Obtaining single crystals containing cationic porphyrins from aqueous solutions: a systematic approach including nano-crystallization, organic modifiers and gel crystallization

Obtaining high-quality single crystals containing charged molecules from aqueous solutions can sometimes be challenging. In this publication, we studied the crystallization of polycationic porphyrins. Crystals of three polycationic porphyrins, [5,10,15,20-tetrakis(1-methylpyridin-1-ium-4-yl)porphyrin, 5-(4-cyanophenyl)-10,15,20-tris(1-methylpyridin-1-ium-4-yl)porphyrin and 5-(4-carboxy­phenyl)-10,15,20-tris(1-methylpyridin-1-ium-4-yl)porphyrin], were obtained with different anions. We started initially with `nano-crystallization' screening in order to identify promising combinations of the cations with suitable anions, followed by optimizing the ratio of anions to cations. Both steps yielded crystals, leading to the determination of one porphyrin-containing crystal structure from each step. In the next step, five different organic solvents were trialled as additives in an aqueous hanging-drop crystallization setup, which led to the determination of three more crystal structures. It was shown that it was possible to improve the quality of the crystals without the organic additive being incorporated into the crystal structure. Finally, crystals of one porphyrin salt were obtained by gel crystallization. These crystals were higher quality than the crystal grown by vapour diffusion, leading to a high-quality and higher-resolution X-ray structure determination. This is the first porphyrin structure to be determined from a crystal grown by gel crystallizaton.

1. Introduction

Our group has developed an aqueous, extremely powerful high-throughput screening (HTS) method, called nano-crystallization, in order to efficiently identify combinations of an organic cation with various organic or inorganic anions that lead to the formation of crystals. The nano-crystallization method can be performed either as a vapour-diffusion technique (Nievergelt et al., 2018; Alvarez et al., 2020) or as an under-oil technique (Babor et al., 2019). As described in these publications, this method allows the crystallization behaviour of a cation with 96 different anion solutions, containing 77 different anions, to be tested simultaneously. The choice of the anions was based on good water solubility, known ability to form crystals [e.g. tetra­fluoro­borate (Kurz et al., 2005), tetra­phenyl­borate (Kuzelka et al., 2002; Medina-Molner et al., 2015) or hexa­fluoro­phosphate (Baumeister et al., 2002; Hernández-Valdés et al., 2020)], safety concerns (therefore azide and perchlorate were not chosen), commercial availability (at least the corresponding acid of the Brønsted bases should be commercially available) and different basicities (pK_b values). The vapour-diffusion variant of this method only needs 100–500 nl of the analyte stock solution per crystallization experiment, potentially yielding high-quality single crystals which can subsequently be analysed directly using a home microsource single-crystal X-ray diffractometer. The cation stock solutions are pipetted into the corresponding wells by a pipetting robot, saving valuable time for the scientist.

However, in some cases, the crystals that are obtained are too small, and optimization of the initial hits must be performed. In the current work, three methods (see Fig. 1) were employed to improve the quality and increase the size of the crystals that were initially obtained:

Figure 1 Optimization steps if the initial nano-crystallization screen does not yield a sufficiently large crystal of the required quality.

(1) reduction of the molar excess of the anion versus the cation,

(2) addition of organic neutral additives, or

(3) gel crystallization.

While the first and the second method were mentioned in individual cases in the supporting information of our original publication on nano-crystallization (Nievergelt et al., 2018), in the present work these methods are tested with a systematic approach.

The nano-crystallization method (Nievergelt et al., 2018; Babor et al., 2019; Alvarez et al., 2020; Rubbiani et al., 2020) employs a molar excess of the anion versus the cation to be crystallized. If crystals of sufficient quality result, this is a very efficient way of crystallizing a substance, because the stoichiometries of anion and cation do not need to be adjusted. On the other hand, lowering the excess amount of the anion might allow the crystal quality to be improved in a very simple way.

As an alternative way to improve the quality of the porphyrin crystals obtained in the HTS within the 96-well plates that are used for nano-crystallization, the addition of neutral organic co-solvents to the aqueous crystallization setup can be considered. Previous research has shown that organic additives can lead to improved X-ray diffraction and extend the diffraction limit. These advantages have been reported in particular for the crystallization of macromolecules like zeolites (Sun & Shen, 2012), DNA (Spingler et al., 2001; Rohner et al., 2016) and proteins (Luberacki et al., 2008; Gosavi et al., 2009; McPherson et al., 2011). The effect of intentionally included organic additives on the aqueous crystallization of inorganic salts has been studied (Paulaime et al., 2003; Nahi et al., 2021). The shape of urea crystals can be influenced by addition of the neutral molecule biuret to the aqueous crystallization solution (Salvalaglio et al., 2012). Most recently, the impact of 1 mol% of added amino acids was studied during the crystallization of α-glycine (Offiler et al., 2025). However, to the best of our knowledge, our work from 2018 (Nievergelt et al., 2018) remains one of the very few reports about improving the crystallization of small molecules from aqueous solution with the help of organic additives for the purpose of single-crystal structure analysis.

Gel crystallization is a method which can be used on almost every system with respect to solvents and analytes to be crystallized. Crystals obtained by gel crystallization can have improved properties, such as quality, size, shape and fewer defects, compared with those obtained using other techniques. Gel crystallization can be used with aqueous and non-aqueous solvents (Choquesillo-Lazarte & García-Ruiz, 2011) and done in either counter-diffusion (Artusio et al., 2021), vapour-diffusion (Choquesillo-Lazarte & García-Ruiz, 2011) or layering (Yaghi et al., 1997; Rizzato et al., 2016) mode. When the latter approach is used, the layering of different ion solutions becomes very simple, reducing mixing of solutions and saving time in the laboratory. Because virtually no solvent evaporation takes place, the sedimentation of ions is reduced to a minimum, which results in fewer impurities in the crystals (Henisch, 2005).

Porphyrins are a class of organic compounds characterized by their macrocyclic structure, composed of four pyrrole subunits linked by methine bridges to form a conjugated aromatic system. The growth of high-quality porphyrin crystals is crucial for obtaining structural information (Tsalu et al., 2015; Kingsbury & Senge, 2021) about the vast diversity of porphyrins, which are present in all living organisms, used as photosensitizers for collecting solar energy (Gu et al., 2022; Mehrzad Sajjadinezhad et al., 2024) and have clinical (Maharjan et al., 2022) as well as potential oncological applications (Lam et al., 2019; Xu et al., 2023; Donohoe et al., 2023; Gao et al., 2024). On the other hand, growing high-quality crystals of porphyrins with sufficient size is a challenge (Lee et al., 2008; Medforth et al., 2016). The tetracationic [5,10,15,20-tetrakis(1-methylpyridin-1-ium-4-yl)porphyrin]⁴⁺ ([TMPyP]⁴⁺), which is a powerful telomerase inhibitor (Wheelhouse et al., 1998), is being evaluated as an anti-bacterial photosensitizer (Malara et al., 2017) and damages DNA by singlet oxygen generation (Tada-Oikawa et al., 2009). Scheidt et al. (2015) have crystallized 5,10,15,20-tetrakis(1-methylpyridin-1-ium-4-yl)porphyrin 5,10,15,20-tetrakis(4-sulfonatophenyl)porphyrin with the help of a U-tube by counter-diffusion in polypropyl­ene glycol (PPG). These authors also mentioned that they were unable to crystallize their molecules of interest with the help of a gel. We have previously shown that the tricationic [5-(4-cyano­phenyl)-10,15,20-tris(1-methylpyridin-1-ium-4-yl)porphyrin]³⁺ ([TriMCNP]³⁺) is an efficient photodynamic therapy (PDT) photosensitizer upon irradiation with light of a wavelength greater than 600 nm (Antoni et al., 2015). Finally, tricationic [5-(4-carboxyphenyl)-10,15,20-tris(1-methylpyridin-1-ium-4-yl)­porphyrin]³⁺ ([TriMCOOP]³⁺) has been tested as a telomerase inhibitor (Shi et al., 2001) and used multiple times as a part of porphyrin conjugates (Mion et al., 2015; Spagnul et al., 2017; Tosto et al., 2024).

To the best of our knowledge, no porphyrins have been crystallized with the help of gel crystallization. Since the chosen cationic porphyrins, [TMPyP]Cl₄, [TriMCNP](NO₃)₃ and [TriMCOOP]Cl₃ (Fig. 2) are all soluble in water above the lower limit of concentration, which we previously found to be important (2 mg ml⁻¹; Nievergelt et al., 2018), `normal' aqueous crystallization was expected to be possible either as vapour diffusion or gel crystallization with either agarose (Moreno & Rosales-Hoz, 2017) or tetra­meth­oxy­silane (TMOS) (Kumar & Steed, 2014; Rizzato et al., 2016; Sumida et al., 2017; Sánchez-Vergara et al., 2017). Sometimes silicate gels are used for gel crystallization, which are prepared from sodium silicate (`water glass') followed by acidification (García-Ruiz et al., 1998). We decided not to use these silicate gels, as they intrinsically contain an additional salt and therefore might interfere with the intended anion exchange of the original nano-crystallization process.

Figure 2 The polycationic porphyrins studied.

2. Results and discussion

The three different techniques used to crystallize the tetracationic [TMPyP]⁴⁺ and the tricationic [TriMCNP]³⁺ and [TriMCOOP]³⁺ porphyrins (Fig. 2) were vapour diffusion with either sitting- or hanging-drop crystallization, and gel crystallization (Fig. 1). We started with the original nano-crystallization vapour-diffusion setup (Nievergelt et al., 2018), during which the cationic compound to be crystallized is screened against 96 different anion solutions simultaneously in a 96-well plate. These sitting-drop crystallizations, each requiring a volume of only 100–500 nl or even less of the porphyrin solution, are set up by a pipetting robot. With these small volumes, only 12–55 µl in total of the saturated porphyrin solution is required for setting up 96 different crystallization trials. As a result of these screenings, [5-(4-carb­oxy­phenyl)-10,15,20-tris(1-methylpyridin-1-ium-4-yl)porphyrin]³⁺ ([TriMCOOP]³⁺) yielded single crystals with benzene­sulfonate as the counter-anion, for which diffraction data could be measured directly on our home X-ray microsource diffractometer to the desired resolution of 0.78 Å. The [TriMCOOP]³⁺ cation crystallized together with three benzene­sulfonate anions (also abbreviated as besylate). This implies that the carb­oxy­lic acid group is protonated (uncharged) and indeed this assumption could be confirmed crystallographically (Supplementary Figure S7).

The tetracationic [5,10,15,20-tetrakis(1-methylpyridin-1-ium-4-yl)porphyrin]⁴⁺ ([TMPyP]⁴⁺) was found to form crystalline material with eight different anions (see Table S1). However, the size and quality of these crystals were found to be insufficient for X-ray single-crystal analysis. On the other hand, one suitable single crystal was found for [TriMCNP]³⁺ (Fig. 3), which showed some diffraction (see below). Previously, [TMPyP](p-tosyl­ate)₄ (Ford et al., 1987) and several [TMPyP]⁴⁺ salts of a calixarene (Di Costanzo et al., 2001; Gulino et al., 2006) have been crystallized with the help of the vapour-diffusion technique, which is also used for protein crystallization.

Figure 3 Image of one of the 96 high-throughput crystallization experiments in the crystal farm after 10 days. Shown is the crystallization using [TriMCNP](NO3)3 and 0.15 M sodium p-toluene­sulfonate. In the top-right corner, the scoring values of the MARCO and Sherlock auto-scoring models, respectively, of the ROCK MAKER software (Formulatrix, Dubai) are shown. The scale bar (top left) has a length of 100 µm.

Therefore, in order to improve the size and quality of the single crystals that were obtained, the ratios of anions to porphyrin cations were optimized, and after that the impact of neutral organic additives was investigated, both in EasyXtal 15-well plates (Fig. 1). Individual wells of these plates have a reservoir with a capacity of 500 µl. The wells are closed airtight to prevent evaporation of the solvents, which results in the crystallization drop to be finally located on the lower side of the closing cap as a hanging drop. With this setup, screening with different concentrations of anion solutions is easy, and efficient timewise. Furthermore, it is possible to include different organic solvents as additives, which can help to prevent unwanted crystallizations in the experiment that can be detrimental to the crystal size and quality obtained.

The eight anions found to crystallize with [TMPyP]⁴⁺, but resulting in too-small crystals, were tested at lower concentrations compared with those employed in the original sitting-drop experiments by using the hanging-drop method (see Table S1). The anion salt concentrations were lowered fivefold in steps of approximately 10% versus the original conditions, as inspired by the literature (McPherson & Cudney, 2014; Dinç et al., 2016). In this way, it was possible to crystallize [TMPyP]⁴⁺ as the naphthalene-2,6-disulfonate salt (see Figure S1) using a concentration of 0.076 M of naphthalene-2,6-disulfonate instead of 0.085 M in the original setup. The other seven anions were then used for crystallization trials via the hanging-drop method, with the incorporation of five different organic solvents as additives (see Table 1). The choice of these five additives was inspired by neutral organic solvents in the additive screen of Hampton Research (CA, USA) and additionally by previous cases that had been reported as successful. The experiments resulted in three more types of well-diffracting single crystals whose structures could be determined in publication quality. These were [TMPyP]⁴⁺ with either bromide having ethyl acetate as an additive, nitrate with methanol or naphthalene-1-sulfonate with dioxane (Figs. 4 and S2–S4). In the case of the [TMPyP]⁴⁺ tetrabromide crystal structure, it was shown with the help of the software Platon (Spek, 2023) that the refined model for the structure contains no voids. In other words, apart from the six clearly identified water molecules, the organic additive (ethyl acetate) could not be identified in the crystal structure. The [TMPyP]⁴⁺ cation has previously been crystallized as the iodide salt (Lourenço et al., 2011). However, the bromide salt described here, which is a hexahydrate crystallizing in the space group P1, is not isostructural with its iodide analogue, which was a tetrahydrate that crystallized in the monoclinic space group P2₁/n.

Table 1
Optimization of the aqueous crystallization of [TMPyP]⁴⁺ using organic additives

Organic additive	Final concentration in volume % of organic additive in reservoir solution	Previously reported by
1,4-Dioxane	5	Cudney et al., 1994; Rohner et al., 2016
Methanol	5	Luberacki et al., 2008
Aceto­nitrile	5	Gosavi et al., 2009
Ethyl acetate	5	Spingler et al., 2001; Rohner et al., 2016
Acetone	4	Nievergelt et al., 2018

Figure 4 Displacement-ellipsoid representation of the bromide salt of [TMPyP]^4+. Ellipsoids are drawn at 50% probability. All atoms in the asymmetric unit apart from two of the disordered hydrogen atoms inside the porphyrin ring are shown.

No diffraction-quality crystals of [TMPyP]⁴⁺ with either di­phenyl acetate, (+)-O,O′-di­benzoyl-D-tartrate or di­hydrogen phosphate as the anion were obtained, even after optimization of the anion-to-cation ratio and tests with organic additives. Finally, improvement of the crystallization of the p-toluene­sulfonate salt of [TMPyP]⁴⁺ was attempted by employing gel crystallization (see Section 3.5). The use of agarose as a gelling agent resulted in the formation of a non-crystalline compound, which was not further analysed. Additionally, gel crystallization using TMOS did not result in the formation of any crystals or other solid material (Table 2).

Table 2
Qualitative results of the gel crystallization of [TMPyP]⁴⁺ and [TriMCNP]³⁺ as their p-toluene­sulfonate salts

Cation and anion	0.5%(m/v) Agarose	9%(v/v) TMOS
[TMPyP]^4+ and p-toluene­sulfonate	Non-crystalline compound	No solid material at all
[TriMCNP]^3+ and p-toluene­sulfonate	Good quality, large crystals	No solid material at all

Comparing the crystallographic data for the crystals containing 5,10,15,20-tetrakis(1-methylpyridin-1-ium-4-yl)porphyrin ([TMPyP]⁴⁺) and different counter anions (Table S4), one can see that all crystallized in the triclinic space group P1. Additionally, all four crystal structures containing [TMPyP]⁴⁺ have an asymmetric unit containing one formula unit, although in the case of the nitrate and naphthalene-1-sulfonate salts there are two symmetry-independent halves of porphyrin cations, which are completed by the action of the inversion centre.

