)	0.8671 (2)	0.88636 (11)	0.0295 (4)
H23a	0.6835 (18)	0.8342 (18)	0.9196 (9)	0.000000
H23b	0.5751 (18)	0.9071 (18)	0.8953 (8)	0.000000
H23c	0.6911 (17)	0.9302 (17)	0.8739 (8)	0.000000
C24	0.7061 (2)	0.7057 (2)	0.82472 (12)	0.0310 (5)
H24a	0.7599 (17)	0.7630 (17)	0.8105 (8)	0.000000
H24b	0.6859 (17)	0.6506 (18)	0.7969 (8)	0.000000
H24c	0.7490 (18)	0.6718 (17)	0.8590 (9)	0.000000

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Rh	0.01328 (7)	0.01661 (7)	0.01734 (7)	0.00040 (5)	0.00389 (5)	0.00059 (5)
H	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
Cl	0.0226 (2)	0.0305 (2)	0.0294 (2)	0.00451 (18)	0.01058 (18)	0.01204 (19)
B	0.0158 (9)	0.0199 (9)	0.0203 (9)	0.0013 (7)	0.0056 (7)	−0.0005 (8)
P1	0.0166 (2)	0.0182 (2)	0.0209 (2)	0.00176 (17)	0.00461 (17)	−0.00071 (17)
P2	0.0139 (2)	0.0183 (2)	0.0200 (2)	0.00061 (16)	0.00429 (16)	−0.00023 (17)
O1	0.0180 (6)	0.0220 (6)	0.0192 (6)	−0.0025 (5)	0.0039 (5)	0.0016 (5)
O2	0.0190 (6)	0.0240 (7)	0.0230 (7)	−0.0030 (5)	0.0020 (5)	0.0049 (5)
C1	0.0200 (8)	0.0173 (8)	0.0223 (8)	0.0004 (7)	0.0084 (7)	−0.0016 (7)
C2	0.0194 (8)	0.0201 (9)	0.0254 (9)	−0.0007 (7)	0.0059 (7)	0.0016 (7)
C3	0.0295 (11)	0.0293 (11)	0.0332 (11)	−0.0014 (9)	0.0053 (9)	0.0101 (9)
H3	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C4	0.0327 (11)	0.0247 (10)	0.0430 (13)	−0.0047 (9)	0.0129 (10)	0.0094 (9)
H4	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C5	0.0223 (9)	0.0217 (9)	0.0397 (12)	−0.0041 (8)	0.0110 (9)	−0.0052 (8)
H5	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C6	0.0182 (8)	0.0237 (9)	0.0264 (10)	0.0010 (7)	0.0055 (7)	−0.0042 (8)
H6	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C7	0.0225 (9)	0.0254 (10)	0.0219 (9)	0.0032 (7)	0.0075 (7)	−0.0040 (7)
H7	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C8	0.0259 (10)	0.0306 (11)	0.0263 (10)	0.0011 (8)	0.0114 (8)	−0.0010 (8)
H8a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H8b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H8c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C9	0.0324 (11)	0.0394 (13)	0.0224 (10)	0.0030 (10)	0.0055 (9)	−0.0049 (9)
H9a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H9b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H9c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C10	0.0197 (8)	0.0244 (9)	0.0244 (9)	0.0053 (7)	0.0043 (7)	0.0050 (7)
H10	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C11	0.0275 (11)	0.0334 (12)	0.0375 (12)	0.0140 (9)	0.0055 (9)	0.0012 (10)
H11a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H11b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H11c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C12	0.0188 (9)	0.0303 (10)	0.0230 (9)	0.0009 (8)	0.0023 (7)	0.0033 (8)
H12a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H12b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H12c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C13	0.0274 (10)	0.0198 (9)	0.0394 (12)	−0.0006 (8)	0.0074 (9)	−0.0062 (8)
H13	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C14	0.0460 (15)	0.0253 (12)	0.0574 (17)	−0.0080 (11)	0.0132 (13)	0.0018 (11)
H14a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H14b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H14c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C15	0.0284 (11)	0.0315 (12)	0.0565 (16)	−0.0053 (10)	0.0005 (11)	−0.0141 (12)
H15a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H15b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H15c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C16	0.0186 (9)	0.0247 (10)	0.0303 (10)	−0.0015 (7)	0.0084 (8)	−0.0077 (8)
H16	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C17	0.0301 (11)	0.0326 (12)	0.0459 (14)	−0.0124 (10)	0.0147 (10)	−0.0174 (11)
H17a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H17b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H17c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C18	0.0399 (13)	0.0408 (13)	0.0257 (11)	−0.0048 (11)	0.0042 (9)	−0.0083 (10)
H18a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H18b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H18c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C19	0.0219 (9)	0.0250 (10)	0.0305 (10)	0.0057 (8)	0.0079 (8)	0.0076 (8)
H19	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C20	0.0405 (14)	0.0421 (14)	0.0290 (11)	0.0058 (12)	−0.0023 (10)	0.0096 (10)
H20a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H20b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H20c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C21	0.0456 (15)	0.0399 (14)	0.0487 (16)	0.0226 (12)	0.0172 (13)	0.0133 (12)
H21a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H21b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H21c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C22	0.0141 (8)	0.0229 (9)	0.0262 (9)	−0.0020 (7)	0.0045 (7)	0.0000 (7)
H22	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C23	0.0219 (10)	0.0275 (11)	0.0386 (12)	−0.0040 (8)	0.0056 (9)	−0.0081 (9)
H23a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H23b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H23c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C24	0.0183 (9)	0.0321 (11)	0.0447 (13)	−0.0035 (8)	0.0114 (9)	−0.0101 (10)
H24a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H24b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H24c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000

Geometric parameters (Å, º)

Rh—H	1.399 (18)	C11—H11c	0.969 (19)
Rh—Cl	2.4214 (7)	C12—H12a	0.93 (2)
Rh—B	1.964 (2)	C12—H12b	0.950 (19)
Rh—P1	2.3395 (7)	C12—H12c	0.918 (19)
Rh—P2	2.3374 (7)	C13—H13	0.995 (19)
H—B	1.998 (19)	C13—C14	1.530 (4)
B—O1	1.424 (3)	C13—C15	1.529 (3)
B—O2	1.418 (2)	C14—H14a	0.972 (19)
P1—C7	1.866 (2)	C14—H14b	0.95 (2)
P1—C10	1.852 (2)	C14—H14c	0.96 (2)
P1—C13	1.878 (2)	C15—H15a	0.918 (19)
P2—C16	1.851 (2)	C15—H15b	0.95 (2)
P2—C19	1.861 (2)	C15—H15c	0.978 (19)
P2—C22	1.856 (2)	C16—H16	0.922 (19)
O1—C1	1.380 (2)	C16—C17	1.529 (3)
O2—C2	1.386 (2)	C16—C18	1.528 (3)
C1—C2	1.382 (3)	C17—H17a	0.973 (19)
C1—C6	1.382 (3)	C17—H17b	0.95 (2)
C2—C3	1.382 (3)	C17—H17c	0.947 (19)
C3—H3	0.952 (19)	C18—H18a	0.955 (19)
C3—C4	1.401 (3)	C18—H18b	0.92 (2)
C4—H4	0.909 (19)	C18—H18c	0.95 (2)
C4—C5	1.385 (3)	C19—H19	0.898 (19)
C5—H5	0.90 (2)	C19—C20	1.527 (3)
C5—C6	1.394 (3)	C19—C21	1.527 (3)
C6—H6	0.928 (19)	C20—H20a	0.975 (19)
C7—H7	0.983 (19)	C20—H20b	0.95 (2)
C7—C8	1.531 (3)	C20—H20c	0.89 (2)
C7—C9	1.527 (3)	C21—H21a	0.998 (19)
C8—H8a	0.92 (2)	C21—H21b	0.84 (2)
C8—H8b	0.978 (19)	C21—H21c	1.012 (19)
C8—H8c	0.954 (19)	C22—H22	0.947 (19)
C9—H9a	0.975 (19)	C22—C23	1.530 (3)
C9—H9b	0.91 (2)	C22—C24	1.530 (3)
C9—H9c	0.90 (2)	C23—H23a	0.91 (2)
C10—H10	0.957 (19)	C23—H23b	0.91 (2)
C10—C11	1.534 (3)	C23—H23c	0.995 (19)
C10—C12	1.532 (3)	C24—H24a	0.982 (19)
C11—H11a	0.932 (19)	C24—H24b	0.89 (2)
C11—H11b	0.93 (2)	C24—H24c	0.92 (2)
Cl—Rh—H	151.3 (8)	H12a—C12—C10	111.9 (12)
B—Rh—H	70.6 (8)	H12b—C12—C10	110.9 (12)
B—Rh—Cl	137.90 (6)	H12b—C12—H12a	105.4 (16)
P1—Rh—H	87.5 (8)	H12c—C12—C10	109.6 (12)
P1—Rh—Cl	87.642 (18)	H12c—C12—H12a	111.6 (16)
P1—Rh—B	93.39 (6)	H12c—C12—H12b	107.2 (16)
P2—Rh—H	88.8 (8)	H13—C13—P1	106.5 (11)
P2—Rh—Cl	92.561 (17)	C14—C13—P1	115.55 (17)
P2—Rh—B	91.39 (6)	C14—C13—H13	106.4 (11)
P2—Rh—P1	172.647 (18)	C15—C13—P1	110.59 (16)
B—H—Rh	68.0 (8)	C15—C13—H13	108.4 (11)
H—B—Rh	41.4 (5)	C15—C13—C14	109.0 (2)
O1—B—Rh	120.04 (14)	H14a—C14—C13	106.8 (12)
O1—B—H	157.3 (6)	H14b—C14—C13	113.4 (12)
O2—B—Rh	131.98 (15)	H14b—C14—H14a	110.3 (16)
O2—B—H	91.9 (5)	H14c—C14—C13	112.0 (12)
O2—B—O1	107.97 (16)	H14c—C14—H14a	107.2 (16)
C7—P1—Rh	119.73 (7)	H14c—C14—H14b	107.0 (16)
C10—P1—Rh	114.26 (7)	H15a—C15—C13	108.8 (12)
C10—P1—C7	105.66 (9)	H15b—C15—C13	111.7 (12)
C13—P1—Rh	110.77 (7)	H15b—C15—H15a	109.7 (17)
C13—P1—C7	100.05 (10)	H15c—C15—C13	112.2 (11)
C13—P1—C10	104.49 (10)	H15c—C15—H15a	107.8 (16)
C16—P2—Rh	117.47 (7)	H15c—C15—H15b	106.6 (16)
C19—P2—Rh	114.56 (7)	H16—C16—P2	107.4 (12)
C19—P2—C16	102.77 (10)	C17—C16—P2	110.44 (15)
C22—P2—Rh	107.97 (7)	C17—C16—H16	107.2 (12)
C22—P2—C16	103.06 (9)	C18—C16—P2	113.14 (16)
C22—P2—C19	110.34 (9)	C18—C16—H16	107.9 (12)
C1—O1—B	106.68 (15)	C18—C16—C17	110.5 (2)
C2—O2—B	106.60 (15)	H17a—C17—C16	112.2 (11)
C2—C1—O1	109.39 (16)	H17b—C17—C16	115.1 (12)
C6—C1—O1	128.31 (18)	H17b—C17—H17a	106.0 (16)
C6—C1—C2	122.29 (18)	H17c—C17—C16	111.1 (11)
C1—C2—O2	109.35 (16)	H17c—C17—H17a	103.0 (16)
C3—C2—O2	128.61 (19)	H17c—C17—H17b	108.6 (17)
C3—C2—C1	122.00 (19)	H18a—C18—C16	110.3 (12)
H3—C3—C2	122.3 (12)	H18b—C18—C16	112.5 (12)
C4—C3—C2	116.0 (2)	H18b—C18—H18a	108.7 (16)
C4—C3—H3	121.6 (12)	H18c—C18—C16	108.8 (12)
H4—C4—C3	117.4 (12)	H18c—C18—H18a	107.4 (16)
C5—C4—C3	121.9 (2)	H18c—C18—H18b	109.0 (17)
C5—C4—H4	120.6 (12)	H19—C19—P2	101.2 (12)
H5—C5—C4	117.5 (12)	C20—C19—P2	112.43 (16)
C6—C5—C4	121.4 (2)	C20—C19—H19	107.0 (12)
C6—C5—H5	121.0 (12)	C21—C19—P2	117.23 (16)
C5—C6—C1	116.35 (19)	C21—C19—H19	107.8 (12)
H6—C6—C1	122.2 (12)	C21—C19—C20	110.2 (2)
H6—C6—C5	121.4 (12)	H20a—C20—C19	109.1 (11)
H7—C7—P1	102.8 (11)	H20b—C20—C19	113.6 (12)
C8—C7—P1	114.21 (14)	H20b—C20—H20a	107.2 (16)
C8—C7—H7	109.6 (11)	H20c—C20—C19	109.2 (12)
C9—C7—P1	111.80 (14)	H20c—C20—H20a	108.8 (16)
C9—C7—H7	108.0 (11)	H20c—C20—H20b	108.9 (17)
C9—C7—C8	109.99 (18)	H21a—C21—C19	110.2 (11)
H8a—C8—C7	110.9 (12)	H21b—C21—C19	112.6 (14)
H8b—C8—C7	111.9 (11)	H21b—C21—H21a	110.5 (17)
H8b—C8—H8a	109.8 (16)	H21c—C21—C19	109.7 (11)
H8c—C8—C7	106.9 (12)	H21c—C21—H21a	106.8 (15)
H8c—C8—H8a	109.4 (16)	H21c—C21—H21b	106.8 (18)
H8c—C8—H8b	107.8 (16)	H22—C22—P2	101.0 (11)
H9a—C9—C7	109.8 (11)	C23—C22—P2	113.28 (14)
H9b—C9—C7	114.5 (12)	C23—C22—H22	105.7 (12)
H9b—C9—H9a	105.8 (16)	C24—C22—P2	116.45 (15)
H9c—C9—C7	109.9 (12)	C24—C22—H22	108.8 (11)
H9c—C9—H9a	109.5 (17)	C24—C22—C23	110.52 (17)
H9c—C9—H9b	107.2 (17)	H23a—C23—C22	113.3 (12)
H10—C10—P1	100.3 (11)	H23b—C23—C22	111.4 (12)
C11—C10—P1	114.49 (15)	H23b—C23—H23a	108.5 (17)
C11—C10—H10	109.1 (11)	H23c—C23—C22	111.1 (11)
C12—C10—P1	112.57 (14)	H23c—C23—H23a	106.6 (16)
C12—C10—H10	107.6 (11)	H23c—C23—H23b	105.5 (16)
C12—C10—C11	111.85 (18)	H24a—C24—C22	108.5 (11)
H11a—C11—C10	107.9 (12)	H24b—C24—C22	113.7 (12)
H11b—C11—C10	112.7 (12)	H24b—C24—H24a	106.2 (16)
H11b—C11—H11a	108.7 (17)	H24c—C24—C22	108.8 (12)
H11c—C11—C10	110.2 (11)	H24c—C24—H24a	108.3 (16)
H11c—C11—H11a	108.3 (16)	H24c—C24—H24b	111.2 (17)
H11c—C11—H11b	108.9 (16)
Rh—B—O1—C1	−178.82 (14)	O1—C1—C6—C5	−178.7 (2)
Rh—B—O2—C2	179.11 (19)	O2—C2—C1—C6	−178.20 (15)
B—O1—C1—C2	−1.17 (16)	O2—C2—C3—C4	178.2 (2)
B—O1—C1—C6	177.30 (15)	C1—C2—C3—C4	0.8 (2)
B—O2—C2—C1	0.57 (16)	C1—C6—C5—C4	0.7 (2)
B—O2—C2—C3	−177.02 (17)	C2—C3—C4—C5	−0.5 (3)
O1—C1—C2—O2	0.38 (16)	C3—C4—C5—C6	−0.3 (3)
O1—C1—C2—C3	178.16 (17)

(SITKUB_IAM_NoMoRe)

Crystal data

C24H47BClO2P2Rh	F(000) = 1213.281
Mr = 578.77	Dx = 1.348 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
a = 11.228 (3) Å	Cell parameters from 925 reflections
b = 11.101 (3) Å	θ = 12.0–24.6°
c = 23.414 (7) Å	µ = 0.82 mm^−1
β = 102.28 (4)°	T = 120 K
V = 2851.6 (14) Å^3	Fragment, colourless
Z = 4	0.6 × 0.4 × 0.2 mm

Data collection

SMART 1K CCD area detector diffractometer	7021 reflections with I ≥ 2u(I)
Radiation source: fine-focus sealed tube	Rint = 0.029
Graphite monochromator	θmax = 29.1°, θmin = 1.8°
ω scans	h = −15→15
33082 measured reflections	k = −15→15
7624 independent reflections	l = −31→31

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.026	Only H-atom coordinates refined
wR(F^2) = 0.063	w = 1/[σ^2(Fo^2) + (0.0339P)^2 + 1.7074P] where P = (Fo^2 + 2Fc^2)/3
S = 1.02	(Δ/σ)max = 0.001
7624 reflections	Δρmax = 0.45 e Å^−3
421 parameters	Δρmin = −0.80 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Rh	0.311325 (10)	0.814910 (10)	0.861852 (5)	0.01580 (4)
H	0.344 (2)	0.791 (2)	0.9223 (10)	0.033687
Cl	0.32707 (4)	0.93355 (4)	0.776977 (18)	0.02695 (8)
B	0.21250 (15)	0.68041 (15)	0.88084 (7)	0.0187 (3)
P1	0.17686 (3)	0.96111 (4)	0.882926 (17)	0.01864 (8)
P2	0.46544 (3)	0.68315 (3)	0.848419 (17)	0.01745 (8)
O1	0.10456 (10)	0.64549 (10)	0.84061 (5)	0.0200 (2)
O2	0.22739 (10)	0.60341 (10)	0.93019 (5)	0.0225 (2)
C1	0.05449 (14)	0.55158 (14)	0.86630 (7)	0.0197 (3)
C2	0.12844 (14)	0.52588 (14)	0.92000 (7)	0.0216 (3)
C3	0.09884 (17)	0.43763 (17)	0.95630 (8)	0.0311 (4)
H3	0.151 (2)	0.421 (3)	0.9941 (12)	0.055786
C4	−0.00965 (18)	0.37461 (17)	0.93504 (9)	0.0330 (4)
H4	−0.033 (3)	0.315 (3)	0.9594 (13)	0.058138
C5	−0.08337 (16)	0.40023 (15)	0.88110 (8)	0.0275 (3)
H5	−0.155 (2)	0.358 (3)	0.8691 (12)	0.048448
C6	−0.05312 (14)	0.49071 (15)	0.84520 (7)	0.0231 (3)
H6	−0.102 (2)	0.507 (2)	0.8078 (11)	0.043466
C7	0.09975 (15)	0.93774 (15)	0.94527 (7)	0.0233 (3)
H7	0.062 (2)	1.018 (2)	0.9488 (11)	0.041514
C8	0.00061 (16)	0.84084 (17)	0.93436 (8)	0.0272 (3)
H8A	0.036 (3)	0.761 (2)	0.9324 (13)	0.052999
H8B	−0.063 (2)	0.856 (3)	0.8981 (12)	0.055194
H8C	−0.038 (2)	0.843 (3)	0.9679 (12)	0.050208
C9	0.19133 (18)	0.9116 (2)	1.00213 (8)	0.0321 (4)
H9A	0.151 (3)	0.904 (3)	1.0362 (11)	0.058991
H9B	0.250 (3)	0.976 (3)	1.0127 (12)	0.061030
H9C	0.231 (3)	0.841 (3)	0.9993 (12)	0.056017
C10	0.05444 (14)	1.00353 (15)	0.81984 (7)	0.0229 (3)
H10	0.100 (2)	1.049 (2)	0.7962 (10)	0.037249
C11	−0.04326 (18)	1.08685 (19)	0.83516 (9)	0.0335 (4)
H11A	−0.089 (3)	1.119 (3)	0.7990 (12)	0.057304
H11B	−0.006 (3)	1.153 (3)	0.8607 (13)	0.054709
H11C	−0.097 (2)	1.041 (3)	0.8539 (13)	0.057309
C12	−0.00187 (15)	0.89408 (16)	0.78414 (7)	0.0247 (3)
H12A	−0.037 (3)	0.839 (3)	0.8064 (12)	0.053644
H12B	0.059 (2)	0.848 (3)	0.7717 (12)	0.049628
H12C	−0.059 (2)	0.919 (2)	0.7504 (11)	0.050188
C13	0.25944 (16)	1.10619 (15)	0.90624 (8)	0.0290 (3)
H13	0.222 (2)	1.141 (2)	0.9365 (12)	0.047655
C14	0.2508 (2)	1.20156 (19)	0.85828 (12)	0.0433 (5)
H14A	0.299 (3)	1.269 (3)	0.8751 (15)	0.072451
H14B	0.167 (3)	1.230 (3)	0.8420 (15)	0.068641
H14C	0.284 (3)	1.172 (3)	0.8241 (14)	0.065301
C15	0.39389 (19)	1.0818 (2)	0.93300 (12)	0.0412 (5)
H15A	0.433 (2)	1.059 (3)	0.9020 (13)	0.056581
H15B	0.404 (2)	1.016 (3)	0.9627 (13)	0.057565
H15C	0.435 (3)	1.155 (3)	0.9518 (15)	0.071268
C16	0.43395 (14)	0.58557 (15)	0.78278 (7)	0.0241 (3)
H16	0.504 (2)	0.537 (2)	0.7826 (11)	0.044142
C17	0.32943 (18)	0.49879 (19)	0.78542 (10)	0.0358 (4)
H17A	0.255 (2)	0.539 (3)	0.7835 (12)	0.051834
H17B	0.342 (3)	0.449 (3)	0.8213 (15)	0.073388
H17C	0.311 (3)	0.450 (3)	0.7494 (14)	0.071258
C18	0.4074 (2)	0.6568 (2)	0.72559 (8)	0.0364 (4)
H18A	0.394 (3)	0.599 (3)	0.6919 (12)	0.066228
H18B	0.474 (3)	0.710 (3)	0.7224 (12)	0.064530
H18C	0.336 (3)	0.706 (3)	0.7243 (12)	0.058895
C19	0.51444 (15)	0.57318 (16)	0.90887 (8)	0.0258 (3)
H19	0.442 (2)	0.539 (2)	0.9101 (11)	0.042480
C20	0.5634 (2)	0.6349 (2)	0.96756 (9)	0.0392 (4)
H20A	0.578 (3)	0.574 (3)	0.9989 (12)	0.069096
H20B	0.510 (3)	0.693 (3)	0.9772 (13)	0.074535
H20C	0.638 (3)	0.670 (3)	0.9663 (14)	0.071186
C21	0.6007 (2)	0.4726 (2)	0.89870 (11)	0.0454 (5)
H21A	0.683 (3)	0.510 (3)	0.8994 (16)	0.080510
H21B	0.568 (4)	0.430 (3)	0.8644 (16)	0.089113
H21C	0.611 (3)	0.411 (3)	0.9316 (14)	0.070545
C22	0.59711 (13)	0.77491 (15)	0.83774 (7)	0.0213 (3)
H22	0.561 (2)	0.823 (2)	0.8032 (11)	0.037850
C23	0.63920 (17)	0.86707 (17)	0.88638 (9)	0.0303 (4)
H23A	0.687 (3)	0.833 (3)	0.9202 (12)	0.053459
H23B	0.575 (3)	0.904 (3)	0.8970 (13)	0.059590
H23C	0.691 (2)	0.930 (2)	0.8735 (12)	0.052620
C24	0.70616 (16)	0.70561 (18)	0.82478 (10)	0.0318 (4)
H24A	0.762 (2)	0.764 (3)	0.8104 (13)	0.056677
H24B	0.683 (2)	0.648 (3)	0.7959 (13)	0.055202
H24C	0.749 (3)	0.671 (3)	0.8589 (14)	0.053350

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Rh	0.01346 (6)	0.01674 (6)	0.01748 (6)	0.00041 (4)	0.00393 (4)	0.00062 (4)
H	0.035000	0.040000	0.025000	0.003000	0.004000	0.001000
Cl	0.02280 (17)	0.0307 (2)	0.02963 (19)	0.00454 (14)	0.01070 (15)	0.01209 (15)
B	0.0164 (7)	0.0201 (7)	0.0202 (7)	0.0013 (6)	0.0056 (6)	−0.0001 (6)
P1	0.01678 (16)	0.01828 (17)	0.02116 (17)	0.00185 (13)	0.00468 (14)	−0.00076 (14)
P2	0.01401 (16)	0.01852 (17)	0.02012 (17)	0.00071 (13)	0.00431 (13)	−0.00022 (13)
O1	0.0186 (5)	0.0220 (5)	0.0195 (5)	−0.0024 (4)	0.0039 (4)	0.0017 (4)
O2	0.0192 (5)	0.0242 (5)	0.0229 (5)	−0.0028 (4)	0.0019 (4)	0.0048 (4)
C1	0.0203 (7)	0.0179 (6)	0.0224 (7)	0.0005 (5)	0.0084 (6)	−0.0014 (5)
C2	0.0194 (7)	0.0205 (7)	0.0254 (7)	−0.0012 (5)	0.0057 (6)	0.0018 (6)
C3	0.0305 (9)	0.0295 (9)	0.0329 (9)	−0.0015 (7)	0.0056 (7)	0.0099 (7)
H3	0.049000	0.071000	0.043000	−0.015000	−0.000000	0.025000
C4	0.0319 (9)	0.0255 (8)	0.0436 (10)	−0.0045 (7)	0.0125 (8)	0.0093 (7)
H4	0.056000	0.059000	0.061000	−0.022000	0.016000	0.021000
C5	0.0229 (7)	0.0218 (7)	0.0399 (9)	−0.0034 (6)	0.0117 (7)	−0.0046 (7)
H5	0.039000	0.047000	0.060000	−0.021000	0.012000	−0.005000
C6	0.0191 (7)	0.0238 (7)	0.0270 (8)	0.0004 (6)	0.0063 (6)	−0.0041 (6)
H6	0.038000	0.052000	0.036000	−0.011000	−0.002000	−0.001000
C7	0.0232 (7)	0.0256 (8)	0.0225 (7)	0.0031 (6)	0.0080 (6)	−0.0036 (6)
H7	0.047000	0.035000	0.047000	0.008000	0.020000	−0.005000
C8	0.0265 (8)	0.0311 (8)	0.0266 (8)	0.0004 (7)	0.0117 (7)	−0.0011 (7)
H8A	0.055000	0.035000	0.077000	−0.001000	0.032000	−0.009000
H8B	0.037000	0.077000	0.048000	−0.011000	0.001000	0.011000
H8C	0.056000	0.057000	0.047000	−0.003000	0.032000	−0.002000
C9	0.0329 (9)	0.0410 (10)	0.0221 (8)	0.0035 (8)	0.0052 (7)	−0.0045 (7)
H9A	0.065000	0.084000	0.031000	0.007000	0.017000	−0.001000
H9B	0.054000	0.080000	0.044000	−0.016000	−0.001000	−0.011000
H9C	0.060000	0.063000	0.042000	0.025000	0.004000	0.002000
C10	0.0200 (7)	0.0244 (7)	0.0242 (7)	0.0056 (6)	0.0040 (6)	0.0046 (6)
H10	0.039000	0.036000	0.038000	0.000000	0.011000	0.008000
C11	0.0275 (9)	0.0342 (9)	0.0381 (10)	0.0148 (7)	0.0056 (8)	0.0011 (8)
H11A	0.052000	0.060000	0.054000	0.028000	−0.002000	0.006000
H11B	0.052000	0.048000	0.061000	0.015000	0.005000	−0.016000
H11C	0.043000	0.065000	0.071000	0.013000	0.028000	0.004000
C12	0.0193 (7)	0.0304 (8)	0.0235 (7)	0.0008 (6)	0.0024 (6)	0.0025 (6)
H12A	0.060000	0.059000	0.042000	−0.025000	0.011000	0.004000
H12B	0.039000	0.048000	0.062000	0.005000	0.011000	−0.018000
H12C	0.046000	0.052000	0.043000	0.006000	−0.012000	0.004000
C13	0.0274 (8)	0.0203 (7)	0.0395 (9)	−0.0003 (6)	0.0075 (7)	−0.0057 (7)
H13	0.052000	0.038000	0.058000	−0.002000	0.023000	−0.016000
C14	0.0484 (13)	0.0254 (9)	0.0573 (14)	−0.0081 (9)	0.0137 (11)	0.0026 (9)
H14A	0.083000	0.037000	0.096000	−0.022000	0.016000	0.003000
H14B	0.062000	0.044000	0.096000	0.008000	0.008000	0.020000
H14C	0.082000	0.058000	0.062000	−0.010000	0.029000	0.008000
C15	0.0278 (9)	0.0327 (10)	0.0591 (13)	−0.0055 (8)	0.0000 (9)	−0.0152 (9)
H15A	0.040000	0.057000	0.077000	−0.003000	0.022000	−0.011000
H15B	0.046000	0.059000	0.060000	0.000000	−0.006000	0.001000
H15C	0.054000	0.054000	0.099000	−0.017000	0.001000	−0.034000
C16	0.0193 (7)	0.0248 (7)	0.0297 (8)	−0.0021 (6)	0.0083 (6)	−0.0076 (6)
H16	0.034000	0.045000	0.055000	0.008000	0.013000	−0.014000
C17	0.0287 (9)	0.0339 (10)	0.0478 (11)	−0.0128 (8)	0.0149 (8)	−0.0180 (9)
H17A	0.031000	0.057000	0.069000	−0.005000	0.014000	−0.020000
H17B	0.076000	0.059000	0.080000	−0.029000	0.005000	0.018000
H17C	0.061000	0.066000	0.092000	−0.022000	0.028000	−0.053000
C18	0.0412 (11)	0.0412 (10)	0.0251 (8)	−0.0039 (9)	0.0036 (8)	−0.0076 (8)
H18A	0.087000	0.074000	0.038000	−0.008000	0.014000	−0.025000
H18B	0.068000	0.087000	0.041000	−0.030000	0.017000	0.001000
H18C	0.063000	0.067000	0.043000	0.014000	0.003000	0.004000
C19	0.0227 (7)	0.0255 (8)	0.0301 (8)	0.0063 (6)	0.0077 (6)	0.0074 (6)
H19	0.031000	0.043000	0.056000	0.001000	0.015000	0.016000
C20	0.0428 (11)	0.0420 (11)	0.0282 (9)	0.0062 (9)	−0.0028 (8)	0.0086 (8)
H20A	0.080000	0.081000	0.041000	0.004000	0.001000	0.027000
H20B	0.102000	0.071000	0.042000	0.031000	−0.004000	−0.011000
H20C	0.054000	0.077000	0.070000	−0.016000	−0.015000	0.020000
C21	0.0459 (12)	0.0407 (12)	0.0537 (13)	0.0243 (10)	0.0201 (10)	0.0161 (10)
H21A	0.063000	0.079000	0.116000	0.038000	0.056000	0.040000
H21B	0.122000	0.052000	0.087000	0.037000	0.008000	−0.014000
H21C	0.080000	0.058000	0.082000	0.036000	0.036000	0.038000
C22	0.0145 (6)	0.0232 (7)	0.0264 (7)	−0.0022 (5)	0.0045 (6)	−0.0002 (6)
H22	0.033000	0.045000	0.035000	−0.001000	0.006000	0.012000
C23	0.0230 (8)	0.0281 (9)	0.0395 (10)	−0.0049 (7)	0.0063 (7)	−0.0092 (7)
H23A	0.057000	0.057000	0.040000	−0.009000	−0.004000	−0.003000
H23B	0.045000	0.056000	0.082000	0.000000	0.023000	−0.030000
H23C	0.049000	0.042000	0.068000	−0.018000	0.015000	−0.003000
C24	0.0180 (7)	0.0328 (9)	0.0469 (11)	−0.0032 (7)	0.0122 (7)	−0.0100 (8)
H24A	0.037000	0.058000	0.084000	−0.008000	0.033000	−0.004000
H24B	0.040000	0.062000	0.067000	−0.004000	0.019000	−0.032000
H24C	0.037000	0.055000	0.065000	0.014000	0.004000	0.002000

Geometric parameters (Å, º)

Rh—H	1.41 (2)	C12—H12A	0.94 (3)
Rh—Cl	2.4217 (7)	C12—H12B	0.95 (3)
Rh—B	1.9666 (17)	C12—H12C	0.95 (2)
Rh—P1	2.3396 (6)	C13—H13	0.98 (3)
Rh—P2	2.3375 (6)	C13—C14	1.531 (3)
B—O1	1.421 (2)	C13—C15	1.530 (3)
B—O2	1.418 (2)	C14—H14A	0.96 (3)
P1—C7	1.8668 (17)	C14—H14B	0.99 (3)
P1—C10	1.8519 (18)	C14—H14C	1.01 (3)
P1—C13	1.8805 (18)	C15—H15A	0.96 (3)
P2—C16	1.8518 (17)	C15—H15B	1.00 (3)
P2—C19	1.8616 (17)	C15—H15C	0.99 (3)
P2—C22	1.8555 (16)	C16—H16	0.95 (2)
O1—C1	1.3815 (18)	C16—C17	1.530 (2)
O2—C2	1.3855 (19)	C16—C18	1.529 (3)
C1—C2	1.381 (2)	C17—H17A	0.94 (3)
C1—C6	1.381 (2)	C17—H17B	0.99 (3)
C2—C3	1.383 (2)	C17—H17C	0.99 (3)
C3—H3	0.97 (3)	C18—H18A	1.00 (3)
C3—C4	1.401 (3)	C18—H18B	0.97 (3)
C4—H4	0.94 (3)	C18—H18C	0.96 (3)
C4—C5	1.384 (3)	C19—H19	0.90 (2)
C5—H5	0.92 (3)	C19—C20	1.529 (3)
C5—C6	1.397 (2)	C19—C21	1.529 (3)
C6—H6	0.95 (2)	C20—H20A	0.99 (3)
C7—H7	1.00 (2)	C20—H20B	0.95 (3)
C7—C8	1.530 (2)	C20—H20C	0.93 (3)
C7—C9	1.527 (3)	C21—H21A	1.01 (3)
C8—H8A	0.98 (3)	C21—H21B	0.94 (4)
C8—H8B	1.00 (3)	C21—H21C	1.01 (3)
C8—H8C	0.98 (2)	C22—H22	0.98 (2)
C9—H9A	1.00 (3)	C22—C23	1.529 (2)
C9—H9B	0.97 (3)	C22—C24	1.530 (2)
C9—H9C	0.91 (3)	C23—H23A	0.94 (3)
C10—H10	0.97 (2)	C23—H23B	0.91 (3)
C10—C11	1.535 (2)	C23—H23C	1.00 (3)
C10—C12	1.533 (2)	C24—H24A	1.01 (3)
C11—H11A	0.96 (3)	C24—H24B	0.93 (3)
C11—H11B	0.98 (3)	C24—H24C	0.92 (3)
C11—H11C	0.96 (3)
Cl—Rh—H	151.2 (10)	H12B—C12—H12A	104 (2)
B—Rh—H	70.8 (10)	H12C—C12—C10	110.5 (17)
B—Rh—Cl	137.86 (5)	H12C—C12—H12A	111 (2)
P1—Rh—H	87.7 (9)	H12C—C12—H12B	108 (2)
P1—Rh—Cl	87.639 (14)	H13—C13—P1	106.5 (15)
P1—Rh—B	93.36 (5)	C14—C13—P1	115.40 (14)
P2—Rh—H	88.6 (9)	C14—C13—H13	107.0 (16)
P2—Rh—Cl	92.555 (14)	C15—C13—P1	110.49 (13)
P2—Rh—B	91.42 (5)	C15—C13—H13	108.2 (16)
P2—Rh—P1	172.662 (14)	C15—C13—C14	109.00 (18)
O1—B—Rh	119.99 (11)	H14A—C14—C13	107 (2)
O2—B—Rh	131.86 (12)	H14B—C14—C13	114.3 (18)
O2—B—O1	108.15 (13)	H14B—C14—H14A	109 (3)
C7—P1—Rh	119.73 (5)	H14C—C14—C13	112.3 (17)
C10—P1—Rh	114.27 (5)	H14C—C14—H14A	108 (3)
C10—P1—C7	105.66 (7)	H14C—C14—H14B	106 (3)
C13—P1—Rh	110.78 (6)	H15A—C15—C13	107.8 (17)
C13—P1—C7	100.03 (8)	H15B—C15—C13	111.6 (16)
C13—P1—C10	104.49 (8)	H15B—C15—H15A	110 (3)
C16—P2—Rh	117.49 (5)	H15C—C15—C13	111.4 (19)
C19—P2—Rh	114.56 (5)	H15C—C15—H15A	108 (3)
C19—P2—C16	102.76 (8)	H15C—C15—H15B	108 (3)
C22—P2—Rh	107.97 (5)	H16—C16—P2	108.8 (15)
C22—P2—C16	103.07 (7)	C17—C16—P2	110.34 (12)
C22—P2—C19	110.32 (8)	C17—C16—H16	106.6 (16)
C1—O1—B	106.61 (12)	C18—C16—P2	113.07 (13)
C2—O2—B	106.43 (12)	C18—C16—H16	107.1 (16)
C2—C1—O1	109.31 (13)	C18—C16—C17	110.66 (16)
C6—C1—O1	128.29 (14)	H17A—C17—C16	112.2 (17)
C6—C1—C2	122.38 (14)	H17B—C17—C16	114.4 (17)
C1—C2—O2	109.47 (13)	H17B—C17—H17A	106 (3)
C3—C2—O2	128.53 (15)	H17C—C17—C16	109.6 (18)
C3—C2—C1	121.96 (15)	H17C—C17—H17A	101 (2)
H3—C3—C2	121.3 (16)	H17C—C17—H17B	112 (3)
C4—C3—C2	116.08 (17)	H18A—C18—C16	109.3 (18)
C4—C3—H3	122.7 (16)	H18B—C18—C16	111.8 (18)
H4—C4—C3	117.6 (18)	H18B—C18—H18A	109 (2)
C5—C4—C3	121.84 (16)	H18C—C18—C16	109.0 (17)
C5—C4—H4	120.6 (18)	H18C—C18—H18A	110 (2)
H5—C5—C4	119.1 (17)	H18C—C18—H18B	108 (3)
C6—C5—C4	121.45 (16)	H19—C19—P2	100.2 (16)
C6—C5—H5	119.5 (17)	C20—C19—P2	112.39 (13)
C5—C6—C1	116.28 (16)	C20—C19—H19	108.3 (17)
H6—C6—C1	121.9 (15)	C21—C19—P2	117.06 (13)
H6—C6—C5	121.7 (15)	C21—C19—H19	107.5 (17)
H7—C7—P1	102.7 (14)	C21—C19—C20	110.40 (17)
C8—C7—P1	114.16 (11)	H20A—C20—C19	109.2 (19)
C8—C7—H7	109.2 (15)	H20B—C20—C19	113.4 (19)
C9—C7—P1	111.71 (12)	H20B—C20—H20A	108 (3)
C9—C7—H7	108.6 (15)	H20C—C20—C19	108 (2)
C9—C7—C8	110.07 (15)	H20C—C20—H20A	108 (2)
H8A—C8—C7	110.8 (16)	H20C—C20—H20B	110 (3)
H8B—C8—C7	112.8 (16)	H21A—C21—C19	108.1 (18)
H8B—C8—H8A	110 (2)	H21B—C21—C19	111 (2)
H8C—C8—C7	106.4 (17)	H21B—C21—H21A	114 (3)
H8C—C8—H8A	108 (2)	H21C—C21—C19	110.4 (17)
H8C—C8—H8B	109 (2)	H21C—C21—H21A	107 (2)
H9A—C9—C7	112.0 (16)	H21C—C21—H21B	106 (3)
H9B—C9—C7	112.3 (18)	H22—C22—P2	102.0 (14)
H9B—C9—H9A	105 (2)	C23—C22—P2	113.32 (12)
H9C—C9—C7	110.4 (17)	C23—C22—H22	105.0 (15)
H9C—C9—H9A	107 (2)	C24—C22—P2	116.41 (12)
H9C—C9—H9B	110 (3)	C24—C22—H22	108.5 (14)
H10—C10—P1	101.3 (14)	C24—C22—C23	110.52 (14)
C11—C10—P1	114.40 (12)	H23A—C23—C22	112.8 (17)
C11—C10—H10	107.9 (14)	H23B—C23—C22	111.6 (18)
C12—C10—P1	112.55 (11)	H23B—C23—H23A	107 (3)
C12—C10—H10	107.9 (15)	H23C—C23—C22	110.6 (16)
C12—C10—C11	111.89 (14)	H23C—C23—H23A	106 (2)
H11A—C11—C10	107.1 (17)	H23C—C23—H23B	108 (2)
H11B—C11—C10	110.9 (16)	H24A—C24—C22	108.7 (16)
H11B—C11—H11A	110 (2)	H24B—C24—C22	112.0 (16)
H11C—C11—C10	109.6 (16)	H24B—C24—H24A	108 (2)
H11C—C11—H11A	109 (2)	H24C—C24—C22	109.3 (18)
H11C—C11—H11B	110 (2)	H24C—C24—H24A	108 (2)
H12A—C12—C10	112.6 (17)	H24C—C24—H24B	111 (3)
H12B—C12—C10	110.7 (16)

(SITKUB_IAM_SHADE3)

Crystal data

C24H47BClO2P2Rh	F(000) = 1213.334
Mr = 578.77	Dx = 1.348 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
a = 11.228 (3) Å	Cell parameters from 925 reflections
b = 11.101 (3) Å	θ = 12.0–24.6°
c = 23.414 (7) Å	µ = 0.82 mm^−1
β = 102.28 (4)°	T = 120 K
V = 2851.6 (14) Å^3	Fragment, colourless
Z = 4	0.6 × 0.4 × 0.2 mm

Data collection

SMART 1K CCD area detector diffractometer	7021 reflections with I ≥ 2u(I)
Radiation source: fine-focus sealed tube	Rint = 0.029
Graphite monochromator	θmax = 29.1°, θmin = 1.8°
ω scans	h = −15→15
33082 measured reflections	k = −15→15
7624 independent reflections	l = −31→31

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.026	Only H-atom coordinates refined
wR(F^2) = 0.057	w = 1/[σ^2(Fo^2) + (0.0229P)^2 + 1.9034P] where P = (Fo^2 + 2Fc^2)/3
S = 1.07	(Δ/σ)max = 0.001
7624 reflections	Δρmax = 0.46 e Å^−3
421 parameters	Δρmin = −0.80 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Rh	0.311323 (10)	0.814908 (10)	0.861852 (5)	0.01582 (4)
H	0.3443 (19)	0.792 (2)	0.9221 (9)	0.032322
Cl	0.32707 (3)	0.93355 (4)	0.776979 (18)	0.02697 (8)
B	0.21260 (15)	0.68048 (15)	0.88084 (7)	0.0186 (3)
P1	0.17687 (3)	0.96110 (3)	0.882933 (17)	0.01869 (7)
P2	0.46544 (3)	0.68316 (3)	0.848425 (16)	0.01750 (7)
O1	0.10455 (10)	0.64546 (10)	0.84062 (5)	0.0200 (2)
O2	0.22740 (10)	0.60344 (10)	0.93018 (5)	0.0225 (2)
C1	0.05450 (13)	0.55162 (13)	0.86630 (7)	0.0196 (3)
C2	0.12841 (14)	0.52589 (14)	0.92001 (7)	0.0217 (3)
C3	0.09883 (17)	0.43768 (17)	0.95626 (8)	0.0311 (4)
H3	0.150 (2)	0.421 (2)	0.9939 (11)	0.047342
C4	−0.00966 (17)	0.37469 (16)	0.93502 (9)	0.0330 (4)
H4	−0.032 (2)	0.316 (2)	0.9593 (12)	0.056272
C5	−0.08336 (15)	0.40023 (15)	0.88107 (8)	0.0275 (3)
H5	−0.155 (2)	0.358 (2)	0.8691 (12)	0.051690
C6	−0.05308 (14)	0.49068 (15)	0.84522 (7)	0.0231 (3)
H6	−0.102 (2)	0.507 (2)	0.8086 (10)	0.040352
C7	0.09979 (14)	0.93770 (15)	0.94526 (7)	0.0232 (3)
H7	0.062 (2)	1.017 (2)	0.9488 (10)	0.036782
C8	0.00062 (16)	0.84085 (17)	0.93439 (8)	0.0272 (3)
H8A	0.035 (2)	0.762 (2)	0.9329 (10)	0.035709
H8B	−0.062 (2)	0.855 (2)	0.8981 (10)	0.035402
H8C	−0.039 (2)	0.842 (2)	0.9671 (10)	0.041290
C9	0.19137 (18)	0.91169 (19)	1.00213 (8)	0.0320 (4)
H9A	0.151 (2)	0.905 (2)	1.0355 (10)	0.046040
H9B	0.251 (2)	0.974 (2)	1.0128 (11)	0.044962
H9C	0.231 (2)	0.841 (2)	0.9998 (10)	0.039648
C10	0.05442 (14)	1.00348 (15)	0.81986 (7)	0.0230 (3)
H10	0.100 (2)	1.049 (2)	0.7962 (10)	0.039751
C11	−0.04330 (17)	1.08681 (18)	0.83516 (9)	0.0335 (4)
H11A	−0.089 (2)	1.119 (2)	0.7991 (12)	0.052412
H11B	−0.007 (2)	1.152 (2)	0.8603 (12)	0.051258
H11C	−0.098 (2)	1.041 (2)	0.8535 (11)	0.045697
C12	−0.00184 (15)	0.89413 (16)	0.78412 (7)	0.0247 (3)
H12A	−0.038 (2)	0.840 (2)	0.8061 (10)	0.036842
H12B	0.059 (2)	0.848 (2)	0.7716 (10)	0.037748
H12C	−0.059 (2)	0.919 (2)	0.7501 (10)	0.045721
C13	0.25946 (16)	1.10615 (15)	0.90621 (8)	0.0290 (3)
H13	0.222 (2)	1.141 (2)	0.9364 (11)	0.044054
C14	0.2507 (2)	1.20154 (19)	0.85830 (11)	0.0434 (5)
H14A	0.299 (2)	1.269 (2)	0.8750 (13)	0.062542
H14B	0.168 (2)	1.230 (2)	0.8417 (13)	0.056505
H14C	0.285 (2)	1.172 (2)	0.8248 (13)	0.054009
C15	0.39388 (18)	1.0819 (2)	0.93298 (11)	0.0411 (5)
H15A	0.433 (2)	1.060 (2)	0.9024 (11)	0.045943
H15B	0.404 (2)	1.018 (2)	0.9626 (11)	0.043998
H15C	0.435 (2)	1.154 (2)	0.9519 (12)	0.054350
C16	0.43396 (14)	0.58558 (15)	0.78279 (7)	0.0242 (3)
H16	0.503 (2)	0.538 (2)	0.7832 (10)	0.038502
C17	0.32939 (18)	0.49890 (19)	0.78536 (10)	0.0356 (4)
H17A	0.254 (2)	0.541 (2)	0.7837 (10)	0.039737
H17B	0.344 (2)	0.449 (2)	0.8203 (11)	0.040400
H17C	0.312 (2)	0.448 (2)	0.7504 (11)	0.047522
C18	0.4073 (2)	0.6568 (2)	0.72560 (8)	0.0363 (4)
H18A	0.393 (2)	0.599 (2)	0.6921 (10)	0.051773
H18B	0.473 (2)	0.710 (3)	0.7222 (11)	0.046636
H18C	0.336 (2)	0.705 (2)	0.7236 (10)	0.044260
C19	0.51450 (15)	0.57320 (15)	0.90888 (7)	0.0259 (3)
H19	0.442 (2)	0.540 (2)	0.9100 (10)	0.033482
C20	0.5634 (2)	0.6349 (2)	0.96752 (9)	0.0391 (4)
H20A	0.577 (2)	0.574 (2)	0.9987 (10)	0.046909
H20B	0.510 (2)	0.693 (2)	0.9768 (10)	0.039358
H20C	0.638 (2)	0.670 (2)	0.9670 (11)	0.045138
C21	0.6008 (2)	0.4727 (2)	0.89871 (11)	0.0449 (5)
H21A	0.682 (2)	0.507 (2)	0.8985 (12)	0.049716
H21B	0.570 (2)	0.430 (2)	0.8651 (12)	0.048184
H21C	0.612 (2)	0.413 (2)	0.9320 (12)	0.051882
C22	0.59711 (13)	0.77490 (15)	0.83776 (7)	0.0214 (3)
H22	0.561 (2)	0.822 (2)	0.8035 (10)	0.037401
C23	0.63923 (16)	0.86708 (17)	0.88638 (9)	0.0302 (4)
H23A	0.687 (2)	0.833 (2)	0.9203 (12)	0.046500
H23B	0.576 (2)	0.904 (2)	0.8963 (11)	0.041464
H23C	0.692 (2)	0.930 (2)	0.8738 (11)	0.049436
C24	0.70615 (16)	0.70565 (18)	0.82480 (10)	0.0317 (4)
H24A	0.761 (2)	0.765 (2)	0.8105 (12)	0.051887
H24B	0.683 (2)	0.648 (2)	0.7958 (11)	0.046881
H24C	0.750 (2)	0.670 (2)	0.8593 (12)	0.048432

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Rh	0.01345 (5)	0.01677 (6)	0.01751 (6)	0.00040 (4)	0.00393 (4)	0.00062 (4)
H	0.032680	0.038910	0.023480	0.001840	0.001720	0.000740
Cl	0.02279 (17)	0.03073 (19)	0.02968 (19)	0.00453 (14)	0.01070 (15)	0.01212 (15)
B	0.0162 (7)	0.0200 (7)	0.0205 (7)	0.0014 (6)	0.0056 (6)	−0.0003 (6)
P1	0.01681 (16)	0.01834 (17)	0.02121 (17)	0.00181 (13)	0.00468 (14)	−0.00076 (14)
P2	0.01404 (16)	0.01855 (17)	0.02022 (17)	0.00067 (13)	0.00433 (13)	−0.00023 (13)
O1	0.0185 (5)	0.0220 (5)	0.0196 (5)	−0.0024 (4)	0.0040 (4)	0.0017 (4)
O2	0.0192 (5)	0.0243 (5)	0.0229 (5)	−0.0029 (4)	0.0019 (4)	0.0048 (4)
C1	0.0203 (7)	0.0178 (6)	0.0225 (7)	0.0005 (5)	0.0084 (5)	−0.0014 (5)
C2	0.0195 (7)	0.0205 (7)	0.0256 (7)	−0.0009 (5)	0.0058 (6)	0.0016 (6)
C3	0.0304 (9)	0.0296 (9)	0.0329 (9)	−0.0015 (7)	0.0055 (7)	0.0100 (7)
H3	0.044560	0.049990	0.047290	−0.000690	0.009350	0.021180
C4	0.0321 (9)	0.0252 (8)	0.0435 (10)	−0.0046 (7)	0.0124 (8)	0.0092 (7)
H4	0.051820	0.044950	0.076950	−0.010800	0.024700	0.020040
C5	0.0229 (7)	0.0219 (7)	0.0400 (9)	−0.0035 (6)	0.0116 (7)	−0.0047 (7)
H5	0.037320	0.045470	0.074290	−0.018570	0.016380	−0.005920
C6	0.0190 (7)	0.0239 (7)	0.0269 (8)	0.0005 (6)	0.0061 (6)	−0.0042 (6)
H6	0.030580	0.049060	0.039730	−0.008160	0.003690	−0.008700
C7	0.0230 (7)	0.0256 (8)	0.0224 (7)	0.0031 (6)	0.0078 (6)	−0.0037 (6)
H7	0.033690	0.034200	0.042930	0.005330	0.009210	−0.010480
C8	0.0263 (8)	0.0311 (9)	0.0267 (8)	0.0008 (7)	0.0116 (7)	−0.0009 (6)
H8A	0.030720	0.031730	0.044630	0.003940	0.007910	−0.002830
H8B	0.028400	0.043500	0.030660	0.002420	−0.001900	0.000740
H8C	0.039250	0.059320	0.029480	−0.007170	0.016690	−0.009640
C9	0.0330 (9)	0.0407 (10)	0.0221 (8)	0.0034 (8)	0.0054 (7)	−0.0048 (7)
H9A	0.038160	0.073290	0.028080	0.003260	0.010210	−0.009470
H9B	0.035710	0.048960	0.046560	−0.008900	0.000540	−0.013840
H9C	0.039690	0.041970	0.034190	0.008400	0.000910	−0.009460
C10	0.0200 (7)	0.0245 (7)	0.0242 (7)	0.0055 (6)	0.0040 (6)	0.0046 (6)
H10	0.037220	0.038570	0.046210	0.006370	0.015040	0.015080
C11	0.0280 (9)	0.0338 (9)	0.0382 (10)	0.0144 (7)	0.0059 (8)	0.0014 (8)
H11A	0.046520	0.055230	0.055150	0.024310	0.010060	0.017860
H11B	0.043680	0.038430	0.071720	0.006480	0.012400	−0.008410
H11C	0.040100	0.042870	0.059520	0.007420	0.022710	0.006680
C12	0.0192 (7)	0.0305 (8)	0.0234 (7)	0.0007 (6)	0.0026 (6)	0.0026 (6)
H12A	0.036650	0.044720	0.031710	−0.003110	0.013000	0.002330
H12B	0.031590	0.046320	0.038210	0.006920	0.013880	−0.001390
H12C	0.038680	0.057200	0.035410	0.011960	−0.005300	0.010060
C13	0.0273 (8)	0.0203 (7)	0.0395 (9)	−0.0004 (6)	0.0075 (7)	−0.0059 (7)
H13	0.038780	0.034260	0.061290	0.001180	0.015510	−0.013290
C14	0.0479 (12)	0.0252 (9)	0.0583 (14)	−0.0081 (9)	0.0141 (11)	0.0023 (9)
H14A	0.058430	0.028570	0.101870	−0.007630	0.019840	0.000620
H14B	0.041800	0.041110	0.089010	0.011490	0.019310	0.015560
H14C	0.058840	0.036700	0.073060	0.009560	0.028780	0.010100
C15	0.0281 (9)	0.0322 (10)	0.0588 (13)	−0.0057 (8)	0.0001 (9)	−0.0149 (9)
H15A	0.036700	0.047240	0.056780	0.000310	0.016430	−0.007020
H15B	0.036480	0.039000	0.055290	−0.001010	0.007010	−0.002640
H15C	0.041110	0.034690	0.085850	−0.008890	0.010360	−0.023270
C16	0.0193 (7)	0.0250 (8)	0.0297 (8)	−0.0018 (6)	0.0084 (6)	−0.0077 (6)
H16	0.027780	0.041750	0.048330	0.005970	0.013380	−0.007270
C17	0.0294 (9)	0.0335 (9)	0.0468 (11)	−0.0124 (8)	0.0146 (8)	−0.0175 (8)
H17A	0.026390	0.038490	0.055320	0.004920	0.010910	−0.004880
H17B	0.037050	0.038640	0.046360	−0.000630	0.010780	−0.000010
H17C	0.044640	0.051450	0.049850	−0.008040	0.017620	−0.026300
C18	0.0408 (11)	0.0417 (11)	0.0249 (8)	−0.0041 (9)	0.0040 (8)	−0.0080 (8)
H18A	0.056330	0.066270	0.036100	0.000480	0.017420	−0.015170
H18B	0.033860	0.063660	0.045950	−0.005190	0.016480	0.004420
H18C	0.033620	0.063630	0.039260	0.013530	0.016120	0.005930
C19	0.0224 (7)	0.0257 (8)	0.0304 (8)	0.0061 (6)	0.0076 (6)	0.0075 (6)
H19	0.025170	0.032970	0.042320	0.001500	0.007210	0.003850
C20	0.0419 (11)	0.0423 (11)	0.0287 (9)	0.0068 (9)	−0.0027 (8)	0.0093 (8)
H20A	0.046030	0.050480	0.039790	0.004140	−0.000810	0.012750
H20B	0.031870	0.041560	0.041680	0.008440	0.001170	−0.003700
H20C	0.023320	0.060530	0.050010	−0.003370	0.004310	−0.004540
C21	0.0455 (12)	0.0404 (11)	0.0526 (13)	0.0234 (10)	0.0187 (10)	0.0154 (10)
H21A	0.028340	0.044670	0.079120	0.003210	0.018120	−0.000460
H21B	0.037700	0.041350	0.063070	0.006610	0.005260	−0.012330
H21C	0.049120	0.044000	0.062800	0.018180	0.012520	0.015150
C22	0.0146 (6)	0.0231 (7)	0.0265 (7)	−0.0020 (5)	0.0046 (6)	0.0000 (6)
H22	0.030800	0.041020	0.042390	0.001040	0.012290	0.006040
C23	0.0223 (8)	0.0282 (8)	0.0400 (10)	−0.0046 (7)	0.0064 (7)	−0.0092 (7)
H23A	0.037660	0.045230	0.051230	0.003680	−0.002620	−0.002220
H23B	0.026730	0.042840	0.056060	0.001720	0.011580	−0.008570
H23C	0.039090	0.045530	0.067760	−0.016160	0.020500	−0.004160
C24	0.0181 (7)	0.0328 (9)	0.0465 (10)	−0.0032 (7)	0.0120 (7)	−0.0100 (8)
H24A	0.033170	0.052090	0.077500	−0.003190	0.027700	0.002660
H24B	0.035300	0.051060	0.056000	0.002260	0.013560	−0.013210
H24C	0.035030	0.057520	0.052510	0.012260	0.008780	0.003260

Geometric parameters (Å, º)

Rh—H	1.40 (2)	C12—H12a	0.94 (2)
Rh—Cl	2.4216 (7)	C12—H12b	0.95 (2)
Rh—B	1.9655 (17)	C12—H12c	0.95 (2)
Rh—P1	2.3395 (6)	C13—H13	0.97 (2)
Rh—P2	2.3375 (6)	C13—C14	1.531 (3)
B—O1	1.423 (2)	C13—C15	1.530 (3)
B—O2	1.418 (2)	C14—H14a	0.95 (3)
P1—C7	1.8664 (17)	C14—H14b	0.98 (3)
P1—C10	1.8518 (18)	C14—H14c	1.00 (3)
P1—C13	1.8800 (18)	C15—H15a	0.95 (2)
P2—C16	1.8517 (17)	C15—H15b	0.98 (3)
P2—C19	1.8615 (17)	C15—H15c	0.98 (2)
P2—C22	1.8553 (16)	C16—H16	0.94 (2)
O1—C1	1.3807 (18)	C16—C17	1.529 (2)
O2—C2	1.3859 (18)	C16—C18	1.529 (3)
C1—C2	1.381 (2)	C17—H17a	0.96 (2)
C1—C6	1.381 (2)	C17—H17b	0.97 (2)
C2—C3	1.382 (2)	C17—H17c	0.98 (2)
C3—H3	0.96 (2)	C18—H18a	1.00 (2)
C3—C4	1.401 (3)	C18—H18b	0.96 (2)
C4—H4	0.93 (2)	C18—H18c	0.96 (2)
C4—C5	1.384 (3)	C19—H19	0.90 (2)
C5—H5	0.92 (2)	C19—C20	1.528 (3)
C5—C6	1.396 (2)	C19—C21	1.529 (3)
C6—H6	0.94 (2)	C20—H20a	0.98 (2)
C7—H7	0.99 (2)	C20—H20b	0.94 (2)
C7—C8	1.530 (2)	C20—H20c	0.93 (2)
C7—C9	1.527 (2)	C21—H21a	0.99 (2)
C8—H8a	0.96 (2)	C21—H21b	0.92 (3)
C8—H8b	0.99 (2)	C21—H21c	1.01 (3)
C8—H8c	0.97 (2)	C22—H22	0.97 (2)
C9—H9a	0.99 (2)	C22—C23	1.529 (2)
C9—H9b	0.95 (2)	C22—C24	1.530 (2)
C9—H9c	0.91 (2)	C23—H23a	0.94 (3)
C10—H10	0.97 (2)	C23—H23b	0.89 (2)
C10—C11	1.535 (2)	C23—H23c	1.00 (2)
C10—C12	1.532 (2)	C24—H24a	1.00 (3)
C11—H11a	0.96 (2)	C24—H24b	0.93 (3)
C11—H11b	0.96 (3)	C24—H24c	0.94 (3)
C11—H11c	0.96 (2)
Cl—Rh—H	151.0 (9)	H12b—C12—H12a	104 (2)
B—Rh—H	71.0 (9)	H12c—C12—C10	110.6 (16)
B—Rh—Cl	137.88 (5)	H12c—C12—H12a	110 (2)
P1—Rh—H	87.7 (9)	H12c—C12—H12b	108 (2)
P1—Rh—Cl	87.642 (14)	H13—C13—P1	106.6 (14)
P1—Rh—B	93.36 (5)	C14—C13—P1	115.41 (14)
P2—Rh—H	88.6 (9)	C14—C13—H13	106.8 (15)
P2—Rh—Cl	92.556 (13)	C15—C13—P1	110.52 (12)
P2—Rh—B	91.41 (5)	C15—C13—H13	108.2 (15)
P2—Rh—P1	172.655 (14)	C15—C13—C14	109.04 (17)
O1—B—Rh	120.02 (11)	H14a—C14—C13	107.3 (18)
O2—B—Rh	131.91 (12)	H14b—C14—C13	114.9 (16)
O2—B—O1	108.07 (13)	H14b—C14—H14a	108 (2)
C7—P1—Rh	119.72 (5)	H14c—C14—C13	112.1 (15)
C10—P1—Rh	114.26 (5)	H14c—C14—H14a	108 (2)
C10—P1—C7	105.65 (7)	H14c—C14—H14b	106 (2)
C13—P1—Rh	110.77 (6)	H15a—C15—C13	108.3 (15)
C13—P1—C7	100.06 (8)	H15b—C15—C13	112.1 (14)
C13—P1—C10	104.50 (8)	H15b—C15—H15a	110 (2)
C16—P2—Rh	117.49 (5)	H15c—C15—C13	111.5 (15)
C19—P2—Rh	114.57 (5)	H15c—C15—H15a	108 (2)
C19—P2—C16	102.76 (8)	H15c—C15—H15b	107 (2)
C22—P2—Rh	107.97 (5)	H16—C16—P2	107.9 (14)
C22—P2—C16	103.08 (7)	C17—C16—P2	110.37 (12)
C22—P2—C19	110.30 (8)	C17—C16—H16	106.9 (15)
C1—O1—B	106.66 (12)	C18—C16—P2	113.05 (12)
C2—O2—B	106.49 (12)	C18—C16—H16	107.8 (15)
C2—C1—O1	109.33 (13)	C18—C16—C17	110.56 (16)
C6—C1—O1	128.33 (14)	H17a—C17—C16	111.8 (14)
C6—C1—C2	122.32 (14)	H17b—C17—C16	113.8 (14)
C1—C2—O2	109.42 (13)	H17b—C17—H17a	107.2 (19)
C3—C2—O2	128.57 (15)	H17c—C17—C16	110.3 (14)
C3—C2—C1	121.97 (15)	H17c—C17—H17a	103.3 (19)
H3—C3—C2	121.4 (14)	H17c—C17—H17b	110 (2)
C4—C3—C2	116.11 (17)	H18a—C18—C16	109.1 (16)
C4—C3—H3	122.5 (14)	H18b—C18—C16	112.4 (15)
H4—C4—C3	117.2 (17)	H18b—C18—H18a	109 (2)
C5—C4—C3	121.84 (16)	H18c—C18—C16	109.7 (14)
C5—C4—H4	120.9 (17)	H18c—C18—H18a	109 (2)
H5—C5—C4	119.0 (17)	H18c—C18—H18b	107 (2)
C6—C5—C4	121.40 (16)	H19—C19—P2	99.9 (14)
C6—C5—H5	119.6 (17)	C20—C19—P2	112.38 (13)
C5—C6—C1	116.34 (15)	C20—C19—H19	108.2 (15)
H6—C6—C1	122.1 (14)	C21—C19—P2	117.05 (13)
H6—C6—C5	121.5 (14)	C21—C19—H19	107.9 (14)
H7—C7—P1	102.9 (13)	C21—C19—C20	110.40 (17)
C8—C7—P1	114.20 (11)	H20a—C20—C19	109.1 (15)
C8—C7—H7	109.0 (13)	H20b—C20—C19	113.0 (14)
C9—C7—P1	111.71 (11)	H20b—C20—H20a	108 (2)
C9—C7—H7	108.5 (13)	H20c—C20—C19	109.2 (16)
C9—C7—C8	110.09 (15)	H20c—C20—H20a	107 (2)
H8a—C8—C7	111.0 (13)	H20c—C20—H20b	110 (2)
H8b—C8—C7	112.7 (14)	H21a—C21—C19	109.7 (15)
H8b—C8—H8a	109.7 (19)	H21b—C21—C19	111.9 (15)
H8c—C8—C7	107.3 (14)	H21b—C21—H21a	112 (2)
H8c—C8—H8a	108 (2)	H21c—C21—C19	110.1 (15)
H8c—C8—H8b	108.3 (19)	H21c—C21—H21a	107 (2)
H9a—C9—C7	111.3 (14)	H21c—C21—H21b	106 (2)
H9b—C9—C7	113.2 (15)	H22—C22—P2	101.9 (13)
H9b—C9—H9a	105 (2)	C23—C22—P2	113.35 (11)
H9c—C9—C7	111.1 (14)	C23—C22—H22	105.2 (14)
H9c—C9—H9a	107 (2)	C24—C22—P2	116.43 (12)
H9c—C9—H9b	108 (2)	C24—C22—H22	108.4 (13)
H10—C10—P1	101.3 (14)	C24—C22—C23	110.50 (14)
C11—C10—P1	114.41 (12)	H23a—C23—C22	112.9 (16)
C11—C10—H10	108.1 (14)	H23b—C23—C22	111.4 (15)
C12—C10—P1	112.59 (11)	H23b—C23—H23a	108 (2)
C12—C10—H10	107.6 (15)	H23c—C23—C22	111.0 (15)
C12—C10—C11	111.89 (14)	H23c—C23—H23a	105 (2)
H11a—C11—C10	107.5 (15)	H23c—C23—H23b	108 (2)
H11b—C11—C10	111.5 (15)	H24a—C24—C22	108.2 (15)
H11b—C11—H11a	109 (2)	H24b—C24—C22	112.3 (15)
H11c—C11—C10	110.1 (14)	H24b—C24—H24a	108 (2)
H11c—C11—H11a	108 (2)	H24c—C24—C22	109.6 (15)
H11c—C11—H11b	110 (2)	H24c—C24—H24a	108 (2)
H12a—C12—C10	112.6 (14)	H24c—C24—H24b	111 (2)
H12b—C12—C10	110.8 (14)

 

(TIWXOP_HAR_0_HADPs)

Crystal data

C20H31N2OSbSi2	Z = 2
Mr = 493.41	F(000) = 503.265
Triclinic, P1	Dx = 1.475 Mg m^−3
a = 7.6028 (5) Å	Mo Kα radiation, λ = 0.71073 Å
b = 11.5896 (8) Å	Cell parameters from 5427 reflections
c = 13.8020 (7) Å	θ = 3.8–29.0°
α = 99.459 (5)°	µ = 1.36 mm^−1
β = 100.012 (5)°	T = 120 K
γ = 107.557 (6)°	Block, colourless
V = 1110.98 (13) Å^3	0.17 × 0.11 × 0.07 mm

Data collection

SuperNova, Dual, Cu at zero, EosS2 diffractometer	4181 reflections with I ≥ 2u(I)
Detector resolution: 8.0856 pixels mm^-1	Rint = 0.030
ω scans	θmax = 26.4°, θmin = 3.4°
Absorption correction: gaussian CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	h = −9→9
Tmin = 0.744, Tmax = 1	k = −13→14
8520 measured reflections	l = −17→13
4543 independent reflections

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.032	Only H-atom coordinates refined
wR(F^2) = 0.075	w = 1/[σ^2(Fo^2) + (0.0331P)^2 + 0.5539P] where P = (Fo^2 + 2Fc^2)/3
S = 1.02	(Δ/σ)max = 0.001
4543 reflections	Δρmax = 1.01 e Å^−3
328 parameters	Δρmin = −0.79 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Sb	0.72530 (3)	0.536326 (18)	0.644329 (13)	0.01312 (8)
H1A	0.880 (4)	0.519 (3)	0.562 (2)	0.000000
Si1	1.01933 (12)	0.42362 (8)	0.76618 (6)	0.01312 (17)
Si2	1.15156 (11)	0.70706 (8)	0.78232 (6)	0.01252 (17)
O	1.1414 (3)	0.5721 (2)	0.80503 (16)	0.0198 (5)
N1	0.7850 (3)	0.4129 (2)	0.72356 (17)	0.0133 (5)
N2	0.9185 (3)	0.6972 (2)	0.73798 (17)	0.0128 (5)
C1	0.6278 (4)	0.3103 (3)	0.7280 (2)	0.0118 (6)
C2	0.5384 (4)	0.2093 (3)	0.6434 (2)	0.0150 (6)
C3	0.3880 (4)	0.1086 (3)	0.6498 (2)	0.0191 (7)
H3	0.320 (4)	0.031 (3)	0.5885 (19)	0.000000
C4	0.3253 (4)	0.1055 (3)	0.7384 (2)	0.0201 (7)
H4	0.210 (4)	0.023 (3)	0.7395 (19)	0.000000
C5	0.4125 (5)	0.2056 (3)	0.8207 (2)	0.0188 (7)
H5	0.366 (4)	0.203 (3)	0.8824 (19)	0.000000
C6	0.5601 (4)	0.3089 (3)	0.8163 (2)	0.0151 (6)
C7	0.6022 (5)	0.2096 (3)	0.5466 (2)	0.0227 (7)
H7A	0.547 (4)	0.131 (3)	0.493 (2)	0.000000
H7B	0.751 (4)	0.230 (3)	0.554 (2)	0.000000
H7C	0.562 (4)	0.276 (3)	0.504 (2)	0.000000
C8	0.6402 (6)	0.4184 (3)	0.9055 (3)	0.0265 (8)
H8A	0.567 (4)	0.452 (3)	0.917 (2)	0.000000
H8B	0.769 (4)	0.490 (3)	0.897 (2)	0.000000
H8C	0.654 (4)	0.388 (3)	0.9776 (19)	0.000000
C9	1.1192 (5)	0.3585 (4)	0.6657 (3)	0.0257 (8)
H9A	1.090 (4)	0.386 (3)	0.599 (2)	0.000000
H9B	1.060 (4)	0.256 (3)	0.641 (2)	0.000000
H9C	1.257 (4)	0.379 (3)	0.687 (2)	0.000000
C10	1.0474 (5)	0.3478 (3)	0.8725 (2)	0.0204 (7)
H10A	1.194 (4)	0.368 (3)	0.904 (2)	0.000000
H10B	0.984 (4)	0.237 (3)	0.849 (2)	0.000000
H10C	0.992 (4)	0.375 (3)	0.929 (2)	0.000000
C11	1.2960 (5)	0.7343 (3)	0.6878 (2)	0.0221 (7)
H11A	1.428 (4)	0.722 (3)	0.712 (2)	0.000000
H11B	1.337 (4)	0.826 (3)	0.673 (2)	0.000000
H11C	1.231 (4)	0.674 (3)	0.616 (2)	0.000000
C12	1.2673 (5)	0.8287 (3)	0.9006 (2)	0.0222 (7)
H12A	1.205 (4)	0.810 (3)	0.964 (2)	0.000000
H12B	1.267 (4)	0.924 (3)	0.899 (2)	0.000000
H12C	1.408 (4)	0.837 (3)	0.928 (2)	0.000000
C13	0.8577 (4)	0.8027 (3)	0.7510 (2)	0.0126 (6)
C14	0.8482 (4)	0.8684 (3)	0.6740 (2)	0.0154 (6)
C15	0.7941 (5)	0.9724 (3)	0.6890 (2)	0.0206 (7)
H15	0.788 (4)	1.021 (3)	0.6316 (19)	0.000000
C16	0.7483 (5)	1.0132 (3)	0.7788 (3)	0.0235 (7)
H16	0.708 (4)	1.097 (3)	0.786 (2)	0.000000
C17	0.7578 (4)	0.9491 (3)	0.8540 (2)	0.0208 (7)
H17	0.734 (4)	0.981 (3)	0.925 (2)	0.000000
C18	0.8088 (4)	0.8426 (3)	0.8413 (2)	0.0166 (6)
C19	0.8962 (5)	0.8277 (3)	0.5761 (2)	0.0233 (7)
H19A	1.023 (4)	0.807 (3)	0.586 (2)	0.000000
H19B	0.918 (4)	0.903 (3)	0.534 (2)	0.000000
H19C	0.790 (4)	0.749 (3)	0.533 (2)	0.000000
C20	0.8015 (5)	0.7710 (4)	0.9224 (3)	0.0257 (8)
H20A	0.866 (4)	0.826 (3)	0.999 (2)	0.000000
H20B	0.870 (4)	0.706 (3)	0.913 (2)	0.000000
H20C	0.666 (4)	0.732 (3)	0.929 (2)	0.000000

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Sb	0.01302 (12)	0.01064 (12)	0.01383 (12)	0.00345 (8)	−0.00095 (8)	0.00318 (8)
H1A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
Si1	0.0137 (4)	0.0114 (4)	0.0146 (4)	0.0052 (3)	0.0017 (3)	0.0041 (3)
Si2	0.0113 (4)	0.0103 (4)	0.0151 (4)	0.0027 (3)	0.0029 (3)	0.0025 (3)
O	0.0141 (11)	0.0130 (11)	0.0297 (12)	0.0024 (9)	0.0000 (9)	0.0071 (9)
N1	0.0122 (12)	0.0128 (13)	0.0144 (12)	0.0041 (10)	0.0020 (10)	0.0029 (10)
N2	0.0119 (12)	0.0132 (13)	0.0149 (12)	0.0057 (10)	0.0024 (10)	0.0053 (10)
C1	0.0115 (14)	0.0109 (15)	0.0145 (14)	0.0043 (12)	0.0052 (11)	0.0033 (12)
C2	0.0129 (15)	0.0134 (16)	0.0162 (14)	0.0024 (12)	0.0015 (12)	0.0024 (12)
C3	0.0170 (16)	0.0136 (17)	0.0214 (16)	0.0016 (13)	0.0004 (13)	0.0015 (13)
H3	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C4	0.0160 (16)	0.0135 (17)	0.0289 (17)	0.0006 (13)	0.0060 (13)	0.0074 (14)
H4	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C5	0.0201 (16)	0.0205 (18)	0.0195 (16)	0.0074 (14)	0.0107 (13)	0.0071 (13)
H5	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C6	0.0160 (15)	0.0148 (16)	0.0150 (14)	0.0052 (13)	0.0055 (12)	0.0032 (12)
C7	0.0264 (19)	0.0220 (19)	0.0162 (16)	0.0058 (15)	0.0065 (14)	−0.0017 (14)
H7A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H7B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H7C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C8	0.033 (2)	0.024 (2)	0.0232 (18)	0.0100 (17)	0.0151 (16)	−0.0017 (15)
H8A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H8B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H8C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C9	0.0214 (19)	0.036 (2)	0.0254 (18)	0.0186 (17)	0.0083 (15)	0.0043 (16)
H9A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H9B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H9C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C10	0.0203 (17)	0.0187 (18)	0.0206 (16)	0.0051 (14)	−0.0002 (14)	0.0085 (13)
H10A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H10B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H10C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C11	0.0208 (18)	0.026 (2)	0.0220 (17)	0.0070 (15)	0.0104 (14)	0.0084 (15)
H11A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H11B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H11C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C12	0.0206 (18)	0.0183 (18)	0.0199 (16)	0.0025 (14)	−0.0008 (14)	−0.0027 (14)
H12A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H12B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H12C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C13	0.0111 (14)	0.0105 (15)	0.0163 (14)	0.0031 (11)	0.0047 (11)	0.0030 (12)
C14	0.0132 (14)	0.0124 (16)	0.0209 (15)	0.0042 (12)	0.0030 (12)	0.0055 (12)
C15	0.0223 (17)	0.0147 (17)	0.0265 (17)	0.0075 (13)	0.0032 (14)	0.0093 (14)
H15	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C16	0.0193 (16)	0.0130 (17)	0.0351 (19)	0.0072 (13)	0.0003 (14)	0.0006 (14)
H16	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C17	0.0203 (17)	0.0186 (18)	0.0226 (17)	0.0088 (14)	0.0049 (14)	−0.0013 (14)
H17	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C18	0.0180 (16)	0.0155 (16)	0.0153 (14)	0.0048 (13)	0.0058 (12)	0.0008 (12)
C19	0.0278 (19)	0.025 (2)	0.0202 (17)	0.0099 (16)	0.0065 (15)	0.0102 (15)
H19A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H19B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H19C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C20	0.032 (2)	0.033 (2)	0.0221 (17)	0.0170 (17)	0.0152 (16)	0.0124 (15)
H20A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H20B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H20C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000

Geometric parameters (Å, º)