As already mentioned, crystallization of the tricationic 5-(4-cyanophenyl)-10,15,20-tris­(1-methylpyridin-1-ium-4-yl)­porphyrin [TriMCNP]³⁺ was also tested with the nano-crystallization screen (Nievergelt et al., 2018). Elongated needle-shaped crystals of [TriMCNP](p-tosyl­ate)₃·(H₂O)_8.75 (Fig. 3) were obtained with 0.15 M sodium p-toluene­sulfonate. These crystals, however, were quite small and only diffracted to a resolution of 1.05 Å (see Tables 2 and S5). Therefore, gel crystallization was employed in an attempt to improve the quality of diffraction. The crystallization experiments were conducted either using 0.5%(m/v) agarose (Gavira & García-Ruiz, 2002) or 9%(v/v) TMOS (Pasero et al., 2025) as a gelling agent. The limited material available did not allow the gellant concentration or the curing temperature to be varied systematically. As in the case of [TMPyP]⁴⁺, the gel crystallization using TMOS did not result in the formation of any [TriMCNP]³⁺-containing crystals or other solid material. In contrast, the agarose gel crystallization experiment yielded after several weeks good, large single crystals of the [TriMCNP]³⁺ p-toluene­sulfonate salt (Table 2, Fig. 5) with the same space group and very similar unit-cell dimensions as the crystals obtained by vapour diffusion (Table 3). These crystals were almost 13 times larger than those from the sitting-drop vapour diffusion crystallization and diffracted to a much better resolution (0.78 versus 1.05 Å). Consequently, a higher-quality crystal structure with lower R_int and R1 values was obtained by employing the agarose gel crystallization. The higher resolution also led to the clear elucidation of the positions of more disordered water molecules, although not all of them could be modelled in a satisfactory way [see Nittinger et al. (2015) for a related discussion about the water molecules in ultra-high-resolution protein structures]. As a consequence, the SQUEEZE procedure within Platon had to be used (Spek, 2015), thereby lowering the number of clearly identifiable water molecules despite the higher resolution. Both structures contain two formula units in the asymmetric unit. To the best of our knowledge, this is the first crystal structure of any compound containing the 5-phenyl-10,15,20-tris(pyridyl)­porphyrin core unit. It is interesting to note that porphyrins with 1-methylpyridin-1-ium-4-yl substituents at the meso positions apparently have a strong propensity to form crystalline materials with aryl sulfonates, as four out of the six structures reported here contain aryl sulfonates. Using the nano-crystallization technique results in an essentially unbiased testing of 77 diverse anions, out of which only six are aryl sulfonates (so only 7.8% of all tested anions). The crystal structures containing the [TMPyP]⁴⁺ cation with the four different anions correspond to a success rate of 5.2% with respect to the 77 anions that were used, while for both [TriMCNP]³⁺ and [TriMCOOP]³⁺ only one anion yielded usable crystals, corresponding to a success rate of 1.3%.

Table 3
Comparison of crystal data for [TriMCNP](p-toluene­sulfonate)₃·nH₂O obtained by vapour diffusion and gel crystallization

	[TriMCNP](p-tosyl­ate)3·(H2O)8.75 (vapour crystallization)	[TriMCNP](p-tosyl­ate)3·(H2O)7 (gel crystallization)
Space group	P21/c	P21/c
a (Å)	17.50074 (18)	17.54006 (8)
b (Å)	25.9751 (3)	25.99854 (12)
c (Å)	30.1002 (4)	30.05455 (13)
β (°)	100.4228 (12)	100.5017 (4)
Volume (Å^3)	13457.2 (3)	13475.78 (10)
Crystal size (mm)	0.44 × 0.034 × 0.03	0.267 × 0.153 × 0.142
θ range (°)	2.263 to 47.692	2.263 to 79.242
Reflections collected	99768	275353
Independent reflections	12390 (Rint = 0.0470)	28905 (Rint = 0.0389)
Reflections observed	10103	25118
Data/restraints/parameters	12390/13/1812	28905/215/1758
Final R factors [I> 2σ(I)]	R1 = 0.0777, wR2 = 0.2123	R1 = 0.0715, wR2 = 0.2108
R factors (all data)	R1 = 0.0929, wR2 = 0.2275	R1 = 0.0780, wR2 = 0.2183

Figure 5 Displacement-ellipsoid representation of the hydrated p-toluene­sulfonate salt of [TriMCNP]^3+ grown by gel crystallization. Ellipsoids are drawn at 50% probability. Only one porphyrin molecule out of two in the asymmetric unit and the corresponding three tosyl­ate anions are shown. All hydrogen atoms, the minor part of a disordered phenyl­ene ring and water molecules are omitted for clarity.

We used the availability of four crystal structures of [TMPyP]⁴⁺ with identical cationic porphyrin units and different anions to evaluate the influence of the anions and solvent molecules upon the in-plane and out-of-plane distortions of the porphyrins. For these calculations, we employed the normal-coordinate structural decomposition (NSD) method, which is readily available at the online server provided by the Senge group at https://www.sengegroup.eu/nsd (Kingsbury & Senge, 2021). The results of these calculations can be found in the supporting information. The in-plane distortions are small for all structures; the out-of-plane distortions are rather moderate for all structures, except for the striking case of the naphthalene-2,6-disulfonate salt (Fig. 6). As discussed in detail by Kingsbury and Senge, the causes of the porphyrin-ring distortion are mainly of an intrinsic nature, such as protonation or alkyl­ation of the inner nitro­gen atoms of the porphyrin ring, metal coordination or the degree of non-hydrogen-atom substitution at the peripheral positions. For the four structures under consideration here, all porphyrin rings are chemically identical, therefore only extrinsic packing effects can account for the remarkable out-of-plane distortion observed in case of the naphthalene-2,6-disulfonate salt. We explain this distortion by the steric impact of the dumbbell shape of the naphthalene-2,6-disulfonate anions, which lie above and, turned by 90°, below the mean porphyrin plane (Fig. 7). The bulky sulfonate groups at both ends of the anion push the parallel-aligned and trans-disposed pyrrole rings out of the plane.

Figure 6 Out-of-plane distortion of the four studied [TMPyP]^4+ salts calculated using the NSD server (Kingsbury & Senge, 2021). From top left to bottom right are shown: the bromide, nitrate (first molecule), naphthalene-1-sulfonate (first molecule) and the naphthalene-2,6-disulfonate salts. Complete data can be found in the supporting information.

Figure 7 Explanation of the extreme out-of-plane distortion of the cation in the [TMPyP]^4+ naphthalene-2,6-disulfonate salt. The meso substituents of the porphyrin, minor disordered parts and all solvent molecules have been omitted for clarity.

3. Materials and methods

3.1. Materials

[TMPyP]Cl₄ was bought from PorphyChem (Longvic, France). [TriMCNP](NO₃)₃ was synthesized as described in Antoni et al. (2015). [TriMCOOP]Cl₃ was a generous donation from PorphyChem. The 15-well plates that were used were from Qiagen (Zug, Switzerland, article number 55408554). The 8 ml glass screw-cap vials were bought from Huberlab (Aesch, Switzerland, product number 9.7611.50). The anion screen was purchased from Molecular Dimensions (Calibre Scientific, Los Angeles, CA, USA).

3.2. Crystallization using semi-automatic crystallization

The crystallization screening experiments were performed with the help of the Gryphon LCP nano-drop handler from Art Robbins Instruments in ARI Intelli-Plates 96-3 LVR. 100–500 nl of a stock solution of the to-be-crystallized cation were mixed with the same volume of the stock solutions of the salt of the counterion and equilibrated against 75 µl of the stock solution of the same counterion. Each cation was tested for crystallization in 96 wells, each well containing a different condition, and with 77 different anions in total. Owing to the high viscosity of some solutions, all pipetting was done with slow speed. Plates were incubated for 5–16 days at 20°C. The Rock Imager 1000 took a picture of each well with normal light (immediately after setting up the plate and then after 2, 5, 10 and 16 days) and cross-polarized light (Nievergelt et al., 2018). The porphyrin stock solutions used were saturated aqueous solutions.

3.3. Optimization of the crystallization of porphyrin cations using hanging-drop crystallization and varying the ratio of cation to anion

Using a 15-well plate, sodium salt solutions (500 µl) with the concentrations given in Table S1 were added into the reservoirs. On the inner side of the seal, a drop of a saturated aqueous [TMPyP]Cl₄ porphyrin solution (1.0 µl) was added using an Eppendorf pipette. A drop of the anion solution (1.0 µl) from the reservoir was added into the drop of the porphyrin solution. The seal was then carefully put onto the well, which was closed tightly to prevent evaporation of the liquids. The plate was then left undisturbed for crystal growth. For each anion, five different concentrations of anions with lower concentrations than those used in the original crystallizations described in Section 3.2 were employed in order to slow down the crystal growth (Table S1).

3.4. Optimization of the crystallization of porphyrin cations with organic neutral additives using hanging-drop crystallization

Into the reservoirs of a 15-well plate, a sodium salt solution (450 µl; in the case of ethyl acetate 475 µl) with the concentration listed in Table S2 was added. To this sodium salt solution, an aqueous solution of an organic additive (50 µl, or pure ethyl acetate 25 µl) was added, as listed in Table S3. The well solution in the reservoir was mixed. On the inner side of the seal a drop of a saturated aqueous [TMPyP]Cl₄ porphyrin solution (1.0 µl) was added using an Eppendorf pipette. A drop of the anion solution (1.0 µl) from the reservoir with the organic additive was added to the drop of the porphyrin solution. The seal was then carefully put onto the well, which was closed tightly to prevent evaporation of the liquids. The plate was then left undisturbed for crystal growth.

3.5. Preparation of porphyrin-cation-containing crystals using gel crystallization

In 1.5 ml vials for gas chromatography (GC), aqueous solutions of either [TriMCNP](NO₃)₃ (76.1 mg in 1.00 ml) or [TMPyP]Cl₄ (100 mg in 1.00 ml) were prepared. In a 50 ml glass beaker, Millipore water (20.0 ml) was added. Agarose (100 mg) was added to the water. The mixture was then stirred and heated to 85°C using a heating plate. In a 50 ml plastic centrifuge tube, water (2.00 ml) was added together with tetra­methyl orthosilicate (TMOS, 0.20 ml). This solution was stirred for 15 minutes. Either a [TriMCNP](NO₃)₃ (0.50 ml) or a [TMPyP]Cl₄ (0.50 ml) solution was carefully injected into the bottom of an 8 ml screw-cap test tube with a syringe. On top of the solution, either not-yet solidified TMOS (0.50 ml) or agarose gel (0.50 ml) solutions were layered using a syringe. The test tubes were then closed and the gel left to solidify overnight. After the gel had solidified, another layer of the corresponding freshly prepared gel solution (1.50 ml) was carefully layered on top of the first layer, to prevent mixing of the two layers. After the second gel layer had solidified, again overnight, a sodium p-toluene­sulfonate (0.15 M, 0.50 ml) solution was carefully layered on top of the first two layers using a syringe. The schematic setup is shown in Fig. 8.

Figure 8 Setup of the gel crystallization by counter-diffusion.

3.6. Calculation of the in-plane and out-of-plane distortions of the porphyrins

The atomic coordinates of each crystal structure in CIF format were read into Mercury (Macrae et al., 2020), all anions and water molecules were removed and the remaining atom list was saved as in the Protein Data Bank (.pdb) file format. In the case of the naphthalene-2,6-disulfonate salt, the meso substituents of the porphyrin had to be removed for the calculations. The .pdb files were read into the NSD server at https://www.sengegroup.eu/nsd (Kingsbury & Senge, 2021).

4. Conclusions

In this paper, we have described a systematic approach for obtaining high-quality crystals of salts of the polycationic, water soluble porphyrins [TMPyP]⁴⁺, [TriMCOOP]³⁺ and [TriMCNP]³⁺. Starting from the nano-crystallization anion screen, which yielded high-quality crystals of one compound for structure determination and other initial crystalline hits, the latter could be improved by manually optimizing the stoichiometric ratio between the anion and cation. Taking the best conditions from this optimization, three more publication-quality single-crystal structures of porphyrin salts were obtained using neutral organic additives. These additives helped to improve the crystallization without being incorporated into the crystal structures. As an additional method for challenging cases, gel crystallization was used successfully for the optimization of one system, leading to the determination of a higher-quality crystal structure with lower R values together with an improvement of the diffraction resolution from 1.05 to 0.78 Å. To the best of our knowledge, the present publication is the first report of the crystallization of a porphyrin with the help of a gel, as well as the first crystal structure of an A₃B porphyrin with the 5-phenyl-10,15,20-tris(pyridyl)­porphyrin core unit.

The proposed decision tree for the nano-crystallization screen is summarized in Fig. 9.

Figure 9 Flow diagram for the nano-crystallization screen. The flow diagram was drawn with the help of diagrams.net (https://www.diagrams.net) by JGraph, 2025, version 28.2.7.

Finally, normal-coordinate structural decomposition (NSD) analysis revealed a rare example of an extrinsic distortion of a porphyrin ring induced by the dumbbell-shaped naphthalene-2,6-disulfonate anions above and, perpendicular to the first anion, below the porphyrin ring.

5. Related literature

The following references are cited in the supporting information: Dolomanov et al. (2009), Rigaku Oxford Diffraction (2024), Sheldrick (2015a, 2015b) and Thorn et al. (2012).