Sb—H1A	1.80 (3)	C9—H9A	1.03 (3)
Sb—N1	2.045 (2)	C9—H9B	1.10 (3)
Sb—N2	2.049 (2)	C9—H9C	0.98 (3)
Si1—O	1.634 (2)	C10—H10A	1.06 (3)
Si1—N1	1.736 (3)	C10—H10B	1.19 (3)
Si1—C9	1.855 (3)	C10—H10C	1.00 (3)
Si1—C10	1.843 (3)	C11—H11A	1.06 (3)
Si2—O	1.627 (2)	C11—H11B	1.08 (3)
Si2—N2	1.734 (2)	C11—H11C	1.06 (3)
Si2—C11	1.852 (3)	C12—H12A	1.09 (3)
Si2—C12	1.850 (3)	C12—H12B	1.11 (3)
N1—C1	1.427 (4)	C12—H12C	1.04 (3)
N2—C13	1.427 (4)	C13—C14	1.409 (4)
C1—C2	1.411 (4)	C13—C18	1.408 (4)
C1—C6	1.404 (4)	C14—C15	1.382 (4)
C2—C3	1.394 (4)	C14—C19	1.499 (4)
C2—C7	1.498 (4)	C15—H15	1.04 (3)
C3—H3	1.05 (3)	C15—C16	1.392 (5)
C3—C4	1.390 (4)	C16—H16	1.10 (3)
C4—H4	1.09 (3)	C16—C17	1.377 (4)
C4—C5	1.385 (4)	C17—H17	1.05 (3)
C5—H5	0.98 (3)	C17—C18	1.395 (4)
C5—C6	1.391 (4)	C18—C20	1.498 (4)
C6—C8	1.502 (4)	C19—H19A	1.05 (3)
C7—H7A	1.00 (3)	C19—H19B	1.11 (3)
C7—H7B	1.07 (3)	C19—H19C	1.03 (3)
C7—H7C	1.13 (3)	C20—H20A	1.08 (3)
C8—H8A	0.79 (3)	C20—H20B	1.05 (3)
C8—H8B	1.11 (3)	C20—H20C	1.02 (3)
C8—H8C	1.11 (3)
N1—Sb—H1A	93.9 (9)	H9B—C9—Si1	113.5 (15)
N2—Sb—H1A	94.1 (10)	H9B—C9—H9A	103 (2)
N2—Sb—N1	98.52 (9)	H9C—C9—Si1	112.9 (16)
N1—Si1—O	106.07 (12)	H9C—C9—H9A	108 (2)
C9—Si1—O	107.45 (15)	H9C—C9—H9B	105 (2)
C9—Si1—N1	113.29 (14)	H10A—C10—Si1	109.4 (15)
C10—Si1—O	109.12 (13)	H10B—C10—Si1	114.3 (14)
C10—Si1—N1	111.59 (14)	H10B—C10—H10A	104 (2)
C10—Si1—C9	109.12 (16)	H10C—C10—Si1	114.5 (16)
N2—Si2—O	106.00 (12)	H10C—C10—H10A	107 (2)
C11—Si2—O	107.18 (14)	H10C—C10—H10B	107 (2)
C11—Si2—N2	113.01 (14)	H11A—C11—Si2	110.6 (15)
C12—Si2—O	109.23 (14)	H11B—C11—Si2	117.0 (15)
C12—Si2—N2	111.34 (14)	H11B—C11—H11A	103 (2)
C12—Si2—C11	109.87 (16)	H11C—C11—Si2	113.8 (16)
Si2—O—Si1	142.57 (14)	H11C—C11—H11A	107 (2)
Si1—N1—Sb	119.67 (13)	H11C—C11—H11B	105 (2)
C1—N1—Sb	116.94 (18)	H12A—C12—Si2	114.2 (16)
C1—N1—Si1	122.8 (2)	H12B—C12—Si2	117.4 (15)
Si2—N2—Sb	120.33 (13)	H12B—C12—H12A	102 (2)
C13—N2—Sb	116.25 (18)	H12C—C12—Si2	112.3 (15)
C13—N2—Si2	122.8 (2)	H12C—C12—H12A	103 (2)
C2—C1—N1	120.2 (2)	H12C—C12—H12B	106 (2)
C6—C1—N1	120.5 (3)	C14—C13—N2	120.3 (2)
C6—C1—C2	119.3 (3)	C18—C13—N2	120.2 (3)
C3—C2—C1	119.5 (3)	C18—C13—C14	119.5 (3)
C7—C2—C1	120.8 (3)	C15—C14—C13	119.6 (3)
C7—C2—C3	119.7 (3)	C19—C14—C13	121.1 (3)
H3—C3—C2	121.4 (15)	C19—C14—C15	119.3 (3)
C4—C3—C2	121.1 (3)	H15—C15—C14	119.0 (15)
C4—C3—H3	117.5 (15)	C16—C15—C14	121.1 (3)
H4—C4—C3	117.6 (14)	C16—C15—H15	119.9 (15)
C5—C4—C3	119.0 (3)	H16—C16—C15	117.2 (14)
C5—C4—H4	123.4 (14)	C17—C16—C15	119.4 (3)
H5—C5—C4	118.3 (16)	C17—C16—H16	123.5 (14)
C6—C5—C4	121.5 (3)	H17—C17—C16	121.7 (15)
C6—C5—H5	120.1 (16)	C18—C17—C16	121.3 (3)
C5—C6—C1	119.5 (3)	C18—C17—H17	116.9 (15)
C8—C6—C1	121.3 (3)	C17—C18—C13	119.1 (3)
C8—C6—C5	119.1 (3)	C20—C18—C13	122.0 (3)
H7A—C7—C2	117.3 (16)	C20—C18—C17	118.8 (3)
H7B—C7—C2	115.2 (14)	H19A—C19—C14	113.5 (15)
H7B—C7—H7A	102 (2)	H19B—C19—C14	111.1 (14)
H7C—C7—C2	113.5 (14)	H19B—C19—H19A	105 (2)
H7C—C7—H7A	100 (2)	H19C—C19—C14	110.0 (15)
H7C—C7—H7B	106 (2)	H19C—C19—H19A	107 (2)
H8A—C8—C6	114 (2)	H19C—C19—H19B	110 (2)
H8B—C8—C6	112.6 (15)	H20A—C20—C18	115.6 (15)
H8B—C8—H8A	108 (3)	H20B—C20—C18	112.3 (15)
H8C—C8—C6	111.3 (15)	H20B—C20—H20A	105 (2)
H8C—C8—H8A	95 (2)	H20C—C20—C18	111.8 (16)
H8C—C8—H8B	116 (2)	H20C—C20—H20A	99 (2)
H9A—C9—Si1	113.6 (16)	H20C—C20—H20B	112 (2)

(TIWXOP_HAR)

Crystal data

C20H31N2OSbSi2	Z = 2
Mr = 493.41	F(000) = 503.265
Triclinic, P1	Dx = 1.475 Mg m^−3
a = 7.6028 (5) Å	Mo Kα radiation, λ = 0.71073 Å
b = 11.5896 (8) Å	Cell parameters from 5427 reflections
c = 13.8020 (7) Å	θ = 3.8–29.0°
α = 99.459 (5)°	µ = 1.36 mm^−1
β = 100.012 (5)°	T = 120 K
γ = 107.557 (6)°	Block, colourless
V = 1110.98 (13) Å^3	0.17 × 0.11 × 0.07 mm

Data collection

SuperNova, Dual, Cu at zero, EosS2 diffractometer	4181 reflections with I ≥ 2u(I)
Detector resolution: 8.0856 pixels mm^-1	Rint = 0.030
ω scans	θmax = 26.4°, θmin = 3.4°
Absorption correction: gaussian CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	h = −9→9
Tmin = 0.744, Tmax = 1	k = −13→14
8520 measured reflections	l = −17→13
4543 independent reflections

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.029	All H-atom parameters refined
wR(F^2) = 0.092	w = 1/[σ^2(Fo^2) + (0.1P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 0.70	(Δ/σ)max = 0.001
4543 reflections	Δρmax = 0.98 e Å^−3
359 parameters	Δρmin = −0.59 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Sb	0.72530 (2)	0.536301 (16)	0.644317 (12)	0.01341 (9)
H1A	0.881 (6)	0.521 (4)	0.565 (3)	0.031 (11)*
Si1	1.01940 (11)	0.42353 (7)	0.76612 (6)	0.01347 (17)
Si2	1.15157 (11)	0.70700 (7)	0.78227 (6)	0.01277 (17)
O	1.1412 (3)	0.57207 (19)	0.80502 (16)	0.0207 (4)
N1	0.7849 (3)	0.4128 (2)	0.72352 (17)	0.0138 (5)
N2	0.9182 (3)	0.6970 (2)	0.73778 (17)	0.0135 (5)
C1	0.6275 (4)	0.3103 (3)	0.7279 (2)	0.0119 (5)
C2	0.5383 (4)	0.2091 (3)	0.6435 (2)	0.0151 (6)
C3	0.3880 (4)	0.1088 (3)	0.6499 (2)	0.0195 (6)
H3	0.316 (6)	0.032 (4)	0.590 (3)	0.032 (10)*
C4	0.3245 (4)	0.1053 (3)	0.7381 (2)	0.0208 (6)
H4	0.205 (6)	0.019 (4)	0.737 (3)	0.033 (11)*
C5	0.4123 (4)	0.2055 (3)	0.8205 (2)	0.0196 (6)
H5	0.360 (5)	0.205 (4)	0.885 (3)	0.029 (10)*
C6	0.5598 (4)	0.3086 (3)	0.8164 (2)	0.0156 (6)
C7	0.6020 (5)	0.2100 (3)	0.5461 (2)	0.0232 (7)
H7A	0.550 (6)	0.126 (4)	0.491 (3)	0.035 (10)*
H7B	0.747 (8)	0.237 (5)	0.559 (4)	0.068 (15)*
H7C	0.557 (9)	0.280 (6)	0.504 (4)	0.078 (18)*
C8	0.6383 (5)	0.4190 (3)	0.9057 (2)	0.0260 (7)
H8A	0.558 (15)	0.478 (10)	0.866 (8)	0.16 (4)*
H8B	0.770 (8)	0.492 (5)	0.900 (4)	0.060 (14)*
H8C	0.640 (9)	0.392 (6)	0.968 (5)	0.085 (19)*
C9	1.1194 (5)	0.3581 (4)	0.6661 (3)	0.0269 (7)
H9A	1.089 (6)	0.381 (4)	0.589 (3)	0.032 (12)*
H9B	1.055 (8)	0.261 (5)	0.634 (4)	0.056 (15)*
H9C	1.265 (8)	0.384 (6)	0.684 (4)	0.070 (17)*
C10	1.0477 (5)	0.3481 (3)	0.8724 (2)	0.0208 (6)
H10A	1.190 (7)	0.368 (4)	0.902 (3)	0.045 (12)*
H10B	0.986 (7)	0.243 (5)	0.849 (3)	0.042 (12)*
H10C	0.980 (10)	0.368 (7)	0.931 (5)	0.11 (2)*
C11	1.2956 (5)	0.7346 (3)	0.6878 (2)	0.0219 (7)
H11A	1.427 (5)	0.722 (4)	0.713 (3)	0.017 (9)*
H11B	1.342 (6)	0.826 (4)	0.671 (3)	0.024 (10)*
H11C	1.237 (6)	0.673 (4)	0.612 (3)	0.034 (11)*
C12	1.2676 (5)	0.8291 (3)	0.9007 (2)	0.0219 (6)
H12A	1.211 (7)	0.813 (5)	0.967 (4)	0.051 (13)*
H12B	1.256 (7)	0.923 (5)	0.895 (4)	0.044 (13)*
H12C	1.412 (9)	0.843 (6)	0.929 (4)	0.082 (18)*
C13	0.8576 (4)	0.8026 (3)	0.7505 (2)	0.0137 (5)
C14	0.8481 (4)	0.8683 (3)	0.6740 (2)	0.0161 (6)
C15	0.7934 (4)	0.9720 (3)	0.6889 (2)	0.0213 (6)
H15	0.783 (7)	1.021 (5)	0.630 (3)	0.053 (13)*
C16	0.7482 (4)	1.0136 (3)	0.7786 (2)	0.0236 (7)
H16	0.706 (5)	1.096 (3)	0.785 (3)	0.017 (8)*
C17	0.7576 (4)	0.9488 (3)	0.8540 (2)	0.0215 (7)
H17	0.742 (6)	0.978 (4)	0.929 (3)	0.044 (12)*
C18	0.8085 (4)	0.8426 (3)	0.8413 (2)	0.0170 (6)
C19	0.8962 (5)	0.8273 (3)	0.5759 (2)	0.0247 (7)
H19A	1.027 (7)	0.809 (5)	0.587 (4)	0.055 (14)*
H19B	0.913 (8)	0.899 (5)	0.540 (4)	0.070 (16)*
H19C	0.797 (8)	0.746 (6)	0.534 (4)	0.072 (17)*
C20	0.8013 (5)	0.7708 (4)	0.9225 (3)	0.0258 (7)
H20A	0.874 (10)	0.822 (7)	0.994 (6)	0.10 (2)*
H20B	0.866 (7)	0.699 (5)	0.913 (4)	0.057 (14)*
H20C	0.671 (11)	0.737 (7)	0.943 (5)	0.10 (2)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Sb	0.01332 (13)	0.01093 (13)	0.01412 (13)	0.00356 (9)	−0.00080 (8)	0.00322 (8)
Si1	0.0142 (4)	0.0116 (4)	0.0151 (4)	0.0055 (3)	0.0019 (3)	0.0041 (3)
Si2	0.0118 (4)	0.0106 (4)	0.0151 (4)	0.0029 (3)	0.0032 (3)	0.0025 (3)
O	0.0144 (10)	0.0131 (10)	0.0311 (11)	0.0017 (8)	−0.0003 (8)	0.0075 (9)
N1	0.0130 (11)	0.0138 (12)	0.0152 (11)	0.0052 (9)	0.0026 (9)	0.0048 (9)
N2	0.0122 (11)	0.0139 (12)	0.0160 (11)	0.0057 (9)	0.0025 (9)	0.0059 (9)
C1	0.0119 (13)	0.0107 (13)	0.0141 (13)	0.0046 (11)	0.0043 (10)	0.0027 (11)
C2	0.0131 (13)	0.0129 (14)	0.0168 (14)	0.0025 (11)	0.0014 (11)	0.0024 (11)
C3	0.0162 (14)	0.0143 (15)	0.0219 (14)	0.0012 (12)	−0.0007 (12)	0.0008 (12)
C4	0.0162 (14)	0.0142 (15)	0.0305 (16)	0.0010 (12)	0.0062 (12)	0.0083 (13)
C5	0.0195 (15)	0.0202 (16)	0.0227 (15)	0.0077 (13)	0.0108 (12)	0.0064 (12)
C6	0.0177 (14)	0.0143 (14)	0.0149 (13)	0.0041 (11)	0.0063 (11)	0.0037 (11)
C7	0.0275 (18)	0.0230 (17)	0.0158 (14)	0.0051 (14)	0.0073 (13)	0.0000 (13)
C8	0.0353 (19)	0.0241 (18)	0.0178 (15)	0.0082 (15)	0.0115 (14)	0.0006 (13)
C9	0.0236 (17)	0.038 (2)	0.0262 (17)	0.0196 (16)	0.0101 (14)	0.0051 (15)
C10	0.0192 (15)	0.0185 (16)	0.0219 (15)	0.0038 (13)	−0.0017 (12)	0.0091 (13)
C11	0.0210 (16)	0.0254 (18)	0.0218 (16)	0.0072 (13)	0.0101 (13)	0.0077 (13)
C12	0.0210 (16)	0.0181 (16)	0.0182 (15)	0.0013 (13)	−0.0012 (12)	−0.0021 (12)
C13	0.0123 (13)	0.0114 (14)	0.0174 (14)	0.0034 (11)	0.0050 (11)	0.0035 (11)
C14	0.0151 (13)	0.0120 (14)	0.0209 (14)	0.0044 (11)	0.0025 (11)	0.0051 (11)
C15	0.0222 (15)	0.0147 (15)	0.0293 (16)	0.0082 (12)	0.0038 (13)	0.0098 (13)
C16	0.0194 (15)	0.0134 (15)	0.0348 (17)	0.0072 (12)	0.0000 (13)	0.0008 (13)
C17	0.0208 (15)	0.0180 (16)	0.0241 (17)	0.0080 (13)	0.0046 (13)	−0.0016 (13)
C18	0.0198 (14)	0.0162 (15)	0.0144 (13)	0.0049 (12)	0.0064 (11)	0.0014 (11)
C19	0.0327 (19)	0.0258 (19)	0.0203 (15)	0.0126 (15)	0.0079 (14)	0.0117 (14)
C20	0.0327 (18)	0.0326 (19)	0.0212 (16)	0.0156 (16)	0.0152 (14)	0.0128 (14)

Geometric parameters (Å, º)

Sb—H1A	1.77 (4)	C9—H9A	1.13 (4)
Sb—N1	2.045 (2)	C9—H9B	1.06 (6)
Sb—N2	2.046 (2)	C9—H9C	1.03 (6)
Si1—O	1.634 (2)	C10—H10A	1.03 (5)
Si1—N1	1.737 (2)	C10—H10B	1.13 (5)
Si1—C9	1.851 (3)	C10—H10C	1.06 (8)
Si1—C10	1.841 (3)	C11—H11A	1.06 (4)
Si2—O	1.627 (2)	C11—H11B	1.09 (4)
Si2—N2	1.735 (2)	C11—H11C	1.10 (4)
Si2—C11	1.851 (3)	C12—H12A	1.10 (5)
Si2—C12	1.854 (3)	C12—H12B	1.14 (5)
N1—C1	1.428 (3)	C12—H12C	1.05 (6)
N2—C13	1.428 (3)	C13—C14	1.404 (4)
C1—C2	1.409 (4)	C13—C18	1.415 (4)
C1—C6	1.406 (4)	C14—C15	1.382 (4)
C2—C3	1.390 (4)	C14—C19	1.502 (4)
C2—C7	1.506 (4)	C15—H15	1.07 (4)
C3—H3	1.04 (4)	C15—C16	1.390 (5)
C3—C4	1.388 (4)	C16—H16	1.09 (4)
C4—H4	1.13 (4)	C16—C17	1.384 (4)
C4—C5	1.386 (4)	C17—H17	1.07 (4)
C5—H5	1.03 (4)	C17—C18	1.391 (4)
C5—C6	1.388 (4)	C18—C20	1.500 (4)
C6—C8	1.509 (4)	C19—H19A	1.07 (5)
C7—H7A	1.06 (4)	C19—H19B	1.02 (6)
C7—H7B	1.03 (5)	C19—H19C	1.02 (6)
C7—H7C	1.17 (6)	C20—H20A	1.02 (8)
C8—H8A	1.19 (11)	C20—H20B	1.09 (5)
C8—H8B	1.12 (5)	C20—H20C	1.06 (7)
C8—H8C	0.96 (6)
N1—Sb—H1A	93.7 (13)	H9B—C9—Si1	116 (3)
N2—Sb—H1A	93.3 (13)	H9B—C9—H9A	91 (3)
N2—Sb—N1	98.56 (9)	H9C—C9—Si1	114 (3)
N1—Si1—O	105.98 (11)	H9C—C9—H9A	103 (4)
C9—Si1—O	107.62 (15)	H9C—C9—H9B	111 (4)
C9—Si1—N1	113.47 (14)	H10A—C10—Si1	109 (2)
C10—Si1—O	109.01 (13)	H10B—C10—Si1	113 (2)
C10—Si1—N1	111.62 (13)	H10B—C10—H10A	105 (3)
C10—Si1—C9	108.94 (16)	H10C—C10—Si1	117 (4)
N2—Si2—O	105.93 (11)	H10C—C10—H10A	110 (4)
C11—Si2—O	107.40 (14)	H10C—C10—H10B	102 (4)
C11—Si2—N2	112.85 (13)	H11A—C11—Si2	109.5 (19)
C12—Si2—O	109.31 (13)	H11B—C11—Si2	120 (2)
C12—Si2—N2	111.38 (14)	H11B—C11—H11A	102 (3)
C12—Si2—C11	109.76 (15)	H11C—C11—Si2	117 (2)
Si2—O—Si1	142.63 (14)	H11C—C11—H11A	104 (3)
Si1—N1—Sb	119.64 (12)	H11C—C11—H11B	102 (3)
C1—N1—Sb	116.88 (17)	H12A—C12—Si2	117 (3)
C1—N1—Si1	122.83 (18)	H12B—C12—Si2	114 (2)
Si2—N2—Sb	120.37 (12)	H12B—C12—H12A	102 (3)
C13—N2—Sb	116.23 (17)	H12C—C12—Si2	115 (3)
C13—N2—Si2	122.71 (19)	H12C—C12—H12A	101 (4)
C2—C1—N1	120.4 (2)	H12C—C12—H12B	107 (4)
C6—C1—N1	120.5 (2)	C14—C13—N2	120.6 (2)
C6—C1—C2	119.2 (2)	C18—C13—N2	119.9 (2)
C3—C2—C1	119.6 (3)	C18—C13—C14	119.4 (3)
C7—C2—C1	120.6 (3)	C15—C14—C13	119.6 (3)
C7—C2—C3	119.8 (3)	C19—C14—C13	120.9 (3)
H3—C3—C2	123 (2)	C19—C14—C15	119.5 (3)
C4—C3—C2	121.4 (3)	H15—C15—C14	120 (3)
C4—C3—H3	115 (2)	C16—C15—C14	121.4 (3)
H4—C4—C3	116 (2)	C16—C15—H15	119 (3)
C5—C4—C3	118.7 (3)	H16—C16—C15	117.3 (18)
C5—C4—H4	125 (2)	C17—C16—C15	118.9 (3)
H5—C5—C4	118 (2)	C17—C16—H16	123.8 (18)
C6—C5—C4	121.6 (3)	H17—C17—C16	125 (2)
C6—C5—H5	120 (2)	C18—C17—C16	121.5 (3)
C5—C6—C1	119.5 (3)	C18—C17—H17	113 (2)
C8—C6—C1	121.4 (3)	C17—C18—C13	119.0 (3)
C8—C6—C5	119.0 (3)	C20—C18—C13	122.0 (3)
H7A—C7—C2	117 (2)	C20—C18—C17	118.9 (3)
H7B—C7—C2	111 (3)	H19A—C19—C14	113 (3)
H7B—C7—H7A	105 (4)	H19B—C19—C14	107 (3)
H7C—C7—C2	112 (3)	H19B—C19—H19A	107 (4)
H7C—C7—H7A	104 (3)	H19C—C19—C14	112 (3)
H7C—C7—H7B	107 (4)	H19C—C19—H19A	105 (4)
H8A—C8—C6	93 (5)	H19C—C19—H19B	113 (4)
H8B—C8—C6	114 (3)	H20A—C20—C18	115 (4)
H8B—C8—H8A	84 (5)	H20B—C20—C18	114 (2)
H8C—C8—C6	111 (4)	H20B—C20—H20A	102 (5)
H8C—C8—H8A	134 (6)	H20C—C20—C18	118 (4)
H8C—C8—H8B	117 (5)	H20C—C20—H20A	94 (5)
H9A—C9—Si1	118 (2)	H20C—C20—H20B	111 (5)

(TIWXOP_HAR_NoMoRe_1)

Crystal data

C20H31N2OSbSi2	Z = 2
Mr = 493.41	F(000) = 503.308
Triclinic, P1	Dx = 1.475 Mg m^−3
a = 7.6028 (5) Å	Mo Kα radiation, λ = 0.71073 Å
b = 11.5896 (8) Å	Cell parameters from 5427 reflections
c = 13.8020 (7) Å	θ = 3.8–29.0°
α = 99.459 (5)°	µ = 1.36 mm^−1
β = 100.012 (5)°	T = 120 K
γ = 107.557 (6)°	Block, colourless
V = 1110.98 (13) Å^3	0.17 × 0.11 × 0.07 mm

Data collection

SuperNova, Dual, Cu at zero, EosS2 diffractometer	4181 reflections with I ≥ 2u(I)
ω scans	Rint = 0.030
Absorption correction: gaussian CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	θmax = 26.4°, θmin = 3.4°
Tmin = 0.744, Tmax = 1	h = −9→9
8520 measured reflections	k = −13→14
4543 independent reflections	l = −17→13

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.028	Only H-atom coordinates refined
wR(F^2) = 0.058	w = 1/[σ^2(Fo^2) + (0.0168P)^2 + 0.5884P] where P = (Fo^2 + 2Fc^2)/3
S = 0.94	(Δ/σ)max = 0.001
4543 reflections	Δρmax = 1.00 e Å^−3
328 parameters	Δρmin = −0.58 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Sb	0.72529 (2)	0.536326 (16)	0.644337 (12)	0.01269 (6)
H1A	0.883 (5)	0.519 (3)	0.563 (2)	0.037997
Si1	1.01936 (10)	0.42363 (7)	0.76616 (5)	0.01387 (15)
Si2	1.15146 (10)	0.70706 (7)	0.78229 (5)	0.01328 (15)
O	1.1415 (2)	0.57206 (17)	0.80499 (13)	0.0209 (4)
N1	0.7850 (3)	0.4128 (2)	0.72353 (14)	0.0141 (4)
N2	0.9184 (3)	0.69716 (19)	0.73798 (14)	0.0136 (4)
C1	0.6279 (3)	0.3103 (2)	0.72797 (17)	0.0128 (5)
C2	0.5386 (4)	0.2094 (2)	0.64344 (18)	0.0157 (5)
C3	0.3880 (4)	0.1084 (3)	0.6496 (2)	0.0199 (6)
H3	0.322 (4)	0.028 (3)	0.588 (2)	0.037734
C4	0.3248 (4)	0.1052 (3)	0.7382 (2)	0.0210 (6)
H4	0.204 (5)	0.019 (3)	0.740 (2)	0.038626
C5	0.4121 (4)	0.2057 (3)	0.8207 (2)	0.0198 (6)
H5	0.359 (5)	0.201 (3)	0.886 (2)	0.039518
C6	0.5603 (4)	0.3091 (2)	0.81647 (18)	0.0162 (5)
C7	0.6022 (4)	0.2095 (3)	0.5464 (2)	0.0236 (6)
H7A	0.539 (5)	0.127 (3)	0.491 (2)	0.043455
H7B	0.750 (5)	0.233 (4)	0.556 (2)	0.054475
H7C	0.576 (5)	0.282 (3)	0.505 (2)	0.047101
C8	0.6392 (5)	0.4182 (3)	0.9058 (2)	0.0276 (7)
H8A	0.559 (6)	0.473 (3)	0.903 (2)	0.052008
H8B	0.776 (5)	0.485 (3)	0.904 (3)	0.051200
H8C	0.647 (5)	0.392 (4)	0.977 (3)	0.061390
C9	1.1193 (4)	0.3581 (3)	0.6658 (2)	0.0273 (7)
H9A	1.091 (5)	0.394 (3)	0.598 (2)	0.037502
H9B	1.053 (5)	0.255 (3)	0.643 (2)	0.037250
H9C	1.267 (5)	0.383 (3)	0.687 (2)	0.033381
C10	1.0476 (4)	0.3477 (3)	0.8726 (2)	0.0217 (6)
H10A	1.194 (5)	0.369 (3)	0.904 (2)	0.044394
H10B	0.979 (5)	0.239 (3)	0.848 (3)	0.045088
H10C	0.978 (5)	0.366 (3)	0.928 (2)	0.047517
C11	1.2960 (4)	0.7345 (3)	0.6877 (2)	0.0231 (6)
H11A	1.429 (5)	0.719 (3)	0.712 (2)	0.035851
H11B	1.337 (5)	0.827 (3)	0.674 (2)	0.044987
H11C	1.223 (5)	0.673 (3)	0.616 (2)	0.040339
C12	1.2676 (4)	0.8291 (3)	0.9008 (2)	0.0230 (6)
H12A	1.207 (6)	0.814 (4)	0.964 (3)	0.070958
H12B	1.268 (7)	0.923 (4)	0.892 (3)	0.106478
H12C	1.407 (5)	0.833 (4)	0.927 (3)	0.074107
C13	0.8577 (3)	0.8027 (2)	0.75089 (18)	0.0138 (5)
C14	0.8481 (4)	0.8683 (2)	0.67410 (18)	0.0161 (5)
C15	0.7940 (4)	0.9724 (3)	0.6889 (2)	0.0215 (6)
H15	0.791 (5)	1.023 (3)	0.631 (2)	0.038001
C16	0.7483 (4)	1.0135 (3)	0.7787 (2)	0.0240 (6)
H16	0.711 (5)	1.100 (3)	0.790 (2)	0.041447
C17	0.7578 (4)	0.9490 (3)	0.8541 (2)	0.0216 (6)
H17	0.729 (5)	0.979 (3)	0.927 (2)	0.040548
C18	0.8086 (4)	0.8425 (2)	0.84123 (18)	0.0172 (6)
C19	0.8962 (4)	0.8275 (3)	0.5759 (2)	0.0242 (6)
H19A	1.024 (5)	0.806 (3)	0.587 (2)	0.037725
H19B	0.915 (5)	0.902 (3)	0.535 (2)	0.039059
H19C	0.786 (5)	0.745 (3)	0.529 (2)	0.034912
C20	0.8013 (5)	0.7709 (3)	0.9226 (2)	0.0265 (7)
H20A	0.870 (5)	0.832 (3)	0.999 (2)	0.055198
H20B	0.869 (5)	0.703 (3)	0.914 (2)	0.044647
H20C	0.662 (5)	0.726 (4)	0.929 (2)	0.049514

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Sb	0.01259 (10)	0.01021 (10)	0.01337 (10)	0.00331 (7)	−0.00108 (7)	0.00309 (7)
H1A	0.050000	0.035000	0.033000	0.016000	0.020000	0.005000
Si1	0.0144 (4)	0.0122 (4)	0.0155 (3)	0.0055 (3)	0.0020 (3)	0.0043 (3)
Si2	0.0120 (3)	0.0110 (4)	0.0159 (3)	0.0030 (3)	0.0030 (3)	0.0027 (3)
O	0.0148 (9)	0.0144 (10)	0.0308 (10)	0.0028 (8)	−0.0001 (8)	0.0078 (8)
N1	0.0131 (11)	0.0140 (12)	0.0148 (10)	0.0043 (9)	0.0023 (9)	0.0037 (9)
N2	0.0126 (11)	0.0138 (11)	0.0157 (10)	0.0059 (9)	0.0023 (9)	0.0049 (8)
C1	0.0122 (12)	0.0112 (13)	0.0159 (12)	0.0043 (10)	0.0048 (10)	0.0037 (10)
C2	0.0136 (13)	0.0141 (14)	0.0170 (12)	0.0029 (11)	0.0015 (10)	0.0026 (10)
C3	0.0166 (14)	0.0141 (14)	0.0239 (14)	0.0014 (11)	0.0006 (11)	0.0026 (11)
H3	0.027000	0.032000	0.039000	−0.002000	0.004000	−0.006000
C4	0.0166 (14)	0.0158 (15)	0.0290 (15)	0.0019 (12)	0.0054 (12)	0.0073 (12)
H4	0.027000	0.039000	0.048000	0.003000	0.017000	0.012000
C5	0.0208 (14)	0.0199 (15)	0.0220 (13)	0.0076 (12)	0.0103 (12)	0.0070 (12)
H5	0.043000	0.046000	0.033000	0.015000	0.021000	0.006000
C6	0.0165 (13)	0.0153 (14)	0.0171 (12)	0.0049 (11)	0.0061 (11)	0.0027 (11)
C7	0.0275 (16)	0.0233 (17)	0.0169 (13)	0.0056 (13)	0.0068 (12)	0.0000 (12)
H7A	0.035000	0.044000	0.032000	−0.001000	0.004000	−0.012000
H7B	0.049000	0.088000	0.040000	0.047000	0.011000	0.006000
H7C	0.063000	0.035000	0.040000	0.004000	0.029000	0.006000
C8	0.0344 (18)	0.0231 (17)	0.0231 (15)	0.0082 (14)	0.0113 (14)	−0.0022 (13)
H8A	0.073000	0.026000	0.042000	0.004000	0.001000	0.005000
H8B	0.044000	0.043000	0.051000	0.015000	−0.013000	−0.006000
H8C	0.057000	0.057000	0.055000	0.008000	0.027000	−0.021000
C9	0.0240 (16)	0.037 (2)	0.0275 (15)	0.0196 (15)	0.0099 (13)	0.0049 (14)
H9A	0.049000	0.041000	0.027000	0.019000	0.009000	0.013000
H9B	0.041000	0.023000	0.043000	0.007000	0.012000	0.000000
H9C	0.027000	0.039000	0.037000	0.016000	0.008000	0.007000
C10	0.0207 (15)	0.0202 (16)	0.0221 (14)	0.0050 (12)	−0.0011 (12)	0.0094 (12)
H10A	0.037000	0.052000	0.043000	0.013000	−0.002000	0.024000
H10B	0.056000	0.022000	0.051000	0.004000	0.009000	0.013000
H10C	0.063000	0.056000	0.049000	0.036000	0.035000	0.028000
C11	0.0213 (15)	0.0272 (17)	0.0233 (14)	0.0075 (13)	0.0105 (12)	0.0084 (13)
H11A	0.033000	0.041000	0.042000	0.020000	0.013000	0.014000
H11B	0.047000	0.039000	0.058000	0.011000	0.029000	0.025000
H11C	0.039000	0.053000	0.027000	0.015000	0.005000	0.008000
C12	0.0229 (16)	0.0196 (16)	0.0192 (14)	0.0031 (13)	0.0006 (12)	−0.0023 (12)
H12A	0.048000	0.096000	0.040000	0.003000	0.008000	−0.019000
H12B	0.140000	0.030000	0.087000	−0.022000	−0.052000	0.025000
H12C	0.033000	0.099000	0.071000	0.030000	−0.015000	−0.018000
C13	0.0126 (12)	0.0112 (13)	0.0174 (12)	0.0034 (10)	0.0045 (10)	0.0031 (10)
C14	0.0146 (13)	0.0132 (14)	0.0207 (13)	0.0048 (11)	0.0030 (10)	0.0057 (11)
C15	0.0220 (14)	0.0152 (15)	0.0283 (15)	0.0077 (12)	0.0028 (12)	0.0082 (12)
H15	0.048000	0.029000	0.040000	0.014000	0.007000	0.018000
C16	0.0203 (14)	0.0139 (15)	0.0349 (16)	0.0070 (12)	0.0006 (12)	0.0017 (12)
H16	0.050000	0.021000	0.050000	0.015000	0.003000	0.003000
C17	0.0207 (14)	0.0186 (16)	0.0245 (14)	0.0086 (12)	0.0050 (12)	−0.0009 (12)
H17	0.053000	0.032000	0.032000	0.015000	0.008000	−0.004000
C18	0.0190 (14)	0.0156 (14)	0.0165 (12)	0.0055 (11)	0.0062 (11)	0.0015 (11)
C19	0.0309 (17)	0.0262 (17)	0.0203 (14)	0.0128 (14)	0.0079 (13)	0.0105 (13)
H19A	0.049000	0.040000	0.037000	0.028000	0.016000	0.013000
H19B	0.049000	0.037000	0.038000	0.013000	0.019000	0.021000
H19C	0.034000	0.036000	0.028000	0.006000	0.003000	0.005000
C20	0.0329 (18)	0.0328 (19)	0.0229 (15)	0.0160 (15)	0.0144 (13)	0.0134 (13)
H20A	0.061000	0.050000	0.030000	−0.006000	−0.010000	0.012000
H20B	0.066000	0.030000	0.049000	0.021000	0.027000	0.016000
H20C	0.050000	0.063000	0.050000	0.025000	0.029000	0.023000

Geometric parameters (Å, º)

Sb—H1A	1.81 (3)	C9—H9A	1.09 (3)
Sb—N1	2.046 (2)	C9—H9B	1.11 (3)
Sb—N2	2.049 (2)	C9—H9C	1.05 (3)
Si1—O	1.6337 (19)	C10—H10A	1.06 (3)
Si1—N1	1.736 (2)	C10—H10B	1.18 (4)
Si1—C9	1.855 (3)	C10—H10C	1.03 (3)
Si1—C10	1.845 (3)	C11—H11A	1.09 (3)
Si2—O	1.6278 (19)	C11—H11B	1.08 (3)
Si2—N2	1.733 (2)	C11—H11C	1.07 (3)
Si2—C11	1.854 (3)	C12—H12A	1.07 (4)
Si2—C12	1.855 (3)	C12—H12B	1.12 (5)
N1—C1	1.426 (3)	C12—H12C	1.04 (4)
N2—C13	1.428 (3)	C13—C14	1.407 (3)
C1—C2	1.410 (3)	C13—C18	1.409 (3)
C1—C6	1.406 (3)	C14—C15	1.383 (4)
C2—C3	1.395 (4)	C14—C19	1.504 (4)
C2—C7	1.501 (3)	C15—H15	1.06 (3)
C3—H3	1.07 (3)	C15—C16	1.392 (4)
C3—C4	1.392 (4)	C16—H16	1.12 (3)
C4—H4	1.14 (3)	C16—C17	1.383 (4)
C4—C5	1.388 (4)	C17—H17	1.08 (3)
C5—H5	1.05 (3)	C17—C18	1.394 (4)
C5—C6	1.393 (4)	C18—C20	1.501 (4)
C6—C8	1.501 (4)	C19—H19A	1.06 (3)
C7—H7A	1.04 (3)	C19—H19B	1.10 (3)
C7—H7B	1.05 (4)	C19—H19C	1.07 (3)
C7—H7C	1.13 (4)	C20—H20A	1.11 (3)
C8—H8A	1.00 (4)	C20—H20B	1.07 (3)
C8—H8B	1.10 (4)	C20—H20C	1.05 (4)
C8—H8C	1.07 (4)
N1—Sb—H1A	93.3 (10)	H9B—C9—Si1	110.9 (16)
N2—Sb—H1A	93.8 (10)	H9B—C9—H9A	107 (2)
N2—Sb—N1	98.55 (8)	H9C—C9—Si1	112.9 (17)
N1—Si1—O	106.14 (10)	H9C—C9—H9A	105 (2)
C9—Si1—O	107.53 (13)	H9C—C9—H9B	110 (2)
C9—Si1—N1	113.34 (12)	H10A—C10—Si1	109.4 (17)
C10—Si1—O	109.11 (11)	H10B—C10—Si1	112.8 (16)
C10—Si1—N1	111.57 (12)	H10B—C10—H10A	107 (3)
C10—Si1—C9	108.98 (14)	H10C—C10—Si1	116.2 (18)
N2—Si2—O	106.04 (10)	H10C—C10—H10A	111 (3)
C11—Si2—O	107.22 (12)	H10C—C10—H10B	100 (3)
C11—Si2—N2	112.98 (12)	H11A—C11—Si2	110.2 (16)
C12—Si2—O	109.26 (12)	H11B—C11—Si2	116.6 (17)
C12—Si2—N2	111.36 (12)	H11B—C11—H11A	105 (3)
C12—Si2—C11	109.77 (14)	H11C—C11—Si2	110.9 (18)
Si2—O—Si1	142.53 (12)	H11C—C11—H11A	108 (2)
Si1—N1—Sb	119.61 (11)	H11C—C11—H11B	106 (2)
C1—N1—Sb	116.93 (15)	H12A—C12—Si2	116 (2)
C1—N1—Si1	122.82 (17)	H12B—C12—Si2	113 (2)
Si2—N2—Sb	120.32 (11)	H12B—C12—H12A	105 (3)
C13—N2—Sb	116.26 (15)	H12C—C12—Si2	110 (2)
C13—N2—Si2	122.74 (17)	H12C—C12—H12A	103 (3)
C2—C1—N1	120.2 (2)	H12C—C12—H12B	109 (3)
C6—C1—N1	120.4 (2)	C14—C13—N2	120.4 (2)
C6—C1—C2	119.4 (2)	C18—C13—N2	120.1 (2)
C3—C2—C1	119.6 (2)	C18—C13—C14	119.5 (2)
C7—C2—C1	120.9 (2)	C15—C14—C13	119.7 (2)
C7—C2—C3	119.5 (2)	C19—C14—C13	121.1 (2)
H3—C3—C2	121.5 (17)	C19—C14—C15	119.2 (2)
C4—C3—C2	121.1 (2)	H15—C15—C14	119.3 (17)
C4—C3—H3	117.2 (17)	C16—C15—C14	121.2 (3)
H4—C4—C3	117.9 (16)	C16—C15—H15	119.5 (17)
C5—C4—C3	118.8 (2)	H16—C16—C15	119.7 (17)
C5—C4—H4	123.2 (16)	C17—C16—C15	119.1 (3)
H5—C5—C4	116.8 (18)	C17—C16—H16	121.1 (17)
C6—C5—C4	121.6 (2)	H17—C17—C16	122.0 (17)
C6—C5—H5	121.6 (18)	C18—C17—C16	121.3 (2)
C5—C6—C1	119.4 (2)	C18—C17—H17	116.7 (17)
C8—C6—C1	121.8 (2)	C17—C18—C13	119.2 (2)
C8—C6—C5	118.8 (2)	C20—C18—C13	122.0 (2)
H7A—C7—C2	115.5 (18)	C20—C18—C17	118.7 (2)
H7B—C7—C2	113.4 (18)	H19A—C19—C14	112.5 (16)
H7B—C7—H7A	108 (3)	H19B—C19—C14	109.8 (16)
H7C—C7—C2	115.2 (16)	H19B—C19—H19A	108 (2)
H7C—C7—H7A	103 (2)	H19C—C19—C14	111.2 (16)
H7C—C7—H7B	101 (3)	H19C—C19—H19A	106 (3)
H8A—C8—C6	110 (2)	H19C—C19—H19B	109 (2)
H8B—C8—C6	113.9 (18)	H20A—C20—C18	112.5 (18)
H8B—C8—H8A	100 (3)	H20B—C20—C18	113.7 (17)
H8C—C8—C6	113 (2)	H20B—C20—H20A	106 (3)
H8C—C8—H8A	109 (3)	H20C—C20—C18	113.4 (19)
H8C—C8—H8B	111 (3)	H20C—C20—H20A	103 (3)
H9A—C9—Si1	111.0 (17)	H20C—C20—H20B	108 (3)
Sb—N1—C1—C2	75.89 (18)	N2—C13—C14—C15	−178.2 (2)
Sb—N1—C1—C6	−104.01 (17)	N2—C13—C14—C19	1.6 (3)
Sb—N2—C13—C14	−75.73 (18)	N2—C13—C18—C17	177.2 (2)
Sb—N2—C13—C18	104.88 (17)	N2—C13—C18—C20	−5.4 (3)
Si1—O—Si2—N2	32.7 (2)	C1—C2—C3—C4	−0.4 (3)
Si1—O—Si2—C11	−88.3 (2)	C1—C6—C5—C4	−2.2 (3)
Si1—O—Si2—C12	152.8 (2)	C2—C3—C4—C5	1.2 (3)
Si1—N1—C1—C2	−94.90 (19)	C3—C4—C5—C6	0.2 (3)
Si1—N1—C1—C6	85.2 (2)	C4—C5—C6—C8	175.8 (3)
Si2—N2—C13—C14	94.83 (19)	C13—C14—C15—C16	−0.1 (3)
Si2—N2—C13—C18	−84.6 (2)	C13—C18—C17—C16	2.3 (3)
N1—C1—C2—C3	178.5 (2)	C14—C15—C16—C17	0.1 (3)
N1—C1—C2—C7	−2.1 (3)	C15—C16—C17—C18	−1.2 (3)
N1—C1—C6—C5	−177.2 (2)	C16—C17—C18—C20	−175.2 (3)
N1—C1—C6—C8	4.9 (3)

(TIWXOP_HAR_NoMoRe)

Crystal data

C20H31N2OSbSi2	Z = 2
Mr = 493.41	F(000) = 503.308
Triclinic, P1	Dx = 1.475 Mg m^−3
a = 7.6028 (5) Å	Mo Kα radiation, λ = 0.71073 Å
b = 11.5896 (8) Å	Cell parameters from 5427 reflections
c = 13.8020 (7) Å	θ = 3.8–29.0°
α = 99.459 (5)°	µ = 1.36 mm^−1
β = 100.012 (5)°	T = 120 K
γ = 107.557 (6)°	Block, colourless
V = 1110.98 (13) Å^3	0.17 × 0.11 × 0.07 mm

Data collection

SuperNova, Dual, Cu at zero, EosS2 diffractometer	4181 reflections with I ≥ 2u(I)
ω scans	Rint = 0.030
Absorption correction: gaussian CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	θmax = 26.4°, θmin = 3.4°
Tmin = 0.744, Tmax = 1	h = −9→9
8520 measured reflections	k = −13→14
4543 independent reflections	l = −17→13

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.029	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.092	w = 1/[σ^2(Fo^2) + (0.1P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 0.70	(Δ/σ)max = 0.001
4543 reflections	Δρmax = 0.97 e Å^−3
328 parameters	Δρmin = −0.58 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Sb	0.72530 (2)	0.536300 (16)	0.644317 (12)	0.01296 (9)
H1A	0.881 (6)	0.519 (4)	0.565 (3)	0.037739
Si1	1.01938 (11)	0.42349 (7)	0.76612 (6)	0.01409 (17)
Si2	1.15155 (11)	0.70701 (7)	0.78226 (6)	0.01337 (17)
O	1.1414 (3)	0.57212 (19)	0.80512 (16)	0.0214 (4)
N1	0.7849 (3)	0.4128 (2)	0.72349 (17)	0.0144 (5)
N2	0.9182 (3)	0.6971 (2)	0.73781 (17)	0.0141 (5)
C1	0.6277 (4)	0.3104 (3)	0.7280 (2)	0.0126 (5)
C2	0.5384 (4)	0.2091 (3)	0.6433 (2)	0.0157 (6)
C3	0.3880 (4)	0.1087 (3)	0.6498 (2)	0.0202 (6)
H3	0.321 (6)	0.029 (4)	0.590 (3)	0.037864
C4	0.3247 (4)	0.1052 (3)	0.7381 (2)	0.0213 (6)
H4	0.208 (6)	0.018 (4)	0.741 (3)	0.038834
C5	0.4121 (4)	0.2055 (3)	0.8206 (2)	0.0202 (6)
H5	0.357 (6)	0.203 (4)	0.886 (3)	0.038201
C6	0.5597 (4)	0.3087 (3)	0.8162 (2)	0.0160 (6)
C7	0.6021 (5)	0.2099 (3)	0.5462 (2)	0.0237 (7)
H7A	0.550 (6)	0.126 (4)	0.490 (3)	0.042963
H7B	0.752 (7)	0.237 (5)	0.558 (3)	0.053028
H7C	0.555 (7)	0.281 (4)	0.503 (3)	0.047773
C8	0.6382 (5)	0.4189 (3)	0.9056 (2)	0.0266 (7)
H8A	0.561 (8)	0.486 (5)	0.864 (4)	0.050852
H8B	0.767 (7)	0.492 (4)	0.900 (4)	0.050199
H8C	0.637 (7)	0.396 (5)	0.967 (4)	0.059975
C9	1.1192 (5)	0.3580 (4)	0.6659 (3)	0.0272 (7)
H9A	1.096 (7)	0.392 (4)	0.590 (3)	0.036985
H9B	1.051 (6)	0.261 (4)	0.634 (3)	0.037614
H9C	1.259 (6)	0.384 (4)	0.680 (3)	0.033226
C10	1.0477 (4)	0.3480 (3)	0.8723 (2)	0.0213 (6)
H10A	1.190 (6)	0.367 (4)	0.902 (3)	0.043113
H10B	0.984 (7)	0.241 (4)	0.848 (3)	0.045082
H10C	0.974 (7)	0.368 (4)	0.928 (3)	0.046477
C11	1.2957 (5)	0.7346 (3)	0.6878 (2)	0.0227 (7)
H11A	1.431 (6)	0.725 (4)	0.715 (3)	0.035334
H11B	1.344 (7)	0.829 (4)	0.672 (3)	0.044878
H11C	1.231 (7)	0.674 (5)	0.614 (3)	0.040827
C12	1.2679 (5)	0.8291 (3)	0.9008 (2)	0.0223 (6)
H12A	1.208 (7)	0.815 (6)	0.968 (4)	0.066423
H12B	1.266 (10)	0.925 (5)	0.892 (5)	0.104374
H12C	1.412 (7)	0.841 (5)	0.926 (4)	0.073063
C13	0.8577 (4)	0.8026 (3)	0.7506 (2)	0.0143 (5)
C14	0.8480 (4)	0.8684 (3)	0.6740 (2)	0.0167 (6)
C15	0.7934 (4)	0.9720 (3)	0.6888 (2)	0.0218 (6)
H15	0.788 (6)	1.022 (4)	0.630 (3)	0.036985
C16	0.7481 (4)	1.0136 (3)	0.7786 (2)	0.0242 (7)
H16	0.708 (6)	1.098 (4)	0.785 (3)	0.040333
C17	0.7576 (4)	0.9489 (3)	0.8541 (2)	0.0221 (7)
H17	0.736 (6)	0.979 (4)	0.929 (3)	0.039539
C18	0.8085 (4)	0.8424 (3)	0.8413 (2)	0.0178 (6)
C19	0.8962 (5)	0.8275 (3)	0.5760 (2)	0.0248 (7)
H19A	1.023 (6)	0.805 (4)	0.586 (3)	0.037725
H19B	0.908 (6)	0.898 (4)	0.536 (3)	0.038696
H19C	0.792 (6)	0.744 (4)	0.530 (3)	0.034912
C20	0.8015 (5)	0.7708 (3)	0.9227 (2)	0.0262 (7)
H20A	0.868 (7)	0.829 (5)	0.998 (3)	0.053644
H20B	0.857 (7)	0.697 (4)	0.910 (3)	0.043488
H20C	0.677 (7)	0.738 (5)	0.944 (3)	0.047472

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Sb	0.01287 (13)	0.01048 (13)	0.01366 (13)	0.00341 (8)	−0.00090 (8)	0.00311 (8)
H1A	0.049000	0.035000	0.033000	0.016000	0.019000	0.005000
Si1	0.0146 (4)	0.0123 (4)	0.0158 (4)	0.0057 (3)	0.0020 (3)	0.0043 (3)
Si2	0.0124 (4)	0.0112 (4)	0.0157 (4)	0.0032 (3)	0.0033 (3)	0.0026 (3)
O	0.0152 (10)	0.0137 (10)	0.0319 (11)	0.0019 (8)	0.0000 (9)	0.0077 (9)
N1	0.0135 (11)	0.0145 (12)	0.0158 (11)	0.0053 (9)	0.0026 (9)	0.0045 (9)
N2	0.0124 (11)	0.0145 (12)	0.0171 (11)	0.0061 (9)	0.0026 (9)	0.0063 (9)
C1	0.0124 (13)	0.0115 (13)	0.0155 (13)	0.0051 (11)	0.0050 (10)	0.0031 (11)
C2	0.0138 (13)	0.0141 (14)	0.0169 (14)	0.0032 (11)	0.0016 (11)	0.0026 (11)
C3	0.0164 (14)	0.0151 (15)	0.0230 (14)	0.0015 (12)	−0.0010 (11)	0.0011 (12)
H3	0.027000	0.032000	0.039000	−0.002000	0.003000	−0.006000
C4	0.0168 (14)	0.0152 (15)	0.0302 (16)	0.0012 (12)	0.0063 (12)	0.0080 (13)
H4	0.027000	0.038000	0.050000	0.003000	0.018000	0.012000
C5	0.0199 (15)	0.0201 (16)	0.0234 (15)	0.0073 (12)	0.0103 (12)	0.0062 (12)
H5	0.043000	0.042000	0.034000	0.015000	0.022000	0.006000
C6	0.0180 (14)	0.0150 (14)	0.0151 (13)	0.0042 (11)	0.0063 (11)	0.0038 (11)
C7	0.0289 (17)	0.0237 (17)	0.0159 (14)	0.0058 (14)	0.0077 (13)	0.0008 (13)
H7A	0.034000	0.044000	0.032000	0.000000	0.003000	−0.012000
H7B	0.047000	0.086000	0.039000	0.045000	0.011000	0.006000
H7C	0.064000	0.036000	0.040000	0.005000	0.028000	0.006000
C8	0.0361 (19)	0.0249 (18)	0.0174 (15)	0.0073 (15)	0.0122 (14)	0.0005 (13)
H8A	0.072000	0.024000	0.042000	0.004000	0.000000	0.006000
H8B	0.045000	0.040000	0.051000	0.016000	−0.014000	−0.005000
H8C	0.058000	0.053000	0.055000	0.008000	0.028000	−0.020000
C9	0.0227 (17)	0.039 (2)	0.0275 (17)	0.0193 (16)	0.0106 (14)	0.0049 (15)
H9A	0.048000	0.041000	0.026000	0.018000	0.009000	0.013000
H9B	0.041000	0.023000	0.043000	0.006000	0.011000	0.000000
H9C	0.026000	0.039000	0.037000	0.015000	0.008000	0.007000
C10	0.0196 (15)	0.0198 (16)	0.0226 (15)	0.0046 (13)	−0.0010 (13)	0.0100 (13)
H10A	0.035000	0.051000	0.042000	0.013000	−0.002000	0.022000
H10B	0.056000	0.022000	0.050000	0.003000	0.009000	0.012000
H10C	0.061000	0.055000	0.048000	0.035000	0.034000	0.027000
C11	0.0221 (16)	0.0272 (18)	0.0217 (15)	0.0079 (14)	0.0109 (13)	0.0081 (13)
H11A	0.033000	0.040000	0.041000	0.019000	0.013000	0.014000
H11B	0.047000	0.039000	0.057000	0.011000	0.028000	0.024000
H11C	0.039000	0.053000	0.027000	0.014000	0.004000	0.007000
C12	0.0219 (16)	0.0183 (16)	0.0182 (14)	0.0011 (13)	−0.0007 (12)	−0.0024 (12)
H12A	0.046000	0.090000	0.038000	0.005000	0.007000	−0.016000
H12B	0.140000	0.030000	0.082000	−0.023000	−0.048000	0.025000
H12C	0.031000	0.099000	0.070000	0.029000	−0.013000	−0.019000
C13	0.0131 (13)	0.0117 (13)	0.0184 (14)	0.0035 (11)	0.0054 (11)	0.0035 (11)
C14	0.0156 (13)	0.0128 (14)	0.0211 (14)	0.0045 (11)	0.0024 (11)	0.0050 (11)
C15	0.0222 (15)	0.0155 (15)	0.0298 (16)	0.0083 (12)	0.0039 (12)	0.0096 (13)
H15	0.047000	0.028000	0.039000	0.014000	0.007000	0.017000
C16	0.0201 (15)	0.0142 (15)	0.0351 (17)	0.0074 (12)	0.0003 (13)	0.0011 (13)
H16	0.049000	0.021000	0.048000	0.015000	0.003000	0.003000
C17	0.0210 (15)	0.0183 (16)	0.0255 (17)	0.0082 (13)	0.0049 (13)	−0.0013 (13)
H17	0.051000	0.032000	0.031000	0.015000	0.007000	−0.004000
C18	0.0206 (14)	0.0169 (15)	0.0155 (13)	0.0053 (12)	0.0069 (11)	0.0018 (11)
C19	0.0330 (18)	0.0266 (18)	0.0200 (15)	0.0132 (15)	0.0080 (14)	0.0116 (14)
H19A	0.049000	0.040000	0.037000	0.028000	0.016000	0.013000
H19B	0.049000	0.037000	0.037000	0.013000	0.019000	0.021000
H19C	0.034000	0.036000	0.028000	0.006000	0.003000	0.005000
C20	0.0331 (18)	0.0326 (19)	0.0220 (16)	0.0157 (15)	0.0159 (14)	0.0128 (14)
H20A	0.057000	0.050000	0.030000	−0.006000	−0.010000	0.012000
H20B	0.063000	0.030000	0.049000	0.021000	0.026000	0.017000
H20C	0.047000	0.061000	0.049000	0.025000	0.027000	0.023000

Geometric parameters (Å, º)

Sb—H1A	1.78 (4)	C9—H9A	1.18 (4)
Sb—N1	2.045 (2)	C9—H9B	1.06 (4)
Sb—N2	2.047 (2)	C9—H9C	0.99 (4)
Si1—O	1.636 (2)	C10—H10A	1.03 (4)
Si1—N1	1.737 (2)	C10—H10B	1.15 (4)
Si1—C9	1.853 (3)	C10—H10C	1.05 (4)
Si1—C10	1.840 (3)	C11—H11A	1.08 (4)
Si2—O	1.627 (2)	C11—H11B	1.11 (5)
Si2—N2	1.735 (2)	C11—H11C	1.08 (4)
Si2—C11	1.851 (3)	C12—H12A	1.12 (5)
Si2—C12	1.855 (3)	C12—H12B	1.14 (6)
N1—C1	1.427 (3)	C12—H12C	1.05 (4)
N2—C13	1.427 (3)	C13—C14	1.406 (4)
C1—C2	1.413 (4)	C13—C18	1.414 (4)
C1—C6	1.404 (4)	C14—C15	1.381 (4)
C2—C3	1.391 (4)	C14—C19	1.502 (4)
C2—C7	1.503 (4)	C15—H15	1.07 (3)
C3—H3	1.05 (4)	C15—C16	1.392 (4)
C3—C4	1.389 (4)	C16—H16	1.11 (4)
C4—H4	1.14 (4)	C16—C17	1.384 (4)
C4—C5	1.387 (4)	C17—H17	1.10 (4)
C5—H5	1.06 (4)	C17—C18	1.394 (4)
C5—C6	1.389 (4)	C18—C20	1.501 (4)
C6—C8	1.509 (4)	C19—H19A	1.07 (4)
C7—H7A	1.05 (4)	C19—H19B	1.05 (4)
C7—H7B	1.06 (5)	C19—H19C	1.06 (4)
C7—H7C	1.19 (5)	C20—H20A	1.08 (5)
C8—H8A	1.25 (5)	C20—H20B	1.07 (4)
C8—H8B	1.11 (5)	C20—H20C	1.02 (4)
C8—H8C	0.94 (5)
N1—Sb—H1A	93.2 (13)	H9B—C9—Si1	115 (2)
N2—Sb—H1A	93.6 (14)	H9B—C9—H9A	97 (3)
N2—Sb—N1	98.58 (9)	H9C—C9—Si1	116 (2)
N1—Si1—O	106.00 (11)	H9C—C9—H9A	97 (3)
C9—Si1—O	107.66 (14)	H9C—C9—H9B	113 (3)
C9—Si1—N1	113.39 (14)	H10A—C10—Si1	109 (2)
C10—Si1—O	109.00 (13)	H10B—C10—Si1	113 (2)
C10—Si1—N1	111.65 (13)	H10B—C10—H10A	105 (3)
C10—Si1—C9	108.96 (16)	H10C—C10—Si1	115 (2)
N2—Si2—O	106.00 (11)	H10C—C10—H10A	113 (3)
C11—Si2—O	107.41 (14)	H10C—C10—H10B	101 (3)
C11—Si2—N2	112.90 (13)	H11A—C11—Si2	109 (2)
C12—Si2—O	109.23 (13)	H11B—C11—Si2	119 (2)
C12—Si2—N2	111.41 (13)	H11B—C11—H11A	100 (3)
C12—Si2—C11	109.70 (15)	H11C—C11—Si2	115 (2)
Si2—O—Si1	142.53 (14)	H11C—C11—H11A	108 (3)
Si1—N1—Sb	119.68 (12)	H11C—C11—H11B	104 (3)
C1—N1—Sb	116.90 (17)	H12A—C12—Si2	117 (3)
C1—N1—Si1	122.78 (18)	H12B—C12—Si2	113 (3)
Si2—N2—Sb	120.32 (12)	H12B—C12—H12A	104 (5)
C13—N2—Sb	116.29 (17)	H12C—C12—Si2	113 (3)
C13—N2—Si2	122.70 (19)	H12C—C12—H12A	104 (4)
C2—C1—N1	120.2 (2)	H12C—C12—H12B	105 (4)
C6—C1—N1	120.7 (2)	C14—C13—N2	120.6 (2)
C6—C1—C2	119.1 (2)	C18—C13—N2	119.9 (2)
C3—C2—C1	119.5 (3)	C18—C13—C14	119.5 (3)
C7—C2—C1	120.7 (3)	C15—C14—C13	119.7 (3)
C7—C2—C3	119.9 (3)	C19—C14—C13	120.9 (3)
H3—C3—C2	122 (2)	C19—C14—C15	119.4 (3)
C4—C3—C2	121.4 (3)	H15—C15—C14	119 (2)
C4—C3—H3	116 (2)	C16—C15—C14	121.4 (3)
H4—C4—C3	119 (2)	C16—C15—H15	120 (2)
C5—C4—C3	118.8 (3)	H16—C16—C15	117 (2)
C5—C4—H4	123 (2)	C17—C16—C15	119.0 (3)
H5—C5—C4	118 (2)	C17—C16—H16	124 (2)
C6—C5—C4	121.5 (3)	H17—C17—C16	124 (2)
C6—C5—H5	121 (2)	C18—C17—C16	121.5 (3)
C5—C6—C1	119.7 (3)	C18—C17—H17	114 (2)
C8—C6—C1	121.4 (3)	C17—C18—C13	119.0 (3)
C8—C6—C5	118.8 (3)	C20—C18—C13	122.1 (3)
H7A—C7—C2	118 (2)	C20—C18—C17	118.8 (3)
H7B—C7—C2	112 (2)	H19A—C19—C14	113 (2)
H7B—C7—H7A	105 (3)	H19B—C19—C14	109 (2)
H7C—C7—C2	112 (2)	H19B—C19—H19A	110 (3)
H7C—C7—H7A	103 (3)	H19C—C19—C14	112 (2)
H7C—C7—H7B	106 (3)	H19C—C19—H19A	103 (3)
H8A—C8—C6	95 (2)	H19C—C19—H19B	109 (3)
H8B—C8—C6	114 (3)	H20A—C20—C18	113 (2)
H8B—C8—H8A	81 (3)	H20B—C20—C18	113 (2)
H8C—C8—C6	113 (3)	H20B—C20—H20A	110 (4)
H8C—C8—H8A	132 (4)	H20C—C20—C18	119 (3)
H8C—C8—H8B	118 (4)	H20C—C20—H20A	90 (4)
H9A—C9—Si1	115 (2)	H20C—C20—H20B	108 (4)

(TIWXOP_HAR_SHADE3_1)

Crystal data

C20H31N2OSbSi2	Z = 2
Mr = 493.41	F(000) = 503.265
Triclinic, P1	Dx = 1.475 Mg m^−3
a = 7.6028 (5) Å	Mo Kα radiation, λ = 0.71073 Å
b = 11.5896 (8) Å	Cell parameters from 5427 reflections
c = 13.8020 (7) Å	θ = 3.8–29.0°
α = 99.459 (5)°	µ = 1.36 mm^−1
β = 100.012 (5)°	T = 120 K
γ = 107.557 (6)°	Block, colourless
V = 1110.98 (13) Å^3	0.17 × 0.11 × 0.07 mm

Data collection

SuperNova, Dual, Cu at zero, EosS2 diffractometer	4181 reflections with I ≥ 2u(I)
ω scans	Rint = 0.030
Absorption correction: gaussian CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	θmax = 26.4°, θmin = 3.4°
Tmin = 0.744, Tmax = 1	h = −9→9
8520 measured reflections	k = −13→14
4543 independent reflections	l = −17→13

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.029	Only H-atom coordinates refined
wR(F^2) = 0.051	w = 1/[σ^2(Fo^2) + (0.P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 1.10	(Δ/σ)max = 0.001
4543 reflections	Δρmax = 0.98 e Å^−3
328 parameters	Δρmin = −0.60 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Sb	0.72530 (2)	0.536332 (16)	0.644355 (11)	0.01314 (6)
H1A	0.882 (4)	0.519 (3)	0.5622 (17)	0.035086
Si1	1.01938 (10)	0.42367 (7)	0.76617 (5)	0.01316 (15)
Si2	1.15148 (10)	0.70706 (7)	0.78231 (5)	0.01256 (15)
O	1.1414 (2)	0.57196 (16)	0.80484 (11)	0.0200 (4)
N1	0.7850 (3)	0.41277 (19)	0.72348 (13)	0.0133 (4)
N2	0.9184 (3)	0.69721 (19)	0.73806 (13)	0.0128 (4)
C1	0.6280 (3)	0.3103 (2)	0.72808 (16)	0.0119 (5)
C2	0.5387 (3)	0.2095 (2)	0.64349 (16)	0.0152 (5)
C3	0.3880 (4)	0.1086 (3)	0.64971 (18)	0.0190 (6)
H3	0.321 (4)	0.029 (3)	0.5887 (18)	0.032574
C4	0.3246 (4)	0.1052 (3)	0.73826 (19)	0.0201 (6)
H4	0.204 (4)	0.020 (3)	0.740 (2)	0.034860
C5	0.4122 (4)	0.2057 (3)	0.82049 (18)	0.0191 (6)
H5	0.361 (4)	0.201 (3)	0.8840 (19)	0.036529
C6	0.5603 (4)	0.3092 (2)	0.81646 (17)	0.0157 (6)
C7	0.6020 (4)	0.2094 (3)	0.54640 (19)	0.0229 (6)
H7A	0.535 (4)	0.128 (3)	0.4910 (19)	0.035548
H7B	0.743 (4)	0.232 (3)	0.5549 (19)	0.031252
H7C	0.573 (4)	0.279 (3)	0.5048 (19)	0.033604
C8	0.6399 (5)	0.4178 (3)	0.9059 (2)	0.0272 (7)
H8A	0.568 (4)	0.467 (3)	0.908 (2)	0.034871
H8B	0.776 (4)	0.483 (3)	0.9034 (19)	0.031311
H8C	0.658 (4)	0.393 (3)	0.980 (2)	0.036431
C9	1.1196 (4)	0.3583 (3)	0.6658 (2)	0.0265 (7)
H9A	1.094 (4)	0.395 (3)	0.599 (2)	0.036751
H9B	1.058 (4)	0.258 (3)	0.643 (2)	0.036219
H9C	1.270 (4)	0.382 (3)	0.687 (2)	0.037410
C10	1.0476 (4)	0.3477 (3)	0.87254 (19)	0.0209 (6)
H10A	1.195 (4)	0.369 (3)	0.905 (2)	0.039642
H10B	0.982 (5)	0.240 (3)	0.849 (2)	0.037140
H10C	0.984 (4)	0.368 (3)	0.9286 (18)	0.033209
C11	1.2960 (4)	0.7344 (3)	0.68763 (19)	0.0226 (6)
H11A	1.427 (4)	0.718 (3)	0.710 (2)	0.036618
H11B	1.336 (4)	0.825 (3)	0.675 (2)	0.036146
H11C	1.222 (4)	0.672 (3)	0.616 (2)	0.036006
C12	1.2674 (4)	0.8288 (3)	0.90078 (19)	0.0224 (6)
H12A	1.210 (4)	0.811 (3)	0.9650 (19)	0.031486
H12B	1.267 (4)	0.920 (3)	0.8937 (19)	0.026163
H12C	1.405 (4)	0.833 (3)	0.9275 (19)	0.031279
C13	0.8577 (3)	0.8027 (2)	0.75099 (16)	0.0130 (5)
C14	0.8483 (3)	0.8683 (2)	0.67420 (17)	0.0153 (5)
C15	0.7942 (4)	0.9724 (3)	0.68896 (19)	0.0208 (6)
H15	0.790 (4)	1.023 (3)	0.6318 (19)	0.035667
C16	0.7483 (4)	1.0135 (3)	0.7787 (2)	0.0233 (6)
H16	0.710 (4)	1.099 (3)	0.790 (2)	0.037105
C17	0.7578 (4)	0.9490 (3)	0.85416 (19)	0.0208 (6)
H17	0.730 (4)	0.979 (3)	0.926 (2)	0.036874
C18	0.8088 (4)	0.8426 (2)	0.84123 (17)	0.0163 (6)
C19	0.8961 (4)	0.8274 (3)	0.57584 (19)	0.0236 (6)
H19A	1.019 (4)	0.805 (3)	0.5869 (19)	0.033683
H19B	0.912 (4)	0.902 (3)	0.5354 (18)	0.038169
H19C	0.784 (4)	0.747 (3)	0.5297 (19)	0.036569
C20	0.8015 (4)	0.7711 (3)	0.9225 (2)	0.0258 (7)
H20A	0.866 (4)	0.829 (3)	0.998 (2)	0.035488
H20B	0.873 (4)	0.706 (3)	0.9176 (19)	0.033384
H20C	0.662 (4)	0.723 (3)	0.923 (2)	0.036538

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Sb	0.01303 (10)	0.01066 (10)	0.01382 (9)	0.00346 (7)	−0.00102 (7)	0.00320 (7)
H1A	0.040890	0.033540	0.033400	0.014310	0.014330	0.005700
Si1	0.0137 (4)	0.0114 (4)	0.0148 (3)	0.0053 (3)	0.0019 (3)	0.0041 (3)
Si2	0.0113 (4)	0.0103 (4)	0.0151 (3)	0.0027 (3)	0.0028 (3)	0.0026 (3)
O	0.0139 (10)	0.0137 (10)	0.0292 (9)	0.0023 (8)	−0.0004 (8)	0.0070 (8)
N1	0.0124 (11)	0.0130 (12)	0.0139 (10)	0.0040 (9)	0.0022 (9)	0.0032 (9)
N2	0.0127 (11)	0.0128 (12)	0.0139 (9)	0.0058 (9)	0.0019 (8)	0.0044 (8)
C1	0.0112 (13)	0.0105 (14)	0.0151 (12)	0.0040 (11)	0.0042 (10)	0.0037 (10)
C2	0.0131 (13)	0.0133 (15)	0.0167 (12)	0.0027 (11)	0.0014 (10)	0.0025 (11)
C3	0.0161 (14)	0.0135 (15)	0.0228 (13)	0.0016 (12)	0.0008 (11)	0.0026 (11)
H3	0.027540	0.024360	0.035490	0.002120	−0.001500	0.001220
C4	0.0157 (14)	0.0149 (16)	0.0280 (14)	0.0019 (12)	0.0049 (12)	0.0068 (12)
H4	0.023800	0.028300	0.049540	0.002990	0.011480	0.009240
C5	0.0207 (15)	0.0197 (16)	0.0211 (13)	0.0081 (13)	0.0108 (12)	0.0077 (12)
H5	0.037680	0.031230	0.041760	0.007760	0.021160	0.006440
C6	0.0153 (14)	0.0146 (15)	0.0171 (12)	0.0046 (12)	0.0060 (11)	0.0022 (11)
C7	0.0245 (16)	0.0232 (17)	0.0174 (13)	0.0050 (14)	0.0068 (13)	−0.0007 (12)
H7A	0.037820	0.029000	0.027260	0.003460	−0.002920	−0.001200
H7B	0.035120	0.030050	0.032420	0.015930	0.006650	0.009820
H7C	0.043910	0.023890	0.032240	0.009450	0.005290	0.012310
C8	0.0322 (19)	0.0224 (18)	0.0254 (14)	0.0088 (15)	0.0119 (14)	−0.0034 (13)
H8A	0.041110	0.025500	0.039290	0.007070	0.015840	0.012370
H8B	0.028660	0.031250	0.032760	0.009900	0.004240	0.007750
H8C	0.044770	0.032880	0.033430	0.011130	0.019950	0.005120
C9	0.0242 (17)	0.035 (2)	0.0268 (15)	0.0192 (15)	0.0099 (13)	0.0044 (14)
H9A	0.048950	0.033830	0.033880	0.016270	0.016200	0.014230
H9B	0.039400	0.020060	0.046190	0.005490	0.014390	0.003810
H9C	0.025680	0.036550	0.052660	0.013860	0.012020	0.008380
C10	0.0210 (16)	0.0187 (16)	0.0205 (14)	0.0048 (13)	−0.0012 (12)	0.0083 (12)
H10A	0.026410	0.047110	0.042180	0.011710	−0.004790	0.016790
H10B	0.047940	0.019970	0.036680	0.005210	0.005670	0.004740
H10C	0.035160	0.033530	0.030320	0.011540	0.007570	0.006180
C11	0.0209 (16)	0.0259 (18)	0.0238 (14)	0.0073 (14)	0.0108 (12)	0.0089 (13)
H11A	0.033600	0.033690	0.051450	0.019400	0.015390	0.013140
H11B	0.038050	0.024370	0.046620	0.004450	0.019400	0.011620
H11C	0.035520	0.034090	0.032330	0.006720	0.007210	0.001840
C12	0.0222 (16)	0.0183 (16)	0.0199 (14)	0.0035 (13)	−0.0003 (12)	−0.0022 (12)
H12A	0.040260	0.029030	0.025380	0.010810	0.008410	0.008040
H12B	0.026050	0.020960	0.033750	0.009170	0.008090	0.009170
H12C	0.024760	0.026870	0.041400	0.009710	−0.000140	0.012400
C13	0.0113 (13)	0.0106 (14)	0.0169 (12)	0.0032 (10)	0.0044 (10)	0.0025 (10)
C14	0.0133 (13)	0.0127 (14)	0.0207 (12)	0.0045 (11)	0.0035 (10)	0.0059 (11)
C15	0.0210 (15)	0.0141 (15)	0.0277 (14)	0.0070 (12)	0.0022 (12)	0.0081 (12)
H15	0.040510	0.025210	0.039640	0.011160	0.000950	0.012150
C16	0.0194 (15)	0.0125 (15)	0.0347 (15)	0.0063 (12)	0.0000 (12)	0.0013 (12)
H16	0.035070	0.020650	0.056180	0.012270	0.009060	0.007020
C17	0.0201 (15)	0.0183 (16)	0.0236 (14)	0.0087 (12)	0.0055 (12)	−0.0008 (12)
H17	0.042470	0.026950	0.043740	0.013300	0.018580	0.003340
C18	0.0180 (14)	0.0147 (15)	0.0160 (12)	0.0051 (12)	0.0059 (11)	0.0015 (11)
C19	0.0298 (18)	0.0259 (18)	0.0200 (14)	0.0129 (15)	0.0073 (13)	0.0105 (12)
H19A	0.042470	0.029170	0.032660	0.017840	0.006730	0.007500
H19B	0.052500	0.026300	0.032480	0.007170	0.007190	0.012960
H19C	0.033970	0.031910	0.032080	0.003740	−0.004850	0.003240
C20	0.0320 (18)	0.0317 (19)	0.0222 (14)	0.0157 (15)	0.0138 (14)	0.0125 (13)
H20A	0.037100	0.032170	0.031280	0.005640	0.008310	0.002780
H20B	0.045290	0.022290	0.035330	0.013520	0.013700	0.005880
H20C	0.029880	0.038040	0.046040	0.010900	0.019810	0.011250

Geometric parameters (Å, º)

Sb—H1A	1.81 (2)	C9—H9A	1.09 (3)
Sb—N1	2.0453 (19)	C9—H9B	1.08 (3)
Sb—N2	2.049 (2)	C9—H9C	1.07 (3)
Si1—O	1.6320 (19)	C10—H10A	1.07 (3)
Si1—N1	1.736 (2)	C10—H10B	1.16 (3)
Si1—C9	1.856 (3)	C10—H10C	1.01 (3)
Si1—C10	1.845 (3)	C11—H11A	1.07 (3)
Si2—O	1.6279 (18)	C11—H11B	1.05 (3)
Si2—N2	1.734 (2)	C11—H11C	1.06 (3)
Si2—C11	1.855 (3)	C12—H12A	1.08 (3)
Si2—C12	1.852 (3)	C12—H12B	1.08 (3)
N1—C1	1.427 (3)	C12—H12C	1.03 (3)
N2—C13	1.427 (3)	C13—C14	1.407 (3)
C1—C2	1.409 (3)	C13—C18	1.407 (3)
C1—C6	1.404 (3)	C14—C15	1.384 (3)
C2—C3	1.396 (3)	C14—C19	1.505 (3)
C2—C7	1.500 (3)	C15—H15	1.06 (2)
C3—H3	1.07 (3)	C15—C16	1.392 (3)
C3—C4	1.392 (3)	C16—H16	1.10 (3)
C4—H4	1.13 (3)	C16—C17	1.382 (3)
C4—C5	1.387 (4)	C17—H17	1.07 (2)
C5—H5	1.02 (2)	C17—C18	1.393 (3)
C5—C6	1.392 (3)	C18—C20	1.499 (3)
C6—C8	1.499 (4)	C19—H19A	1.03 (3)
C7—H7A	1.03 (3)	C19—H19B	1.09 (3)
C7—H7B	1.00 (3)	C19—H19C	1.06 (3)
C7—H7C	1.12 (3)	C20—H20A	1.08 (3)
C8—H8A	0.90 (3)	C20—H20B	1.05 (3)
C8—H8B	1.09 (3)	C20—H20C	1.04 (3)
C8—H8C	1.10 (3)
N1—Sb—H1A	93.7 (8)	H9B—C9—Si1	111.6 (15)
N2—Sb—H1A	94.0 (9)	H9B—C9—H9A	108 (2)
N2—Sb—N1	98.56 (7)	H9C—C9—Si1	113.3 (16)
N1—Si1—O	106.13 (10)	H9C—C9—H9A	105 (2)
C9—Si1—O	107.45 (12)	H9C—C9—H9B	108 (2)
C9—Si1—N1	113.37 (12)	H10A—C10—Si1	109.8 (15)
C10—Si1—O	109.17 (11)	H10B—C10—Si1	113.3 (13)
C10—Si1—N1	111.60 (11)	H10B—C10—H10A	106 (2)
C10—Si1—C9	108.93 (14)	H10C—C10—Si1	116.6 (15)
N2—Si2—O	106.00 (10)	H10C—C10—H10A	108 (2)
C11—Si2—O	107.15 (11)	H10C—C10—H10B	102 (2)
C11—Si2—N2	113.00 (11)	H11A—C11—Si2	110.7 (15)
C12—Si2—O	109.29 (11)	H11B—C11—Si2	116.3 (15)
C12—Si2—N2	111.32 (12)	H11B—C11—H11A	105 (2)
C12—Si2—C11	109.86 (13)	H11C—C11—Si2	110.3 (16)
Si2—O—Si1	142.65 (11)	H11C—C11—H11A	107 (2)
Si1—N1—Sb	119.63 (11)	H11C—C11—H11B	107 (2)
C1—N1—Sb	117.00 (15)	H12A—C12—Si2	115.2 (16)
C1—N1—Si1	122.75 (16)	H12B—C12—Si2	113.7 (14)
Si2—N2—Sb	120.27 (11)	H12B—C12—H12A	106 (2)
C13—N2—Sb	116.28 (15)	H12C—C12—Si2	111.2 (16)
C13—N2—Si2	122.76 (16)	H12C—C12—H12A	100 (2)
C2—C1—N1	120.12 (19)	H12C—C12—H12B	109 (2)
C6—C1—N1	120.4 (2)	C14—C13—N2	120.3 (2)
C6—C1—C2	119.4 (2)	C18—C13—N2	120.2 (2)
C3—C2—C1	119.6 (2)	C18—C13—C14	119.5 (2)
C7—C2—C1	121.1 (2)	C15—C14—C13	119.7 (2)
C7—C2—C3	119.4 (2)	C19—C14—C13	121.2 (2)
H3—C3—C2	121.8 (15)	C19—C14—C15	119.1 (2)
C4—C3—C2	121.2 (2)	H15—C15—C14	119.4 (15)
C4—C3—H3	116.9 (15)	C16—C15—C14	121.1 (2)
H4—C4—C3	118.4 (14)	C16—C15—H15	119.5 (15)
C5—C4—C3	118.6 (2)	H16—C16—C15	120.1 (15)
C5—C4—H4	122.9 (14)	C17—C16—C15	119.2 (3)
H5—C5—C4	116.7 (17)	C17—C16—H16	120.7 (15)
C6—C5—C4	121.8 (2)	H17—C17—C16	122.2 (15)
C6—C5—H5	121.4 (17)	C18—C17—C16	121.3 (2)
C5—C6—C1	119.3 (2)	C18—C17—H17	116.5 (15)
C8—C6—C1	121.8 (2)	C17—C18—C13	119.3 (2)
C8—C6—C5	118.9 (2)	C20—C18—C13	122.0 (2)
H7A—C7—C2	114.9 (15)	C20—C18—C17	118.7 (2)
H7B—C7—C2	114.3 (15)	H19A—C19—C14	111.9 (14)
H7B—C7—H7A	109 (2)	H19B—C19—C14	108.8 (15)
H7C—C7—C2	115.3 (14)	H19B—C19—H19A	110 (2)
H7C—C7—H7A	101 (2)	H19C—C19—C14	110.4 (15)
H7C—C7—H7B	101 (2)	H19C—C19—H19A	108 (2)
H8A—C8—C6	112.5 (19)	H19C—C19—H19B	108 (2)
H8B—C8—C6	112.9 (15)	H20A—C20—C18	114.0 (15)
H8B—C8—H8A	102 (2)	H20B—C20—C18	114.9 (15)
H8C—C8—C6	114.8 (16)	H20B—C20—H20A	103 (2)
H8C—C8—H8A	106 (2)	H20C—C20—C18	111.6 (16)
H8C—C8—H8B	108 (2)	H20C—C20—H20A	105 (2)
H9A—C9—Si1	110.9 (15)	H20C—C20—H20B	107 (2)
Sb—N1—C1—C2	75.81 (17)	N2—C13—C14—C15	−178.2 (2)
Sb—N1—C1—C6	−103.79 (16)	N2—C13—C14—C19	1.8 (3)
Sb—N2—C13—C14	−75.76 (17)	N2—C13—C18—C17	177.2 (2)
Sb—N2—C13—C18	104.94 (17)	N2—C13—C18—C20	−5.5 (3)
Si1—O—Si2—N2	32.62 (19)	C1—C2—C3—C4	−0.3 (3)
Si1—O—Si2—C11	−88.3 (2)	C1—C6—C5—C4	−2.4 (3)
Si1—O—Si2—C12	152.69 (19)	C2—C3—C4—C5	1.1 (3)
Si1—N1—C1—C2	−95.11 (18)	C3—C4—C5—C6	0.2 (3)
Si1—N1—C1—C6	85.29 (19)	C4—C5—C6—C8	176.1 (3)
Si2—N2—C13—C14	94.77 (19)	C13—C14—C15—C16	−0.1 (3)
Si2—N2—C13—C18	−84.53 (19)	C13—C18—C17—C16	2.2 (3)
N1—C1—C2—C3	178.6 (2)	C14—C15—C16—C17	0.2 (3)
N1—C1—C2—C7	−2.0 (3)	C15—C16—C17—C18	−1.3 (3)
N1—C1—C6—C5	−177.2 (2)	C16—C17—C18—C20	−175.2 (3)
N1—C1—C6—C8	4.3 (3)

(TIWXOP_HAR_SHADE3)

Crystal data

C20H31N2OSbSi2	Z = 2
Mr = 493.41	F(000) = 503.265
Triclinic, P1	Dx = 1.475 Mg m^−3
a = 7.6028 (5) Å	Mo Kα radiation, λ = 0.71073 Å
b = 11.5896 (8) Å	Cell parameters from 5427 reflections
c = 13.8020 (7) Å	θ = 3.8–29.0°
α = 99.459 (5)°	µ = 1.36 mm^−1
β = 100.012 (5)°	T = 120 K
γ = 107.557 (6)°	Block, colourless
V = 1110.98 (13) Å^3	0.17 × 0.11 × 0.07 mm

Data collection

SuperNova, Dual, Cu at zero, EosS2 diffractometer	4181 reflections with I ≥ 2u(I)
ω scans	Rint = 0.030
Absorption correction: gaussian CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	θmax = 26.4°, θmin = 3.4°
Tmin = 0.744, Tmax = 1	h = −9→9
8520 measured reflections	k = −13→14
4543 independent reflections	l = −17→13

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.029	Only H-atom coordinates refined
wR(F^2) = 0.051	w = 1/[σ^2(Fo^2) + (0.P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 1.10	(Δ/σ)max = 0.001
4543 reflections	Δρmax = 0.98 e Å^−3
328 parameters	Δρmin = −0.60 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Sb	0.72530 (2)	0.536332 (16)	0.644355 (11)	0.01314 (6)
H1A	0.883 (4)	0.519 (3)	0.5623 (17)	0.034208
Si1	1.01938 (10)	0.42367 (7)	0.76617 (5)	0.01316 (15)
Si2	1.15148 (10)	0.70706 (7)	0.78231 (5)	0.01257 (15)
O	1.1414 (2)	0.57197 (16)	0.80485 (11)	0.0200 (4)
N1	0.7850 (3)	0.41277 (19)	0.72348 (13)	0.0133 (4)
N2	0.9183 (3)	0.69720 (19)	0.73805 (13)	0.0128 (4)
C1	0.6280 (3)	0.3103 (2)	0.72810 (16)	0.0119 (5)
C2	0.5387 (3)	0.2095 (2)	0.64349 (16)	0.0152 (5)
C3	0.3880 (4)	0.1086 (3)	0.64972 (18)	0.0190 (6)
H3	0.321 (4)	0.028 (3)	0.5880 (18)	0.034182
C4	0.3246 (4)	0.1052 (3)	0.73826 (19)	0.0201 (6)
H4	0.204 (4)	0.020 (3)	0.740 (2)	0.037619
C5	0.4122 (4)	0.2057 (3)	0.82052 (18)	0.0191 (6)
H5	0.361 (4)	0.201 (3)	0.8841 (19)	0.038068
C6	0.5603 (4)	0.3092 (2)	0.81647 (17)	0.0157 (6)
C7	0.6020 (4)	0.2094 (3)	0.54644 (19)	0.0229 (6)
H7A	0.534 (4)	0.127 (3)	0.4908 (19)	0.036160
H7B	0.744 (4)	0.232 (3)	0.5548 (19)	0.030744
H7C	0.573 (4)	0.279 (3)	0.5053 (19)	0.033258
C8	0.6398 (5)	0.4179 (3)	0.9059 (2)	0.0273 (7)
H8A	0.567 (4)	0.466 (3)	0.910 (2)	0.035053
H8B	0.775 (4)	0.483 (3)	0.9028 (19)	0.030218
H8C	0.658 (4)	0.393 (3)	0.980 (2)	0.036860
C9	1.1196 (4)	0.3583 (3)	0.6658 (2)	0.0265 (7)
H9A	1.094 (4)	0.395 (3)	0.599 (2)	0.036599
H9B	1.058 (4)	0.257 (3)	0.643 (2)	0.036544
H9C	1.270 (4)	0.382 (3)	0.688 (2)	0.038496
C10	1.0476 (4)	0.3477 (3)	0.87251 (19)	0.0209 (6)
H10A	1.196 (4)	0.369 (3)	0.905 (2)	0.041565
H10B	0.982 (5)	0.240 (3)	0.849 (2)	0.037949
H10C	0.985 (4)	0.368 (3)	0.9285 (18)	0.033866
C11	1.2960 (4)	0.7344 (3)	0.68765 (19)	0.0226 (6)
H11A	1.427 (4)	0.718 (3)	0.710 (2)	0.037970
H11B	1.337 (4)	0.825 (3)	0.674 (2)	0.036743
H11C	1.222 (4)	0.673 (3)	0.617 (2)	0.035913
C12	1.2674 (4)	0.8287 (3)	0.90076 (19)	0.0225 (6)
H12A	1.210 (4)	0.811 (3)	0.9649 (19)	0.032302
H12B	1.267 (4)	0.921 (3)	0.8940 (19)	0.026763
H12C	1.406 (4)	0.833 (3)	0.9279 (19)	0.033058
C13	0.8577 (3)	0.8027 (2)	0.75101 (16)	0.0130 (5)
C14	0.8483 (3)	0.8683 (2)	0.67421 (17)	0.0153 (5)
C15	0.7941 (4)	0.9724 (3)	0.68896 (19)	0.0208 (6)
H15	0.789 (4)	1.023 (3)	0.6311 (19)	0.037225
C16	0.7483 (4)	1.0135 (3)	0.7787 (2)	0.0233 (6)
H16	0.710 (4)	1.098 (3)	0.790 (2)	0.039587
C17	0.7579 (4)	0.9490 (3)	0.85419 (19)	0.0208 (6)
H17	0.731 (4)	0.979 (3)	0.926 (2)	0.038294
C18	0.8088 (4)	0.8426 (2)	0.84124 (17)	0.0164 (6)
C19	0.8960 (4)	0.8274 (3)	0.57588 (19)	0.0236 (6)
H19A	1.020 (4)	0.806 (3)	0.5868 (19)	0.033224
H19B	0.912 (4)	0.903 (3)	0.5350 (19)	0.039050
H19C	0.785 (4)	0.748 (3)	0.5302 (19)	0.036487
C20	0.8015 (4)	0.7711 (3)	0.9225 (2)	0.0258 (7)
H20A	0.866 (4)	0.829 (3)	0.999 (2)	0.036058
H20B	0.873 (4)	0.707 (3)	0.9173 (19)	0.032458
H20C	0.662 (4)	0.723 (3)	0.924 (2)	0.036591

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Sb	0.01304 (10)	0.01066 (10)	0.01382 (9)	0.00346 (7)	−0.00102 (7)	0.00320 (7)
H1A	0.040790	0.032100	0.032450	0.013930	0.014720	0.005490
Si1	0.0138 (4)	0.0114 (4)	0.0148 (3)	0.0053 (3)	0.0019 (3)	0.0041 (3)
Si2	0.0113 (4)	0.0103 (4)	0.0151 (3)	0.0027 (3)	0.0028 (3)	0.0026 (3)
O	0.0140 (10)	0.0136 (10)	0.0292 (9)	0.0024 (8)	−0.0004 (8)	0.0070 (8)
N1	0.0123 (11)	0.0130 (12)	0.0139 (10)	0.0040 (9)	0.0022 (9)	0.0032 (9)
N2	0.0127 (11)	0.0129 (12)	0.0139 (9)	0.0058 (9)	0.0020 (8)	0.0045 (8)
C1	0.0112 (13)	0.0104 (14)	0.0150 (12)	0.0039 (11)	0.0042 (10)	0.0036 (10)
C2	0.0131 (13)	0.0134 (15)	0.0166 (12)	0.0026 (11)	0.0015 (10)	0.0025 (11)
C3	0.0162 (14)	0.0134 (15)	0.0227 (13)	0.0014 (12)	0.0007 (11)	0.0024 (11)
H3	0.031310	0.023960	0.034930	−0.000260	−0.000130	0.000220
C4	0.0157 (14)	0.0150 (16)	0.0280 (14)	0.0021 (12)	0.0050 (12)	0.0069 (12)
H4	0.028300	0.028460	0.051450	0.000440	0.015010	0.008280
C5	0.0205 (15)	0.0197 (16)	0.0212 (13)	0.0081 (13)	0.0105 (12)	0.0077 (12)
H5	0.041680	0.030720	0.042490	0.006670	0.024340	0.005810
C6	0.0153 (14)	0.0147 (15)	0.0171 (12)	0.0048 (12)	0.0060 (11)	0.0023 (11)
C7	0.0244 (16)	0.0233 (17)	0.0176 (13)	0.0050 (14)	0.0068 (13)	−0.0007 (12)
H7A	0.040630	0.027910	0.026330	0.002030	−0.002120	−0.001600
H7B	0.036300	0.028670	0.031580	0.015630	0.008140	0.009840
H7C	0.044490	0.022970	0.030880	0.008370	0.005450	0.011930
C8	0.0321 (19)	0.0226 (18)	0.0254 (14)	0.0086 (15)	0.0122 (14)	−0.0037 (13)
H8A	0.042520	0.024780	0.039370	0.006810	0.017430	0.012120
H8B	0.028360	0.029970	0.030920	0.009690	0.003610	0.007300
H8C	0.048650	0.031850	0.031640	0.011060	0.020610	0.004800
C9	0.0245 (17)	0.035 (2)	0.0268 (15)	0.0193 (15)	0.0100 (13)	0.0045 (14)
H9A	0.049730	0.033240	0.034200	0.016750	0.017590	0.014620
H9B	0.041320	0.019990	0.046930	0.007000	0.015940	0.004680
H9C	0.025930	0.037980	0.055680	0.015580	0.012920	0.009530
C10	0.0211 (16)	0.0188 (16)	0.0205 (14)	0.0049 (13)	−0.0012 (12)	0.0083 (12)
H10A	0.028880	0.049150	0.044100	0.014010	−0.005880	0.017830
H10B	0.051430	0.020320	0.036610	0.007230	0.006350	0.005520
H10C	0.038410	0.033710	0.029290	0.012700	0.007550	0.006450
C11	0.0210 (16)	0.0259 (18)	0.0238 (14)	0.0072 (14)	0.0108 (12)	0.0089 (13)
H11A	0.032600	0.034710	0.054890	0.018640	0.016130	0.013010
H11B	0.038470	0.023860	0.047680	0.003110	0.020510	0.010990
H11C	0.035680	0.033240	0.032650	0.006090	0.008200	0.001520
C12	0.0223 (16)	0.0183 (16)	0.0199 (14)	0.0034 (13)	−0.0003 (12)	−0.0022 (12)
H12A	0.042070	0.029050	0.024450	0.009780	0.007520	0.007350
H12B	0.027090	0.020510	0.033500	0.007660	0.008080	0.008310
H12C	0.024710	0.028210	0.043210	0.008220	−0.001720	0.011860
C13	0.0114 (13)	0.0105 (14)	0.0169 (12)	0.0033 (10)	0.0044 (10)	0.0026 (10)
C14	0.0134 (13)	0.0127 (14)	0.0206 (12)	0.0046 (11)	0.0035 (10)	0.0058 (11)
C15	0.0212 (15)	0.0141 (15)	0.0277 (14)	0.0071 (12)	0.0023 (12)	0.0082 (12)
H15	0.047530	0.025450	0.039020	0.014140	0.002850	0.012900
C16	0.0192 (15)	0.0126 (15)	0.0346 (15)	0.0062 (12)	0.0000 (12)	0.0012 (12)
H16	0.043120	0.021650	0.057770	0.016390	0.012730	0.008380
C17	0.0198 (15)	0.0182 (16)	0.0238 (14)	0.0086 (12)	0.0053 (12)	−0.0008 (12)
H17	0.048150	0.026940	0.044320	0.015310	0.022020	0.003940
C18	0.0178 (14)	0.0148 (15)	0.0161 (12)	0.0050 (12)	0.0058 (11)	0.0014 (11)
C19	0.0298 (18)	0.0258 (18)	0.0202 (14)	0.0129 (15)	0.0074 (13)	0.0105 (12)
H19A	0.043770	0.027640	0.031850	0.017710	0.007960	0.007070
H19B	0.057610	0.025310	0.031790	0.008380	0.008580	0.013010
H19C	0.035950	0.031160	0.030980	0.004510	−0.004900	0.003140
C20	0.0321 (18)	0.0318 (19)	0.0224 (14)	0.0159 (15)	0.0141 (14)	0.0126 (13)
H20A	0.040840	0.031230	0.030200	0.005670	0.009470	0.002530
H20B	0.045350	0.021120	0.033470	0.013180	0.013180	0.005620
H20C	0.031010	0.037470	0.046490	0.011400	0.021250	0.011440

Geometric parameters (Å, º)

Sb—H1A	1.82 (2)	C9—H9A	1.08 (3)
Sb—N1	2.0453 (19)	C9—H9B	1.09 (3)
Sb—N2	2.049 (2)	C9—H9C	1.07 (3)
Si1—O	1.6320 (19)	C10—H10A	1.08 (3)
Si1—N1	1.736 (2)	C10—H10B	1.16 (3)
Si1—C9	1.856 (3)	C10—H10C	1.01 (3)
Si1—C10	1.845 (3)	C11—H11A	1.07 (3)
Si2—O	1.6279 (18)	C11—H11B	1.06 (3)
Si2—N2	1.734 (2)	C11—H11C	1.06 (3)
Si2—C11	1.855 (3)	C12—H12A	1.07 (3)
Si2—C12	1.852 (3)	C12—H12B	1.08 (3)
N1—C1	1.427 (3)	C12—H12C	1.03 (3)
N2—C13	1.427 (3)	C13—C14	1.407 (3)
C1—C2	1.409 (3)	C13—C18	1.407 (3)
C1—C6	1.404 (3)	C14—C15	1.384 (3)
C2—C3	1.396 (3)	C14—C19	1.504 (3)
C2—C7	1.500 (3)	C15—H15	1.06 (3)
C3—H3	1.07 (3)	C15—C16	1.393 (3)
C3—C4	1.392 (3)	C16—H16	1.10 (3)
C4—H4	1.13 (3)	C16—C17	1.383 (3)
C4—C5	1.387 (4)	C17—H17	1.07 (2)
C5—H5	1.02 (2)	C17—C18	1.393 (3)
C5—C6	1.392 (3)	C18—C20	1.499 (3)
C6—C8	1.498 (4)	C19—H19A	1.04 (3)
C7—H7A	1.04 (3)	C19—H19B	1.10 (3)
C7—H7B	1.01 (3)	C19—H19C	1.06 (3)
C7—H7C	1.11 (3)	C20—H20A	1.09 (3)
C8—H8A	0.90 (3)	C20—H20B	1.05 (3)
C8—H8B	1.09 (3)	C20—H20C	1.04 (3)
C8—H8C	1.10 (3)
N1—Sb—H1A	93.6 (8)	H9B—C9—Si1	111.8 (15)
N2—Sb—H1A	93.9 (9)	H9B—C9—H9A	108 (2)
N2—Sb—N1	98.56 (7)	H9C—C9—Si1	113.4 (16)
N1—Si1—O	106.14 (10)	H9C—C9—H9A	105 (2)
C9—Si1—O	107.44 (12)	H9C—C9—H9B	108 (2)
C9—Si1—N1	113.37 (12)	H10A—C10—Si1	109.9 (15)
C10—Si1—O	109.18 (11)	H10B—C10—Si1	113.3 (13)
C10—Si1—N1	111.61 (11)	H10B—C10—H10A	106 (2)
C10—Si1—C9	108.93 (14)	H10C—C10—Si1	116.6 (15)
N2—Si2—O	106.00 (10)	H10C—C10—H10A	108 (2)
C11—Si2—O	107.15 (11)	H10C—C10—H10B	102 (2)
C11—Si2—N2	113.00 (11)	H11A—C11—Si2	110.9 (15)
C12—Si2—O	109.28 (11)	H11B—C11—Si2	116.5 (15)
C12—Si2—N2	111.33 (12)	H11B—C11—H11A	105 (2)
C12—Si2—C11	109.86 (13)	H11C—C11—Si2	110.5 (16)
Si2—O—Si1	142.64 (11)	H11C—C11—H11A	107 (2)
Si1—N1—Sb	119.63 (11)	H11C—C11—H11B	107 (2)
C1—N1—Sb	117.02 (15)	H12A—C12—Si2	115.3 (16)
C1—N1—Si1	122.74 (16)	H12B—C12—Si2	113.9 (14)
Si2—N2—Sb	120.27 (11)	H12B—C12—H12A	106 (2)
C13—N2—Sb	116.30 (15)	H12C—C12—Si2	111.3 (16)
C13—N2—Si2	122.74 (16)	H12C—C12—H12A	100 (2)
C2—C1—N1	120.10 (19)	H12C—C12—H12B	109 (2)
C6—C1—N1	120.4 (2)	C14—C13—N2	120.3 (2)
C6—C1—C2	119.5 (2)	C18—C13—N2	120.2 (2)
C3—C2—C1	119.5 (2)	C18—C13—C14	119.5 (2)
C7—C2—C1	121.1 (2)	C15—C14—C13	119.7 (2)
C7—C2—C3	119.4 (2)	C19—C14—C13	121.2 (2)
H3—C3—C2	121.7 (15)	C19—C14—C15	119.1 (2)
C4—C3—C2	121.2 (2)	H15—C15—C14	119.3 (15)
C4—C3—H3	117.0 (15)	C16—C15—C14	121.1 (2)
H4—C4—C3	118.3 (14)	C16—C15—H15	119.6 (16)
C5—C4—C3	118.6 (2)	H16—C16—C15	120.0 (15)
C5—C4—H4	123.1 (14)	C17—C16—C15	119.2 (3)
H5—C5—C4	116.6 (17)	C17—C16—H16	120.8 (15)
C6—C5—C4	121.8 (2)	H17—C17—C16	122.3 (15)
C6—C5—H5	121.5 (17)	C18—C17—C16	121.3 (2)
C5—C6—C1	119.3 (2)	C18—C17—H17	116.4 (15)
C8—C6—C1	121.8 (2)	C17—C18—C13	119.3 (2)
C8—C6—C5	118.9 (2)	C20—C18—C13	122.0 (2)
H7A—C7—C2	114.8 (15)	C20—C18—C17	118.7 (2)
H7B—C7—C2	114.3 (14)	H19A—C19—C14	112.1 (14)
H7B—C7—H7A	108 (2)	H19B—C19—C14	108.9 (15)
H7C—C7—C2	115.2 (14)	H19B—C19—H19A	109 (2)
H7C—C7—H7A	101 (2)	H19C—C19—C14	110.4 (15)
H7C—C7—H7B	101 (2)	H19C—C19—H19A	108 (2)
H8A—C8—C6	113 (2)	H19C—C19—H19B	108 (2)
H8B—C8—C6	112.7 (14)	H20A—C20—C18	113.9 (15)
H8B—C8—H8A	103 (2)	H20B—C20—C18	114.6 (15)
H8C—C8—C6	114.7 (16)	H20B—C20—H20A	103 (2)
H8C—C8—H8A	105 (2)	H20C—C20—C18	111.5 (16)
H8C—C8—H8B	108 (2)	H20C—C20—H20A	105 (2)
H9A—C9—Si1	111.0 (15)	H20C—C20—H20B	107 (2)
Sb—N1—C1—C2	75.80 (17)	N2—C13—C14—C15	−178.3 (2)
Sb—N1—C1—C6	−103.78 (16)	N2—C13—C14—C19	1.8 (3)
Sb—N2—C13—C14	−75.75 (17)	N2—C13—C18—C17	177.2 (2)
Sb—N2—C13—C18	104.93 (17)	N2—C13—C18—C20	−5.5 (3)
Si1—O—Si2—N2	32.61 (19)	C1—C2—C3—C4	−0.3 (3)
Si1—O—Si2—C11	−88.3 (2)	C1—C6—C5—C4	−2.4 (3)
Si1—O—Si2—C12	152.70 (19)	C2—C3—C4—C5	1.1 (3)
Si1—N1—C1—C2	−95.12 (18)	C3—C4—C5—C6	0.3 (3)
Si1—N1—C1—C6	85.30 (19)	C4—C5—C6—C8	176.1 (3)
Si2—N2—C13—C14	94.79 (19)	C13—C14—C15—C16	−0.1 (3)
Si2—N2—C13—C18	−84.53 (19)	C13—C18—C17—C16	2.2 (3)
N1—C1—C2—C3	178.6 (2)	C14—C15—C16—C17	0.2 (3)
N1—C1—C2—C7	−2.0 (3)	C15—C16—C17—C18	−1.3 (3)
N1—C1—C6—C5	−177.3 (2)	C16—C17—C18—C20	−175.2 (3)
N1—C1—C6—C8	4.3 (3)

(TIWXOP_IAM_0_HADPs)

Crystal data

C20H31N2OSbSi2	Z = 2
Mr = 493.41	F(000) = 503.336
Triclinic, P1	Dx = 1.475 Mg m^−3
a = 7.6028 (5) Å	Mo Kα radiation, λ = 0.71073 Å
b = 11.5896 (8) Å	Cell parameters from 5427 reflections
c = 13.8020 (7) Å	θ = 3.8–29.0°
α = 99.459 (5)°	µ = 1.36 mm^−1
β = 100.012 (5)°	T = 120 K
γ = 107.557 (6)°	Block, colourless
V = 1110.98 (13) Å^3	0.17 × 0.11 × 0.07 mm

Data collection

SuperNova, Dual, Cu at zero, EosS2 diffractometer	4181 reflections with I ≥ 2u(I)
Detector resolution: 8.0856 pixels mm^-1	Rint = 0.030
ω scans	θmax = 26.4°, θmin = 3.4°
Absorption correction: gaussian CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	h = −9→9
Tmin = 0.744, Tmax = 1	k = −13→14
8520 measured reflections	l = −17→13
4543 independent reflections

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.033	Only H-atom coordinates refined
wR(F^2) = 0.071	w = 1/[σ^2(Fo^2) + (0.0213P)^2 + 1.0839P] where P = (Fo^2 + 2Fc^2)/3
S = 1.05	(Δ/σ)max = −0.001
4543 reflections	Δρmax = 0.99 e Å^−3
328 parameters	Δρmin = −0.64 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Sb	0.72530 (3)	0.536327 (19)	0.644330 (14)	0.01423 (7)
H	0.876 (4)	0.516 (3)	0.5669 (19)	0.000000
Si1	1.01942 (12)	0.42367 (8)	0.76618 (6)	0.01325 (18)
Si2	1.15153 (12)	0.70707 (8)	0.78233 (6)	0.01258 (17)
O	1.1412 (3)	0.5721 (2)	0.80478 (16)	0.0187 (5)
N1	0.7854 (3)	0.4132 (2)	0.72367 (17)	0.0128 (5)
N2	0.9187 (3)	0.6970 (2)	0.73816 (17)	0.0121 (5)
C1	0.6274 (4)	0.3099 (3)	0.7279 (2)	0.0121 (6)
C2	0.5381 (4)	0.2092 (3)	0.6437 (2)	0.0151 (6)
C3	0.3885 (5)	0.1091 (3)	0.6502 (2)	0.0190 (7)
H3	0.331 (4)	0.045 (3)	0.599 (2)	0.000000
C4	0.3257 (5)	0.1058 (3)	0.7382 (3)	0.0204 (7)
H4	0.229 (4)	0.032 (3)	0.7399 (19)	0.000000
C5	0.4127 (5)	0.2056 (3)	0.8202 (2)	0.0189 (7)
H5	0.373 (4)	0.204 (3)	0.878 (2)	0.000000
C6	0.5600 (4)	0.3087 (3)	0.8163 (2)	0.0153 (6)
C7	0.6024 (5)	0.2097 (4)	0.5466 (2)	0.0219 (7)
H7a	0.550 (4)	0.137 (3)	0.500 (2)	0.000000
H7b	0.729 (4)	0.227 (3)	0.554 (2)	0.000000
H7c	0.563 (4)	0.268 (3)	0.508 (2)	0.000000
C8	0.6393 (6)	0.4181 (4)	0.9057 (3)	0.0261 (8)
H8a	0.573 (4)	0.458 (3)	0.907 (2)	0.000000
H8b	0.753 (4)	0.473 (3)	0.903 (2)	0.000000
H8c	0.638 (4)	0.394 (3)	0.969 (2)	0.000000
C9	1.1191 (5)	0.3587 (4)	0.6662 (3)	0.0249 (8)
H9a	1.090 (4)	0.385 (3)	0.605 (2)	0.000000
H9b	1.067 (4)	0.271 (3)	0.647 (2)	0.000000
H9c	1.245 (4)	0.376 (3)	0.683 (2)	0.000000
C10	1.0474 (5)	0.3481 (3)	0.8722 (3)	0.0199 (7)
H10a	1.176 (4)	0.365 (3)	0.898 (2)	0.000000
H10b	0.990 (4)	0.251 (3)	0.8500 (19)	0.000000
H10c	0.995 (4)	0.370 (3)	0.919 (2)	0.000000
C11	1.2955 (5)	0.7344 (4)	0.6881 (3)	0.0214 (7)
H11a	1.412 (4)	0.724 (3)	0.710 (2)	0.000000
H11b	1.332 (4)	0.817 (3)	0.6765 (19)	0.000000
H11c	1.234 (4)	0.680 (3)	0.626 (2)	0.000000
C12	1.2668 (5)	0.8282 (3)	0.9003 (3)	0.0214 (7)
H12a	1.213 (4)	0.810 (3)	0.953 (2)	0.000000
H12b	1.266 (4)	0.908 (3)	0.897 (2)	0.000000
H12c	1.385 (4)	0.834 (3)	0.925 (2)	0.000000
C13	0.8573 (4)	0.8031 (3)	0.7510 (2)	0.0130 (6)
C14	0.8480 (4)	0.8684 (3)	0.6743 (2)	0.0150 (6)
C15	0.7940 (5)	0.9722 (3)	0.6895 (3)	0.0202 (7)
H15	0.788 (4)	1.014 (3)	0.641 (2)	0.000000
C16	0.7486 (5)	1.0128 (3)	0.7785 (3)	0.0237 (7)
H16	0.715 (4)	1.084 (3)	0.788 (2)	0.000000
C17	0.7580 (5)	0.9490 (3)	0.8536 (2)	0.0206 (7)
H17	0.737 (4)	0.977 (3)	0.916 (2)	0.000000
C18	0.8088 (4)	0.8427 (3)	0.8411 (2)	0.0164 (6)
C19	0.8966 (5)	0.8275 (4)	0.5761 (3)	0.0227 (7)
H19a	1.012 (4)	0.810 (3)	0.586 (2)	0.000000
H19b	0.913 (4)	0.894 (3)	0.539 (2)	0.000000
H19c	0.801 (4)	0.761 (3)	0.538 (2)	0.000000
C20	0.8015 (6)	0.7709 (4)	0.9224 (3)	0.0251 (8)
H20a	0.855 (4)	0.822 (3)	0.989 (2)	0.000000
H20b	0.864 (4)	0.716 (3)	0.917 (2)	0.000000
H20c	0.681 (4)	0.733 (3)	0.926 (2)	0.000000

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Sb	0.01409 (12)	0.01169 (12)	0.01500 (12)	0.00379 (8)	−0.00074 (8)	0.00345 (8)
H	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
Si1	0.0138 (4)	0.0115 (4)	0.0148 (4)	0.0052 (3)	0.0016 (3)	0.0040 (3)
Si2	0.0114 (4)	0.0101 (4)	0.0152 (4)	0.0026 (3)	0.0028 (3)	0.0025 (3)
O	0.0130 (11)	0.0118 (12)	0.0283 (12)	0.0019 (9)	−0.0005 (9)	0.0072 (9)
N1	0.0123 (13)	0.0123 (13)	0.0140 (12)	0.0043 (11)	0.0018 (10)	0.0048 (10)
N2	0.0108 (12)	0.0108 (13)	0.0150 (12)	0.0048 (10)	0.0015 (10)	0.0033 (10)
C1	0.0104 (14)	0.0107 (15)	0.0175 (15)	0.0054 (12)	0.0043 (12)	0.0051 (12)
C2	0.0133 (15)	0.0157 (17)	0.0170 (15)	0.0064 (13)	0.0017 (12)	0.0047 (12)
C3	0.0166 (16)	0.0130 (17)	0.0219 (16)	0.0037 (13)	−0.0026 (13)	−0.0003 (13)
H3	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C4	0.0136 (16)	0.0140 (17)	0.0333 (18)	0.0021 (14)	0.0051 (14)	0.0103 (14)
H4	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C5	0.0205 (17)	0.0229 (19)	0.0197 (16)	0.0114 (15)	0.0105 (14)	0.0088 (14)
H5	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C6	0.0156 (16)	0.0156 (17)	0.0170 (15)	0.0082 (13)	0.0044 (12)	0.0040 (12)
C7	0.0246 (19)	0.0213 (19)	0.0167 (16)	0.0055 (16)	0.0053 (14)	−0.0002 (14)
H7a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H7b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H7c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C8	0.031 (2)	0.023 (2)	0.0247 (19)	0.0083 (17)	0.0136 (16)	0.0006 (16)
H8a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H8b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H8c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C9	0.0212 (19)	0.033 (2)	0.0266 (19)	0.0170 (17)	0.0072 (15)	0.0055 (16)
H9a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H9b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H9c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C10	0.0180 (18)	0.0171 (18)	0.0220 (17)	0.0041 (14)	−0.0005 (14)	0.0062 (14)
H10a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H10b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H10c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C11	0.0194 (18)	0.024 (2)	0.0220 (18)	0.0065 (15)	0.0073 (15)	0.0069 (15)
H11a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H11b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H11c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C12	0.0208 (18)	0.0174 (19)	0.0209 (17)	0.0035 (15)	0.0012 (15)	0.0007 (14)
H12a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H12b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H12c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C13	0.0086 (14)	0.0096 (15)	0.0190 (15)	0.0014 (12)	0.0025 (12)	0.0023 (12)
C14	0.0100 (15)	0.0125 (16)	0.0201 (15)	0.0014 (12)	0.0013 (12)	0.0038 (12)
C15	0.0188 (17)	0.0149 (17)	0.0263 (17)	0.0045 (14)	0.0007 (14)	0.0100 (14)
H15	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C16	0.0163 (17)	0.0113 (17)	0.039 (2)	0.0057 (14)	−0.0015 (15)	−0.0007 (15)
H16	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C17	0.0170 (17)	0.0198 (18)	0.0217 (17)	0.0064 (14)	0.0040 (14)	−0.0032 (14)
H17	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C18	0.0137 (15)	0.0159 (17)	0.0164 (15)	0.0021 (13)	0.0034 (12)	0.0007 (12)
C19	0.027 (2)	0.024 (2)	0.0203 (17)	0.0092 (16)	0.0055 (15)	0.0104 (15)
H19a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H19b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H19c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C20	0.030 (2)	0.032 (2)	0.0229 (18)	0.0158 (18)	0.0139 (16)	0.0112 (16)
H20a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H20b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H20c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000

Geometric parameters (Å, º)

Sb—H	1.74 (3)	C9—H9a	0.95 (3)
Sb—N1	2.044 (2)	C9—H9b	0.94 (3)
Sb—N2	2.049 (2)	C9—H9c	0.90 (3)
Si1—O	1.633 (2)	C10—H10a	0.92 (3)
Si1—N1	1.734 (3)	C10—H10b	1.05 (3)
Si1—C9	1.848 (3)	C10—H10c	0.85 (3)
Si1—C10	1.838 (3)	C11—H11a	0.94 (3)
Si2—O	1.625 (2)	C11—H11b	0.96 (3)
Si2—N2	1.730 (2)	C11—H11c	0.93 (3)
Si2—C11	1.847 (3)	C12—H12a	0.91 (3)
Si2—C12	1.844 (3)	C12—H12b	0.93 (3)
N1—C1	1.435 (4)	C12—H12c	0.88 (3)
N2—C13	1.437 (4)	C13—C14	1.402 (4)
C1—C2	1.406 (4)	C13—C18	1.403 (4)
C1—C6	1.404 (4)	C14—C15	1.381 (4)
C2—C3	1.386 (4)	C14—C19	1.505 (4)
C2—C7	1.504 (4)	C15—H15	0.90 (3)
C3—H3	0.88 (3)	C15—C16	1.380 (5)
C3—C4	1.382 (5)	C16—H16	0.93 (3)
C4—H4	0.95 (3)	C16—C17	1.374 (5)
C4—C5	1.380 (5)	C17—H17	0.92 (3)
C5—H5	0.90 (3)	C17—C18	1.391 (4)
C5—C6	1.386 (4)	C18—C20	1.502 (5)
C6—C8	1.503 (5)	C19—H19a	0.95 (3)
C7—H7a	0.90 (3)	C19—H19b	0.98 (3)
C7—H7b	0.91 (3)	C19—H19c	0.89 (3)
C7—H7c	1.00 (3)	C20—H20a	0.95 (3)
C8—H8a	0.78 (3)	C20—H20b	0.90 (3)
C8—H8b	0.91 (3)	C20—H20c	0.90 (3)
C8—H8c	0.96 (3)
N1—Sb—H	92.1 (9)	H9b—C9—Si1	111.6 (17)
N2—Sb—H	94.6 (9)	H9b—C9—H9a	105 (2)
N2—Sb—N1	98.29 (10)	H9c—C9—Si1	115.0 (18)
N1—Si1—O	105.88 (12)	H9c—C9—H9a	108 (2)
C9—Si1—O	107.43 (16)	H9c—C9—H9b	105 (2)
C9—Si1—N1	113.42 (15)	H10a—C10—Si1	108.4 (17)
C10—Si1—O	109.23 (14)	H10b—C10—Si1	113.0 (14)
C10—Si1—N1	111.62 (14)	H10b—C10—H10a	105 (2)
C10—Si1—C9	109.07 (17)	H10c—C10—Si1	113.3 (19)
N2—Si2—O	105.85 (12)	H10c—C10—H10a	111 (3)
C11—Si2—O	107.21 (15)	H10c—C10—H10b	106 (2)
C11—Si2—N2	113.03 (14)	H11a—C11—Si2	110.1 (16)
C12—Si2—O	109.33 (15)	H11b—C11—Si2	116.1 (16)
C12—Si2—N2	111.34 (15)	H11b—C11—H11a	103 (2)
C12—Si2—C11	109.87 (17)	H11c—C11—Si2	111.5 (17)
Si2—O—Si1	142.79 (14)	H11c—C11—H11a	109 (2)
Si1—N1—Sb	119.81 (13)	H11c—C11—H11b	107 (2)
C1—N1—Sb	116.83 (18)	H12a—C12—Si2	112.8 (18)
C1—N1—Si1	122.7 (2)	H12b—C12—Si2	115.6 (17)
Si2—N2—Sb	120.49 (13)	H12b—C12—H12a	106 (2)
C13—N2—Sb	116.04 (18)	H12c—C12—Si2	112.8 (18)
C13—N2—Si2	122.8 (2)	H12c—C12—H12a	101 (2)
C2—C1—N1	120.5 (2)	H12c—C12—H12b	108 (3)
C6—C1—N1	120.2 (3)	C14—C13—N2	120.3 (3)
C6—C1—C2	119.3 (3)	C18—C13—N2	119.9 (3)
C3—C2—C1	119.6 (3)	C18—C13—C14	119.7 (3)
C7—C2—C1	120.6 (3)	C15—C14—C13	119.3 (3)
C7—C2—C3	119.9 (3)	C19—C14—C13	121.2 (3)
H3—C3—C2	121.5 (18)	C19—C14—C15	119.5 (3)
C4—C3—C2	121.3 (3)	H15—C15—C14	119.8 (18)
C4—C3—H3	117.2 (18)	C16—C15—C14	121.3 (3)
H4—C4—C3	117.6 (16)	C16—C15—H15	118.9 (18)
C5—C4—C3	118.9 (3)	H16—C16—C15	120.0 (17)
C5—C4—H4	123.4 (16)	C17—C16—C15	119.4 (3)
H5—C5—C4	119.2 (18)	C17—C16—H16	120.6 (17)
C6—C5—C4	121.7 (3)	H17—C17—C16	121.7 (18)
C6—C5—H5	119.1 (18)	C18—C17—C16	121.3 (3)
C5—C6—C1	119.2 (3)	C18—C17—H17	116.9 (18)
C8—C6—C1	121.7 (3)	C17—C18—C13	118.9 (3)
C8—C6—C5	119.1 (3)	C20—C18—C13	122.1 (3)
H7a—C7—C2	114.5 (18)	C20—C18—C17	118.9 (3)
H7b—C7—C2	114.9 (17)	H19a—C19—C14	112.5 (16)
H7b—C7—H7a	104 (2)	H19b—C19—C14	109.5 (16)
H7c—C7—C2	113.1 (15)	H19b—C19—H19a	107 (2)
H7c—C7—H7a	101 (2)	H19c—C19—C14	109.3 (18)
H7c—C7—H7b	108 (2)	H19c—C19—H19a	110 (3)
H8a—C8—C6	111 (2)	H19c—C19—H19b	108 (2)
H8b—C8—C6	112.7 (17)	H20a—C20—C18	113.5 (17)
H8b—C8—H8a	104 (3)	H20b—C20—C18	113.5 (18)
H8c—C8—C6	112.5 (17)	H20b—C20—H20a	106 (2)
H8c—C8—H8a	101 (3)	H20c—C20—C18	111.7 (18)
H8c—C8—H8b	115 (2)	H20c—C20—H20a	101 (2)
H9a—C9—Si1	112.2 (16)	H20c—C20—H20b	111 (3)
Sb—N1—C1—C2	75.6 (2)	N2—C13—C14—C15	−178.1 (3)
Sb—N1—C1—C6	−104.2 (2)	N2—C13—C14—C19	1.6 (3)
Sb—N2—C13—C14	−75.7 (2)	N2—C13—C18—C17	177.1 (3)
Sb—N2—C13—C18	105.1 (2)	N2—C13—C18—C20	−5.7 (4)
Si1—O—Si2—N2	32.7 (3)	C1—C2—C3—C4	−0.4 (4)
Si1—O—Si2—C11	−88.2 (3)	C1—C6—C5—C4	−2.4 (4)
Si1—O—Si2—C12	152.7 (2)	C2—C3—C4—C5	1.0 (4)
Si1—N1—C1—C2	−94.8 (2)	C3—C4—C5—C6	0.4 (4)
Si1—N1—C1—C6	85.4 (2)	C4—C5—C6—C8	175.7 (3)
Si2—N2—C13—C14	94.7 (2)	C13—C14—C15—C16	−0.2 (3)
Si2—N2—C13—C18	−84.5 (2)	C13—C18—C17—C16	2.1 (4)
N1—C1—C2—C3	178.5 (3)	C14—C15—C16—C17	0.2 (4)
N1—C1—C2—C7	−2.0 (3)	C15—C16—C17—C18	−1.2 (4)
N1—C1—C6—C5	−177.2 (3)	C16—C17—C18—C20	−175.1 (3)
N1—C1—C6—C8	4.8 (4)

(TIWXOP_IAM_NoMoRe)

Crystal data

C20H31N2OSbSi2	Z = 2
Mr = 493.41	F(000) = 503.308
Triclinic, P1	Dx = 1.475 Mg m^−3
a = 7.6028 (5) Å	Mo Kα radiation, λ = 0.71073 Å
b = 11.5896 (8) Å	Cell parameters from 5427 reflections
c = 13.8020 (7) Å	θ = 3.8–29.0°
α = 99.459 (5)°	µ = 1.36 mm^−1
β = 100.012 (5)°	T = 120 K
γ = 107.557 (6)°	Block, colourless
V = 1110.98 (13) Å^3	0.17 × 0.11 × 0.07 mm

Data collection

SuperNova, Dual, Cu at zero, EosS2 diffractometer	4181 reflections with I ≥ 2u(I)
ω scans	Rint = 0.030
Absorption correction: gaussian CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	θmax = 26.4°, θmin = 3.4°
Tmin = 0.744, Tmax = 1	h = −9→9
8520 measured reflections	k = −13→14
4543 independent reflections	l = −17→13

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.031	Only H-atom coordinates refined
wR(F^2) = 0.064	w = 1/[σ^2(Fo^2) + (0.0168P)^2 + 0.5884P] where P = (Fo^2 + 2Fc^2)/3
S = 1.06	(Δ/σ)max = 0.001
4543 reflections	Δρmax = 1.05 e Å^−3
328 parameters	Δρmin = −0.58 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Sb	0.72530 (3)	0.536326 (18)	0.644334 (13)	0.01443 (7)
H1A	0.877 (5)	0.516 (3)	0.567 (2)	0.037997
Si1	1.01946 (11)	0.42367 (7)	0.76617 (6)	0.01339 (17)
Si2	1.15147 (11)	0.70705 (7)	0.78231 (5)	0.01274 (17)
O	1.1412 (3)	0.57212 (19)	0.80475 (14)	0.0187 (4)
N1	0.7853 (3)	0.4131 (2)	0.72364 (16)	0.0126 (5)
N2	0.9187 (3)	0.6969 (2)	0.73814 (16)	0.0121 (5)
C1	0.6275 (4)	0.3101 (3)	0.7279 (2)	0.0123 (6)
C2	0.5381 (4)	0.2092 (3)	0.6437 (2)	0.0151 (6)
C3	0.3885 (4)	0.1090 (3)	0.6499 (2)	0.0191 (6)
H3	0.329 (5)	0.042 (3)	0.597 (3)	0.037734
C4	0.3253 (4)	0.1056 (3)	0.7381 (2)	0.0205 (7)
H4	0.224 (5)	0.030 (3)	0.739 (2)	0.038626
C5	0.4127 (4)	0.2057 (3)	0.8203 (2)	0.0192 (6)
H5	0.370 (5)	0.203 (3)	0.880 (2)	0.039518
C6	0.5599 (4)	0.3088 (3)	0.8164 (2)	0.0155 (6)
C7	0.6027 (5)	0.2097 (3)	0.5464 (2)	0.0225 (7)
H7A	0.545 (5)	0.136 (4)	0.497 (3)	0.043455
H7B	0.730 (6)	0.229 (4)	0.554 (3)	0.054475
H7C	0.570 (6)	0.269 (4)	0.510 (3)	0.047101
C8	0.6386 (5)	0.4182 (3)	0.9055 (3)	0.0269 (8)
H8A	0.575 (6)	0.467 (4)	0.905 (3)	0.052008
H8B	0.755 (6)	0.469 (4)	0.906 (3)	0.051200
H8C	0.642 (6)	0.395 (4)	0.970 (3)	0.061390
C9	1.1193 (5)	0.3584 (4)	0.6661 (3)	0.0258 (7)
H9A	1.093 (5)	0.388 (3)	0.606 (3)	0.037502
H9B	1.062 (5)	0.270 (4)	0.646 (3)	0.037250
H9C	1.252 (5)	0.377 (3)	0.683 (2)	0.033381
C10	1.0475 (5)	0.3482 (3)	0.8723 (2)	0.0207 (7)
H10A	1.171 (6)	0.365 (4)	0.899 (3)	0.044394
H10B	0.986 (6)	0.252 (4)	0.849 (3)	0.045088
H10C	0.991 (6)	0.368 (4)	0.920 (3)	0.047517
C11	1.2955 (5)	0.7346 (3)	0.6879 (2)	0.0221 (7)
H11A	1.412 (5)	0.724 (3)	0.709 (3)	0.035851
H11B	1.334 (5)	0.816 (4)	0.677 (3)	0.044987
H11C	1.228 (5)	0.679 (4)	0.625 (3)	0.040339
C12	1.2673 (5)	0.8287 (3)	0.9005 (2)	0.0217 (7)
H12A	1.215 (6)	0.813 (5)	0.951 (3)	0.070958
H12B	1.269 (8)	0.910 (4)	0.894 (3)	0.106478
H12C	1.386 (6)	0.832 (5)	0.925 (3)	0.074107
C13	0.8574 (4)	0.8031 (3)	0.7509 (2)	0.0134 (6)
C14	0.8480 (4)	0.8684 (3)	0.6744 (2)	0.0151 (6)
C15	0.7936 (4)	0.9722 (3)	0.6893 (2)	0.0204 (7)
H15	0.787 (5)	1.016 (3)	0.639 (2)	0.038001
C16	0.7486 (4)	1.0132 (3)	0.7784 (2)	0.0234 (7)
H16	0.715 (5)	1.087 (3)	0.789 (3)	0.041447
C17	0.7580 (4)	0.9489 (3)	0.8538 (2)	0.0208 (7)
H17	0.736 (5)	0.977 (3)	0.918 (3)	0.040548
C18	0.8088 (4)	0.8427 (3)	0.8411 (2)	0.0163 (6)
C19	0.8966 (5)	0.8272 (3)	0.5759 (2)	0.0232 (7)
H19A	1.010 (6)	0.808 (3)	0.587 (2)	0.037725
H19B	0.909 (5)	0.892 (4)	0.540 (2)	0.039059
H19C	0.799 (5)	0.759 (4)	0.536 (2)	0.034912
C20	0.8011 (5)	0.7709 (4)	0.9226 (2)	0.0256 (7)
H20A	0.863 (6)	0.825 (4)	0.990 (3)	0.055198
H20B	0.861 (6)	0.713 (4)	0.917 (3)	0.044647
H20C	0.681 (6)	0.732 (4)	0.927 (3)	0.049514

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Sb	0.01430 (11)	0.01187 (11)	0.01519 (11)	0.00385 (8)	−0.00069 (8)	0.00350 (7)
H1A	0.050000	0.035000	0.033000	0.016000	0.020000	0.005000
Si1	0.0139 (4)	0.0117 (4)	0.0149 (4)	0.0053 (3)	0.0018 (3)	0.0040 (3)
Si2	0.0116 (4)	0.0103 (4)	0.0153 (4)	0.0027 (3)	0.0028 (3)	0.0026 (3)
O	0.0128 (10)	0.0121 (11)	0.0283 (11)	0.0019 (9)	−0.0007 (9)	0.0074 (9)
N1	0.0122 (12)	0.0124 (13)	0.0139 (11)	0.0044 (10)	0.0020 (9)	0.0051 (9)
N2	0.0109 (12)	0.0108 (13)	0.0148 (11)	0.0049 (10)	0.0014 (9)	0.0031 (9)
C1	0.0105 (14)	0.0103 (15)	0.0181 (14)	0.0051 (11)	0.0041 (11)	0.0052 (11)
C2	0.0133 (14)	0.0160 (16)	0.0168 (14)	0.0068 (12)	0.0017 (11)	0.0047 (12)
C3	0.0159 (15)	0.0135 (16)	0.0232 (15)	0.0039 (13)	−0.0023 (12)	0.0013 (13)
H3	0.027000	0.032000	0.039000	−0.002000	0.004000	−0.006000
C4	0.0135 (15)	0.0157 (17)	0.0328 (17)	0.0034 (13)	0.0048 (13)	0.0103 (14)
H4	0.027000	0.039000	0.048000	0.003000	0.017000	0.012000
C5	0.0203 (16)	0.0222 (18)	0.0213 (15)	0.0115 (14)	0.0100 (13)	0.0088 (13)
H5	0.043000	0.046000	0.033000	0.015000	0.021000	0.006000
C6	0.0154 (15)	0.0157 (16)	0.0173 (14)	0.0080 (12)	0.0043 (12)	0.0037 (12)
C7	0.0271 (18)	0.0219 (18)	0.0161 (15)	0.0060 (15)	0.0062 (14)	0.0013 (13)
H7A	0.035000	0.044000	0.032000	−0.001000	0.004000	−0.012000
H7B	0.049000	0.088000	0.040000	0.047000	0.011000	0.006000
H7C	0.063000	0.035000	0.040000	0.004000	0.029000	0.006000
C8	0.032 (2)	0.023 (2)	0.0233 (16)	0.0068 (16)	0.0113 (16)	−0.0011 (15)
H8A	0.073000	0.026000	0.042000	0.004000	0.001000	0.005000
H8B	0.044000	0.043000	0.051000	0.015000	−0.013000	−0.006000
H8C	0.057000	0.057000	0.055000	0.008000	0.027000	−0.021000
C9	0.0232 (18)	0.034 (2)	0.0269 (17)	0.0180 (16)	0.0084 (15)	0.0057 (15)
H9A	0.049000	0.041000	0.027000	0.019000	0.009000	0.013000
H9B	0.041000	0.023000	0.043000	0.007000	0.012000	0.000000
H9C	0.027000	0.039000	0.037000	0.016000	0.008000	0.007000
C10	0.0186 (16)	0.0174 (17)	0.0228 (16)	0.0039 (14)	−0.0019 (13)	0.0071 (13)
H10A	0.037000	0.052000	0.043000	0.013000	−0.002000	0.024000
H10B	0.056000	0.022000	0.051000	0.004000	0.009000	0.013000
H10C	0.063000	0.056000	0.049000	0.036000	0.035000	0.028000
C11	0.0195 (17)	0.0252 (19)	0.0230 (16)	0.0072 (15)	0.0079 (14)	0.0075 (14)
H11A	0.033000	0.041000	0.042000	0.020000	0.013000	0.014000
H11B	0.047000	0.039000	0.058000	0.011000	0.029000	0.025000
H11C	0.039000	0.053000	0.027000	0.015000	0.005000	0.008000
C12	0.0221 (17)	0.0181 (17)	0.0195 (16)	0.0032 (14)	0.0020 (13)	0.0000 (13)
H12A	0.048000	0.096000	0.040000	0.003000	0.008000	−0.019000
H12B	0.140000	0.030000	0.087000	−0.022000	−0.052000	0.025000
H12C	0.033000	0.099000	0.071000	0.030000	−0.015000	−0.018000
C13	0.0092 (13)	0.0093 (14)	0.0199 (14)	0.0015 (11)	0.0027 (11)	0.0023 (11)
C14	0.0108 (14)	0.0127 (15)	0.0196 (14)	0.0018 (12)	0.0013 (11)	0.0038 (12)
C15	0.0179 (16)	0.0143 (16)	0.0275 (16)	0.0043 (13)	0.0004 (13)	0.0084 (13)
H15	0.048000	0.029000	0.040000	0.014000	0.007000	0.018000
C16	0.0160 (16)	0.0116 (16)	0.0377 (18)	0.0047 (13)	−0.0015 (14)	0.0002 (14)
H16	0.050000	0.021000	0.050000	0.015000	0.003000	0.003000
C17	0.0162 (16)	0.0187 (17)	0.0235 (16)	0.0055 (13)	0.0033 (13)	−0.0033 (13)
H17	0.053000	0.032000	0.032000	0.015000	0.008000	−0.004000
C18	0.0141 (15)	0.0153 (16)	0.0164 (14)	0.0023 (12)	0.0030 (12)	0.0011 (12)
C19	0.0297 (19)	0.0242 (19)	0.0197 (16)	0.0115 (16)	0.0069 (14)	0.0106 (14)
H19A	0.049000	0.040000	0.037000	0.028000	0.016000	0.013000
H19B	0.049000	0.037000	0.038000	0.013000	0.019000	0.021000
H19C	0.034000	0.036000	0.028000	0.006000	0.003000	0.005000
C20	0.031 (2)	0.031 (2)	0.0228 (16)	0.0151 (17)	0.0135 (15)	0.0124 (15)
H20A	0.061000	0.050000	0.030000	−0.006000	−0.010000	0.012000
H20B	0.066000	0.030000	0.049000	0.021000	0.027000	0.016000
H20C	0.050000	0.063000	0.050000	0.025000	0.029000	0.023000

Geometric parameters (Å, º)

Sb—H1A	1.74 (3)	C9—H9A	0.96 (3)
Sb—N1	2.044 (2)	C9—H9B	0.96 (4)
Sb—N2	2.049 (2)	C9—H9C	0.94 (4)
Si1—O	1.633 (2)	C10—H10A	0.90 (4)
Si1—N1	1.735 (2)	C10—H10B	1.04 (4)
Si1—C9	1.850 (3)	C10—H10C	0.89 (4)
Si1—C10	1.839 (3)	C11—H11A	0.94 (4)
Si2—O	1.625 (2)	C11—H11B	0.94 (4)
Si2—N2	1.730 (2)	C11—H11C	0.95 (4)
Si2—C11	1.849 (3)	C12—H12A	0.88 (4)
Si2—C12	1.849 (3)	C12—H12B	0.95 (5)
N1—C1	1.433 (3)	C12—H12C	0.90 (4)
N2—C13	1.438 (3)	C13—C14	1.401 (4)
C1—C2	1.406 (4)	C13—C18	1.403 (4)
C1—C6	1.406 (4)	C14—C15	1.382 (4)
C2—C3	1.385 (4)	C14—C19	1.510 (4)
C2—C7	1.509 (4)	C15—H15	0.93 (3)
C3—H3	0.91 (3)	C15—C16	1.381 (4)
C3—C4	1.386 (4)	C16—H16	0.95 (4)
C4—H4	0.98 (4)	C16—C17	1.379 (4)
C4—C5	1.383 (4)	C17—H17	0.95 (3)
C5—H5	0.94 (3)	C17—C18	1.390 (4)
C5—C6	1.385 (4)	C18—C20	1.505 (4)
C6—C8	1.501 (4)	C19—H19A	0.95 (4)
C7—H7A	0.93 (4)	C19—H19B	0.96 (4)
C7—H7B	0.91 (4)	C19—H19C	0.91 (4)
C7—H7C	0.99 (4)	C20—H20A	0.98 (4)
C8—H8A	0.85 (4)	C20—H20B	0.92 (4)
C8—H8B	0.90 (4)	C20—H20C	0.91 (4)
C8—H8C	0.97 (4)
N1—Sb—H1A	91.9 (11)	H9B—C9—Si1	111 (2)
N2—Sb—H1A	94.5 (12)	H9B—C9—H9A	105 (3)
N2—Sb—N1	98.30 (9)	H9C—C9—Si1	116 (2)
N1—Si1—O	105.91 (11)	H9C—C9—H9A	106 (3)
C9—Si1—O	107.49 (15)	H9C—C9—H9B	107 (3)
C9—Si1—N1	113.45 (14)	H10A—C10—Si1	109 (2)
C10—Si1—O	109.19 (13)	H10B—C10—Si1	111.6 (19)
C10—Si1—N1	111.61 (13)	H10B—C10—H10A	107 (3)
C10—Si1—C9	109.01 (16)	H10C—C10—Si1	114 (2)
N2—Si2—O	105.86 (11)	H10C—C10—H10A	110 (3)
C11—Si2—O	107.27 (14)	H10C—C10—H10B	104 (3)
C11—Si2—N2	112.99 (13)	H11A—C11—Si2	111 (2)
C12—Si2—O	109.39 (13)	H11B—C11—Si2	117 (2)
C12—Si2—N2	111.39 (14)	H11B—C11—H11A	102 (3)
C12—Si2—C11	109.75 (16)	H11C—C11—Si2	109 (2)
Si2—O—Si1	142.78 (13)	H11C—C11—H11A	110 (3)
Si1—N1—Sb	119.77 (12)	H11C—C11—H11B	108 (3)
C1—N1—Sb	116.85 (17)	H12A—C12—Si2	113 (3)
C1—N1—Si1	122.70 (18)	H12B—C12—Si2	114 (3)
Si2—N2—Sb	120.51 (12)	H12B—C12—H12A	107 (4)
C13—N2—Sb	116.03 (17)	H12C—C12—Si2	112 (3)
C13—N2—Si2	122.75 (19)	H12C—C12—H12A	101 (4)
C2—C1—N1	120.6 (2)	H12C—C12—H12B	109 (4)
C6—C1—N1	120.2 (2)	C14—C13—N2	120.4 (2)
C6—C1—C2	119.2 (3)	C18—C13—N2	119.9 (2)
C3—C2—C1	119.8 (2)	C18—C13—C14	119.7 (3)
C7—C2—C1	120.5 (3)	C15—C14—C13	119.5 (3)
C7—C2—C3	119.7 (3)	C19—C14—C13	121.1 (3)
H3—C3—C2	122 (2)	C19—C14—C15	119.5 (3)
C4—C3—C2	121.2 (3)	H15—C15—C14	120 (2)
C4—C3—H3	117 (2)	C16—C15—C14	121.3 (3)
H4—C4—C3	117 (2)	C16—C15—H15	118 (2)
C5—C4—C3	118.7 (3)	H16—C16—C15	121 (2)
C5—C4—H4	124 (2)	C17—C16—C15	119.2 (3)
H5—C5—C4	119 (2)	C17—C16—H16	120 (2)
C6—C5—C4	121.9 (3)	H17—C17—C16	122 (2)
C6—C5—H5	119 (2)	C18—C17—C16	121.3 (3)
C5—C6—C1	119.2 (3)	C18—C17—H17	117 (2)
C8—C6—C1	121.7 (3)	C17—C18—C13	119.0 (3)
C8—C6—C5	119.1 (3)	C20—C18—C13	122.2 (3)
H7A—C7—C2	114 (2)	C20—C18—C17	118.8 (3)
H7B—C7—C2	114 (2)	H19A—C19—C14	112 (2)
H7B—C7—H7A	107 (3)	H19B—C19—C14	109 (2)
H7C—C7—C2	114 (2)	H19B—C19—H19A	110 (3)
H7C—C7—H7A	101 (3)	H19C—C19—C14	110 (2)
H7C—C7—H7B	105 (3)	H19C—C19—H19A	110 (3)
H8A—C8—C6	113 (3)	H19C—C19—H19B	107 (3)
H8B—C8—C6	113 (2)	H20A—C20—C18	112 (2)
H8B—C8—H8A	102 (4)	H20B—C20—C18	114 (2)
H8C—C8—C6	114 (2)	H20B—C20—H20A	105 (3)
H8C—C8—H8A	106 (3)	H20C—C20—C18	113 (2)
H8C—C8—H8B	109 (3)	H20C—C20—H20A	104 (3)
H9A—C9—Si1	111 (2)	H20C—C20—H20B	108 (4)
Sb—N1—C1—C2	75.7 (2)	N2—C13—C14—C15	−178.2 (3)
Sb—N1—C1—C6	−104.11 (19)	N2—C13—C14—C19	1.7 (3)
Sb—N2—C13—C14	−75.7 (2)	N2—C13—C18—C17	177.1 (3)
Sb—N2—C13—C18	105.12 (19)	N2—C13—C18—C20	−5.7 (3)
Si1—O—Si2—N2	32.6 (2)	C1—C2—C3—C4	−0.4 (3)
Si1—O—Si2—C11	−88.3 (2)	C1—C6—C5—C4	−2.4 (3)
Si1—O—Si2—C12	152.8 (2)	C2—C3—C4—C5	1.1 (4)
Si1—N1—C1—C2	−94.8 (2)	C3—C4—C5—C6	0.4 (3)
Si1—N1—C1—C6	85.4 (2)	C4—C5—C6—C8	175.5 (3)
Si2—N2—C13—C14	94.6 (2)	C13—C14—C15—C16	0.1 (3)
Si2—N2—C13—C18	−84.5 (2)	C13—C18—C17—C16	2.1 (3)
N1—C1—C2—C3	178.5 (3)	C14—C15—C16—C17	−0.1 (4)
N1—C1—C2—C7	−2.0 (3)	C15—C16—C17—C18	−1.1 (4)
N1—C1—C6—C5	−177.2 (3)	C16—C17—C18—C20	−175.1 (3)
N1—C1—C6—C8	5.0 (3)

(TIWXOP_IAM_SHADE3)

Crystal data

C20H31N2OSbSi2	Z = 2
Mr = 493.41	F(000) = 503.265
Triclinic, P1	Dx = 1.475 Mg m^−3
a = 7.6028 (5) Å	Mo Kα radiation, λ = 0.71073 Å
b = 11.5896 (8) Å	Cell parameters from 5427 reflections
c = 13.8020 (7) Å	θ = 3.8–29.0°
α = 99.459 (5)°	µ = 1.36 mm^−1
β = 100.012 (5)°	T = 120 K
γ = 107.557 (6)°	Block, colourless
V = 1110.98 (13) Å^3	0.17 × 0.11 × 0.07 mm

Data collection

SuperNova, Dual, Cu at zero, EosS2 diffractometer	4181 reflections with I ≥ 2u(I)
Detector resolution: 8.0856 pixels mm^-1	Rint = 0.030
ω scans	θmax = 26.4°, θmin = 3.4°
Absorption correction: gaussian CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	h = −9→9
Tmin = 0.744, Tmax = 1	k = −13→14
8520 measured reflections	l = −17→13
4543 independent reflections

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.031	Only H-atom coordinates refined
wR(F^2) = 0.066	w = 1/[σ^2(Fo^2) + (0.0163P)^2 + 1.0071P] where P = (Fo^2 + 2Fc^2)/3
S = 1.04	(Δ/σ)max = 0.001
4543 reflections	Δρmax = 1.02 e Å^−3
328 parameters	Δρmin = −0.61 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Sb	0.72530 (3)	0.536323 (18)	0.644331 (14)	0.01488 (7)
H1A	0.876 (5)	0.515 (3)	0.567 (2)	0.035086
Si1	1.01944 (11)	0.42367 (8)	0.76616 (6)	0.01272 (17)
Si2	1.15149 (11)	0.70706 (8)	0.78232 (6)	0.01206 (17)
O	1.1412 (3)	0.57210 (19)	0.80470 (15)	0.0180 (5)
N1	0.7853 (3)	0.4132 (2)	0.72364 (16)	0.0120 (5)
N2	0.9187 (3)	0.6969 (2)	0.73815 (17)	0.0115 (5)
C1	0.6275 (4)	0.3100 (3)	0.7279 (2)	0.0116 (6)
C2	0.5380 (4)	0.2092 (3)	0.6437 (2)	0.0144 (6)
C3	0.3886 (4)	0.1091 (3)	0.6500 (2)	0.0185 (7)
H3	0.330 (5)	0.045 (4)	0.599 (3)	0.032574
C4	0.3254 (4)	0.1057 (3)	0.7382 (2)	0.0199 (7)
H4	0.226 (5)	0.031 (4)	0.739 (3)	0.034860
C5	0.4128 (4)	0.2057 (3)	0.8202 (2)	0.0186 (7)
H5	0.373 (5)	0.203 (3)	0.878 (3)	0.036529
C6	0.5600 (4)	0.3088 (3)	0.8164 (2)	0.0148 (6)
C7	0.6024 (5)	0.2097 (3)	0.5463 (2)	0.0217 (7)
H7A	0.546 (5)	0.136 (4)	0.499 (3)	0.035548
H7B	0.725 (6)	0.228 (4)	0.554 (3)	0.031252
H7C	0.569 (5)	0.270 (4)	0.509 (3)	0.033604
C8	0.6388 (6)	0.4182 (4)	0.9056 (3)	0.0258 (8)
H8A	0.578 (6)	0.463 (4)	0.907 (3)	0.034871
H8B	0.751 (6)	0.469 (4)	0.905 (3)	0.031311
H8C	0.644 (5)	0.395 (4)	0.970 (3)	0.036431
C9	1.1194 (5)	0.3585 (4)	0.6661 (3)	0.0250 (8)
H9A	1.094 (6)	0.387 (4)	0.606 (3)	0.036751
H9B	1.065 (5)	0.272 (4)	0.647 (3)	0.036219
H9C	1.252 (6)	0.377 (4)	0.683 (3)	0.037410
C10	1.0477 (5)	0.3481 (3)	0.8723 (2)	0.0199 (7)
H10A	1.174 (6)	0.366 (4)	0.899 (3)	0.039642
H10B	0.988 (6)	0.255 (4)	0.850 (3)	0.037140
H10C	0.995 (5)	0.370 (4)	0.919 (3)	0.033209
C11	1.2955 (5)	0.7346 (4)	0.6879 (2)	0.0214 (7)
H11A	1.411 (6)	0.723 (4)	0.708 (3)	0.036618
H11B	1.332 (5)	0.815 (4)	0.677 (3)	0.036146
H11C	1.230 (5)	0.679 (4)	0.625 (3)	0.036006
C12	1.2672 (5)	0.8284 (3)	0.9005 (2)	0.0211 (7)
H12A	1.216 (5)	0.811 (3)	0.952 (3)	0.031486
H12B	1.265 (5)	0.904 (4)	0.895 (3)	0.026163
H12C	1.387 (5)	0.833 (3)	0.925 (3)	0.031279
C13	0.8574 (4)	0.8031 (3)	0.7509 (2)	0.0127 (6)
C14	0.8480 (4)	0.8683 (3)	0.6744 (2)	0.0145 (6)
C15	0.7937 (4)	0.9722 (3)	0.6894 (2)	0.0198 (7)
H15	0.787 (5)	1.015 (3)	0.640 (3)	0.035667
C16	0.7486 (5)	1.0130 (3)	0.7785 (3)	0.0229 (7)
H16	0.716 (5)	1.084 (4)	0.789 (3)	0.037105
C17	0.7581 (4)	0.9489 (3)	0.8537 (2)	0.0202 (7)
H17	0.737 (5)	0.976 (3)	0.916 (3)	0.036874
C18	0.8088 (4)	0.8427 (3)	0.8411 (2)	0.0157 (6)
C19	0.8963 (5)	0.8272 (4)	0.5759 (2)	0.0225 (7)
H19A	1.007 (6)	0.806 (3)	0.587 (3)	0.033683
H19B	0.908 (6)	0.890 (4)	0.540 (3)	0.038169
H19C	0.799 (6)	0.759 (4)	0.537 (3)	0.036569
C20	0.8012 (6)	0.7709 (4)	0.9226 (3)	0.0248 (8)
H20A	0.860 (5)	0.823 (4)	0.988 (3)	0.035488
H20B	0.863 (6)	0.716 (4)	0.918 (3)	0.033384
H20C	0.682 (6)	0.731 (4)	0.926 (3)	0.036538

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Sb	0.01474 (11)	0.01231 (11)	0.01566 (11)	0.00400 (8)	−0.00059 (8)	0.00361 (8)
H1A	0.040890	0.033540	0.033400	0.014310	0.014330	0.005700
Si1	0.0133 (4)	0.0110 (4)	0.0142 (4)	0.0050 (3)	0.0016 (3)	0.0039 (3)
Si2	0.0109 (4)	0.0097 (4)	0.0146 (4)	0.0025 (3)	0.0026 (3)	0.0024 (3)
O	0.0122 (11)	0.0113 (11)	0.0275 (11)	0.0016 (9)	−0.0008 (9)	0.0071 (9)
N1	0.0117 (12)	0.0118 (13)	0.0131 (11)	0.0042 (10)	0.0018 (10)	0.0050 (10)
N2	0.0103 (12)	0.0101 (13)	0.0141 (11)	0.0045 (10)	0.0013 (10)	0.0028 (10)
C1	0.0098 (14)	0.0097 (15)	0.0173 (14)	0.0048 (12)	0.0039 (11)	0.0050 (11)
C2	0.0128 (15)	0.0152 (16)	0.0161 (14)	0.0065 (12)	0.0017 (12)	0.0047 (12)
C3	0.0152 (16)	0.0128 (16)	0.0225 (16)	0.0035 (13)	−0.0025 (13)	0.0008 (13)
H3	0.027540	0.024360	0.035490	0.002120	−0.001500	0.001220
C4	0.0128 (16)	0.0146 (17)	0.0324 (18)	0.0030 (13)	0.0047 (13)	0.0101 (14)
H4	0.023800	0.028300	0.049540	0.002990	0.011480	0.009240
C5	0.0198 (17)	0.0222 (18)	0.0204 (15)	0.0115 (14)	0.0101 (13)	0.0089 (13)
H5	0.037680	0.031230	0.041760	0.007760	0.021160	0.006440
C6	0.0148 (15)	0.0150 (16)	0.0168 (14)	0.0077 (13)	0.0042 (12)	0.0037 (12)
C7	0.0248 (18)	0.0218 (19)	0.0158 (16)	0.0053 (15)	0.0058 (14)	0.0004 (14)
H7A	0.037820	0.029000	0.027260	0.003460	−0.002920	−0.001200
H7B	0.035120	0.030050	0.032420	0.015930	0.006650	0.009820
H7C	0.043910	0.023890	0.032240	0.009450	0.005290	0.012310
C8	0.031 (2)	0.023 (2)	0.0228 (17)	0.0072 (16)	0.0118 (16)	−0.0006 (15)
H8A	0.041110	0.025500	0.039290	0.007070	0.015840	0.012370
H8B	0.028660	0.031250	0.032760	0.009900	0.004240	0.007750
H8C	0.044770	0.032880	0.033430	0.011130	0.019950	0.005120
C9	0.0228 (19)	0.033 (2)	0.0263 (18)	0.0178 (17)	0.0087 (15)	0.0057 (16)
H9A	0.048950	0.033830	0.033880	0.016270	0.016200	0.014230
H9B	0.039400	0.020060	0.046190	0.005490	0.014390	0.003810
H9C	0.025680	0.036550	0.052660	0.013860	0.012020	0.008380
C10	0.0187 (17)	0.0163 (18)	0.0214 (17)	0.0038 (14)	−0.0018 (14)	0.0060 (14)
H10A	0.026410	0.047110	0.042180	0.011710	−0.004790	0.016790
H10B	0.047940	0.019970	0.036680	0.005210	0.005670	0.004740
H10C	0.035160	0.033530	0.030320	0.011540	0.007570	0.006180
C11	0.0190 (17)	0.0240 (19)	0.0226 (17)	0.0069 (15)	0.0079 (14)	0.0071 (15)
H11A	0.033600	0.033690	0.051450	0.019400	0.015390	0.013140
H11B	0.038050	0.024370	0.046620	0.004450	0.019400	0.011620
H11C	0.035520	0.034090	0.032330	0.006720	0.007210	0.001840
C12	0.0218 (18)	0.0169 (18)	0.0198 (16)	0.0037 (15)	0.0014 (14)	0.0005 (14)
H12A	0.040260	0.029030	0.025380	0.010810	0.008410	0.008040
H12B	0.026050	0.020960	0.033750	0.009170	0.008090	0.009170
H12C	0.024760	0.026870	0.041400	0.009710	−0.000140	0.012400
C13	0.0085 (14)	0.0087 (15)	0.0189 (14)	0.0013 (11)	0.0026 (11)	0.0021 (12)
C14	0.0099 (14)	0.0120 (15)	0.0192 (15)	0.0014 (12)	0.0011 (12)	0.0036 (12)
C15	0.0174 (16)	0.0138 (17)	0.0270 (17)	0.0042 (13)	0.0003 (13)	0.0087 (14)
H15	0.040510	0.025210	0.039640	0.011160	0.000950	0.012150
C16	0.0155 (16)	0.0110 (16)	0.0372 (19)	0.0048 (13)	−0.0018 (14)	0.0000 (14)
H16	0.035070	0.020650	0.056180	0.012270	0.009060	0.007020
C17	0.0160 (16)	0.0184 (18)	0.0227 (16)	0.0056 (14)	0.0035 (13)	−0.0035 (14)
H17	0.042470	0.026950	0.043740	0.013300	0.018580	0.003340
C18	0.0133 (15)	0.0148 (16)	0.0159 (14)	0.0020 (13)	0.0028 (12)	0.0007 (12)
C19	0.029 (2)	0.024 (2)	0.0191 (16)	0.0113 (16)	0.0067 (15)	0.0108 (14)
H19A	0.042470	0.029170	0.032660	0.017840	0.006730	0.007500
H19B	0.052500	0.026300	0.032480	0.007170	0.007190	0.012960
H19C	0.033970	0.031910	0.032080	0.003740	−0.004850	0.003240
C20	0.030 (2)	0.030 (2)	0.0220 (17)	0.0147 (17)	0.0133 (16)	0.0115 (15)
H20A	0.037100	0.032170	0.031280	0.005640	0.008310	0.002780
H20B	0.045290	0.022290	0.035330	0.013520	0.013700	0.005880
H20C	0.029880	0.038040	0.046040	0.010900	0.019810	0.011250

Geometric parameters (Å, º)

Sb—H1A	1.73 (3)	C9—H9A	0.95 (4)
Sb—N1	2.044 (2)	C9—H9B	0.94 (4)
Sb—N2	2.049 (2)	C9—H9C	0.94 (4)
Si1—O	1.633 (2)	C10—H10A	0.91 (4)
Si1—N1	1.735 (2)	C10—H10B	1.01 (4)
Si1—C9	1.850 (3)	C10—H10C	0.86 (4)
Si1—C10	1.840 (3)	C11—H11A	0.93 (4)
Si2—O	1.625 (2)	C11—H11B	0.94 (4)
Si2—N2	1.730 (2)	C11—H11C	0.95 (4)
Si2—C11	1.849 (3)	C12—H12A	0.89 (4)
Si2—C12	1.847 (3)	C12—H12B	0.90 (4)
N1—C1	1.433 (4)	C12—H12C	0.90 (4)
N2—C13	1.437 (4)	C13—C14	1.401 (4)
C1—C2	1.406 (4)	C13—C18	1.404 (4)
C1—C6	1.405 (4)	C14—C15	1.382 (4)
C2—C3	1.384 (4)	C14—C19	1.509 (4)
C2—C7	1.509 (4)	C15—H15	0.91 (3)
C3—H3	0.88 (4)	C15—C16	1.381 (5)
C3—C4	1.386 (4)	C16—H16	0.93 (4)
C4—H4	0.97 (4)	C16—C17	1.377 (5)
C4—C5	1.382 (4)	C17—H17	0.92 (3)
C5—H5	0.90 (3)	C17—C18	1.390 (4)
C5—C6	1.384 (4)	C18—C20	1.504 (4)
C6—C8	1.501 (4)	C19—H19A	0.94 (4)
C7—H7A	0.92 (4)	C19—H19B	0.94 (4)
C7—H7B	0.87 (4)	C19—H19C	0.91 (4)
C7—H7C	1.01 (4)	C20—H20A	0.95 (4)
C8—H8A	0.80 (4)	C20—H20B	0.90 (4)
C8—H8B	0.88 (4)	C20—H20C	0.89 (4)
C8—H8C	0.96 (4)
N1—Sb—H1A	91.7 (12)	H9B—C9—Si1	111 (2)
N2—Sb—H1A	94.6 (12)	H9B—C9—H9A	106 (3)
N2—Sb—N1	98.30 (9)	H9C—C9—Si1	116 (2)
N1—Si1—O	105.89 (12)	H9C—C9—H9A	105 (3)
C9—Si1—O	107.46 (15)	H9C—C9—H9B	107 (3)
C9—Si1—N1	113.47 (14)	H10A—C10—Si1	109 (2)
C10—Si1—O	109.21 (13)	H10B—C10—Si1	112 (2)
C10—Si1—N1	111.65 (14)	H10B—C10—H10A	108 (3)
C10—Si1—C9	108.98 (17)	H10C—C10—Si1	113 (2)
N2—Si2—O	105.84 (12)	H10C—C10—H10A	109 (3)
C11—Si2—O	107.26 (14)	H10C—C10—H10B	105 (3)
C11—Si2—N2	112.98 (14)	H11A—C11—Si2	111 (2)
C12—Si2—O	109.32 (14)	H11B—C11—Si2	116 (2)
C12—Si2—N2	111.42 (14)	H11B—C11—H11A	103 (3)
C12—Si2—C11	109.81 (16)	H11C—C11—Si2	110 (2)
Si2—O—Si1	142.83 (14)	H11C—C11—H11A	109 (3)
Si1—N1—Sb	119.79 (13)	H11C—C11—H11B	108 (3)
C1—N1—Sb	116.87 (18)	H12A—C12—Si2	113 (2)
C1—N1—Si1	122.66 (19)	H12B—C12—Si2	114 (2)
Si2—N2—Sb	120.50 (13)	H12B—C12—H12A	107 (3)
C13—N2—Sb	116.03 (17)	H12C—C12—Si2	112 (2)
C13—N2—Si2	122.75 (19)	H12C—C12—H12A	101 (3)
C2—C1—N1	120.6 (2)	H12C—C12—H12B	109 (3)
C6—C1—N1	120.2 (2)	C14—C13—N2	120.4 (2)
C6—C1—C2	119.2 (3)	C18—C13—N2	119.9 (3)
C3—C2—C1	119.7 (3)	C18—C13—C14	119.7 (3)
C7—C2—C1	120.5 (3)	C15—C14—C13	119.4 (3)
C7—C2—C3	119.7 (3)	C19—C14—C13	121.1 (3)
H3—C3—C2	122 (2)	C19—C14—C15	119.5 (3)
C4—C3—C2	121.2 (3)	H15—C15—C14	120 (2)
C4—C3—H3	117 (2)	C16—C15—C14	121.3 (3)
H4—C4—C3	117 (2)	C16—C15—H15	119 (2)
C5—C4—C3	118.7 (3)	H16—C16—C15	121 (2)
C5—C4—H4	124 (2)	C17—C16—C15	119.2 (3)
H5—C5—C4	119 (2)	C17—C16—H16	120 (2)
C6—C5—C4	121.9 (3)	H17—C17—C16	122 (2)
C6—C5—H5	119 (2)	C18—C17—C16	121.4 (3)
C5—C6—C1	119.2 (3)	C18—C17—H17	117 (2)
C8—C6—C1	121.7 (3)	C17—C18—C13	118.9 (3)
C8—C6—C5	119.1 (3)	C20—C18—C13	122.2 (3)
H7A—C7—C2	114 (2)	C20—C18—C17	118.8 (3)
H7B—C7—C2	114 (2)	H19A—C19—C14	111 (2)
H7B—C7—H7A	107 (3)	H19B—C19—C14	109 (2)
H7C—C7—C2	114 (2)	H19B—C19—H19A	111 (3)
H7C—C7—H7A	101 (3)	H19C—C19—C14	110 (2)
H7C—C7—H7B	105 (3)	H19C—C19—H19A	108 (3)
H8A—C8—C6	114 (3)	H19C—C19—H19B	107 (3)
H8B—C8—C6	113 (2)	H20A—C20—C18	112 (2)
H8B—C8—H8A	102 (4)	H20B—C20—C18	114 (2)
H8C—C8—C6	114 (2)	H20B—C20—H20A	104 (3)
H8C—C8—H8A	104 (3)	H20C—C20—C18	112 (2)
H8C—C8—H8B	109 (3)	H20C—C20—H20A	104 (3)
H9A—C9—Si1	112 (2)	H20C—C20—H20B	109 (4)