Supporting information

Computing details

(TMPyP)(nitrate)4(H2O)2.5

Crystal data

4(NO3)·2.5(O)·2(C22H19N4)·0.5[]	Z = 2
Mr = 966.86	F(000) = 1004
Triclinic, P1	Dx = 1.258 Mg m^−3
a = 6.38190 (9) Å	Cu Kα radiation, λ = 1.54184 Å
b = 16.2135 (2) Å	Cell parameters from 24054 reflections
c = 25.1193 (3) Å	θ = 2.8–77.7°
α = 82.8804 (11)°	µ = 0.82 mm^−1
β = 87.3709 (11)°	T = 160 K
γ = 81.8943 (11)°	Needle, red
V = 2552.29 (6) Å^3	0.21 × 0.05 × 0.04 mm

Data collection

XtaLAB Synergy, Dualflex, HyPix diffractometer	10919 independent reflections
Radiation source: micro-focus sealed X-ray tube, PhotonJet (Cu) X-ray Source	9365 reflections with I > 2σ(I)
Mirror monochromator	Rint = 0.043
Detector resolution: 10.0000 pixels mm^-1	θmax = 79.3°, θmin = 2.8°
ω scans	h = −7→8
Absorption correction: multi-scan CrysAlisPro 1.171.43.130a (Rigaku Oxford Diffraction, 2024) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	k = −18→20
Tmin = 0.834, Tmax = 1.000	l = −31→31
53886 measured reflections

Refinement

Refinement on F^2	Primary atom site location: dual
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.102	H-atom parameters constrained
wR(F^2) = 0.318	w = 1/[σ^2(Fo^2) + (0.2064P)^2 + 2.540P] where P = (Fo^2 + 2Fc^2)/3
S = 1.03	(Δ/σ)max = 0.001
10919 reflections	Δρmax = 1.14 e Å^−3
647 parameters	Δρmin = −0.53 e Å^−3
37 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	Occ. (<1)
O1	1.1516 (4)	0.26436 (17)	0.20827 (11)	0.0606 (6)
O2	0.9269 (5)	0.3587 (3)	0.16777 (15)	0.0929 (12)
O3	1.1270 (5)	0.3933 (2)	0.22522 (16)	0.0860 (11)
N6	1.0651 (4)	0.3399 (2)	0.20091 (12)	0.0525 (7)
O4	1.3883 (8)	0.5770 (5)	0.2969 (2)	0.101 (2)	0.705 (9)
O5	1.5056 (9)	0.6173 (4)	0.3612 (2)	0.102 (2)	0.705 (9)
O6	1.5811 (14)	0.6840 (6)	0.2880 (3)	0.127 (3)	0.705 (9)
N5	1.4828 (5)	0.6323 (3)	0.31108 (16)	0.0731 (10)
O8	0.913 (3)	0.2340 (10)	−0.1691 (7)	0.185 (6)*	0.5
O31	1.0189 (15)	0.2267 (6)	−0.1207 (4)	0.116 (3)*	0.5
O32	1.167 (3)	0.2047 (13)	−0.1933 (6)	0.224 (8)*	0.5
O33	1.3256 (11)	0.2116 (4)	−0.1182 (3)	0.0823 (17)*	0.5
N36	1.1849 (14)	0.2153 (6)	−0.1447 (4)	0.093 (2)*	0.5
O34	1.7327 (6)	−0.02736 (18)	0.09926 (14)	0.0804 (9)
O35	1.6715 (4)	0.09418 (17)	0.05595 (11)	0.0625 (7)
O36	1.6315 (6)	0.0810 (3)	0.14082 (13)	0.0916 (11)
N37	1.6805 (4)	0.04882 (19)	0.09910 (11)	0.0483 (6)
O37	1.5488 (19)	0.1151 (9)	0.3686 (6)	0.171 (5)*	0.5
O38	1.227 (2)	0.1090 (11)	0.3879 (6)	0.215 (7)*	0.5
O39	1.333 (3)	0.0884 (13)	0.3101 (6)	0.250 (9)*	0.5
N35	1.3785 (15)	0.1046 (4)	0.3549 (4)	0.090 (2)*	0.5
O46	1.5840 (17)	−0.0504 (5)	0.2252 (3)	0.207 (4)
N1	0.3723 (4)	0.40560 (16)	0.47432 (10)	0.0412 (5)
N2	0.7341 (4)	0.49345 (16)	0.43835 (10)	0.0407 (5)
H2	0.642419	0.494291	0.465601	0.049*
N3	0.7106 (5)	0.2305 (2)	0.26856 (12)	0.0571 (7)
N4	1.2975 (5)	0.7907 (2)	0.38260 (15)	0.0648 (8)
C1	0.2151 (5)	0.36342 (19)	0.49908 (12)	0.0416 (6)
C2	0.1906 (5)	0.2911 (2)	0.47225 (14)	0.0491 (7)
H2A	0.094777	0.251593	0.482168	0.059*
C3	0.3318 (5)	0.2912 (2)	0.43023 (13)	0.0491 (7)
H3	0.352503	0.252385	0.404436	0.059*
C4	0.4449 (5)	0.36225 (19)	0.43243 (12)	0.0422 (6)
C5	0.6169 (5)	0.37840 (19)	0.39746 (12)	0.0426 (6)
C6	0.7506 (5)	0.43802 (19)	0.40090 (11)	0.0415 (6)
C7	0.9275 (5)	0.4543 (2)	0.36627 (12)	0.0460 (7)
H7	0.979875	0.424046	0.337281	0.055*
C8	1.0080 (5)	0.5204 (2)	0.38189 (13)	0.0463 (7)
H8	1.126404	0.544542	0.365861	0.056*
C9	0.8816 (5)	0.54733 (19)	0.42703 (11)	0.0412 (6)
C10	0.9014 (5)	0.61592 (19)	0.45425 (12)	0.0417 (6)
C11	0.6575 (5)	0.3277 (2)	0.35176 (12)	0.0450 (6)
C12	0.8369 (6)	0.2685 (3)	0.34778 (15)	0.0585 (9)
H12	0.942596	0.261508	0.374002	0.070*
C13	0.8614 (7)	0.2201 (3)	0.30592 (16)	0.0632 (9)
H13	0.983537	0.179740	0.303299	0.076*
C14	0.5458 (6)	0.2903 (3)	0.26988 (14)	0.0601 (9)
H14	0.446589	0.298866	0.242007	0.072*
C15	0.5166 (5)	0.3396 (3)	0.31037 (14)	0.0547 (8)
H15	0.398606	0.382445	0.310234	0.066*
C16	0.7315 (8)	0.1760 (3)	0.22493 (18)	0.0766 (13)
H16A	0.853103	0.132184	0.231394	0.115*
H16B	0.752947	0.209807	0.190490	0.115*
H16C	0.602401	0.149936	0.224026	0.115*
C17	1.0458 (5)	0.67422 (19)	0.42956 (13)	0.0448 (6)
C18	1.0088 (6)	0.7151 (2)	0.37749 (14)	0.0526 (8)
H18	0.895832	0.702955	0.357704	0.063*
C19	1.1351 (7)	0.7722 (3)	0.35540 (17)	0.0644 (10)
H19	1.108693	0.799630	0.320212	0.077*
C20	1.3394 (6)	0.7509 (2)	0.43181 (17)	0.0604 (9)
H20	1.455571	0.763011	0.450445	0.072*
C21	1.2166 (5)	0.6932 (2)	0.45541 (15)	0.0533 (8)
H21	1.249220	0.665528	0.490234	0.064*
C22	1.4349 (10)	0.8529 (3)	0.3579 (3)	0.0997 (18)
H22A	1.455615	0.847971	0.319486	0.150*
H22B	1.572427	0.841967	0.375141	0.150*
H22C	1.367219	0.909619	0.362896	0.150*
N31	0.8553 (3)	0.40187 (14)	−0.01479 (9)	0.0343 (5)
N32	1.2103 (3)	0.41851 (14)	0.05060 (9)	0.0343 (5)
H32	1.113913	0.453083	0.032028	0.041*
N33	1.2040 (4)	0.02246 (16)	0.07689 (12)	0.0475 (6)
N34	1.8524 (4)	0.56554 (16)	0.19003 (10)	0.0424 (5)
C31	0.6887 (4)	0.40324 (17)	−0.04739 (10)	0.0358 (5)
C32	0.6362 (5)	0.31923 (19)	−0.04881 (12)	0.0423 (6)
H32A	0.528365	0.303845	−0.068930	0.051*
C33	0.7705 (5)	0.26761 (18)	−0.01598 (12)	0.0416 (6)
H33	0.773606	0.208714	−0.007479	0.050*
C34	0.9099 (4)	0.31944 (17)	0.00390 (10)	0.0355 (5)
C35	1.0819 (4)	0.28642 (17)	0.03679 (10)	0.0352 (5)
C36	1.2215 (4)	0.33271 (17)	0.05750 (10)	0.0350 (5)
C37	1.4052 (4)	0.30065 (18)	0.08803 (11)	0.0380 (6)
H37	1.456081	0.243117	0.098006	0.046*
C38	1.4944 (4)	0.36737 (18)	0.10027 (11)	0.0386 (6)
H38	1.617132	0.364450	0.120800	0.046*
C39	1.3710 (4)	0.44243 (17)	0.07685 (10)	0.0349 (5)
C40	1.4130 (4)	0.52456 (17)	0.07772 (10)	0.0354 (5)
C41	1.1233 (4)	0.19402 (17)	0.05087 (11)	0.0359 (5)
C42	1.1192 (5)	0.15833 (18)	0.10400 (11)	0.0396 (6)
H42	1.088262	0.192984	0.131979	0.047*
C43	1.1604 (5)	0.07208 (19)	0.11607 (13)	0.0452 (7)
H43	1.157668	0.047744	0.152461	0.054*
C44	1.2106 (5)	0.0554 (2)	0.02497 (14)	0.0482 (7)
H44	1.242830	0.019395	−0.002214	0.058*
C45	1.1711 (5)	0.1407 (2)	0.01102 (12)	0.0432 (6)
H45	1.176353	0.163375	−0.025675	0.052*
C46	1.2443 (7)	−0.0697 (2)	0.0907 (2)	0.0697 (11)
H46A	1.109403	−0.092541	0.093927	0.105*
H46B	1.316791	−0.083082	0.124881	0.105*
H46C	1.333421	−0.094640	0.062408	0.105*
C47	1.5743 (4)	0.53562 (17)	0.11625 (10)	0.0356 (5)
C48	1.7529 (4)	0.5731 (2)	0.09993 (11)	0.0411 (6)
H48	1.781234	0.588337	0.062835	0.049*
C49	1.8887 (5)	0.5880 (2)	0.13743 (12)	0.0435 (6)
H49	2.009363	0.614568	0.126086	0.052*
C50	1.6877 (5)	0.5257 (2)	0.20662 (12)	0.0448 (6)
H50	1.668361	0.507701	0.243751	0.054*
C51	1.5459 (5)	0.51028 (19)	0.17081 (11)	0.0399 (6)
H51	1.428500	0.482374	0.183246	0.048*
C52	1.9981 (6)	0.5849 (2)	0.22961 (15)	0.0560 (8)
H52A	1.919236	0.621595	0.254005	0.084*
H52B	2.110758	0.613216	0.210746	0.084*
H52C	2.060628	0.532661	0.250268	0.084*
O10	1.349 (2)	0.6545 (10)	0.2725 (6)	0.107 (4)*	0.295 (9)
O12	1.607 (3)	0.6808 (12)	0.3129 (9)	0.117 (4)*	0.295 (9)
O11	1.488 (3)	0.5656 (9)	0.3337 (7)	0.117 (4)*	0.295 (9)
O7	0.606 (2)	0.2628 (8)	−0.1816 (5)	0.141 (4)*	0.5
O9	1.535 (4)	0.0654 (14)	0.3240 (9)	0.230 (8)*	0.5

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
O1	0.0619 (15)	0.0593 (15)	0.0639 (15)	−0.0067 (12)	−0.0108 (12)	−0.0186 (12)
O2	0.0675 (18)	0.122 (3)	0.088 (2)	0.0210 (18)	−0.0442 (17)	−0.034 (2)
O3	0.080 (2)	0.0640 (17)	0.119 (3)	0.0085 (15)	−0.0450 (19)	−0.0372 (18)
N6	0.0458 (14)	0.0643 (17)	0.0493 (15)	−0.0027 (12)	−0.0140 (11)	−0.0144 (13)
O4	0.063 (3)	0.173 (6)	0.086 (4)	−0.049 (3)	0.014 (2)	−0.062 (4)
O5	0.102 (4)	0.116 (4)	0.080 (3)	0.047 (3)	−0.043 (3)	−0.033 (3)
O6	0.110 (5)	0.161 (6)	0.109 (5)	−0.032 (4)	0.041 (5)	−0.010 (5)
N5	0.0420 (15)	0.115 (3)	0.0687 (19)	−0.0081 (16)	0.0007 (13)	−0.0406 (19)
O34	0.096 (2)	0.0488 (15)	0.091 (2)	−0.0066 (14)	0.0041 (18)	0.0091 (14)
O35	0.0651 (16)	0.0559 (14)	0.0653 (16)	−0.0108 (12)	−0.0051 (12)	0.0011 (12)
O36	0.081 (2)	0.138 (3)	0.0658 (18)	−0.015 (2)	0.0007 (15)	−0.052 (2)
N37	0.0364 (12)	0.0596 (16)	0.0519 (15)	−0.0100 (11)	−0.0005 (10)	−0.0151 (12)
O46	0.305 (10)	0.163 (6)	0.123 (5)	0.003 (6)	0.063 (6)	0.036 (4)
N1	0.0390 (12)	0.0463 (13)	0.0378 (12)	0.0011 (10)	−0.0073 (9)	−0.0086 (10)
N2	0.0406 (12)	0.0453 (13)	0.0357 (11)	−0.0007 (10)	−0.0036 (9)	−0.0080 (10)
N3	0.0585 (17)	0.0700 (19)	0.0477 (15)	−0.0100 (14)	−0.0016 (12)	−0.0244 (14)
N4	0.0573 (17)	0.0532 (17)	0.078 (2)	−0.0014 (14)	0.0066 (15)	0.0053 (15)
C1	0.0395 (14)	0.0443 (15)	0.0400 (14)	0.0018 (11)	−0.0087 (11)	−0.0065 (11)
C2	0.0497 (17)	0.0489 (17)	0.0504 (17)	−0.0058 (13)	−0.0068 (13)	−0.0124 (13)
C3	0.0510 (17)	0.0499 (17)	0.0482 (16)	−0.0033 (13)	−0.0050 (13)	−0.0156 (13)
C4	0.0392 (14)	0.0460 (15)	0.0416 (14)	0.0017 (11)	−0.0100 (11)	−0.0107 (12)
C5	0.0421 (14)	0.0470 (15)	0.0379 (14)	0.0028 (12)	−0.0082 (11)	−0.0092 (11)
C6	0.0430 (14)	0.0434 (14)	0.0360 (13)	0.0042 (11)	−0.0069 (11)	−0.0066 (11)
C7	0.0462 (15)	0.0507 (16)	0.0397 (14)	0.0022 (13)	−0.0027 (12)	−0.0087 (12)
C8	0.0439 (15)	0.0499 (16)	0.0437 (15)	−0.0007 (12)	−0.0003 (12)	−0.0068 (12)
C9	0.0408 (14)	0.0450 (15)	0.0363 (13)	0.0027 (11)	−0.0058 (11)	−0.0062 (11)
C10	0.0382 (14)	0.0447 (15)	0.0408 (14)	0.0010 (11)	−0.0086 (11)	−0.0048 (11)
C11	0.0466 (15)	0.0500 (16)	0.0386 (14)	−0.0017 (13)	−0.0056 (12)	−0.0104 (12)
C12	0.0567 (19)	0.068 (2)	0.0501 (18)	0.0107 (16)	−0.0150 (15)	−0.0194 (16)
C13	0.065 (2)	0.068 (2)	0.055 (2)	0.0095 (18)	−0.0051 (16)	−0.0226 (17)
C14	0.0449 (17)	0.092 (3)	0.0471 (17)	−0.0055 (17)	−0.0091 (13)	−0.0243 (18)
C15	0.0433 (16)	0.073 (2)	0.0469 (17)	0.0046 (15)	−0.0091 (13)	−0.0163 (15)
C16	0.087 (3)	0.092 (3)	0.062 (2)	−0.024 (2)	0.009 (2)	−0.044 (2)
C17	0.0433 (15)	0.0427 (15)	0.0454 (15)	0.0044 (12)	−0.0049 (12)	−0.0043 (12)
C18	0.0553 (18)	0.0539 (18)	0.0449 (16)	0.0030 (14)	−0.0049 (13)	−0.0021 (14)
C19	0.069 (2)	0.059 (2)	0.057 (2)	0.0042 (18)	0.0000 (17)	0.0093 (17)
C20	0.0508 (18)	0.0545 (19)	0.073 (2)	−0.0027 (15)	−0.0073 (16)	−0.0008 (17)
C21	0.0479 (17)	0.0537 (18)	0.0565 (19)	−0.0028 (14)	−0.0108 (14)	−0.0005 (15)
C22	0.093 (4)	0.072 (3)	0.128 (5)	−0.020 (3)	0.017 (3)	0.020 (3)
N31	0.0350 (11)	0.0384 (11)	0.0305 (10)	−0.0077 (9)	−0.0062 (8)	−0.0031 (8)
N32	0.0343 (11)	0.0362 (11)	0.0331 (10)	−0.0057 (8)	−0.0075 (8)	−0.0036 (8)
N33	0.0405 (13)	0.0360 (12)	0.0678 (17)	−0.0046 (10)	−0.0097 (11)	−0.0108 (11)
N34	0.0427 (12)	0.0452 (13)	0.0414 (12)	−0.0030 (10)	−0.0133 (10)	−0.0119 (10)
C31	0.0356 (13)	0.0398 (13)	0.0338 (12)	−0.0105 (10)	−0.0061 (10)	−0.0033 (10)
C32	0.0441 (15)	0.0426 (14)	0.0429 (14)	−0.0139 (12)	−0.0127 (11)	−0.0026 (11)
C33	0.0440 (14)	0.0392 (14)	0.0440 (15)	−0.0124 (11)	−0.0124 (11)	−0.0023 (11)
C34	0.0368 (13)	0.0386 (13)	0.0322 (12)	−0.0094 (10)	−0.0038 (10)	−0.0028 (10)
C35	0.0358 (12)	0.0398 (13)	0.0309 (12)	−0.0070 (10)	−0.0028 (9)	−0.0051 (10)
C36	0.0346 (12)	0.0390 (13)	0.0318 (12)	−0.0057 (10)	−0.0048 (9)	−0.0041 (10)
C37	0.0375 (13)	0.0380 (13)	0.0393 (13)	−0.0038 (10)	−0.0092 (10)	−0.0061 (10)
C38	0.0370 (13)	0.0412 (14)	0.0383 (13)	−0.0045 (11)	−0.0096 (10)	−0.0054 (11)
C39	0.0336 (12)	0.0401 (13)	0.0319 (12)	−0.0063 (10)	−0.0052 (9)	−0.0047 (10)
C40	0.0337 (12)	0.0425 (14)	0.0314 (12)	−0.0087 (10)	−0.0045 (9)	−0.0042 (10)
C41	0.0325 (12)	0.0407 (13)	0.0364 (13)	−0.0063 (10)	−0.0039 (9)	−0.0093 (10)
C42	0.0422 (14)	0.0402 (14)	0.0374 (13)	−0.0070 (11)	−0.0052 (11)	−0.0057 (11)
C43	0.0448 (15)	0.0433 (15)	0.0477 (16)	−0.0100 (12)	−0.0109 (12)	0.0014 (12)
C44	0.0420 (15)	0.0473 (16)	0.0590 (18)	−0.0070 (12)	−0.0019 (13)	−0.0193 (14)
C45	0.0410 (14)	0.0491 (16)	0.0425 (15)	−0.0081 (12)	−0.0027 (11)	−0.0151 (12)
C46	0.066 (2)	0.0358 (16)	0.108 (3)	−0.0046 (15)	−0.019 (2)	−0.0081 (18)
C47	0.0361 (12)	0.0392 (13)	0.0325 (12)	−0.0047 (10)	−0.0062 (10)	−0.0069 (10)
C48	0.0370 (13)	0.0529 (16)	0.0348 (13)	−0.0081 (12)	−0.0023 (10)	−0.0080 (11)
C49	0.0355 (13)	0.0526 (16)	0.0452 (15)	−0.0089 (12)	−0.0056 (11)	−0.0117 (12)
C50	0.0506 (16)	0.0509 (16)	0.0342 (13)	−0.0074 (13)	−0.0081 (12)	−0.0063 (12)
C51	0.0414 (14)	0.0453 (15)	0.0341 (13)	−0.0091 (11)	−0.0029 (10)	−0.0050 (11)
C52	0.0565 (19)	0.065 (2)	0.0518 (18)	−0.0081 (16)	−0.0229 (15)	−0.0195 (15)