 

(XAXMEP_HAR_0_HADPs)

Crystal data

C28H52OsP·BF4	V = 1457.79 (4) Å^3
Mr = 696.74	Z = 2
Triclinic, P1	F(000) = 702.711
a = 8.9295 (2) Å	Dx = 1.587 Mg m^−3
b = 9.7179 (1) Å	Mo Kα radiation, λ = 0.71073 Å
c = 17.1819 (1) Å	µ = 4.47 mm^−1
α = 94.114 (1)°	T = 199 K
β = 90.034 (1)°	0.3 × 0.1 × 0.04 mm
γ = 101.369 (1)°

Data collection

Absorption correction: integration	Rint = 0.033
Tmin = 0.529, Tmax = 0.844	θmax = 28.3°, θmin = 2.1°
9506 measured reflections	h = −11→11
6629 independent reflections	k = −12→12
5952 reflections with I ≥ 2u(I)	l = −22→13

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.035	Only H-atom coordinates refined
wR(F^2) = 0.092	w = 1/[σ^2(Fo^2) + (0.042P)^2 + 6.0312P] where P = (Fo^2 + 2Fc^2)/3
S = 1.07	(Δ/σ)max = 0.001
6629 reflections	Δρmax = 0.88 e Å^−3
472 parameters	Δρmin = −1.53 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Os	0.22260 (2)	0.24112 (2)	0.197799 (10)	0.01856 (7)
H1	0.309 (6)	0.411 (5)	0.227 (3)	0.000000
H2	0.140 (5)	0.124 (5)	0.255 (3)	0.000000
H3	0.351 (6)	0.176 (5)	0.244 (3)	0.000000
H4	0.411 (6)	0.300 (6)	0.224 (3)	0.000000
C1	0.0490 (6)	0.2378 (6)	0.0980 (3)	0.0248 (10)
C2	0.0773 (6)	0.0987 (6)	0.1022 (3)	0.0249 (10)
C3	0.2379 (7)	0.1021 (6)	0.0889 (3)	0.0288 (11)
C4	0.3082 (6)	0.2455 (6)	0.0745 (3)	0.0283 (11)
C5	0.1909 (6)	0.3281 (6)	0.0811 (3)	0.0266 (11)
C6	−0.1042 (7)	0.2794 (7)	0.0989 (4)	0.0381 (14)
H6A	−0.134 (6)	0.276 (5)	0.038 (3)	0.000000
H6B	−0.099 (5)	0.388 (5)	0.123 (3)	0.000000
H6C	−0.192 (6)	0.192 (5)	0.127 (3)	0.000000
C8	0.3139 (10)	−0.0209 (8)	0.0810 (4)	0.0507 (18)
H8A	0.425 (5)	−0.010 (5)	0.102 (3)	0.000000
H8B	0.329 (6)	−0.068 (5)	0.022 (3)	0.000000
H8C	0.255 (5)	−0.128 (5)	0.116 (3)	0.000000
C7	−0.0419 (8)	−0.0330 (7)	0.1066 (4)	0.0393 (14)
H7A	0.014 (5)	−0.084 (4)	0.125 (2)	0.000000
H7B	−0.070 (6)	−0.108 (5)	0.053 (3)	0.000000
H7C	−0.150 (6)	−0.005 (5)	0.116 (3)	0.000000
C9	0.4680 (8)	0.2960 (9)	0.0495 (4)	0.0461 (16)
H9A	0.469 (6)	0.295 (5)	−0.017 (3)	0.000000
H9B	0.543 (6)	0.227 (5)	0.072 (3)	0.000000
H9C	0.515 (5)	0.402 (5)	0.063 (3)	0.000000
C10	0.2108 (8)	0.4766 (7)	0.0594 (4)	0.0399 (15)
H10A	0.213 (5)	0.471 (5)	−0.005 (3)	0.000000
H10B	0.324 (6)	0.543 (5)	0.082 (3)	0.000000
H10C	0.116 (5)	0.526 (5)	0.082 (3)	0.000000
P	0.11844 (13)	0.33051 (12)	0.31286 (7)	0.0155 (2)
C11	0.1600 (5)	0.5249 (5)	0.3290 (3)	0.0198 (9)
H11	0.112 (5)	0.550 (5)	0.384 (3)	0.000000
C12	0.3329 (6)	0.5863 (5)	0.3363 (3)	0.0255 (11)
H12A	0.392 (5)	0.532 (5)	0.378 (3)	0.000000
H12B	0.383 (5)	0.559 (5)	0.281 (3)	0.000000
C13	0.3647 (7)	0.7461 (6)	0.3526 (4)	0.0347 (13)
H13A	0.316 (5)	0.774 (5)	0.404 (3)	0.000000
H13B	0.495 (6)	0.788 (5)	0.358 (3)	0.000000
C14	0.2916 (7)	0.8153 (6)	0.2896 (4)	0.0367 (14)
H14A	0.344 (5)	0.799 (5)	0.233 (3)	0.000000
H14B	0.313 (5)	0.927 (5)	0.307 (3)	0.000000
C15	0.1202 (7)	0.7571 (6)	0.2840 (4)	0.0354 (13)
H15A	0.060 (5)	0.806 (5)	0.236 (3)	0.000000
H15B	0.066 (5)	0.781 (5)	0.345 (3)	0.000000
C16	0.0858 (6)	0.5968 (5)	0.2670 (3)	0.0268 (11)
H16A	−0.042 (5)	0.565 (5)	0.270 (3)	0.000000
H16B	0.118 (5)	0.558 (5)	0.208 (3)	0.000000
C21	−0.0929 (5)	0.2831 (5)	0.3143 (3)	0.0179 (9)
H21	−0.131 (6)	0.342 (5)	0.265 (3)	0.000000
C22	−0.1597 (6)	0.1268 (5)	0.2915 (3)	0.0222 (10)
H22A	−0.113 (5)	0.090 (5)	0.235 (3)	0.000000
H22B	−0.133 (5)	0.055 (5)	0.333 (3)	0.000000
C23	−0.3343 (6)	0.0997 (5)	0.2820 (3)	0.0258 (11)
H23A	−0.367 (5)	0.164 (5)	0.233 (3)	0.000000
H23B	−0.388 (5)	−0.017 (5)	0.265 (3)	0.000000
C24	−0.4069 (6)	0.1489 (6)	0.3568 (3)	0.0247 (10)
H24A	−0.528 (5)	0.144 (5)	0.347 (3)	0.000000
H24B	−0.391 (6)	0.082 (5)	0.413 (3)	0.000000
C25	−0.3417 (6)	0.3033 (6)	0.3800 (3)	0.0270 (11)
H25A	−0.394 (5)	0.342 (5)	0.432 (3)	0.000000
H25B	−0.370 (5)	0.366 (5)	0.336 (3)	0.000000
C26	−0.1670 (6)	0.3304 (6)	0.3896 (3)	0.0247 (10)
H26A	−0.124 (5)	0.434 (5)	0.407 (3)	0.000000
H26B	−0.140 (5)	0.258 (5)	0.435 (3)	0.000000
C31	0.2016 (5)	0.2742 (5)	0.4026 (3)	0.0174 (9)
H31	0.334 (5)	0.278 (5)	0.398 (3)	0.000000
C32	0.1879 (6)	0.3638 (5)	0.4798 (3)	0.0213 (10)
H32A	0.241 (5)	0.478 (5)	0.476 (3)	0.000000
H32B	0.069 (5)	0.346 (5)	0.496 (3)	0.000000
C33	0.2768 (7)	0.3168 (6)	0.5460 (3)	0.0275 (11)
H33A	0.413 (6)	0.329 (5)	0.529 (3)	0.000000
H33B	0.262 (6)	0.362 (5)	0.609 (3)	0.000000
C34	0.2204 (6)	0.1606 (6)	0.5576 (3)	0.0249 (10)
H34A	0.290 (5)	0.120 (5)	0.599 (3)	0.000000
H34B	0.110 (5)	0.143 (5)	0.577 (3)	0.000000
C35	0.2315 (6)	0.0700 (5)	0.4824 (3)	0.0247 (10)
H35A	0.188 (5)	−0.049 (5)	0.491 (3)	0.000000
H35B	0.363 (5)	0.069 (4)	0.465 (2)	0.000000
C36	0.1442 (6)	0.1177 (5)	0.4153 (3)	0.0215 (10)
H36A	0.019 (5)	0.109 (5)	0.426 (3)	0.000000
H36B	0.147 (5)	0.052 (5)	0.364 (3)	0.000000
B	0.3090 (9)	0.3654 (9)	0.8137 (4)	0.0416 (17)
F1	0.1956 (6)	0.3611 (5)	0.8668 (3)	0.0739 (15)
F2	0.2643 (7)	0.2598 (7)	0.7558 (3)	0.0917 (19)
F3	0.4453 (7)	0.3552 (8)	0.8466 (4)	0.095 (2)
F4	0.3290 (7)	0.4935 (7)	0.7811 (4)	0.100 (2)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Os	0.01901 (10)	0.02373 (10)	0.01323 (10)	0.00523 (7)	0.00141 (6)	0.00045 (6)
H1	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H2	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H3	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H4	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C1	0.024 (3)	0.030 (3)	0.020 (2)	0.004 (2)	−0.0007 (19)	0.0048 (19)
C2	0.032 (3)	0.029 (3)	0.013 (2)	0.005 (2)	−0.0052 (19)	−0.0020 (18)
C3	0.042 (3)	0.029 (3)	0.017 (2)	0.013 (2)	−0.001 (2)	−0.0023 (19)
C4	0.030 (3)	0.040 (3)	0.015 (2)	0.009 (2)	0.008 (2)	0.003 (2)
C5	0.029 (3)	0.033 (3)	0.017 (2)	0.002 (2)	0.0055 (19)	0.0071 (19)
C6	0.030 (3)	0.053 (4)	0.034 (3)	0.011 (3)	−0.010 (2)	0.008 (3)
H6A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H6B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H6C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C8	0.070 (5)	0.051 (4)	0.042 (4)	0.041 (4)	0.007 (4)	−0.002 (3)
H8A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H8B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H8C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C7	0.047 (4)	0.034 (3)	0.033 (3)	−0.002 (3)	−0.012 (3)	0.005 (2)
H7A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H7B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H7C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C9	0.035 (3)	0.063 (5)	0.038 (4)	0.007 (3)	0.012 (3)	0.002 (3)
H9A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H9B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H9C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C10	0.056 (4)	0.033 (3)	0.030 (3)	0.003 (3)	0.006 (3)	0.014 (2)
H10A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H10B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H10C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
P	0.0155 (5)	0.0160 (5)	0.0152 (5)	0.0034 (4)	0.0016 (4)	0.0015 (4)
C11	0.020 (2)	0.019 (2)	0.020 (2)	0.0020 (18)	0.0020 (18)	0.0011 (17)
H11	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C12	0.020 (2)	0.017 (2)	0.039 (3)	0.0028 (18)	−0.002 (2)	0.005 (2)
H12A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H12B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C13	0.035 (3)	0.016 (2)	0.050 (4)	0.000 (2)	−0.010 (3)	−0.001 (2)
H13A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H13B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C14	0.031 (3)	0.020 (3)	0.059 (4)	0.001 (2)	−0.001 (3)	0.010 (3)
H14A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H14B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C15	0.029 (3)	0.022 (3)	0.056 (4)	0.004 (2)	−0.006 (3)	0.009 (2)
H15A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H15B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C16	0.033 (3)	0.024 (2)	0.025 (3)	0.008 (2)	−0.009 (2)	0.001 (2)
H16A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H16B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C21	0.020 (2)	0.015 (2)	0.018 (2)	0.0033 (17)	0.0034 (17)	−0.0017 (16)
H21	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C22	0.019 (2)	0.020 (2)	0.027 (3)	0.0021 (18)	0.0015 (19)	−0.0043 (19)
H22A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H22B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C23	0.023 (3)	0.022 (2)	0.028 (3)	−0.0014 (19)	0.000 (2)	−0.002 (2)
H23A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H23B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C24	0.015 (2)	0.029 (3)	0.029 (3)	0.0013 (19)	0.0045 (19)	0.003 (2)
H24A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H24B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C25	0.022 (2)	0.029 (3)	0.030 (3)	0.007 (2)	0.008 (2)	−0.001 (2)
H25A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H25B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C26	0.017 (2)	0.030 (3)	0.025 (3)	0.005 (2)	0.0045 (19)	−0.007 (2)
H26A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H26B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C31	0.017 (2)	0.017 (2)	0.018 (2)	0.0050 (17)	0.0005 (17)	−0.0001 (17)
H31	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C32	0.029 (3)	0.022 (2)	0.015 (2)	0.010 (2)	−0.0039 (19)	−0.0008 (17)
H32A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H32B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C33	0.038 (3)	0.028 (3)	0.015 (2)	0.004 (2)	−0.007 (2)	0.0024 (19)
H33A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H33B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C34	0.027 (3)	0.030 (3)	0.019 (2)	0.005 (2)	0.000 (2)	0.0075 (19)
H34A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H34B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C35	0.031 (3)	0.025 (2)	0.020 (2)	0.009 (2)	0.003 (2)	0.0034 (19)
H35A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H35B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C36	0.032 (3)	0.016 (2)	0.015 (2)	0.0024 (19)	−0.0018 (19)	0.0011 (17)
H36A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H36B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
B	0.041 (4)	0.052 (4)	0.029 (3)	0.001 (3)	0.009 (3)	0.004 (3)
F1	0.088 (4)	0.071 (3)	0.056 (3)	0.002 (3)	0.030 (3)	−0.004 (2)
F2	0.080 (4)	0.121 (5)	0.067 (4)	0.024 (3)	−0.010 (3)	−0.047 (3)
F3	0.071 (4)	0.138 (6)	0.080 (4)	0.030 (4)	−0.030 (3)	0.008 (4)
F4	0.086 (4)	0.098 (4)	0.123 (5)	0.011 (3)	0.009 (4)	0.066 (4)

Geometric parameters (Å, º)

Os—H1	1.72 (5)	C14—H14A	1.09 (5)
Os—H2	1.63 (4)	C14—H14B	1.09 (4)
Os—H3	1.65 (5)	C14—C15	1.524 (8)
Os—H4	1.72 (5)	C15—H15A	1.16 (5)
Os—C1	2.305 (5)	C15—H15B	1.18 (5)
Os—C2	2.294 (5)	C15—C16	1.534 (7)
Os—C3	2.248 (5)	C16—H16A	1.12 (5)
Os—C4	2.254 (5)	C16—H16B	1.12 (5)
Os—C5	2.270 (5)	C21—H21	1.15 (5)
Os—P	2.3669 (11)	C21—C22	1.541 (6)
C1—C2	1.431 (7)	C21—C26	1.536 (6)
C1—C5	1.435 (7)	C22—H22A	1.12 (5)
C1—C6	1.500 (8)	C22—H22B	1.09 (5)
C2—C3	1.447 (8)	C22—C23	1.536 (7)
C2—C7	1.500 (8)	C23—H23A	1.16 (4)
C3—C4	1.450 (8)	C23—H23B	1.16 (5)
C3—C8	1.485 (8)	C23—C24	1.527 (7)
C4—C5	1.440 (8)	C24—H24A	1.08 (5)
C4—C9	1.488 (8)	C24—H24B	1.23 (5)
C5—C10	1.493 (8)	C24—C25	1.523 (7)
C6—H6A	1.08 (5)	C25—H25A	1.09 (4)
C6—H6B	1.10 (4)	C25—H25B	1.07 (4)
C6—H6C	1.17 (5)	C25—C26	1.537 (7)
C8—H8A	1.04 (5)	C26—H26A	1.03 (4)
C8—H8B	1.10 (5)	C26—H26B	1.14 (5)
C8—H8C	1.26 (4)	C31—H31	1.18 (5)
C7—H7A	0.85 (4)	C31—C32	1.553 (6)
C7—H7B	1.12 (5)	C31—C36	1.538 (6)
C7—H7C	1.07 (5)	C32—H32A	1.12 (5)
C9—H9A	1.14 (5)	C32—H32B	1.09 (5)
C9—H9B	1.12 (5)	C32—C33	1.533 (7)
C9—H9C	1.04 (5)	C33—H33A	1.24 (5)
C10—H10A	1.10 (5)	C33—H33B	1.15 (5)
C10—H10B	1.14 (5)	C33—C34	1.529 (7)
C10—H10C	1.11 (5)	C34—H34A	1.09 (5)
P—C11	1.853 (5)	C34—H34B	1.03 (5)
P—C21	1.853 (5)	C34—C35	1.526 (7)
P—C31	1.873 (5)	C35—H35A	1.17 (5)
C11—H11	1.07 (4)	C35—H35B	1.21 (4)
C11—C12	1.542 (7)	C35—C36	1.540 (7)
C11—C16	1.533 (7)	C36—H36A	1.12 (5)
C12—H12A	1.11 (4)	C36—H36B	1.05 (5)
C12—H12B	1.09 (5)	B—F1	1.360 (8)
C12—C13	1.528 (7)	B—F2	1.375 (9)
C13—H13A	1.03 (5)	B—F3	1.366 (10)
C13—H13B	1.16 (5)	B—F4	1.381 (10)
C13—C14	1.526 (9)
H2—Os—H1	125 (2)	C12—C11—H11	106 (2)
H3—Os—H1	92 (3)	C16—C11—P	112.9 (3)
H3—Os—H2	69 (2)	C16—C11—H11	108 (2)
H4—Os—H1	53 (2)	C16—C11—C12	110.6 (4)
H4—Os—H2	111 (3)	H12A—C12—C11	112 (2)
H4—Os—H3	45 (2)	H12B—C12—C11	107 (2)
C1—Os—H1	110.7 (18)	H12B—C12—H12A	102 (3)
C1—Os—H2	105.6 (17)	C13—C12—C11	111.6 (4)
C1—Os—H3	153.2 (18)	C13—C12—H12A	113 (2)
C1—Os—H4	142.6 (19)	C13—C12—H12B	110 (2)
C2—Os—H1	145.1 (18)	H13A—C13—C12	111 (3)
C2—Os—H2	84.1 (17)	H13B—C13—C12	109 (2)
C2—Os—H3	117.9 (18)	H13B—C13—H13A	108 (4)
C2—Os—H4	139.7 (18)	C14—C13—C12	110.7 (5)
C2—Os—C1	36.25 (18)	C14—C13—H13A	105 (3)
C3—Os—H1	132.8 (18)	C14—C13—H13B	112 (3)
C3—Os—H2	99.9 (17)	H14A—C14—C13	111 (3)
C3—Os—H3	92.6 (18)	H14B—C14—C13	106 (2)
C3—Os—H4	102.6 (18)	H14B—C14—H14A	109 (3)
C3—Os—C1	61.7 (2)	C15—C14—C13	110.5 (5)
C3—Os—C2	37.1 (2)	C15—C14—H14A	110 (3)
C4—Os—H1	96.0 (18)	C15—C14—H14B	110 (2)
C4—Os—H2	137.5 (17)	H15A—C15—C14	113 (2)
C4—Os—H3	103.4 (18)	H15B—C15—C14	108 (2)
C4—Os—H4	85.0 (19)	H15B—C15—H15A	109 (3)
C4—Os—C1	61.69 (19)	C16—C15—C14	111.4 (5)
C4—Os—C2	61.8 (2)	C16—C15—H15A	108 (2)
C4—Os—C3	37.6 (2)	C16—C15—H15B	107 (2)
C5—Os—H1	85.0 (18)	C15—C16—C11	111.0 (4)
C5—Os—H2	141.8 (17)	H16A—C16—C11	109 (2)
C5—Os—H3	139.2 (18)	H16A—C16—C15	105 (2)
C5—Os—H4	106.2 (19)	H16B—C16—C11	109 (2)
C5—Os—C1	36.54 (18)	H16B—C16—C15	115 (2)
C5—Os—C2	60.94 (19)	H16B—C16—H16A	107 (3)
C5—Os—C3	62.0 (2)	H21—C21—P	104 (2)
C5—Os—C4	37.1 (2)	C22—C21—P	114.5 (3)
P—Os—H1	66.8 (17)	C22—C21—H21	105 (2)
P—Os—H2	64.4 (17)	C26—C21—P	115.5 (3)
P—Os—H3	94.5 (18)	C26—C21—H21	108 (2)
P—Os—H4	96.6 (18)	C26—C21—C22	109.7 (4)
P—Os—C1	107.10 (13)	H22A—C22—C21	112 (2)
P—Os—C2	123.23 (14)	H22B—C22—C21	114 (2)
P—Os—C3	158.88 (16)	H22B—C22—H22A	104 (3)
P—Os—C4	155.73 (15)	C23—C22—C21	111.6 (4)
P—Os—C5	120.91 (14)	C23—C22—H22A	107 (2)
C2—C1—Os	71.4 (3)	C23—C22—H22B	107 (2)
C5—C1—Os	70.4 (3)	H23A—C23—C22	110 (2)
C5—C1—C2	107.7 (5)	H23B—C23—C22	113 (2)
C6—C1—Os	130.5 (4)	H23B—C23—H23A	107 (3)
C6—C1—C2	126.5 (5)	C24—C23—C22	110.5 (4)
C6—C1—C5	125.2 (5)	C24—C23—H23A	107 (2)
C1—C2—Os	72.3 (3)	C24—C23—H23B	110 (2)
C3—C2—Os	69.7 (3)	H24A—C24—C23	110 (2)
C3—C2—C1	108.5 (5)	H24B—C24—C23	114 (2)
C7—C2—Os	131.2 (4)	H24B—C24—H24A	109 (3)
C7—C2—C1	126.0 (5)	C25—C24—C23	111.0 (4)
C7—C2—C3	124.8 (5)	C25—C24—H24A	105 (2)
C2—C3—Os	73.2 (3)	C25—C24—H24B	108 (2)
C4—C3—Os	71.4 (3)	H25A—C25—C24	113 (2)
C4—C3—C2	107.5 (5)	H25B—C25—C24	109 (2)
C8—C3—Os	126.9 (4)	H25B—C25—H25A	104 (3)
C8—C3—C2	126.5 (6)	C26—C25—C24	111.3 (4)
C8—C3—C4	125.6 (6)	C26—C25—H25A	111 (2)
C3—C4—Os	71.0 (3)	C26—C25—H25B	109 (2)
C5—C4—Os	72.1 (3)	C25—C26—C21	110.7 (4)
C5—C4—C3	107.4 (5)	H26A—C26—C21	112 (3)
C9—C4—Os	126.9 (4)	H26A—C26—C25	111 (3)
C9—C4—C3	126.6 (6)	H26B—C26—C21	105 (2)
C9—C4—C5	125.8 (6)	H26B—C26—C25	107 (2)
C1—C5—Os	73.1 (3)	H26B—C26—H26A	111 (3)
C4—C5—Os	70.8 (3)	H31—C31—P	112 (2)
C4—C5—C1	108.8 (5)	C32—C31—P	116.4 (3)
C10—C5—Os	130.4 (4)	C32—C31—H31	103 (2)
C10—C5—C1	126.1 (5)	C36—C31—P	113.1 (3)
C10—C5—C4	124.2 (5)	C36—C31—H31	101 (2)
H6A—C6—C1	104 (3)	C36—C31—C32	109.3 (4)
H6B—C6—C1	113 (2)	H32A—C32—C31	113 (3)
H6B—C6—H6A	107 (4)	H32B—C32—C31	109 (2)
H6C—C6—C1	109 (2)	H32B—C32—H32A	113 (3)
H6C—C6—H6A	108 (4)	C33—C32—C31	110.6 (4)
H6C—C6—H6B	116 (3)	C33—C32—H32A	104 (3)
H8A—C8—C3	119 (3)	C33—C32—H32B	107 (3)
H8B—C8—C3	118 (3)	H33A—C33—C32	110 (2)
H8B—C8—H8A	99 (4)	H33B—C33—C32	118 (2)
H8C—C8—C3	117 (2)	H33B—C33—H33A	112 (3)
H8C—C8—H8A	98 (3)	C34—C33—C32	111.0 (4)
H8C—C8—H8B	102 (3)	C34—C33—H33A	105 (2)
H7A—C7—C2	98 (3)	C34—C33—H33B	99 (2)
H7B—C7—C2	120 (3)	H34A—C34—C33	113 (2)
H7B—C7—H7A	91 (4)	H34B—C34—C33	110 (3)
H7C—C7—C2	109 (3)	H34B—C34—H34A	108 (4)
H7C—C7—H7A	140 (4)	C35—C34—C33	111.2 (4)
H7C—C7—H7B	100 (4)	C35—C34—H34A	103 (2)
H9A—C9—C4	109 (3)	C35—C34—H34B	110 (3)
H9B—C9—C4	109 (3)	H35A—C35—C34	111 (2)
H9B—C9—H9A	112 (4)	H35B—C35—C34	112 (2)
H9C—C9—C4	117 (3)	H35B—C35—H35A	100 (3)
H9C—C9—H9A	99 (4)	C36—C35—C34	110.6 (4)
H9C—C9—H9B	111 (4)	C36—C35—H35A	111 (2)
H10A—C10—C5	106 (2)	C36—C35—H35B	111 (2)
H10B—C10—C5	112 (3)	C35—C36—C31	111.7 (4)
H10B—C10—H10A	108 (4)	H36A—C36—C31	104 (2)
H10C—C10—C5	111 (3)	H36A—C36—C35	114 (2)
H10C—C10—H10A	112 (4)	H36B—C36—C31	113 (3)
H10C—C10—H10B	109 (4)	H36B—C36—C35	111 (3)
C11—P—Os	114.82 (16)	H36B—C36—H36A	104 (3)
C21—P—Os	112.94 (15)	F2—B—F1	108.8 (6)
C21—P—C11	103.8 (2)	F3—B—F1	112.6 (7)
C31—P—Os	111.66 (15)	F3—B—F2	111.0 (7)
C31—P—C11	102.8 (2)	F4—B—F1	107.9 (7)
C31—P—C21	110.1 (2)	F4—B—F2	108.8 (7)
H11—C11—P	107 (2)	F4—B—F3	107.7 (7)
C12—C11—P	112.4 (3)
Os—C1—C2—C3	−60.6 (3)	C1—C5—C4—C9	173.4 (5)
Os—C1—C2—C7	128.5 (3)	C2—C3—C4—C5	1.5 (4)
Os—C1—C5—C4	62.2 (3)	C2—C3—C4—C9	−172.9 (5)
Os—C1—C5—C10	−128.1 (3)	C3—C4—C5—C10	−170.9 (4)
Os—C2—C1—C5	61.4 (3)	P—C11—C12—C13	−177.8 (4)
Os—C2—C1—C6	−127.1 (3)	P—C11—C16—C15	178.6 (4)
Os—C2—C3—C4	−63.6 (3)	P—C21—C22—C23	−171.4 (4)
Os—C2—C3—C8	123.8 (4)	P—C21—C26—C25	172.3 (4)
Os—C3—C2—C1	62.2 (3)	P—C31—C32—C33	−173.3 (4)
Os—C3—C2—C7	−126.7 (3)	P—C31—C36—C35	171.8 (3)
Os—C3—C4—C5	−63.3 (3)	C11—C12—C13—C14	−56.3 (5)
Os—C3—C4—C9	122.3 (4)	C11—C16—C15—C14	56.4 (5)
Os—C4—C3—C2	64.8 (3)	C12—C13—C14—C15	57.2 (6)
Os—C4—C3—C8	−122.5 (4)	C13—C14—C15—C16	−57.5 (6)
Os—C4—C5—C1	−63.6 (3)	C21—C22—C23—C24	−56.6 (5)
Os—C4—C5—C10	126.4 (3)	C21—C26—C25—C24	57.0 (5)
Os—C5—C1—C2	−62.1 (3)	C22—C23—C24—C25	56.0 (5)
Os—C5—C1—C6	126.3 (3)	C23—C24—C25—C26	−56.6 (5)
Os—C5—C4—C3	62.6 (3)	C31—C32—C33—C34	−57.5 (4)
Os—C5—C4—C9	−123.0 (4)	C31—C36—C35—C34	56.4 (4)
C1—C2—C3—C4	−1.4 (4)	C32—C33—C34—C35	56.8 (5)
C1—C2—C3—C8	−174.0 (5)	C33—C34—C35—C36	−55.6 (5)
C1—C5—C4—C3	−1.0 (5)

(XAXMEP_HAR)

Crystal data

C28H52OsP·BF4	V = 1457.79 (4) Å^3
Mr = 696.74	Z = 2
Triclinic, P1	F(000) = 111.426
a = 8.9295 (2) Å	Dx = 1.587 Mg m^−3
b = 9.7179 (1) Å	Mo Kα radiation, λ = 0.71073 Å
c = 17.1819 (1) Å	µ = 4.47 mm^−1
α = 94.114 (1)°	T = 199 K
β = 90.034 (1)°	0.3 × 0.1 × 0.04 mm
γ = 101.369 (1)°

Data collection

Absorption correction: integration	Rint = 0.033
Tmin = 0.529, Tmax = 0.844	θmax = 28.3°, θmin = 2.1°
9506 measured reflections	h = −11→11
6629 independent reflections	k = −12→12
5952 reflections with I ≥ 2u(I)	l = −22→13

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.033	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.080	w = 1/[σ^2(Fo^2) + (0.020P)^2 + 7.050P] where P = (Fo^2 + 2Fc^2)/3
S = 1.09	(Δ/σ)max = 0.001
6629 reflections	Δρmax = 0.86 e Å^−3
522 parameters	Δρmin = −1.51 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Os	0.22260 (2)	0.241115 (19)	0.197802 (10)	0.01844 (6)
H1	0.309 (5)	0.409 (5)	0.227 (3)	0.000100*
H2	0.141 (6)	0.115 (6)	0.254 (3)	0.019 (14)*
H3	0.348 (7)	0.169 (7)	0.244 (4)	0.024 (16)*
H4	0.406 (8)	0.292 (8)	0.230 (4)	0.04 (2)*
C1	0.0490 (6)	0.2383 (5)	0.0980 (3)	0.0247 (10)
C2	0.0772 (6)	0.0985 (5)	0.1023 (3)	0.0247 (10)
C3	0.2379 (6)	0.1023 (5)	0.0889 (3)	0.0286 (11)
C4	0.3083 (6)	0.2457 (6)	0.0745 (3)	0.0284 (11)
C5	0.1909 (6)	0.3281 (5)	0.0811 (3)	0.0268 (10)
C6	−0.1043 (7)	0.2793 (7)	0.0989 (4)	0.0383 (13)
H6A	−0.142 (9)	0.278 (8)	0.038 (5)	0.07 (3)*
H6B	−0.094 (9)	0.384 (9)	0.125 (5)	0.06 (2)*
H6C	−0.191 (9)	0.192 (9)	0.125 (5)	0.07 (2)*
C8	0.3149 (10)	−0.0210 (8)	0.0812 (4)	0.0503 (18)
H8A	0.439 (13)	0.005 (11)	0.106 (6)	0.10 (4)*
H8B	0.315 (17)	−0.072 (16)	0.019 (10)	0.18 (6)*
H8C	0.270 (11)	−0.111 (10)	0.119 (6)	0.09 (3)*
C7	−0.0407 (8)	−0.0335 (7)	0.1069 (4)	0.0402 (14)
H7A	0.016 (10)	−0.097 (9)	0.131 (6)	0.08 (3)*
H7B	−0.075 (13)	−0.096 (11)	0.059 (7)	0.11 (4)*
H7C	−0.155 (12)	−0.008 (11)	0.122 (6)	0.10 (3)*
C9	0.4685 (8)	0.2970 (9)	0.0497 (4)	0.0470 (16)
H9A	0.469 (9)	0.294 (8)	−0.015 (5)	0.06 (2)*
H9B	0.544 (9)	0.237 (8)	0.069 (5)	0.06 (2)*
H9C	0.521 (11)	0.417 (10)	0.065 (6)	0.08 (3)*
C10	0.2111 (8)	0.4766 (6)	0.0593 (4)	0.0398 (14)
H10A	0.214 (10)	0.480 (9)	−0.006 (6)	0.08 (3)*
H10B	0.321 (12)	0.547 (10)	0.083 (6)	0.10 (3)*
H10C	0.118 (9)	0.526 (8)	0.082 (5)	0.06 (2)*
P	0.11843 (12)	0.33049 (11)	0.31287 (6)	0.0154 (2)
C11	0.1600 (5)	0.5251 (5)	0.3290 (3)	0.0198 (9)
H11	0.112 (7)	0.550 (6)	0.387 (4)	0.037 (17)*
C12	0.3328 (5)	0.5861 (5)	0.3363 (3)	0.0254 (10)
H12A	0.395 (7)	0.530 (6)	0.380 (4)	0.034 (17)*
H12B	0.381 (7)	0.556 (6)	0.279 (4)	0.032 (16)*
C13	0.3644 (7)	0.7463 (5)	0.3527 (4)	0.0350 (13)
H13A	0.317 (7)	0.777 (7)	0.408 (4)	0.038 (17)*
H13B	0.493 (11)	0.783 (10)	0.360 (6)	0.10 (3)*
C14	0.2916 (7)	0.8154 (6)	0.2896 (4)	0.0374 (13)
H14A	0.353 (9)	0.798 (8)	0.231 (5)	0.07 (2)*
H14B	0.318 (9)	0.926 (9)	0.302 (5)	0.07 (2)*
C15	0.1203 (6)	0.7572 (6)	0.2841 (4)	0.0356 (13)
H15A	0.060 (7)	0.806 (7)	0.240 (4)	0.041 (18)*
H15B	0.065 (7)	0.780 (7)	0.345 (4)	0.039 (18)*
C16	0.0856 (6)	0.5967 (5)	0.2671 (3)	0.0268 (10)
H16A	−0.040 (9)	0.559 (8)	0.264 (5)	0.07 (2)*
H16B	0.123 (7)	0.563 (6)	0.208 (4)	0.036 (17)*
C21	−0.0928 (5)	0.2830 (4)	0.3143 (3)	0.0179 (8)
H21	−0.128 (6)	0.343 (6)	0.265 (3)	0.025 (15)*
C22	−0.1596 (5)	0.1268 (5)	0.2915 (3)	0.0221 (9)
H22A	−0.109 (8)	0.087 (7)	0.234 (4)	0.043 (19)*
H22B	−0.132 (8)	0.059 (7)	0.333 (4)	0.048 (19)*
C23	−0.3341 (6)	0.1000 (5)	0.2819 (3)	0.0255 (10)
H23A	−0.365 (7)	0.164 (7)	0.232 (4)	0.036 (17)*
H23B	−0.382 (8)	−0.019 (7)	0.265 (4)	0.041 (18)*
C24	−0.4069 (5)	0.1489 (5)	0.3569 (3)	0.0248 (10)
H24A	−0.531 (7)	0.139 (6)	0.349 (4)	0.039 (17)*
H24B	−0.394 (8)	0.077 (7)	0.410 (4)	0.042 (19)*
C25	−0.3420 (6)	0.3035 (5)	0.3798 (3)	0.0264 (10)
H25A	−0.394 (8)	0.338 (7)	0.433 (4)	0.06 (2)*
H25B	−0.376 (8)	0.368 (7)	0.335 (4)	0.05 (2)*
C26	−0.1671 (5)	0.3303 (5)	0.3896 (3)	0.0245 (10)
H26A	−0.126 (7)	0.436 (7)	0.406 (4)	0.041 (17)*
H26B	−0.139 (7)	0.260 (6)	0.437 (4)	0.036 (17)*
C31	0.2016 (5)	0.2744 (4)	0.4026 (3)	0.0175 (8)
H31	0.334 (5)	0.278 (5)	0.396 (3)	0.000100*
C32	0.1877 (6)	0.3638 (5)	0.4797 (3)	0.0215 (9)
H32A	0.231 (9)	0.480 (8)	0.475 (5)	0.06 (2)*
H32B	0.065 (7)	0.348 (6)	0.494 (3)	0.030 (15)*
C33	0.2766 (6)	0.3167 (5)	0.5460 (3)	0.0272 (10)
H33A	0.407 (7)	0.329 (7)	0.535 (4)	0.038 (18)*
H33B	0.261 (8)	0.365 (7)	0.608 (4)	0.05 (2)*
C34	0.2204 (6)	0.1606 (5)	0.5576 (3)	0.0248 (10)
H34A	0.284 (8)	0.120 (7)	0.601 (4)	0.044 (18)*
H34B	0.109 (7)	0.140 (6)	0.578 (4)	0.033 (15)*
C35	0.2319 (6)	0.0699 (5)	0.4823 (3)	0.0246 (10)
H35A	0.178 (8)	−0.054 (7)	0.486 (4)	0.05 (2)*
H35B	0.360 (8)	0.070 (7)	0.463 (4)	0.05 (2)*
C36	0.1442 (6)	0.1176 (5)	0.4153 (3)	0.0214 (9)
H36A	0.016 (6)	0.104 (6)	0.427 (3)	0.025 (14)*
H36B	0.140 (7)	0.051 (6)	0.365 (4)	0.037 (16)*
B	0.3092 (9)	0.3653 (8)	0.8135 (4)	0.0424 (16)
F1	0.1955 (6)	0.3609 (5)	0.8668 (3)	0.0738 (14)
F2	0.2644 (6)	0.2598 (6)	0.7558 (3)	0.0905 (17)
F3	0.4452 (6)	0.3548 (7)	0.8468 (3)	0.0953 (18)
F4	0.3292 (7)	0.4932 (6)	0.7810 (4)	0.101 (2)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Os	0.01894 (9)	0.02358 (10)	0.01309 (9)	0.00521 (6)	0.00143 (6)	0.00048 (6)
C1	0.024 (2)	0.030 (3)	0.019 (2)	0.003 (2)	−0.0007 (18)	0.0042 (18)
C2	0.032 (3)	0.028 (2)	0.013 (2)	0.004 (2)	−0.0047 (18)	−0.0012 (17)
C3	0.041 (3)	0.029 (3)	0.018 (2)	0.013 (2)	−0.001 (2)	−0.0022 (18)
C4	0.030 (3)	0.040 (3)	0.016 (2)	0.009 (2)	0.0083 (19)	0.0030 (19)
C5	0.030 (3)	0.033 (3)	0.017 (2)	0.002 (2)	0.0051 (19)	0.0068 (19)
C6	0.029 (3)	0.054 (4)	0.033 (3)	0.011 (3)	−0.009 (2)	0.009 (3)
C8	0.074 (5)	0.048 (4)	0.039 (4)	0.040 (4)	0.009 (3)	−0.002 (3)
C7	0.051 (4)	0.035 (3)	0.028 (3)	−0.008 (3)	−0.008 (3)	0.001 (2)
C9	0.036 (3)	0.070 (5)	0.036 (3)	0.011 (3)	0.013 (3)	0.006 (3)
C10	0.057 (4)	0.032 (3)	0.030 (3)	0.003 (3)	0.006 (3)	0.013 (2)
P	0.0155 (5)	0.0160 (5)	0.0148 (5)	0.0033 (4)	0.0015 (4)	0.0014 (4)
C11	0.020 (2)	0.019 (2)	0.019 (2)	0.0018 (17)	0.0017 (17)	0.0017 (16)
C12	0.019 (2)	0.018 (2)	0.039 (3)	0.0017 (17)	−0.002 (2)	0.0042 (19)
C13	0.035 (3)	0.017 (2)	0.050 (4)	−0.001 (2)	−0.011 (3)	0.000 (2)
C14	0.032 (3)	0.020 (2)	0.060 (4)	0.001 (2)	−0.002 (3)	0.011 (2)
C15	0.030 (3)	0.022 (3)	0.056 (4)	0.004 (2)	−0.007 (3)	0.010 (2)
C16	0.031 (3)	0.023 (2)	0.026 (2)	0.007 (2)	−0.009 (2)	0.0013 (19)
C21	0.020 (2)	0.016 (2)	0.018 (2)	0.0034 (16)	0.0035 (17)	−0.0014 (16)
C22	0.019 (2)	0.020 (2)	0.026 (2)	0.0026 (17)	0.0016 (18)	−0.0035 (18)
C23	0.023 (2)	0.022 (2)	0.028 (3)	−0.0014 (19)	0.0008 (19)	−0.0032 (19)
C24	0.014 (2)	0.030 (2)	0.029 (3)	0.0014 (18)	0.0045 (18)	0.003 (2)
C25	0.022 (2)	0.029 (3)	0.028 (3)	0.006 (2)	0.008 (2)	−0.001 (2)
C26	0.017 (2)	0.031 (3)	0.024 (2)	0.0047 (19)	0.0048 (18)	−0.0068 (19)
C31	0.018 (2)	0.017 (2)	0.018 (2)	0.0047 (16)	0.0005 (16)	−0.0004 (16)
C32	0.030 (3)	0.021 (2)	0.015 (2)	0.0101 (19)	−0.0039 (18)	−0.0004 (17)
C33	0.037 (3)	0.028 (2)	0.015 (2)	0.004 (2)	−0.006 (2)	0.0019 (18)
C34	0.027 (3)	0.030 (3)	0.017 (2)	0.005 (2)	−0.0005 (19)	0.0075 (18)
C35	0.032 (3)	0.024 (2)	0.019 (2)	0.009 (2)	0.0018 (19)	0.0032 (18)
C36	0.033 (3)	0.016 (2)	0.015 (2)	0.0028 (18)	−0.0018 (18)	0.0008 (16)
B	0.041 (4)	0.054 (4)	0.030 (3)	0.001 (3)	0.009 (3)	0.004 (3)
F1	0.088 (3)	0.072 (3)	0.056 (3)	0.003 (3)	0.030 (2)	−0.003 (2)
F2	0.081 (3)	0.119 (4)	0.065 (3)	0.022 (3)	−0.009 (3)	−0.045 (3)
F3	0.071 (3)	0.138 (5)	0.082 (4)	0.032 (3)	−0.030 (3)	0.008 (3)
F4	0.087 (4)	0.099 (4)	0.122 (5)	0.009 (3)	0.010 (3)	0.066 (4)

Geometric parameters (Å, º)

Os—H1	1.70 (4)	C14—H14A	1.16 (8)
Os—H2	1.67 (5)	C14—H14B	1.06 (8)
Os—H3	1.66 (6)	C14—C15	1.523 (8)
Os—H4	1.69 (7)	C15—H15A	1.12 (7)
Os—C1	2.305 (5)	C15—H15B	1.18 (7)
Os—C2	2.294 (4)	C15—C16	1.535 (7)
Os—C3	2.247 (5)	C16—H16A	1.11 (8)
Os—C4	2.254 (5)	C16—H16B	1.11 (6)
Os—C5	2.270 (5)	C21—H21	1.13 (6)
Os—P	2.3670 (11)	C21—C22	1.540 (6)
C1—C2	1.436 (7)	C21—C26	1.537 (6)
C1—C5	1.433 (7)	C22—H22A	1.15 (7)
C1—C6	1.499 (8)	C22—H22B	1.07 (7)
C2—C3	1.447 (7)	C22—C23	1.536 (7)
C2—C7	1.498 (7)	C23—H23A	1.15 (6)
C3—C4	1.450 (7)	C23—H23B	1.17 (6)
C3—C8	1.493 (8)	C23—C24	1.530 (7)
C4—C5	1.440 (7)	C24—H24A	1.10 (6)
C4—C9	1.492 (8)	C24—H24B	1.21 (7)
C5—C10	1.493 (7)	C24—C25	1.524 (7)
C6—H6A	1.10 (9)	C25—H25A	1.08 (8)
C6—H6B	1.06 (8)	C25—H25B	1.11 (7)
C6—H6C	1.15 (8)	C25—C26	1.539 (7)
C8—H8A	1.17 (11)	C26—H26A	1.04 (6)
C8—H8B	1.14 (16)	C26—H26B	1.16 (6)
C8—H8C	1.14 (10)	C31—H31	1.18 (4)
C7—H7A	0.99 (9)	C31—C32	1.551 (6)
C7—H7B	1.00 (11)	C31—C36	1.540 (6)
C7—H7C	1.12 (11)	C32—H32A	1.12 (8)
C9—H9A	1.12 (8)	C32—H32B	1.10 (6)
C9—H9B	1.05 (8)	C32—C33	1.534 (6)
C9—H9C	1.18 (10)	C33—H33A	1.16 (6)
C10—H10A	1.12 (9)	C33—H33B	1.15 (7)
C10—H10B	1.13 (10)	C33—C34	1.529 (7)
C10—H10C	1.10 (8)	C34—H34A	1.08 (7)
P—C11	1.854 (5)	C34—H34B	1.04 (6)
P—C21	1.852 (5)	C34—C35	1.528 (7)
P—C31	1.872 (5)	C35—H35A	1.21 (7)
C11—H11	1.12 (6)	C35—H35B	1.19 (7)
C11—C12	1.542 (6)	C35—C36	1.540 (6)
C11—C16	1.531 (6)	C36—H36A	1.14 (6)
C12—H12A	1.17 (6)	C36—H36B	1.05 (6)
C12—H12B	1.11 (6)	B—F1	1.364 (8)
C12—C13	1.531 (7)	B—F2	1.374 (9)
C13—H13A	1.08 (7)	B—F3	1.366 (9)
C13—H13B	1.14 (10)	B—F4	1.379 (9)
C13—C14	1.524 (8)
H2—Os—H1	128 (3)	C12—C11—H11	106 (3)
H3—Os—H1	94 (3)	C16—C11—P	112.9 (3)
H3—Os—H2	67 (3)	C16—C11—H11	108 (3)
H4—Os—H1	55 (3)	C16—C11—C12	110.8 (4)
H4—Os—H2	106 (3)	H12A—C12—C11	113 (3)
H4—Os—H3	44 (3)	H12B—C12—C11	105 (3)
C1—Os—H1	110.7 (16)	H12B—C12—H12A	103 (4)
C1—Os—H2	105.3 (19)	C13—C12—C11	111.4 (4)
C1—Os—H3	151 (2)	C13—C12—H12A	113 (3)
C1—Os—H4	147 (3)	C13—C12—H12B	111 (3)
C2—Os—H1	145.3 (16)	H13A—C13—C12	112 (3)
C2—Os—H2	82.5 (19)	H13B—C13—C12	107 (5)
C2—Os—H3	116 (2)	H13B—C13—H13A	105 (6)
C2—Os—H4	141 (2)	C14—C13—C12	110.7 (5)
C2—Os—C1	36.40 (17)	C14—C13—H13A	107 (3)
C3—Os—H1	132.7 (16)	C14—C13—H13B	115 (5)
C3—Os—H2	97.5 (19)	H14A—C14—C13	108 (4)
C3—Os—H3	91 (2)	H14B—C14—C13	109 (5)
C3—Os—H4	104 (2)	H14B—C14—H14A	104 (6)
C3—Os—C1	61.78 (18)	C15—C14—C13	110.4 (5)
C3—Os—C2	37.14 (19)	C15—C14—H14A	113 (4)
C4—Os—H1	95.9 (16)	C15—C14—H14B	113 (4)
C4—Os—H2	135.0 (19)	H15A—C15—C14	114 (3)
C4—Os—H3	103 (2)	H15B—C15—C14	109 (3)
C4—Os—H4	89 (2)	H15B—C15—H15A	107 (5)
C4—Os—C1	61.71 (18)	C16—C15—C14	111.5 (5)
C4—Os—C2	61.87 (18)	C16—C15—H15A	109 (3)
C4—Os—C3	37.58 (19)	C16—C15—H15B	107 (3)
C5—Os—H1	85.0 (16)	C15—C16—C11	110.9 (4)
C5—Os—H2	141.1 (19)	H16A—C16—C11	112 (4)
C5—Os—H3	139 (2)	H16A—C16—C15	109 (4)
C5—Os—H4	111 (3)	H16B—C16—C11	109 (3)
C5—Os—C1	36.48 (17)	H16B—C16—C15	113 (3)
C5—Os—C2	61.00 (17)	H16B—C16—H16A	102 (5)
C5—Os—C3	62.01 (18)	H21—C21—P	103 (3)
C5—Os—C4	37.11 (18)	C22—C21—P	114.6 (3)
P—Os—H1	66.9 (16)	C22—C21—H21	106 (3)
P—Os—H2	67.0 (19)	C26—C21—P	115.5 (3)
P—Os—H3	95 (2)	C26—C21—H21	108 (3)
P—Os—H4	94 (2)	C26—C21—C22	109.7 (4)
P—Os—C1	107.04 (13)	H22A—C22—C21	112 (3)
P—Os—C2	123.20 (13)	H22B—C22—C21	113 (4)
P—Os—C3	158.88 (15)	H22B—C22—H22A	103 (5)
P—Os—C4	155.70 (14)	C23—C22—C21	111.5 (4)
P—Os—C5	120.90 (14)	C23—C22—H22A	108 (3)
C2—C1—Os	71.4 (3)	C23—C22—H22B	108 (4)
C5—C1—Os	70.4 (3)	H23A—C23—C22	109 (3)
C5—C1—C2	107.7 (4)	H23B—C23—C22	110 (3)
C6—C1—Os	130.6 (4)	H23B—C23—H23A	108 (4)
C6—C1—C2	126.2 (5)	C24—C23—C22	110.4 (4)
C6—C1—C5	125.5 (5)	C24—C23—H23A	108 (3)
C1—C2—Os	72.2 (3)	C24—C23—H23B	111 (3)
C3—C2—Os	69.7 (3)	H24A—C24—C23	111 (3)
C3—C2—C1	108.3 (4)	H24B—C24—C23	112 (3)
C7—C2—Os	131.0 (3)	H24B—C24—H24A	105 (5)
C7—C2—C1	126.5 (5)	C25—C24—C23	110.9 (4)
C7—C2—C3	124.5 (5)	C25—C24—H24A	107 (3)
C2—C3—Os	73.2 (3)	C25—C24—H24B	111 (3)
C4—C3—Os	71.5 (3)	H25A—C25—C24	111 (4)
C4—C3—C2	107.7 (4)	H25B—C25—C24	109 (4)
C8—C3—Os	126.6 (4)	H25B—C25—H25A	104 (5)
C8—C3—C2	126.6 (5)	C26—C25—C24	111.1 (4)
C8—C3—C4	125.3 (6)	C26—C25—H25A	111 (4)
C3—C4—Os	70.9 (3)	C26—C25—H25B	111 (4)
C5—C4—Os	72.1 (3)	C25—C26—C21	110.8 (4)
C5—C4—C3	107.3 (4)	H26A—C26—C21	111 (4)
C9—C4—Os	126.7 (4)	H26A—C26—C25	110 (4)
C9—C4—C3	126.9 (5)	H26B—C26—C21	106 (3)
C9—C4—C5	125.6 (5)	H26B—C26—C25	108 (3)
C1—C5—Os	73.1 (3)	H26B—C26—H26A	111 (5)
C4—C5—Os	70.8 (3)	H31—C31—P	112 (2)
C4—C5—C1	109.0 (4)	C32—C31—P	116.4 (3)
C10—C5—Os	130.5 (4)	C32—C31—H31	104 (2)
C10—C5—C1	126.1 (5)	C36—C31—P	113.1 (3)
C10—C5—C4	124.1 (5)	C36—C31—H31	100 (2)
H6A—C6—C1	107 (4)	C36—C31—C32	109.3 (4)
H6B—C6—C1	110 (4)	H32A—C32—C31	113 (4)
H6B—C6—H6A	108 (6)	H32B—C32—C31	107 (3)
H6C—C6—C1	108 (4)	H32B—C32—H32A	108 (5)
H6C—C6—H6A	105 (6)	C33—C32—C31	110.6 (4)
H6C—C6—H6B	118 (6)	C33—C32—H32A	108 (4)
H8A—C8—C3	113 (5)	C33—C32—H32B	110 (3)
H8B—C8—C3	115 (8)	H33A—C33—C32	114 (3)
H8B—C8—H8A	109 (9)	H33B—C33—C32	117 (4)
H8C—C8—C3	116 (5)	H33B—C33—H33A	108 (5)
H8C—C8—H8A	97 (7)	C34—C33—C32	111.2 (4)
H8C—C8—H8B	106 (8)	C34—C33—H33A	105 (3)
H7A—C7—C2	103 (5)	C34—C33—H33B	100 (3)
H7B—C7—C2	121 (6)	H34A—C34—C33	114 (3)
H7B—C7—H7A	97 (8)	H34B—C34—C33	112 (3)
H7C—C7—C2	111 (5)	H34B—C34—H34A	103 (5)
H7C—C7—H7A	130 (7)	C35—C34—C33	111.1 (4)
H7C—C7—H7B	97 (8)	C35—C34—H34A	106 (4)
H9A—C9—C4	108 (4)	C35—C34—H34B	110 (3)
H9B—C9—C4	113 (4)	H35A—C35—C34	114 (3)
H9B—C9—H9A	110 (6)	H35B—C35—C34	113 (4)
H9C—C9—C4	117 (5)	H35B—C35—H35A	103 (5)
H9C—C9—H9A	100 (6)	C36—C35—C34	110.5 (4)
H9C—C9—H9B	109 (6)	C36—C35—H35A	105 (3)
H10A—C10—C5	110 (5)	C36—C35—H35B	109 (4)
H10B—C10—C5	114 (5)	C35—C36—C31	111.8 (4)
H10B—C10—H10A	106 (7)	H36A—C36—C31	106 (3)
H10C—C10—C5	111 (4)	H36A—C36—C35	113 (3)
H10C—C10—H10A	109 (6)	H36B—C36—C31	114 (3)
H10C—C10—H10B	106 (6)	H36B—C36—C35	112 (3)
C11—P—Os	114.81 (15)	H36B—C36—H36A	99 (4)
C21—P—Os	112.92 (14)	F2—B—F1	108.7 (6)
C21—P—C11	103.9 (2)	F3—B—F1	112.3 (6)
C31—P—Os	111.69 (14)	F3—B—F2	111.1 (7)
C31—P—C11	102.7 (2)	F4—B—F1	107.9 (7)
C31—P—C21	110.1 (2)	F4—B—F2	108.8 (6)
H11—C11—P	106 (3)	F4—B—F3	107.9 (6)
C12—C11—P	112.3 (3)

(XAXMEP_HAR_NoMoRe_1)

Crystal data

C28H52OsP·BF4	V = 1457.79 (4) Å^3
Mr = 696.74	Z = 2
Triclinic, P1	F(000) = 702.711
a = 8.9295 (2) Å	Dx = 1.587 Mg m^−3
b = 9.7179 (1) Å	Mo Kα radiation, λ = 0.71073 Å
c = 17.1819 (1) Å	µ = 4.47 mm^−1
α = 94.114 (1)°	T = 199 K
β = 90.034 (1)°	0.3 × 0.1 × 0.04 mm
γ = 101.369 (1)°

Data collection

Absorption correction: integration	Rint = 0.033
Tmin = 0.529, Tmax = 0.844	θmax = 28.3°, θmin = 2.1°
9506 measured reflections	h = −11→11
6629 independent reflections	k = −12→12
5952 reflections with I ≥ 2u(I)	l = −22→13

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.033	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.081	w = 1/[σ^2(Fo^2) + (0.0208P)^2 + 6.6819P] where P = (Fo^2 + 2Fc^2)/3
S = 1.09	(Δ/σ)max = 0.001
6629 reflections	Δρmax = 1.36 e Å^−3
472 parameters	Δρmin = −1.50 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Os	0.22259 (2)	0.241116 (19)	0.197802 (10)	0.01843 (6)
H1	0.309 (9)	0.407 (7)	0.225 (4)	0.062359
H2	0.146 (8)	0.111 (7)	0.253 (4)	0.045750
H3	0.350 (10)	0.168 (9)	0.243 (4)	0.059676
H4	0.403 (8)	0.289 (11)	0.230 (5)	0.065392
C1	0.0491 (6)	0.2381 (5)	0.0980 (3)	0.0244 (10)
C2	0.0773 (6)	0.0986 (5)	0.1022 (3)	0.0247 (10)
C3	0.2379 (6)	0.1023 (5)	0.0888 (3)	0.0285 (11)
C4	0.3082 (6)	0.2455 (6)	0.0744 (3)	0.0283 (11)
C5	0.1909 (6)	0.3280 (5)	0.0810 (3)	0.0267 (10)
C6	−0.1040 (7)	0.2795 (7)	0.0988 (4)	0.0383 (13)
H6A	−0.141 (9)	0.277 (9)	0.037 (4)	0.058654
H6B	−0.096 (9)	0.385 (9)	0.125 (5)	0.065989
H6C	−0.190 (9)	0.194 (10)	0.126 (5)	0.069781
C8	0.3145 (9)	−0.0208 (7)	0.0812 (4)	0.0499 (17)
H8A	0.435 (11)	0.002 (9)	0.104 (6)	0.094093
H8B	0.326 (10)	−0.067 (8)	0.022 (5)	0.073508
H8C	0.271 (12)	−0.108 (8)	0.119 (5)	0.082772
C7	−0.0401 (8)	−0.0335 (6)	0.1067 (3)	0.0396 (14)
H7A	0.018 (11)	−0.098 (8)	0.132 (6)	0.088265
H7B	−0.079 (11)	−0.096 (11)	0.052 (5)	0.100239
H7C	−0.146 (9)	−0.011 (8)	0.125 (5)	0.066411
C9	0.4682 (7)	0.2966 (8)	0.0496 (4)	0.0468 (16)
H9A	0.470 (8)	0.289 (9)	−0.016 (4)	0.063881
H9B	0.548 (9)	0.234 (9)	0.071 (5)	0.069451
H9C	0.517 (8)	0.411 (9)	0.065 (4)	0.059874
C10	0.2108 (8)	0.4765 (6)	0.0592 (3)	0.0397 (14)
H10A	0.211 (10)	0.477 (8)	−0.006 (4)	0.060153
H10B	0.319 (9)	0.546 (8)	0.082 (5)	0.064075
H10C	0.117 (10)	0.526 (7)	0.083 (5)	0.062123
P	0.11844 (12)	0.33050 (11)	0.31288 (6)	0.0154 (2)
C11	0.1601 (5)	0.5251 (5)	0.3290 (3)	0.0197 (9)
H11	0.112 (7)	0.549 (6)	0.387 (4)	0.035993
C12	0.3329 (5)	0.5861 (5)	0.3363 (3)	0.0253 (10)
H12A	0.394 (8)	0.532 (7)	0.380 (4)	0.051849
H12B	0.384 (7)	0.558 (7)	0.280 (4)	0.047302
C13	0.3645 (7)	0.7462 (5)	0.3527 (4)	0.0349 (13)
H13A	0.318 (10)	0.776 (8)	0.407 (5)	0.068377
H13B	0.495 (8)	0.791 (8)	0.359 (5)	0.064022
C14	0.2916 (7)	0.8154 (6)	0.2897 (4)	0.0372 (13)
H14A	0.351 (9)	0.799 (9)	0.232 (5)	0.067336
H14B	0.318 (9)	0.927 (8)	0.302 (6)	0.084782
C15	0.1203 (6)	0.7571 (5)	0.2840 (4)	0.0356 (13)
H15A	0.059 (9)	0.808 (8)	0.240 (5)	0.076469
H15B	0.063 (9)	0.782 (7)	0.341 (5)	0.068134
C16	0.0857 (6)	0.5968 (5)	0.2671 (3)	0.0267 (10)
H16A	−0.040 (7)	0.560 (7)	0.264 (4)	0.042974
H16B	0.123 (8)	0.564 (7)	0.209 (4)	0.046466
C21	−0.0928 (5)	0.2830 (4)	0.3143 (3)	0.0178 (8)
H21	−0.127 (7)	0.340 (7)	0.264 (4)	0.035316
C22	−0.1595 (5)	0.1268 (5)	0.2915 (3)	0.0219 (9)
H22A	−0.112 (7)	0.089 (7)	0.234 (4)	0.047450
H22B	−0.132 (7)	0.058 (6)	0.334 (4)	0.042904
C23	−0.3342 (6)	0.1000 (5)	0.2820 (3)	0.0251 (10)
H23A	−0.366 (8)	0.163 (8)	0.232 (4)	0.045642
H23B	−0.382 (7)	−0.018 (7)	0.266 (4)	0.046199
C24	−0.4069 (5)	0.1489 (5)	0.3568 (3)	0.0247 (10)
H24A	−0.532 (7)	0.140 (7)	0.348 (4)	0.045541
H24B	−0.392 (8)	0.075 (7)	0.409 (4)	0.046267
C25	−0.3420 (6)	0.3036 (5)	0.3799 (3)	0.0265 (10)
H25A	−0.392 (8)	0.335 (8)	0.437 (4)	0.056304
H25B	−0.378 (8)	0.366 (7)	0.333 (4)	0.047854
C26	−0.1671 (5)	0.3303 (5)	0.3896 (3)	0.0245 (10)
H26A	−0.125 (7)	0.435 (7)	0.407 (4)	0.045760
H26B	−0.139 (7)	0.260 (7)	0.437 (4)	0.043631
C31	0.2016 (5)	0.2743 (4)	0.4026 (3)	0.0173 (8)
H31	0.334 (7)	0.279 (7)	0.394 (4)	0.033658
C32	0.1878 (6)	0.3638 (5)	0.4797 (3)	0.0214 (9)
H32A	0.233 (8)	0.479 (6)	0.476 (4)	0.040894
H32B	0.065 (7)	0.350 (7)	0.494 (4)	0.038467
C33	0.2766 (6)	0.3167 (5)	0.5459 (3)	0.0270 (10)
H33A	0.409 (8)	0.330 (7)	0.532 (4)	0.046477
H33B	0.263 (8)	0.367 (7)	0.606 (4)	0.044469
C34	0.2206 (6)	0.1605 (5)	0.5576 (3)	0.0247 (10)
H34A	0.285 (9)	0.120 (7)	0.604 (4)	0.055121
H34B	0.109 (8)	0.141 (7)	0.578 (4)	0.043948
C35	0.2317 (6)	0.0699 (5)	0.4823 (3)	0.0244 (10)
H35A	0.177 (9)	−0.052 (7)	0.488 (4)	0.053883
H35B	0.361 (9)	0.074 (7)	0.466 (4)	0.055013
C36	0.1441 (6)	0.1176 (5)	0.4153 (3)	0.0211 (9)
H36A	0.015 (7)	0.102 (7)	0.426 (4)	0.039601
H36B	0.141 (8)	0.051 (6)	0.362 (4)	0.046760
B	0.3092 (8)	0.3654 (8)	0.8135 (4)	0.0419 (16)
F1	0.1955 (6)	0.3610 (5)	0.8668 (3)	0.0738 (14)
F2	0.2643 (6)	0.2598 (6)	0.7558 (3)	0.0907 (17)
F3	0.4451 (6)	0.3551 (7)	0.8467 (3)	0.0954 (18)
F4	0.3291 (7)	0.4933 (6)	0.7811 (4)	0.102 (2)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Os	0.01892 (9)	0.02358 (10)	0.01307 (9)	0.00521 (6)	0.00143 (6)	0.00047 (6)
H1	0.074000	0.047000	0.049000	−0.023000	0.025000	−0.015000
H2	0.064000	0.036000	0.034000	0.000000	0.014000	0.008000
H3	0.081000	0.076000	0.038000	0.053000	−0.005000	0.008000
H4	0.029000	0.116000	0.048000	0.012000	−0.006000	−0.009000
C1	0.024 (2)	0.030 (2)	0.019 (2)	0.004 (2)	−0.0004 (18)	0.0039 (18)
C2	0.032 (3)	0.028 (2)	0.013 (2)	0.004 (2)	−0.0047 (18)	−0.0011 (17)
C3	0.041 (3)	0.029 (3)	0.018 (2)	0.013 (2)	−0.001 (2)	−0.0022 (18)
C4	0.030 (3)	0.040 (3)	0.016 (2)	0.009 (2)	0.0085 (19)	0.0032 (19)
C5	0.030 (3)	0.032 (3)	0.017 (2)	0.002 (2)	0.0051 (19)	0.0070 (18)
C6	0.028 (3)	0.056 (4)	0.033 (3)	0.011 (3)	−0.008 (2)	0.009 (3)
H6A	0.057000	0.088000	0.039000	0.032000	−0.013000	0.010000
H6B	0.069000	0.070000	0.069000	0.045000	−0.013000	−0.014000
H6C	0.039000	0.110000	0.070000	0.028000	0.016000	0.035000
C8	0.074 (5)	0.049 (4)	0.038 (3)	0.041 (4)	0.009 (3)	−0.002 (3)
H8A	0.087000	0.075000	0.130000	0.055000	−0.048000	−0.035000
H8B	0.104000	0.061000	0.059000	0.036000	−0.002000	−0.027000
H8C	0.134000	0.039000	0.083000	0.032000	0.006000	0.015000
C7	0.049 (4)	0.034 (3)	0.029 (3)	−0.008 (3)	−0.007 (3)	0.002 (2)
H7A	0.096000	0.036000	0.128000	−0.003000	0.036000	0.018000
H7B	0.098000	0.127000	0.042000	−0.066000	−0.033000	0.024000
H7C	0.054000	0.073000	0.055000	−0.022000	0.021000	−0.016000
C9	0.035 (3)	0.069 (5)	0.036 (3)	0.009 (3)	0.013 (3)	0.004 (3)
H9A	0.046000	0.113000	0.026000	0.001000	0.011000	0.001000
H9B	0.045000	0.103000	0.068000	0.034000	0.010000	0.004000
H9C	0.039000	0.083000	0.047000	−0.011000	0.005000	−0.003000
C10	0.057 (4)	0.031 (3)	0.030 (3)	0.002 (3)	0.006 (3)	0.013 (2)
H10A	0.095000	0.050000	0.033000	0.003000	0.002000	0.018000
H10B	0.072000	0.047000	0.063000	−0.017000	−0.006000	0.015000
H10C	0.094000	0.038000	0.059000	0.022000	0.002000	0.010000
P	0.0155 (5)	0.0160 (5)	0.0147 (5)	0.0033 (4)	0.0015 (4)	0.0014 (4)
C11	0.020 (2)	0.019 (2)	0.020 (2)	0.0018 (17)	0.0017 (17)	0.0018 (16)
H11	0.050000	0.031000	0.026000	0.006000	0.006000	0.001000
C12	0.020 (2)	0.017 (2)	0.038 (3)	0.0016 (17)	−0.002 (2)	0.0040 (19)
H12A	0.042000	0.048000	0.064000	−0.003000	−0.019000	0.027000
H12B	0.035000	0.049000	0.054000	0.003000	0.006000	−0.008000
C13	0.035 (3)	0.017 (2)	0.050 (3)	−0.001 (2)	−0.011 (3)	0.000 (2)
H13A	0.091000	0.050000	0.054000	−0.005000	−0.011000	−0.012000
H13B	0.042000	0.054000	0.089000	−0.014000	−0.014000	0.023000
C14	0.032 (3)	0.020 (2)	0.060 (4)	0.001 (2)	−0.001 (3)	0.012 (2)
H14A	0.059000	0.088000	0.057000	0.008000	0.013000	0.037000
H14B	0.070000	0.039000	0.141000	−0.011000	−0.007000	0.038000
C15	0.029 (3)	0.022 (2)	0.056 (4)	0.004 (2)	−0.007 (3)	0.010 (2)
H15A	0.069000	0.056000	0.111000	0.012000	−0.008000	0.052000
H15B	0.074000	0.039000	0.090000	0.013000	0.010000	−0.010000
C16	0.032 (3)	0.023 (2)	0.026 (2)	0.007 (2)	−0.009 (2)	0.0015 (19)
H16A	0.035000	0.042000	0.055000	0.011000	0.000000	0.015000
H16B	0.060000	0.056000	0.026000	0.016000	0.001000	0.008000
C21	0.019 (2)	0.016 (2)	0.018 (2)	0.0030 (16)	0.0035 (16)	−0.0016 (16)
H21	0.033000	0.041000	0.034000	0.009000	−0.001000	0.012000
C22	0.018 (2)	0.020 (2)	0.026 (2)	0.0025 (17)	0.0017 (18)	−0.0038 (18)
H22A	0.036000	0.057000	0.044000	0.005000	0.008000	−0.021000
H22B	0.037000	0.034000	0.058000	0.005000	−0.002000	0.011000
C23	0.023 (2)	0.022 (2)	0.028 (2)	−0.0016 (18)	0.0008 (19)	−0.0031 (19)
H23A	0.039000	0.066000	0.033000	0.010000	−0.001000	0.012000
H23B	0.033000	0.046000	0.053000	−0.003000	0.001000	−0.011000
C24	0.015 (2)	0.029 (2)	0.029 (3)	0.0013 (18)	0.0048 (18)	0.0027 (19)
H24A	0.025000	0.055000	0.057000	0.011000	0.003000	−0.002000
H24B	0.047000	0.054000	0.038000	0.007000	0.009000	0.013000
C25	0.022 (2)	0.028 (2)	0.029 (3)	0.0058 (19)	0.007 (2)	−0.001 (2)
H25A	0.040000	0.070000	0.056000	0.014000	0.011000	−0.024000
H25B	0.039000	0.040000	0.067000	0.013000	−0.002000	0.006000
C26	0.017 (2)	0.031 (3)	0.025 (2)	0.0046 (19)	0.0047 (18)	−0.0071 (19)
H26A	0.037000	0.041000	0.055000	0.005000	0.002000	−0.018000
H26B	0.042000	0.062000	0.028000	0.012000	0.003000	0.006000
C31	0.017 (2)	0.017 (2)	0.018 (2)	0.0048 (16)	0.0008 (16)	−0.0003 (16)
H31	0.029000	0.038000	0.036000	0.010000	0.004000	0.007000
C32	0.030 (2)	0.022 (2)	0.015 (2)	0.0103 (19)	−0.0040 (18)	−0.0005 (16)
H32A	0.061000	0.024000	0.033000	−0.004000	−0.008000	0.005000
H32B	0.043000	0.047000	0.029000	0.019000	0.000000	−0.001000
C33	0.038 (3)	0.028 (2)	0.014 (2)	0.004 (2)	−0.006 (2)	0.0018 (18)
H33A	0.036000	0.051000	0.053000	0.006000	−0.007000	0.015000
H33B	0.063000	0.039000	0.028000	0.002000	−0.011000	0.002000
C34	0.027 (3)	0.030 (2)	0.017 (2)	0.004 (2)	−0.0002 (18)	0.0073 (18)
H34A	0.074000	0.046000	0.045000	0.004000	−0.017000	0.023000
H34B	0.047000	0.045000	0.036000	−0.001000	0.007000	0.005000
C35	0.032 (3)	0.024 (2)	0.019 (2)	0.009 (2)	0.0018 (19)	0.0033 (18)
H35A	0.086000	0.024000	0.048000	−0.001000	0.005000	0.011000
H35B	0.064000	0.049000	0.061000	0.029000	0.011000	0.015000
C36	0.032 (3)	0.016 (2)	0.015 (2)	0.0026 (18)	−0.0017 (18)	0.0015 (16)
H36A	0.035000	0.043000	0.037000	−0.003000	0.003000	0.007000
H36B	0.075000	0.029000	0.031000	0.000000	0.006000	−0.005000
B	0.040 (4)	0.054 (4)	0.029 (3)	0.002 (3)	0.009 (3)	0.004 (3)
F1	0.087 (3)	0.073 (3)	0.055 (3)	0.003 (3)	0.030 (2)	−0.003 (2)
F2	0.081 (3)	0.119 (4)	0.065 (3)	0.022 (3)	−0.010 (3)	−0.045 (3)
F3	0.071 (3)	0.137 (5)	0.082 (4)	0.031 (3)	−0.031 (3)	0.008 (3)
F4	0.087 (4)	0.099 (4)	0.124 (5)	0.009 (3)	0.010 (4)	0.067 (4)

Geometric parameters (Å, º)

Os—H1	1.68 (7)	C14—H14A	1.14 (8)
Os—H2	1.67 (6)	C14—H14B	1.07 (8)
Os—H3	1.68 (7)	C14—C15	1.523 (8)
Os—H4	1.66 (7)	C15—H15A	1.13 (8)
Os—C1	2.305 (5)	C15—H15B	1.14 (8)
Os—C2	2.293 (4)	C15—C16	1.534 (7)
Os—C3	2.248 (5)	C16—H16A	1.11 (6)
Os—C4	2.254 (5)	C16—H16B	1.10 (7)
Os—C5	2.270 (5)	C21—H21	1.14 (6)
Os—P	2.3671 (11)	C21—C22	1.540 (6)
C1—C2	1.434 (7)	C21—C26	1.536 (6)
C1—C5	1.432 (7)	C22—H22A	1.14 (6)
C1—C6	1.499 (7)	C22—H22B	1.08 (6)
C2—C3	1.446 (7)	C22—C23	1.537 (6)
C2—C7	1.496 (7)	C23—H23A	1.15 (7)
C3—C4	1.448 (7)	C23—H23B	1.16 (6)
C3—C8	1.489 (8)	C23—C24	1.528 (7)
C4—C5	1.440 (7)	C24—H24A	1.12 (6)
C4—C9	1.490 (8)	C24—H24B	1.21 (7)
C5—C10	1.493 (7)	C24—C25	1.525 (7)
C6—H6A	1.10 (7)	C25—H25A	1.12 (7)
C6—H6B	1.08 (8)	C25—H25B	1.12 (7)
C6—H6C	1.14 (8)	C25—C26	1.539 (7)
C8—H8A	1.12 (9)	C26—H26A	1.04 (6)
C8—H8B	1.09 (8)	C26—H26B	1.16 (7)
C8—H8C	1.12 (9)	C31—H31	1.18 (6)
C7—H7A	1.00 (10)	C31—C32	1.550 (6)
C7—H7B	1.10 (9)	C31—C36	1.539 (6)
C7—H7C	1.06 (8)	C32—H32A	1.12 (6)
C9—H9A	1.12 (7)	C32—H32B	1.10 (6)
C9—H9B	1.11 (8)	C32—C33	1.533 (6)
C9—H9C	1.13 (8)	C33—H33A	1.18 (7)
C10—H10A	1.11 (7)	C33—H33B	1.13 (7)
C10—H10B	1.12 (7)	C33—C34	1.529 (7)
C10—H10C	1.11 (8)	C34—H34A	1.12 (7)
P—C11	1.854 (5)	C34—H34B	1.04 (6)
P—C21	1.852 (4)	C34—C35	1.526 (7)
P—C31	1.872 (5)	C35—H35A	1.20 (6)
C11—H11	1.11 (6)	C35—H35B	1.18 (7)
C11—C12	1.542 (6)	C35—C36	1.541 (6)
C11—C16	1.532 (6)	C36—H36A	1.15 (6)
C12—H12A	1.15 (7)	C36—H36B	1.08 (6)
C12—H12B	1.11 (7)	B—F1	1.364 (8)
C12—C13	1.531 (7)	B—F2	1.374 (8)
C13—H13A	1.07 (8)	B—F3	1.365 (9)
C13—H13B	1.16 (7)	B—F4	1.378 (9)
C13—C14	1.525 (8)
H2—Os—H1	129 (4)	C12—C11—H11	106 (3)
H3—Os—H1	95 (4)	C16—C11—P	112.8 (3)
H3—Os—H2	65 (4)	C16—C11—H11	109 (3)
H4—Os—H1	55 (4)	C16—C11—C12	110.8 (4)
H4—Os—H2	104 (4)	H12A—C12—C11	113 (3)
H4—Os—H3	43 (4)	H12B—C12—C11	107 (3)
C1—Os—H1	110 (3)	H12B—C12—H12A	103 (5)
C1—Os—H2	106 (2)	C13—C12—C11	111.4 (4)
C1—Os—H3	151 (3)	C13—C12—H12A	112 (4)
C1—Os—H4	148 (3)	C13—C12—H12B	110 (4)
C2—Os—H1	145 (3)	H13A—C13—C12	111 (4)
C2—Os—H2	82 (2)	H13B—C13—C12	111 (4)
C2—Os—H3	115 (3)	H13B—C13—H13A	105 (6)
C2—Os—H4	141 (3)	C14—C13—C12	110.8 (5)
C2—Os—C1	36.34 (17)	C14—C13—H13A	107 (5)
C3—Os—H1	132 (2)	C14—C13—H13B	112 (4)
C3—Os—H2	96 (2)	H14A—C14—C13	109 (4)
C3—Os—H3	91 (3)	H14B—C14—C13	109 (5)
C3—Os—H4	104 (3)	H14B—C14—H14A	104 (6)
C3—Os—C1	61.72 (18)	C15—C14—C13	110.4 (5)
C3—Os—C2	37.12 (18)	C15—C14—H14A	112 (4)
C4—Os—H1	95 (2)	C15—C14—H14B	113 (5)
C4—Os—H2	133 (2)	H15A—C15—C14	114 (4)
C4—Os—H3	103 (3)	H15B—C15—C14	110 (4)
C4—Os—H4	89 (3)	H15B—C15—H15A	103 (6)
C4—Os—C1	61.67 (18)	C16—C15—C14	111.5 (5)
C4—Os—C2	61.80 (18)	C16—C15—H15A	110 (4)
C4—Os—C3	37.51 (19)	C16—C15—H15B	108 (4)
C5—Os—H1	85 (3)	C15—C16—C11	110.9 (4)
C5—Os—H2	142 (2)	H16A—C16—C11	112 (3)
C5—Os—H3	139 (3)	H16A—C16—C15	108 (3)
C5—Os—H4	111 (3)	H16B—C16—C11	110 (4)
C5—Os—C1	36.48 (17)	H16B—C16—C15	113 (4)
C5—Os—C2	60.94 (17)	H16B—C16—H16A	103 (5)
C5—Os—C3	61.96 (18)	H21—C21—P	102 (3)
C5—Os—C4	37.10 (18)	C22—C21—P	114.5 (3)
P—Os—H1	68 (2)	C22—C21—H21	104 (3)
P—Os—H2	69 (2)	C26—C21—P	115.5 (3)
P—Os—H3	96 (3)	C26—C21—H21	110 (3)
P—Os—H4	94 (3)	C26—C21—C22	109.8 (4)
P—Os—C1	107.09 (12)	H22A—C22—C21	112 (3)
P—Os—C2	123.24 (13)	H22B—C22—C21	112 (3)
P—Os—C3	158.90 (14)	H22B—C22—H22A	106 (5)
P—Os—C4	155.74 (14)	C23—C22—C21	111.4 (4)
P—Os—C5	120.93 (13)	C23—C22—H22A	107 (3)
C2—C1—Os	71.4 (3)	C23—C22—H22B	108 (3)
C5—C1—Os	70.5 (3)	H23A—C23—C22	110 (3)
C5—C1—C2	107.7 (4)	H23B—C23—C22	110 (3)
C6—C1—Os	130.5 (4)	H23B—C23—H23A	108 (5)
C6—C1—C2	126.4 (5)	C24—C23—C22	110.5 (4)
C6—C1—C5	125.3 (5)	C24—C23—H23A	108 (4)
C1—C2—Os	72.3 (3)	C24—C23—H23B	110 (3)
C3—C2—Os	69.7 (3)	H24A—C24—C23	110 (4)
C3—C2—C1	108.4 (4)	H24B—C24—C23	111 (3)
C7—C2—Os	131.1 (3)	H24B—C24—H24A	107 (5)
C7—C2—C1	126.6 (5)	C25—C24—C23	111.0 (4)
C7—C2—C3	124.3 (5)	C25—C24—H24A	106 (4)
C2—C3—Os	73.2 (3)	C25—C24—H24B	112 (3)
C4—C3—Os	71.5 (3)	H25A—C25—C24	109 (4)
C4—C3—C2	107.6 (4)	H25B—C25—C24	107 (4)
C8—C3—Os	126.6 (4)	H25B—C25—H25A	109 (5)
C8—C3—C2	126.5 (5)	C26—C25—C24	111.0 (4)
C8—C3—C4	125.4 (5)	C26—C25—H25A	109 (4)
C3—C4—Os	71.0 (3)	C26—C25—H25B	112 (4)
C5—C4—Os	72.1 (3)	C25—C26—C21	110.8 (4)
C5—C4—C3	107.3 (4)	H26A—C26—C21	112 (4)
C9—C4—Os	126.8 (4)	H26A—C26—C25	110 (4)
C9—C4—C3	126.8 (5)	H26B—C26—C21	106 (3)
C9—C4—C5	125.7 (5)	H26B—C26—C25	108 (3)
C1—C5—Os	73.1 (3)	H26B—C26—H26A	110 (5)
C4—C5—Os	70.8 (3)	H31—C31—P	109 (3)
C4—C5—C1	108.9 (4)	C32—C31—P	116.4 (3)
C10—C5—Os	130.5 (4)	C32—C31—H31	106 (3)
C10—C5—C1	126.0 (5)	C36—C31—P	113.1 (3)
C10—C5—C4	124.2 (5)	C36—C31—H31	102 (3)
H6A—C6—C1	107 (4)	C36—C31—C32	109.3 (4)
H6B—C6—C1	111 (4)	H32A—C32—C31	113 (3)
H6B—C6—H6A	109 (6)	H32B—C32—C31	108 (3)
H6C—C6—C1	109 (4)	H32B—C32—H32A	108 (5)
H6C—C6—H6A	106 (6)	C33—C32—C31	110.6 (4)
H6C—C6—H6B	116 (6)	C33—C32—H32A	107 (3)
H8A—C8—C3	114 (4)	C33—C32—H32B	110 (3)
H8B—C8—C3	117 (5)	H33A—C33—C32	112 (3)
H8B—C8—H8A	103 (7)	H33B—C33—C32	116 (4)
H8C—C8—C3	116 (5)	H33B—C33—H33A	109 (5)
H8C—C8—H8A	96 (7)	C34—C33—C32	111.3 (4)
H8C—C8—H8B	108 (6)	C34—C33—H33A	106 (3)
H7A—C7—C2	103 (5)	C34—C33—H33B	102 (3)
H7B—C7—C2	118 (4)	H34A—C34—C33	114 (4)
H7B—C7—H7A	101 (8)	H34B—C34—C33	111 (4)
H7C—C7—C2	111 (4)	H34B—C34—H34A	103 (5)
H7C—C7—H7A	126 (7)	C35—C34—C33	111.1 (4)
H7C—C7—H7B	98 (7)	C35—C34—H34A	107 (4)
H9A—C9—C4	108 (4)	C35—C34—H34B	110 (4)
H9B—C9—C4	112 (4)	H35A—C35—C34	112 (3)
H9B—C9—H9A	108 (6)	H35B—C35—C34	110 (4)
H9C—C9—C4	116 (4)	H35B—C35—H35A	106 (5)
H9C—C9—H9A	103 (6)	C36—C35—C34	110.6 (4)
H9C—C9—H9B	108 (6)	C36—C35—H35A	106 (4)
H10A—C10—C5	109 (4)	C36—C35—H35B	111 (4)
H10B—C10—C5	114 (4)	C35—C36—C31	111.7 (4)
H10B—C10—H10A	107 (6)	H36A—C36—C31	107 (3)
H10C—C10—C5	110 (4)	H36A—C36—C35	112 (3)
H10C—C10—H10A	110 (6)	H36B—C36—C31	112 (3)
H10C—C10—H10B	106 (6)	H36B—C36—C35	113 (4)
C11—P—Os	114.82 (15)	H36B—C36—H36A	99 (5)
C21—P—Os	112.93 (14)	F2—B—F1	108.7 (6)
C21—P—C11	103.9 (2)	F3—B—F1	112.4 (6)
C31—P—Os	111.70 (14)	F3—B—F2	111.1 (7)
C31—P—C11	102.7 (2)	F4—B—F1	107.9 (6)
C31—P—C21	110.1 (2)	F4—B—F2	108.9 (6)
H11—C11—P	106 (3)	F4—B—F3	107.8 (6)
C12—C11—P	112.3 (3)
Os—C1—C2—C3	−60.7 (3)	C1—C5—C4—C9	173.6 (4)
Os—C1—C2—C7	128.4 (3)	C2—C3—C4—C5	1.4 (4)
Os—C1—C5—C4	62.1 (3)	C2—C3—C4—C9	−173.1 (4)
Os—C1—C5—C10	−128.1 (3)	C3—C4—C5—C10	−170.9 (4)
Os—C2—C1—C5	61.4 (3)	P—C11—C12—C13	−177.8 (4)
Os—C2—C1—C6	−127.1 (3)	P—C11—C16—C15	178.7 (4)
Os—C2—C3—C4	−63.6 (3)	P—C21—C22—C23	−171.4 (3)
Os—C2—C3—C8	123.4 (4)	P—C21—C26—C25	172.1 (4)
Os—C3—C2—C1	62.3 (3)	P—C31—C32—C33	−173.4 (4)
Os—C3—C2—C7	−126.6 (3)	P—C31—C36—C35	171.7 (3)
Os—C3—C4—C5	−63.3 (3)	C11—C12—C13—C14	−56.4 (5)
Os—C3—C4—C9	122.2 (4)	C11—C16—C15—C14	56.2 (5)
Os—C4—C3—C2	64.7 (3)	C12—C13—C14—C15	57.2 (5)
Os—C4—C3—C8	−122.2 (4)	C13—C14—C15—C16	−57.4 (5)
Os—C4—C5—C1	−63.6 (3)	C21—C22—C23—C24	−56.8 (4)
Os—C4—C5—C10	126.5 (3)	C21—C26—C25—C24	57.2 (4)
Os—C5—C1—C2	−62.1 (3)	C22—C23—C24—C25	56.4 (4)
Os—C5—C1—C6	126.4 (3)	C23—C24—C25—C26	−56.8 (5)
Os—C5—C4—C3	62.7 (3)	C31—C32—C33—C34	−57.4 (4)
Os—C5—C4—C9	−122.8 (4)	C31—C36—C35—C34	56.5 (4)
C1—C2—C3—C4	−1.3 (4)	C32—C33—C34—C35	56.7 (5)
C1—C2—C3—C8	−174.3 (4)	C33—C34—C35—C36	−55.6 (4)
C1—C5—C4—C3	−0.9 (4)

(XAXMEP_HAR_NoMoRe)

Crystal data

C28H52OsP·BF4	V = 1457.79 (4) Å^3
Mr = 696.74	Z = 2
Triclinic, P1	F(000) = 702.711
a = 8.9295 (2) Å	Dx = 1.587 Mg m^−3
b = 9.7179 (1) Å	Mo Kα radiation, λ = 0.71073 Å
c = 17.1819 (1) Å	µ = 4.47 mm^−1
α = 94.114 (1)°	T = 199 K
β = 90.034 (1)°	0.3 × 0.1 × 0.04 mm
γ = 101.369 (1)°

Data collection

Absorption correction: integration	Rint = 0.033
Tmin = 0.529, Tmax = 0.844	θmax = 28.3°, θmin = 2.1°
9506 measured reflections	h = −11→11
6629 independent reflections	k = −12→12
5952 reflections with I ≥ 2u(I)	l = −22→13

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.033	Only H-atom coordinates refined
wR(F^2) = 0.081	w = 1/[σ^2(Fo^2) + (0.0209P)^2 + 6.6628P] where P = (Fo^2 + 2Fc^2)/3
S = 1.09	(Δ/σ)max = 0.001
6629 reflections	Δρmax = 1.36 e Å^−3
472 parameters	Δρmin = −1.50 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Os	0.22259 (2)	0.241116 (19)	0.197802 (10)	0.01843 (6)
H1	0.309 (9)	0.407 (7)	0.225 (4)	0.060796
H2	0.146 (8)	0.111 (7)	0.253 (4)	0.046432
H3	0.350 (10)	0.167 (9)	0.243 (4)	0.059811
H4	0.402 (8)	0.289 (11)	0.230 (5)	0.064993
C1	0.0491 (6)	0.2381 (5)	0.0980 (3)	0.0244 (10)
C2	0.0773 (6)	0.0986 (5)	0.1022 (3)	0.0246 (10)
C3	0.2379 (6)	0.1023 (5)	0.0889 (3)	0.0285 (11)
C4	0.3082 (6)	0.2455 (6)	0.0744 (3)	0.0283 (11)
C5	0.1909 (6)	0.3280 (5)	0.0810 (3)	0.0267 (10)
C6	−0.1040 (7)	0.2795 (7)	0.0988 (4)	0.0383 (13)
H6A	−0.141 (9)	0.277 (9)	0.037 (5)	0.063748
H6B	−0.096 (9)	0.385 (9)	0.125 (5)	0.069079
H6C	−0.190 (9)	0.194 (10)	0.126 (5)	0.074737
C8	0.3146 (9)	−0.0209 (7)	0.0812 (4)	0.0498 (17)
H8A	0.435 (11)	0.003 (10)	0.104 (7)	0.106274
H8B	0.325 (12)	−0.068 (9)	0.022 (5)	0.090756
H8C	0.272 (12)	−0.108 (9)	0.120 (6)	0.091844
C7	−0.0401 (8)	−0.0335 (6)	0.1067 (3)	0.0396 (14)
H7A	0.018 (11)	−0.098 (8)	0.131 (7)	0.098508
H7B	−0.080 (12)	−0.095 (11)	0.052 (5)	0.111988
H7C	−0.146 (9)	−0.012 (9)	0.126 (5)	0.074813
C9	0.4682 (7)	0.2966 (8)	0.0496 (4)	0.0469 (16)
H9A	0.470 (9)	0.289 (9)	−0.015 (4)	0.065746
H9B	0.548 (9)	0.233 (9)	0.071 (5)	0.074005
H9C	0.517 (8)	0.411 (9)	0.065 (5)	0.060420
C10	0.2108 (8)	0.4765 (6)	0.0593 (3)	0.0397 (14)
H10A	0.211 (10)	0.477 (8)	−0.005 (4)	0.060803
H10B	0.319 (9)	0.546 (8)	0.082 (5)	0.064583
H10C	0.117 (10)	0.526 (7)	0.083 (5)	0.062644
P	0.11844 (12)	0.33050 (11)	0.31287 (6)	0.0154 (2)
C11	0.1601 (5)	0.5251 (5)	0.3290 (3)	0.0197 (9)
H11	0.112 (7)	0.548 (6)	0.387 (4)	0.036130
C12	0.3329 (5)	0.5861 (5)	0.3363 (3)	0.0253 (10)
H12A	0.394 (8)	0.532 (7)	0.380 (4)	0.053801
H12B	0.384 (7)	0.558 (7)	0.280 (4)	0.048507
C13	0.3645 (7)	0.7462 (5)	0.3527 (4)	0.0349 (13)
H13A	0.318 (10)	0.776 (8)	0.407 (5)	0.068587
H13B	0.495 (8)	0.791 (8)	0.359 (5)	0.064220
C14	0.2916 (7)	0.8154 (6)	0.2897 (4)	0.0373 (13)
H14A	0.351 (9)	0.799 (9)	0.232 (5)	0.067289
H14B	0.318 (9)	0.927 (8)	0.302 (6)	0.084723
C15	0.1203 (6)	0.7571 (5)	0.2840 (4)	0.0356 (13)
H15A	0.059 (9)	0.808 (8)	0.240 (5)	0.077378
H15B	0.063 (9)	0.782 (8)	0.341 (5)	0.068943
C16	0.0857 (6)	0.5968 (5)	0.2671 (3)	0.0267 (10)
H16A	−0.040 (7)	0.560 (7)	0.264 (4)	0.043746
H16B	0.122 (8)	0.564 (7)	0.209 (4)	0.047162
C21	−0.0928 (5)	0.2830 (4)	0.3143 (3)	0.0178 (8)
H21	−0.127 (7)	0.340 (7)	0.264 (4)	0.035453
C22	−0.1595 (5)	0.1268 (5)	0.2915 (3)	0.0219 (9)
H22A	−0.112 (7)	0.089 (7)	0.234 (4)	0.047834
H22B	−0.132 (7)	0.058 (6)	0.334 (4)	0.043239
C23	−0.3342 (6)	0.1000 (5)	0.2820 (3)	0.0251 (10)
H23A	−0.366 (8)	0.163 (8)	0.232 (4)	0.045480
H23B	−0.383 (7)	−0.018 (7)	0.266 (4)	0.045886
C24	−0.4069 (5)	0.1489 (5)	0.3568 (3)	0.0247 (10)
H24A	−0.532 (7)	0.140 (7)	0.348 (4)	0.045937
H24B	−0.392 (8)	0.075 (7)	0.409 (4)	0.046614
C25	−0.3420 (6)	0.3036 (5)	0.3799 (3)	0.0264 (10)
H25A	−0.392 (8)	0.335 (8)	0.437 (4)	0.057433
H25B	−0.378 (8)	0.366 (7)	0.333 (5)	0.049056
C26	−0.1671 (5)	0.3303 (5)	0.3896 (3)	0.0245 (10)
H26A	−0.125 (7)	0.435 (7)	0.407 (4)	0.046628
H26B	−0.139 (7)	0.260 (7)	0.437 (4)	0.044116
C31	0.2016 (5)	0.2744 (4)	0.4026 (3)	0.0173 (8)
H31	0.334 (7)	0.279 (7)	0.394 (4)	0.033659
C32	0.1878 (6)	0.3638 (5)	0.4797 (3)	0.0214 (9)
H32A	0.233 (8)	0.479 (6)	0.475 (4)	0.042755
H32B	0.066 (7)	0.350 (7)	0.494 (4)	0.039620
C33	0.2766 (6)	0.3167 (5)	0.5459 (3)	0.0270 (10)
H33A	0.409 (8)	0.330 (7)	0.532 (4)	0.046666
H33B	0.263 (8)	0.367 (7)	0.606 (4)	0.044259
C34	0.2205 (6)	0.1605 (5)	0.5576 (3)	0.0247 (10)
H34A	0.285 (9)	0.120 (7)	0.604 (4)	0.055952
H34B	0.109 (8)	0.141 (7)	0.578 (4)	0.044869
C35	0.2318 (6)	0.0699 (5)	0.4823 (3)	0.0244 (10)
H35A	0.177 (9)	−0.052 (7)	0.488 (4)	0.053327
H35B	0.361 (9)	0.074 (7)	0.466 (4)	0.054456
C36	0.1441 (6)	0.1176 (5)	0.4153 (3)	0.0211 (9)
H36A	0.015 (7)	0.102 (7)	0.426 (4)	0.039890
H36B	0.141 (8)	0.051 (6)	0.362 (4)	0.046761
B	0.3092 (8)	0.3654 (8)	0.8135 (4)	0.0419 (16)
F1	0.1955 (6)	0.3610 (5)	0.8668 (3)	0.0738 (14)
F2	0.2643 (6)	0.2598 (6)	0.7558 (3)	0.0907 (17)
F3	0.4451 (6)	0.3551 (7)	0.8467 (3)	0.0954 (18)
F4	0.3291 (7)	0.4933 (6)	0.7811 (4)	0.102 (2)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Os	0.01892 (9)	0.02358 (10)	0.01308 (9)	0.00521 (6)	0.00143 (6)	0.00047 (6)
H1	0.072000	0.046000	0.048000	−0.022000	0.023000	−0.014000
H2	0.065000	0.036000	0.035000	−0.000000	0.015000	0.008000
H3	0.082000	0.075000	0.038000	0.052000	−0.005000	0.008000
H4	0.030000	0.114000	0.048000	0.012000	−0.007000	−0.008000
C1	0.024 (2)	0.030 (2)	0.019 (2)	0.004 (2)	−0.0004 (18)	0.0039 (18)
C2	0.032 (3)	0.028 (2)	0.013 (2)	0.004 (2)	−0.0047 (18)	−0.0011 (17)
C3	0.041 (3)	0.029 (3)	0.018 (2)	0.013 (2)	−0.001 (2)	−0.0022 (18)
C4	0.030 (3)	0.040 (3)	0.016 (2)	0.009 (2)	0.0085 (19)	0.0032 (19)
C5	0.030 (3)	0.032 (3)	0.017 (2)	0.002 (2)	0.0051 (19)	0.0070 (18)
C6	0.028 (3)	0.056 (4)	0.033 (3)	0.011 (3)	−0.008 (2)	0.009 (3)
H6A	0.061000	0.095000	0.044000	0.035000	−0.016000	0.010000
H6B	0.070000	0.071000	0.076000	0.045000	−0.011000	−0.015000
H6C	0.039000	0.112000	0.084000	0.029000	0.020000	0.041000
C8	0.074 (5)	0.049 (4)	0.038 (3)	0.040 (4)	0.009 (3)	−0.002 (3)
H8A	0.088000	0.076000	0.165000	0.055000	−0.051000	−0.030000
H8B	0.147000	0.070000	0.063000	0.052000	0.003000	−0.028000
H8C	0.138000	0.041000	0.106000	0.034000	0.019000	0.024000
C7	0.049 (4)	0.034 (3)	0.029 (3)	−0.008 (3)	−0.007 (3)	0.002 (2)
H7A	0.095000	0.037000	0.159000	−0.003000	0.039000	0.021000
H7B	0.106000	0.140000	0.052000	−0.075000	−0.040000	0.027000
H7C	0.060000	0.078000	0.067000	−0.025000	0.029000	−0.019000
C9	0.035 (3)	0.069 (5)	0.036 (3)	0.009 (3)	0.013 (3)	0.004 (3)
H9A	0.051000	0.109000	0.030000	0.000000	0.015000	0.000000
H9B	0.045000	0.100000	0.086000	0.035000	0.013000	0.010000
H9C	0.039000	0.081000	0.051000	−0.011000	0.004000	−0.001000
C10	0.057 (4)	0.031 (3)	0.030 (3)	0.002 (3)	0.006 (3)	0.013 (2)
H10A	0.093000	0.053000	0.035000	0.005000	0.003000	0.020000
H10B	0.071000	0.046000	0.067000	−0.016000	−0.006000	0.015000
H10C	0.093000	0.038000	0.062000	0.023000	0.003000	0.010000
P	0.0155 (5)	0.0160 (5)	0.0147 (5)	0.0033 (4)	0.0015 (4)	0.0014 (4)
C11	0.020 (2)	0.019 (2)	0.020 (2)	0.0018 (17)	0.0017 (17)	0.0018 (16)
H11	0.050000	0.031000	0.026000	0.005000	0.006000	0.001000
C12	0.020 (2)	0.017 (2)	0.038 (3)	0.0016 (17)	−0.002 (2)	0.0039 (19)
H12A	0.043000	0.050000	0.067000	−0.003000	−0.019000	0.029000
H12B	0.035000	0.050000	0.056000	0.002000	0.007000	−0.009000
C13	0.035 (3)	0.017 (2)	0.050 (3)	−0.001 (2)	−0.011 (3)	0.000 (2)
H13A	0.092000	0.050000	0.054000	−0.004000	−0.011000	−0.012000
H13B	0.042000	0.054000	0.090000	−0.013000	−0.014000	0.023000
C14	0.032 (3)	0.020 (2)	0.060 (4)	0.001 (2)	−0.001 (3)	0.012 (2)
H14A	0.058000	0.089000	0.057000	0.008000	0.013000	0.038000
H14B	0.068000	0.040000	0.142000	−0.011000	−0.006000	0.039000
C15	0.029 (3)	0.022 (2)	0.056 (4)	0.004 (2)	−0.007 (3)	0.010 (2)
H15A	0.068000	0.057000	0.114000	0.012000	−0.008000	0.054000
H15B	0.073000	0.040000	0.092000	0.012000	0.011000	−0.010000
C16	0.032 (3)	0.023 (2)	0.026 (2)	0.007 (2)	−0.009 (2)	0.0015 (19)
H16A	0.035000	0.043000	0.056000	0.010000	0.000000	0.016000
H16B	0.061000	0.057000	0.026000	0.016000	0.001000	0.008000
C21	0.019 (2)	0.016 (2)	0.018 (2)	0.0030 (16)	0.0035 (16)	−0.0016 (16)
H21	0.033000	0.041000	0.034000	0.008000	−0.001000	0.012000
C22	0.019 (2)	0.020 (2)	0.026 (2)	0.0026 (17)	0.0017 (18)	−0.0038 (18)
H22A	0.036000	0.057000	0.045000	0.005000	0.008000	−0.022000
H22B	0.037000	0.034000	0.059000	0.005000	−0.002000	0.011000
C23	0.023 (2)	0.022 (2)	0.028 (2)	−0.0016 (18)	0.0008 (19)	−0.0031 (19)
H23A	0.039000	0.065000	0.033000	0.009000	−0.002000	0.011000
H23B	0.033000	0.044000	0.054000	−0.003000	0.001000	−0.012000
C24	0.015 (2)	0.029 (2)	0.029 (3)	0.0013 (18)	0.0048 (18)	0.0027 (19)
H24A	0.026000	0.055000	0.057000	0.011000	0.003000	−0.003000
H24B	0.048000	0.054000	0.038000	0.007000	0.009000	0.013000
C25	0.022 (2)	0.028 (2)	0.029 (3)	0.0058 (19)	0.007 (2)	−0.001 (2)
H25A	0.041000	0.071000	0.057000	0.014000	0.011000	−0.026000
H25B	0.041000	0.039000	0.069000	0.012000	−0.002000	0.005000
C26	0.017 (2)	0.031 (3)	0.024 (2)	0.0047 (19)	0.0047 (18)	−0.0071 (19)
H26A	0.038000	0.041000	0.056000	0.004000	0.002000	−0.019000
H26B	0.042000	0.063000	0.028000	0.011000	0.003000	0.006000
C31	0.017 (2)	0.017 (2)	0.018 (2)	0.0048 (16)	0.0008 (16)	−0.0003 (16)
H31	0.029000	0.038000	0.036000	0.010000	0.003000	0.007000
C32	0.030 (2)	0.022 (2)	0.015 (2)	0.0103 (19)	−0.0040 (18)	−0.0005 (16)
H32A	0.065000	0.024000	0.034000	−0.005000	−0.009000	0.005000
H32B	0.045000	0.048000	0.030000	0.021000	−0.001000	−0.002000
C33	0.038 (3)	0.028 (2)	0.014 (2)	0.004 (2)	−0.006 (2)	0.0018 (18)
H33A	0.035000	0.052000	0.053000	0.005000	−0.008000	0.014000
H33B	0.062000	0.039000	0.028000	0.001000	−0.012000	0.002000
C34	0.027 (3)	0.030 (2)	0.017 (2)	0.004 (2)	−0.0002 (18)	0.0073 (18)
H34A	0.076000	0.046000	0.045000	0.003000	−0.019000	0.023000
H34B	0.046000	0.047000	0.037000	−0.002000	0.007000	0.003000
C35	0.032 (3)	0.024 (2)	0.019 (2)	0.009 (2)	0.0018 (19)	0.0033 (18)
H35A	0.084000	0.024000	0.048000	−0.002000	0.004000	0.011000
H35B	0.062000	0.049000	0.061000	0.028000	0.011000	0.015000
C36	0.032 (3)	0.016 (2)	0.015 (2)	0.0027 (18)	−0.0017 (18)	0.0015 (16)
H36A	0.034000	0.044000	0.038000	−0.003000	0.002000	0.008000
H36B	0.075000	0.029000	0.031000	0.000000	0.005000	−0.005000
B	0.040 (4)	0.054 (4)	0.029 (3)	0.002 (3)	0.009 (3)	0.004 (3)
F1	0.087 (3)	0.073 (3)	0.055 (3)	0.003 (3)	0.030 (2)	−0.003 (2)
F2	0.082 (3)	0.119 (4)	0.065 (3)	0.022 (3)	−0.010 (3)	−0.046 (3)
F3	0.071 (3)	0.137 (5)	0.082 (4)	0.031 (3)	−0.031 (3)	0.008 (3)
F4	0.087 (4)	0.099 (4)	0.124 (5)	0.009 (3)	0.010 (4)	0.066 (4)

Geometric parameters (Å, º)

Os—H1	1.68 (6)	C14—H14A	1.14 (8)
Os—H2	1.67 (6)	C14—H14B	1.07 (8)
Os—H3	1.68 (7)	C14—C15	1.523 (8)
Os—H4	1.66 (7)	C15—H15A	1.13 (8)
Os—C1	2.305 (5)	C15—H15B	1.14 (8)
Os—C2	2.294 (4)	C15—C16	1.534 (7)
Os—C3	2.248 (5)	C16—H16A	1.11 (6)
Os—C4	2.254 (5)	C16—H16B	1.10 (7)
Os—C5	2.270 (5)	C21—H21	1.14 (6)
Os—P	2.3671 (11)	C21—C22	1.540 (6)
C1—C2	1.434 (7)	C21—C26	1.536 (6)
C1—C5	1.432 (7)	C22—H22A	1.14 (6)
C1—C6	1.499 (7)	C22—H22B	1.08 (7)
C2—C3	1.446 (7)	C22—C23	1.536 (6)
C2—C7	1.496 (7)	C23—H23A	1.15 (7)
C3—C4	1.448 (7)	C23—H23B	1.16 (6)
C3—C8	1.490 (8)	C23—C24	1.528 (7)
C4—C5	1.440 (7)	C24—H24A	1.12 (6)
C4—C9	1.490 (8)	C24—H24B	1.21 (7)
C5—C10	1.493 (7)	C24—C25	1.525 (7)
C6—H6A	1.10 (7)	C25—H25A	1.12 (7)
C6—H6B	1.08 (8)	C25—H25B	1.12 (7)
C6—H6C	1.14 (8)	C25—C26	1.539 (7)
C8—H8A	1.12 (9)	C26—H26A	1.04 (6)
C8—H8B	1.09 (8)	C26—H26B	1.16 (7)
C8—H8C	1.12 (9)	C31—H31	1.19 (6)
C7—H7A	1.00 (10)	C31—C32	1.550 (6)
C7—H7B	1.10 (9)	C31—C36	1.539 (6)
C7—H7C	1.05 (8)	C32—H32A	1.12 (6)
C9—H9A	1.11 (7)	C32—H32B	1.10 (6)
C9—H9B	1.10 (8)	C32—C33	1.533 (6)
C9—H9C	1.13 (8)	C33—H33A	1.18 (7)
C10—H10A	1.11 (7)	C33—H33B	1.13 (7)
C10—H10B	1.12 (8)	C33—C34	1.529 (7)
C10—H10C	1.11 (8)	C34—H34A	1.12 (7)
P—C11	1.854 (5)	C34—H34B	1.04 (7)
P—C21	1.852 (4)	C34—C35	1.526 (7)
P—C31	1.872 (5)	C35—H35A	1.20 (6)
C11—H11	1.11 (6)	C35—H35B	1.18 (7)
C11—C12	1.541 (6)	C35—C36	1.541 (6)
C11—C16	1.532 (6)	C36—H36A	1.15 (6)
C12—H12A	1.15 (7)	C36—H36B	1.08 (6)
C12—H12B	1.11 (7)	B—F1	1.364 (8)
C12—C13	1.531 (7)	B—F2	1.374 (8)
C13—H13A	1.07 (8)	B—F3	1.365 (9)
C13—H13B	1.16 (7)	B—F4	1.378 (9)
C13—C14	1.525 (8)
H2—Os—H1	129 (4)	C12—C11—H11	106 (3)
H3—Os—H1	95 (4)	C16—C11—P	112.8 (3)
H3—Os—H2	65 (4)	C16—C11—H11	109 (3)
H4—Os—H1	55 (4)	C16—C11—C12	110.8 (4)
H4—Os—H2	104 (4)	H12A—C12—C11	113 (3)
H4—Os—H3	43 (4)	H12B—C12—C11	107 (3)
C1—Os—H1	110 (3)	H12B—C12—H12A	103 (5)
C1—Os—H2	106 (3)	C13—C12—C11	111.4 (4)
C1—Os—H3	151 (3)	C13—C12—H12A	112 (4)
C1—Os—H4	148 (3)	C13—C12—H12B	110 (4)
C2—Os—H1	145 (3)	H13A—C13—C12	111 (4)
C2—Os—H2	82 (2)	H13B—C13—C12	111 (4)
C2—Os—H3	115 (3)	H13B—C13—H13A	105 (6)
C2—Os—H4	141 (3)	C14—C13—C12	110.8 (5)
C2—Os—C1	36.34 (17)	C14—C13—H13A	107 (5)
C3—Os—H1	132 (2)	C14—C13—H13B	112 (4)
C3—Os—H2	96 (2)	H14A—C14—C13	109 (4)
C3—Os—H3	91 (3)	H14B—C14—C13	109 (5)
C3—Os—H4	104 (3)	H14B—C14—H14A	104 (6)
C3—Os—C1	61.72 (18)	C15—C14—C13	110.4 (5)
C3—Os—C2	37.12 (18)	C15—C14—H14A	112 (4)
C4—Os—H1	95 (2)	C15—C14—H14B	113 (5)
C4—Os—H2	133 (2)	H15A—C15—C14	114 (4)
C4—Os—H3	103 (3)	H15B—C15—C14	110 (4)
C4—Os—H4	89 (3)	H15B—C15—H15A	103 (6)
C4—Os—C1	61.67 (18)	C16—C15—C14	111.5 (5)
C4—Os—C2	61.80 (18)	C16—C15—H15A	110 (4)
C4—Os—C3	37.51 (19)	C16—C15—H15B	107 (4)
C5—Os—H1	85 (3)	C15—C16—C11	110.9 (4)
C5—Os—H2	142 (2)	H16A—C16—C11	112 (3)
C5—Os—H3	139 (3)	H16A—C16—C15	108 (3)
C5—Os—H4	111 (3)	H16B—C16—C11	110 (4)
C5—Os—C1	36.47 (17)	H16B—C16—C15	113 (4)
C5—Os—C2	60.94 (17)	H16B—C16—H16A	103 (5)
C5—Os—C3	61.96 (18)	H21—C21—P	102 (3)
C5—Os—C4	37.10 (18)	C22—C21—P	114.5 (3)
P—Os—H1	68 (2)	C22—C21—H21	104 (3)
P—Os—H2	69 (2)	C26—C21—P	115.5 (3)
P—Os—H3	96 (3)	C26—C21—H21	110 (3)
P—Os—H4	94 (3)	C26—C21—C22	109.8 (4)
P—Os—C1	107.09 (12)	H22A—C22—C21	112 (3)
P—Os—C2	123.24 (13)	H22B—C22—C21	112 (3)
P—Os—C3	158.90 (14)	H22B—C22—H22A	106 (5)
P—Os—C4	155.74 (14)	C23—C22—C21	111.4 (4)
P—Os—C5	120.93 (13)	C23—C22—H22A	107 (3)
C2—C1—Os	71.4 (3)	C23—C22—H22B	108 (3)
C5—C1—Os	70.5 (3)	H23A—C23—C22	110 (3)
C5—C1—C2	107.7 (4)	H23B—C23—C22	110 (3)
C6—C1—Os	130.5 (4)	H23B—C23—H23A	108 (5)
C6—C1—C2	126.4 (5)	C24—C23—C22	110.5 (4)
C6—C1—C5	125.3 (5)	C24—C23—H23A	108 (4)
C1—C2—Os	72.3 (3)	C24—C23—H23B	110 (3)
C3—C2—Os	69.7 (3)	H24A—C24—C23	110 (4)
C3—C2—C1	108.4 (4)	H24B—C24—C23	111 (3)
C7—C2—Os	131.1 (3)	H24B—C24—H24A	107 (5)
C7—C2—C1	126.6 (5)	C25—C24—C23	111.0 (4)
C7—C2—C3	124.3 (5)	C25—C24—H24A	106 (4)
C2—C3—Os	73.2 (3)	C25—C24—H24B	112 (3)
C4—C3—Os	71.5 (3)	H25A—C25—C24	109 (4)
C4—C3—C2	107.6 (4)	H25B—C25—C24	107 (4)
C8—C3—Os	126.6 (4)	H25B—C25—H25A	109 (5)
C8—C3—C2	126.5 (5)	C26—C25—C24	111.0 (4)
C8—C3—C4	125.4 (5)	C26—C25—H25A	109 (4)
C3—C4—Os	71.0 (3)	C26—C25—H25B	112 (4)
C5—C4—Os	72.1 (3)	C25—C26—C21	110.8 (4)
C5—C4—C3	107.3 (4)	H26A—C26—C21	112 (4)
C9—C4—Os	126.7 (4)	H26A—C26—C25	110 (4)
C9—C4—C3	126.8 (5)	H26B—C26—C21	106 (3)
C9—C4—C5	125.7 (5)	H26B—C26—C25	108 (3)
C1—C5—Os	73.1 (3)	H26B—C26—H26A	110 (5)
C4—C5—Os	70.8 (3)	H31—C31—P	109 (3)
C4—C5—C1	108.9 (4)	C32—C31—P	116.4 (3)
C10—C5—Os	130.5 (4)	C32—C31—H31	106 (3)
C10—C5—C1	126.0 (5)	C36—C31—P	113.1 (3)
C10—C5—C4	124.2 (5)	C36—C31—H31	102 (3)
H6A—C6—C1	107 (4)	C36—C31—C32	109.3 (4)
H6B—C6—C1	111 (4)	H32A—C32—C31	113 (3)
H6B—C6—H6A	109 (6)	H32B—C32—C31	108 (3)
H6C—C6—C1	109 (4)	H32B—C32—H32A	108 (5)
H6C—C6—H6A	105 (6)	C33—C32—C31	110.6 (4)
H6C—C6—H6B	116 (7)	C33—C32—H32A	107 (3)
H8A—C8—C3	114 (4)	C33—C32—H32B	111 (3)
H8B—C8—C3	117 (5)	H33A—C33—C32	112 (3)
H8B—C8—H8A	104 (7)	H33B—C33—C32	116 (4)
H8C—C8—C3	116 (5)	H33B—C33—H33A	109 (5)
H8C—C8—H8A	96 (7)	C34—C33—C32	111.3 (4)
H8C—C8—H8B	108 (7)	C34—C33—H33A	106 (3)
H7A—C7—C2	103 (5)	C34—C33—H33B	102 (3)
H7B—C7—C2	118 (5)	H34A—C34—C33	114 (4)
H7B—C7—H7A	101 (8)	H34B—C34—C33	112 (4)
H7C—C7—C2	112 (4)	H34B—C34—H34A	103 (5)
H7C—C7—H7A	126 (7)	C35—C34—C33	111.1 (4)
H7C—C7—H7B	98 (7)	C35—C34—H34A	107 (4)
H9A—C9—C4	108 (4)	C35—C34—H34B	110 (4)
H9B—C9—C4	112 (4)	H35A—C35—C34	112 (3)
H9B—C9—H9A	108 (6)	H35B—C35—C34	110 (4)
H9C—C9—C4	116 (4)	H35B—C35—H35A	106 (5)
H9C—C9—H9A	103 (6)	C36—C35—C34	110.6 (4)
H9C—C9—H9B	109 (6)	C36—C35—H35A	106 (4)
H10A—C10—C5	109 (4)	C36—C35—H35B	111 (4)
H10B—C10—C5	114 (4)	C35—C36—C31	111.7 (4)
H10B—C10—H10A	107 (6)	H36A—C36—C31	107 (3)
H10C—C10—C5	110 (4)	H36A—C36—C35	112 (3)
H10C—C10—H10A	110 (6)	H36B—C36—C31	112 (3)
H10C—C10—H10B	106 (6)	H36B—C36—C35	113 (4)
C11—P—Os	114.82 (15)	H36B—C36—H36A	99 (5)
C21—P—Os	112.93 (14)	F2—B—F1	108.7 (6)
C21—P—C11	103.9 (2)	F3—B—F1	112.4 (6)
C31—P—Os	111.70 (14)	F3—B—F2	111.1 (7)
C31—P—C11	102.7 (2)	F4—B—F1	107.9 (6)
C31—P—C21	110.1 (2)	F4—B—F2	108.9 (6)
H11—C11—P	105 (3)	F4—B—F3	107.8 (6)
C12—C11—P	112.3 (3)

(XAXMEP_HAR_SHADE3_1)

Crystal data

C28H52OsP·BF4	V = 1457.79 (4) Å^3
Mr = 696.74	Z = 2
Triclinic, P1	F(000) = 111.426
a = 8.9295 (2) Å	Dx = 1.587 Mg m^−3
b = 9.7179 (1) Å	Mo Kα radiation, λ = 0.71073 Å
c = 17.1819 (1) Å	µ = 4.47 mm^−1
α = 94.114 (1)°	T = 199 K
β = 90.034 (1)°	0.3 × 0.1 × 0.04 mm
γ = 101.369 (1)°

Data collection

Absorption correction: integration	Rint = 0.033
Tmin = 0.529, Tmax = 0.844	θmax = 28.3°, θmin = 2.1°
9506 measured reflections	h = −11→11
6629 independent reflections	k = −12→12
5952 reflections with I ≥ 2u(I)	l = −22→13

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.034	Only H-atom coordinates refined
wR(F^2) = 0.082	w = 1/[σ^2(Fo^2) + (0.0239P)^2 + 6.6229P] where P = (Fo^2 + 2Fc^2)/3
S = 1.09	(Δ/σ)max = 0.001
6629 reflections	Δρmax = 1.22 e Å^−3
472 parameters	Δρmin = −1.52 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Os	0.22260 (2)	0.241115 (19)	0.197802 (10)	0.01848 (6)
H1	0.308 (8)	0.408 (7)	0.226 (4)	0.040974
H2	0.144 (8)	0.111 (7)	0.252 (4)	0.038964
H3	0.347 (8)	0.169 (8)	0.243 (4)	0.043022
H4	0.404 (8)	0.291 (9)	0.229 (4)	0.043156
C1	0.0490 (6)	0.2382 (5)	0.0980 (3)	0.0248 (10)
C2	0.0772 (6)	0.0985 (5)	0.1022 (3)	0.0248 (10)
C3	0.2379 (6)	0.1023 (5)	0.0889 (3)	0.0286 (11)
C4	0.3082 (6)	0.2456 (6)	0.0745 (3)	0.0285 (11)
C5	0.1909 (6)	0.3281 (5)	0.0811 (3)	0.0268 (10)
C6	−0.1043 (7)	0.2791 (7)	0.0988 (4)	0.0381 (13)
H6A	−0.141 (9)	0.278 (8)	0.037 (4)	0.054468
H6B	−0.094 (8)	0.382 (7)	0.123 (4)	0.046330
H6C	−0.190 (8)	0.190 (8)	0.125 (4)	0.046817
C8	0.3148 (9)	−0.0208 (7)	0.0811 (4)	0.0501 (17)
H8A	0.436 (9)	0.001 (8)	0.105 (4)	0.054728
H8B	0.321 (9)	−0.070 (8)	0.020 (4)	0.059024
H8C	0.267 (9)	−0.111 (8)	0.119 (4)	0.051393
C7	−0.0407 (8)	−0.0333 (6)	0.1067 (3)	0.0396 (14)
H7A	0.014 (8)	−0.093 (7)	0.130 (4)	0.041900
H7B	−0.074 (9)	−0.101 (8)	0.056 (4)	0.050714
H7C	−0.152 (8)	−0.008 (7)	0.121 (4)	0.045021
C9	0.4682 (7)	0.2966 (8)	0.0496 (4)	0.0468 (16)
H9A	0.473 (9)	0.294 (9)	−0.016 (4)	0.064749
H9B	0.546 (9)	0.235 (9)	0.070 (4)	0.058438
H9C	0.519 (8)	0.412 (9)	0.064 (5)	0.056297
C10	0.2111 (8)	0.4764 (6)	0.0592 (3)	0.0396 (14)
H10A	0.212 (9)	0.482 (8)	−0.006 (4)	0.058931
H10B	0.320 (8)	0.545 (8)	0.082 (4)	0.052384
H10C	0.119 (8)	0.526 (7)	0.081 (4)	0.050690
P	0.11842 (12)	0.33049 (11)	0.31287 (6)	0.0155 (2)
C11	0.1601 (5)	0.5250 (5)	0.3290 (3)	0.0199 (9)
H11	0.112 (7)	0.550 (6)	0.386 (4)	0.032280
C12	0.3329 (5)	0.5861 (5)	0.3363 (3)	0.0255 (10)
H12A	0.394 (7)	0.531 (6)	0.380 (4)	0.035614
H12B	0.381 (7)	0.557 (7)	0.279 (4)	0.036827
C13	0.3644 (7)	0.7461 (5)	0.3527 (4)	0.0350 (13)
H13A	0.318 (8)	0.777 (7)	0.408 (4)	0.044558
H13B	0.494 (8)	0.789 (7)	0.360 (4)	0.046359
C14	0.2916 (7)	0.8155 (6)	0.2897 (4)	0.0373 (13)
H14A	0.351 (8)	0.799 (7)	0.231 (4)	0.046384
H14B	0.319 (8)	0.928 (7)	0.303 (4)	0.052054
C15	0.1203 (6)	0.7571 (5)	0.2839 (4)	0.0356 (13)
H15A	0.060 (8)	0.807 (7)	0.239 (4)	0.047779
H15B	0.066 (8)	0.780 (7)	0.344 (4)	0.045528
C16	0.0857 (6)	0.5967 (5)	0.2671 (3)	0.0268 (10)
H16A	−0.039 (7)	0.560 (6)	0.265 (4)	0.036230
H16B	0.122 (7)	0.563 (6)	0.208 (4)	0.037341
C21	−0.0928 (5)	0.2831 (4)	0.3143 (3)	0.0180 (8)
H21	−0.127 (7)	0.342 (6)	0.266 (4)	0.030769
C22	−0.1595 (5)	0.1268 (5)	0.2915 (3)	0.0221 (9)
H22A	−0.111 (7)	0.088 (6)	0.234 (4)	0.033834
H22B	−0.132 (7)	0.059 (6)	0.333 (4)	0.034014
C23	−0.3341 (6)	0.0999 (5)	0.2819 (3)	0.0255 (10)
H23A	−0.366 (7)	0.163 (7)	0.232 (4)	0.040537
H23B	−0.381 (7)	−0.019 (7)	0.264 (4)	0.041858
C24	−0.4069 (5)	0.1489 (5)	0.3568 (3)	0.0249 (10)
H24A	−0.532 (7)	0.139 (7)	0.349 (4)	0.047100
H24B	−0.394 (8)	0.076 (7)	0.410 (4)	0.042458
C25	−0.3420 (6)	0.3035 (5)	0.3799 (3)	0.0266 (10)
H25A	−0.394 (7)	0.337 (7)	0.433 (4)	0.045575
H25B	−0.377 (7)	0.367 (7)	0.336 (4)	0.042029
C26	−0.1671 (5)	0.3303 (5)	0.3896 (3)	0.0246 (10)
H26A	−0.126 (7)	0.436 (6)	0.406 (4)	0.035499
H26B	−0.139 (7)	0.260 (6)	0.436 (4)	0.035220
C31	0.2016 (5)	0.2743 (4)	0.4026 (3)	0.0175 (8)
H31	0.333 (7)	0.280 (6)	0.394 (4)	0.029460
C32	0.1877 (6)	0.3638 (5)	0.4797 (3)	0.0215 (9)
H32A	0.233 (7)	0.479 (6)	0.475 (4)	0.034797
H32B	0.066 (7)	0.349 (6)	0.494 (4)	0.035250
C33	0.2765 (6)	0.3167 (5)	0.5461 (3)	0.0273 (10)
H33A	0.407 (7)	0.329 (7)	0.536 (4)	0.039366
H33B	0.261 (8)	0.363 (7)	0.609 (4)	0.042469
C34	0.2204 (6)	0.1606 (5)	0.5576 (3)	0.0249 (10)
H34A	0.285 (8)	0.121 (7)	0.602 (4)	0.043646
H34B	0.109 (8)	0.140 (7)	0.579 (4)	0.040542
C35	0.2318 (6)	0.0698 (5)	0.4823 (3)	0.0246 (10)
H35A	0.180 (8)	−0.053 (7)	0.487 (4)	0.040266
H35B	0.359 (7)	0.071 (7)	0.464 (4)	0.038140
C36	0.1442 (6)	0.1176 (5)	0.4153 (3)	0.0214 (9)
H36A	0.017 (7)	0.103 (6)	0.427 (4)	0.032552
H36B	0.141 (7)	0.051 (6)	0.365 (3)	0.031894
B	0.3092 (9)	0.3653 (8)	0.8135 (4)	0.0425 (16)
F1	0.1955 (6)	0.3609 (5)	0.8668 (3)	0.0739 (14)
F2	0.2644 (6)	0.2599 (6)	0.7558 (3)	0.0906 (17)
F3	0.4452 (6)	0.3549 (7)	0.8468 (3)	0.0953 (18)
F4	0.3292 (7)	0.4933 (6)	0.7811 (4)	0.101 (2)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Os	0.01897 (9)	0.02363 (10)	0.01313 (9)	0.00522 (6)	0.00143 (6)	0.00047 (6)
H1	0.045920	0.032740	0.039910	−0.002590	0.005980	0.002020
H2	0.043170	0.037000	0.033500	−0.000400	0.008230	0.003890
H3	0.047130	0.048740	0.039730	0.022890	0.000810	0.010140
H4	0.025770	0.056780	0.046430	0.007450	−0.002310	0.002480
C1	0.024 (2)	0.030 (3)	0.019 (2)	0.003 (2)	−0.0006 (18)	0.0042 (18)
C2	0.032 (3)	0.028 (2)	0.013 (2)	0.004 (2)	−0.0046 (18)	−0.0013 (17)
C3	0.041 (3)	0.029 (3)	0.018 (2)	0.012 (2)	−0.001 (2)	−0.0021 (18)
C4	0.030 (3)	0.040 (3)	0.016 (2)	0.009 (2)	0.0083 (19)	0.0031 (19)
C5	0.030 (3)	0.033 (3)	0.017 (2)	0.002 (2)	0.0051 (19)	0.0067 (18)
C6	0.029 (3)	0.053 (4)	0.034 (3)	0.010 (3)	−0.009 (2)	0.008 (3)
H6A	0.056970	0.080150	0.029190	0.019980	−0.014170	0.005920
H6B	0.043550	0.040130	0.054580	0.008670	−0.012000	−0.002510
H6C	0.036130	0.053020	0.050670	0.003640	0.001030	0.013970
C8	0.073 (5)	0.049 (4)	0.039 (4)	0.040 (4)	0.009 (3)	−0.002 (3)
H8A	0.051870	0.068830	0.047120	0.026220	0.002030	−0.010990
H8B	0.078240	0.072460	0.029240	0.028730	0.006970	−0.015500
H8C	0.065920	0.049030	0.040730	0.018320	0.009730	−0.006040
C7	0.049 (4)	0.034 (3)	0.029 (3)	−0.006 (3)	−0.009 (3)	0.002 (2)
H7A	0.057760	0.033950	0.033130	0.010670	−0.006570	−0.007810
H7B	0.060650	0.051250	0.037710	0.010710	−0.014860	−0.012830
H7C	0.047120	0.046520	0.038530	0.004950	0.000890	−0.004510
C9	0.035 (3)	0.068 (5)	0.037 (3)	0.010 (3)	0.013 (3)	0.005 (3)
H9A	0.059300	0.107830	0.028280	0.016760	0.015530	0.012090
H9B	0.049690	0.079880	0.052180	0.025590	0.016810	0.012710
H9C	0.045450	0.070080	0.049710	0.002510	0.013770	0.004380
C10	0.055 (4)	0.032 (3)	0.030 (3)	0.003 (3)	0.006 (3)	0.013 (2)
H10A	0.073810	0.072370	0.029620	0.006120	0.001820	0.020260
H10B	0.041090	0.059120	0.053970	−0.002890	−0.003590	0.019740
H10C	0.049720	0.051460	0.054020	0.012780	0.006480	0.017330
P	0.0156 (5)	0.0161 (5)	0.0149 (5)	0.0033 (4)	0.0015 (4)	0.0014 (4)
C11	0.020 (2)	0.019 (2)	0.020 (2)	0.0019 (17)	0.0017 (17)	0.0016 (16)
H11	0.035670	0.029450	0.031450	0.007560	0.001610	−0.002760
C12	0.019 (2)	0.018 (2)	0.039 (3)	0.0017 (17)	−0.002 (2)	0.0042 (19)
H12A	0.033980	0.033510	0.038810	0.003650	−0.007020	0.007480
H12B	0.033410	0.037560	0.036910	0.001450	0.002840	0.000580
C13	0.035 (3)	0.017 (2)	0.050 (3)	−0.001 (2)	−0.011 (3)	0.000 (2)
H13A	0.054380	0.030340	0.046690	0.005410	−0.005490	−0.004230
H13B	0.034920	0.037180	0.063130	−0.003760	−0.007790	0.008030
C14	0.032 (3)	0.020 (2)	0.060 (4)	0.001 (2)	−0.001 (3)	0.011 (2)
H14A	0.045850	0.040290	0.051660	0.002470	−0.002910	0.011100
H14B	0.053960	0.024460	0.074180	−0.002950	−0.010190	0.009420
C15	0.029 (3)	0.022 (2)	0.056 (4)	0.004 (2)	−0.006 (3)	0.010 (2)
H15A	0.048290	0.033950	0.063380	0.008960	−0.010750	0.016860
H15B	0.047840	0.032690	0.055540	0.009080	−0.001550	−0.003380
C16	0.032 (3)	0.024 (2)	0.026 (2)	0.007 (2)	−0.009 (2)	0.0012 (19)
H16A	0.026860	0.033790	0.048920	0.006600	−0.002790	0.007350
H16B	0.043370	0.035100	0.033850	0.007340	−0.000620	0.005720
C21	0.020 (2)	0.016 (2)	0.018 (2)	0.0033 (16)	0.0035 (16)	−0.0015 (16)
H21	0.029910	0.031160	0.032050	0.006480	−0.001840	0.006620
C22	0.019 (2)	0.020 (2)	0.026 (2)	0.0027 (17)	0.0017 (18)	−0.0035 (18)
H22A	0.034430	0.035890	0.029300	0.005050	0.001030	−0.005100
H22B	0.036100	0.030510	0.034780	0.002790	−0.002370	0.008590
C23	0.023 (2)	0.022 (2)	0.028 (3)	−0.0014 (18)	0.0008 (19)	−0.0030 (19)
H23A	0.035170	0.045380	0.041540	0.007040	−0.003470	0.009050
H23B	0.034220	0.034930	0.050330	−0.006130	−0.004010	−0.002010
C24	0.015 (2)	0.030 (2)	0.029 (3)	0.0013 (18)	0.0048 (18)	0.003 (2)
H24A	0.023690	0.055480	0.060450	0.003610	0.002270	0.004600
H24B	0.039930	0.042850	0.043080	0.002060	0.006130	0.009930
C25	0.022 (2)	0.029 (2)	0.029 (3)	0.0061 (19)	0.007 (2)	−0.001 (2)
H25A	0.034810	0.053620	0.048440	0.011880	0.012390	−0.004150
H25B	0.032590	0.042660	0.052490	0.009560	−0.000640	0.008800
C26	0.017 (2)	0.031 (3)	0.025 (2)	0.0047 (19)	0.0048 (18)	−0.0069 (19)
H26A	0.032390	0.030340	0.042140	0.004930	0.002630	−0.004860
H26B	0.037330	0.038810	0.031620	0.011010	0.005500	0.007070
C31	0.017 (2)	0.018 (2)	0.018 (2)	0.0048 (16)	0.0007 (16)	−0.0003 (16)
H31	0.025400	0.034500	0.029410	0.008480	0.000620	0.001500
C32	0.030 (2)	0.022 (2)	0.015 (2)	0.0101 (19)	−0.0039 (18)	−0.0005 (16)
H32A	0.041090	0.027380	0.033160	0.001360	−0.002120	−0.001410
H32B	0.033380	0.042940	0.030470	0.012000	0.003690	−0.002730
C33	0.037 (3)	0.028 (2)	0.015 (2)	0.004 (2)	−0.006 (2)	0.0020 (18)
H33A	0.035770	0.044860	0.037800	0.008790	−0.004290	0.003040
H33B	0.057260	0.043720	0.024230	0.008230	−0.005120	−0.007490
C34	0.027 (3)	0.030 (3)	0.017 (2)	0.005 (2)	−0.0004 (19)	0.0074 (18)
H34A	0.056730	0.048300	0.027560	0.012230	−0.009090	0.008910
H34B	0.043500	0.046080	0.032040	0.008680	0.004250	0.003280
C35	0.032 (3)	0.024 (2)	0.019 (2)	0.009 (2)	0.0020 (19)	0.0030 (18)
H35A	0.052890	0.030820	0.036500	0.004780	−0.003270	0.008270
H35B	0.037440	0.045920	0.034450	0.016590	−0.003140	0.002670
C36	0.033 (3)	0.016 (2)	0.015 (2)	0.0027 (18)	−0.0016 (18)	0.0009 (16)
H36A	0.029840	0.034620	0.034160	0.007710	0.004210	0.005290
H36B	0.042050	0.029020	0.024640	0.008900	−0.000860	−0.003080
B	0.041 (4)	0.054 (4)	0.030 (3)	0.001 (3)	0.009 (3)	0.004 (3)
F1	0.088 (3)	0.072 (3)	0.056 (3)	0.003 (3)	0.030 (2)	−0.004 (2)
F2	0.081 (3)	0.119 (4)	0.066 (3)	0.022 (3)	−0.009 (3)	−0.045 (3)
F3	0.071 (3)	0.138 (5)	0.081 (4)	0.032 (3)	−0.030 (3)	0.008 (3)
F4	0.087 (4)	0.099 (4)	0.122 (5)	0.010 (3)	0.010 (4)	0.065 (4)

Geometric parameters (Å, º)

Os—H1	1.69 (6)	C14—H14A	1.15 (7)
Os—H2	1.67 (6)	C14—H14B	1.08 (6)
Os—H3	1.65 (7)	C14—C15	1.523 (8)
Os—H4	1.67 (7)	C15—H15A	1.13 (7)
Os—C1	2.306 (5)	C15—H15B	1.17 (7)
Os—C2	2.294 (4)	C15—C16	1.534 (7)
Os—C3	2.247 (5)	C16—H16A	1.10 (6)
Os—C4	2.254 (5)	C16—H16B	1.11 (6)
Os—C5	2.270 (5)	C21—H21	1.12 (6)
Os—P	2.3671 (11)	C21—C22	1.540 (6)
C1—C2	1.435 (7)	C21—C26	1.536 (6)
C1—C5	1.433 (7)	C22—H22A	1.15 (6)
C1—C6	1.499 (7)	C22—H22B	1.06 (6)
C2—C3	1.447 (7)	C22—C23	1.536 (7)
C2—C7	1.496 (7)	C23—H23A	1.15 (7)
C3—C4	1.450 (7)	C23—H23B	1.17 (6)
C3—C8	1.490 (8)	C23—C24	1.530 (7)
C4—C5	1.439 (7)	C24—H24A	1.11 (6)
C4—C9	1.490 (8)	C24—H24B	1.21 (7)
C5—C10	1.492 (7)	C24—C25	1.524 (7)
C6—H6A	1.11 (7)	C25—H25A	1.09 (6)
C6—H6B	1.04 (7)	C25—H25B	1.09 (7)
C6—H6C	1.15 (7)	C25—C26	1.539 (7)
C8—H8A	1.13 (8)	C26—H26A	1.04 (6)
C8—H8B	1.13 (7)	C26—H26B	1.15 (6)
C8—H8C	1.14 (8)	C31—H31	1.18 (6)
C7—H7A	0.94 (7)	C31—C32	1.550 (6)
C7—H7B	1.05 (7)	C31—C36	1.539 (6)
C7—H7C	1.09 (7)	C32—H32A	1.12 (6)
C9—H9A	1.12 (7)	C32—H32B	1.10 (6)
C9—H9B	1.07 (8)	C32—C33	1.534 (6)
C9—H9C	1.13 (8)	C33—H33A	1.17 (7)
C10—H10A	1.12 (7)	C33—H33B	1.16 (6)
C10—H10B	1.12 (7)	C33—C34	1.529 (7)
C10—H10C	1.09 (7)	C34—H34A	1.08 (6)
P—C11	1.854 (5)	C34—H34B	1.05 (6)
P—C21	1.852 (5)	C34—C35	1.528 (7)
P—C31	1.873 (5)	C35—H35A	1.20 (6)
C11—H11	1.11 (6)	C35—H35B	1.17 (6)
C11—C12	1.542 (6)	C35—C36	1.539 (6)
C11—C16	1.531 (6)	C36—H36A	1.14 (6)
C12—H12A	1.15 (6)	C36—H36B	1.04 (6)
C12—H12B	1.11 (6)	B—F1	1.365 (8)
C12—C13	1.530 (7)	B—F2	1.372 (9)
C13—H13A	1.08 (7)	B—F3	1.366 (9)
C13—H13B	1.15 (6)	B—F4	1.379 (9)
C13—C14	1.525 (8)
H2—Os—H1	130 (3)	C12—C11—H11	106 (3)
H3—Os—H1	95 (4)	C16—C11—P	112.9 (3)
H3—Os—H2	66 (3)	C16—C11—H11	108 (3)
H4—Os—H1	55 (3)	C16—C11—C12	110.8 (4)
H4—Os—H2	106 (4)	H12A—C12—C11	113 (3)
H4—Os—H3	44 (3)	H12B—C12—C11	105 (3)
C1—Os—H1	110 (2)	H12B—C12—H12A	103 (5)
C1—Os—H2	105 (2)	C13—C12—C11	111.4 (4)
C1—Os—H3	151 (3)	C13—C12—H12A	113 (3)
C1—Os—H4	147 (3)	C13—C12—H12B	111 (3)
C2—Os—H1	145 (2)	H13A—C13—C12	112 (3)
C2—Os—H2	82 (2)	H13B—C13—C12	110 (3)
C2—Os—H3	115 (3)	H13B—C13—H13A	104 (5)
C2—Os—H4	141 (3)	C14—C13—C12	110.8 (5)
C2—Os—C1	36.37 (17)	C14—C13—H13A	107 (4)
C3—Os—H1	132 (2)	C14—C13—H13B	113 (4)
C3—Os—H2	96 (2)	H14A—C14—C13	109 (4)
C3—Os—H3	91 (3)	H14B—C14—C13	108 (4)
C3—Os—H4	104 (3)	H14B—C14—H14A	104 (5)
C3—Os—C1	61.77 (18)	C15—C14—C13	110.4 (5)
C3—Os—C2	37.13 (19)	C15—C14—H14A	112 (4)
C4—Os—H1	95 (2)	C15—C14—H14B	113 (4)
C4—Os—H2	133 (2)	H15A—C15—C14	113 (4)
C4—Os—H3	103 (2)	H15B—C15—C14	109 (3)
C4—Os—H4	88 (3)	H15B—C15—H15A	107 (5)
C4—Os—C1	61.69 (18)	C16—C15—C14	111.5 (5)
C4—Os—C2	61.85 (18)	C16—C15—H15A	109 (3)
C4—Os—C3	37.59 (19)	C16—C15—H15B	107 (3)
C5—Os—H1	84 (2)	C15—C16—C11	111.0 (4)
C5—Os—H2	141 (2)	H16A—C16—C11	111 (3)
C5—Os—H3	139 (3)	H16A—C16—C15	109 (3)
C5—Os—H4	111 (3)	H16B—C16—C11	109 (3)
C5—Os—C1	36.49 (17)	H16B—C16—C15	113 (3)
C5—Os—C2	60.98 (18)	H16B—C16—H16A	104 (5)
C5—Os—C3	62.01 (18)	H21—C21—P	103 (3)
C5—Os—C4	37.09 (18)	C22—C21—P	114.5 (3)
P—Os—H1	67 (2)	C22—C21—H21	105 (3)
P—Os—H2	69 (2)	C26—C21—P	115.5 (3)
P—Os—H3	96 (2)	C26—C21—H21	108 (3)
P—Os—H4	94 (3)	C26—C21—C22	109.8 (4)
P—Os—C1	107.05 (13)	H22A—C22—C21	112 (3)
P—Os—C2	123.21 (13)	H22B—C22—C21	113 (3)
P—Os—C3	158.87 (15)	H22B—C22—H22A	104 (5)
P—Os—C4	155.70 (14)	C23—C22—C21	111.5 (4)
P—Os—C5	120.91 (13)	C23—C22—H22A	108 (3)
C2—C1—Os	71.4 (3)	C23—C22—H22B	108 (3)
C5—C1—Os	70.4 (3)	H23A—C23—C22	110 (3)
C5—C1—C2	107.7 (4)	H23B—C23—C22	110 (3)
C6—C1—Os	130.6 (4)	H23B—C23—H23A	107 (5)
C6—C1—C2	126.2 (5)	C24—C23—C22	110.4 (4)
C6—C1—C5	125.5 (5)	C24—C23—H23A	108 (3)
C1—C2—Os	72.2 (3)	C24—C23—H23B	112 (3)
C3—C2—Os	69.7 (3)	H24A—C24—C23	111 (4)
C3—C2—C1	108.4 (4)	H24B—C24—C23	112 (3)
C7—C2—Os	131.1 (3)	H24B—C24—H24A	104 (5)
C7—C2—C1	126.5 (5)	C25—C24—C23	110.9 (4)
C7—C2—C3	124.5 (5)	C25—C24—H24A	107 (4)
C2—C3—Os	73.2 (3)	C25—C24—H24B	111 (3)
C4—C3—Os	71.5 (3)	H25A—C25—C24	110 (3)
C4—C3—C2	107.6 (4)	H25B—C25—C24	109 (4)
C8—C3—Os	126.7 (4)	H25B—C25—H25A	104 (5)
C8—C3—C2	126.6 (5)	C26—C25—C24	111.1 (4)
C8—C3—C4	125.3 (5)	C26—C25—H25A	110 (4)
C3—C4—Os	71.0 (3)	C26—C25—H25B	112 (3)
C5—C4—Os	72.1 (3)	C25—C26—C21	110.8 (4)
C5—C4—C3	107.3 (4)	H26A—C26—C21	112 (3)
C9—C4—Os	126.8 (4)	H26A—C26—C25	109 (3)
C9—C4—C3	126.7 (5)	H26B—C26—C21	106 (3)
C9—C4—C5	125.7 (5)	H26B—C26—C25	108 (3)
C1—C5—Os	73.1 (3)	H26B—C26—H26A	111 (5)
C4—C5—Os	70.8 (3)	H31—C31—P	109 (3)
C4—C5—C1	109.0 (4)	C32—C31—P	116.4 (3)
C10—C5—Os	130.5 (4)	C32—C31—H31	106 (3)
C10—C5—C1	126.1 (5)	C36—C31—P	113.1 (3)
C10—C5—C4	124.1 (5)	C36—C31—H31	102 (3)
H6A—C6—C1	107 (4)	C36—C31—C32	109.3 (4)
H6B—C6—C1	110 (4)	H32A—C32—C31	113 (3)
H6B—C6—H6A	107 (6)	H32B—C32—C31	108 (3)
H6C—C6—C1	108 (4)	H32B—C32—H32A	109 (5)
H6C—C6—H6A	105 (5)	C33—C32—C31	110.7 (4)
H6C—C6—H6B	120 (6)	C33—C32—H32A	107 (3)
H8A—C8—C3	114 (4)	C33—C32—H32B	110 (3)
H8B—C8—C3	116 (4)	H33A—C33—C32	114 (3)
H8B—C8—H8A	106 (5)	H33B—C33—C32	118 (4)
H8C—C8—C3	116 (4)	H33B—C33—H33A	107 (5)
H8C—C8—H8A	97 (6)	C34—C33—C32	111.1 (4)
H8C—C8—H8B	106 (5)	C34—C33—H33A	105 (3)
H7A—C7—C2	102 (4)	C34—C33—H33B	99 (3)
H7B—C7—C2	121 (4)	H34A—C34—C33	114 (4)
H7B—C7—H7A	96 (5)	H34B—C34—C33	112 (4)
H7C—C7—C2	111 (4)	H34B—C34—H34A	102 (5)
H7C—C7—H7A	131 (6)	C35—C34—C33	111.2 (4)
H7C—C7—H7B	98 (5)	C35—C34—H34A	106 (4)
H9A—C9—C4	110 (4)	C35—C34—H34B	111 (4)
H9B—C9—C4	113 (4)	H35A—C35—C34	113 (3)
H9B—C9—H9A	109 (6)	H35B—C35—C34	113 (3)
H9C—C9—C4	117 (4)	H35B—C35—H35A	104 (5)
H9C—C9—H9A	100 (6)	C36—C35—C34	110.6 (4)
H9C—C9—H9B	108 (6)	C36—C35—H35A	107 (3)
H10A—C10—C5	112 (4)	C36—C35—H35B	109 (3)
H10B—C10—C5	114 (4)	C35—C36—C31	111.7 (4)
H10B—C10—H10A	106 (5)	H36A—C36—C31	107 (3)
H10C—C10—C5	112 (4)	H36A—C36—C35	112 (3)
H10C—C10—H10A	107 (6)	H36B—C36—C31	114 (3)
H10C—C10—H10B	107 (6)	H36B—C36—C35	112 (3)
C11—P—Os	114.81 (15)	H36B—C36—H36A	99 (4)
C21—P—Os	112.93 (14)	F2—B—F1	108.8 (6)
C21—P—C11	103.9 (2)	F3—B—F1	112.3 (6)
C31—P—Os	111.68 (14)	F3—B—F2	111.1 (7)
C31—P—C11	102.7 (2)	F4—B—F1	107.9 (7)
C31—P—C21	110.1 (2)	F4—B—F2	108.8 (6)
H11—C11—P	106 (3)	F4—B—F3	107.8 (6)
C12—C11—P	112.3 (3)
Os—C1—C2—C3	−60.6 (3)	C1—C5—C4—C9	173.5 (4)
Os—C1—C2—C7	128.4 (3)	C2—C3—C4—C5	1.4 (4)
Os—C1—C5—C4	62.1 (3)	C2—C3—C4—C9	−173.0 (4)
Os—C1—C5—C10	−128.2 (3)	C3—C4—C5—C10	−170.9 (4)
Os—C2—C1—C5	61.4 (3)	P—C11—C12—C13	−177.8 (4)
Os—C2—C1—C6	−127.2 (3)	P—C11—C16—C15	178.7 (4)
Os—C2—C3—C4	−63.6 (3)	P—C21—C22—C23	−171.3 (3)
Os—C2—C3—C8	123.6 (4)	P—C21—C26—C25	172.2 (4)
Os—C3—C2—C1	62.2 (3)	P—C31—C32—C33	−173.4 (4)
Os—C3—C2—C7	−126.6 (3)	P—C31—C36—C35	171.7 (3)
Os—C3—C4—C5	−63.3 (3)	C11—C12—C13—C14	−56.4 (5)
Os—C3—C4—C9	122.2 (4)	C11—C16—C15—C14	56.1 (5)
Os—C4—C3—C2	64.8 (3)	C12—C13—C14—C15	57.2 (5)
Os—C4—C3—C8	−122.3 (4)	C13—C14—C15—C16	−57.3 (5)
Os—C4—C5—C1	−63.6 (3)	C21—C22—C23—C24	−56.7 (4)
Os—C4—C5—C10	126.5 (3)	C21—C26—C25—C24	57.1 (4)
Os—C5—C1—C2	−62.0 (3)	C22—C23—C24—C25	56.3 (4)
Os—C5—C1—C6	126.5 (3)	C23—C24—C25—C26	−56.8 (5)
Os—C5—C4—C3	62.6 (3)	C31—C32—C33—C34	−57.4 (4)
Os—C5—C4—C9	−122.9 (4)	C31—C36—C35—C34	56.5 (4)
C1—C2—C3—C4	−1.4 (4)	C32—C33—C34—C35	56.7 (5)
C1—C2—C3—C8	−174.2 (4)	C33—C34—C35—C36	−55.6 (4)
C1—C5—C4—C3	−1.0 (4)

(XAXMEP_HAR_SHADE3)

Crystal data

C28H52OsP·BF4	V = 1457.79 (4) Å^3
Mr = 696.74	Z = 2
Triclinic, P1	F(000) = 111.426
a = 8.9295 (2) Å	Dx = 1.587 Mg m^−3
b = 9.7179 (1) Å	Mo Kα radiation, λ = 0.71073 Å
c = 17.1819 (1) Å	µ = 4.47 mm^−1
α = 94.114 (1)°	T = 199 K
β = 90.034 (1)°	0.3 × 0.1 × 0.04 mm
γ = 101.369 (1)°

Data collection

Absorption correction: integration	Rint = 0.033
Tmin = 0.529, Tmax = 0.844	θmax = 28.3°, θmin = 2.1°
9506 measured reflections	h = −11→11
6629 independent reflections	k = −12→12
5952 reflections with I ≥ 2u(I)	l = −22→13