Geometric parameters (Å, º)

O1—N6	1.265 (4)	C18—H18	0.9500
O2—N6	1.221 (4)	C18—C19	1.363 (6)
O3—N6	1.237 (4)	C19—H19	0.9500
O4—N5	1.243 (6)	C20—H20	0.9500
O5—N5	1.263 (6)	C20—C21	1.367 (5)
O6—N5	1.195 (8)	C21—H21	0.9500
N5—O10	1.305 (12)	C22—H22A	0.9800
N5—O12	1.199 (15)	C22—H22B	0.9800
N5—O11	1.154 (13)	C22—H22C	0.9800
O31—N36	1.197 (8)	N31—C31	1.368 (3)
O32—N36	1.266 (9)	N31—C34	1.362 (3)
O33—N36	1.133 (8)	N32—H32	0.8800
O34—N37	1.233 (4)	N32—C36	1.372 (3)
O35—N37	1.231 (4)	N32—C39	1.369 (3)
O36—N37	1.236 (4)	N33—C43	1.342 (4)
O37—N35	1.195 (9)	N33—C44	1.348 (5)
O38—N35	1.245 (9)	N33—C46	1.481 (4)
O39—N35	1.245 (9)	N34—C49	1.345 (4)
N1—C1	1.376 (4)	N34—C50	1.334 (4)
N1—C4	1.365 (4)	N34—C52	1.482 (4)
N2—H2	0.8800	C31—C32	1.453 (4)
N2—C6	1.370 (4)	C31—C40^ii	1.408 (4)
N2—C9	1.370 (4)	C32—H32A	0.9500
N3—C13	1.354 (5)	C32—C33	1.344 (4)
N3—C14	1.329 (5)	C33—H33	0.9500
N3—C16	1.480 (4)	C33—C34	1.450 (4)
N4—C19	1.354 (6)	C34—C35	1.408 (4)
N4—C20	1.341 (5)	C35—C36	1.398 (4)
N4—C22	1.488 (6)	C35—C41	1.485 (4)
C1—C2	1.453 (4)	C36—C37	1.430 (4)
C1—C10^i	1.409 (4)	C37—H37	0.9500
C2—H2A	0.9500	C37—C38	1.364 (4)
C2—C3	1.356 (5)	C38—H38	0.9500
C3—H3	0.9500	C38—C39	1.429 (4)
C3—C4	1.451 (5)	C39—C40	1.398 (4)
C4—C5	1.407 (4)	C40—C47	1.488 (3)
C5—C6	1.389 (4)	C41—C42	1.388 (4)
C5—C11	1.486 (4)	C41—C45	1.399 (4)
C6—C7	1.427 (4)	C42—H42	0.9500
C7—H7	0.9500	C42—C43	1.384 (4)
C7—C8	1.359 (5)	C43—H43	0.9500
C8—H8	0.9500	C44—H44	0.9500
C8—C9	1.438 (4)	C44—C45	1.373 (5)
C9—C10	1.399 (4)	C45—H45	0.9500
C10—C17	1.475 (4)	C46—H46A	0.9800
C11—C12	1.394 (5)	C46—H46B	0.9800
C11—C15	1.384 (4)	C46—H46C	0.9800
C12—H12	0.9500	C47—C48	1.388 (4)
C12—C13	1.378 (5)	C47—C51	1.392 (4)
C13—H13	0.9500	C48—H48	0.9500
C14—H14	0.9500	C48—C49	1.374 (4)
C14—C15	1.360 (5)	C49—H49	0.9500
C15—H15	0.9500	C50—H50	0.9500
C16—H16A	0.9800	C50—C51	1.373 (4)
C16—H16B	0.9800	C51—H51	0.9500
C16—H16C	0.9800	C52—H52A	0.9800
C17—C18	1.406 (4)	C52—H52B	0.9800
C17—C21	1.383 (5)	C52—H52C	0.9800
O2—N6—O1	118.3 (3)	C17—C21—H21	119.4
O2—N6—O3	121.5 (4)	C20—C21—C17	121.3 (3)
O3—N6—O1	120.1 (3)	C20—C21—H21	119.4
O4—N5—O5	107.9 (6)	N4—C22—H22A	109.5
O6—N5—O4	134.5 (6)	N4—C22—H22B	109.5
O6—N5—O5	116.1 (6)	N4—C22—H22C	109.5
O12—N5—O10	113.5 (10)	H22A—C22—H22B	109.5
O11—N5—O10	117.8 (10)	H22A—C22—H22C	109.5
O11—N5—O12	127.7 (11)	H22B—C22—H22C	109.5
O31—N36—O32	113.5 (13)	C34—N31—C31	105.0 (2)
O33—N36—O31	112.8 (10)	C36—N32—H32	125.0
O33—N36—O32	133.5 (14)	C39—N32—H32	125.0
O34—N37—O36	122.1 (4)	C39—N32—C36	110.0 (2)
O35—N37—O34	119.1 (3)	C43—N33—C44	120.8 (3)
O35—N37—O36	118.8 (3)	C43—N33—C46	119.7 (3)
O37—N35—O38	119.1 (10)	C44—N33—C46	119.4 (3)
O37—N35—O39	126.8 (11)	C49—N34—C52	119.4 (3)
O39—N35—O38	114.1 (10)	C50—N34—C49	120.5 (2)
C4—N1—C1	105.0 (2)	C50—N34—C52	120.1 (3)
C6—N2—H2	125.1	N31—C31—C32	111.0 (2)
C9—N2—H2	125.1	N31—C31—C40^ii	125.0 (2)
C9—N2—C6	109.8 (2)	C40^ii—C31—C32	124.0 (2)
C13—N3—C16	119.8 (3)	C31—C32—H32A	126.8
C14—N3—C13	120.7 (3)	C33—C32—C31	106.3 (2)
C14—N3—C16	119.4 (3)	C33—C32—H32A	126.8
C19—N4—C22	120.8 (4)	C32—C33—H33	126.7
C20—N4—C19	119.9 (3)	C32—C33—C34	106.5 (2)
C20—N4—C22	119.3 (4)	C34—C33—H33	126.7
N1—C1—C2	110.9 (3)	N31—C34—C33	111.1 (2)
N1—C1—C10^i	125.3 (3)	N31—C34—C35	125.8 (2)
C10^i—C1—C2	123.7 (3)	C35—C34—C33	123.1 (3)
C1—C2—H2A	126.9	C34—C35—C41	118.1 (2)
C3—C2—C1	106.3 (3)	C36—C35—C34	126.0 (3)
C3—C2—H2A	126.9	C36—C35—C41	115.9 (2)
C2—C3—H3	126.8	N32—C36—C35	125.8 (2)
C2—C3—C4	106.4 (3)	N32—C36—C37	107.0 (2)
C4—C3—H3	126.8	C35—C36—C37	127.2 (3)
N1—C4—C3	111.3 (3)	C36—C37—H37	126.1
N1—C4—C5	126.0 (3)	C38—C37—C36	107.8 (2)
C5—C4—C3	122.6 (3)	C38—C37—H37	126.1
C4—C5—C11	116.8 (3)	C37—C38—H38	125.9
C6—C5—C4	126.5 (3)	C37—C38—C39	108.1 (2)
C6—C5—C11	116.7 (3)	C39—C38—H38	125.9
N2—C6—C5	125.7 (3)	N32—C39—C38	107.0 (2)
N2—C6—C7	107.1 (3)	N32—C39—C40	126.3 (2)
C5—C6—C7	127.2 (3)	C40—C39—C38	126.7 (2)
C6—C7—H7	125.9	C31^ii—C40—C47	118.0 (2)
C8—C7—C6	108.3 (3)	C39—C40—C31^ii	126.0 (2)
C8—C7—H7	125.9	C39—C40—C47	115.9 (2)
C7—C8—H8	126.2	C42—C41—C35	120.9 (2)
C7—C8—C9	107.6 (3)	C42—C41—C45	118.2 (3)
C9—C8—H8	126.2	C45—C41—C35	120.9 (2)
N2—C9—C8	107.0 (3)	C41—C42—H42	120.1
N2—C9—C10	125.9 (3)	C43—C42—C41	119.8 (3)
C10—C9—C8	127.1 (3)	C43—C42—H42	120.1
C1^i—C10—C17	117.8 (3)	N33—C43—C42	120.7 (3)
C9—C10—C1^i	125.4 (3)	N33—C43—H43	119.7
C9—C10—C17	116.7 (3)	C42—C43—H43	119.7
C12—C11—C5	122.7 (3)	N33—C44—H44	119.7
C15—C11—C5	120.0 (3)	N33—C44—C45	120.6 (3)
C15—C11—C12	117.4 (3)	C45—C44—H44	119.7
C11—C12—H12	119.9	C41—C45—H45	120.0
C13—C12—C11	120.2 (3)	C44—C45—C41	119.9 (3)
C13—C12—H12	119.9	C44—C45—H45	120.0
N3—C13—C12	119.7 (3)	N33—C46—H46A	109.5
N3—C13—H13	120.2	N33—C46—H46B	109.5
C12—C13—H13	120.2	N33—C46—H46C	109.5
N3—C14—H14	119.4	H46A—C46—H46B	109.5
N3—C14—C15	121.3 (3)	H46A—C46—H46C	109.5
C15—C14—H14	119.4	H46B—C46—H46C	109.5
C11—C15—H15	119.8	C48—C47—C40	122.1 (2)
C14—C15—C11	120.5 (3)	C48—C47—C51	117.8 (2)
C14—C15—H15	119.8	C51—C47—C40	120.1 (2)
N3—C16—H16A	109.5	C47—C48—H48	120.0
N3—C16—H16B	109.5	C49—C48—C47	120.0 (3)
N3—C16—H16C	109.5	C49—C48—H48	120.0
H16A—C16—H16B	109.5	N34—C49—C48	120.7 (3)
H16A—C16—H16C	109.5	N34—C49—H49	119.7
H16B—C16—H16C	109.5	C48—C49—H49	119.7
C18—C17—C10	119.6 (3)	N34—C50—H50	119.5
C21—C17—C10	123.5 (3)	N34—C50—C51	121.0 (3)
C21—C17—C18	116.9 (3)	C51—C50—H50	119.5
C17—C18—H18	120.0	C47—C51—H51	120.0
C19—C18—C17	119.9 (4)	C50—C51—C47	119.9 (3)
C19—C18—H18	120.0	C50—C51—H51	120.0
N4—C19—C18	121.3 (3)	N34—C52—H52A	109.5
N4—C19—H19	119.3	N34—C52—H52B	109.5
C18—C19—H19	119.3	N34—C52—H52C	109.5
N4—C20—H20	119.7	H52A—C52—H52B	109.5
N4—C20—C21	120.6 (4)	H52A—C52—H52C	109.5
C21—C20—H20	119.7	H52B—C52—H52C	109.5
N1—C1—C2—C3	−1.3 (4)	N31—C31—C32—C33	1.1 (3)
N1—C4—C5—C6	3.7 (5)	N31—C34—C35—C36	2.5 (5)
N1—C4—C5—C11	−175.1 (3)	N31—C34—C35—C41	−176.9 (2)
N2—C6—C7—C8	−2.4 (3)	N32—C36—C37—C38	2.2 (3)
N2—C9—C10—C1^i	6.0 (5)	N32—C39—C40—C31^ii	−6.9 (5)
N2—C9—C10—C17	−169.5 (3)	N32—C39—C40—C47	170.3 (2)
N3—C14—C15—C11	−0.8 (6)	N33—C44—C45—C41	−0.1 (5)
N4—C20—C21—C17	−0.3 (6)	N34—C50—C51—C47	0.7 (5)
C1—N1—C4—C3	0.2 (3)	C31—N31—C34—C33	−1.8 (3)
C1—N1—C4—C5	−175.3 (3)	C31—N31—C34—C35	176.3 (3)
C1—C2—C3—C4	1.4 (3)	C31—C32—C33—C34	−2.1 (3)
C1^i—C10—C17—C18	−116.8 (3)	C31^ii—C40—C47—C48	−58.7 (4)
C1^i—C10—C17—C21	61.7 (4)	C31^ii—C40—C47—C51	119.4 (3)
C2—C3—C4—N1	−1.0 (4)	C32—C33—C34—N31	2.5 (3)
C2—C3—C4—C5	174.7 (3)	C32—C33—C34—C35	−175.6 (3)
C3—C4—C5—C6	−171.3 (3)	C33—C34—C35—C36	−179.7 (3)
C3—C4—C5—C11	9.8 (4)	C33—C34—C35—C41	1.0 (4)
C4—N1—C1—C2	0.7 (3)	C34—N31—C31—C32	0.5 (3)
C4—N1—C1—C10^i	177.8 (3)	C34—N31—C31—C40^ii	−176.7 (3)
C4—C5—C6—N2	−2.0 (5)	C34—C35—C36—N32	2.2 (4)
C4—C5—C6—C7	179.0 (3)	C34—C35—C36—C37	−175.6 (3)
C4—C5—C11—C12	−112.3 (4)	C34—C35—C41—C42	−120.1 (3)
C4—C5—C11—C15	69.1 (4)	C34—C35—C41—C45	61.0 (4)
C5—C6—C7—C8	176.8 (3)	C35—C36—C37—C38	−179.7 (3)
C5—C11—C12—C13	176.7 (4)	C35—C41—C42—C43	−179.4 (3)
C5—C11—C15—C14	−176.3 (4)	C35—C41—C45—C44	179.5 (3)
C6—N2—C9—C8	−4.1 (3)	C36—N32—C39—C38	1.8 (3)
C6—N2—C9—C10	175.1 (3)	C36—N32—C39—C40	178.3 (3)
C6—C5—C11—C12	68.7 (4)	C36—C35—C41—C42	60.5 (3)
C6—C5—C11—C15	−109.9 (4)	C36—C35—C41—C45	−118.4 (3)
C6—C7—C8—C9	−0.1 (3)	C36—C37—C38—C39	−1.1 (3)
C7—C8—C9—N2	2.6 (3)	C37—C38—C39—N32	−0.4 (3)
C7—C8—C9—C10	−176.7 (3)	C37—C38—C39—C40	−176.9 (3)
C8—C9—C10—C1^i	−174.9 (3)	C38—C39—C40—C31^ii	168.9 (3)
C8—C9—C10—C17	9.6 (4)	C38—C39—C40—C47	−13.9 (4)
C9—N2—C6—C5	−175.1 (3)	C39—N32—C36—C35	179.4 (3)
C9—N2—C6—C7	4.1 (3)	C39—N32—C36—C37	−2.5 (3)
C9—C10—C17—C18	59.0 (4)	C39—C40—C47—C48	123.8 (3)
C9—C10—C17—C21	−122.5 (3)	C39—C40—C47—C51	−58.1 (4)
C10^i—C1—C2—C3	−178.5 (3)	C40^ii—C31—C32—C33	178.3 (3)
C10—C17—C18—C19	176.7 (3)	C40—C47—C48—C49	174.8 (3)
C10—C17—C21—C20	−176.6 (3)	C40—C47—C51—C50	−175.7 (3)
C11—C5—C6—N2	176.9 (3)	C41—C35—C36—N32	−178.5 (2)
C11—C5—C6—C7	−2.1 (4)	C41—C35—C36—C37	3.8 (4)
C11—C12—C13—N3	0.2 (7)	C41—C42—C43—N33	−0.1 (4)
C12—C11—C15—C14	5.1 (6)	C42—C41—C45—C44	0.6 (4)
C13—N3—C14—C15	−4.0 (6)	C43—N33—C44—C45	−0.5 (5)
C14—N3—C13—C12	4.3 (6)	C44—N33—C43—C42	0.6 (4)
C15—C11—C12—C13	−4.7 (6)	C45—C41—C42—C43	−0.5 (4)
C16—N3—C13—C12	−177.2 (4)	C46—N33—C43—C42	−179.1 (3)
C16—N3—C14—C15	177.5 (4)	C46—N33—C44—C45	179.2 (3)
C17—C18—C19—N4	0.1 (6)	C47—C48—C49—N34	1.1 (5)
C18—C17—C21—C20	1.9 (5)	C48—C47—C51—C50	2.6 (4)
C19—N4—C20—C21	−1.5 (6)	C49—N34—C50—C51	−3.2 (5)
C20—N4—C19—C18	1.6 (6)	C50—N34—C49—C48	2.3 (5)
C21—C17—C18—C19	−1.8 (5)	C51—C47—C48—C49	−3.4 (4)
C22—N4—C19—C18	179.7 (4)	C52—N34—C49—C48	−178.1 (3)
C22—N4—C20—C21	−179.7 (4)	C52—N34—C50—C51	177.2 (3)

Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+2, −y+1, −z.

(TMPyP)(2,6-naphthalenedisulfonate]2(H2O)7.5

Crystal data

2(C10H6O6S2)·7.5(H2O)·HO·C44H38N8	Z = 2
Mr = 1403.48	F(000) = 1468
Triclinic, P1	Dx = 1.465 Mg m^−3
a = 14.7794 (2) Å	Cu Kα radiation, λ = 1.54184 Å
b = 15.2582 (2) Å	Cell parameters from 54959 reflections
c = 16.0581 (3) Å	θ = 3.1–79.1°
α = 72.391 (1)°	µ = 2.09 mm^−1
β = 68.206 (2)°	T = 160 K
γ = 89.592 (1)°	Needle, red
V = 3182.12 (10) Å^3	0.24 × 0.09 × 0.06 mm

Data collection

XtaLAB Synergy, Dualflex, HyPix diffractometer	13577 independent reflections
Radiation source: micro-focus sealed X-ray tube, PhotonJet (Cu) X-ray Source	12530 reflections with I > 2σ(I)
Mirror monochromator	Rint = 0.039
Detector resolution: 10.0000 pixels mm^-1	θmax = 79.6°, θmin = 3.1°
ω scans	h = −18→18
Absorption correction: gaussian CrysAlisPro 1.171.43.130a (Rigaku Oxford Diffraction, 2024) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	k = −19→16
Tmin = 0.554, Tmax = 1.000	l = −20→18
89349 measured reflections

Refinement

Refinement on F^2	30 restraints
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.102	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.329	w = 1/[σ^2(Fo^2) + (0.1309P)^2 + 18.5266P] where P = (Fo^2 + 2Fc^2)/3
S = 1.16	(Δ/σ)max < 0.001
13577 reflections	Δρmax = 0.95 e Å^−3
938 parameters	Δρmin = −0.54 e Å^−3

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.

Refinement. Refined as a 2-component twin.

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

	x	y	z	Uiso*/Ueq	Occ. (<1)
S1	0.1084 (2)	0.74570 (13)	0.52052 (17)	0.0420 (9)	0.836 (11)
S2	0.36613 (10)	0.25057 (10)	0.48393 (10)	0.0336 (3)
S3	0.78853 (14)	0.37560 (12)	0.01618 (12)	0.0471 (4)
S4	0.27521 (11)	0.13919 (10)	0.00661 (11)	0.0375 (3)
S5	0.1392 (9)	0.7541 (7)	0.5423 (9)	0.036 (3)*	0.164 (11)
O1	0.1685 (5)	0.8306 (4)	0.4524 (5)	0.0526 (18)	0.836 (11)
O2	0.4698 (3)	0.2817 (3)	0.4480 (4)	0.0449 (11)
O3	0.0923 (5)	0.7390 (4)	0.6199 (4)	0.0643 (16)
O4	0.0206 (5)	0.7277 (4)	0.5088 (5)	0.0762 (18)
O5	0.3281 (3)	0.1883 (3)	0.5807 (3)	0.0452 (11)
O6	0.3392 (4)	0.2118 (3)	0.4229 (4)	0.0478 (11)
O7	0.8828 (4)	0.3743 (5)	−0.0540 (4)	0.0752 (19)
O8	0.2144 (4)	0.1161 (4)	0.1059 (4)	0.0588 (14)
O9	0.7635 (5)	0.4681 (4)	0.0125 (5)	0.0708 (17)
O10	0.7766 (5)	0.3209 (4)	0.1118 (4)	0.0578 (14)
O11	0.2356 (5)	0.2020 (4)	−0.0545 (5)	0.0662 (16)
O12	0.3035 (4)	0.0578 (3)	−0.0206 (3)	0.0461 (11)
O13	0.8030 (4)	0.1395 (4)	0.1911 (4)	0.0594 (13)
H13A	0.801 (7)	0.135 (7)	0.248 (3)	0.089*
H13B	0.804 (7)	0.197 (3)	0.158 (6)	0.089*
O14	1.0253 (5)	0.2934 (4)	0.0151 (4)	0.0624 (14)
H14A	0.994 (4)	0.326 (6)	−0.017 (6)	0.094*
H14B	1.015 (9)	0.239 (4)	0.012 (8)	0.094*
O15	0.9655 (4)	0.0973 (5)	0.0637 (5)	0.0662 (16)
H15A	0.915 (6)	0.111 (8)	0.105 (7)	0.099*
H15B	0.959 (7)	0.083 (8)	0.017 (6)	0.099*
O16	0.9001 (5)	0.0338 (4)	−0.0494 (5)	0.0656 (16)
H16A	0.841 (3)	0.004 (8)	−0.031 (8)	0.098*
H16B	0.924 (7)	−0.027 (8)	−0.058 (8)	0.098*
O17	0.0981 (7)	0.9934 (5)	0.4627 (6)	0.106 (3)
H17A	0.112 (6)	0.941 (3)	0.455 (7)	0.159*
O18	0.7690 (6)	0.1448 (7)	0.3711 (6)	0.104 (3)
H18A	0.801 (11)	0.162 (4)	0.400 (9)	0.156*
H18B	0.756 (4)	0.0815 (9)	0.399 (3)	0.156*
O19	0.2045 (7)	1.0402 (6)	0.5477 (7)	0.111 (3)
H19A	0.167 (9)	1.036 (6)	0.517 (9)	0.167*
H19B	0.248 (7)	1.087 (6)	0.512 (8)	0.167*
O20	0.5824 (8)	0.1455 (9)	0.4951 (7)	0.125 (4)
H20A	0.550859	0.110973	0.478131	0.187*
H20B	0.640136	0.161224	0.449256	0.187*
O21	0.4299 (14)	0.0149 (10)	0.5655 (15)	0.098 (5)	0.5
H21A	0.375601	−0.009970	0.568450	0.147*	0.5
H21B	0.414474	0.064687	0.580597	0.147*	0.5
O22	0.195 (3)	0.843 (2)	0.489 (3)	0.060 (6)	0.164 (11)
N1	0.3835 (3)	0.5157 (3)	0.2451 (3)	0.0277 (9)
H1	0.355951	0.563053	0.260040	0.033*
N2	0.4506 (3)	0.6868 (3)	0.2570 (3)	0.0271 (9)
N3	0.2696 (3)	0.7654 (3)	0.2573 (3)	0.0275 (9)
H3	0.286182	0.708759	0.269735	0.033*
N4	0.1994 (3)	0.5914 (3)	0.2530 (3)	0.0271 (9)
N5	0.0968 (4)	0.1940 (3)	0.2492 (4)	0.0371 (11)
N6	0.8246 (4)	0.4622 (3)	0.2011 (4)	0.0343 (10)
N7	0.5208 (4)	1.0970 (3)	0.2668 (4)	0.0324 (10)
N8	−0.1373 (3)	0.8537 (3)	0.2234 (4)	0.0340 (10)
C1	0.3377 (4)	0.4462 (4)	0.2314 (4)	0.0277 (10)
C2	0.4096 (4)	0.3856 (4)	0.2049 (4)	0.0313 (11)
H2	0.399360	0.331807	0.190019	0.038*
C3	0.4948 (4)	0.4183 (4)	0.2048 (4)	0.0307 (11)
H3A	0.554716	0.391773	0.189499	0.037*
C4	0.4779 (4)	0.5003 (3)	0.2320 (4)	0.0277 (10)
C5	0.5442 (4)	0.5535 (4)	0.2470 (4)	0.0292 (11)
C6	0.5256 (4)	0.6372 (4)	0.2669 (4)	0.0279 (10)
C7	0.5846 (4)	0.6843 (4)	0.2994 (4)	0.0310 (11)
H7	0.639552	0.663026	0.313473	0.037*
C8	0.5469 (4)	0.7629 (4)	0.3057 (4)	0.0297 (11)
H8	0.569117	0.807992	0.325859	0.036*
C9	0.4650 (4)	0.7661 (4)	0.2755 (4)	0.0273 (10)
C10	0.4113 (4)	0.8421 (4)	0.2631 (4)	0.0280 (10)
C11	0.3241 (4)	0.8417 (3)	0.2479 (4)	0.0265 (10)
C12	0.2746 (4)	0.9205 (4)	0.2208 (4)	0.0313 (11)
H12	0.296765	0.983515	0.207212	0.038*
C13	0.1908 (4)	0.8883 (4)	0.2184 (4)	0.0298 (11)
H13	0.143704	0.924726	0.202243	0.036*
C14	0.1857 (4)	0.7893 (4)	0.2445 (4)	0.0288 (11)
C15	0.1101 (4)	0.7275 (4)	0.2546 (4)	0.0284 (10)
C16	0.1156 (4)	0.6331 (4)	0.2665 (4)	0.0283 (10)
C17	0.0314 (4)	0.5654 (4)	0.2928 (4)	0.0302 (11)
H17	−0.035247	0.576524	0.308488	0.036*
C18	0.0675 (4)	0.4843 (4)	0.2904 (4)	0.0318 (11)
H18	0.031232	0.426993	0.304294	0.038*
C19	0.1735 (4)	0.5023 (4)	0.2621 (4)	0.0273 (10)
C20	0.2388 (4)	0.4371 (4)	0.2439 (4)	0.0295 (11)
C21	0.6417 (4)	0.5222 (4)	0.2360 (4)	0.0279 (10)
C22	0.6521 (4)	0.4315 (4)	0.2831 (4)	0.0302 (11)
H22	0.596008	0.389510	0.327932	0.036*
C23	0.7443 (4)	0.4039 (4)	0.2638 (4)	0.0345 (12)
H23	0.751263	0.342297	0.295462	0.041*
C24	0.8170 (4)	0.5506 (4)	0.1570 (4)	0.0345 (12)
H24	0.874490	0.591692	0.113900	0.041*
C25	0.7265 (4)	0.5818 (4)	0.1740 (4)	0.0321 (11)
H25	0.721913	0.644462	0.143170	0.039*
C26	0.9213 (5)	0.4273 (5)	0.1762 (5)	0.0432 (15)
H26A	0.931085	0.399565	0.126229	0.065*
H26B	0.923925	0.380400	0.232259	0.065*
H26C	0.973025	0.478635	0.153430	0.065*
C27	0.4493 (4)	0.9306 (4)	0.2654 (4)	0.0278 (10)
C28	0.5464 (4)	0.9692 (4)	0.2095 (4)	0.0314 (11)
H28	0.589183	0.938314	0.169964	0.038*
C29	0.5802 (4)	1.0517 (4)	0.2117 (4)	0.0328 (11)
H29	0.646552	1.077253	0.173710	0.039*
C30	0.4274 (4)	1.0612 (4)	0.3211 (5)	0.0363 (12)
H30	0.386158	1.094087	0.359288	0.044*
C31	0.3898 (4)	0.9781 (4)	0.3231 (4)	0.0326 (11)
H31	0.323811	0.953138	0.363438	0.039*
C32	0.5589 (5)	1.1864 (4)	0.2664 (6)	0.0493 (17)
H32A	0.504233	1.215883	0.299574	0.074*
H32B	0.592904	1.226826	0.200784	0.074*
H32C	0.604875	1.175750	0.298409	0.074*
C33	0.0197 (4)	0.7670 (4)	0.2485 (4)	0.0291 (11)
C34	−0.0277 (4)	0.8229 (4)	0.3017 (4)	0.0329 (11)
H34	−0.006524	0.831016	0.348241	0.039*
C35	−0.1039 (4)	0.8659 (4)	0.2876 (4)	0.0367 (12)
H35	−0.134330	0.905157	0.323282	0.044*
C36	−0.0957 (4)	0.7968 (4)	0.1733 (4)	0.0354 (12)
H36	−0.120578	0.787149	0.129621	0.042*
C37	−0.0179 (4)	0.7527 (4)	0.1849 (4)	0.0328 (11)
H37	0.010467	0.712435	0.149769	0.039*
C38	−0.2174 (4)	0.9038 (5)	0.2051 (5)	0.0419 (14)
H38A	−0.189478	0.961191	0.151630	0.063*
H38B	−0.258767	0.918749	0.261596	0.063*
H38C	−0.257201	0.864785	0.189820	0.063*
C39	0.1973 (4)	0.3503 (4)	0.2400 (4)	0.0292 (11)
C40	0.1500 (4)	0.3539 (4)	0.1779 (4)	0.0346 (12)
H40	0.152113	0.410966	0.131574	0.042*
C41	0.1010 (4)	0.2753 (4)	0.1843 (5)	0.0373 (13)
H41	0.069278	0.278094	0.141996	0.045*
C42	0.1468 (5)	0.1868 (4)	0.3053 (5)	0.0381 (13)
H42	0.146550	0.128143	0.348270	0.046*
C43	0.1985 (5)	0.2642 (4)	0.3011 (4)	0.0359 (12)
H43	0.234848	0.258385	0.339946	0.043*
C44	0.0328 (5)	0.1125 (5)	0.2610 (6)	0.0528 (18)
H44A	−0.036079	0.123864	0.284960	0.079*
H44B	0.042505	0.057346	0.306056	0.079*
H44C	0.049746	0.102748	0.199628	0.079*
C51	0.1431 (5)	0.5778 (4)	0.4990 (5)	0.0434 (15)
H51	0.078329	0.575222	0.500482	0.052*
C52	0.1840 (5)	0.6546 (5)	0.5019 (5)	0.0467 (16)
C53	0.2812 (6)	0.6638 (5)	0.4964 (5)	0.0495 (17)
H53	0.308594	0.719189	0.497778	0.059*
C54	0.3358 (5)	0.5908 (4)	0.4889 (5)	0.0418 (14)
H54	0.401728	0.596656	0.483740	0.050*
C55	0.3474 (4)	0.4296 (4)	0.4836 (4)	0.0338 (12)
H55	0.413433	0.432694	0.478649	0.041*
C56	0.3033 (5)	0.3508 (4)	0.4858 (4)	0.0334 (11)
C57	0.2046 (5)	0.3434 (4)	0.4928 (4)	0.0370 (12)
H57	0.174374	0.286996	0.496061	0.044*
C58	0.1550 (5)	0.4168 (5)	0.4946 (5)	0.0400 (13)
H58	0.090056	0.412740	0.496568	0.048*
C59	0.1964 (5)	0.5003 (4)	0.4938 (4)	0.0375 (13)
C60	0.2951 (5)	0.5073 (4)	0.4887 (4)	0.0368 (12)
C61	0.4669 (5)	0.1669 (5)	−0.0139 (5)	0.0444 (15)
H61	0.471894	0.105883	−0.017211	0.053*
C62	0.3825 (5)	0.2034 (5)	−0.0072 (5)	0.0427 (14)
C63	0.3720 (5)	0.2963 (5)	−0.0040 (5)	0.0437 (14)
H63	0.312079	0.321709	0.000846	0.052*
C64	0.4501 (6)	0.3471 (5)	−0.0082 (5)	0.0464 (15)
H64	0.445181	0.409178	−0.008131	0.056*
C65	0.6160 (5)	0.3612 (5)	−0.0087 (4)	0.0442 (14)
H65	0.610592	0.422994	−0.007822	0.053*
C66	0.6988 (5)	0.3208 (4)	−0.0062 (4)	0.0398 (13)
C67	0.7095 (6)	0.2299 (5)	−0.0139 (5)	0.0446 (15)
H67	0.768356	0.203583	−0.015526	0.053*
C68	0.6365 (5)	0.1812 (5)	−0.0189 (5)	0.0454 (15)
H68	0.644877	0.121058	−0.024266	0.055*
C69	0.5499 (5)	0.2178 (4)	−0.0162 (4)	0.0400 (14)
C70	0.5371 (5)	0.3089 (4)	−0.0126 (4)	0.0421 (14)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
S1	0.0502 (14)	0.0284 (9)	0.0405 (11)	0.0080 (8)	−0.0084 (10)	−0.0133 (7)
S2	0.0357 (7)	0.0311 (7)	0.0372 (7)	0.0055 (5)	−0.0164 (6)	−0.0127 (6)
S3	0.0564 (10)	0.0479 (9)	0.0373 (8)	−0.0111 (7)	−0.0184 (7)	−0.0135 (7)
S4	0.0413 (8)	0.0308 (7)	0.0395 (8)	0.0039 (6)	−0.0145 (6)	−0.0115 (6)
O1	0.067 (4)	0.029 (3)	0.042 (3)	0.006 (3)	−0.001 (3)	−0.010 (2)
O2	0.032 (2)	0.040 (2)	0.056 (3)	0.0052 (18)	−0.011 (2)	−0.013 (2)
O3	0.077 (4)	0.050 (3)	0.049 (3)	0.011 (3)	0.000 (3)	−0.024 (2)
O4	0.071 (4)	0.061 (4)	0.102 (5)	0.031 (3)	−0.032 (4)	−0.036 (4)
O5	0.044 (2)	0.045 (3)	0.042 (2)	0.001 (2)	−0.019 (2)	−0.005 (2)
O6	0.062 (3)	0.046 (3)	0.057 (3)	0.023 (2)	−0.034 (2)	−0.034 (2)
O7	0.055 (3)	0.116 (6)	0.053 (3)	−0.017 (3)	−0.013 (3)	−0.034 (3)
O8	0.061 (3)	0.049 (3)	0.048 (3)	0.002 (2)	0.004 (2)	−0.024 (2)
O9	0.101 (5)	0.043 (3)	0.082 (4)	−0.006 (3)	−0.046 (4)	−0.024 (3)
O10	0.081 (4)	0.055 (3)	0.042 (3)	−0.013 (3)	−0.031 (3)	−0.012 (2)
O11	0.076 (4)	0.040 (3)	0.091 (4)	0.002 (3)	−0.057 (4)	−0.001 (3)
O12	0.047 (3)	0.042 (2)	0.050 (3)	0.007 (2)	−0.012 (2)	−0.024 (2)
O13	0.063 (3)	0.053 (3)	0.058 (3)	0.000 (3)	−0.019 (3)	−0.017 (3)
O14	0.070 (4)	0.064 (4)	0.052 (3)	−0.007 (3)	−0.023 (3)	−0.017 (3)
O15	0.054 (3)	0.084 (4)	0.069 (4)	−0.004 (3)	−0.023 (3)	−0.038 (3)
O16	0.074 (4)	0.056 (3)	0.070 (4)	−0.009 (3)	−0.040 (3)	−0.010 (3)
O17	0.134 (7)	0.042 (3)	0.110 (6)	0.029 (4)	−0.025 (5)	−0.010 (4)
O18	0.086 (5)	0.172 (9)	0.087 (5)	0.039 (6)	−0.046 (4)	−0.071 (6)
O19	0.106 (6)	0.081 (5)	0.130 (7)	−0.024 (4)	0.000 (5)	−0.066 (5)
O20	0.096 (6)	0.167 (10)	0.092 (6)	0.049 (6)	−0.038 (5)	−0.015 (6)
O21	0.124 (13)	0.051 (7)	0.142 (15)	0.034 (8)	−0.086 (13)	−0.021 (9)
O22	0.070 (9)	0.039 (8)	0.044 (8)	−0.007 (8)	0.003 (8)	−0.010 (7)
N1	0.030 (2)	0.024 (2)	0.037 (2)	0.0049 (17)	−0.0166 (19)	−0.0161 (18)
N2	0.030 (2)	0.023 (2)	0.036 (2)	0.0074 (17)	−0.0170 (19)	−0.0164 (18)
N3	0.031 (2)	0.022 (2)	0.038 (2)	0.0064 (17)	−0.0187 (19)	−0.0146 (18)
N4	0.031 (2)	0.024 (2)	0.033 (2)	0.0049 (17)	−0.0153 (18)	−0.0134 (18)
N5	0.035 (3)	0.031 (2)	0.050 (3)	0.003 (2)	−0.014 (2)	−0.025 (2)
N6	0.033 (2)	0.033 (2)	0.047 (3)	0.0077 (19)	−0.020 (2)	−0.021 (2)
N7	0.037 (2)	0.023 (2)	0.038 (2)	0.0036 (18)	−0.013 (2)	−0.0129 (19)
N8	0.028 (2)	0.034 (2)	0.039 (3)	0.0050 (19)	−0.015 (2)	−0.008 (2)
C1	0.034 (3)	0.024 (2)	0.032 (3)	0.004 (2)	−0.017 (2)	−0.013 (2)
C2	0.033 (3)	0.028 (3)	0.041 (3)	0.007 (2)	−0.017 (2)	−0.020 (2)
C3	0.032 (3)	0.027 (3)	0.042 (3)	0.008 (2)	−0.017 (2)	−0.019 (2)
C4	0.032 (3)	0.022 (2)	0.034 (3)	0.0061 (19)	−0.016 (2)	−0.012 (2)
C5	0.031 (3)	0.027 (2)	0.035 (3)	0.006 (2)	−0.016 (2)	−0.013 (2)
C6	0.031 (3)	0.025 (2)	0.035 (3)	0.005 (2)	−0.017 (2)	−0.013 (2)
C7	0.031 (3)	0.031 (3)	0.038 (3)	0.004 (2)	−0.018 (2)	−0.013 (2)
C8	0.032 (3)	0.029 (3)	0.035 (3)	0.002 (2)	−0.017 (2)	−0.014 (2)
C9	0.029 (2)	0.026 (2)	0.033 (3)	0.004 (2)	−0.013 (2)	−0.015 (2)
C10	0.033 (3)	0.025 (2)	0.032 (3)	0.003 (2)	−0.014 (2)	−0.015 (2)
C11	0.032 (3)	0.023 (2)	0.031 (3)	0.0056 (19)	−0.016 (2)	−0.013 (2)
C12	0.037 (3)	0.023 (2)	0.039 (3)	0.005 (2)	−0.018 (2)	−0.013 (2)
C13	0.034 (3)	0.023 (2)	0.039 (3)	0.008 (2)	−0.020 (2)	−0.012 (2)
C14	0.033 (3)	0.027 (3)	0.034 (3)	0.008 (2)	−0.017 (2)	−0.015 (2)
C15	0.030 (3)	0.028 (3)	0.032 (3)	0.006 (2)	−0.014 (2)	−0.014 (2)
C16	0.027 (2)	0.030 (3)	0.033 (3)	0.005 (2)	−0.014 (2)	−0.015 (2)
C17	0.027 (3)	0.030 (3)	0.038 (3)	0.003 (2)	−0.015 (2)	−0.015 (2)
C18	0.034 (3)	0.031 (3)	0.035 (3)	0.000 (2)	−0.015 (2)	−0.013 (2)
C19	0.031 (3)	0.026 (2)	0.032 (3)	0.003 (2)	−0.016 (2)	−0.014 (2)
C20	0.033 (3)	0.027 (3)	0.034 (3)	0.003 (2)	−0.017 (2)	−0.013 (2)
C21	0.031 (3)	0.025 (2)	0.034 (3)	0.003 (2)	−0.017 (2)	−0.014 (2)
C22	0.033 (3)	0.024 (2)	0.036 (3)	0.005 (2)	−0.016 (2)	−0.010 (2)
C23	0.038 (3)	0.027 (3)	0.047 (3)	0.009 (2)	−0.023 (3)	−0.015 (2)
C24	0.033 (3)	0.032 (3)	0.040 (3)	−0.001 (2)	−0.014 (2)	−0.013 (2)
C25	0.033 (3)	0.028 (3)	0.037 (3)	0.004 (2)	−0.015 (2)	−0.011 (2)
C26	0.033 (3)	0.051 (4)	0.062 (4)	0.014 (3)	−0.026 (3)	−0.031 (3)
C27	0.032 (3)	0.024 (2)	0.034 (3)	0.004 (2)	−0.015 (2)	−0.014 (2)
C28	0.032 (3)	0.029 (3)	0.035 (3)	0.005 (2)	−0.011 (2)	−0.017 (2)
C29	0.031 (3)	0.028 (3)	0.040 (3)	0.004 (2)	−0.011 (2)	−0.014 (2)
C30	0.037 (3)	0.027 (3)	0.046 (3)	0.005 (2)	−0.013 (3)	−0.018 (2)
C31	0.032 (3)	0.029 (3)	0.040 (3)	0.002 (2)	−0.011 (2)	−0.017 (2)
C32	0.052 (4)	0.030 (3)	0.065 (4)	0.000 (3)	−0.014 (3)	−0.024 (3)
C33	0.027 (2)	0.026 (2)	0.035 (3)	0.003 (2)	−0.013 (2)	−0.011 (2)
C34	0.031 (3)	0.036 (3)	0.039 (3)	0.007 (2)	−0.014 (2)	−0.021 (2)
C35	0.034 (3)	0.035 (3)	0.043 (3)	0.007 (2)	−0.014 (3)	−0.016 (3)
C36	0.034 (3)	0.040 (3)	0.036 (3)	0.004 (2)	−0.018 (2)	−0.012 (2)
C37	0.033 (3)	0.036 (3)	0.039 (3)	0.008 (2)	−0.018 (2)	−0.020 (2)
C38	0.031 (3)	0.044 (3)	0.045 (3)	0.009 (2)	−0.017 (3)	−0.004 (3)
C39	0.029 (3)	0.027 (3)	0.039 (3)	0.006 (2)	−0.018 (2)	−0.015 (2)
C40	0.039 (3)	0.034 (3)	0.041 (3)	0.009 (2)	−0.022 (3)	−0.018 (2)
C41	0.037 (3)	0.041 (3)	0.049 (3)	0.009 (2)	−0.023 (3)	−0.028 (3)
C42	0.044 (3)	0.026 (3)	0.045 (3)	0.004 (2)	−0.015 (3)	−0.016 (2)
C43	0.042 (3)	0.030 (3)	0.042 (3)	0.007 (2)	−0.022 (3)	−0.014 (2)
C44	0.043 (4)	0.043 (4)	0.070 (5)	−0.010 (3)	−0.008 (3)	−0.033 (4)
C51	0.047 (4)	0.035 (3)	0.042 (3)	0.013 (3)	−0.009 (3)	−0.013 (3)
C52	0.054 (4)	0.036 (3)	0.038 (3)	0.011 (3)	−0.005 (3)	−0.011 (3)
C53	0.063 (4)	0.031 (3)	0.042 (3)	0.000 (3)	−0.005 (3)	−0.014 (3)
C54	0.044 (3)	0.034 (3)	0.042 (3)	0.000 (3)	−0.008 (3)	−0.016 (3)
C55	0.033 (3)	0.035 (3)	0.037 (3)	0.007 (2)	−0.015 (2)	−0.015 (2)
C56	0.042 (3)	0.031 (3)	0.031 (3)	0.006 (2)	−0.015 (2)	−0.013 (2)
C57	0.038 (3)	0.039 (3)	0.037 (3)	0.004 (2)	−0.011 (2)	−0.019 (3)
C58	0.040 (3)	0.045 (3)	0.042 (3)	0.011 (3)	−0.018 (3)	−0.022 (3)
C59	0.043 (3)	0.040 (3)	0.031 (3)	0.012 (3)	−0.013 (2)	−0.014 (2)
C60	0.045 (3)	0.032 (3)	0.032 (3)	0.006 (2)	−0.012 (2)	−0.012 (2)
C61	0.058 (4)	0.039 (3)	0.038 (3)	0.006 (3)	−0.017 (3)	−0.017 (3)
C62	0.049 (4)	0.047 (4)	0.034 (3)	0.003 (3)	−0.018 (3)	−0.013 (3)
C63	0.055 (4)	0.042 (3)	0.045 (3)	0.013 (3)	−0.027 (3)	−0.021 (3)
C64	0.065 (4)	0.040 (3)	0.049 (4)	0.016 (3)	−0.032 (3)	−0.023 (3)
C65	0.057 (4)	0.043 (3)	0.034 (3)	0.003 (3)	−0.017 (3)	−0.013 (3)
C66	0.048 (3)	0.040 (3)	0.031 (3)	−0.005 (3)	−0.015 (3)	−0.011 (2)
C67	0.056 (4)	0.041 (3)	0.041 (3)	−0.004 (3)	−0.020 (3)	−0.017 (3)
C68	0.055 (4)	0.039 (3)	0.048 (4)	0.005 (3)	−0.019 (3)	−0.023 (3)
C69	0.057 (4)	0.033 (3)	0.032 (3)	0.004 (3)	−0.015 (3)	−0.016 (2)
C70	0.056 (4)	0.034 (3)	0.032 (3)	0.009 (3)	−0.015 (3)	−0.007 (2)