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.034	Only H-atom coordinates refined
wR(F^2) = 0.082	w = 1/[σ^2(Fo^2) + (0.0236P)^2 + 6.6604P] where P = (Fo^2 + 2Fc^2)/3
S = 1.09	(Δ/σ)max = 0.001
6629 reflections	Δρmax = 1.22 e Å^−3
472 parameters	Δρmin = −1.52 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Os	0.22260 (2)	0.241115 (19)	0.197802 (10)	0.01847 (6)
H1	0.308 (8)	0.408 (7)	0.226 (4)	0.040913
H2	0.144 (8)	0.111 (7)	0.252 (4)	0.039009
H3	0.347 (8)	0.169 (8)	0.243 (4)	0.042804
H4	0.404 (8)	0.291 (9)	0.229 (4)	0.043268
C1	0.0490 (6)	0.2382 (5)	0.0980 (3)	0.0248 (10)
C2	0.0772 (6)	0.0985 (5)	0.1022 (3)	0.0248 (10)
C3	0.2379 (6)	0.1023 (5)	0.0889 (3)	0.0286 (11)
C4	0.3083 (6)	0.2456 (6)	0.0745 (3)	0.0285 (11)
C5	0.1909 (6)	0.3281 (5)	0.0811 (3)	0.0268 (10)
C6	−0.1043 (7)	0.2791 (7)	0.0988 (4)	0.0381 (13)
H6A	−0.142 (9)	0.278 (8)	0.037 (4)	0.055717
H6B	−0.094 (8)	0.382 (7)	0.123 (4)	0.046981
H6C	−0.190 (8)	0.190 (8)	0.124 (4)	0.047475
C8	0.3148 (9)	−0.0208 (7)	0.0811 (4)	0.0500 (17)
H8A	0.436 (9)	0.001 (8)	0.105 (4)	0.054388
H8B	0.320 (9)	−0.070 (8)	0.020 (4)	0.059867
H8C	0.267 (9)	−0.111 (8)	0.119 (4)	0.051088
C7	−0.0407 (8)	−0.0333 (6)	0.1067 (3)	0.0396 (14)
H7A	0.014 (8)	−0.093 (7)	0.130 (4)	0.041981
H7B	−0.075 (9)	−0.101 (8)	0.056 (4)	0.050742
H7C	−0.152 (8)	−0.008 (7)	0.121 (4)	0.045337
C9	0.4682 (7)	0.2966 (8)	0.0496 (4)	0.0468 (16)
H9A	0.473 (9)	0.293 (9)	−0.016 (4)	0.065899
H9B	0.546 (9)	0.235 (8)	0.070 (4)	0.058765
H9C	0.519 (9)	0.412 (9)	0.064 (5)	0.057630
C10	0.2111 (8)	0.4764 (6)	0.0592 (3)	0.0395 (14)
H10A	0.212 (9)	0.482 (8)	−0.006 (4)	0.060567
H10B	0.320 (8)	0.545 (8)	0.082 (4)	0.053133
H10C	0.119 (8)	0.526 (7)	0.081 (4)	0.051219
P	0.11842 (12)	0.33049 (11)	0.31287 (6)	0.0155 (2)
C11	0.1601 (5)	0.5250 (5)	0.3290 (3)	0.0199 (9)
H11	0.112 (7)	0.550 (6)	0.387 (4)	0.032750
C12	0.3329 (5)	0.5861 (5)	0.3363 (3)	0.0255 (10)
H12A	0.394 (7)	0.531 (6)	0.380 (4)	0.035855
H12B	0.381 (7)	0.557 (7)	0.279 (4)	0.036854
C13	0.3644 (7)	0.7461 (5)	0.3527 (4)	0.0350 (13)
H13A	0.318 (8)	0.777 (7)	0.408 (4)	0.045219
H13B	0.494 (8)	0.789 (7)	0.360 (4)	0.047268
C14	0.2916 (7)	0.8154 (6)	0.2897 (4)	0.0373 (13)
H14A	0.351 (8)	0.799 (7)	0.231 (4)	0.047153
H14B	0.319 (8)	0.928 (7)	0.303 (4)	0.052939
C15	0.1203 (6)	0.7571 (5)	0.2839 (4)	0.0356 (13)
H15A	0.060 (8)	0.807 (7)	0.239 (4)	0.049008
H15B	0.066 (8)	0.780 (7)	0.344 (4)	0.045957
C16	0.0857 (6)	0.5967 (5)	0.2671 (3)	0.0268 (10)
H16A	−0.039 (7)	0.560 (6)	0.265 (4)	0.036761
H16B	0.123 (7)	0.563 (7)	0.208 (4)	0.037484
C21	−0.0928 (5)	0.2831 (4)	0.3143 (3)	0.0180 (8)
H21	−0.127 (7)	0.342 (6)	0.266 (4)	0.031190
C22	−0.1595 (5)	0.1268 (5)	0.2915 (3)	0.0221 (9)
H22A	−0.111 (7)	0.088 (6)	0.234 (4)	0.034084
H22B	−0.132 (7)	0.059 (6)	0.333 (4)	0.034402
C23	−0.3341 (6)	0.0999 (5)	0.2819 (3)	0.0255 (10)
H23A	−0.366 (7)	0.163 (7)	0.232 (4)	0.041365
H23B	−0.381 (7)	−0.019 (7)	0.264 (4)	0.042966
C24	−0.4069 (5)	0.1489 (5)	0.3568 (3)	0.0249 (10)
H24A	−0.532 (7)	0.139 (7)	0.349 (4)	0.049057
H24B	−0.394 (8)	0.076 (7)	0.409 (4)	0.044281
C25	−0.3420 (6)	0.3035 (5)	0.3799 (3)	0.0266 (10)
H25A	−0.394 (7)	0.337 (7)	0.434 (4)	0.047428
H25B	−0.377 (7)	0.367 (7)	0.336 (4)	0.043396
C26	−0.1671 (5)	0.3303 (5)	0.3896 (3)	0.0246 (10)
H26A	−0.126 (7)	0.436 (6)	0.406 (4)	0.036255
H26B	−0.139 (7)	0.260 (6)	0.437 (4)	0.035920
C31	0.2016 (5)	0.2743 (4)	0.4026 (3)	0.0175 (8)
H31	0.333 (7)	0.280 (6)	0.394 (4)	0.030192
C32	0.1877 (6)	0.3638 (5)	0.4797 (3)	0.0215 (9)
H32A	0.233 (7)	0.479 (6)	0.475 (4)	0.035788
H32B	0.066 (7)	0.349 (6)	0.494 (4)	0.036096
C33	0.2765 (6)	0.3167 (5)	0.5461 (3)	0.0273 (10)
H33A	0.407 (8)	0.329 (7)	0.536 (4)	0.041130
H33B	0.261 (8)	0.364 (7)	0.609 (4)	0.045304
C34	0.2204 (6)	0.1606 (5)	0.5576 (3)	0.0249 (10)
H34A	0.284 (8)	0.121 (7)	0.602 (4)	0.046084
H34B	0.109 (8)	0.140 (7)	0.579 (4)	0.042570
C35	0.2317 (6)	0.0698 (5)	0.4823 (3)	0.0246 (10)
H35A	0.180 (8)	−0.053 (7)	0.487 (4)	0.041940
H35B	0.359 (8)	0.072 (7)	0.464 (4)	0.039445
C36	0.1442 (6)	0.1176 (5)	0.4153 (3)	0.0214 (9)
H36A	0.017 (7)	0.103 (6)	0.427 (4)	0.033149
H36B	0.140 (7)	0.051 (6)	0.365 (3)	0.032159
B	0.3092 (9)	0.3653 (8)	0.8135 (4)	0.0425 (16)
F1	0.1955 (6)	0.3609 (5)	0.8668 (3)	0.0739 (14)
F2	0.2644 (6)	0.2599 (6)	0.7558 (3)	0.0906 (17)
F3	0.4452 (6)	0.3549 (7)	0.8468 (3)	0.0953 (18)
F4	0.3292 (7)	0.4933 (6)	0.7811 (4)	0.101 (2)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Os	0.01896 (9)	0.02362 (10)	0.01313 (9)	0.00522 (6)	0.00143 (6)	0.00047 (6)
H1	0.045820	0.032400	0.040130	−0.002680	0.006040	0.001900
H2	0.043450	0.037070	0.033340	−0.000170	0.008230	0.003720
H3	0.046880	0.048390	0.039660	0.022900	0.000500	0.009840
H4	0.025590	0.056920	0.046790	0.007540	−0.002300	0.002110
C1	0.024 (2)	0.030 (3)	0.019 (2)	0.003 (2)	−0.0006 (18)	0.0042 (18)
C2	0.032 (3)	0.028 (2)	0.013 (2)	0.004 (2)	−0.0046 (18)	−0.0013 (17)
C3	0.041 (3)	0.029 (3)	0.018 (2)	0.012 (2)	−0.001 (2)	−0.0021 (18)
C4	0.030 (3)	0.040 (3)	0.016 (2)	0.009 (2)	0.0083 (19)	0.0031 (19)
C5	0.030 (3)	0.033 (3)	0.017 (2)	0.002 (2)	0.0051 (19)	0.0067 (18)
C6	0.029 (3)	0.053 (4)	0.034 (3)	0.010 (3)	−0.009 (2)	0.008 (3)
H6A	0.058700	0.081540	0.029970	0.020610	−0.015180	0.006150
H6B	0.044190	0.040510	0.055750	0.009210	−0.012430	−0.002060
H6C	0.036510	0.053450	0.051740	0.003740	0.000410	0.013340
C8	0.073 (5)	0.049 (4)	0.039 (3)	0.040 (4)	0.009 (3)	−0.002 (3)
H8A	0.050520	0.068020	0.048240	0.026070	0.002030	−0.011310
H8B	0.078930	0.073540	0.029860	0.028860	0.007630	−0.016270
H8C	0.065250	0.048140	0.041440	0.018400	0.009620	−0.006250
C7	0.049 (4)	0.034 (3)	0.029 (3)	−0.006 (3)	−0.009 (3)	0.002 (2)
H7A	0.057760	0.035320	0.032220	0.011440	−0.006070	−0.008100
H7B	0.060370	0.050660	0.038470	0.010270	−0.015430	−0.013160
H7C	0.046660	0.047400	0.039000	0.004820	0.000370	−0.004380
C9	0.035 (3)	0.068 (5)	0.037 (3)	0.010 (3)	0.013 (3)	0.005 (3)
H9A	0.061240	0.108550	0.028600	0.015880	0.016530	0.012120
H9B	0.049510	0.079620	0.053290	0.025060	0.017480	0.011980
H9C	0.046430	0.071020	0.051360	0.001460	0.014970	0.005020
C10	0.055 (4)	0.032 (3)	0.030 (3)	0.003 (3)	0.006 (3)	0.013 (2)
H10A	0.076970	0.073630	0.030100	0.006240	0.001960	0.021150
H10B	0.042240	0.058900	0.055180	−0.003260	−0.002990	0.020350
H10C	0.050900	0.050980	0.055080	0.013100	0.006110	0.017810
P	0.0156 (5)	0.0161 (5)	0.0149 (5)	0.0033 (4)	0.0015 (4)	0.0014 (4)
C11	0.020 (2)	0.019 (2)	0.020 (2)	0.0019 (17)	0.0017 (17)	0.0016 (16)
H11	0.036200	0.029720	0.032000	0.007730	0.002220	−0.003390
C12	0.019 (2)	0.018 (2)	0.039 (3)	0.0017 (17)	−0.002 (2)	0.0043 (19)
H12A	0.033870	0.034350	0.038820	0.003950	−0.006970	0.006980
H12B	0.033330	0.037810	0.036890	0.001700	0.003460	0.000420
C13	0.035 (3)	0.017 (2)	0.050 (3)	−0.001 (2)	−0.011 (3)	0.000 (2)
H13A	0.054980	0.030510	0.047850	0.005740	−0.004820	−0.005260
H13B	0.035130	0.037800	0.064730	−0.003970	−0.007490	0.006910
C14	0.032 (3)	0.020 (2)	0.060 (4)	0.001 (2)	−0.001 (3)	0.011 (2)
H14A	0.046330	0.041110	0.052620	0.002310	−0.001780	0.011660
H14B	0.054480	0.024530	0.076120	−0.003060	−0.009270	0.009110
C15	0.029 (3)	0.022 (2)	0.056 (4)	0.004 (2)	−0.006 (3)	0.010 (2)
H15A	0.049340	0.034330	0.065990	0.009910	−0.010600	0.017100
H15B	0.047890	0.032780	0.056690	0.009580	−0.000560	−0.004670
C16	0.032 (3)	0.024 (2)	0.026 (2)	0.007 (2)	−0.009 (2)	0.0012 (19)
H16A	0.026890	0.034120	0.050290	0.007030	−0.002590	0.007230
H16B	0.043540	0.035560	0.033750	0.007600	−0.000330	0.005870
C21	0.020 (2)	0.016 (2)	0.018 (2)	0.0033 (16)	0.0035 (16)	−0.0015 (16)
H21	0.030020	0.031400	0.033030	0.006700	−0.001820	0.006610
C22	0.019 (2)	0.020 (2)	0.026 (2)	0.0027 (17)	0.0016 (18)	−0.0035 (18)
H22A	0.034820	0.036170	0.029380	0.005250	0.001110	−0.005450
H22B	0.036920	0.030530	0.035030	0.002760	−0.001680	0.008410
C23	0.023 (2)	0.022 (2)	0.028 (3)	−0.0014 (18)	0.0008 (19)	−0.0031 (19)
H23A	0.034990	0.046060	0.043660	0.007640	−0.003480	0.008530
H23B	0.034960	0.035190	0.052320	−0.006490	−0.003590	−0.002920
C24	0.015 (2)	0.029 (2)	0.029 (3)	0.0013 (18)	0.0049 (18)	0.003 (2)
H24A	0.024070	0.056510	0.064640	0.003650	0.003980	0.003210
H24B	0.042030	0.043630	0.045180	0.001370	0.008600	0.009420
C25	0.022 (2)	0.029 (2)	0.029 (3)	0.0061 (19)	0.007 (2)	−0.001 (2)
H25A	0.036080	0.054360	0.051650	0.011790	0.014460	−0.005520
H25B	0.032780	0.043090	0.055860	0.009710	−0.000030	0.007940
C26	0.017 (2)	0.031 (3)	0.024 (2)	0.0047 (19)	0.0048 (18)	−0.0069 (19)
H26A	0.033130	0.030540	0.043300	0.004860	0.003600	−0.005520
H26B	0.038720	0.038970	0.031860	0.010480	0.006630	0.006880
C31	0.017 (2)	0.018 (2)	0.018 (2)	0.0048 (16)	0.0007 (16)	−0.0003 (16)
H31	0.026390	0.035430	0.029780	0.009010	0.000060	0.001240
C32	0.030 (2)	0.022 (2)	0.015 (2)	0.0101 (19)	−0.0039 (18)	−0.0005 (16)
H32A	0.042690	0.027930	0.033800	0.001420	−0.002080	−0.002180
H32B	0.035060	0.043460	0.030660	0.011970	0.004660	−0.003020
C33	0.037 (3)	0.028 (2)	0.015 (2)	0.004 (2)	−0.006 (2)	0.0020 (18)
H33A	0.038680	0.046570	0.038510	0.009520	−0.005750	0.002630
H33B	0.063030	0.046610	0.023900	0.008830	−0.005280	−0.007870
C34	0.027 (3)	0.030 (3)	0.017 (2)	0.005 (2)	−0.0003 (19)	0.0074 (18)
H34A	0.062500	0.049830	0.027620	0.013050	−0.010060	0.009020
H34B	0.048370	0.047360	0.031780	0.008850	0.004680	0.003210
C35	0.032 (3)	0.024 (2)	0.019 (2)	0.009 (2)	0.0020 (19)	0.0030 (18)
H35A	0.057140	0.031080	0.037060	0.005260	−0.003580	0.008530
H35B	0.039920	0.046940	0.035120	0.017700	−0.004350	0.002330
C36	0.033 (3)	0.016 (2)	0.015 (2)	0.0027 (18)	−0.0016 (18)	0.0009 (16)
H36A	0.031200	0.034990	0.034050	0.007530	0.004980	0.005130
H36B	0.043150	0.028940	0.024320	0.008790	−0.000800	−0.003150
B	0.041 (4)	0.054 (4)	0.030 (3)	0.001 (3)	0.009 (3)	0.004 (3)
F1	0.088 (3)	0.072 (3)	0.056 (3)	0.003 (3)	0.030 (2)	−0.004 (2)
F2	0.081 (3)	0.119 (4)	0.065 (3)	0.022 (3)	−0.009 (3)	−0.045 (3)
F3	0.071 (3)	0.138 (5)	0.081 (4)	0.032 (3)	−0.030 (3)	0.008 (3)
F4	0.087 (4)	0.099 (4)	0.122 (5)	0.010 (3)	0.010 (4)	0.065 (4)

Geometric parameters (Å, º)

Os—H1	1.69 (6)	C14—H14A	1.15 (7)
Os—H2	1.67 (6)	C14—H14B	1.08 (6)
Os—H3	1.65 (7)	C14—C15	1.523 (8)
Os—H4	1.67 (7)	C15—H15A	1.14 (7)
Os—C1	2.306 (5)	C15—H15B	1.17 (7)
Os—C2	2.294 (4)	C15—C16	1.534 (7)
Os—C3	2.247 (5)	C16—H16A	1.10 (6)
Os—C4	2.254 (5)	C16—H16B	1.11 (6)
Os—C5	2.270 (5)	C21—H21	1.12 (6)
Os—P	2.3671 (11)	C21—C22	1.540 (6)
C1—C2	1.436 (7)	C21—C26	1.536 (6)
C1—C5	1.433 (7)	C22—H22A	1.15 (6)
C1—C6	1.499 (7)	C22—H22B	1.06 (6)
C2—C3	1.447 (7)	C22—C23	1.536 (7)
C2—C7	1.496 (7)	C23—H23A	1.15 (7)
C3—C4	1.450 (7)	C23—H23B	1.17 (6)
C3—C8	1.491 (8)	C23—C24	1.530 (7)
C4—C5	1.439 (7)	C24—H24A	1.11 (6)
C4—C9	1.490 (8)	C24—H24B	1.20 (7)
C5—C10	1.492 (7)	C24—C25	1.524 (7)
C6—H6A	1.11 (7)	C25—H25A	1.09 (6)
C6—H6B	1.04 (7)	C25—H25B	1.09 (7)
C6—H6C	1.15 (7)	C25—C26	1.539 (7)
C8—H8A	1.13 (8)	C26—H26A	1.04 (6)
C8—H8B	1.13 (7)	C26—H26B	1.15 (6)
C8—H8C	1.14 (8)	C31—H31	1.18 (6)
C7—H7A	0.94 (7)	C31—C32	1.550 (6)
C7—H7B	1.05 (7)	C31—C36	1.539 (6)
C7—H7C	1.09 (7)	C32—H32A	1.12 (6)
C9—H9A	1.12 (7)	C32—H32B	1.10 (6)
C9—H9B	1.07 (8)	C32—C33	1.534 (6)
C9—H9C	1.14 (8)	C33—H33A	1.16 (7)
C10—H10A	1.12 (7)	C33—H33B	1.16 (6)
C10—H10B	1.12 (7)	C33—C34	1.529 (7)
C10—H10C	1.09 (7)	C34—H34A	1.08 (6)
P—C11	1.854 (5)	C34—H34B	1.05 (7)
P—C21	1.852 (5)	C34—C35	1.528 (7)
P—C31	1.873 (5)	C35—H35A	1.20 (6)
C11—H11	1.11 (6)	C35—H35B	1.18 (7)
C11—C12	1.542 (6)	C35—C36	1.539 (6)
C11—C16	1.532 (6)	C36—H36A	1.13 (6)
C12—H12A	1.15 (6)	C36—H36B	1.04 (6)
C12—H12B	1.11 (6)	B—F1	1.365 (8)
C12—C13	1.530 (7)	B—F2	1.372 (9)
C13—H13A	1.08 (7)	B—F3	1.366 (9)
C13—H13B	1.15 (6)	B—F4	1.379 (9)
C13—C14	1.525 (8)
H2—Os—H1	130 (3)	C12—C11—H11	106 (3)
H3—Os—H1	95 (4)	C16—C11—P	112.9 (3)
H3—Os—H2	66 (3)	C16—C11—H11	108 (3)
H4—Os—H1	55 (3)	C16—C11—C12	110.8 (4)
H4—Os—H2	106 (4)	H12A—C12—C11	113 (3)
H4—Os—H3	44 (3)	H12B—C12—C11	105 (3)
C1—Os—H1	110 (2)	H12B—C12—H12A	103 (5)
C1—Os—H2	105 (2)	C13—C12—C11	111.4 (4)
C1—Os—H3	151 (3)	C13—C12—H12A	113 (3)
C1—Os—H4	147 (3)	C13—C12—H12B	111 (3)
C2—Os—H1	145 (2)	H13A—C13—C12	112 (3)
C2—Os—H2	82 (2)	H13B—C13—C12	110 (3)
C2—Os—H3	115 (3)	H13B—C13—H13A	104 (5)
C2—Os—H4	141 (3)	C14—C13—C12	110.8 (5)
C2—Os—C1	36.37 (17)	C14—C13—H13A	107 (4)
C3—Os—H1	132 (2)	C14—C13—H13B	113 (4)
C3—Os—H2	96 (2)	H14A—C14—C13	109 (4)
C3—Os—H3	91 (3)	H14B—C14—C13	108 (4)
C3—Os—H4	104 (3)	H14B—C14—H14A	104 (5)
C3—Os—C1	61.77 (18)	C15—C14—C13	110.4 (5)
C3—Os—C2	37.13 (19)	C15—C14—H14A	112 (4)
C4—Os—H1	95 (2)	C15—C14—H14B	113 (4)
C4—Os—H2	133 (2)	H15A—C15—C14	113 (4)
C4—Os—H3	103 (2)	H15B—C15—C14	109 (3)
C4—Os—H4	88 (3)	H15B—C15—H15A	107 (5)
C4—Os—C1	61.70 (18)	C16—C15—C14	111.5 (5)
C4—Os—C2	61.85 (18)	C16—C15—H15A	109 (3)
C4—Os—C3	37.59 (19)	C16—C15—H15B	107 (3)
C5—Os—H1	84 (2)	C15—C16—C11	111.0 (4)
C5—Os—H2	141 (2)	H16A—C16—C11	111 (3)
C5—Os—H3	139 (3)	H16A—C16—C15	109 (3)
C5—Os—H4	111 (3)	H16B—C16—C11	109 (3)
C5—Os—C1	36.49 (17)	H16B—C16—C15	113 (3)
C5—Os—C2	60.98 (17)	H16B—C16—H16A	104 (5)
C5—Os—C3	62.01 (18)	H21—C21—P	103 (3)
C5—Os—C4	37.09 (18)	C22—C21—P	114.5 (3)
P—Os—H1	67 (2)	C22—C21—H21	105 (3)
P—Os—H2	69 (2)	C26—C21—P	115.5 (3)
P—Os—H3	96 (2)	C26—C21—H21	108 (3)
P—Os—H4	94 (3)	C26—C21—C22	109.8 (4)
P—Os—C1	107.05 (13)	H22A—C22—C21	112 (3)
P—Os—C2	123.21 (13)	H22B—C22—C21	113 (3)
P—Os—C3	158.87 (15)	H22B—C22—H22A	104 (5)
P—Os—C4	155.70 (14)	C23—C22—C21	111.5 (4)
P—Os—C5	120.91 (13)	C23—C22—H22A	108 (3)
C2—C1—Os	71.4 (3)	C23—C22—H22B	108 (3)
C5—C1—Os	70.4 (3)	H23A—C23—C22	110 (3)
C5—C1—C2	107.7 (4)	H23B—C23—C22	110 (3)
C6—C1—Os	130.6 (4)	H23B—C23—H23A	107 (5)
C6—C1—C2	126.2 (5)	C24—C23—C22	110.4 (4)
C6—C1—C5	125.5 (5)	C24—C23—H23A	108 (3)
C1—C2—Os	72.2 (3)	C24—C23—H23B	112 (3)
C3—C2—Os	69.7 (3)	H24A—C24—C23	111 (4)
C3—C2—C1	108.4 (4)	H24B—C24—C23	112 (3)
C7—C2—Os	131.1 (3)	H24B—C24—H24A	104 (5)
C7—C2—C1	126.5 (5)	C25—C24—C23	110.9 (4)
C7—C2—C3	124.5 (5)	C25—C24—H24A	107 (4)
C2—C3—Os	73.2 (3)	C25—C24—H24B	111 (3)
C4—C3—Os	71.5 (3)	H25A—C25—C24	110 (4)
C4—C3—C2	107.6 (4)	H25B—C25—C24	109 (4)
C8—C3—Os	126.7 (4)	H25B—C25—H25A	104 (5)
C8—C3—C2	126.6 (5)	C26—C25—C24	111.1 (4)
C8—C3—C4	125.3 (5)	C26—C25—H25A	110 (4)
C3—C4—Os	71.0 (3)	C26—C25—H25B	112 (3)
C5—C4—Os	72.1 (3)	C25—C26—C21	110.8 (4)
C5—C4—C3	107.3 (4)	H26A—C26—C21	112 (3)
C9—C4—Os	126.8 (4)	H26A—C26—C25	109 (3)
C9—C4—C3	126.7 (5)	H26B—C26—C21	106 (3)
C9—C4—C5	125.7 (5)	H26B—C26—C25	108 (3)
C1—C5—Os	73.1 (3)	H26B—C26—H26A	111 (5)
C4—C5—Os	70.8 (3)	H31—C31—P	109 (3)
C4—C5—C1	109.0 (4)	C32—C31—P	116.4 (3)
C10—C5—Os	130.5 (4)	C32—C31—H31	106 (3)
C10—C5—C1	126.1 (5)	C36—C31—P	113.1 (3)
C10—C5—C4	124.1 (5)	C36—C31—H31	102 (3)
H6A—C6—C1	107 (4)	C36—C31—C32	109.3 (4)
H6B—C6—C1	110 (4)	H32A—C32—C31	113 (3)
H6B—C6—H6A	107 (6)	H32B—C32—C31	108 (3)
H6C—C6—C1	108 (4)	H32B—C32—H32A	108 (5)
H6C—C6—H6A	105 (5)	C33—C32—C31	110.7 (4)
H6C—C6—H6B	120 (6)	C33—C32—H32A	107 (3)
H8A—C8—C3	114 (4)	C33—C32—H32B	110 (3)
H8B—C8—C3	116 (4)	H33A—C33—C32	114 (3)
H8B—C8—H8A	106 (5)	H33B—C33—C32	118 (4)
H8C—C8—C3	116 (4)	H33B—C33—H33A	107 (5)
H8C—C8—H8A	97 (6)	C34—C33—C32	111.1 (4)
H8C—C8—H8B	106 (5)	C34—C33—H33A	105 (3)
H7A—C7—C2	102 (4)	C34—C33—H33B	99 (4)
H7B—C7—C2	121 (4)	H34A—C34—C33	114 (4)
H7B—C7—H7A	96 (5)	H34B—C34—C33	112 (4)
H7C—C7—C2	111 (4)	H34B—C34—H34A	102 (5)
H7C—C7—H7A	131 (6)	C35—C34—C33	111.2 (4)
H7C—C7—H7B	98 (5)	C35—C34—H34A	106 (4)
H9A—C9—C4	110 (4)	C35—C34—H34B	111 (4)
H9B—C9—C4	113 (4)	H35A—C35—C34	113 (3)
H9B—C9—H9A	109 (6)	H35B—C35—C34	113 (3)
H9C—C9—C4	117 (4)	H35B—C35—H35A	104 (5)
H9C—C9—H9A	100 (6)	C36—C35—C34	110.6 (4)
H9C—C9—H9B	108 (6)	C36—C35—H35A	107 (3)
H10A—C10—C5	112 (4)	C36—C35—H35B	109 (3)
H10B—C10—C5	114 (4)	C35—C36—C31	111.7 (4)
H10B—C10—H10A	106 (5)	H36A—C36—C31	107 (3)
H10C—C10—C5	111 (4)	H36A—C36—C35	112 (3)
H10C—C10—H10A	107 (6)	H36B—C36—C31	114 (3)
H10C—C10—H10B	107 (6)	H36B—C36—C35	112 (3)
C11—P—Os	114.81 (15)	H36B—C36—H36A	99 (4)
C21—P—Os	112.93 (14)	F2—B—F1	108.8 (6)
C21—P—C11	103.9 (2)	F3—B—F1	112.3 (6)
C31—P—Os	111.68 (14)	F3—B—F2	111.2 (7)
C31—P—C11	102.7 (2)	F4—B—F1	107.9 (7)
C31—P—C21	110.1 (2)	F4—B—F2	108.8 (6)
H11—C11—P	106 (3)	F4—B—F3	107.8 (6)
C12—C11—P	112.3 (3)
Os—C1—C2—C3	−60.6 (3)	C1—C5—C4—C9	173.6 (4)
Os—C1—C2—C7	128.4 (3)	C2—C3—C4—C5	1.4 (4)
Os—C1—C5—C4	62.1 (3)	C2—C3—C4—C9	−173.0 (4)
Os—C1—C5—C10	−128.2 (3)	C3—C4—C5—C10	−170.9 (4)
Os—C2—C1—C5	61.4 (3)	P—C11—C12—C13	−177.8 (4)
Os—C2—C1—C6	−127.2 (3)	P—C11—C16—C15	178.7 (4)
Os—C2—C3—C4	−63.6 (3)	P—C21—C22—C23	−171.3 (3)
Os—C2—C3—C8	123.6 (4)	P—C21—C26—C25	172.2 (4)
Os—C3—C2—C1	62.2 (3)	P—C31—C32—C33	−173.4 (4)
Os—C3—C2—C7	−126.6 (3)	P—C31—C36—C35	171.7 (3)
Os—C3—C4—C5	−63.3 (3)	C11—C12—C13—C14	−56.4 (5)
Os—C3—C4—C9	122.2 (4)	C11—C16—C15—C14	56.2 (5)
Os—C4—C3—C2	64.8 (3)	C12—C13—C14—C15	57.2 (5)
Os—C4—C3—C8	−122.3 (4)	C13—C14—C15—C16	−57.3 (5)
Os—C4—C5—C1	−63.6 (3)	C21—C22—C23—C24	−56.7 (4)
Os—C4—C5—C10	126.5 (3)	C21—C26—C25—C24	57.1 (4)
Os—C5—C1—C2	−62.0 (3)	C22—C23—C24—C25	56.3 (4)
Os—C5—C1—C6	126.5 (3)	C23—C24—C25—C26	−56.8 (5)
Os—C5—C4—C3	62.6 (3)	C31—C32—C33—C34	−57.4 (4)
Os—C5—C4—C9	−122.9 (4)	C31—C36—C35—C34	56.5 (4)
C1—C2—C3—C4	−1.4 (4)	C32—C33—C34—C35	56.6 (5)
C1—C2—C3—C8	−174.2 (4)	C33—C34—C35—C36	−55.6 (4)
C1—C5—C4—C3	−1.0 (4)

(XAXMEP_IAM_0_HADPs)

Crystal data

C28H52OsP·BF4	V = 1457.79 (4) Å^3
Mr = 696.74	Z = 2
Triclinic, P1	F(000) = 111.479
a = 8.9295 (2) Å	Dx = 1.587 Mg m^−3
b = 9.7179 (1) Å	Mo Kα radiation, λ = 0.71073 Å
c = 17.1819 (1) Å	µ = 4.47 mm^−1
α = 94.114 (1)°	T = 199 K
β = 90.034 (1)°	0.3 × 0.1 × 0.04 mm
γ = 101.369 (1)°

Data collection

Absorption correction: integration	Rint = 0.033
Tmin = 0.529, Tmax = 0.844	θmax = 28.3°, θmin = 2.1°
9506 measured reflections	h = −11→11
6629 independent reflections	k = −12→12
5952 reflections with I ≥ 2u(I)	l = −22→13

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.035	Only H-atom coordinates refined
wR(F^2) = 0.084	w = 1/[σ^2(Fo^2) + (0.0212P)^2 + 8.1935P] where P = (Fo^2 + 2Fc^2)/3
S = 1.08	(Δ/σ)max = 0.001
6629 reflections	Δρmax = 0.90 e Å^−3
472 parameters	Δρmin = −1.54 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Os	0.22259 (2)	0.24111 (2)	0.197793 (11)	0.01880 (6)
H	0.308 (5)	0.400 (4)	0.226 (3)	0.000000
Ha	0.142 (5)	0.127 (4)	0.254 (3)	0.000000
Hb	0.343 (5)	0.172 (4)	0.241 (3)	0.000000
Hc	0.398 (5)	0.299 (4)	0.227 (3)	0.000000
C1	0.0491 (6)	0.2379 (6)	0.0980 (3)	0.0241 (10)
C2	0.0775 (6)	0.0987 (5)	0.1021 (3)	0.0243 (10)
C3	0.2376 (7)	0.1025 (6)	0.0888 (3)	0.0280 (11)
C4	0.3079 (6)	0.2453 (6)	0.0744 (3)	0.0277 (11)
C5	0.1909 (6)	0.3277 (6)	0.0810 (3)	0.0262 (11)
C6	−0.1040 (7)	0.2794 (8)	0.0990 (4)	0.0367 (13)
H6a	−0.132 (5)	0.278 (4)	0.047 (3)	0.000000
H6b	−0.099 (5)	0.370 (5)	0.119 (3)	0.000000
H6c	−0.180 (5)	0.202 (5)	0.123 (3)	0.000000
C8	0.3144 (10)	−0.0207 (8)	0.0811 (4)	0.0483 (18)
H8a	0.416 (5)	−0.002 (5)	0.102 (3)	0.000000
H8b	0.318 (5)	−0.059 (5)	0.031 (3)	0.000000
H8c	0.274 (5)	−0.089 (5)	0.114 (3)	0.000000
C7	−0.0401 (9)	−0.0335 (7)	0.1067 (4)	0.0374 (14)
H7a	0.011 (5)	−0.081 (5)	0.126 (3)	0.000000
H7b	−0.063 (5)	−0.094 (5)	0.059 (3)	0.000000
H7c	−0.124 (6)	−0.014 (5)	0.117 (3)	0.000000
C9	0.4678 (8)	0.2963 (9)	0.0495 (4)	0.0445 (16)
H9a	0.467 (5)	0.291 (4)	−0.009 (3)	0.000000
H9b	0.531 (5)	0.238 (5)	0.067 (3)	0.000000
H9c	0.510 (5)	0.390 (5)	0.063 (3)	0.000000
C10	0.2104 (8)	0.4764 (7)	0.0593 (4)	0.0379 (14)
H10a	0.214 (5)	0.475 (4)	0.005 (3)	0.000000
H10b	0.302 (5)	0.531 (5)	0.077 (3)	0.000000
H10c	0.128 (5)	0.520 (5)	0.079 (3)	0.000000
P	0.11848 (13)	0.33052 (12)	0.31286 (7)	0.0149 (2)
C11	0.1600 (5)	0.5250 (5)	0.3289 (3)	0.0190 (9)
H11	0.118 (5)	0.547 (4)	0.378 (3)	0.000000
C12	0.3329 (6)	0.5863 (5)	0.3362 (3)	0.0244 (10)
H12a	0.384 (5)	0.538 (5)	0.373 (3)	0.000000
H12b	0.376 (5)	0.561 (5)	0.289 (3)	0.000000
C13	0.3644 (7)	0.7462 (6)	0.3525 (4)	0.0336 (13)
H13a	0.323 (5)	0.771 (5)	0.398 (3)	0.000000
H13b	0.477 (5)	0.787 (5)	0.357 (3)	0.000000
C14	0.2916 (7)	0.8153 (6)	0.2898 (4)	0.0355 (13)
H14a	0.340 (5)	0.800 (5)	0.241 (3)	0.000000
H14b	0.311 (5)	0.911 (5)	0.303 (3)	0.000000
C15	0.1204 (7)	0.7572 (6)	0.2841 (4)	0.0343 (13)
H15a	0.068 (5)	0.799 (5)	0.243 (3)	0.000000
H15b	0.071 (5)	0.779 (4)	0.338 (3)	0.000000
C16	0.0860 (6)	0.5969 (5)	0.2671 (3)	0.0256 (11)
H16a	−0.023 (5)	0.564 (5)	0.267 (3)	0.000000
H16b	0.116 (5)	0.565 (4)	0.215 (3)	0.000000
C21	−0.0928 (5)	0.2831 (5)	0.3143 (3)	0.0172 (9)
H21	−0.125 (5)	0.335 (5)	0.271 (3)	0.000000
C22	−0.1598 (5)	0.1268 (5)	0.2915 (3)	0.0212 (10)
H22a	−0.122 (5)	0.093 (5)	0.243 (3)	0.000000
H22b	−0.135 (5)	0.068 (5)	0.329 (3)	0.000000
C23	−0.3342 (6)	0.1001 (5)	0.2821 (3)	0.0247 (10)
H23a	−0.365 (5)	0.151 (5)	0.238 (3)	0.000000
H23b	−0.378 (5)	−0.004 (5)	0.266 (3)	0.000000
C24	−0.4067 (5)	0.1489 (5)	0.3567 (3)	0.0239 (10)
H24a	−0.514 (5)	0.143 (4)	0.349 (3)	0.000000
H24b	−0.393 (5)	0.086 (4)	0.407 (3)	0.000000
C25	−0.3419 (6)	0.3033 (6)	0.3799 (3)	0.0257 (10)
H25a	−0.387 (5)	0.337 (4)	0.427 (3)	0.000000
H25b	−0.367 (5)	0.355 (5)	0.341 (3)	0.000000
C26	−0.1673 (6)	0.3300 (6)	0.3896 (3)	0.0236 (10)
H26a	−0.129 (5)	0.419 (5)	0.404 (3)	0.000000
H26b	−0.140 (5)	0.266 (5)	0.431 (3)	0.000000
C31	0.2015 (5)	0.2742 (5)	0.4025 (3)	0.0167 (9)
H31	0.324 (5)	0.278 (5)	0.397 (3)	0.000000
C32	0.1878 (6)	0.3637 (5)	0.4798 (3)	0.0204 (9)
H32a	0.228 (5)	0.464 (5)	0.473 (3)	0.000000
H32b	0.080 (5)	0.349 (4)	0.494 (3)	0.000000
C33	0.2766 (7)	0.3166 (6)	0.5459 (3)	0.0266 (11)
H33a	0.399 (5)	0.330 (4)	0.532 (3)	0.000000
H33b	0.268 (5)	0.362 (5)	0.596 (3)	0.000000
C34	0.2205 (6)	0.1607 (6)	0.5575 (3)	0.0240 (10)
H34a	0.279 (5)	0.123 (5)	0.594 (3)	0.000000
H34b	0.123 (5)	0.145 (5)	0.575 (3)	0.000000
C35	0.2317 (6)	0.0702 (5)	0.4824 (3)	0.0239 (10)
H35a	0.187 (5)	−0.039 (5)	0.490 (3)	0.000000
H35b	0.340 (5)	0.072 (4)	0.466 (3)	0.000000
C36	0.1442 (6)	0.1175 (5)	0.4154 (3)	0.0206 (9)
H36a	0.031 (5)	0.107 (4)	0.425 (3)	0.000000
H36b	0.142 (5)	0.060 (5)	0.369 (3)	0.000000
B	0.3095 (9)	0.3657 (9)	0.8136 (4)	0.0418 (17)
F1	0.1953 (6)	0.3612 (5)	0.8669 (3)	0.0714 (14)
F2	0.2643 (6)	0.2596 (7)	0.7558 (3)	0.0881 (18)
F3	0.4455 (6)	0.3554 (7)	0.8467 (3)	0.0917 (18)
F4	0.3290 (7)	0.4934 (6)	0.7810 (4)	0.098 (2)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Os	0.01931 (10)	0.02394 (10)	0.01344 (9)	0.00525 (7)	0.00143 (6)	0.00051 (6)
H	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
Ha	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
Hb	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
Hc	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C1	0.025 (3)	0.031 (3)	0.016 (2)	0.004 (2)	−0.0015 (19)	0.0035 (19)
C2	0.032 (3)	0.030 (3)	0.009 (2)	0.005 (2)	−0.0056 (19)	−0.0022 (18)
C3	0.042 (3)	0.030 (3)	0.014 (2)	0.013 (2)	−0.002 (2)	−0.0032 (19)
C4	0.031 (3)	0.041 (3)	0.012 (2)	0.009 (2)	0.0068 (19)	0.002 (2)
C5	0.031 (3)	0.034 (3)	0.013 (2)	0.003 (2)	0.0044 (19)	0.0062 (19)
C6	0.030 (3)	0.050 (4)	0.031 (3)	0.009 (3)	−0.009 (2)	0.008 (3)
H6a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H6b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H6c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C8	0.070 (5)	0.050 (4)	0.035 (4)	0.038 (4)	0.008 (3)	−0.002 (3)
H8a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H8b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H8c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C7	0.043 (4)	0.035 (3)	0.030 (3)	−0.002 (3)	−0.009 (3)	0.002 (3)
H7a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H7b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H7c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C9	0.036 (4)	0.061 (5)	0.036 (4)	0.010 (3)	0.011 (3)	0.004 (3)
H9a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H9b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H9c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C10	0.052 (4)	0.033 (3)	0.028 (3)	0.002 (3)	0.005 (3)	0.013 (2)
H10a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H10b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H10c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
P	0.0150 (5)	0.0154 (5)	0.0143 (5)	0.0032 (4)	0.0016 (4)	0.0014 (4)
C11	0.020 (2)	0.018 (2)	0.018 (2)	0.0018 (18)	0.0025 (18)	0.0004 (17)
H11	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C12	0.019 (2)	0.018 (2)	0.037 (3)	0.0031 (18)	−0.002 (2)	0.004 (2)
H12a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H12b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C13	0.033 (3)	0.017 (2)	0.048 (4)	−0.001 (2)	−0.009 (3)	−0.001 (2)
H13a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H13b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C14	0.032 (3)	0.018 (3)	0.056 (4)	0.002 (2)	0.000 (3)	0.009 (2)
H14a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H14b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C15	0.029 (3)	0.022 (3)	0.053 (4)	0.005 (2)	−0.007 (3)	0.010 (2)
H15a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H15b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C16	0.029 (3)	0.024 (3)	0.024 (3)	0.007 (2)	−0.009 (2)	0.0011 (19)
H16a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H16b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C21	0.019 (2)	0.015 (2)	0.017 (2)	0.0034 (17)	0.0033 (17)	−0.0006 (16)
H21	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C22	0.019 (2)	0.019 (2)	0.025 (2)	0.0026 (18)	0.0016 (19)	−0.0036 (19)
H22a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H22b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C23	0.023 (3)	0.020 (2)	0.027 (3)	−0.0014 (19)	0.000 (2)	−0.0025 (19)
H23a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H23b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C24	0.013 (2)	0.029 (3)	0.029 (3)	0.0015 (19)	0.0040 (19)	0.004 (2)
H24a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H24b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C25	0.022 (2)	0.028 (3)	0.028 (3)	0.007 (2)	0.007 (2)	−0.001 (2)
H25a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H25b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C26	0.017 (2)	0.028 (3)	0.025 (3)	0.004 (2)	0.0039 (19)	−0.007 (2)
H26a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H26b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C31	0.016 (2)	0.017 (2)	0.017 (2)	0.0047 (17)	0.0005 (17)	0.0000 (16)
H31	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C32	0.028 (3)	0.021 (2)	0.014 (2)	0.0094 (19)	−0.0033 (18)	−0.0006 (17)
H32a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H32b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C33	0.037 (3)	0.028 (3)	0.014 (2)	0.004 (2)	−0.006 (2)	0.0010 (19)
H33a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H33b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C34	0.025 (3)	0.030 (3)	0.018 (2)	0.005 (2)	−0.0001 (19)	0.0078 (19)
H34a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H34b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C35	0.030 (3)	0.023 (2)	0.020 (2)	0.008 (2)	0.003 (2)	0.0037 (19)
H35a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H35b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C36	0.030 (3)	0.016 (2)	0.015 (2)	0.0025 (19)	−0.0016 (19)	0.0007 (17)
H36a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H36b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
B	0.042 (4)	0.052 (4)	0.029 (3)	0.002 (3)	0.009 (3)	0.004 (3)
F1	0.085 (4)	0.069 (3)	0.054 (3)	0.003 (3)	0.030 (3)	−0.004 (2)
F2	0.079 (4)	0.115 (5)	0.064 (3)	0.021 (3)	−0.009 (3)	−0.045 (3)
F3	0.068 (3)	0.132 (5)	0.079 (4)	0.028 (3)	−0.030 (3)	0.009 (4)
F4	0.084 (4)	0.094 (4)	0.120 (5)	0.010 (3)	0.010 (4)	0.064 (4)

Geometric parameters (Å, º)

Os—H	1.62 (4)	C14—H14a	0.95 (5)
Os—Ha	1.59 (4)	C14—H14b	0.92 (4)
Os—Hb	1.58 (4)	C14—C15	1.522 (8)
Os—Hc	1.62 (4)	C15—H15a	1.00 (4)
Os—C1	2.304 (5)	C15—H15b	1.06 (4)
Os—C2	2.294 (5)	C15—C16	1.533 (7)
Os—C3	2.248 (5)	C16—H16a	0.96 (4)
Os—C4	2.254 (5)	C16—H16b	0.98 (5)
Os—C5	2.270 (5)	C21—H21	1.00 (4)
Os—P	2.3669 (11)	C21—C22	1.541 (6)
C1—C2	1.431 (7)	C21—C26	1.536 (6)
C1—C5	1.433 (7)	C22—H22a	0.96 (5)
C1—C6	1.500 (8)	C22—H22b	0.94 (5)
C2—C3	1.441 (8)	C22—C23	1.534 (7)
C2—C7	1.498 (8)	C23—H23a	1.00 (4)
C3—C4	1.445 (8)	C23—H23b	1.03 (4)
C3—C8	1.491 (8)	C23—C24	1.524 (7)
C4—C5	1.436 (8)	C24—H24a	0.96 (4)
C4—C9	1.490 (8)	C24—H24b	1.12 (4)
C5—C10	1.496 (8)	C24—C25	1.522 (7)
C6—H6a	0.93 (5)	C25—H25a	0.97 (4)
C6—H6b	0.91 (5)	C25—H25b	0.92 (5)
C6—H6c	1.02 (4)	C25—C26	1.536 (7)
C8—H8a	0.96 (5)	C26—H26a	0.88 (5)
C8—H8b	0.91 (5)	C26—H26b	1.04 (4)
C8—H8c	0.93 (5)	C31—H31	1.10 (4)
C7—H7a	0.79 (5)	C31—C32	1.554 (6)
C7—H7b	0.97 (5)	C31—C36	1.540 (6)
C7—H7c	0.82 (5)	C32—H32a	0.99 (4)
C9—H9a	1.00 (5)	C32—H32b	0.98 (4)
C9—H9b	0.94 (5)	C32—C33	1.532 (7)
C9—H9c	0.93 (5)	C33—H33a	1.10 (4)
C10—H10a	0.93 (5)	C33—H33b	0.95 (4)
C10—H10b	0.92 (5)	C33—C34	1.527 (7)
C10—H10c	0.97 (5)	C34—H34a	0.96 (5)
P—C11	1.853 (5)	C34—H34b	0.91 (5)
P—C21	1.852 (5)	C34—C35	1.524 (7)
P—C31	1.871 (5)	C35—H35a	1.08 (4)
C11—H11	0.94 (5)	C35—H35b	1.00 (4)
C11—C12	1.543 (7)	C35—C36	1.537 (7)
C11—C16	1.531 (7)	C36—H36a	1.01 (4)
C12—H12a	0.98 (5)	C36—H36b	0.93 (5)
C12—H12b	0.94 (5)	B—F1	1.368 (8)
C12—C13	1.529 (7)	B—F2	1.379 (9)
C13—H13a	0.91 (5)	B—F3	1.366 (9)
C13—H13b	1.01 (4)	B—F4	1.377 (9)
C13—C14	1.520 (9)
Ha—Os—H	125 (2)	C12—C11—H11	106 (3)
Hb—Os—H	93 (2)	C16—C11—P	113.0 (3)
Hb—Os—Ha	68 (2)	C16—C11—H11	108 (3)
Hc—Os—H	51 (2)	C16—C11—C12	110.6 (4)
Hc—Os—Ha	109 (2)	H12a—C12—C11	112 (3)
Hc—Os—Hb	47 (2)	H12b—C12—C11	107 (3)
C1—Os—H	111.8 (15)	H12b—C12—H12a	101 (4)
C1—Os—Ha	105.7 (16)	C13—C12—C11	111.5 (4)
C1—Os—Hb	151.1 (16)	C13—C12—H12a	114 (3)
C1—Os—Hc	144.5 (15)	C13—C12—H12b	111 (3)
C2—Os—H	146.0 (15)	H13a—C13—C12	111 (3)
C2—Os—Ha	84.4 (15)	H13b—C13—C12	112 (3)
C2—Os—Hb	115.6 (15)	H13b—C13—H13a	107 (4)
C2—Os—Hc	142.2 (15)	C14—C13—C12	110.9 (5)
C2—Os—C1	36.26 (18)	C14—C13—H13a	106 (3)
C3—Os—H	132.5 (15)	C14—C13—H13b	110 (3)
C3—Os—Ha	100.3 (15)	H14a—C14—C13	109 (3)
C3—Os—Hb	91.0 (16)	H14b—C14—C13	107 (3)
C3—Os—Hc	105.2 (15)	H14b—C14—H14a	108 (4)
C3—Os—C1	61.57 (19)	C15—C14—C13	110.5 (5)
C3—Os—C2	37.0 (2)	C15—C14—H14a	111 (3)
C4—Os—H	95.9 (15)	C15—C14—H14b	111 (3)
C4—Os—Ha	137.7 (15)	H15a—C15—C14	113 (3)
C4—Os—Hb	102.8 (16)	H15b—C15—C14	109 (2)
C4—Os—Hc	87.6 (15)	H15b—C15—H15a	108 (3)
C4—Os—C1	61.60 (19)	C16—C15—C14	111.4 (5)
C4—Os—C2	61.64 (19)	C16—C15—H15a	108 (3)
C4—Os—C3	37.4 (2)	C16—C15—H15b	107 (2)
C5—Os—H	85.7 (15)	C15—C16—C11	111.0 (4)
C5—Os—Ha	141.8 (16)	H16a—C16—C11	110 (3)
C5—Os—Hb	138.9 (16)	H16a—C16—C15	109 (3)
C5—Os—Hc	108.0 (15)	H16b—C16—C11	109 (3)
C5—Os—C1	36.50 (18)	H16b—C16—C15	114 (3)
C5—Os—C2	60.82 (19)	H16b—C16—H16a	103 (4)
C5—Os—C3	61.80 (19)	H21—C21—P	103 (2)
C5—Os—C4	37.01 (19)	C22—C21—P	114.6 (3)
P—Os—H	67.2 (15)	C22—C21—H21	105 (2)
P—Os—Ha	64.1 (15)	C26—C21—P	115.6 (3)
P—Os—Hb	95.7 (16)	C26—C21—H21	108 (3)
P—Os—Hc	93.9 (15)	C26—C21—C22	109.6 (4)
P—Os—C1	107.12 (13)	H22a—C22—C21	113 (3)
P—Os—C2	123.31 (14)	H22b—C22—C21	112 (3)
P—Os—C3	158.86 (15)	H22b—C22—H22a	105 (4)
P—Os—C4	155.74 (15)	C23—C22—C21	111.5 (4)
P—Os—C5	121.00 (14)	C23—C22—H22a	106 (3)
C2—C1—Os	71.5 (3)	C23—C22—H22b	108 (3)
C5—C1—Os	70.4 (3)	H23a—C23—C22	111 (3)
C5—C1—C2	107.6 (5)	H23b—C23—C22	111 (2)
C6—C1—Os	130.4 (4)	H23b—C23—H23a	104 (3)
C6—C1—C2	126.5 (5)	C24—C23—C22	110.5 (4)
C6—C1—C5	125.3 (5)	C24—C23—H23a	108 (3)
C1—C2—Os	72.3 (3)	C24—C23—H23b	111 (2)
C3—C2—Os	69.8 (3)	H24a—C24—C23	110 (3)
C3—C2—C1	108.5 (5)	H24b—C24—C23	113 (2)
C7—C2—Os	130.9 (4)	H24b—C24—H24a	107 (3)
C7—C2—C1	126.5 (5)	C25—C24—C23	111.1 (4)
C7—C2—C3	124.4 (5)	C25—C24—H24a	106 (3)
C2—C3—Os	73.2 (3)	C25—C24—H24b	109 (2)
C4—C3—Os	71.5 (3)	H25a—C25—C24	113 (3)
C4—C3—C2	107.7 (5)	H25b—C25—C24	108 (3)
C8—C3—Os	126.5 (4)	H25b—C25—H25a	106 (4)
C8—C3—C2	126.6 (6)	C26—C25—C24	111.1 (4)
C8—C3—C4	125.3 (6)	C26—C25—H25a	110 (3)
C3—C4—Os	71.0 (3)	C26—C25—H25b	109 (3)
C5—C4—Os	72.1 (3)	C25—C26—C21	110.9 (4)
C5—C4—C3	107.3 (5)	H26a—C26—C21	111 (3)
C9—C4—Os	126.7 (4)	H26a—C26—C25	111 (3)
C9—C4—C3	126.8 (6)	H26b—C26—C21	105 (2)
C9—C4—C5	125.6 (6)	H26b—C26—C25	109 (2)
C1—C5—Os	73.1 (3)	H26b—C26—H26a	110 (4)
C4—C5—Os	70.9 (3)	H31—C31—P	112 (2)
C4—C5—C1	108.9 (5)	C32—C31—P	116.5 (3)
C10—C5—Os	130.3 (4)	C32—C31—H31	104 (2)
C10—C5—C1	125.8 (5)	C36—C31—P	113.3 (3)
C10—C5—C4	124.4 (5)	C36—C31—H31	101 (2)
H6a—C6—C1	105 (3)	C36—C31—C32	109.2 (4)
H6b—C6—C1	112 (3)	H32a—C32—C31	110 (3)
H6b—C6—H6a	106 (4)	H32b—C32—C31	109 (3)
H6c—C6—C1	108 (3)	H32b—C32—H32a	110 (4)
H6c—C6—H6a	108 (4)	C33—C32—C31	110.7 (4)
H6c—C6—H6b	117 (4)	C33—C32—H32a	109 (3)
H8a—C8—C3	114 (3)	C33—C32—H32b	108 (3)
H8b—C8—C3	114 (3)	H33a—C33—C32	111 (2)
H8b—C8—H8a	107 (4)	H33b—C33—C32	116 (3)
H8c—C8—C3	112 (3)	H33b—C33—H33a	108 (3)
H8c—C8—H8a	96 (4)	C34—C33—C32	111.2 (4)
H8c—C8—H8b	111 (4)	C34—C33—H33a	107 (2)
H7a—C7—C2	99 (3)	C34—C33—H33b	104 (3)
H7b—C7—C2	117 (3)	H34a—C34—C33	115 (3)
H7b—C7—H7a	94 (4)	H34b—C34—C33	110 (3)
H7c—C7—C2	110 (3)	H34b—C34—H34a	106 (4)
H7c—C7—H7a	134 (5)	C35—C34—C33	111.2 (4)
H7c—C7—H7b	102 (4)	C35—C34—H34a	103 (3)
H9a—C9—C4	107 (3)	C35—C34—H34b	110 (3)
H9b—C9—C4	110 (3)	H35a—C35—C34	111 (2)
H9b—C9—H9a	109 (4)	H35b—C35—C34	113 (3)
H9c—C9—C4	116 (3)	H35b—C35—H35a	104 (3)
H9c—C9—H9a	103 (4)	C36—C35—C34	110.7 (4)
H9c—C9—H9b	111 (4)	C36—C35—H35a	109 (2)
H10a—C10—C5	108 (3)	C36—C35—H35b	109 (3)
H10b—C10—C5	113 (3)	C35—C36—C31	111.7 (4)
H10b—C10—H10a	105 (4)	H36a—C36—C31	105 (2)
H10c—C10—C5	111 (3)	H36a—C36—C35	113 (3)
H10c—C10—H10a	111 (4)	H36b—C36—C31	112 (3)
H10c—C10—H10b	108 (4)	H36b—C36—C35	113 (3)
C11—P—Os	114.81 (15)	H36b—C36—H36a	100 (4)
C21—P—Os	112.93 (15)	F2—B—F1	108.6 (6)
C21—P—C11	103.9 (2)	F3—B—F1	112.5 (6)
C31—P—Os	111.66 (14)	F3—B—F2	111.1 (7)
C31—P—C11	102.8 (2)	F4—B—F1	107.8 (7)
C31—P—C21	110.1 (2)	F4—B—F2	108.8 (7)
H11—C11—P	107 (3)	F4—B—F3	107.9 (6)
C12—C11—P	112.3 (3)
Os—C1—C2—C3	−60.7 (3)	C1—C5—C4—C9	173.6 (5)
Os—C1—C2—C7	128.2 (3)	C2—C3—C4—C5	1.4 (4)
Os—C1—C5—C4	62.2 (3)	C2—C3—C4—C9	−173.1 (4)
Os—C1—C5—C10	−127.9 (3)	C3—C4—C5—C10	−170.9 (4)
Os—C2—C1—C5	61.5 (3)	P—C11—C12—C13	−177.9 (4)
Os—C2—C1—C6	−127.0 (3)	P—C11—C16—C15	178.6 (4)
Os—C2—C3—C4	−63.7 (3)	P—C21—C22—C23	−171.4 (4)
Os—C2—C3—C8	123.4 (4)	P—C21—C26—C25	172.2 (4)
Os—C3—C2—C1	62.3 (3)	P—C31—C32—C33	−173.3 (4)
Os—C3—C2—C7	−126.4 (3)	P—C31—C36—C35	171.8 (3)
Os—C3—C4—C5	−63.4 (3)	C11—C12—C13—C14	−56.3 (5)
Os—C3—C4—C9	122.1 (4)	C11—C16—C15—C14	56.4 (5)
Os—C4—C3—C2	64.8 (3)	C12—C13—C14—C15	57.2 (6)
Os—C4—C3—C8	−122.1 (4)	C13—C14—C15—C16	−57.4 (6)
Os—C4—C5—C1	−63.6 (3)	C21—C22—C23—C24	−56.7 (5)
Os—C4—C5—C10	126.3 (3)	C21—C26—C25—C24	57.1 (5)
Os—C5—C1—C2	−62.2 (3)	C22—C23—C24—C25	56.3 (5)
Os—C5—C1—C6	126.2 (3)	C23—C24—C25—C26	−56.7 (5)
Os—C5—C4—C3	62.7 (3)	C31—C32—C33—C34	−57.5 (4)
Os—C5—C4—C9	−122.8 (4)	C31—C36—C35—C34	56.6 (4)
C1—C2—C3—C4	−1.4 (4)	C32—C33—C34—C35	56.8 (5)
C1—C2—C3—C8	−174.3 (5)	C33—C34—C35—C36	−55.7 (5)
C1—C5—C4—C3	−0.9 (5)

(XAXMEP_IAM_NoMoRe)

Crystal data

C28H52OsP·BF4	V = 1457.79 (4) Å^3
Mr = 696.74	Z = 2
Triclinic, P1	F(000) = 702.711
a = 8.9295 (2) Å	Dx = 1.587 Mg m^−3
b = 9.7179 (1) Å	Mo Kα radiation, λ = 0.71073 Å
c = 17.1819 (1) Å	µ = 4.47 mm^−1
α = 94.114 (1)°	T = 199 K
β = 90.034 (1)°	0.3 × 0.1 × 0.04 mm
γ = 101.369 (1)°

Data collection

Absorption correction: integration	Rint = 0.033
Tmin = 0.529, Tmax = 0.844	θmax = 28.3°, θmin = 2.1°
9506 measured reflections	h = −11→11
6629 independent reflections	k = −12→12
5952 reflections with I ≥ 2u(I)	l = −22→13

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.033	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.080	w = 1/[σ^2(Fo^2) + (0.0158P)^2 + 7.5545P] where P = (Fo^2 + 2Fc^2)/3
S = 1.09	(Δ/σ)max = 0.001
6629 reflections	Δρmax = 1.36 e Å^−3
472 parameters	Δρmin = −1.57 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Os	0.22259 (2)	0.24111 (2)	0.197796 (10)	0.01877 (6)
H1	0.307 (9)	0.399 (7)	0.224 (4)	0.062359
H2	0.146 (8)	0.120 (6)	0.253 (4)	0.045750
H3	0.343 (9)	0.167 (8)	0.241 (4)	0.059676
H4	0.392 (8)	0.288 (10)	0.230 (4)	0.065392
C1	0.0492 (6)	0.2381 (5)	0.0980 (3)	0.0240 (10)
C2	0.0776 (6)	0.0988 (5)	0.1021 (3)	0.0244 (10)
C3	0.2376 (6)	0.1025 (5)	0.0887 (3)	0.0282 (11)
C4	0.3080 (6)	0.2453 (6)	0.0744 (3)	0.0280 (11)
C5	0.1909 (6)	0.3277 (5)	0.0810 (3)	0.0265 (10)
C6	−0.1038 (7)	0.2796 (7)	0.0989 (4)	0.0375 (13)
H6A	−0.137 (8)	0.278 (8)	0.046 (4)	0.058654
H6B	−0.098 (9)	0.371 (9)	0.122 (5)	0.065989
H6C	−0.177 (8)	0.205 (9)	0.123 (5)	0.069781
C8	0.3148 (10)	−0.0208 (8)	0.0813 (4)	0.0490 (17)
H8A	0.424 (11)	0.001 (9)	0.103 (6)	0.094093
H8B	0.319 (10)	−0.060 (8)	0.033 (5)	0.073508
H8C	0.273 (11)	−0.096 (8)	0.116 (5)	0.082772
C7	−0.0401 (8)	−0.0336 (7)	0.1068 (4)	0.0391 (14)
H7A	0.008 (11)	−0.087 (8)	0.130 (6)	0.088265
H7B	−0.066 (10)	−0.087 (10)	0.059 (5)	0.100239
H7C	−0.128 (9)	−0.017 (8)	0.126 (5)	0.066411
C9	0.4681 (8)	0.2966 (9)	0.0496 (4)	0.0458 (16)
H9A	0.468 (8)	0.288 (9)	−0.009 (4)	0.063881
H9B	0.535 (9)	0.240 (9)	0.066 (5)	0.069451
H9C	0.509 (8)	0.397 (9)	0.066 (4)	0.059874
C10	0.2106 (8)	0.4766 (6)	0.0593 (4)	0.0386 (14)
H10A	0.213 (9)	0.476 (7)	0.004 (4)	0.060153
H10B	0.304 (9)	0.535 (8)	0.078 (5)	0.064075
H10C	0.126 (10)	0.520 (7)	0.081 (5)	0.062123
P	0.11847 (13)	0.33050 (11)	0.31286 (6)	0.0151 (2)
C11	0.1600 (5)	0.5250 (5)	0.3290 (3)	0.0193 (9)
H11	0.118 (7)	0.546 (6)	0.380 (4)	0.035993
C12	0.3331 (6)	0.5862 (5)	0.3362 (3)	0.0249 (10)
H12A	0.388 (8)	0.537 (7)	0.375 (4)	0.051849
H12B	0.378 (7)	0.561 (7)	0.288 (4)	0.047302
C13	0.3642 (7)	0.7464 (5)	0.3527 (4)	0.0344 (13)
H13A	0.323 (10)	0.771 (8)	0.402 (5)	0.068377
H13B	0.480 (8)	0.787 (7)	0.357 (5)	0.064022
C14	0.2917 (7)	0.8153 (6)	0.2897 (4)	0.0366 (13)
H14A	0.343 (9)	0.799 (9)	0.239 (5)	0.067336
H14B	0.315 (9)	0.911 (8)	0.300 (6)	0.084782
C15	0.1203 (7)	0.7572 (6)	0.2842 (4)	0.0351 (13)
H15A	0.066 (9)	0.800 (8)	0.246 (5)	0.076469
H15B	0.069 (9)	0.778 (7)	0.336 (5)	0.068134
C16	0.0858 (6)	0.5968 (5)	0.2671 (3)	0.0262 (10)
H16A	−0.025 (7)	0.561 (7)	0.264 (4)	0.042974
H16B	0.119 (8)	0.568 (7)	0.216 (4)	0.046466
C21	−0.0928 (5)	0.2831 (4)	0.3143 (3)	0.0173 (8)
H21	−0.123 (7)	0.332 (6)	0.270 (4)	0.035316
C22	−0.1596 (5)	0.1266 (5)	0.2915 (3)	0.0215 (9)
H22A	−0.121 (7)	0.092 (7)	0.242 (4)	0.047450
H22B	−0.133 (7)	0.067 (7)	0.330 (4)	0.042904
C23	−0.3341 (6)	0.1003 (5)	0.2821 (3)	0.0247 (10)
H23A	−0.365 (7)	0.153 (7)	0.237 (4)	0.045642
H23B	−0.375 (7)	−0.005 (7)	0.267 (4)	0.046199
C24	−0.4068 (5)	0.1488 (5)	0.3567 (3)	0.0243 (10)
H24A	−0.517 (7)	0.141 (7)	0.350 (4)	0.045541
H24B	−0.394 (7)	0.083 (7)	0.404 (4)	0.046267
C25	−0.3421 (6)	0.3036 (5)	0.3798 (3)	0.0260 (10)
H25A	−0.386 (8)	0.333 (7)	0.431 (4)	0.056304
H25B	−0.371 (7)	0.359 (7)	0.339 (4)	0.047854
C26	−0.1672 (5)	0.3301 (6)	0.3895 (3)	0.0240 (10)
H26A	−0.128 (7)	0.423 (7)	0.404 (4)	0.045760
H26B	−0.140 (7)	0.267 (7)	0.433 (4)	0.043631
C31	0.2013 (5)	0.2743 (5)	0.4025 (3)	0.0169 (8)
H31	0.323 (7)	0.278 (6)	0.393 (4)	0.033658
C32	0.1878 (6)	0.3639 (5)	0.4797 (3)	0.0209 (9)
H32A	0.224 (8)	0.467 (6)	0.474 (4)	0.040894
H32B	0.076 (7)	0.351 (7)	0.493 (4)	0.038467
C33	0.2765 (6)	0.3166 (5)	0.5459 (3)	0.0267 (10)
H33A	0.397 (7)	0.330 (7)	0.533 (4)	0.046477
H33B	0.267 (8)	0.364 (7)	0.596 (4)	0.044469
C34	0.2206 (6)	0.1606 (5)	0.5576 (3)	0.0243 (10)
H34A	0.278 (9)	0.125 (7)	0.598 (4)	0.055121
H34B	0.119 (8)	0.144 (7)	0.575 (4)	0.043948
C35	0.2316 (6)	0.0701 (5)	0.4824 (3)	0.0241 (10)
H35A	0.182 (9)	−0.041 (6)	0.489 (4)	0.053883
H35B	0.347 (8)	0.076 (7)	0.468 (4)	0.055013
C36	0.1442 (6)	0.1175 (5)	0.4153 (3)	0.0207 (9)
H36A	0.029 (7)	0.102 (6)	0.426 (4)	0.039601
H36B	0.142 (8)	0.057 (6)	0.367 (4)	0.046760
B	0.3097 (9)	0.3655 (8)	0.8136 (4)	0.0419 (16)
F1	0.1952 (6)	0.3611 (5)	0.8669 (3)	0.0717 (14)
F2	0.2642 (6)	0.2597 (6)	0.7558 (3)	0.0880 (17)
F3	0.4455 (6)	0.3554 (7)	0.8467 (3)	0.0925 (18)
F4	0.3290 (7)	0.4932 (6)	0.7810 (4)	0.099 (2)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Os	0.01929 (9)	0.02390 (10)	0.01340 (9)	0.00525 (6)	0.00143 (6)	0.00051 (6)
H1	0.074000	0.047000	0.049000	−0.023000	0.025000	−0.015000
H2	0.064000	0.036000	0.034000	−0.000000	0.014000	0.008000
H3	0.081000	0.076000	0.038000	0.053000	−0.005000	0.008000
H4	0.029000	0.116000	0.048000	0.012000	−0.006000	−0.009000
C1	0.025 (2)	0.031 (3)	0.016 (2)	0.004 (2)	−0.0012 (18)	0.0029 (18)
C2	0.033 (3)	0.030 (2)	0.009 (2)	0.004 (2)	−0.0054 (18)	−0.0017 (17)
C3	0.042 (3)	0.030 (3)	0.014 (2)	0.013 (2)	−0.002 (2)	−0.0031 (18)
C4	0.032 (3)	0.041 (3)	0.012 (2)	0.009 (2)	0.0072 (19)	0.0022 (19)
C5	0.031 (3)	0.034 (3)	0.013 (2)	0.002 (2)	0.0039 (19)	0.0060 (18)
C6	0.028 (3)	0.055 (4)	0.032 (3)	0.011 (3)	−0.008 (2)	0.009 (3)
H6A	0.057000	0.088000	0.039000	0.032000	−0.013000	0.010000
H6B	0.069000	0.070000	0.069000	0.045000	−0.013000	−0.014000
H6C	0.039000	0.110000	0.070000	0.028000	0.016000	0.035000
C8	0.073 (5)	0.047 (4)	0.037 (3)	0.039 (4)	0.008 (3)	−0.002 (3)
H8A	0.087000	0.075000	0.130000	0.055000	−0.048000	−0.035000
H8B	0.104000	0.061000	0.059000	0.036000	−0.002000	−0.027000
H8C	0.134000	0.039000	0.083000	0.032000	0.006000	0.015000
C7	0.049 (4)	0.034 (3)	0.027 (3)	−0.008 (3)	−0.006 (3)	0.001 (2)
H7A	0.096000	0.036000	0.128000	−0.003000	0.036000	0.018000
H7B	0.098000	0.127000	0.042000	−0.066000	−0.033000	0.024000
H7C	0.054000	0.073000	0.055000	−0.022000	0.021000	−0.016000
C9	0.035 (3)	0.067 (5)	0.036 (3)	0.009 (3)	0.012 (3)	0.004 (3)
H9A	0.046000	0.113000	0.026000	0.001000	0.011000	0.001000
H9B	0.045000	0.103000	0.068000	0.034000	0.010000	0.004000
H9C	0.039000	0.083000	0.047000	−0.011000	0.005000	−0.003000
C10	0.055 (4)	0.031 (3)	0.029 (3)	0.002 (3)	0.005 (3)	0.013 (2)
H10A	0.095000	0.050000	0.033000	0.003000	0.002000	0.018000
H10B	0.072000	0.047000	0.063000	−0.017000	−0.006000	0.015000
H10C	0.094000	0.038000	0.059000	0.022000	0.002000	0.010000
P	0.0153 (5)	0.0156 (5)	0.0144 (5)	0.0032 (4)	0.0014 (4)	0.0014 (4)
C11	0.020 (2)	0.018 (2)	0.019 (2)	0.0017 (17)	0.0022 (17)	0.0011 (16)
H11	0.050000	0.031000	0.026000	0.006000	0.006000	0.001000
C12	0.019 (2)	0.018 (2)	0.037 (3)	0.0022 (18)	−0.002 (2)	0.0041 (19)
H12A	0.042000	0.048000	0.064000	−0.003000	−0.019000	0.027000
H12B	0.035000	0.049000	0.054000	0.003000	0.006000	−0.008000
C13	0.034 (3)	0.017 (2)	0.049 (3)	−0.002 (2)	−0.011 (3)	−0.001 (2)
H13A	0.091000	0.050000	0.054000	−0.005000	−0.011000	−0.012000
H13B	0.042000	0.054000	0.089000	−0.014000	−0.014000	0.023000
C14	0.031 (3)	0.020 (2)	0.058 (4)	0.001 (2)	−0.001 (3)	0.012 (2)
H14A	0.059000	0.088000	0.057000	0.008000	0.013000	0.037000
H14B	0.070000	0.039000	0.141000	−0.011000	−0.007000	0.038000
C15	0.029 (3)	0.022 (3)	0.055 (4)	0.005 (2)	−0.006 (3)	0.010 (2)
H15A	0.069000	0.056000	0.111000	0.012000	−0.008000	0.052000
H15B	0.074000	0.039000	0.090000	0.013000	0.010000	−0.010000
C16	0.030 (3)	0.024 (2)	0.025 (2)	0.007 (2)	−0.009 (2)	0.0015 (19)
H16A	0.035000	0.042000	0.055000	0.011000	0.000000	0.015000
H16B	0.060000	0.056000	0.026000	0.016000	0.001000	0.008000
C21	0.019 (2)	0.015 (2)	0.017 (2)	0.0030 (16)	0.0032 (17)	−0.0010 (16)
H21	0.033000	0.041000	0.034000	0.009000	−0.001000	0.012000
C22	0.019 (2)	0.019 (2)	0.025 (2)	0.0027 (17)	0.0017 (18)	−0.0039 (18)
H22A	0.036000	0.057000	0.044000	0.005000	0.008000	−0.021000
H22B	0.037000	0.034000	0.058000	0.005000	−0.002000	0.011000
C23	0.023 (2)	0.021 (2)	0.028 (3)	−0.0017 (18)	0.0002 (19)	−0.0029 (19)
H23A	0.039000	0.066000	0.033000	0.010000	−0.001000	0.012000
H23B	0.033000	0.046000	0.053000	−0.003000	0.001000	−0.011000
C24	0.014 (2)	0.029 (3)	0.029 (3)	0.0014 (18)	0.0043 (18)	0.004 (2)
H24A	0.025000	0.055000	0.057000	0.011000	0.003000	−0.002000
H24B	0.047000	0.054000	0.038000	0.007000	0.009000	0.013000
C25	0.022 (2)	0.028 (3)	0.029 (3)	0.006 (2)	0.007 (2)	−0.001 (2)
H25A	0.040000	0.070000	0.056000	0.014000	0.011000	−0.024000
H25B	0.039000	0.040000	0.067000	0.013000	−0.002000	0.006000
C26	0.017 (2)	0.030 (3)	0.024 (2)	0.0047 (19)	0.0044 (18)	−0.0067 (19)
H26A	0.037000	0.041000	0.055000	0.005000	0.002000	−0.018000
H26B	0.042000	0.062000	0.028000	0.012000	0.003000	0.006000
C31	0.016 (2)	0.017 (2)	0.018 (2)	0.0046 (16)	0.0007 (16)	−0.0001 (16)
H31	0.029000	0.038000	0.036000	0.010000	0.004000	0.007000
C32	0.029 (2)	0.021 (2)	0.015 (2)	0.0098 (19)	−0.0036 (18)	−0.0006 (17)
H32A	0.061000	0.024000	0.033000	−0.004000	−0.008000	0.005000
H32B	0.043000	0.047000	0.029000	0.019000	0.000000	−0.001000
C33	0.037 (3)	0.028 (3)	0.014 (2)	0.004 (2)	−0.006 (2)	0.0013 (18)
H33A	0.036000	0.051000	0.053000	0.006000	−0.007000	0.015000
H33B	0.063000	0.039000	0.028000	0.002000	−0.011000	0.002000
C34	0.026 (3)	0.030 (3)	0.017 (2)	0.004 (2)	−0.0004 (19)	0.0072 (18)
H34A	0.074000	0.046000	0.045000	0.004000	−0.017000	0.023000
H34B	0.047000	0.045000	0.036000	−0.001000	0.007000	0.005000
C35	0.031 (3)	0.024 (2)	0.019 (2)	0.009 (2)	0.0021 (19)	0.0037 (18)
H35A	0.086000	0.024000	0.048000	−0.001000	0.005000	0.011000
H35B	0.064000	0.049000	0.061000	0.029000	0.011000	0.015000
C36	0.030 (3)	0.016 (2)	0.015 (2)	0.0027 (18)	−0.0014 (18)	0.0015 (16)
H36A	0.035000	0.043000	0.037000	−0.003000	0.003000	0.007000
H36B	0.075000	0.029000	0.031000	0.000000	0.006000	−0.005000
B	0.040 (4)	0.054 (4)	0.029 (3)	0.002 (3)	0.009 (3)	0.004 (3)
F1	0.085 (3)	0.071 (3)	0.053 (3)	0.004 (3)	0.030 (2)	−0.003 (2)
F2	0.080 (3)	0.114 (4)	0.063 (3)	0.021 (3)	−0.009 (3)	−0.045 (3)
F3	0.068 (3)	0.132 (5)	0.081 (4)	0.029 (3)	−0.030 (3)	0.009 (3)
F4	0.084 (4)	0.096 (4)	0.122 (5)	0.009 (3)	0.011 (3)	0.065 (4)

Geometric parameters (Å, º)

Os—H1	1.60 (6)	C14—H14A	1.00 (8)
Os—H2	1.61 (6)	C14—H14B	0.92 (8)
Os—H3	1.61 (7)	C14—C15	1.524 (8)
Os—H4	1.58 (7)	C15—H15A	0.99 (8)
Os—C1	2.305 (5)	C15—H15B	1.03 (8)
Os—C2	2.292 (5)	C15—C16	1.534 (7)
Os—C3	2.248 (5)	C16—H16A	0.98 (6)
Os—C4	2.255 (5)	C16—H16B	0.97 (7)
Os—C5	2.270 (5)	C21—H21	0.98 (6)
Os—P	2.3669 (11)	C21—C22	1.542 (6)
C1—C2	1.433 (7)	C21—C26	1.535 (6)
C1—C5	1.430 (7)	C22—H22A	0.97 (6)
C1—C6	1.499 (8)	C22—H22B	0.96 (7)
C2—C3	1.441 (7)	C22—C23	1.535 (7)
C2—C7	1.499 (8)	C23—H23A	1.02 (7)
C3—C4	1.445 (7)	C23—H23B	1.03 (6)
C3—C8	1.494 (8)	C23—C24	1.523 (7)
C4—C5	1.437 (7)	C24—H24A	0.98 (6)
C4—C9	1.491 (8)	C24—H24B	1.09 (7)
C5—C10	1.496 (7)	C24—C25	1.525 (7)
C6—H6A	0.95 (7)	C25—H25A	1.01 (7)
C6—H6B	0.94 (8)	C25—H25B	0.98 (7)
C6—H6C	0.99 (8)	C25—C26	1.539 (7)
C8—H8A	1.02 (9)	C26—H26A	0.92 (6)
C8—H8B	0.90 (8)	C26—H26B	1.05 (7)
C8—H8C	1.00 (9)	C31—H31	1.09 (6)
C7—H7A	0.86 (10)	C31—C32	1.552 (6)
C7—H7B	0.94 (9)	C31—C36	1.540 (6)
C7—H7C	0.89 (8)	C32—H32A	1.00 (6)
C9—H9A	1.00 (7)	C32—H32B	1.01 (6)
C9—H9B	0.94 (8)	C32—C33	1.532 (6)
C9—H9C	1.00 (8)	C33—H33A	1.08 (7)
C10—H10A	0.95 (7)	C33—H33B	0.96 (7)
C10—H10B	0.95 (7)	C33—C34	1.528 (7)
C10—H10C	0.99 (8)	C34—H34A	0.99 (7)
P—C11	1.854 (5)	C34—H34B	0.94 (7)
P—C21	1.852 (5)	C34—C35	1.525 (7)
P—C31	1.870 (5)	C35—H35A	1.10 (6)
C11—H11	0.97 (6)	C35—H35B	1.05 (7)
C11—C12	1.544 (6)	C35—C36	1.538 (7)
C11—C16	1.531 (7)	C36—H36A	1.03 (6)
C12—H12A	1.02 (7)	C36—H36B	0.98 (6)
C12—H12B	0.96 (7)	B—F1	1.370 (8)
C12—C13	1.533 (7)	B—F2	1.377 (9)
C13—H13A	0.96 (8)	B—F3	1.363 (9)
C13—H13B	1.03 (7)	B—F4	1.379 (9)
C13—C14	1.520 (8)
H2—Os—H1	128 (3)	C12—C11—H11	106 (4)
H3—Os—H1	95 (4)	C16—C11—P	112.9 (3)
H3—Os—H2	66 (4)	C16—C11—H11	109 (4)
H4—Os—H1	54 (4)	C16—C11—C12	110.7 (4)
H4—Os—H2	104 (4)	H12A—C12—C11	113 (4)
H4—Os—H3	44 (4)	H12B—C12—C11	107 (4)
C1—Os—H1	111 (3)	H12B—C12—H12A	101 (6)
C1—Os—H2	106 (2)	C13—C12—C11	111.2 (4)
C1—Os—H3	150 (3)	C13—C12—H12A	113 (4)
C1—Os—H4	148 (3)	C13—C12—H12B	111 (4)
C2—Os—H1	145 (3)	H13A—C13—C12	110 (5)
C2—Os—H2	83 (2)	H13B—C13—C12	111 (4)
C2—Os—H3	114 (3)	H13B—C13—H13A	106 (6)
C2—Os—H4	142 (3)	C14—C13—C12	110.8 (5)
C2—Os—C1	36.31 (17)	C14—C13—H13A	108 (5)
C3—Os—H1	132 (2)	C14—C13—H13B	111 (4)
C3—Os—H2	98 (2)	H14A—C14—C13	109 (4)
C3—Os—H3	90 (3)	H14B—C14—C13	109 (6)
C3—Os—H4	105 (3)	H14B—C14—H14A	104 (7)
C3—Os—C1	61.59 (18)	C15—C14—C13	110.3 (5)
C3—Os—C2	37.00 (19)	C15—C14—H14A	112 (5)
C4—Os—H1	95 (2)	C15—C14—H14B	113 (5)
C4—Os—H2	135 (2)	H15A—C15—C14	114 (4)
C4—Os—H3	102 (3)	H15B—C15—C14	111 (4)
C4—Os—H4	90 (3)	H15B—C15—H15A	104 (6)
C4—Os—C1	61.58 (18)	C16—C15—C14	111.4 (5)
C4—Os—C2	61.66 (19)	C16—C15—H15A	109 (5)
C4—Os—C3	37.43 (19)	C16—C15—H15B	107 (4)
C5—Os—H1	85 (3)	C15—C16—C11	110.9 (4)
C5—Os—H2	142 (2)	H16A—C16—C11	111 (4)
C5—Os—H3	139 (3)	H16A—C16—C15	110 (4)
C5—Os—H4	112 (3)	H16B—C16—C11	109 (4)
C5—Os—C1	36.43 (17)	H16B—C16—C15	113 (4)
C5—Os—C2	60.82 (18)	H16B—C16—H16A	102 (5)
C5—Os—C3	61.79 (19)	H21—C21—P	102 (3)
C5—Os—C4	37.02 (19)	C22—C21—P	114.5 (3)
P—Os—H1	68 (2)	C22—C21—H21	104 (4)
P—Os—H2	67 (2)	C26—C21—P	115.6 (3)
P—Os—H3	96 (2)	C26—C21—H21	110 (4)
P—Os—H4	93 (3)	C26—C21—C22	109.7 (4)
P—Os—C1	107.12 (13)	H22A—C22—C21	113 (4)
P—Os—C2	123.31 (13)	H22B—C22—C21	111 (4)
P—Os—C3	158.88 (15)	H22B—C22—H22A	105 (6)
P—Os—C4	155.74 (14)	C23—C22—C21	111.3 (4)
P—Os—C5	120.99 (14)	C23—C22—H22A	106 (4)
C2—C1—Os	71.4 (3)	C23—C22—H22B	109 (4)
C5—C1—Os	70.5 (3)	H23A—C23—C22	111 (4)
C5—C1—C2	107.6 (4)	H23B—C23—C22	109 (4)
C6—C1—Os	130.4 (4)	H23B—C23—H23A	106 (5)
C6—C1—C2	126.5 (5)	C24—C23—C22	110.7 (4)
C6—C1—C5	125.3 (5)	C24—C23—H23A	109 (4)
C1—C2—Os	72.3 (3)	C24—C23—H23B	112 (4)
C3—C2—Os	69.8 (3)	H24A—C24—C23	112 (4)
C3—C2—C1	108.4 (4)	H24B—C24—C23	111 (4)
C7—C2—Os	130.9 (3)	H24B—C24—H24A	105 (5)
C7—C2—C1	126.5 (5)	C25—C24—C23	111.0 (4)
C7—C2—C3	124.4 (5)	C25—C24—H24A	106 (4)
C2—C3—Os	73.2 (3)	C25—C24—H24B	111 (4)
C4—C3—Os	71.5 (3)	H25A—C25—C24	110 (4)
C4—C3—C2	107.7 (4)	H25B—C25—C24	108 (4)
C8—C3—Os	126.3 (4)	H25B—C25—H25A	109 (6)
C8—C3—C2	126.6 (6)	C26—C25—C24	110.9 (4)
C8—C3—C4	125.3 (6)	C26—C25—H25A	108 (4)
C3—C4—Os	71.0 (3)	C26—C25—H25B	111 (4)
C5—C4—Os	72.1 (3)	C25—C26—C21	110.9 (4)
C5—C4—C3	107.2 (4)	H26A—C26—C21	110 (4)
C9—C4—Os	126.6 (4)	H26A—C26—C25	111 (4)
C9—C4—C3	126.9 (5)	H26B—C26—C21	106 (3)
C9—C4—C5	125.6 (5)	H26B—C26—C25	109 (3)
C1—C5—Os	73.1 (3)	H26B—C26—H26A	109 (6)
C4—C5—Os	70.9 (3)	H31—C31—P	108 (3)
C4—C5—C1	109.0 (4)	C32—C31—P	116.5 (3)
C10—C5—Os	130.3 (4)	C32—C31—H31	107 (3)
C10—C5—C1	125.9 (5)	C36—C31—P	113.3 (3)
C10—C5—C4	124.3 (5)	C36—C31—H31	102 (3)
H6A—C6—C1	108 (4)	C36—C31—C32	109.3 (4)
H6B—C6—C1	112 (5)	H32A—C32—C31	112 (4)
H6B—C6—H6A	109 (6)	H32B—C32—C31	108 (3)
H6C—C6—C1	108 (4)	H32B—C32—H32A	106 (5)
H6C—C6—H6A	106 (6)	C33—C32—C31	110.7 (4)
H6C—C6—H6B	115 (7)	C33—C32—H32A	110 (4)
H8A—C8—C3	113 (4)	C33—C32—H32B	110 (4)
H8B—C8—C3	115 (5)	H33A—C33—C32	111 (4)
H8B—C8—H8A	107 (7)	H33B—C33—C32	114 (4)
H8C—C8—C3	114 (5)	H33B—C33—H33A	108 (5)
H8C—C8—H8A	97 (7)	C34—C33—C32	111.3 (4)
H8C—C8—H8B	109 (7)	C34—C33—H33A	107 (3)
H7A—C7—C2	103 (6)	C34—C33—H33B	105 (4)
H7B—C7—C2	115 (5)	H34A—C34—C33	114 (4)
H7B—C7—H7A	101 (9)	H34B—C34—C33	110 (4)
H7C—C7—C2	112 (5)	H34B—C34—H34A	104 (6)
H7C—C7—H7A	119 (8)	C35—C34—C33	111.1 (4)
H7C—C7—H7B	105 (7)	C35—C34—H34A	107 (4)
H9A—C9—C4	107 (4)	C35—C34—H34B	110 (4)
H9B—C9—C4	112 (5)	H35A—C35—C34	112 (4)
H9B—C9—H9A	107 (6)	H35B—C35—C34	110 (4)
H9C—C9—C4	114 (4)	H35B—C35—H35A	107 (5)
H9C—C9—H9A	106 (6)	C36—C35—C34	110.8 (4)
H9C—C9—H9B	110 (6)	C36—C35—H35A	107 (4)
H10A—C10—C5	108 (4)	C36—C35—H35B	111 (4)
H10B—C10—C5	114 (5)	C35—C36—C31	111.8 (4)
H10B—C10—H10A	107 (6)	H36A—C36—C31	108 (4)
H10C—C10—C5	110 (4)	H36A—C36—C35	112 (4)
H10C—C10—H10A	111 (6)	H36B—C36—C31	112 (4)
H10C—C10—H10B	107 (6)	H36B—C36—C35	113 (4)
C11—P—Os	114.82 (15)	H36B—C36—H36A	99 (5)
C21—P—Os	112.93 (14)	F2—B—F1	108.5 (6)
C21—P—C11	103.8 (2)	F3—B—F1	112.6 (6)
C31—P—Os	111.73 (14)	F3—B—F2	111.3 (7)
C31—P—C11	102.8 (2)	F4—B—F1	107.7 (6)
C31—P—C21	110.0 (2)	F4—B—F2	108.7 (6)
H11—C11—P	106 (3)	F4—B—F3	108.0 (6)
C12—C11—P	112.2 (3)
Os—C1—C2—C3	−60.8 (3)	C1—C5—C4—C9	173.8 (4)
Os—C1—C2—C7	128.2 (3)	C2—C3—C4—C5	1.3 (4)
Os—C1—C5—C4	62.2 (3)	C2—C3—C4—C9	−173.2 (4)
Os—C1—C5—C10	−127.9 (3)	C3—C4—C5—C10	−171.0 (4)
Os—C2—C1—C5	61.5 (3)	P—C11—C12—C13	−177.8 (4)
Os—C2—C1—C6	−127.0 (3)	P—C11—C16—C15	178.6 (4)
Os—C2—C3—C4	−63.6 (3)	P—C21—C22—C23	−171.4 (4)
Os—C2—C3—C8	123.1 (4)	P—C21—C26—C25	172.1 (4)
Os—C3—C2—C1	62.4 (3)	P—C31—C32—C33	−173.3 (4)
Os—C3—C2—C7	−126.4 (3)	P—C31—C36—C35	171.7 (3)
Os—C3—C4—C5	−63.4 (3)	C11—C12—C13—C14	−56.7 (5)
Os—C3—C4—C9	122.0 (4)	C11—C16—C15—C14	56.5 (5)
Os—C4—C3—C2	64.7 (3)	C12—C13—C14—C15	57.6 (5)
Os—C4—C3—C8	−121.9 (4)	C13—C14—C15—C16	−57.7 (6)
Os—C4—C5—C1	−63.6 (3)	C21—C22—C23—C24	−56.9 (4)
Os—C4—C5—C10	126.3 (3)	C21—C26—C25—C24	57.2 (5)
Os—C5—C1—C2	−62.1 (3)	C22—C23—C24—C25	56.5 (5)
Os—C5—C1—C6	126.3 (3)	C23—C24—C25—C26	−56.8 (5)
Os—C5—C4—C3	62.7 (3)	C31—C32—C33—C34	−57.3 (4)
Os—C5—C4—C9	−122.6 (4)	C31—C36—C35—C34	56.4 (4)
C1—C2—C3—C4	−1.3 (4)	C32—C33—C34—C35	56.6 (5)
C1—C2—C3—C8	−174.6 (4)	C33—C34—C35—C36	−55.5 (5)
C1—C5—C4—C3	−0.8 (4)