Geometric parameters (Å, º)

S1—O1	1.449 (6)	C17—H17	0.9500
S1—O3	1.494 (7)	C17—C18	1.349 (8)
S1—O4	1.420 (8)	C18—H18	0.9500
S1—C52	1.803 (7)	C18—C19	1.462 (8)
S2—O2	1.447 (5)	C19—C20	1.400 (7)
S2—O5	1.449 (5)	C20—C39	1.491 (7)
S2—O6	1.454 (5)	C21—C22	1.400 (7)
S2—C56	1.785 (6)	C21—C25	1.389 (8)
S3—O7	1.435 (6)	C22—H22	0.9500
S3—O9	1.446 (6)	C22—C23	1.373 (8)
S3—O10	1.454 (5)	C23—H23	0.9500
S3—C66	1.772 (6)	C24—H24	0.9500
S4—O8	1.440 (5)	C24—C25	1.373 (8)
S4—O11	1.440 (5)	C25—H25	0.9500
S4—O12	1.447 (5)	C26—H26A	0.9800
S4—C62	1.775 (7)	C26—H26B	0.9800
S5—O3	1.128 (12)	C26—H26C	0.9800
S5—O4	2.090 (19)	C27—C28	1.397 (8)
S5—O22	1.43 (3)	C27—C31	1.396 (7)
S5—C52	1.851 (13)	C28—H28	0.9500
O13—H13A	0.877 (18)	C28—C29	1.373 (8)
O13—H13B	0.875 (18)	C29—H29	0.9500
O14—H14A	0.869 (19)	C30—H30	0.9500
O14—H14B	0.86 (2)	C30—C31	1.377 (8)
O15—H15A	0.87 (2)	C31—H31	0.9500
O15—H15B	0.87 (2)	C32—H32A	0.9800
O16—H16A	0.89 (2)	C32—H32B	0.9800
O16—H16B	1.03 (11)	C32—H32C	0.9800
O17—H17A	0.860 (2)	C33—C34	1.393 (8)
O18—H18A	0.86 (2)	C33—C37	1.398 (8)
O18—H18B	0.920 (5)	C34—H34	0.9500
O19—H19A	0.87 (2)	C34—C35	1.356 (8)
O19—H19B	0.866 (17)	C35—H35	0.9500
O20—H20A	0.8681	C36—H36	0.9500
O20—H20B	0.8703	C36—C37	1.372 (8)
O21—H21A	0.8690	C37—H37	0.9500
O21—H21B	0.8698	C38—H38A	0.9800
N1—H1	0.8800	C38—H38B	0.9800
N1—C1	1.376 (6)	C38—H38C	0.9800
N1—C4	1.361 (7)	C39—C40	1.404 (8)
N2—C6	1.368 (7)	C39—C43	1.385 (8)
N2—C9	1.366 (6)	C40—H40	0.9500
N3—H3	0.8800	C40—C41	1.362 (8)
N3—C11	1.358 (7)	C41—H41	0.9500
N3—C14	1.360 (7)	C42—H42	0.9500
N4—C16	1.363 (7)	C42—C43	1.381 (8)
N4—C19	1.364 (6)	C43—H43	0.9500
N5—C41	1.342 (9)	C44—H44A	0.9800
N5—C42	1.342 (8)	C44—H44B	0.9800
N5—C44	1.489 (7)	C44—H44C	0.9800
N6—C23	1.342 (8)	C51—H51	0.9500
N6—C24	1.346 (8)	C51—C52	1.343 (10)
N6—C26	1.476 (7)	C51—C59	1.422 (8)
N7—C29	1.348 (7)	C52—C53	1.411 (11)
N7—C30	1.339 (8)	C53—H53	0.9500
N7—C32	1.476 (7)	C53—C54	1.379 (10)
N8—C35	1.355 (8)	C54—H54	0.9500
N8—C36	1.352 (8)	C54—C60	1.413 (9)
N8—C38	1.478 (7)	C55—H55	0.9500
C1—C2	1.433 (7)	C55—C56	1.357 (8)
C1—C20	1.401 (8)	C55—C60	1.418 (8)
C2—H2	0.9500	C56—C57	1.424 (9)
C2—C3	1.356 (8)	C57—H57	0.9500
C3—H3A	0.9500	C57—C58	1.337 (9)
C3—C4	1.437 (7)	C58—H58	0.9500
C4—C5	1.408 (7)	C58—C59	1.412 (9)
C5—C6	1.410 (7)	C59—C60	1.432 (9)
C5—C21	1.479 (7)	C61—H61	0.9500
C6—C7	1.456 (7)	C61—C62	1.342 (10)
C7—H7	0.9500	C61—C69	1.439 (10)
C7—C8	1.335 (8)	C62—C63	1.439 (9)
C8—H8	0.9500	C63—H63	0.9500
C8—C9	1.457 (7)	C63—C64	1.364 (10)
C9—C10	1.408 (7)	C64—H64	0.9500
C10—C11	1.399 (7)	C64—C70	1.394 (10)
C10—C27	1.480 (7)	C65—H65	0.9500
C11—C12	1.441 (7)	C65—C66	1.373 (10)
C12—H12	0.9500	C65—C70	1.448 (10)
C12—C13	1.355 (8)	C66—C67	1.432 (9)
C13—H13	0.9500	C67—H67	0.9500
C13—C14	1.434 (7)	C67—C68	1.355 (9)
C14—C15	1.397 (7)	C68—H68	0.9500
C15—C16	1.401 (7)	C68—C69	1.385 (10)
C15—C33	1.486 (7)	C69—C70	1.418 (9)
C16—C17	1.467 (7)
O1—S1—O3	112.0 (4)	C24—C25—H25	119.8
O1—S1—C52	105.3 (4)	N6—C26—H26A	109.5
O3—S1—C52	102.3 (4)	N6—C26—H26B	109.5
O4—S1—O1	113.9 (5)	N6—C26—H26C	109.5
O4—S1—O3	113.3 (4)	H26A—C26—H26B	109.5
O4—S1—C52	109.0 (4)	H26A—C26—H26C	109.5
O2—S2—O5	113.3 (3)	H26B—C26—H26C	109.5
O2—S2—O6	113.6 (3)	C28—C27—C10	120.8 (5)
O2—S2—C56	106.8 (3)	C31—C27—C10	121.5 (5)
O5—S2—O6	110.9 (3)	C31—C27—C28	117.7 (5)
O5—S2—C56	106.1 (3)	C27—C28—H28	120.0
O6—S2—C56	105.4 (3)	C29—C28—C27	120.0 (5)
O7—S3—O9	113.3 (4)	C29—C28—H28	120.0
O7—S3—O10	113.3 (4)	N7—C29—C28	121.1 (5)
O7—S3—C66	107.8 (3)	N7—C29—H29	119.5
O9—S3—O10	110.6 (4)	C28—C29—H29	119.5
O9—S3—C66	106.7 (4)	N7—C30—H30	119.2
O10—S3—C66	104.5 (3)	N7—C30—C31	121.6 (5)
O8—S4—O12	112.2 (3)	C31—C30—H30	119.2
O8—S4—C62	104.2 (3)	C27—C31—H31	120.2
O11—S4—O8	113.7 (4)	C30—C31—C27	119.5 (5)
O11—S4—O12	113.0 (4)	C30—C31—H31	120.2
O11—S4—C62	104.7 (3)	N7—C32—H32A	109.5
O12—S4—C62	108.3 (3)	N7—C32—H32B	109.5
O3—S5—O4	93.5 (9)	N7—C32—H32C	109.5
O3—S5—O22	119.1 (18)	H32A—C32—H32B	109.5
O3—S5—C52	117.4 (8)	H32A—C32—H32C	109.5
O22—S5—O4	115 (2)	H32B—C32—H32C	109.5
O22—S5—C52	118.3 (16)	C34—C33—C15	121.7 (5)
C52—S5—O4	83.6 (7)	C34—C33—C37	117.6 (5)
H13A—O13—H13B	111 (10)	C37—C33—C15	120.7 (5)
H14A—O14—H14B	102 (10)	C33—C34—H34	119.7
H15A—O15—H15B	119 (10)	C35—C34—C33	120.5 (5)
H16A—O16—H16B	84 (9)	C35—C34—H34	119.7
H18A—O18—H18B	104 (3)	N8—C35—C34	121.0 (5)
H19A—O19—H19B	107 (3)	N8—C35—H35	119.5
H20A—O20—H20B	104.5	C34—C35—H35	119.5
H21A—O21—H21B	104.6	N8—C36—H36	119.7
C1—N1—H1	125.0	N8—C36—C37	120.6 (5)
C4—N1—H1	125.0	C37—C36—H36	119.7
C4—N1—C1	109.9 (4)	C33—C37—H37	119.9
C9—N2—C6	105.4 (4)	C36—C37—C33	120.1 (5)
C11—N3—H3	125.0	C36—C37—H37	119.9
C11—N3—C14	109.9 (4)	N8—C38—H38A	109.5
C14—N3—H3	125.0	N8—C38—H38B	109.5
C16—N4—C19	105.8 (4)	N8—C38—H38C	109.5
C41—N5—C42	120.5 (5)	H38A—C38—H38B	109.5
C41—N5—C44	119.2 (6)	H38A—C38—H38C	109.5
C42—N5—C44	120.3 (6)	H38B—C38—H38C	109.5
C23—N6—C24	120.5 (5)	C40—C39—C20	120.6 (5)
C23—N6—C26	119.5 (5)	C43—C39—C20	121.6 (5)
C24—N6—C26	119.9 (5)	C43—C39—C40	117.7 (5)
C29—N7—C32	119.8 (5)	C39—C40—H40	120.2
C30—N7—C29	120.0 (5)	C41—C40—C39	119.7 (6)
C30—N7—C32	120.2 (5)	C41—C40—H40	120.2
C35—N8—C38	121.0 (5)	N5—C41—C40	121.3 (6)
C36—N8—C35	120.1 (5)	N5—C41—H41	119.4
C36—N8—C38	119.0 (5)	C40—C41—H41	119.4
N1—C1—C2	106.7 (5)	N5—C42—H42	119.8
N1—C1—C20	125.5 (5)	N5—C42—C43	120.5 (6)
C20—C1—C2	127.7 (5)	C43—C42—H42	119.8
C1—C2—H2	125.8	C39—C43—H43	120.0
C3—C2—C1	108.3 (5)	C42—C43—C39	120.0 (6)
C3—C2—H2	125.8	C42—C43—H43	120.0
C2—C3—H3A	126.2	N5—C44—H44A	109.5
C2—C3—C4	107.6 (5)	N5—C44—H44B	109.5
C4—C3—H3A	126.2	N5—C44—H44C	109.5
N1—C4—C3	107.4 (4)	H44A—C44—H44B	109.5
N1—C4—C5	125.5 (5)	H44A—C44—H44C	109.5
C5—C4—C3	127.0 (5)	H44B—C44—H44C	109.5
C4—C5—C6	124.2 (5)	C52—C51—H51	119.9
C4—C5—C21	117.9 (5)	C52—C51—C59	120.3 (7)
C6—C5—C21	117.8 (5)	C59—C51—H51	119.9
N2—C6—C5	124.9 (5)	C51—C52—S1	118.0 (6)
N2—C6—C7	110.3 (4)	C51—C52—S5	136.2 (7)
C5—C6—C7	124.8 (5)	C51—C52—C53	122.4 (6)
C6—C7—H7	126.5	C53—C52—S1	119.5 (5)
C8—C7—C6	107.0 (5)	C53—C52—S5	99.4 (7)
C8—C7—H7	126.5	C52—C53—H53	120.6
C7—C8—H8	126.7	C54—C53—C52	118.8 (6)
C7—C8—C9	106.5 (5)	C54—C53—H53	120.6
C9—C8—H8	126.7	C53—C54—H54	119.5
N2—C9—C8	110.6 (4)	C53—C54—C60	121.0 (7)
N2—C9—C10	124.9 (5)	C60—C54—H54	119.5
C10—C9—C8	124.5 (5)	C56—C55—H55	119.9
C9—C10—C27	118.4 (5)	C56—C55—C60	120.1 (6)
C11—C10—C9	125.2 (5)	C60—C55—H55	119.9
C11—C10—C27	116.4 (5)	C55—C56—S2	120.9 (5)
N3—C11—C10	125.6 (5)	C55—C56—C57	121.7 (5)
N3—C11—C12	107.3 (4)	C57—C56—S2	117.3 (4)
C10—C11—C12	127.1 (5)	C56—C57—H57	120.4
C11—C12—H12	126.3	C58—C57—C56	119.1 (6)
C13—C12—C11	107.4 (5)	C58—C57—H57	120.4
C13—C12—H12	126.3	C57—C58—H58	119.1
C12—C13—H13	126.1	C57—C58—C59	121.8 (6)
C12—C13—C14	107.9 (5)	C59—C58—H58	119.1
C14—C13—H13	126.1	C51—C59—C60	118.6 (6)
N3—C14—C13	107.3 (5)	C58—C59—C51	122.2 (6)
N3—C14—C15	125.3 (5)	C58—C59—C60	119.2 (6)
C15—C14—C13	127.4 (5)	C54—C60—C55	123.1 (6)
C14—C15—C16	124.6 (5)	C54—C60—C59	118.9 (6)
C14—C15—C33	116.7 (5)	C55—C60—C59	118.0 (6)
C16—C15—C33	118.7 (5)	C62—C61—H61	119.1
N4—C16—C15	125.2 (5)	C62—C61—C69	121.8 (6)
N4—C16—C17	110.4 (5)	C69—C61—H61	119.1
C15—C16—C17	124.4 (5)	C61—C62—S4	123.0 (6)
C16—C17—H17	126.8	C61—C62—C63	121.1 (6)
C18—C17—C16	106.4 (5)	C63—C62—S4	115.7 (5)
C18—C17—H17	126.8	C62—C63—H63	120.8
C17—C18—H18	126.8	C64—C63—C62	118.5 (7)
C17—C18—C19	106.3 (5)	C64—C63—H63	120.8
C19—C18—H18	126.8	C63—C64—H64	119.6
N4—C19—C18	110.7 (5)	C63—C64—C70	120.8 (6)
N4—C19—C20	125.3 (5)	C70—C64—H64	119.6
C20—C19—C18	123.9 (5)	C66—C65—H65	120.2
C1—C20—C39	118.4 (5)	C66—C65—C70	119.6 (6)
C19—C20—C1	125.4 (5)	C70—C65—H65	120.2
C19—C20—C39	116.1 (5)	C65—C66—S3	120.9 (5)
C22—C21—C5	121.8 (5)	C65—C66—C67	120.0 (6)
C25—C21—C5	120.2 (5)	C67—C66—S3	118.9 (5)
C25—C21—C22	117.9 (5)	C66—C67—H67	119.7
C21—C22—H22	120.3	C68—C67—C66	120.5 (7)
C23—C22—C21	119.3 (5)	C68—C67—H67	119.7
C23—C22—H22	120.3	C67—C68—H68	119.6
N6—C23—C22	121.4 (5)	C67—C68—C69	120.9 (6)
N6—C23—H23	119.3	C69—C68—H68	119.6
C22—C23—H23	119.3	C68—C69—C61	123.5 (6)
N6—C24—H24	119.8	C68—C69—C70	120.8 (6)
N6—C24—C25	120.4 (5)	C70—C69—C61	115.6 (6)
C25—C24—H24	119.8	C64—C70—C65	119.8 (6)
C21—C25—H25	119.8	C64—C70—C69	122.1 (7)
C24—C25—C21	120.4 (5)	C69—C70—C65	118.0 (6)
S1—C52—C53—C54	175.5 (5)	C14—N3—C11—C10	175.1 (5)
S2—C56—C57—C58	179.8 (5)	C14—N3—C11—C12	−4.2 (6)
S3—C66—C67—C68	171.6 (5)	C14—C15—C16—N4	−12.4 (9)
S4—C62—C63—C64	175.9 (5)	C14—C15—C16—C17	169.3 (5)
S5—C52—C53—C54	165.7 (7)	C14—C15—C33—C34	−50.5 (8)
O1—S1—C52—C51	−135.2 (6)	C14—C15—C33—C37	126.3 (6)
O1—S1—C52—C53	48.4 (7)	C15—C16—C17—C18	175.7 (5)
O2—S2—C56—C55	−19.2 (6)	C15—C33—C34—C35	173.1 (5)
O2—S2—C56—C57	162.8 (5)	C15—C33—C37—C36	−173.7 (5)
O3—S1—C52—C51	107.6 (6)	C16—N4—C19—C18	−5.0 (6)
O3—S1—C52—C53	−68.8 (6)	C16—N4—C19—C20	172.9 (5)
O3—S5—C52—C51	62.0 (18)	C16—C15—C33—C34	131.9 (6)
O3—S5—C52—C53	−101.4 (13)	C16—C15—C33—C37	−51.3 (8)
O4—S1—C52—C51	−12.6 (7)	C16—C17—C18—C19	−0.3 (6)
O4—S1—C52—C53	171.0 (6)	C17—C18—C19—N4	3.4 (6)
O4—S5—C52—C51	−28.6 (10)	C17—C18—C19—C20	−174.6 (5)
O4—S5—C52—C53	168.0 (5)	C18—C19—C20—C1	−169.3 (5)
O5—S2—C56—C55	101.9 (5)	C18—C19—C20—C39	9.2 (8)
O5—S2—C56—C57	−76.1 (5)	C19—N4—C16—C15	−173.7 (5)
O6—S2—C56—C55	−140.4 (5)	C19—N4—C16—C17	4.8 (6)
O6—S2—C56—C57	41.7 (5)	C19—C20—C39—C40	55.6 (7)
O7—S3—C66—C65	−131.8 (6)	C19—C20—C39—C43	−120.5 (6)
O7—S3—C66—C67	53.4 (6)	C20—C1—C2—C3	−177.5 (6)
O8—S4—C62—C61	101.8 (6)	C20—C39—C40—C41	−171.1 (5)
O8—S4—C62—C63	−73.9 (6)	C20—C39—C43—C42	170.4 (6)
O9—S3—C66—C65	−9.8 (6)	C21—C5—C6—N2	163.6 (5)
O9—S3—C66—C67	175.4 (5)	C21—C5—C6—C7	−15.3 (8)
O10—S3—C66—C65	107.4 (6)	C21—C22—C23—N6	0.4 (9)
O10—S3—C66—C67	−67.4 (6)	C22—C21—C25—C24	2.8 (8)
O11—S4—C62—C61	−138.6 (6)	C23—N6—C24—C25	−1.5 (9)
O11—S4—C62—C63	45.7 (6)	C24—N6—C23—C22	1.7 (9)
O12—S4—C62—C61	−17.8 (7)	C25—C21—C22—C23	−2.6 (8)
O12—S4—C62—C63	166.5 (5)	C26—N6—C23—C22	−174.5 (5)
O22—S5—C52—C51	−144 (2)	C26—N6—C24—C25	174.7 (5)
O22—S5—C52—C53	53 (2)	C27—C10—C11—N3	−169.6 (5)
N1—C1—C2—C3	1.0 (7)	C27—C10—C11—C12	9.6 (8)
N1—C1—C20—C19	7.4 (9)	C27—C28—C29—N7	−0.4 (9)
N1—C1—C20—C39	−171.0 (5)	C28—C27—C31—C30	1.8 (9)
N1—C4—C5—C6	−8.1 (9)	C29—N7—C30—C31	0.5 (9)
N1—C4—C5—C21	175.5 (5)	C30—N7—C29—C28	0.5 (9)
N2—C6—C7—C8	−2.0 (7)	C31—C27—C28—C29	−0.8 (8)
N2—C9—C10—C11	13.0 (9)	C32—N7—C29—C28	−179.0 (6)
N2—C9—C10—C27	−166.5 (5)	C32—N7—C30—C31	−180.0 (6)
N3—C11—C12—C13	2.2 (6)	C33—C15—C16—N4	165.1 (5)
N3—C14—C15—C16	−9.4 (9)	C33—C15—C16—C17	−13.3 (8)
N3—C14—C15—C33	173.1 (5)	C33—C34—C35—N8	1.7 (9)
N4—C16—C17—C18	−2.8 (6)	C34—C33—C37—C36	3.2 (9)
N4—C19—C20—C1	13.1 (9)	C35—N8—C36—C37	−1.7 (9)
N4—C19—C20—C39	−168.4 (5)	C36—N8—C35—C34	1.2 (9)
N5—C42—C43—C39	1.4 (9)	C37—C33—C34—C35	−3.8 (9)
N6—C24—C25—C21	−0.8 (9)	C38—N8—C35—C34	−177.3 (6)
N7—C30—C31—C27	−1.7 (9)	C38—N8—C36—C37	176.7 (6)
N8—C36—C37—C33	−0.5 (9)	C39—C40—C41—N5	0.1 (9)
C1—N1—C4—C3	2.3 (6)	C40—C39—C43—C42	−5.8 (9)
C1—N1—C4—C5	−175.0 (5)	C41—N5—C42—C43	4.0 (9)
C1—C2—C3—C4	0.4 (7)	C42—N5—C41—C40	−4.7 (9)
C1—C20—C39—C40	−125.8 (6)	C43—C39—C40—C41	5.0 (9)
C1—C20—C39—C43	58.1 (8)	C44—N5—C41—C40	172.8 (6)
C2—C1—C20—C19	−174.3 (6)	C44—N5—C42—C43	−173.6 (6)
C2—C1—C20—C39	7.3 (9)	C51—C52—C53—C54	−0.8 (11)
C2—C3—C4—N1	−1.6 (7)	C51—C59—C60—C54	−0.1 (9)
C2—C3—C4—C5	175.6 (6)	C51—C59—C60—C55	179.9 (6)
C3—C4—C5—C6	175.2 (6)	C52—C51—C59—C58	177.3 (6)
C3—C4—C5—C21	−1.3 (9)	C52—C51—C59—C60	−2.0 (9)
C4—N1—C1—C2	−2.1 (6)	C52—C53—C54—C60	−1.3 (10)
C4—N1—C1—C20	176.5 (5)	C53—C54—C60—C55	−178.3 (6)
C4—C5—C6—N2	−12.9 (9)	C53—C54—C60—C59	1.7 (10)
C4—C5—C6—C7	168.3 (6)	C55—C56—C57—C58	1.8 (9)
C4—C5—C21—C22	−52.0 (8)	C56—C55—C60—C54	178.6 (6)
C4—C5—C21—C25	124.7 (6)	C56—C55—C60—C59	−1.4 (9)
C5—C6—C7—C8	176.9 (5)	C56—C57—C58—C59	−2.7 (9)
C5—C21—C22—C23	174.2 (5)	C57—C58—C59—C51	−177.8 (6)
C5—C21—C25—C24	−174.1 (5)	C57—C58—C59—C60	1.4 (9)
C6—N2—C9—C8	−4.8 (6)	C58—C59—C60—C54	−179.3 (6)
C6—N2—C9—C10	172.5 (5)	C58—C59—C60—C55	0.7 (9)
C6—C5—C21—C22	131.3 (6)	C59—C51—C52—S1	−173.9 (5)
C6—C5—C21—C25	−52.0 (7)	C59—C51—C52—S5	−158.1 (8)
C6—C7—C8—C9	−1.0 (6)	C59—C51—C52—C53	2.5 (10)
C7—C8—C9—N2	3.7 (7)	C60—C55—C56—S2	−177.6 (4)
C7—C8—C9—C10	−173.6 (5)	C60—C55—C56—C57	0.2 (9)
C8—C9—C10—C11	−170.1 (5)	C61—C62—C63—C64	0.2 (10)
C8—C9—C10—C27	10.5 (8)	C61—C69—C70—C64	−0.7 (9)
C9—N2—C6—C5	−174.7 (5)	C61—C69—C70—C65	176.2 (6)
C9—N2—C6—C7	4.2 (6)	C62—C61—C69—C68	177.1 (7)
C9—C10—C11—N3	10.9 (9)	C62—C61—C69—C70	−1.0 (9)
C9—C10—C11—C12	−169.9 (5)	C62—C63—C64—C70	−1.9 (10)
C9—C10—C27—C28	50.8 (8)	C63—C64—C70—C65	−174.7 (6)
C9—C10—C27—C31	−129.0 (6)	C63—C64—C70—C69	2.2 (10)
C10—C11—C12—C13	−177.1 (5)	C65—C66—C67—C68	−3.3 (10)
C10—C27—C28—C29	179.4 (5)	C66—C65—C70—C64	175.4 (6)
C10—C27—C31—C30	−178.4 (5)	C66—C65—C70—C69	−1.6 (9)
C11—N3—C14—C13	4.5 (6)	C66—C67—C68—C69	−0.3 (10)
C11—N3—C14—C15	−176.0 (5)	C67—C68—C69—C61	−175.1 (6)
C11—C10—C27—C28	−128.7 (6)	C67—C68—C69—C70	2.9 (10)
C11—C10—C27—C31	51.5 (8)	C68—C69—C70—C64	−178.9 (6)
C11—C12—C13—C14	0.5 (6)	C68—C69—C70—C65	−1.9 (9)
C12—C13—C14—N3	−3.0 (6)	C69—C61—C62—S4	−174.1 (5)
C12—C13—C14—C15	177.5 (6)	C69—C61—C62—C63	1.3 (10)
C13—C14—C15—C16	170.0 (6)	C70—C65—C66—S3	−170.6 (5)
C13—C14—C15—C33	−7.5 (9)	C70—C65—C66—C67	4.2 (9)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O13—H13A···O18	0.88 (2)	1.92 (2)	2.771 (9)	164 (8)
O13—H13B···O10	0.88 (2)	1.91 (2)	2.766 (8)	166 (8)
O14—H14A···O7	0.87 (2)	2.01 (2)	2.840 (10)	160 (7)
O14—H14B···O15	0.86 (2)	2.09 (5)	2.907 (9)	157 (11)
O15—H15A···O13	0.87 (2)	1.87 (2)	2.737 (9)	178 (12)
O15—H15B···O16	0.87 (2)	1.92 (4)	2.747 (8)	159 (11)
O16—H16A···O12^i	0.89 (2)	2.10 (2)	2.978 (8)	174 (12)
O16—H16B···O15^ii	1.03 (11)	1.93 (9)	2.808 (10)	141 (9)
O17—H17A···O1	0.86 (1)	1.88 (2)	2.713 (9)	164 (7)
O18—H18A···O3^iii	0.86 (2)	2.06 (6)	2.792 (11)	142 (9)
O18—H18B···O19^iii	0.92 (1)	1.98 (2)	2.822 (14)	152 (4)
O19—H19A···O17	0.87 (2)	1.81 (2)	2.654 (14)	163 (9)
O19—H19B···O6^iv	0.87 (2)	2.10 (2)	2.961 (9)	172 (11)
O20—H20A···O21^v	0.87	2.22	2.92 (2)	138
O20—H20A···O21	0.87	2.06	2.67 (2)	127
O20—H20B···O18	0.87	1.92	2.740 (13)	157
N1—H1···N2	0.88	2.34	2.884 (6)	121