(XAXMEP_IAM_SHADE3)

Crystal data

C28H52OsP·BF4	V = 1457.79 (4) Å^3
Mr = 696.74	Z = 2
Triclinic, P1	F(000) = 111.426
a = 8.9295 (2) Å	Dx = 1.587 Mg m^−3
b = 9.7179 (1) Å	Mo Kα radiation, λ = 0.71073 Å
c = 17.1819 (1) Å	µ = 4.47 mm^−1
α = 94.114 (1)°	T = 199 K
β = 90.034 (1)°	0.3 × 0.1 × 0.04 mm
γ = 101.369 (1)°

Data collection

Absorption correction: integration	Rint = 0.033
Tmin = 0.529, Tmax = 0.844	θmax = 28.3°, θmin = 2.1°
9506 measured reflections	h = −11→11
6629 independent reflections	k = −12→12
5952 reflections with I ≥ 2u(I)	l = −22→13

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.034	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.081	w = 1/[σ^2(Fo^2) + (0.0154P)^2 + 8.1129P] where P = (Fo^2 + 2Fc^2)/3
S = 1.08	(Δ/σ)max = 0.001
6629 reflections	Δρmax = 1.32 e Å^−3
328 parameters	Δρmin = −1.53 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Os	0.22259 (2)	0.24111 (2)	0.197794 (10)	0.01879 (6)
H1	0.305 (7)	0.402 (6)	0.223 (4)	0.040974
H2	0.144 (7)	0.119 (6)	0.252 (4)	0.038964
H3	0.343 (7)	0.171 (7)	0.240 (4)	0.043022
H4	0.394 (7)	0.292 (7)	0.228 (4)	0.043156
C1	0.0491 (6)	0.2382 (5)	0.0980 (3)	0.0243 (10)
C2	0.0775 (6)	0.0987 (5)	0.1022 (3)	0.0247 (10)
C3	0.2376 (6)	0.1025 (5)	0.0888 (3)	0.0283 (11)
C4	0.3080 (6)	0.2454 (6)	0.0744 (3)	0.0282 (11)
C5	0.1909 (6)	0.3277 (5)	0.0810 (3)	0.0266 (10)
C6	−0.1039 (6)	0.2795 (7)	0.0988 (3)	0.0372 (13)
H6A	−0.140000	0.280900	0.045100	0.054468
H6B	−0.094800	0.373400	0.125600	0.046330
H6C	−0.176600	0.211500	0.126400	0.046817
C8	0.3147 (9)	−0.0212 (7)	0.0812 (4)	0.0487 (17)
H8A	0.421700	0.007900	0.098600	0.054728
H8B	0.310600	−0.058900	0.026700	0.059024
H8C	0.262300	−0.094400	0.113800	0.051393
C7	−0.0404 (7)	−0.0340 (6)	0.1068 (3)	0.0388 (14)
H7A	−0.002800	−0.095900	0.141500	0.041900
H7B	−0.059600	−0.082000	0.054600	0.050714
H7C	−0.135200	−0.010500	0.127400	0.045021
C9	0.4684 (7)	0.2964 (8)	0.0495 (4)	0.0458 (15)
H9A	0.472500	0.290500	−0.007500	0.064749
H9B	0.534800	0.237900	0.070100	0.058438
H9C	0.503300	0.394400	0.069900	0.056297
C10	0.2108 (7)	0.4767 (6)	0.0593 (3)	0.0384 (13)
H10A	0.211400	0.478400	0.002300	0.058931
H10B	0.307500	0.531200	0.081200	0.052384
H10C	0.126000	0.518000	0.080200	0.050690
P	0.11845 (13)	0.33050 (11)	0.31287 (6)	0.0151 (2)
C11	0.1599 (5)	0.5249 (5)	0.3290 (3)	0.0194 (9)
H11	0.114500	0.548500	0.380100	0.032280
C12	0.3330 (5)	0.5862 (5)	0.3361 (3)	0.0250 (10)
H12A	0.377400	0.543200	0.378700	0.035614
H12B	0.383000	0.562200	0.286900	0.036827
C13	0.3641 (6)	0.7463 (5)	0.3526 (4)	0.0345 (13)
H13A	0.322200	0.770300	0.404000	0.044558
H13B	0.475800	0.783200	0.354500	0.046359
C14	0.2918 (7)	0.8156 (6)	0.2898 (4)	0.0367 (13)
H14A	0.339100	0.797600	0.238900	0.046384
H14B	0.310300	0.918500	0.302300	0.052054
C15	0.1204 (6)	0.7570 (5)	0.2841 (4)	0.0351 (13)
H15A	0.075300	0.801200	0.242100	0.047779
H15B	0.072500	0.781300	0.333900	0.045528
C16	0.0857 (6)	0.5967 (5)	0.2671 (3)	0.0264 (10)
H16A	−0.026100	0.561700	0.266500	0.036230
H16B	0.124800	0.572700	0.215000	0.037341
C21	−0.0927 (5)	0.2831 (4)	0.3143 (3)	0.0174 (8)
H21	−0.128600	0.335800	0.272500	0.030769
C22	−0.1596 (5)	0.1265 (5)	0.2916 (3)	0.0217 (9)
H22A	−0.114600	0.097700	0.241900	0.033834
H22B	−0.132400	0.068400	0.332300	0.034014
C23	−0.3340 (6)	0.1002 (5)	0.2821 (3)	0.0249 (10)
H23A	−0.361300	0.151700	0.238200	0.040537
H23B	−0.374000	−0.001400	0.269700	0.041858
C24	−0.4070 (5)	0.1489 (5)	0.3566 (3)	0.0245 (10)
H24A	−0.518800	0.135600	0.348400	0.047100
H24B	−0.387900	0.091300	0.399300	0.042458
C25	−0.3420 (6)	0.3036 (5)	0.3798 (3)	0.0260 (10)
H25A	−0.387700	0.331500	0.429400	0.045575
H25B	−0.369400	0.362000	0.339200	0.042029
C26	−0.1672 (5)	0.3303 (5)	0.3895 (3)	0.0241 (10)
H26A	−0.127600	0.431800	0.402500	0.035499
H26B	−0.140000	0.278000	0.433000	0.035220
C31	0.2012 (5)	0.2742 (5)	0.4026 (3)	0.0170 (8)
H31	0.313400	0.284800	0.393000	0.029460
C32	0.1877 (6)	0.3638 (5)	0.4798 (3)	0.0210 (9)
H32A	0.228600	0.464200	0.472400	0.034797
H32B	0.078800	0.353700	0.493800	0.035250
C33	0.2762 (6)	0.3166 (5)	0.5460 (3)	0.0269 (10)
H33A	0.386500	0.333400	0.533600	0.039366
H33B	0.263700	0.372600	0.594900	0.042469
C34	0.2204 (6)	0.1606 (5)	0.5577 (3)	0.0243 (10)
H34A	0.282800	0.132000	0.599000	0.043646
H34B	0.113000	0.144600	0.574700	0.040542
C35	0.2316 (6)	0.0702 (5)	0.4823 (3)	0.0242 (10)
H35A	0.188800	−0.029600	0.490500	0.040266
H35B	0.340300	0.077900	0.468300	0.038140
C36	0.1443 (6)	0.1175 (5)	0.4153 (3)	0.0208 (9)
H36A	0.033900	0.101400	0.427400	0.032552
H36B	0.156700	0.060100	0.366700	0.031894
B	0.3098 (9)	0.3654 (8)	0.8136 (4)	0.0424 (16)
F1	0.1952 (6)	0.3610 (5)	0.8669 (3)	0.0717 (14)
F2	0.2644 (6)	0.2597 (6)	0.7558 (3)	0.0880 (17)
F3	0.4455 (6)	0.3553 (7)	0.8466 (3)	0.0923 (18)
F4	0.3291 (7)	0.4931 (6)	0.7809 (4)	0.098 (2)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Os	0.01931 (9)	0.02392 (10)	0.01342 (9)	0.00526 (6)	0.00144 (6)	0.00051 (6)
H1	0.045920	0.032740	0.039910	−0.002590	0.005980	0.002020
H2	0.043170	0.037000	0.033500	−0.000400	0.008230	0.003890
H3	0.047130	0.048740	0.039730	0.022890	0.000810	0.010140
H4	0.025770	0.056780	0.046430	0.007450	−0.002310	0.002480
C1	0.026 (2)	0.031 (3)	0.016 (2)	0.004 (2)	−0.0012 (18)	0.0031 (18)
C2	0.034 (3)	0.030 (2)	0.010 (2)	0.004 (2)	−0.0054 (18)	−0.0018 (17)
C3	0.042 (3)	0.030 (3)	0.015 (2)	0.013 (2)	−0.002 (2)	−0.0030 (18)
C4	0.032 (3)	0.041 (3)	0.012 (2)	0.009 (2)	0.0071 (19)	0.0021 (19)
C5	0.031 (3)	0.034 (3)	0.014 (2)	0.002 (2)	0.0039 (19)	0.0056 (19)
C6	0.028 (3)	0.053 (4)	0.032 (3)	0.010 (3)	−0.008 (2)	0.009 (3)
H6A	0.056970	0.080150	0.029190	0.019980	−0.014170	0.005920
H6B	0.043550	0.040130	0.054580	0.008670	−0.012000	−0.002510
H6C	0.036130	0.053020	0.050670	0.003640	0.001030	0.013970
C8	0.070 (5)	0.048 (4)	0.038 (3)	0.036 (3)	0.009 (3)	−0.002 (3)
H8A	0.051870	0.068830	0.047120	0.026220	0.002030	−0.010990
H8B	0.078240	0.072460	0.029240	0.028730	0.006970	−0.015500
H8C	0.065920	0.049030	0.040730	0.018320	0.009730	−0.006040
C7	0.049 (4)	0.034 (3)	0.026 (3)	−0.008 (3)	−0.006 (2)	0.001 (2)
H7A	0.057760	0.033950	0.033130	0.010670	−0.006570	−0.007810
H7B	0.060650	0.051250	0.037710	0.010710	−0.014860	−0.012830
H7C	0.047120	0.046520	0.038530	0.004950	0.000890	−0.004510
C9	0.036 (3)	0.066 (4)	0.036 (3)	0.010 (3)	0.012 (3)	0.004 (3)
H9A	0.059300	0.107830	0.028280	0.016760	0.015530	0.012090
H9B	0.049690	0.079880	0.052180	0.025590	0.016810	0.012710
H9C	0.045450	0.070080	0.049710	0.002510	0.013770	0.004380
C10	0.053 (4)	0.032 (3)	0.030 (3)	0.002 (3)	0.005 (3)	0.013 (2)
H10A	0.073810	0.072370	0.029620	0.006120	0.001820	0.020260
H10B	0.041090	0.059120	0.053970	−0.002890	−0.003590	0.019740
H10C	0.049720	0.051460	0.054020	0.012780	0.006480	0.017330
P	0.0153 (5)	0.0157 (5)	0.0145 (5)	0.0032 (4)	0.0015 (4)	0.0014 (4)
C11	0.020 (2)	0.018 (2)	0.019 (2)	0.0018 (17)	0.0021 (17)	0.0010 (16)
H11	0.035670	0.029450	0.031450	0.007560	0.001610	−0.002760
C12	0.020 (2)	0.018 (2)	0.037 (3)	0.0022 (18)	−0.002 (2)	0.0049 (19)
H12A	0.033980	0.033510	0.038810	0.003650	−0.007020	0.007480
H12B	0.033410	0.037560	0.036910	0.001450	0.002840	0.000580
C13	0.034 (3)	0.017 (2)	0.049 (3)	−0.002 (2)	−0.010 (3)	0.000 (2)
H13A	0.054380	0.030340	0.046690	0.005410	−0.005490	−0.004230
H13B	0.034920	0.037180	0.063130	−0.003760	−0.007790	0.008030
C14	0.032 (3)	0.021 (2)	0.057 (4)	0.002 (2)	−0.001 (3)	0.011 (2)
H14A	0.045850	0.040290	0.051660	0.002470	−0.002910	0.011100
H14B	0.053960	0.024460	0.074180	−0.002950	−0.010190	0.009420
C15	0.030 (3)	0.022 (2)	0.054 (4)	0.005 (2)	−0.006 (3)	0.010 (2)
H15A	0.048290	0.033950	0.063380	0.008960	−0.010750	0.016860
H15B	0.047840	0.032690	0.055540	0.009080	−0.001550	−0.003380
C16	0.030 (3)	0.024 (2)	0.025 (2)	0.007 (2)	−0.009 (2)	0.0015 (19)
H16A	0.026860	0.033790	0.048920	0.006600	−0.002790	0.007350
H16B	0.043370	0.035100	0.033850	0.007340	−0.000620	0.005720
C21	0.019 (2)	0.015 (2)	0.017 (2)	0.0032 (16)	0.0033 (16)	−0.0010 (16)
H21	0.029910	0.031160	0.032050	0.006480	−0.001840	0.006620
C22	0.019 (2)	0.020 (2)	0.025 (2)	0.0026 (17)	0.0019 (18)	−0.0036 (17)
H22A	0.034430	0.035890	0.029300	0.005050	0.001030	−0.005100
H22B	0.036100	0.030510	0.034780	0.002790	−0.002370	0.008590
C23	0.023 (2)	0.020 (2)	0.028 (2)	−0.0018 (18)	0.0002 (19)	−0.0026 (18)
H23A	0.035170	0.045380	0.041540	0.007040	−0.003470	0.009050
H23B	0.034220	0.034930	0.050330	−0.006130	−0.004010	−0.002010
C24	0.015 (2)	0.029 (2)	0.029 (3)	0.0016 (18)	0.0039 (18)	0.004 (2)
H24A	0.023690	0.055480	0.060450	0.003610	0.002270	0.004600
H24B	0.039930	0.042850	0.043080	0.002060	0.006130	0.009930
C25	0.022 (2)	0.028 (2)	0.028 (3)	0.0062 (19)	0.0074 (19)	−0.0010 (19)
H25A	0.034810	0.053620	0.048440	0.011880	0.012390	−0.004150
H25B	0.032590	0.042660	0.052490	0.009560	−0.000640	0.008800
C26	0.018 (2)	0.030 (2)	0.023 (2)	0.0051 (19)	0.0044 (18)	−0.0060 (19)
H26A	0.032390	0.030340	0.042140	0.004930	0.002630	−0.004860
H26B	0.037330	0.038810	0.031620	0.011010	0.005500	0.007070
C31	0.015 (2)	0.018 (2)	0.018 (2)	0.0044 (16)	0.0007 (16)	−0.0001 (16)
H31	0.025400	0.034500	0.029410	0.008480	0.000620	0.001500
C32	0.029 (2)	0.021 (2)	0.015 (2)	0.0096 (19)	−0.0035 (18)	−0.0005 (16)
H32A	0.041090	0.027380	0.033160	0.001360	−0.002120	−0.001410
H32B	0.033380	0.042940	0.030470	0.012000	0.003690	−0.002730
C33	0.036 (3)	0.028 (2)	0.015 (2)	0.004 (2)	−0.0054 (19)	0.0013 (18)
H33A	0.035770	0.044860	0.037800	0.008790	−0.004290	0.003040
H33B	0.057260	0.043720	0.024230	0.008230	−0.005120	−0.007490
C34	0.027 (2)	0.030 (3)	0.017 (2)	0.004 (2)	−0.0007 (18)	0.0069 (18)
H34A	0.056730	0.048300	0.027560	0.012230	−0.009090	0.008910
H34B	0.043500	0.046080	0.032040	0.008680	0.004250	0.003280
C35	0.031 (3)	0.023 (2)	0.020 (2)	0.0084 (19)	0.0026 (19)	0.0038 (18)
H35A	0.052890	0.030820	0.036500	0.004780	−0.003270	0.008270
H35B	0.037440	0.045920	0.034450	0.016590	−0.003140	0.002670
C36	0.030 (2)	0.016 (2)	0.015 (2)	0.0029 (18)	−0.0008 (18)	0.0014 (16)
H36A	0.029840	0.034620	0.034160	0.007710	0.004210	0.005290
H36B	0.042050	0.029020	0.024640	0.008900	−0.000860	−0.003080
B	0.041 (4)	0.054 (4)	0.030 (3)	0.002 (3)	0.009 (3)	0.004 (3)
F1	0.085 (3)	0.071 (3)	0.053 (3)	0.004 (3)	0.030 (2)	−0.003 (2)
F2	0.079 (3)	0.114 (4)	0.064 (3)	0.020 (3)	−0.008 (3)	−0.045 (3)
F3	0.069 (3)	0.132 (5)	0.080 (4)	0.030 (3)	−0.030 (3)	0.009 (3)
F4	0.083 (4)	0.095 (4)	0.121 (5)	0.009 (3)	0.011 (3)	0.065 (4)

Geometric parameters (Å, º)

Os—H1	1.62 (6)	C14—H14A	0.991 (7)
Os—H2	1.61 (6)	C14—H14B	0.989 (5)
Os—H3	1.59 (6)	C14—C15	1.525 (8)
Os—H4	1.59 (6)	C15—H15A	0.990 (6)
Os—C1	2.305 (5)	C15—H15B	0.991 (6)
Os—C2	2.293 (5)	C15—C16	1.534 (7)
Os—C3	2.247 (5)	C16—H16A	0.989 (5)
Os—C4	2.254 (5)	C16—H16B	0.990 (5)
Os—C5	2.270 (5)	C21—H21	1.000 (4)
Os—P	2.3670 (11)	C21—C22	1.543 (6)
C1—C2	1.435 (7)	C21—C26	1.535 (6)
C1—C5	1.431 (7)	C22—H22A	0.989 (5)
C1—C6	1.497 (7)	C22—H22B	0.989 (5)
C2—C3	1.442 (7)	C22—C23	1.534 (7)
C2—C7	1.502 (7)	C23—H23A	0.990 (5)
C3—C4	1.446 (7)	C23—H23B	0.989 (5)
C3—C8	1.497 (8)	C23—C24	1.525 (7)
C4—C5	1.436 (7)	C24—H24A	0.990 (5)
C4—C9	1.493 (8)	C24—H24B	0.988 (5)
C5—C10	1.497 (7)	C24—C25	1.525 (7)
C6—H6A	0.979 (6)	C25—H25A	0.988 (5)
C6—H6B	0.981 (6)	C25—H25B	0.990 (5)
C6—H6C	0.979 (6)	C25—C26	1.538 (7)
C8—H8A	0.982 (8)	C26—H26A	0.989 (5)
C8—H8B	0.978 (6)	C26—H26B	0.990 (5)
C8—H8C	0.982 (7)	C31—H31	1.002 (4)
C7—H7A	0.980 (6)	C31—C32	1.552 (6)
C7—H7B	0.980 (6)	C31—C36	1.539 (6)
C7—H7C	0.979 (7)	C32—H32A	0.989 (5)
C9—H9A	0.979 (6)	C32—H32B	0.990 (5)
C9—H9B	0.981 (7)	C32—C33	1.533 (6)
C9—H9C	0.980 (7)	C33—H33A	0.992 (5)
C10—H10A	0.980 (6)	C33—H33B	0.986 (5)
C10—H10B	0.980 (6)	C33—C34	1.528 (7)
C10—H10C	0.981 (7)	C34—H34A	0.990 (5)
P—C11	1.853 (5)	C34—H34B	0.988 (5)
P—C21	1.851 (5)	C34—C35	1.526 (7)
P—C31	1.871 (5)	C35—H35A	0.990 (5)
C11—H11	0.999 (4)	C35—H35B	0.990 (5)
C11—C12	1.544 (6)	C35—C36	1.536 (6)
C11—C16	1.531 (6)	C36—H36A	0.992 (5)
C12—H12A	0.988 (5)	C36—H36B	0.989 (4)
C12—H12B	0.990 (5)	B—F1	1.371 (8)
C12—C13	1.532 (7)	B—F2	1.377 (9)
C13—H13A	0.989 (6)	B—F3	1.362 (9)
C13—H13B	0.991 (6)	B—F4	1.378 (9)
C13—C14	1.520 (8)
H2—Os—H1	129 (3)	C12—C11—H11	106.8 (4)
H3—Os—H1	95 (3)	C16—C11—P	112.9 (3)
H3—Os—H2	67 (3)	C16—C11—H11	107.0 (4)
H4—Os—H1	54 (3)	C16—C11—C12	110.6 (4)
H4—Os—H2	106 (3)	H12A—C12—C11	109.3 (4)
H4—Os—H3	45 (3)	H12B—C12—C11	109.3 (4)
C1—Os—H1	110 (2)	H12B—C12—H12A	108.0 (5)
C1—Os—H2	105 (2)	C13—C12—C11	111.2 (4)
C1—Os—H3	150 (2)	C13—C12—H12A	109.4 (5)
C1—Os—H4	147 (2)	C13—C12—H12B	109.4 (4)
C2—Os—H1	144 (2)	H13A—C13—C12	109.6 (5)
C2—Os—H2	83 (2)	H13B—C13—C12	109.5 (5)
C2—Os—H3	115 (2)	H13B—C13—H13A	108.1 (5)
C2—Os—H4	142 (2)	C14—C13—C12	110.9 (4)
C2—Os—C1	36.37 (17)	C14—C13—H13A	109.4 (5)
C3—Os—H1	132 (2)	C14—C13—H13B	109.3 (5)
C3—Os—H2	97 (2)	H14A—C14—C13	109.6 (5)
C3—Os—H3	90 (2)	H14B—C14—C13	109.8 (5)
C3—Os—H4	105 (2)	H14B—C14—H14A	108.1 (5)
C3—Os—C1	61.65 (18)	C15—C14—C13	110.2 (5)
C3—Os—C2	37.01 (19)	C15—C14—H14A	109.5 (5)
C4—Os—H1	95 (2)	C15—C14—H14B	109.7 (5)
C4—Os—H2	135 (2)	H15A—C15—C14	109.3 (5)
C4—Os—H3	102 (2)	H15B—C15—C14	109.2 (5)
C4—Os—H4	89 (2)	H15B—C15—H15A	108.0 (5)
C4—Os—C1	61.64 (18)	C16—C15—C14	111.6 (5)
C4—Os—C2	61.72 (19)	C16—C15—H15A	109.3 (5)
C4—Os—C3	37.48 (19)	C16—C15—H15B	109.3 (5)
C5—Os—H1	84 (2)	C15—C16—C11	110.9 (4)
C5—Os—H2	141 (2)	H16A—C16—C11	109.4 (4)
C5—Os—H3	138 (2)	H16A—C16—C15	109.5 (5)
C5—Os—H4	110 (2)	H16B—C16—C11	109.5 (4)
C5—Os—C1	36.45 (17)	H16B—C16—C15	109.4 (5)
C5—Os—C2	60.86 (18)	H16B—C16—H16A	108.1 (5)
C5—Os—C3	61.82 (19)	H21—C21—P	105.2 (3)
C5—Os—C4	37.02 (19)	C22—C21—P	114.6 (3)
P—Os—H1	68 (2)	C22—C21—H21	105.3 (4)
P—Os—H2	67 (2)	C26—C21—P	115.6 (3)
P—Os—H3	96 (2)	C26—C21—H21	105.4 (4)
P—Os—H4	94 (2)	C26—C21—C22	109.7 (4)
P—Os—C1	107.07 (13)	H22A—C22—C21	109.4 (4)
P—Os—C2	123.28 (13)	H22B—C22—C21	109.4 (4)
P—Os—C3	158.86 (15)	H22B—C22—H22A	108.1 (4)
P—Os—C4	155.72 (14)	C23—C22—C21	111.3 (4)
P—Os—C5	120.99 (14)	C23—C22—H22A	109.2 (4)
C2—C1—Os	71.3 (3)	C23—C22—H22B	109.3 (4)
C5—C1—Os	70.4 (3)	H23A—C23—C22	109.5 (4)
C5—C1—C2	107.5 (4)	H23B—C23—C22	109.5 (4)
C6—C1—Os	130.6 (4)	H23B—C23—H23A	108.2 (5)
C6—C1—C2	126.4 (5)	C24—C23—C22	110.7 (4)
C6—C1—C5	125.5 (5)	C24—C23—H23A	109.5 (4)
C1—C2—Os	72.3 (3)	C24—C23—H23B	109.5 (4)
C3—C2—Os	69.8 (3)	H24A—C24—C23	109.4 (4)
C3—C2—C1	108.4 (4)	H24B—C24—C23	109.5 (4)
C7—C2—Os	130.9 (3)	H24B—C24—H24A	108.2 (4)
C7—C2—C1	126.6 (5)	C25—C24—C23	111.0 (4)
C7—C2—C3	124.4 (5)	C25—C24—H24A	109.3 (4)
C2—C3—Os	73.2 (3)	C25—C24—H24B	109.4 (4)
C4—C3—Os	71.5 (3)	H25A—C25—C24	109.4 (4)
C4—C3—C2	107.8 (4)	H25B—C25—C24	109.4 (5)
C8—C3—Os	126.5 (4)	H25B—C25—H25A	108.1 (5)
C8—C3—C2	126.5 (5)	C26—C25—C24	111.1 (4)
C8—C3—C4	125.3 (5)	C26—C25—H25A	109.5 (4)
C3—C4—Os	71.0 (3)	C26—C25—H25B	109.4 (4)
C5—C4—Os	72.1 (3)	C25—C26—C21	110.9 (4)
C5—C4—C3	107.2 (4)	H26A—C26—C21	109.4 (4)
C9—C4—Os	126.7 (4)	H26A—C26—C25	109.5 (4)
C9—C4—C3	126.8 (5)	H26B—C26—C21	109.4 (4)
C9—C4—C5	125.8 (5)	H26B—C26—C25	109.5 (4)
C1—C5—Os	73.1 (3)	H26B—C26—H26A	108.2 (5)
C4—C5—Os	70.9 (3)	H31—C31—P	105.6 (3)
C4—C5—C1	109.1 (4)	C32—C31—P	116.5 (3)
C10—C5—Os	130.3 (4)	C32—C31—H31	105.6 (4)
C10—C5—C1	125.8 (5)	C36—C31—P	113.3 (3)
C10—C5—C4	124.2 (5)	C36—C31—H31	105.5 (4)
H6A—C6—C1	109.4 (5)	C36—C31—C32	109.3 (4)
H6B—C6—C1	109.4 (5)	H32A—C32—C31	109.5 (4)
H6B—C6—H6A	109.5 (6)	H32B—C32—C31	109.4 (4)
H6C—C6—C1	109.5 (5)	H32B—C32—H32A	108.2 (4)
H6C—C6—H6A	109.6 (5)	C33—C32—C31	110.7 (4)
H6C—C6—H6B	109.4 (6)	C33—C32—H32A	109.5 (4)
H8A—C8—C3	109.7 (6)	C33—C32—H32B	109.4 (4)
H8B—C8—C3	109.8 (6)	H33A—C33—C32	109.3 (4)
H8B—C8—H8A	109.5 (6)	H33B—C33—C32	109.6 (5)
H8C—C8—C3	109.3 (6)	H33B—C33—H33A	108.1 (5)
H8C—C8—H8A	109.2 (6)	C34—C33—C32	111.3 (4)
H8C—C8—H8B	109.4 (7)	C34—C33—H33A	109.1 (5)
H7A—C7—C2	109.4 (5)	C34—C33—H33B	109.3 (4)
H7B—C7—C2	109.4 (5)	H34A—C34—C33	109.5 (4)
H7B—C7—H7A	109.4 (6)	H34B—C34—C33	109.5 (4)
H7C—C7—C2	109.4 (5)	H34B—C34—H34A	108.2 (4)
H7C—C7—H7A	109.5 (6)	C35—C34—C33	111.0 (4)
H7C—C7—H7B	109.6 (6)	C35—C34—H34A	109.3 (4)
H9A—C9—C4	109.5 (6)	C35—C34—H34B	109.2 (4)
H9B—C9—C4	109.5 (6)	H35A—C35—C34	109.4 (4)
H9B—C9—H9A	109.4 (6)	H35B—C35—C34	109.4 (4)
H9C—C9—C4	109.4 (5)	H35B—C35—H35A	108.0 (4)
H9C—C9—H9A	109.6 (7)	C36—C35—C34	110.9 (4)
H9C—C9—H9B	109.4 (6)	C36—C35—H35A	109.5 (4)
H10A—C10—C5	109.5 (5)	C36—C35—H35B	109.5 (4)
H10B—C10—C5	109.5 (5)	C35—C36—C31	111.8 (4)
H10B—C10—H10A	109.6 (5)	H36A—C36—C31	109.0 (4)
H10C—C10—C5	109.4 (5)	H36A—C36—C35	109.3 (4)
H10C—C10—H10A	109.5 (6)	H36B—C36—C31	109.3 (4)
H10C—C10—H10B	109.4 (6)	H36B—C36—C35	109.4 (4)
C11—P—Os	114.82 (15)	H36B—C36—H36A	107.9 (4)
C21—P—Os	112.93 (14)	F2—B—F1	108.5 (6)
C21—P—C11	103.8 (2)	F3—B—F1	112.6 (6)
C31—P—Os	111.73 (14)	F3—B—F2	111.3 (7)
C31—P—C11	102.8 (2)	F4—B—F1	107.8 (6)
C31—P—C21	110.0 (2)	F4—B—F2	108.6 (6)
H11—C11—P	106.8 (3)	F4—B—F3	108.0 (6)
C12—C11—P	112.2 (3)

 

bis(chlorodimethylsilyl)hydrido(bis)cyclopentadienyl niobium (ZEYVAA_HAR_0_HADPs)

Crystal data

C14H23Cl2NbSi2	F(000) = 833.537
Mr = 411.32	Dx = 1.481 Mg m^−3
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
a = 16.584 (3) Å	Cell parameters from 24 reflections
b = 13.214 (3) Å	µ = 1.06 mm^−1
c = 8.419 (2) Å	T = 173 K
V = 1844.9 (7) Å^3	Block, pale beige
Z = 4	0.52 × 0.44 × 0.26 mm

Data collection

Enraf-Nonius CAD-4 diffractometer	Rint = 0.024
Absorption correction: psi scans	θmax = 30.0°, θmin = 2.5°
Tmin = 0.843, Tmax = 0.937	h = 0→23
2674 measured reflections	k = 0→18
2221 independent reflections	l = 0→9
2212 reflections with I ≥ 2u(I)

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.050	Only H-atom coordinates refined
wR(F^2) = 0.163	w = 1/[σ^2(Fo^2) + (0.1296P)^2 + 6.4728P] where P = (Fo^2 + 2Fc^2)/3
S = 0.97	(Δ/σ)max = 0.001
2221 reflections	Δρmax = 1.20 e Å^−3
127 parameters	Δρmin = −2.91 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Nb	0.17844 (3)	0.25	0.09931 (6)	0.02056 (18)
Si	0.11311 (6)	0.09476 (8)	0.23810 (14)	0.0249 (3)
Cl	0.15084 (8)	−0.05037 (8)	0.14537 (16)	0.0382 (3)
C3	0.2693 (4)	0.25	0.3192 (8)	0.0335 (13)
H3A	0.245 (3)	0.25	0.425 (6)	0.000000
C2	0.3148 (2)	0.1961 (4)	0.0773 (6)	0.0357 (10)
H2A	0.330 (2)	0.148 (3)	−0.018 (4)	0.000000
C5	0.1021 (3)	0.1631 (4)	−0.0996 (5)	0.0352 (10)
H5A	0.074 (2)	0.086 (3)	−0.097 (4)	0.000000
C6	0.0575 (4)	0.25	−0.0550 (8)	0.0335 (12)
H6A	0.004 (3)	0.25	−0.004 (6)	0.000000
C4	0.1751 (3)	0.1966 (4)	−0.1693 (6)	0.0434 (12)
H4A	0.228 (2)	0.146 (3)	−0.210 (4)	0.000000
C8	0.1347 (3)	0.0770 (4)	0.4555 (6)	0.0397 (10)
H8A	0.201 (2)	0.064 (3)	0.481 (5)	0.000000
H8B	0.095 (2)	0.012 (3)	0.499 (4)	0.000000
H8C	0.1146 (19)	0.135 (3)	0.516 (4)	0.000000
C1	0.2876 (3)	0.1626 (3)	0.2259 (6)	0.0357 (10)
H1A	0.287 (2)	0.084 (3)	0.270 (4)	0.000000
C7	0.0003 (3)	0.0833 (4)	0.2224 (7)	0.0373 (10)
H7A	−0.023 (2)	0.083 (3)	0.099 (4)	0.000000
H7B	−0.027 (2)	0.146 (3)	0.290 (4)	0.000000
H7C	−0.013 (2)	0.015 (3)	0.308 (4)	0.000000
H	0.105 (3)	0.25	0.275 (7)	0.000000

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Nb	0.0178 (2)	0.0177 (2)	0.0261 (3)	−0.000000	−0.00145 (15)	0.000000
Si	0.0230 (5)	0.0203 (5)	0.0312 (6)	−0.0014 (4)	−0.0001 (4)	0.0012 (4)
Cl	0.0446 (6)	0.0223 (4)	0.0476 (7)	0.0051 (4)	0.0002 (5)	−0.0014 (4)
C3	0.026 (3)	0.038 (3)	0.036 (4)	−0.000000	−0.001 (2)	0.000000
H3A	0.000000	0.000000	0.000000	−0.000000	0.000000	0.000000
C2	0.0231 (18)	0.035 (2)	0.049 (3)	0.0046 (15)	0.0050 (16)	0.000 (2)
H2A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C5	0.044 (2)	0.030 (2)	0.032 (2)	−0.0033 (18)	−0.0108 (17)	−0.0038 (16)
H5A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C6	0.029 (3)	0.035 (3)	0.036 (3)	−0.000000	−0.006 (2)	0.000000
H6A	0.000000	0.000000	0.000000	−0.000000	0.000000	0.000000
C4	0.043 (3)	0.049 (3)	0.039 (3)	0.009 (2)	0.0001 (19)	−0.013 (2)
H4A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C8	0.050 (3)	0.036 (2)	0.033 (3)	0.000 (2)	0.000 (2)	0.0048 (19)
H8A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H8B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H8C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C1	0.0265 (18)	0.0295 (19)	0.051 (3)	0.0041 (16)	−0.0100 (18)	0.0055 (18)
H1A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C7	0.0250 (18)	0.037 (2)	0.050 (3)	−0.0084 (16)	0.0028 (18)	−0.003 (2)
H7A	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H7B	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H7C	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H	0.000000	0.000000	0.000000	−0.000000	0.000000	0.000000

Geometric parameters (Å, º)

Nb—Si^i	2.5975 (12)	C3—C1	1.430 (6)
Nb—Si	2.5975 (12)	C2—C2^i	1.424 (10)
Nb—C3	2.387 (7)	C2—H2A	1.06 (4)
Nb—C2	2.379 (4)	C2—C1	1.403 (7)
Nb—C2^i	2.379 (4)	C5—H5A	1.12 (4)
Nb—C5	2.393 (4)	C5—C6	1.417 (6)
Nb—C5^i	2.393 (4)	C5—C4	1.417 (7)
Nb—C6	2.390 (6)	C6—H6A	0.99 (5)
Nb—C4	2.369 (5)	C4—C4^i	1.410 (12)
Nb—C4^i	2.369 (5)	C4—H4A	1.16 (4)
Nb—C1^i	2.397 (4)	C8—H8A	1.13 (4)
Nb—C1	2.397 (4)	C8—H8B	1.14 (4)
Nb—H	1.92 (6)	C8—H8C	0.98 (3)
Si—Cl	2.1630 (15)	C1—H1A	1.11 (4)
Si—C8	1.880 (5)	C7—H7A	1.11 (4)
Si—C7	1.881 (5)	C7—H7B	1.10 (4)
C3—H3A	0.97 (5)	C7—H7C	1.17 (4)
C3—C1^i	1.430 (6)
Si^i—Nb—Si	104.32 (5)	C1^i—Nb—C1	57.6 (2)
C3—Nb—Si	85.09 (10)	H—Nb—Si^i	52.23 (8)
C3—Nb—Si^i	85.09 (10)	H—Nb—Si	52.23 (8)
C2—Nb—Si	101.27 (13)	H—Nb—C3	78.7 (17)
C2^i—Nb—Si^i	101.27 (13)	H—Nb—C2	131.7 (16)
C2^i—Nb—Si	131.92 (13)	H—Nb—C2^i	131.7 (16)
C2—Nb—Si^i	131.92 (13)	H—Nb—C5	101.7 (15)
C2—Nb—C3	57.3 (2)	H—Nb—C5^i	101.7 (15)
C2^i—Nb—C3	57.3 (2)	H—Nb—C6	83.4 (17)
C2^i—Nb—C2	34.8 (2)	H—Nb—C4^i	136.2 (15)
C5—Nb—Si	73.45 (12)	H—Nb—C4	136.2 (15)
C5^i—Nb—Si	118.25 (13)	H—Nb—C1^i	97.9 (15)
C5^i—Nb—Si^i	73.45 (12)	H—Nb—C1	97.9 (15)
C5—Nb—Si^i	118.25 (13)	Cl—Si—Nb	114.65 (6)
C5—Nb—C3	151.25 (12)	C8—Si—Nb	117.23 (17)
C5^i—Nb—C3	151.25 (12)	C8—Si—Cl	100.70 (17)
C5^i—Nb—C2^i	107.75 (18)	C7—Si—Nb	116.52 (17)
C5—Nb—C2	107.75 (18)	C7—Si—Cl	101.01 (16)
C5—Nb—C2^i	126.31 (18)	C7—Si—C8	104.3 (2)
C5^i—Nb—C2	126.31 (18)	H3A—C3—Nb	117 (3)
C5^i—Nb—C5	57.4 (2)	C1—C3—Nb	73.0 (3)
C6—Nb—Si	83.94 (11)	C1^i—C3—Nb	73.0 (3)
C6—Nb—Si^i	83.94 (11)	C1—C3—H3A	126.0 (3)
C6—Nb—C3	162.1 (2)	C1^i—C3—H3A	126.0 (3)
C6—Nb—C2	139.1 (2)	C1^i—C3—C1	107.9 (6)
C6—Nb—C2^i	139.1 (2)	C2^i—C2—Nb	72.59 (12)
C6—Nb—C5	34.47 (15)	H2A—C2—Nb	118.2 (19)
C6—Nb—C5^i	34.47 (15)	C1—C2—Nb	73.7 (2)
C4^i—Nb—Si^i	100.64 (15)	C1—C2—H2A	124 (2)
C4^i—Nb—Si	130.89 (14)	H5A—C5—Nb	129.8 (19)
C4—Nb—Si^i	130.89 (14)	C6—C5—Nb	72.7 (3)
C4—Nb—Si	100.64 (15)	C6—C5—H5A	121 (2)
C4—Nb—C3	139.01 (19)	C4—C5—Nb	71.8 (3)
C4^i—Nb—C3	139.01 (19)	C4—C5—H5A	130 (2)
C4—Nb—C2^i	92.11 (19)	C4—C5—C6	107.6 (5)
C4^i—Nb—C2^i	81.87 (18)	C5^i—C6—Nb	72.9 (3)
C4^i—Nb—C2	92.11 (19)	C5—C6—Nb	72.9 (3)
C4—Nb—C2	81.87 (18)	C5^i—C6—C5	108.3 (6)
C4—Nb—C5^i	57.49 (17)	H6A—C6—Nb	121 (3)
C4^i—Nb—C5^i	34.61 (18)	H6A—C6—C5^i	125.9 (3)
C4—Nb—C5	34.61 (18)	H6A—C6—C5	125.9 (3)
C4^i—Nb—C5	57.49 (17)	C5—C4—Nb	73.6 (3)
C4—Nb—C6	57.4 (2)	C4^i—C4—Nb	72.69 (18)
C4^i—Nb—C6	57.4 (2)	C4^i—C4—C5	108.2 (3)
C4^i—Nb—C4	34.6 (3)	H4A—C4—Nb	115.9 (19)
C1^i—Nb—Si	119.70 (13)	H4A—C4—C5	126 (2)
C1—Nb—Si	74.59 (11)	H8A—C8—Si	113 (2)
C1^i—Nb—Si^i	74.59 (11)	H8B—C8—Si	107.2 (19)
C1—Nb—Si^i	119.70 (13)	H8B—C8—H8A	112 (3)
C1—Nb—C3	34.77 (14)	H8C—C8—Si	110 (2)
C1^i—Nb—C3	34.77 (14)	H8C—C8—H8A	111 (3)
C1^i—Nb—C2^i	34.15 (17)	H8C—C8—H8B	103 (3)
C1—Nb—C2^i	57.38 (17)	C3—C1—Nb	72.2 (3)
C1^i—Nb—C2	57.38 (17)	C2—C1—Nb	72.2 (2)
C1—Nb—C2	34.15 (17)	C2—C1—C3	107.6 (4)
C1^i—Nb—C5^i	118.63 (17)	H1A—C1—Nb	127 (2)
C1—Nb—C5^i	160.37 (18)	H1A—C1—C3	125 (2)
C1^i—Nb—C5	160.37 (18)	H1A—C1—C2	127 (2)
C1—Nb—C5	118.63 (17)	H7A—C7—Si	114 (2)
C1^i—Nb—C6	151.09 (11)	H7B—C7—Si	108.0 (19)
C1—Nb—C6	151.09 (11)	H7B—C7—H7A	111 (3)
C1—Nb—C4^i	125.83 (19)	H7C—C7—Si	101.7 (19)
C1^i—Nb—C4	125.83 (19)	H7C—C7—H7A	120 (3)
C1—Nb—C4	107.37 (18)	H7C—C7—H7B	101 (3)
C1^i—Nb—C4^i	107.37 (18)

Symmetry code: (i) x, −y+1/2, z.

bis(chlorodimethylsilyl)hydrido(bis)cyclopentadienyl niobium (ZEYVAA_HAR)

Crystal data

C14H23Cl2NbSi2	F(000) = 833.472
Mr = 411.32	Dx = 1.481 Mg m^−3
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
a = 16.584 (3) Å	Cell parameters from 24 reflections
b = 13.214 (3) Å	µ = 1.06 mm^−1
c = 8.419 (2) Å	T = 173 K
V = 1844.9 (7) Å^3	Block, pale beige
Z = 4	0.52 × 0.44 × 0.26 mm

Data collection

Enraf-Nonius CAD-4 diffractometer	Rint = 0.024
Absorption correction: psi scans	θmax = 30.0°, θmin = 2.5°
Tmin = 0.843, Tmax = 0.937	h = 0→23
2674 measured reflections	k = 0→18
2221 independent reflections	l = 0→9
2212 reflections with I ≥ 2u(I)

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.051	All H-atom parameters refined
wR(F^2) = 0.178	w = 1/[σ^2(Fo^2) + (0.1P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 1.73	(Δ/σ)max = 0.001
2221 reflections	Δρmax = 1.20 e Å^−3
140 parameters	Δρmin = −3.29 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Nb	0.17846 (2)	0.25	0.09928 (5)	0.0237 (2)
Si	0.11318 (6)	0.09472 (7)	0.23810 (12)	0.0233 (3)
Cl	0.15086 (7)	−0.05033 (7)	0.14529 (14)	0.0365 (3)
C3	0.2695 (3)	0.25	0.3192 (8)	0.0324 (11)
H3A	0.250 (4)	0.25	0.420 (7)	0.025 (14)*
C2	0.3149 (2)	0.1965 (4)	0.0779 (6)	0.0342 (9)
H2A	0.335 (3)	0.143 (5)	−0.026 (7)	0.038 (15)*
C5	0.1026 (3)	0.1633 (3)	−0.1002 (4)	0.0326 (8)
H5A	0.091 (5)	0.088 (6)	−0.097 (7)	0.058 (19)*
C6	0.0579 (3)	0.25	−0.0557 (7)	0.0316 (10)
H6A	0.005 (5)	0.25	−0.017 (11)	0.06 (2)*
C4	0.1750 (3)	0.1970 (4)	−0.1691 (6)	0.0416 (11)
H4A	0.219 (5)	0.156 (6)	−0.225 (10)	0.09 (3)*
C8	0.1344 (3)	0.0772 (3)	0.4558 (6)	0.0380 (9)
H8A	0.196 (5)	0.054 (7)	0.477 (10)	0.07 (2)*
H8B	0.095 (3)	0.005 (5)	0.509 (7)	0.037 (15)*
H8C	0.117 (4)	0.132 (6)	0.513 (8)	0.08 (2)*
C1	0.2875 (2)	0.1626 (3)	0.2262 (5)	0.0333 (8)
H1A	0.285 (6)	0.091 (7)	0.267 (11)	0.11 (3)*
C7	0.0005 (2)	0.0833 (3)	0.2222 (6)	0.0358 (9)
H7A	−0.010 (4)	0.078 (5)	0.100 (7)	0.043 (16)*
H7B	−0.023 (6)	0.122 (8)	0.279 (13)	0.12 (3)*
H7C	−0.019 (4)	0.015 (5)	0.305 (8)	0.049 (17)*
H	0.099 (4)	0.25	0.261 (7)	0.023 (17)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Nb	0.0206 (3)	0.0204 (3)	0.0303 (4)	−0.000000	−0.00133 (12)	0.000000
Si	0.0213 (4)	0.0190 (4)	0.0295 (6)	−0.0017 (3)	0.0000 (3)	0.0010 (3)
Cl	0.0426 (6)	0.0204 (4)	0.0464 (6)	0.0052 (3)	0.0006 (4)	−0.0015 (4)
C3	0.024 (2)	0.037 (3)	0.036 (3)	−0.000000	−0.003 (2)	0.000000
C2	0.0208 (16)	0.032 (2)	0.050 (3)	0.0049 (13)	0.0054 (14)	−0.0007 (17)
C5	0.043 (2)	0.0273 (17)	0.028 (2)	−0.0037 (16)	−0.0103 (14)	−0.0036 (13)
C6	0.029 (3)	0.032 (2)	0.034 (3)	−0.000000	−0.008 (2)	0.000000
C4	0.040 (2)	0.045 (3)	0.040 (3)	0.0086 (17)	0.0023 (16)	−0.013 (2)
C8	0.047 (2)	0.0336 (19)	0.034 (2)	−0.0012 (18)	−0.0034 (19)	0.0050 (17)
C1	0.0246 (15)	0.0255 (16)	0.050 (2)	0.0043 (13)	−0.0098 (15)	0.0052 (15)
C7	0.0238 (17)	0.0332 (18)	0.050 (3)	−0.0069 (14)	0.0035 (16)	−0.0045 (18)

Geometric parameters (Å, º)

Nb—Si^i	2.5977 (10)	C3—C1	1.426 (5)
Nb—Si	2.5977 (10)	C2—C2^i	1.415 (10)
Nb—C3	2.389 (6)	C2—H2A	1.17 (6)
Nb—C2	2.378 (4)	C2—C1	1.402 (6)
Nb—C2^i	2.378 (4)	C5—H5A	1.01 (7)
Nb—C5	2.391 (4)	C5—C6	1.415 (6)
Nb—C5^i	2.391 (4)	C5—C4	1.406 (7)
Nb—C6	2.388 (5)	C6—H6A	0.94 (9)
Nb—C4^i	2.366 (5)	C4—C4^i	1.401 (11)
Nb—C4	2.366 (5)	C4—H4A	1.02 (8)
Nb—C1^i	2.397 (4)	C8—H8A	1.08 (8)
Nb—C1	2.397 (4)	C8—H8B	1.24 (6)
Nb—H	1.90 (7)	C8—H8C	0.91 (8)
Si—Cl	2.1622 (13)	C1—H1A	1.01 (10)
Si—C8	1.880 (5)	C7—H7A	1.05 (6)
Si—C7	1.879 (4)	C7—H7B	0.80 (11)
C3—H3A	0.91 (6)	C7—H7C	1.19 (7)
C3—C1^i	1.426 (5)
Si^i—Nb—Si	104.35 (4)	C1^i—Nb—C1	57.58 (18)
C3—Nb—Si	85.10 (9)	H—Nb—Si^i	52.18 (4)
C3—Nb—Si^i	85.10 (9)	H—Nb—Si	52.18 (4)
C2—Nb—Si	101.29 (12)	H—Nb—C3	83 (2)
C2^i—Nb—Si^i	101.29 (12)	H—Nb—C2	135.8 (19)
C2^i—Nb—Si	131.73 (12)	H—Nb—C2^i	135.8 (19)
C2—Nb—Si^i	131.73 (12)	H—Nb—C5	97.9 (18)
C2—Nb—C3	57.13 (19)	H—Nb—C5^i	97.9 (18)
C2^i—Nb—C3	57.13 (19)	H—Nb—C6	79 (2)
C2^i—Nb—C2	34.6 (2)	H—Nb—C4^i	132.0 (19)
C5—Nb—Si	73.63 (10)	H—Nb—C4	132.0 (19)
C5^i—Nb—Si	118.38 (11)	H—Nb—C1^i	101.8 (18)
C5^i—Nb—Si^i	73.63 (10)	H—Nb—C1	101.8 (18)
C5—Nb—Si^i	118.38 (11)	Cl—Si—Nb	114.66 (5)
C5—Nb—C3	151.27 (10)	C8—Si—Nb	117.22 (15)
C5^i—Nb—C3	151.27 (10)	C8—Si—Cl	100.90 (15)
C5^i—Nb—C2^i	107.77 (16)	C7—Si—Nb	116.47 (15)
C5—Nb—C2	107.77 (16)	C7—Si—Cl	100.98 (15)
C5—Nb—C2^i	126.18 (16)	C7—Si—C8	104.2 (2)
C5^i—Nb—C2	126.18 (16)	H3A—C3—Nb	120 (4)
C5^i—Nb—C5	57.3 (2)	C1—C3—Nb	73.0 (3)
C6—Nb—Si	84.07 (10)	C1^i—C3—Nb	73.0 (3)
C6—Nb—Si^i	84.07 (10)	C1—C3—H3A	126.0 (3)
C6—Nb—C3	162.3 (2)	C1^i—C3—H3A	126.0 (3)
C6—Nb—C2	139.10 (19)	C1^i—C3—C1	108.0 (6)
C6—Nb—C2^i	139.10 (19)	C2^i—C2—Nb	72.70 (11)
C6—Nb—C5	34.46 (13)	H2A—C2—Nb	120 (3)
C6—Nb—C5^i	34.46 (13)	C1—C2—Nb	73.7 (2)
C4^i—Nb—Si^i	100.70 (14)	C1—C2—H2A	124 (3)
C4^i—Nb—Si	130.80 (12)	H5A—C5—Nb	123 (4)
C4—Nb—Si^i	130.80 (12)	C6—C5—Nb	72.6 (3)
C4—Nb—Si	100.70 (14)	C6—C5—H5A	133 (4)
C4—Nb—C3	139.06 (17)	C4—C5—Nb	71.8 (3)
C4^i—Nb—C3	139.06 (17)	C4—C5—H5A	119 (4)
C4—Nb—C2^i	92.24 (17)	C4—C5—C6	107.5 (4)
C4^i—Nb—C2^i	82.12 (16)	C5^i—C6—Nb	72.9 (3)
C4^i—Nb—C2	92.24 (17)	C5—C6—Nb	72.9 (3)
C4—Nb—C2	82.12 (16)	C5^i—C6—C5	108.1 (5)
C4—Nb—C5^i	57.21 (15)	H6A—C6—Nb	126 (6)
C4^i—Nb—C5^i	34.38 (16)	H6A—C6—C5^i	125.7 (5)
C4—Nb—C5	34.38 (16)	H6A—C6—C5	125.7 (5)
C4^i—Nb—C5	57.21 (15)	C5—C4—Nb	73.8 (3)
C4—Nb—C6	57.18 (19)	C4^i—C4—Nb	72.77 (10)
C4^i—Nb—C6	57.18 (19)	C4^i—C4—C5	108.46 (17)
C4^i—Nb—C4	34.5 (3)	H4A—C4—Nb	126 (5)
C1^i—Nb—Si	119.62 (11)	H4A—C4—C5	129 (5)
C1—Nb—Si	74.54 (10)	H8A—C8—Si	112 (4)
C1^i—Nb—Si^i	74.54 (10)	H8B—C8—Si	110 (3)
C1—Nb—Si^i	119.62 (11)	H8B—C8—H8A	102 (5)
C1—Nb—C3	34.68 (13)	H8C—C8—Si	111 (5)
C1^i—Nb—C3	34.68 (13)	H8C—C8—H8A	116 (6)
C1^i—Nb—C2^i	34.14 (16)	H8C—C8—H8B	105 (5)
C1—Nb—C2^i	57.24 (15)	C3—C1—Nb	72.3 (3)
C1^i—Nb—C2	57.24 (15)	C2—C1—Nb	72.2 (2)
C1—Nb—C2	34.14 (16)	C2—C1—C3	107.4 (4)
C1^i—Nb—C5^i	118.65 (14)	H1A—C1—Nb	125 (6)
C1—Nb—C5^i	160.23 (16)	H1A—C1—C3	124 (5)
C1^i—Nb—C5	160.23 (16)	H1A—C1—C2	128 (5)
C1—Nb—C5	118.65 (14)	H7A—C7—Si	104 (4)
C1^i—Nb—C6	151.11 (9)	H7B—C7—Si	113 (8)
C1—Nb—C6	151.11 (9)	H7B—C7—H7A	123 (9)
C1—Nb—C4^i	125.92 (16)	H7C—C7—Si	107 (3)
C1^i—Nb—C4	125.92 (16)	H7C—C7—H7A	119 (5)
C1—Nb—C4	107.55 (15)	H7C—C7—H7B	90 (8)
C1^i—Nb—C4^i	107.55 (15)

Symmetry code: (i) x, −y+1/2, z.

(ZEYVAA_HAR_NoMoRe_1)

Crystal data

C14H23Cl2NbSi2	F(000) = 833.537
Mr = 411.32	Dx = 1.481 Mg m^−3
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
a = 16.584 (3) Å	Cell parameters from 24 reflections
b = 13.214 (3) Å	µ = 1.06 mm^−1
c = 8.419 (2) Å	T = 173 K
V = 1844.9 (7) Å^3	Block, pale beige
Z = 4	0.52 × 0.44 × 0.26 mm

Data collection

Enraf-Nonius CAD-4 diffractometer	Rint = 0.024
Absorption correction: psi scans	θmax = 30.0°, θmin = 2.5°
Tmin = 0.843, Tmax = 0.937	h = 0→23
2674 measured reflections	k = 0→18
2221 independent reflections	l = 0→9
2212 reflections with I ≥ 2u(I)

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.040	Only H-atom coordinates refined
wR(F^2) = 0.123	w = 1/[σ^2(Fo^2) + (0.0613P)^2 + 12.0566P] where P = (Fo^2 + 2Fc^2)/3
S = 0.96	(Δ/σ)max = 0.001
2221 reflections	Δρmax = 1.21 e Å^−3
127 parameters	Δρmin = −2.73 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Nb	0.17844 (3)	0.25	0.09926 (6)	0.01973 (14)
Si	0.11308 (6)	0.09477 (8)	0.23815 (14)	0.0241 (2)
Cl	0.15084 (7)	−0.05032 (7)	0.14538 (15)	0.0375 (3)
C3	0.2694 (4)	0.25	0.3191 (8)	0.0335 (13)
H3A	0.246 (5)	0.25	0.429 (10)	0.057000
C2	0.3149 (2)	0.1961 (3)	0.0773 (6)	0.0356 (10)
H2A	0.335 (4)	0.144 (5)	−0.021 (8)	0.057333
C5	0.1022 (3)	0.1630 (3)	−0.0992 (5)	0.0341 (9)
H5A	0.083 (5)	0.087 (5)	−0.100 (8)	0.064333
C6	0.0577 (4)	0.25	−0.0550 (8)	0.0323 (12)
H6A	0.001 (5)	0.25	−0.005 (11)	0.054667
C4	0.1751 (3)	0.1967 (4)	−0.1693 (6)	0.0419 (11)
H4A	0.225 (4)	0.149 (6)	−0.215 (8)	0.073333
C8	0.1348 (3)	0.0772 (4)	0.4557 (6)	0.0385 (10)
H8A	0.200 (4)	0.062 (6)	0.480 (8)	0.070333
H8B	0.097 (4)	0.012 (5)	0.502 (8)	0.063333
H8C	0.109 (5)	0.140 (5)	0.515 (8)	0.073000
C1	0.2873 (2)	0.1626 (3)	0.2271 (6)	0.0348 (9)
H1A	0.285 (4)	0.082 (5)	0.270 (9)	0.057000
C7	0.0006 (3)	0.0831 (4)	0.2226 (6)	0.0373 (10)
H7A	−0.024 (4)	0.081 (6)	0.101 (8)	0.064000
H7B	−0.027 (4)	0.147 (5)	0.285 (10)	0.071667
H7C	−0.019 (4)	0.016 (5)	0.292 (8)	0.061667
H	0.103 (5)	0.25	0.265 (10)	0.039667

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Nb	0.0175 (2)	0.0175 (2)	0.0242 (3)	−0.000000	−0.00143 (16)	0.000000
Si	0.0229 (4)	0.0201 (4)	0.0293 (6)	−0.0015 (4)	0.0000 (4)	0.0010 (4)
Cl	0.0443 (6)	0.0223 (4)	0.0458 (6)	0.0049 (4)	0.0002 (5)	−0.0015 (4)
C3	0.025 (2)	0.039 (3)	0.037 (4)	−0.000000	0.000 (2)	0.000000
H3A	0.050000	0.079000	0.042000	−0.000000	−0.008000	0.000000
C2	0.0225 (17)	0.034 (2)	0.051 (3)	0.0040 (15)	0.0040 (17)	−0.0003 (19)
H2A	0.047000	0.056000	0.069000	0.012000	0.011000	−0.015000
C5	0.044 (2)	0.0290 (19)	0.030 (2)	−0.0033 (17)	−0.0095 (17)	−0.0029 (16)
H5A	0.088000	0.038000	0.067000	−0.016000	−0.018000	−0.010000
C6	0.030 (3)	0.033 (3)	0.034 (3)	−0.000000	−0.006 (2)	0.000000
H6A	0.032000	0.079000	0.053000	−0.000000	−0.001000	0.000000
C4	0.043 (3)	0.047 (3)	0.036 (3)	0.007 (2)	0.000 (2)	−0.013 (2)
H4A	0.065000	0.097000	0.058000	0.027000	0.004000	−0.028000
C8	0.048 (3)	0.037 (2)	0.030 (2)	0.001 (2)	0.002 (2)	0.0065 (19)
H8A	0.055000	0.096000	0.060000	−0.005000	−0.015000	0.022000
H8B	0.075000	0.055000	0.060000	−0.011000	0.008000	0.021000
H8C	0.117000	0.056000	0.046000	0.012000	−0.002000	−0.006000
C1	0.0250 (17)	0.0300 (19)	0.049 (3)	0.0044 (15)	−0.0090 (17)	0.0052 (19)
H1A	0.049000	0.040000	0.082000	0.010000	−0.006000	0.018000
C7	0.0247 (18)	0.036 (2)	0.052 (3)	−0.0087 (16)	0.0012 (18)	−0.002 (2)
H7A	0.047000	0.076000	0.069000	−0.019000	−0.017000	0.011000
H7B	0.040000	0.060000	0.115000	−0.001000	0.017000	−0.024000
H7C	0.057000	0.056000	0.072000	−0.026000	0.005000	0.010000
H	0.035000	0.042000	0.042000	−0.000000	0.005000	0.000000

Geometric parameters (Å, º)

Nb—Si^i	2.5979 (11)	C3—C1	1.422 (6)
Nb—Si	2.5979 (11)	C2—C2^i	1.425 (9)
Nb—C3	2.388 (7)	C2—H2A	1.13 (6)
Nb—C2	2.381 (4)	C2—C1	1.413 (7)
Nb—C2^i	2.381 (4)	C5—H5A	1.06 (6)
Nb—C5	2.390 (4)	C5—C6	1.415 (6)
Nb—C5^i	2.390 (4)	C5—C4	1.417 (7)
Nb—C6	2.386 (6)	C6—H6A	1.02 (9)
Nb—C4^i	2.369 (5)	C4—C4^i	1.410 (11)
Nb—C4	2.369 (5)	C4—H4A	1.10 (6)
Nb—C1^i	2.399 (4)	C8—H8A	1.13 (7)
Nb—C1	2.399 (4)	C8—H8B	1.13 (6)
Nb—H	1.87 (8)	C8—H8C	1.06 (7)
Si—Cl	2.1629 (15)	C1—H1A	1.12 (6)
Si—C8	1.881 (5)	C7—H7A	1.10 (6)
Si—C7	1.877 (5)	C7—H7B	1.10 (7)
C3—H3A	1.00 (9)	C7—H7C	1.11 (6)
C3—C1^i	1.422 (6)
Si^i—Nb—Si	104.28 (5)	C1^i—Nb—C1	57.6 (2)
C3—Nb—Si	85.11 (10)	H—Nb—Si^i	52.15 (4)
C3—Nb—Si^i	85.11 (10)	H—Nb—Si	52.15 (4)
C2—Nb—Si	101.27 (11)	H—Nb—C3	81 (2)
C2^i—Nb—Si^i	101.27 (11)	H—Nb—C2	134 (2)
C2^i—Nb—Si	131.92 (12)	H—Nb—C2^i	134 (2)
C2—Nb—Si^i	131.92 (12)	H—Nb—C5	100 (2)
C2—Nb—C3	57.27 (19)	H—Nb—C5^i	100 (2)
C2^i—Nb—C3	57.27 (19)	H—Nb—C6	81 (2)
C2^i—Nb—C2	34.8 (2)	H—Nb—C4^i	134 (2)
C5—Nb—Si	73.40 (11)	H—Nb—C4	134 (2)
C5^i—Nb—Si	118.26 (12)	H—Nb—C1^i	100 (2)
C5^i—Nb—Si^i	73.40 (11)	H—Nb—C1	100 (2)
C5—Nb—Si^i	118.26 (12)	Cl—Si—Nb	114.62 (6)
C5—Nb—C3	151.19 (11)	C8—Si—Nb	117.14 (16)
C5^i—Nb—C3	151.19 (11)	C8—Si—Cl	100.75 (16)
C5^i—Nb—C2^i	107.75 (17)	C7—Si—Nb	116.62 (16)
C5—Nb—C2	107.75 (17)	C7—Si—Cl	100.95 (16)
C5—Nb—C2^i	126.36 (17)	C7—Si—C8	104.4 (2)
C5^i—Nb—C2	126.36 (17)	H3A—C3—Nb	118 (5)
C5^i—Nb—C5	57.5 (2)	C1—C3—Nb	73.1 (3)
C6—Nb—Si	83.97 (10)	C1^i—C3—Nb	73.1 (3)
C6—Nb—Si^i	83.97 (10)	C1—C3—H3A	125.7 (3)
C6—Nb—C3	162.2 (2)	C1^i—C3—H3A	125.7 (3)
C6—Nb—C2	139.07 (19)	C1^i—C3—C1	108.6 (6)
C6—Nb—C2^i	139.07 (19)	C2^i—C2—Nb	72.58 (11)
C6—Nb—C5	34.47 (14)	H2A—C2—Nb	121 (3)
C6—Nb—C5^i	34.47 (14)	C1—C2—Nb	73.5 (2)
C4^i—Nb—Si^i	100.66 (14)	C1—C2—H2A	124 (4)
C4^i—Nb—Si	130.90 (13)	H5A—C5—Nb	128 (4)
C4—Nb—Si^i	130.90 (13)	C6—C5—Nb	72.6 (3)
C4—Nb—Si	100.66 (14)	C6—C5—H5A	128 (4)
C4—Nb—C3	138.97 (19)	C4—C5—Nb	71.9 (3)
C4^i—Nb—C3	138.97 (19)	C4—C5—H5A	124 (4)
C4—Nb—C2^i	92.12 (18)	C4—C5—C6	107.4 (4)
C4^i—Nb—C2^i	81.89 (17)	C5^i—C6—Nb	72.9 (3)
C4^i—Nb—C2	92.12 (18)	C5—C6—Nb	72.9 (3)
C4—Nb—C2	81.89 (17)	C5^i—C6—C5	108.6 (6)
C4—Nb—C5^i	57.55 (16)	H6A—C6—Nb	123 (5)
C4^i—Nb—C5^i	34.65 (17)	H6A—C6—C5^i	125.7 (3)
C4—Nb—C5	34.65 (17)	H6A—C6—C5	125.7 (3)
C4^i—Nb—C5	57.55 (16)	C5—C4—Nb	73.5 (3)
C4—Nb—C6	57.4 (2)	C4^i—C4—Nb	72.69 (12)
C4^i—Nb—C6	57.4 (2)	C4^i—C4—C5	108.3 (3)
C4^i—Nb—C4	34.6 (3)	H4A—C4—Nb	119 (4)
C1^i—Nb—Si	119.50 (12)	H4A—C4—C5	127 (4)
C1—Nb—Si	74.45 (11)	H8A—C8—Si	112 (4)
C1^i—Nb—Si^i	74.45 (11)	H8B—C8—Si	109 (4)
C1—Nb—Si^i	119.50 (12)	H8B—C8—H8A	110 (5)
C1—Nb—C3	34.57 (14)	H8C—C8—Si	106 (4)
C1^i—Nb—C3	34.57 (14)	H8C—C8—H8A	117 (6)
C1^i—Nb—C2^i	34.38 (16)	H8C—C8—H8B	102 (5)
C1—Nb—C2^i	57.52 (16)	C3—C1—Nb	72.3 (3)
C1^i—Nb—C2	57.52 (16)	C2—C1—Nb	72.1 (2)
C1—Nb—C2	34.38 (16)	C2—C1—C3	107.4 (4)
C1^i—Nb—C5^i	118.72 (16)	H1A—C1—Nb	125 (3)
C1—Nb—C5^i	160.66 (17)	H1A—C1—C3	126 (4)
C1^i—Nb—C5	160.66 (17)	H1A—C1—C2	127 (4)
C1—Nb—C5	118.72 (16)	H7A—C7—Si	115 (4)
C1^i—Nb—C6	151.14 (11)	H7B—C7—Si	109 (4)
C1—Nb—C6	151.14 (11)	H7B—C7—H7A	108 (6)
C1—Nb—C4^i	126.09 (18)	H7C—C7—Si	109 (4)
C1^i—Nb—C4	126.09 (18)	H7C—C7—H7A	111 (5)
C1—Nb—C4	107.60 (17)	H7C—C7—H7B	104 (5)
C1^i—Nb—C4^i	107.60 (17)
Nb—C3—C1—C2	64.0 (3)	Nb—C4—C5—C6	64.4 (3)
Nb—C3—C1^i—C2^i	−64.0 (3)	Nb^i—C4—C5—C6	64.4 (3)
Nb—C2^i—C2—C1	−65.4 (3)	Nb—C4—C4^i—C5^i	−65.4 (3)
Nb—C2—C2^i—C1^i	65.4 (3)	Nb—C4^i—C4—C5	65.4 (3)
Nb—C2—C1—C3	−64.2 (3)	Nb—C1—C3—C1^i	−65.0 (2)
Nb^i—C2—C1—C3	−64.2 (3)	Nb—C1^i—C3^i—C1	65.0 (2)
Nb—C5—C6—C5^i	64.7 (3)	Nb—C1^i—C2^i—C2	−64.76 (11)
Nb—C5^i—C6^i—C5	−64.7 (3)	Nb—C1—C2—C2^i	64.76 (11)
Nb—C5—C4—C4^i	−64.87 (10)	C3—C1—C2—C2^i	0.6 (4)
Nb—C5^i—C4^i—C4	64.87 (10)	C3—C1^i—C2^i—C2	−0.6 (4)
Nb—C6—C5—C4	−63.9 (3)	C5—C6—C5^i—C4^i	−0.8 (5)
Nb—C6—C5^i—C4^i	63.9 (3)	C5—C4—C4^i—C5^i	0.0 (6)

Symmetry code: (i) x, −y+1/2, z.

(ZEYVAA_HAR_NoMoRe)

Crystal data

C14H23Cl2NbSi2	F(000) = 833.537
Mr = 411.32	Dx = 1.481 Mg m^−3
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
a = 16.584 (3) Å	Cell parameters from 24 reflections
b = 13.214 (3) Å	µ = 1.06 mm^−1
c = 8.419 (2) Å	T = 173 K
V = 1844.9 (7) Å^3	Block, pale beige
Z = 4	0.52 × 0.44 × 0.26 mm

Data collection

Enraf-Nonius CAD-4 diffractometer	Rint = 0.024
Absorption correction: psi scans	θmax = 30.0°, θmin = 2.5°
Tmin = 0.843, Tmax = 0.937	h = 0→23
2674 measured reflections	k = 0→18
2221 independent reflections	l = 0→9
2212 reflections with I ≥ 2u(I)

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.050	Only H-atom coordinates refined
wR(F^2) = 0.171	w = 1/[σ^2(Fo^2) + (0.1P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 1.66	(Δ/σ)max = 0.001
2221 reflections	Δρmax = 1.12 e Å^−3
127 parameters	Δρmin = −3.05 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Nb	0.17844 (2)	0.25	0.09932 (5)	0.0214 (2)
Si	0.11312 (5)	0.09474 (6)	0.23815 (12)	0.0257 (2)
Cl	0.15083 (6)	−0.05040 (6)	0.14527 (13)	0.0391 (3)
C3	0.2696 (3)	0.25	0.3189 (7)	0.0345 (10)
H3A	0.249 (5)	0.25	0.423 (8)	0.056667
C2	0.3149 (2)	0.1962 (4)	0.0775 (6)	0.0367 (9)
H2A	0.332 (3)	0.145 (5)	−0.020 (8)	0.056333
C5	0.1023 (3)	0.1632 (3)	−0.1002 (4)	0.0359 (8)
H5A	0.084 (5)	0.086 (5)	−0.096 (6)	0.064667
C6	0.0575 (3)	0.25	−0.0555 (7)	0.0342 (10)
H6A	0.001 (4)	0.25	−0.012 (9)	0.054333
C4	0.1753 (3)	0.1967 (4)	−0.1696 (6)	0.0438 (10)
H4A	0.225 (4)	0.146 (6)	−0.225 (7)	0.073000
C8	0.1343 (3)	0.0773 (3)	0.4563 (5)	0.0405 (8)
H8A	0.200 (4)	0.059 (6)	0.481 (8)	0.069667
H8B	0.097 (4)	0.008 (5)	0.503 (8)	0.063000
H8C	0.117 (4)	0.136 (5)	0.509 (6)	0.072000
C1	0.2874 (2)	0.1624 (3)	0.2263 (5)	0.0360 (8)
H1A	0.287 (4)	0.079 (4)	0.265 (8)	0.057333
C7	0.0005 (2)	0.0835 (3)	0.2227 (6)	0.0384 (8)
H7A	−0.018 (4)	0.082 (6)	0.104 (7)	0.063333
H7B	−0.028 (3)	0.144 (5)	0.281 (9)	0.071333
H7C	−0.017 (4)	0.014 (5)	0.296 (8)	0.061333
H	0.103 (4)	0.25	0.267 (8)	0.039333

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Nb	0.0183 (3)	0.0181 (3)	0.0278 (3)	−0.000000	−0.00137 (12)	0.000000
Si	0.0235 (4)	0.0212 (4)	0.0325 (5)	−0.0016 (3)	0.0000 (3)	0.0011 (3)
Cl	0.0451 (6)	0.0226 (4)	0.0496 (6)	0.0051 (3)	0.0003 (4)	−0.0017 (4)
C3	0.026 (2)	0.039 (2)	0.039 (3)	−0.000000	−0.003 (2)	0.000000
H3A	0.050000	0.079000	0.041000	−0.000000	−0.009000	0.000000
C2	0.0231 (15)	0.036 (2)	0.051 (2)	0.0044 (12)	0.0046 (13)	−0.0015 (17)
H2A	0.046000	0.054000	0.069000	0.012000	0.012000	−0.014000
C5	0.045 (2)	0.0302 (17)	0.033 (2)	−0.0041 (16)	−0.0113 (14)	−0.0044 (12)
H5A	0.089000	0.038000	0.067000	−0.017000	−0.018000	−0.010000
C6	0.031 (2)	0.033 (2)	0.039 (3)	−0.000000	−0.009 (2)	0.000000
H6A	0.031000	0.080000	0.052000	−0.000000	−0.002000	0.000000
C4	0.043 (2)	0.047 (2)	0.041 (3)	0.0086 (16)	0.0018 (16)	−0.0124 (19)
H4A	0.066000	0.096000	0.057000	0.027000	0.004000	−0.028000
C8	0.050 (2)	0.0359 (18)	0.035 (2)	−0.0005 (17)	−0.0037 (18)	0.0062 (16)
H8A	0.054000	0.096000	0.059000	−0.004000	−0.015000	0.022000
H8B	0.075000	0.054000	0.060000	−0.011000	0.009000	0.021000
H8C	0.115000	0.055000	0.046000	0.012000	−0.002000	−0.006000
C1	0.0263 (15)	0.0296 (16)	0.052 (2)	0.0043 (13)	−0.0097 (14)	0.0045 (15)
H1A	0.049000	0.041000	0.082000	0.010000	−0.005000	0.019000
C7	0.0256 (16)	0.0365 (17)	0.053 (2)	−0.0078 (13)	0.0018 (15)	−0.0024 (17)
H7A	0.047000	0.074000	0.069000	−0.019000	−0.017000	0.010000
H7B	0.039000	0.060000	0.115000	−0.001000	0.017000	−0.025000
H7C	0.057000	0.055000	0.072000	−0.027000	0.005000	0.009000
H	0.035000	0.042000	0.041000	−0.000000	0.005000	0.000000

Geometric parameters (Å, º)

Nb—Si^i	2.5979 (10)	C3—C1	1.426 (5)
Nb—Si	2.5979 (10)	C2—C2^i	1.421 (9)
Nb—C3	2.388 (5)	C2—H2A	1.10 (6)
Nb—C2	2.379 (3)	C2—C1	1.407 (6)
Nb—C2^i	2.379 (3)	C5—H5A	1.06 (6)
Nb—C5	2.394 (3)	C5—C6	1.417 (5)
Nb—C5^i	2.394 (3)	C5—C4	1.416 (6)
Nb—C6	2.391 (5)	C6—H6A	1.01 (7)
Nb—C4	2.372 (5)	C4—C4^i	1.410 (10)
Nb—C4^i	2.372 (5)	C4—H4A	1.16 (6)
Nb—C1^i	2.398 (3)	C8—H8A	1.14 (7)
Nb—C1	2.398 (3)	C8—H8B	1.18 (6)
Nb—H	1.89 (7)	C8—H8C	0.94 (6)
Si—Cl	2.1634 (13)	C1—H1A	1.14 (6)
Si—C8	1.884 (5)	C7—H7A	1.04 (6)
Si—C7	1.878 (4)	C7—H7B	1.04 (6)
C3—H3A	0.94 (7)	C7—H7C	1.15 (6)
C3—C1^i	1.426 (5)
Si^i—Nb—Si	104.32 (4)	C1^i—Nb—C1	57.73 (18)
C3—Nb—Si	85.17 (9)	H—Nb—Si^i	52.17 (4)
C3—Nb—Si^i	85.17 (9)	H—Nb—Si	52.17 (4)
C2—Nb—Si	101.27 (11)	H—Nb—C3	81 (2)
C2^i—Nb—Si^i	101.27 (11)	H—Nb—C2	134 (2)
C2^i—Nb—Si	131.87 (11)	H—Nb—C2^i	134 (2)
C2—Nb—Si^i	131.87 (11)	H—Nb—C5	100.0 (19)
C2—Nb—C3	57.16 (17)	H—Nb—C5^i	100.0 (19)
C2^i—Nb—C3	57.16 (17)	H—Nb—C6	81 (2)
C2^i—Nb—C2	34.8 (2)	H—Nb—C4^i	134 (2)
C5—Nb—Si	73.58 (10)	H—Nb—C4	134 (2)
C5^i—Nb—Si	118.29 (11)	H—Nb—C1^i	99.6 (19)
C5^i—Nb—Si^i	73.58 (10)	H—Nb—C1	99.6 (19)
C5—Nb—Si^i	118.29 (11)	Cl—Si—Nb	114.64 (5)
C5—Nb—C3	151.29 (10)	C8—Si—Nb	117.21 (14)
C5^i—Nb—C3	151.29 (10)	C8—Si—Cl	100.97 (14)
C5^i—Nb—C2^i	107.72 (16)	C7—Si—Nb	116.48 (14)
C5—Nb—C2	107.72 (16)	C7—Si—Cl	101.10 (14)
C5—Nb—C2^i	126.21 (16)	C7—Si—C8	104.1 (2)
C5^i—Nb—C2	126.21 (16)	H3A—C3—Nb	120 (5)
C5^i—Nb—C5	57.24 (18)	C1—C3—Nb	73.0 (3)
C6—Nb—Si	84.00 (9)	C1^i—C3—Nb	73.0 (3)
C6—Nb—Si^i	84.00 (9)	C1—C3—H3A	125.7 (3)
C6—Nb—C3	162.3 (2)	C1^i—C3—H3A	125.7 (3)
C6—Nb—C2	139.06 (18)	C1^i—C3—C1	108.5 (5)
C6—Nb—C2^i	139.06 (18)	C2^i—C2—Nb	72.62 (11)
C6—Nb—C5	34.45 (12)	H2A—C2—Nb	119 (3)
C6—Nb—C5^i	34.45 (12)	C1—C2—Nb	73.6 (2)
C4^i—Nb—Si^i	100.70 (13)	C1—C2—H2A	124 (4)
C4^i—Nb—Si	130.92 (12)	H5A—C5—Nb	126 (3)
C4—Nb—Si^i	130.92 (12)	C6—C5—Nb	72.7 (2)
C4—Nb—Si	100.70 (13)	C6—C5—H5A	128 (4)
C4—Nb—C3	138.83 (16)	C4—C5—Nb	71.9 (2)
C4^i—Nb—C3	138.83 (16)	C4—C5—H5A	124 (4)
C4—Nb—C2^i	92.05 (16)	C4—C5—C6	107.8 (4)
C4^i—Nb—C2^i	81.85 (15)	C5^i—C6—Nb	72.9 (2)
C4^i—Nb—C2	92.05 (16)	C5—C6—Nb	72.9 (2)
C4—Nb—C2	81.85 (15)	C5^i—C6—C5	108.1 (5)
C4—Nb—C5^i	57.39 (14)	H6A—C6—Nb	126 (4)
C4^i—Nb—C5^i	34.56 (15)	H6A—C6—C5^i	125.8 (4)
C4—Nb—C5	34.56 (15)	H6A—C6—C5	125.8 (4)
C4^i—Nb—C5	57.39 (14)	C5—C4—Nb	73.6 (2)
C4—Nb—C6	57.42 (17)	C4^i—C4—Nb	72.7 (2)
C4^i—Nb—C6	57.42 (17)	C4^i—C4—C5	108.2 (3)
C4^i—Nb—C4	34.6 (3)	H4A—C4—Nb	123 (3)
C1^i—Nb—Si	119.66 (10)	H4A—C4—C5	126 (4)
C1—Nb—Si	74.47 (9)	H8A—C8—Si	113 (4)
C1^i—Nb—Si^i	74.47 (9)	H8B—C8—Si	109 (3)
C1—Nb—Si^i	119.66 (10)	H8B—C8—H8A	106 (5)
C1—Nb—C3	34.67 (12)	H8C—C8—Si	108 (4)
C1^i—Nb—C3	34.67 (12)	H8C—C8—H8A	113 (6)
C1^i—Nb—C2^i	34.25 (15)	H8C—C8—H8B	109 (5)
C1—Nb—C2^i	57.45 (14)	C3—C1—Nb	72.3 (2)
C1^i—Nb—C2	57.45 (14)	C2—C1—Nb	72.1 (2)
C1—Nb—C2	34.25 (15)	C2—C1—C3	107.2 (4)
C1^i—Nb—C5^i	118.64 (14)	H1A—C1—Nb	126 (3)
C1—Nb—C5^i	160.36 (15)	H1A—C1—C3	129 (3)
C1^i—Nb—C5	160.36 (15)	H1A—C1—C2	124 (3)
C1—Nb—C5	118.64 (14)	H7A—C7—Si	111 (4)
C1^i—Nb—C6	151.04 (9)	H7B—C7—Si	111 (3)
C1—Nb—C6	151.04 (9)	H7B—C7—H7A	110 (6)
C1—Nb—C4^i	125.86 (15)	H7C—C7—Si	106 (3)
C1^i—Nb—C4	125.86 (15)	H7C—C7—H7A	115 (5)
C1—Nb—C4	107.39 (14)	H7C—C7—H7B	104 (5)
C1^i—Nb—C4^i	107.39 (14)

Symmetry code: (i) x, −y+1/2, z.

(ZEYVAA_HAR_SHADE3_1)

Crystal data

C14H23Cl2NbSi2	F(000) = 833.472
Mr = 411.32	Dx = 1.481 Mg m^−3
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
a = 16.584 (3) Å	Cell parameters from 24 reflections
b = 13.214 (3) Å	µ = 1.06 mm^−1
c = 8.419 (2) Å	T = 173 K
V = 1844.9 (7) Å^3	Block, pale beige
Z = 4	0.52 × 0.44 × 0.26 mm

Data collection

Enraf-Nonius CAD-4 diffractometer	Rint = 0.024
Absorption correction: psi scans	θmax = 30.0°, θmin = 2.5°
Tmin = 0.843, Tmax = 0.937	h = 0→23
2674 measured reflections	k = 0→18
2221 independent reflections	l = 0→9
2212 reflections with I ≥ 2u(I)

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.051	Only H-atom coordinates refined
wR(F^2) = 0.179	w = 1/[σ^2(Fo^2) + (0.1P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 1.74	(Δ/σ)max = 0.001
2221 reflections	Δρmax = 1.24 e Å^−3
127 parameters	Δρmin = −3.30 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Nb	0.17845 (2)	0.25	0.09930 (5)	0.0237 (2)
Si	0.11318 (6)	0.09474 (7)	0.23808 (12)	0.0233 (3)
Cl	0.15086 (7)	−0.05033 (7)	0.14529 (14)	0.0364 (3)
C3	0.2696 (3)	0.25	0.3191 (8)	0.0323 (11)
H3A	0.251 (5)	0.25	0.417 (8)	0.044970
C2	0.3149 (2)	0.1967 (4)	0.0777 (6)	0.0343 (9)
H2A	0.340 (4)	0.138 (7)	−0.028 (9)	0.056477
C5	0.1028 (3)	0.1632 (3)	−0.1002 (4)	0.0323 (8)
H5A	0.079 (5)	0.082 (5)	−0.101 (6)	0.045790
C6	0.0579 (3)	0.25	−0.0558 (7)	0.0313 (10)
H6A	0.008 (5)	0.25	−0.015 (10)	0.045797
C4	0.1751 (3)	0.1973 (4)	−0.1693 (6)	0.0414 (11)
H4A	0.227 (4)	0.152 (5)	−0.229 (7)	0.055093
C8	0.1345 (3)	0.0774 (3)	0.4562 (6)	0.0380 (9)
H8A	0.201 (4)	0.057 (6)	0.473 (9)	0.058207
H8B	0.100 (4)	0.006 (6)	0.511 (8)	0.066400
H8C	0.117 (4)	0.135 (5)	0.511 (7)	0.057897
C1	0.2873 (2)	0.1624 (3)	0.2263 (5)	0.0332 (8)
H1A	0.294 (4)	0.088 (4)	0.269 (7)	0.047100
C7	0.0006 (2)	0.0829 (3)	0.2219 (6)	0.0362 (9)
H7A	−0.019 (5)	0.072 (6)	0.095 (8)	0.058297
H7B	−0.018 (4)	0.126 (5)	0.262 (8)	0.057417
H7C	−0.016 (4)	0.011 (5)	0.301 (9)	0.063100
H	0.097 (5)	0.25	0.262 (9)	0.039583

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Nb	0.0205 (3)	0.0203 (3)	0.0302 (4)	−0.000000	−0.00136 (12)	0.000000
Si	0.0213 (4)	0.0190 (4)	0.0295 (6)	−0.0015 (3)	0.0000 (3)	0.0010 (3)
Cl	0.0424 (6)	0.0204 (4)	0.0465 (6)	0.0049 (3)	0.0006 (4)	−0.0015 (4)
C3	0.025 (2)	0.037 (3)	0.035 (3)	−0.000000	−0.004 (2)	0.000000
H3A	0.047690	0.046820	0.040400	−0.000000	−0.008490	0.000000
C2	0.0212 (16)	0.032 (2)	0.050 (3)	0.0048 (13)	0.0051 (14)	0.0003 (17)
H2A	0.047050	0.055640	0.066740	0.007800	0.019930	−0.006190
C5	0.042 (2)	0.0281 (17)	0.027 (2)	−0.0038 (16)	−0.0102 (14)	−0.0039 (13)
H5A	0.055780	0.032840	0.048750	−0.005780	−0.005580	−0.006360
C6	0.028 (2)	0.031 (2)	0.035 (3)	−0.000000	−0.008 (2)	0.000000
H6A	0.035250	0.042300	0.059840	−0.000000	−0.009820	0.000000
C4	0.040 (2)	0.046 (3)	0.039 (3)	0.0092 (17)	0.0011 (16)	−0.013 (2)
H4A	0.066850	0.051060	0.047370	0.003330	0.017540	−0.007000
C8	0.048 (2)	0.0339 (19)	0.032 (2)	−0.0011 (18)	−0.0036 (18)	0.0055 (17)
H8A	0.054450	0.065600	0.054570	0.007790	−0.011290	0.012770
H8B	0.086790	0.055040	0.057370	−0.020160	0.003130	0.020740
H8C	0.077530	0.053280	0.042880	0.010860	0.004130	−0.002190
C1	0.0245 (15)	0.0264 (16)	0.049 (2)	0.0048 (13)	−0.0098 (15)	0.0047 (15)
H1A	0.042860	0.037680	0.060760	0.010030	−0.003650	0.005770
C7	0.0242 (17)	0.0316 (17)	0.053 (3)	−0.0060 (14)	0.0036 (16)	−0.0063 (17)
H7A	0.045190	0.066570	0.063130	−0.013350	−0.012700	−0.002690
H7B	0.039230	0.052020	0.081000	−0.000850	0.010260	−0.013280
H7C	0.052530	0.048680	0.088090	−0.018360	0.006870	0.014630
H	0.034520	0.043560	0.040670	−0.000000	0.006060	0.000000

Geometric parameters (Å, º)

Nb—Si	2.5973 (10)	C3—C1	1.427 (5)
Nb—Si^i	2.5973 (10)	C2—C2^i	1.410 (10)
Nb—C3	2.390 (6)	C2—H2A	1.25 (7)
Nb—C2	2.377 (4)	C2—C1	1.406 (6)
Nb—C2^i	2.377 (4)	C5—H5A	1.14 (6)
Nb—C5^i	2.390 (4)	C5—C6	1.419 (5)
Nb—C5	2.390 (4)	C5—C4	1.406 (6)
Nb—C6	2.388 (5)	C6—H6A	0.90 (8)
Nb—C4^i	2.367 (5)	C4—C4^i	1.393 (11)
Nb—C4	2.367 (5)	C4—H4A	1.16 (6)
Nb—C1	2.396 (4)	C8—H8A	1.14 (7)
Nb—C1^i	2.396 (4)	C8—H8B	1.19 (6)
Nb—H	1.92 (7)	C8—H8C	0.94 (6)
Si—Cl	2.1624 (13)	C1—H1A	1.05 (6)
Si—C8	1.884 (5)	C7—H7A	1.13 (6)
Si—C7	1.878 (4)	C7—H7B	0.73 (6)
C3—H3A	0.88 (7)	C7—H7C	1.19 (7)
C3—C1^i	1.427 (5)
Si^i—Nb—Si	104.35 (4)	C1^i—Nb—C1	57.75 (18)
C3—Nb—Si	85.15 (9)	H—Nb—Si^i	52.19 (6)
C3—Nb—Si^i	85.15 (9)	H—Nb—Si	52.19 (6)
C2—Nb—Si	101.35 (12)	H—Nb—C3	84 (2)
C2^i—Nb—Si^i	101.35 (12)	H—Nb—C2	136 (2)
C2^i—Nb—Si	131.71 (12)	H—Nb—C2^i	136 (2)
C2—Nb—Si^i	131.71 (12)	H—Nb—C5	98 (2)
C2—Nb—C3	57.10 (19)	H—Nb—C5^i	98 (2)
C2^i—Nb—C3	57.10 (19)	H—Nb—C6	79 (2)
C2^i—Nb—C2	34.5 (2)	H—Nb—C4^i	132 (2)
C5—Nb—Si	73.63 (10)	H—Nb—C4	132 (2)
C5^i—Nb—Si	118.48 (11)	H—Nb—C1^i	102 (2)
C5^i—Nb—Si^i	73.63 (10)	H—Nb—C1	102 (2)
C5—Nb—Si^i	118.48 (11)	Cl—Si—Nb	114.66 (5)
C5—Nb—C3	151.20 (10)	C8—Si—Nb	117.15 (14)
C5^i—Nb—C3	151.20 (10)	C8—Si—Cl	100.93 (15)
C5^i—Nb—C2^i	107.66 (16)	C7—Si—Nb	116.59 (15)
C5—Nb—C2	107.66 (16)	C7—Si—Cl	100.77 (15)
C5—Nb—C2^i	126.03 (17)	C7—Si—C8	104.3 (2)
C5^i—Nb—C2	126.03 (17)	H3A—C3—Nb	120 (5)
C5^i—Nb—C5	57.40 (19)	C1—C3—Nb	72.9 (3)
C6—Nb—Si	84.09 (10)	C1^i—C3—Nb	72.9 (3)
C6—Nb—Si^i	84.09 (10)	C1—C3—H3A	125.8 (3)
C6—Nb—C3	162.4 (2)	C1^i—C3—H3A	125.8 (3)
C6—Nb—C2	139.05 (19)	C1^i—C3—C1	108.4 (6)
C6—Nb—C2^i	139.05 (19)	C2^i—C2—Nb	72.75 (11)
C6—Nb—C5	34.55 (13)	H2A—C2—Nb	124 (3)
C6—Nb—C5^i	34.55 (13)	C1—C2—Nb	73.6 (2)
C4^i—Nb—Si^i	100.81 (14)	C1—C2—H2A	123 (4)
C4^i—Nb—Si	130.72 (12)	H5A—C5—Nb	129 (3)
C4—Nb—Si^i	130.72 (12)	C6—C5—Nb	72.6 (3)
C4—Nb—Si	100.81 (14)	C6—C5—H5A	125 (4)
C4—Nb—C3	139.01 (17)	C4—C5—Nb	71.9 (3)
C4^i—Nb—C3	139.01 (17)	C4—C5—H5A	126 (4)
C4—Nb—C2^i	92.11 (17)	C4—C5—C6	107.3 (4)
C4^i—Nb—C2^i	82.09 (16)	C5^i—C6—Nb	72.8 (3)
C4^i—Nb—C2	92.11 (17)	C5—C6—Nb	72.8 (3)
C4—Nb—C2	82.09 (16)	C5^i—C6—C5	108.0 (5)
C4—Nb—C5^i	57.13 (15)	H6A—C6—Nb	124 (5)
C4^i—Nb—C5^i	34.38 (15)	H6A—C6—C5^i	125.9 (4)
C4—Nb—C5	34.38 (15)	H6A—C6—C5	125.9 (4)
C4^i—Nb—C5	57.13 (15)	C5—C4—Nb	73.7 (2)
C4—Nb—C6	57.16 (18)	C4^i—C4—Nb	72.9 (3)
C4^i—Nb—C6	57.16 (18)	C4^i—C4—C5	108.7 (3)
C4^i—Nb—C4	34.2 (3)	H4A—C4—Nb	123 (3)
C1^i—Nb—Si	119.66 (11)	H4A—C4—C5	130 (3)
C1—Nb—Si	74.45 (10)	H8A—C8—Si	109 (4)
C1^i—Nb—Si^i	74.45 (10)	H8B—C8—Si	113 (4)
C1—Nb—Si^i	119.66 (11)	H8B—C8—H8A	103 (5)
C1—Nb—C3	34.69 (12)	H8C—C8—Si	109 (4)
C1^i—Nb—C3	34.69 (12)	H8C—C8—H8A	115 (6)
C1^i—Nb—C2^i	34.26 (16)	H8C—C8—H8B	108 (5)
C1—Nb—C2^i	57.32 (15)	C3—C1—Nb	72.4 (3)
C1^i—Nb—C2	57.32 (15)	C2—C1—Nb	72.1 (2)
C1—Nb—C2	34.26 (16)	C2—C1—C3	107.0 (4)
C1^i—Nb—C5^i	118.49 (14)	H1A—C1—Nb	133 (3)
C1—Nb—C5^i	160.19 (16)	H1A—C1—C3	126 (3)
C1^i—Nb—C5	160.19 (16)	H1A—C1—C2	125 (3)
C1—Nb—C5	118.49 (14)	H7A—C7—Si	111 (4)
C1^i—Nb—C6	151.02 (9)	H7B—C7—Si	109 (5)
C1—Nb—C6	151.02 (9)	H7B—C7—H7A	115 (7)
C1—Nb—C4^i	125.88 (16)	H7C—C7—Si	105 (3)
C1^i—Nb—C4	125.88 (16)	H7C—C7—H7A	112 (5)
C1—Nb—C4	107.57 (15)	H7C—C7—H7B	105 (6)
C1^i—Nb—C4^i	107.57 (15)
Nb—C3—C1—C2	64.3 (3)	Nb—C4—C5—C6	64.5 (3)
Nb—C3—C1^i—C2^i	−64.3 (3)	Nb^i—C4—C5—C6	64.5 (3)
Nb—C2^i—C2—C1	−65.3 (3)	Nb—C4—C4^i—C5^i	−65.5 (3)
Nb—C2—C2^i—C1^i	65.3 (3)	Nb—C4^i—C4—C5	65.5 (3)
Nb—C2—C1—C3	−64.5 (3)	Nb—C1—C3—C1^i	−64.8 (2)
Nb^i—C2—C1—C3	−64.5 (3)	Nb—C1^i—C3^i—C1	64.8 (2)
Nb—C5—C6—C5^i	64.8 (2)	Nb—C1^i—C2^i—C2	−64.77 (8)
Nb—C5^i—C6^i—C5	−64.8 (2)	Nb—C1—C2—C2^i	64.77 (8)
Nb—C5—C4—C4^i	−65.0	C3—C1—C2—C2^i	0.3 (3)
Nb—C5^i—C4^i—C4	65.0	C3—C1^i—C2^i—C2	−0.3 (3)
Nb—C6—C5—C4	−64.0 (3)	C5—C6—C5^i—C4^i	−0.8 (5)
Nb—C6—C5^i—C4^i	64.0 (3)	C5—C4—C4^i—C5^i	0.0 (5)

Symmetry code: (i) x, −y+1/2, z.

bis(chlorodimethylsilyl)hydrido(bis)cyclopentadienyl niobium (ZEYVAA_HAR_SHADE3)

Crystal data

C14H23Cl2NbSi2	F(000) = 833.472
Mr = 411.32	Dx = 1.481 Mg m^−3
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
a = 16.584 (3) Å	Cell parameters from 24 reflections
b = 13.214 (3) Å	µ = 1.06 mm^−1
c = 8.419 (2) Å	T = 173 K
V = 1844.9 (7) Å^3	Block, pale beige
Z = 4	0.52 × 0.44 × 0.26 mm

Data collection

Enraf-Nonius CAD-4 diffractometer	Rint = 0.024
Absorption correction: psi scans	θmax = 30.0°, θmin = 2.5°
Tmin = 0.843, Tmax = 0.937	h = 0→23
2674 measured reflections	k = 0→18
2221 independent reflections	l = 0→9
2212 reflections with I ≥ 2u(I)

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.051	Only H-atom coordinates refined
wR(F^2) = 0.179	w = 1/[σ^2(Fo^2) + (0.1P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 1.74	(Δ/σ)max = 0.001
2221 reflections	Δρmax = 1.24 e Å^−3
127 parameters	Δρmin = −3.30 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Nb	0.17845 (2)	0.25	0.09930 (5)	0.0237 (2)
Si	0.11317 (6)	0.09474 (7)	0.23808 (12)	0.0233 (3)
Cl	0.15086 (7)	−0.05033 (7)	0.14528 (14)	0.0364 (3)
C3	0.2696 (3)	0.25	0.3191 (8)	0.0324 (11)
H3A	0.251 (5)	0.25	0.417 (8)	0.046047
C2	0.3149 (2)	0.1967 (4)	0.0777 (6)	0.0343 (9)
H2A	0.340 (4)	0.138 (7)	−0.028 (9)	0.060813
C5	0.1028 (3)	0.1632 (3)	−0.1002 (4)	0.0323 (8)
H5A	0.079 (5)	0.083 (5)	−0.101 (7)	0.046680
C6	0.0579 (3)	0.25	−0.0558 (7)	0.0313 (10)
H6A	0.008 (5)	0.25	−0.016 (10)	0.045990
C4	0.1751 (3)	0.1973 (4)	−0.1693 (6)	0.0414 (10)
H4A	0.227 (4)	0.152 (5)	−0.230 (7)	0.058553
C8	0.1345 (3)	0.0773 (3)	0.4562 (6)	0.0381 (9)
H8A	0.201 (4)	0.057 (6)	0.472 (9)	0.058630
H8B	0.100 (4)	0.006 (6)	0.511 (8)	0.066623
H8C	0.117 (4)	0.136 (5)	0.511 (7)	0.056990
C1	0.2873 (2)	0.1624 (3)	0.2263 (5)	0.0332 (8)
H1A	0.294 (4)	0.088 (4)	0.269 (8)	0.050080
C7	0.0006 (2)	0.0828 (3)	0.2218 (6)	0.0363 (9)
H7A	−0.018 (4)	0.072 (6)	0.095 (7)	0.056390
H7B	−0.017 (4)	0.125 (5)	0.257 (8)	0.055230
H7C	−0.016 (4)	0.011 (5)	0.302 (9)	0.061373
H	0.098 (5)	0.25	0.262 (9)	0.041670

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Nb	0.0205 (3)	0.0203 (3)	0.0302 (4)	−0.000000	−0.00136 (12)	0.000000
Si	0.0213 (4)	0.0190 (4)	0.0295 (6)	−0.0015 (3)	0.0000 (3)	0.0010 (3)
Cl	0.0424 (6)	0.0204 (4)	0.0465 (6)	0.0049 (3)	0.0006 (4)	−0.0015 (4)
C3	0.025 (2)	0.037 (3)	0.035 (3)	−0.000000	−0.003 (2)	0.000000
H3A	0.046760	0.046280	0.045100	−0.000000	−0.007590	0.000000
C2	0.0212 (16)	0.032 (2)	0.050 (3)	0.0048 (13)	0.0051 (14)	0.0003 (17)
H2A	0.049510	0.059830	0.073100	0.007470	0.021670	−0.007770
C5	0.042 (2)	0.0281 (17)	0.027 (2)	−0.0038 (16)	−0.0102 (14)	−0.0039 (13)
H5A	0.055710	0.033270	0.051060	−0.005280	−0.003220	−0.006460
C6	0.028 (2)	0.031 (2)	0.035 (3)	−0.000000	−0.008 (2)	0.000000
H6A	0.036400	0.041080	0.060490	−0.000000	−0.008230	0.000000
C4	0.040 (2)	0.046 (3)	0.039 (3)	0.0090 (17)	0.0010 (16)	−0.013 (2)
H4A	0.067070	0.055410	0.053180	0.001900	0.020260	−0.007040
C8	0.048 (2)	0.0339 (19)	0.032 (2)	−0.0012 (18)	−0.0037 (18)	0.0056 (17)
H8A	0.051310	0.064850	0.059730	0.007910	−0.013280	0.011300
H8B	0.085910	0.055150	0.058810	−0.020990	0.000180	0.019050
H8C	0.073830	0.051950	0.045190	0.010420	0.001220	−0.004390
C1	0.0245 (15)	0.0263 (16)	0.049 (2)	0.0048 (13)	−0.0098 (15)	0.0047 (15)
H1A	0.043420	0.039510	0.067310	0.010160	−0.003550	0.005020
C7	0.0242 (17)	0.0314 (18)	0.053 (3)	−0.0060 (14)	0.0036 (16)	−0.0063 (17)
H7A	0.046550	0.064410	0.058210	−0.011190	−0.012680	−0.004070
H7B	0.040150	0.049220	0.076320	−0.000000	0.008320	−0.015070
H7C	0.053590	0.047760	0.082770	−0.016760	0.006440	0.013280
H	0.035740	0.044370	0.044900	−0.000000	0.005560	0.000000

Geometric parameters (Å, º)

Nb—Si^i	2.5973 (10)	C3—C1	1.427 (5)
Nb—Si	2.5973 (10)	C2—C2^i	1.410 (10)
Nb—C3	2.390 (6)	C2—H2A	1.25 (8)
Nb—C2	2.377 (4)	C2—C1	1.406 (6)
Nb—C2^i	2.377 (4)	C5—H5A	1.13 (6)
Nb—C5	2.390 (4)	C5—C6	1.419 (5)
Nb—C5^i	2.390 (4)	C5—C4	1.406 (6)
Nb—C6	2.388 (5)	C6—H6A	0.89 (8)
Nb—C4^i	2.367 (5)	C4—C4^i	1.393 (11)
Nb—C4	2.367 (5)	C4—H4A	1.17 (6)
Nb—C1^i	2.396 (4)	C8—H8A	1.14 (7)
Nb—C1	2.396 (4)	C8—H8B	1.19 (7)
Nb—H	1.92 (8)	C8—H8C	0.95 (6)
Si—Cl	2.1624 (13)	C1—H1A	1.05 (6)
Si—C8	1.884 (5)	C7—H7A	1.13 (6)
Si—C7	1.878 (4)	C7—H7B	0.70 (6)
C3—H3A	0.88 (7)	C7—H7C	1.20 (7)
C3—C1^i	1.427 (5)
Si^i—Nb—Si	104.35 (4)	C1^i—Nb—C1	57.75 (18)
C3—Nb—Si	85.15 (9)	H—Nb—Si^i	52.19 (5)
C3—Nb—Si^i	85.15 (9)	H—Nb—Si	52.19 (5)
C2—Nb—Si	101.35 (12)	H—Nb—C3	84 (2)
C2^i—Nb—Si^i	101.35 (12)	H—Nb—C2	136 (2)
C2^i—Nb—Si	131.71 (12)	H—Nb—C2^i	136 (2)
C2—Nb—Si^i	131.71 (12)	H—Nb—C5	98 (2)
C2—Nb—C3	57.09 (19)	H—Nb—C5^i	98 (2)
C2^i—Nb—C3	57.09 (19)	H—Nb—C6	79 (2)
C2^i—Nb—C2	34.5 (2)	H—Nb—C4^i	132 (2)
C5—Nb—Si	73.63 (10)	H—Nb—C4	132 (2)
C5^i—Nb—Si	118.48 (11)	H—Nb—C1^i	102 (2)
C5^i—Nb—Si^i	73.63 (10)	H—Nb—C1	102 (2)
C5—Nb—Si^i	118.48 (11)	Cl—Si—Nb	114.66 (5)
C5—Nb—C3	151.20 (10)	C8—Si—Nb	117.15 (14)
C5^i—Nb—C3	151.20 (10)	C8—Si—Cl	100.93 (15)
C5^i—Nb—C2^i	107.66 (16)	C7—Si—Nb	116.60 (15)
C5—Nb—C2	107.66 (16)	C7—Si—Cl	100.75 (15)
C5—Nb—C2^i	126.03 (17)	C7—Si—C8	104.3 (2)
C5^i—Nb—C2	126.03 (17)	H3A—C3—Nb	120 (5)
C5^i—Nb—C5	57.40 (19)	C1—C3—Nb	72.9 (3)
C6—Nb—Si	84.09 (10)	C1^i—C3—Nb	72.9 (3)
C6—Nb—Si^i	84.09 (10)	C1—C3—H3A	125.8 (3)
C6—Nb—C3	162.4 (2)	C1^i—C3—H3A	125.8 (3)
C6—Nb—C2	139.05 (19)	C1^i—C3—C1	108.4 (6)
C6—Nb—C2^i	139.05 (19)	C2^i—C2—Nb	72.75 (11)
C6—Nb—C5	34.54 (13)	H2A—C2—Nb	124 (3)
C6—Nb—C5^i	34.54 (13)	C1—C2—Nb	73.6 (2)
C4^i—Nb—Si^i	100.81 (14)	C1—C2—H2A	123 (4)
C4^i—Nb—Si	130.72 (12)	H5A—C5—Nb	129 (3)
C4—Nb—Si^i	130.72 (12)	C6—C5—Nb	72.7 (3)
C4—Nb—Si	100.81 (14)	C6—C5—H5A	125 (4)
C4—Nb—C3	139.01 (17)	C4—C5—Nb	71.9 (3)
C4^i—Nb—C3	139.01 (17)	C4—C5—H5A	126 (4)
C4—Nb—C2^i	92.11 (17)	C4—C5—C6	107.3 (4)
C4^i—Nb—C2^i	82.09 (16)	C5^i—C6—Nb	72.8 (3)
C4^i—Nb—C2	92.11 (17)	C5—C6—Nb	72.8 (3)
C4—Nb—C2	82.09 (16)	C5^i—C6—C5	108.0 (5)
C4—Nb—C5^i	57.13 (15)	H6A—C6—Nb	125 (5)
C4^i—Nb—C5^i	34.38 (15)	H6A—C6—C5^i	125.9 (4)
C4—Nb—C5	34.38 (15)	H6A—C6—C5	125.9 (4)
C4^i—Nb—C5	57.13 (15)	C5—C4—Nb	73.7 (2)
C4—Nb—C6	57.16 (18)	C4^i—C4—Nb	72.9 (3)
C4^i—Nb—C6	57.16 (18)	C4^i—C4—C5	108.7 (3)
C4^i—Nb—C4	34.2 (3)	H4A—C4—Nb	123 (3)
C1^i—Nb—Si	119.65 (11)	H4A—C4—C5	130 (3)
C1—Nb—Si	74.45 (10)	H8A—C8—Si	109 (4)
C1^i—Nb—Si^i	74.45 (10)	H8B—C8—Si	113 (4)
C1—Nb—Si^i	119.65 (11)	H8B—C8—H8A	103 (5)
C1—Nb—C3	34.68 (12)	H8C—C8—Si	109 (4)
C1^i—Nb—C3	34.68 (12)	H8C—C8—H8A	115 (5)
C1^i—Nb—C2^i	34.27 (16)	H8C—C8—H8B	108 (5)
C1—Nb—C2^i	57.31 (15)	C3—C1—Nb	72.4 (3)
C1^i—Nb—C2	57.31 (15)	C2—C1—Nb	72.1 (2)
C1—Nb—C2	34.27 (16)	C2—C1—C3	107.0 (4)
C1^i—Nb—C5^i	118.50 (14)	H1A—C1—Nb	133 (3)
C1—Nb—C5^i	160.20 (16)	H1A—C1—C3	126 (4)
C1^i—Nb—C5	160.20 (16)	H1A—C1—C2	125 (4)
C1—Nb—C5	118.50 (14)	H7A—C7—Si	111 (4)
C1^i—Nb—C6	151.03 (9)	H7B—C7—Si	109 (5)
C1—Nb—C6	151.03 (9)	H7B—C7—H7A	113 (7)
C1—Nb—C4^i	125.89 (16)	H7C—C7—Si	105 (3)
C1^i—Nb—C4	125.89 (16)	H7C—C7—H7A	111 (5)
C1—Nb—C4	107.58 (15)	H7C—C7—H7B	107 (6)
C1^i—Nb—C4^i	107.58 (15)
Nb—C3—C1—C2	64.3 (3)	Nb—C4—C5—C6	64.5 (3)
Nb—C3—C1^i—C2^i	−64.3 (3)	Nb^i—C4—C5—C6	64.5 (3)
Nb—C2^i—C2—C1	−65.3 (3)	Nb—C4—C4^i—C5^i	−65.5 (3)
Nb—C2—C2^i—C1^i	65.3 (3)	Nb—C4^i—C4—C5	65.5 (3)
Nb—C2—C1—C3	−64.5 (3)	Nb—C1—C3—C1^i	−64.8 (2)
Nb^i—C2—C1—C3	−64.5 (3)	Nb—C1^i—C3^i—C1	64.8 (2)
Nb—C5—C6—C5^i	64.8 (2)	Nb—C1^i—C2^i—C2	−64.77 (8)
Nb—C5^i—C6^i—C5	−64.8 (2)	Nb—C1—C2—C2^i	64.77 (8)
Nb—C5—C4—C4^i	−65.0	C3—C1—C2—C2^i	0.3 (3)
Nb—C5^i—C4^i—C4	65.0	C3—C1^i—C2^i—C2	−0.3 (3)
Nb—C6—C5—C4	−64.0 (3)	C5—C6—C5^i—C4^i	−0.8 (5)
Nb—C6—C5^i—C4^i	64.0 (3)	C5—C4—C4^i—C5^i	0.0 (5)

Symmetry code: (i) x, −y+1/2, z.

bis(chlorodimethylsilyl)hydrido(bis)cyclopentadienyl niobium (ZEYVAA_IAM_0_HADPs)

Crystal data

C14H23Cl2NbSi2	F(000) = 833.697
Mr = 411.32	Dx = 1.481 Mg m^−3
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
a = 16.584 (3) Å	Cell parameters from 24 reflections
b = 13.214 (3) Å	µ = 1.06 mm^−1
c = 8.419 (2) Å	T = 173 K
V = 1844.9 (7) Å^3	Block, pale beige
Z = 4	0.52 × 0.44 × 0.26 mm

Data collection

Enraf-Nonius CAD-4 diffractometer	Rint = 0.024
Absorption correction: psi scans	θmax = 30.0°, θmin = 2.5°
Tmin = 0.843, Tmax = 0.937	h = 0→23
2674 measured reflections	k = 0→18
2221 independent reflections	l = 0→9
2212 reflections with I ≥ 2u(I)

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.046	Only H-atom coordinates refined
wR(F^2) = 0.131	w = 1/[σ^2(Fo^2) + (0.0613P)^2 + 13.3474P] where P = (Fo^2 + 2Fc^2)/3
S = 1.00	(Δ/σ)max = 0.001
2221 reflections	Δρmax = 1.24 e Å^−3
127 parameters	Δρmin = −2.69 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Nb	0.17845 (3)	0.25	0.09927 (6)	0.01974 (15)
Si	0.11308 (7)	0.09478 (8)	0.23806 (15)	0.0240 (2)
Cl	0.15085 (8)	−0.05036 (8)	0.14542 (16)	0.0374 (3)
C3	0.2694 (4)	0.25	0.3186 (9)	0.0326 (13)
H3	0.250 (3)	0.25	0.413 (7)	0.000000
C2	0.3148 (3)	0.1962 (4)	0.0780 (6)	0.0348 (10)
H2	0.332 (2)	0.150 (3)	−0.010 (4)	0.000000
C5	0.1024 (3)	0.1633 (4)	−0.0995 (5)	0.0337 (10)
H5	0.079 (2)	0.096 (3)	−0.098 (4)	0.000000
C6	0.0578 (4)	0.25	−0.0553 (8)	0.0316 (13)
H6	0.014 (3)	0.25	−0.014 (7)	0.000000
C4	0.1746 (3)	0.1968 (4)	−0.1693 (6)	0.0417 (12)
H4	0.219 (2)	0.155 (3)	−0.204 (4)	0.000000
C8	0.1346 (3)	0.0772 (4)	0.4550 (6)	0.0378 (10)
H8a	0.190 (2)	0.066 (3)	0.472 (4)	0.000000
H8b	0.099 (2)	0.019 (3)	0.496 (4)	0.000000
H8c	0.115 (2)	0.131 (3)	0.514 (4)	0.000000
C1	0.2875 (3)	0.1631 (4)	0.2264 (7)	0.0347 (10)
H1	0.285 (2)	0.093 (3)	0.259 (4)	0.000000
C7	0.0008 (3)	0.0830 (4)	0.2222 (7)	0.0356 (10)
H7a	−0.023 (2)	0.084 (3)	0.117 (5)	0.000000
H7b	−0.021 (2)	0.137 (3)	0.271 (5)	0.000000
H7c	−0.014 (2)	0.022 (3)	0.285 (4)	0.000000
H	0.107 (3)	0.25	0.273 (6)	0.000000

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Nb	0.0176 (2)	0.0175 (2)	0.0241 (3)	−0.000000	−0.00144 (18)	0.000000
Si	0.0229 (5)	0.0198 (5)	0.0292 (6)	−0.0014 (4)	0.0000 (4)	0.0009 (4)
Cl	0.0444 (6)	0.0222 (4)	0.0456 (7)	0.0051 (4)	0.0001 (5)	−0.0016 (4)
C3	0.024 (3)	0.040 (3)	0.034 (4)	−0.000000	0.000 (2)	0.000000
H3	0.000000	0.000000	0.000000	−0.000000	0.000000	0.000000
C2	0.0205 (18)	0.034 (2)	0.050 (3)	0.0043 (16)	0.0029 (18)	−0.002 (2)
H2	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C5	0.045 (3)	0.030 (2)	0.026 (2)	−0.0035 (19)	−0.0114 (19)	−0.0021 (17)
H5	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C6	0.028 (3)	0.036 (3)	0.031 (3)	−0.000000	−0.006 (3)	0.000000
H6	0.000000	0.000000	0.000000	−0.000000	0.000000	0.000000
C4	0.043 (3)	0.050 (3)	0.032 (3)	0.009 (2)	−0.002 (2)	−0.014 (2)
H4	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C8	0.046 (3)	0.037 (2)	0.031 (3)	0.002 (2)	0.004 (2)	0.006 (2)
H8a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H8b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H8c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C1	0.0238 (19)	0.030 (2)	0.051 (3)	0.0042 (16)	−0.0105 (19)	0.006 (2)
H1	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
C7	0.0250 (19)	0.034 (2)	0.048 (3)	−0.0073 (17)	0.002 (2)	−0.003 (2)
H7a	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H7b	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H7c	0.000000	0.000000	0.000000	0.000000	0.000000	0.000000
H	0.000000	0.000000	0.000000	−0.000000	0.000000	0.000000

Geometric parameters (Å, º)

Nb—Si^i	2.5976 (12)	C3—C1	1.419 (7)
Nb—Si	2.5976 (12)	C2—C2^i	1.423 (10)
Nb—C3	2.384 (7)	C2—H2	1.00 (4)
Nb—C2	2.378 (4)	C2—C1	1.399 (7)
Nb—C2^i	2.378 (4)	C5—H5	0.97 (4)
Nb—C5	2.388 (4)	C5—C6	1.414 (6)
Nb—C5^i	2.388 (4)	C5—C4	1.406 (7)
Nb—C6	2.387 (7)	C6—H6	0.81 (6)
Nb—C4	2.369 (5)	C4—C4^i	1.406 (12)
Nb—C4^i	2.369 (5)	C4—H4	0.97 (4)
Nb—C1^i	2.395 (4)	C8—H8a	0.94 (4)
Nb—C1	2.395 (4)	C8—H8b	1.03 (4)
Nb—H	1.89 (5)	C8—H8c	0.93 (4)
Si—Cl	2.1631 (16)	C1—H1	0.96 (4)
Si—C8	1.875 (5)	C7—H7a	0.97 (4)
Si—C7	1.874 (5)	C7—H7b	0.90 (4)
C3—H3	0.86 (6)	C7—H7c	0.99 (4)
C3—C1^i	1.419 (7)
Si^i—Nb—Si	104.29 (5)	C1^i—Nb—C1	57.3 (2)
C3—Nb—Si	85.16 (11)	H—Nb—Si^i	52.25 (9)
C3—Nb—Si^i	85.16 (11)	H—Nb—Si	52.25 (9)
C2—Nb—Si	101.23 (12)	H—Nb—C3	78.2 (16)
C2^i—Nb—Si^i	101.23 (12)	H—Nb—C2	131.1 (15)
C2^i—Nb—Si	131.85 (13)	H—Nb—C2^i	131.1 (15)
C2—Nb—Si^i	131.85 (13)	H—Nb—C5	102.2 (14)
C2—Nb—C3	57.1 (2)	H—Nb—C5^i	102.2 (14)
C2^i—Nb—C3	57.1 (2)	H—Nb—C6	84.0 (16)
C2^i—Nb—C2	34.8 (2)	H—Nb—C4^i	136.5 (15)
C5—Nb—Si	73.49 (12)	H—Nb—C4	136.5 (15)
C5^i—Nb—Si	118.28 (13)	H—Nb—C1^i	97.4 (14)
C5^i—Nb—Si^i	73.49 (12)	H—Nb—C1	97.4 (14)
C5—Nb—Si^i	118.28 (13)	Cl—Si—Nb	114.65 (6)
C5—Nb—C3	151.24 (12)	C8—Si—Nb	117.15 (17)
C5^i—Nb—C3	151.24 (12)	C8—Si—Cl	100.73 (18)
C5^i—Nb—C2^i	107.81 (18)	C7—Si—Nb	116.62 (17)
C5—Nb—C2	107.81 (18)	C7—Si—Cl	100.88 (17)
C5—Nb—C2^i	126.37 (19)	C7—Si—C8	104.4 (3)
C5^i—Nb—C2	126.37 (19)	H3—C3—Nb	119 (4)
C5^i—Nb—C5	57.4 (2)	C1—C3—Nb	73.2 (3)
C6—Nb—Si	84.00 (11)	C1^i—C3—Nb	73.2 (3)
C6—Nb—Si^i	84.00 (11)	C1—C3—H3	125.9 (3)
C6—Nb—C3	162.3 (2)	C1^i—C3—H3	125.9 (3)
C6—Nb—C2	139.1 (2)	C1^i—C3—C1	108.1 (6)
C6—Nb—C2^i	139.1 (2)	C2^i—C2—Nb	72.59 (12)
C6—Nb—C5	34.45 (15)	H2—C2—Nb	120 (2)
C6—Nb—C5^i	34.45 (15)	C1—C2—Nb	73.6 (2)
C4^i—Nb—Si^i	100.59 (15)	C1—C2—H2	124 (2)
C4^i—Nb—Si	130.73 (14)	H5—C5—Nb	130 (2)
C4—Nb—Si^i	130.73 (14)	C6—C5—Nb	72.7 (3)
C4—Nb—Si	100.59 (15)	C6—C5—H5	122 (2)
C4—Nb—C3	139.1 (2)	C4—C5—Nb	72.0 (3)
C4^i—Nb—C3	139.1 (2)	C4—C5—H5	130 (2)
C4—Nb—C2^i	92.43 (19)	C4—C5—C6	107.5 (5)
C4^i—Nb—C2^i	82.23 (19)	C5^i—C6—Nb	72.8 (3)
C4^i—Nb—C2	92.43 (19)	C5—C6—Nb	72.8 (3)
C4—Nb—C2	82.23 (19)	C5^i—C6—C5	108.3 (6)
C4—Nb—C5^i	57.28 (18)	H6—C6—Nb	121 (4)
C4^i—Nb—C5^i	34.37 (18)	H6—C6—C5^i	125.8 (3)
C4—Nb—C5	34.37 (18)	H6—C6—C5	125.8 (3)
C4^i—Nb—C5	57.28 (18)	C5—C4—Nb	73.6 (3)
C4—Nb—C6	57.1 (2)	C4^i—C4—Nb	72.73 (11)
C4^i—Nb—C6	57.1 (2)	C4^i—C4—C5	108.4 (3)
C4^i—Nb—C4	34.5 (3)	H4—C4—Nb	116 (2)
C1^i—Nb—Si	119.53 (13)	H4—C4—C5	127 (2)
C1—Nb—Si	74.67 (12)	H8a—C8—Si	111 (2)
C1^i—Nb—Si^i	74.67 (12)	H8b—C8—Si	108 (2)
C1—Nb—Si^i	119.53 (13)	H8b—C8—H8a	114 (3)
C1—Nb—C3	34.54 (15)	H8c—C8—Si	111 (2)
C1^i—Nb—C3	34.54 (15)	H8c—C8—H8a	112 (3)
C1^i—Nb—C2^i	34.08 (18)	H8c—C8—H8b	101 (3)
C1—Nb—C2^i	57.23 (17)	C3—C1—Nb	72.3 (3)
C1^i—Nb—C2	57.23 (17)	C2—C1—Nb	72.3 (3)
C1—Nb—C2	34.08 (18)	C2—C1—C3	107.7 (4)
C1^i—Nb—C5^i	118.79 (17)	H1—C1—Nb	123 (2)
C1—Nb—C5^i	160.38 (19)	H1—C1—C3	128 (2)
C1^i—Nb—C5	160.38 (19)	H1—C1—C2	125 (2)
C1—Nb—C5	118.79 (17)	H7a—C7—Si	118 (2)
C1^i—Nb—C6	151.25 (12)	H7b—C7—Si	108 (2)
C1—Nb—C6	151.25 (12)	H7b—C7—H7a	104 (3)
C1—Nb—C4^i	126.1 (2)	H7c—C7—Si	106 (2)
C1^i—Nb—C4	126.1 (2)	H7c—C7—H7a	114 (3)
C1—Nb—C4	107.72 (19)	H7c—C7—H7b	107 (3)
C1^i—Nb—C4^i	107.72 (19)
Nb—C3—C1—C2	64.1 (3)	Nb—C4—C5—C6	64.6 (4)
Nb—C3—C1^i—C2^i	−64.1 (3)	Nb^i—C4—C5—C6	64.6 (4)
Nb—C2^i—C2—C1	−65.6 (3)	Nb—C4—C4^i—C5^i	−65.5 (4)
Nb—C2—C2^i—C1^i	65.6 (3)	Nb—C4^i—C4—C5	65.5 (4)
Nb—C2—C1—C3	−64.1 (3)	Nb—C1—C3—C1^i	−65.3 (3)
Nb^i—C2—C1—C3	−64.1 (3)	Nb—C1^i—C3^i—C1	65.3 (3)
Nb—C5—C6—C5^i	64.7 (3)	Nb—C1^i—C2^i—C2	−64.86 (12)
Nb—C5^i—C6^i—C5	−64.7 (3)	Nb—C1—C2—C2^i	64.86 (12)
Nb—C5—C4—C4^i	−64.92 (11)	C3—C1—C2—C2^i	0.8 (4)
Nb—C5^i—C4^i—C4	64.92 (11)	C3—C1^i—C2^i—C2	−0.8 (4)
Nb—C6—C5—C4	−64.1 (3)	C5—C6—C5^i—C4^i	−0.6 (5)
Nb—C6—C5^i—C4^i	64.1 (3)	C5—C4—C4^i—C5^i	0.0 (6)

Symmetry code: (i) x, −y+1/2, z.

(ZEYVAA_IAM_NoMoRe)

Crystal data

C14H23Cl2NbSi2	F(000) = 833.537
Mr = 411.32	Dx = 1.481 Mg m^−3
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
a = 16.584 (3) Å	Cell parameters from 24 reflections
b = 13.214 (3) Å	µ = 1.06 mm^−1
c = 8.419 (2) Å	T = 173 K
V = 1844.9 (7) Å^3	Block, pale beige
Z = 4	0.52 × 0.44 × 0.26 mm

Data collection

Enraf-Nonius CAD-4 diffractometer	Rint = 0.024
Absorption correction: psi scans	θmax = 30.0°, θmin = 2.5°
Tmin = 0.843, Tmax = 0.937	h = 0→23
2674 measured reflections	k = 0→18
2221 independent reflections	l = 0→9
2212 reflections with I ≥ 2u(I)

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.042	Only H-atom coordinates refined
wR(F^2) = 0.126	w = 1/[σ^2(Fo^2) + (0.0613P)^2 + 12.0566P] where P = (Fo^2 + 2Fc^2)/3
S = 0.99	(Δ/σ)max = 0.001
2221 reflections	Δρmax = 1.23 e Å^−3
127 parameters	Δρmin = −2.80 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Nb	0.17844 (3)	0.25	0.09926 (6)	0.01994 (14)
Si	0.11307 (7)	0.09480 (8)	0.23812 (14)	0.0242 (2)
Cl	0.15086 (7)	−0.05034 (8)	0.14537 (15)	0.0376 (3)
C3	0.2695 (4)	0.25	0.3185 (9)	0.0337 (13)
H3A	0.251 (6)	0.25	0.417 (11)	0.057000
C2	0.3149 (2)	0.1961 (4)	0.0779 (6)	0.0355 (10)
H2A	0.332 (4)	0.150 (5)	−0.011 (8)	0.057333
C5	0.1023 (3)	0.1632 (3)	−0.0994 (5)	0.0336 (9)
H5A	0.086 (5)	0.098 (5)	−0.097 (8)	0.064333
C6	0.0578 (4)	0.25	−0.0551 (8)	0.0317 (12)
H6A	0.010 (5)	0.25	−0.014 (11)	0.054667
C4	0.1748 (3)	0.1968 (4)	−0.1692 (6)	0.0417 (11)
H4A	0.219 (4)	0.155 (6)	−0.209 (8)	0.073333
C8	0.1346 (3)	0.0773 (4)	0.4555 (6)	0.0383 (10)
H8A	0.190 (4)	0.065 (6)	0.479 (8)	0.070333
H8B	0.102 (4)	0.018 (5)	0.497 (8)	0.063333
H8C	0.111 (5)	0.134 (5)	0.510 (8)	0.073000
C1	0.2874 (2)	0.1630 (3)	0.2270 (6)	0.0347 (10)
H1A	0.283 (4)	0.093 (5)	0.263 (8)	0.057000
C7	0.0008 (3)	0.0831 (4)	0.2228 (7)	0.0366 (10)
H7A	−0.020 (4)	0.081 (6)	0.117 (8)	0.064000
H7B	−0.021 (4)	0.138 (5)	0.276 (10)	0.071667
H7C	−0.016 (4)	0.023 (5)	0.278 (8)	0.061667
H	0.106 (5)	0.25	0.261 (10)	0.039667

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Nb	0.0178 (2)	0.0177 (2)	0.0244 (3)	−0.000000	−0.00146 (17)	0.000000
Si	0.0231 (5)	0.0201 (4)	0.0294 (6)	−0.0015 (4)	0.0000 (4)	0.0009 (4)
Cl	0.0445 (6)	0.0223 (4)	0.0460 (7)	0.0050 (4)	0.0002 (5)	−0.0016 (4)
C3	0.023 (3)	0.040 (3)	0.037 (4)	−0.000000	−0.002 (2)	0.000000
H3A	0.050000	0.079000	0.042000	−0.000000	−0.008000	0.000000
C2	0.0202 (17)	0.035 (2)	0.052 (3)	0.0040 (15)	0.0026 (17)	−0.001 (2)
H2A	0.047000	0.056000	0.069000	0.012000	0.011000	−0.015000
C5	0.044 (2)	0.0303 (19)	0.026 (2)	−0.0034 (18)	−0.0110 (18)	−0.0025 (16)
H5A	0.088000	0.038000	0.067000	−0.016000	−0.018000	−0.010000
C6	0.030 (3)	0.034 (3)	0.031 (3)	−0.000000	−0.007 (2)	0.000000
H6A	0.032000	0.079000	0.053000	−0.000000	−0.001000	0.000000
C4	0.044 (3)	0.049 (3)	0.032 (3)	0.008 (2)	−0.002 (2)	−0.014 (2)
H4A	0.065000	0.097000	0.058000	0.027000	0.004000	−0.028000
C8	0.047 (3)	0.037 (2)	0.031 (2)	0.001 (2)	0.002 (2)	0.0069 (19)
H8A	0.055000	0.096000	0.060000	−0.005000	−0.015000	0.022000
H8B	0.075000	0.055000	0.060000	−0.011000	0.008000	0.021000
H8C	0.117000	0.056000	0.046000	0.012000	−0.002000	−0.006000
C1	0.0230 (18)	0.0307 (19)	0.050 (3)	0.0044 (15)	−0.0105 (18)	0.0049 (19)
H1A	0.049000	0.040000	0.082000	0.010000	−0.006000	0.018000
C7	0.0247 (18)	0.035 (2)	0.050 (3)	−0.0083 (17)	0.0011 (19)	−0.002 (2)
H7A	0.047000	0.076000	0.069000	−0.019000	−0.017000	0.011000
H7B	0.040000	0.060000	0.115000	−0.001000	0.017000	−0.024000
H7C	0.057000	0.056000	0.072000	−0.026000	0.005000	0.010000
H	0.035000	0.042000	0.042000	−0.000000	0.005000	0.000000

Geometric parameters (Å, º)

Nb—Si^i	2.5977 (12)	C3—C1	1.415 (6)
Nb—Si	2.5977 (12)	C2—C2^i	1.424 (9)
Nb—C3	2.385 (7)	C2—H2A	1.00 (6)
Nb—C2	2.379 (4)	C2—C1	1.406 (7)
Nb—C2^i	2.379 (4)	C5—H5A	0.91 (6)
Nb—C5	2.389 (4)	C5—C6	1.413 (6)
Nb—C5^i	2.389 (4)	C5—C4	1.409 (7)
Nb—C6	2.385 (6)	C6—H6A	0.86 (9)
Nb—C4	2.367 (5)	C4—C4^i	1.406 (11)
Nb—C4^i	2.367 (5)	C4—H4A	0.98 (6)
Nb—C1^i	2.396 (4)	C8—H8A	0.95 (7)
Nb—C1	2.396 (4)	C8—H8B	1.02 (7)
Nb—H	1.82 (8)	C8—H8C	0.96 (7)
Si—Cl	2.1635 (15)	C1—H1A	0.98 (6)
Si—C8	1.879 (5)	C7—H7A	0.95 (7)
Si—C7	1.872 (5)	C7—H7B	0.93 (7)
C3—H3A	0.89 (9)	C7—H7C	0.97 (6)
C3—C1^i	1.415 (6)
Si^i—Nb—Si	104.27 (5)	C1^i—Nb—C1	57.3 (2)
C3—Nb—Si	85.17 (10)	H—Nb—Si^i	52.15 (5)
C3—Nb—Si^i	85.17 (10)	H—Nb—Si	52.15 (5)
C2—Nb—Si	101.23 (12)	H—Nb—C3	81 (3)
C2^i—Nb—Si^i	101.23 (12)	H—Nb—C2	134 (2)
C2^i—Nb—Si	131.86 (12)	H—Nb—C2^i	134 (2)
C2—Nb—Si^i	131.86 (12)	H—Nb—C5	100 (2)
C2—Nb—C3	57.1 (2)	H—Nb—C5^i	100 (2)
C2^i—Nb—C3	57.1 (2)	H—Nb—C6	81 (3)
C2^i—Nb—C2	34.8 (2)	H—Nb—C4^i	134 (2)
C5—Nb—Si	73.47 (12)	H—Nb—C4	134 (2)
C5^i—Nb—Si	118.25 (12)	H—Nb—C1^i	100 (2)
C5^i—Nb—Si^i	73.47 (12)	H—Nb—C1	100 (2)
C5—Nb—Si^i	118.25 (12)	Cl—Si—Nb	114.62 (6)
C5—Nb—C3	151.24 (11)	C8—Si—Nb	117.13 (17)
C5^i—Nb—C3	151.24 (11)	C8—Si—Cl	100.79 (17)
C5^i—Nb—C2^i	107.83 (17)	C7—Si—Nb	116.67 (17)
C5—Nb—C2	107.83 (17)	C7—Si—Cl	100.96 (17)
C5—Nb—C2^i	126.40 (18)	C7—Si—C8	104.3 (2)
C5^i—Nb—C2	126.40 (18)	H3A—C3—Nb	120 (6)
C5^i—Nb—C5	57.4 (2)	C1—C3—Nb	73.2 (3)
C6—Nb—Si	83.99 (11)	C1^i—C3—Nb	73.2 (3)
C6—Nb—Si^i	83.99 (11)	C1—C3—H3A	125.7 (3)
C6—Nb—C3	162.3 (2)	C1^i—C3—H3A	125.7 (3)
C6—Nb—C2	139.1 (2)	C1^i—C3—C1	108.6 (6)
C6—Nb—C2^i	139.1 (2)	C2^i—C2—Nb	72.59 (11)
C6—Nb—C5	34.43 (14)	H2A—C2—Nb	120 (4)
C6—Nb—C5^i	34.43 (14)	C1—C2—Nb	73.5 (2)
C4^i—Nb—Si^i	100.63 (14)	C1—C2—H2A	125 (4)
C4^i—Nb—Si	130.78 (13)	H5A—C5—Nb	127 (4)
C4—Nb—Si^i	130.78 (13)	C6—C5—Nb	72.7 (3)
C4—Nb—Si	100.63 (14)	C6—C5—H5A	128 (5)
C4—Nb—C3	139.05 (19)	C4—C5—Nb	72.0 (3)
C4^i—Nb—C3	139.05 (19)	C4—C5—H5A	124 (5)
C4—Nb—C2^i	92.36 (19)	C4—C5—C6	107.4 (4)
C4^i—Nb—C2^i	82.15 (18)	C5^i—C6—Nb	72.9 (3)
C4^i—Nb—C2	92.36 (19)	C5—C6—Nb	72.9 (3)
C4—Nb—C2	82.15 (18)	C5^i—C6—C5	108.4 (6)
C4—Nb—C5^i	57.35 (17)	H6A—C6—Nb	123 (6)
C4^i—Nb—C5^i	34.46 (17)	H6A—C6—C5^i	125.7 (4)
C4—Nb—C5	34.46 (17)	H6A—C6—C5	125.7 (4)
C4^i—Nb—C5	57.35 (17)	C5—C4—Nb	73.6 (3)
C4—Nb—C6	57.2 (2)	C4^i—C4—Nb	72.73 (11)
C4^i—Nb—C6	57.2 (2)	C4^i—C4—C5	108.3 (3)
C4^i—Nb—C4	34.5 (3)	H4A—C4—Nb	118 (4)
C1^i—Nb—Si	119.43 (13)	H4A—C4—C5	127 (5)
C1—Nb—Si	74.57 (11)	H8A—C8—Si	114 (4)
C1^i—Nb—Si^i	74.57 (11)	H8B—C8—Si	109 (4)
C1—Nb—Si^i	119.43 (13)	H8B—C8—H8A	109 (6)
C1—Nb—C3	34.43 (14)	H8C—C8—Si	107 (4)
C1^i—Nb—C3	34.43 (14)	H8C—C8—H8A	115 (7)
C1^i—Nb—C2^i	34.24 (17)	H8C—C8—H8B	102 (5)
C1—Nb—C2^i	57.34 (16)	C3—C1—Nb	72.4 (3)
C1^i—Nb—C2	57.34 (16)	C2—C1—Nb	72.2 (2)
C1—Nb—C2	34.24 (17)	C2—C1—C3	107.6 (4)
C1^i—Nb—C5^i	118.86 (16)	H1A—C1—Nb	123 (4)
C1—Nb—C5^i	160.57 (18)	H1A—C1—C3	126 (4)
C1^i—Nb—C5	160.57 (18)	H1A—C1—C2	126 (4)
C1—Nb—C5	118.86 (16)	H7A—C7—Si	115 (4)
C1^i—Nb—C6	151.26 (11)	H7B—C7—Si	107 (4)
C1—Nb—C6	151.26 (11)	H7B—C7—H7A	109 (7)
C1—Nb—C4^i	126.18 (19)	H7C—C7—Si	108 (4)
C1^i—Nb—C4	126.18 (19)	H7C—C7—H7A	109 (6)
C1—Nb—C4	107.79 (18)	H7C—C7—H7B	108 (6)
C1^i—Nb—C4^i	107.79 (18)
Nb—C3—C1—C2	64.1 (3)	Nb—C4—C5—C6	64.5 (3)
Nb—C3—C1^i—C2^i	−64.1 (3)	Nb^i—C4—C5—C6	64.5 (3)
Nb—C2^i—C2—C1	−65.5 (3)	Nb—C4—C4^i—C5^i	−65.5 (4)
Nb—C2—C2^i—C1^i	65.5 (3)	Nb—C4^i—C4—C5	65.5 (4)
Nb—C2—C1—C3	−64.2 (3)	Nb—C1—C3—C1^i	−65.2 (2)
Nb^i—C2—C1—C3	−64.2 (3)	Nb—C1^i—C3^i—C1	65.2 (2)
Nb—C5—C6—C5^i	64.7 (3)	Nb—C1^i—C2^i—C2	−64.85 (11)
Nb—C5^i—C6^i—C5	−64.7 (3)	Nb—C1—C2—C2^i	64.85 (11)
Nb—C5—C4—C4^i	−64.93 (10)	C3—C1—C2—C2^i	0.7 (4)
Nb—C5^i—C4^i—C4	64.93 (10)	C3—C1^i—C2^i—C2	−0.7 (4)
Nb—C6—C5—C4	−64.0 (3)	C5—C6—C5^i—C4^i	−0.7 (5)
Nb—C6—C5^i—C4^i	64.0 (3)	C5—C4—C4^i—C5^i	0.0 (6)

Symmetry code: (i) x, −y+1/2, z.

bis(chlorodimethylsilyl)hydrido(bis)cyclopentadienyl niobium (ZEYVAA_IAM_SHADE3)

Crystal data

C14H23Cl2NbSi2	F(000) = 833.472
Mr = 411.32	Dx = 1.481 Mg m^−3
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
a = 16.584 (3) Å	Cell parameters from 24 reflections
b = 13.214 (3) Å	µ = 1.06 mm^−1
c = 8.419 (2) Å	T = 173 K
V = 1844.9 (7) Å^3	Block, pale beige
Z = 4	0.52 × 0.44 × 0.26 mm

Data collection

Enraf-Nonius CAD-4 diffractometer	Rint = 0.024
Absorption correction: psi scans	θmax = 30.0°, θmin = 2.5°
Tmin = 0.843, Tmax = 0.937	h = 0→23
2674 measured reflections	k = 0→18
2221 independent reflections	l = 0→9
2212 reflections with I ≥ 2u(I)

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	0 constraints
R[F^2 > 2σ(F^2)] = 0.043	Only H-atom coordinates refined
wR(F^2) = 0.126	w = 1/[σ^2(Fo^2) + (0.0542P)^2 + 15.6655P] where P = (Fo^2 + 2Fc^2)/3
S = 0.98	(Δ/σ)max = 0.001
2221 reflections	Δρmax = 1.33 e Å^−3
115 parameters	Δρmin = −2.92 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Nb	0.178440	0.250000	0.099260	0.02234 (15)
Si	0.11307 (7)	0.09481 (8)	0.23813 (15)	0.0217 (2)
Cl	0.15084 (8)	−0.05034 (8)	0.14543 (16)	0.0349 (3)
C3	0.269500	0.250000	0.318500	0.0312 (13)
H3A	0.250000	0.250000	0.413000	0.044970
C2	0.3149 (3)	0.1962 (4)	0.0780 (7)	0.0329 (10)
H2A	0.331 (4)	0.150 (6)	−0.011 (8)	0.056477
C5	0.1025 (3)	0.1635 (4)	−0.0994 (6)	0.0308 (9)
H5A	0.089 (4)	0.105 (5)	−0.098 (7)	0.045790
C6	0.057900	0.250000	−0.055400	0.0289 (13)
H6A	0.011000	0.250000	−0.014000	0.045797
C4	0.1745 (3)	0.1968 (4)	−0.1689 (6)	0.0392 (12)
H4A	0.219 (4)	0.157 (5)	−0.206 (8)	0.055093
C8	0.1345 (4)	0.0774 (4)	0.4551 (6)	0.0357 (10)
H8A	0.185 (4)	0.065 (6)	0.479 (9)	0.058207
H8B	0.101 (5)	0.018 (6)	0.497 (9)	0.066400
H8C	0.112 (5)	0.133 (6)	0.510 (8)	0.057897
C1	0.2872 (3)	0.1630 (4)	0.2271 (6)	0.0321 (10)
H1A	0.286 (4)	0.097 (5)	0.257 (8)	0.047100
C7	0.0008 (3)	0.0832 (4)	0.2230 (7)	0.0336 (10)
H7A	−0.016 (4)	0.084 (6)	0.128 (9)	0.058297
H7B	−0.018 (4)	0.133 (5)	0.273 (10)	0.057417
H7C	−0.010 (4)	0.022 (5)	0.274 (10)	0.063100
H	0.106000	0.250000	0.258000	0.039583

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Nb	0.0201 (2)	0.0201 (2)	0.0269 (3)	−0.000000	−0.00143 (18)	0.000000
Si	0.0210 (5)	0.0179 (5)	0.0261 (6)	−0.0014 (4)	0.0000 (4)	0.0009 (4)
Cl	0.0420 (6)	0.0201 (4)	0.0425 (7)	0.0048 (4)	0.0002 (5)	−0.0015 (4)
C3	0.021 (3)	0.039 (3)	0.034 (4)	−0.000000	−0.001 (2)	0.000000
H3A	0.047690	0.046820	0.040400	−0.000000	−0.008490	0.000000
C2	0.0182 (18)	0.032 (2)	0.049 (3)	0.0044 (16)	0.0027 (18)	−0.002 (2)
H2A	0.047050	0.055640	0.066740	0.007800	0.019930	−0.006190
C5	0.042 (2)	0.027 (2)	0.023 (2)	−0.0039 (18)	−0.0107 (18)	−0.0022 (17)
H5A	0.055780	0.032840	0.048750	−0.005780	−0.005580	−0.006360
C6	0.028 (3)	0.031 (3)	0.028 (3)	−0.000000	−0.007 (2)	0.000000
H6A	0.035250	0.042300	0.059840	−0.000000	−0.009820	0.000000
C4	0.042 (3)	0.047 (3)	0.029 (3)	0.008 (2)	−0.003 (2)	−0.014 (2)
H4A	0.066850	0.051060	0.047370	0.003330	0.017540	−0.007000
C8	0.044 (3)	0.035 (2)	0.028 (3)	0.002 (2)	0.003 (2)	0.006 (2)
H8A	0.054450	0.065600	0.054570	0.007790	−0.011290	0.012770
H8B	0.086790	0.055040	0.057370	−0.020160	0.003130	0.020740
H8C	0.077530	0.053280	0.042880	0.010860	0.004130	−0.002190
C1	0.0213 (18)	0.028 (2)	0.047 (3)	0.0042 (16)	−0.0104 (18)	0.005 (2)
H1A	0.042860	0.037680	0.060760	0.010030	−0.003650	0.005770
C7	0.0232 (19)	0.032 (2)	0.045 (3)	−0.0080 (17)	0.0006 (19)	−0.002 (2)
H7A	0.045190	0.066570	0.063130	−0.013350	−0.012700	−0.002690
H7B	0.039230	0.052020	0.081000	−0.000850	0.010260	−0.013280
H7C	0.052530	0.048680	0.088090	−0.018360	0.006870	0.014630
H	0.034520	0.043560	0.040670	−0.000000	0.006060	0.000000

Geometric parameters (Å, º)

Nb—Si^i	2.5976 (12)	C3—C1	1.414 (5)
Nb—Si	2.5976 (12)	C2—C2^i	1.421 (10)
Nb—C3	2.3848 (4)	C2—H2A	1.00 (7)
Nb—C2	2.379 (4)	C2—C1	1.407 (7)
Nb—C2^i	2.379 (4)	C5—H5A	0.81 (6)
Nb—C5	2.386 (4)	C5—C6	1.411 (5)
Nb—C5^i	2.386 (4)	C5—C4	1.402 (8)
Nb—C6	2.3857 (4)	C6—H6A	0.8523 (1)
Nb—C4	2.366 (5)	C4—C4^i	1.406 (11)
Nb—C4^i	2.366 (5)	C4—H4A	0.96 (7)
Nb—C1^i	2.395 (4)	C8—H8A	0.88 (7)
Nb—C1	2.395 (4)	C8—H8B	1.02 (7)
Nb—H	1.7970 (3)	C8—H8C	0.94 (7)
Si—Cl	2.1634 (16)	C1—H1A	0.90 (6)
Si—C8	1.875 (5)	C7—H7A	0.85 (7)
Si—C7	1.872 (5)	C7—H7B	0.84 (7)
C3—H3A	0.8588 (2)	C7—H7C	0.93 (7)
C3—C1^i	1.414 (5)
Si^i—Nb—Si	104.27 (4)	C1^i—Nb—C1	57.4 (2)
C3—Nb—Si	85.18 (3)	H—Nb—Si^i	52.14 (3)
C3—Nb—Si^i	85.18 (3)	H—Nb—Si	52.14 (3)
C2—Nb—Si	101.25 (12)	H—Nb—C3	81.2
C2^i—Nb—Si^i	101.25 (12)	H—Nb—C2	133.79 (13)
C2^i—Nb—Si	131.82 (12)	H—Nb—C2^i	133.79 (13)
C2—Nb—Si^i	131.82 (12)	H—Nb—C5	99.69 (13)
C2—Nb—C3	57.03 (13)	H—Nb—C5^i	99.69 (13)
C2^i—Nb—C3	57.03 (13)	H—Nb—C6	81.1
C2^i—Nb—C2	34.8 (2)	H—Nb—C4^i	133.75 (14)
C5—Nb—Si	73.55 (12)	H—Nb—C4	133.75 (14)
C5^i—Nb—Si	118.25 (13)	H—Nb—C1^i	99.75 (13)
C5^i—Nb—Si^i	73.55 (12)	H—Nb—C1	99.75 (13)
C5—Nb—Si^i	118.25 (13)	Cl—Si—Nb	114.63 (6)
C5—Nb—C3	151.29 (12)	C8—Si—Nb	117.14 (18)
C5^i—Nb—C3	151.29 (12)	C8—Si—Cl	100.83 (18)
C5^i—Nb—C2^i	107.85 (18)	C7—Si—Nb	116.70 (18)
C5—Nb—C2	107.85 (18)	C7—Si—Cl	100.98 (18)
C5—Nb—C2^i	126.36 (19)	C7—Si—C8	104.2 (3)
C5^i—Nb—C2	126.36 (19)	H3A—C3—Nb	118.6
C5^i—Nb—C5	57.3 (2)	C1—C3—Nb	73.18 (18)
C6—Nb—Si	84.03 (3)	C1^i—C3—Nb	73.18 (18)
C6—Nb—Si^i	84.03 (3)	C1—C3—H3A	125.6 (2)
C6—Nb—C3	162.4	C1^i—C3—H3A	125.6 (2)
C6—Nb—C2	139.12 (13)	C1^i—C3—C1	108.7 (4)
C6—Nb—C2^i	139.12 (13)	C2^i—C2—Nb	72.62 (12)
C6—Nb—C5	34.39 (12)	H2A—C2—Nb	119 (4)
C6—Nb—C5^i	34.39 (12)	C1—C2—Nb	73.5 (2)
C4^i—Nb—Si^i	100.58 (15)	C1—C2—H2A	124 (4)
C4^i—Nb—Si	130.75 (14)	H5A—C5—Nb	127 (5)
C4—Nb—Si^i	130.75 (14)	C6—C5—Nb	72.80 (18)
C4—Nb—Si	100.58 (15)	C6—C5—H5A	129 (5)
C4—Nb—C3	139.11 (13)	C4—C5—Nb	72.1 (3)
C4^i—Nb—C3	139.11 (13)	C4—C5—H5A	123 (5)
C4—Nb—C2^i	92.46 (19)	C4—C5—C6	107.6 (4)
C4^i—Nb—C2^i	82.26 (19)	C5^i—C6—Nb	72.81 (18)
C4^i—Nb—C2	92.46 (19)	C5—C6—Nb	72.81 (18)
C4—Nb—C2	82.26 (19)	C5^i—C6—C5	108.3 (4)
C4—Nb—C5^i	57.24 (18)	H6A—C6—Nb	122.8
C4^i—Nb—C5^i	34.32 (18)	H6A—C6—C5^i	125.8 (2)
C4—Nb—C5	34.32 (18)	H6A—C6—C5	125.8 (2)
C4^i—Nb—C5	57.24 (18)	C5—C4—Nb	73.6 (3)
C4—Nb—C6	57.06 (13)	C4^i—C4—Nb	72.71 (13)
C4^i—Nb—C6	57.06 (13)	C4^i—C4—C5	108.3 (3)
C4^i—Nb—C4	34.6 (3)	H4A—C4—Nb	117 (4)
C1^i—Nb—Si	119.41 (13)	H4A—C4—C5	128 (4)
C1—Nb—Si	74.53 (12)	H8A—C8—Si	115 (5)
C1^i—Nb—Si^i	74.53 (12)	H8B—C8—Si	109 (4)
C1—Nb—Si^i	119.41 (13)	H8B—C8—H8A	107 (6)
C1—Nb—C3	34.42 (13)	H8C—C8—Si	108 (4)
C1^i—Nb—C3	34.42 (13)	H8C—C8—H8A	114 (7)
C1^i—Nb—C2^i	34.28 (18)	H8C—C8—H8B	103 (6)
C1—Nb—C2^i	57.35 (17)	C3—C1—Nb	72.40 (17)
C1^i—Nb—C2	57.35 (17)	C2—C1—Nb	72.2 (3)
C1—Nb—C2	34.28 (18)	C2—C1—C3	107.4 (4)
C1^i—Nb—C5^i	118.89 (17)	H1A—C1—Nb	125 (4)
C1—Nb—C5^i	160.56 (18)	H1A—C1—C3	129 (4)
C1^i—Nb—C5	160.56 (18)	H1A—C1—C2	124 (4)
C1—Nb—C5	118.89 (17)	H7A—C7—Si	113 (5)
C1^i—Nb—C6	151.24 (12)	H7B—C7—Si	106 (5)
C1—Nb—C6	151.24 (12)	H7B—C7—H7A	110 (7)
C1—Nb—C4^i	126.3 (2)	H7C—C7—Si	103 (5)
C1^i—Nb—C4	126.3 (2)	H7C—C7—H7A	112 (7)
C1—Nb—C4	107.87 (19)	H7C—C7—H7B	112 (7)
C1^i—Nb—C4^i	107.87 (19)
Nb—C3—C1—C2	64.2 (3)	Nb—C4—C5—C6	64.6 (2)
Nb—C3—C1^i—C2^i	−64.2 (3)	Nb^i—C4—C5—C6	64.6 (2)
Nb—C2^i—C2—C1	−65.4 (3)	Nb—C4—C4^i—C5^i	−65.6 (4)
Nb—C2—C2^i—C1^i	65.4 (3)	Nb—C4^i—C4—C5	65.6 (4)
Nb—C2—C1—C3	−64.31 (19)	Nb—C1—C3—C1^i	−65.05 (14)
Nb^i—C2—C1—C3	−64.31 (19)	Nb—C1^i—C3^i—C1	65.05 (14)
Nb—C5—C6—C5^i	64.67 (12)	Nb—C1^i—C2^i—C2	−64.84 (10)
Nb—C5^i—C6^i—C5	−64.67 (12)	Nb—C1—C2—C2^i	64.84 (10)
Nb—C5—C4—C4^i	−64.95 (6)	C3—C1—C2—C2^i	0.5 (3)
Nb—C5^i—C4^i—C4	64.95 (6)	C3—C1^i—C2^i—C2	−0.5 (3)
Nb—C6—C5—C4	−64.1 (3)	C5—C6—C5^i—C4^i	−0.5 (2)
Nb—C6—C5^i—C4^i	64.1 (3)	C5—C4—C4^i—C5^i	0.0 (6)

Symmetry code: (i) x, −y+1/2, z.