Symmetry codes: (i) −x+1, −y, −z; (ii) −x+2, −y, −z; (iii) −x+1, −y+1, −z+1; (iv) x, y+1, z; (v) −x+1, −y, −z+1.

(TMPyP)(1-naphthalenesulfonate)4

Crystal data

4(C10H7O3S)·O·H2O·2(C22H19N4)·0.5[]	Z = 2
Mr = 1541.70	F(000) = 1608
Triclinic, P1	Dx = 1.303 Mg m^−3
a = 15.19786 (17) Å	Cu Kα radiation, λ = 1.54184 Å
b = 17.1894 (2) Å	Cell parameters from 22312 reflections
c = 17.9323 (2) Å	θ = 2.8–79.1°
α = 116.0657 (13)°	µ = 1.69 mm^−1
β = 94.3459 (11)°	T = 160 K
γ = 106.3405 (11)°	Plate, red
V = 3928.68 (10) Å^3	0.10 × 0.06 × 0.03 mm

Data collection

XtaLAB Synergy, Dualflex, HyPix diffractometer	16109 independent reflections
Radiation source: micro-focus sealed X-ray tube, PhotonJet (Cu) X-ray Source	12127 reflections with I > 2σ(I)
Mirror monochromator	Rint = 0.033
Detector resolution: 10.0000 pixels mm^-1	θmax = 79.5°, θmin = 2.8°
ω scans	h = −19→19
Absorption correction: gaussian CrysAlisPro 1.171.43.130a (Rigaku Oxford Diffraction, 2024) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	k = −21→13
Tmin = 0.860, Tmax = 1.000	l = −20→22
61206 measured reflections

Refinement

Refinement on F^2	47 restraints
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.075	H-atom parameters constrained
wR(F^2) = 0.228	w = 1/[σ^2(Fo^2) + (0.1202P)^2 + 3.1423P] where P = (Fo^2 + 2Fc^2)/3
S = 1.05	(Δ/σ)max = 0.001
16109 reflections	Δρmax = 1.25 e Å^−3
1141 parameters	Δρmin = −0.64 e Å^−3

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	Occ. (<1)
S61	0.69727 (6)	0.39859 (8)	0.42652 (6)	0.0688 (3)
O61	0.7564 (2)	0.4730 (3)	0.50740 (19)	0.0955 (10)
O62	0.6005 (2)	0.3930 (3)	0.4159 (2)	0.1066 (12)
O63	0.7049 (2)	0.3109 (2)	0.40826 (19)	0.0794 (8)
C61	0.7418 (3)	0.4246 (3)	0.3478 (2)	0.0642 (9)
C62	0.6831 (4)	0.4388 (3)	0.2978 (3)	0.0946 (15)
H62	0.621283	0.435877	0.305563	0.113*
C63	0.7163 (8)	0.4582 (5)	0.2337 (4)	0.141 (3)
H63	0.675910	0.467165	0.197581	0.169*
C64	0.8047 (8)	0.4641 (4)	0.2235 (4)	0.142 (4)
H64	0.825149	0.477698	0.180406	0.171*
C65	0.9654 (6)	0.4593 (3)	0.2688 (4)	0.124 (3)
H65	0.988611	0.472492	0.226417	0.149*
C66	1.0219 (5)	0.4492 (4)	0.3210 (5)	0.122 (3)
H66	1.084688	0.455113	0.314974	0.147*
C67	0.9923 (3)	0.4304 (3)	0.3840 (3)	0.0843 (14)
H67	1.034648	0.424120	0.420947	0.101*
C68	0.9013 (3)	0.4206 (2)	0.3933 (2)	0.0626 (9)
H68	0.881386	0.406734	0.436389	0.075*
C69	0.8369 (3)	0.4307 (2)	0.3399 (2)	0.0610 (9)
C70	0.8679 (4)	0.4505 (3)	0.2749 (3)	0.0922 (17)
S71	0.58489 (13)	0.69685 (14)	0.93654 (11)	0.0488 (5)	0.664 (4)
S72	0.5404 (2)	0.6469 (2)	0.90226 (19)	0.0409 (7)	0.336 (4)
O71	0.5280 (3)	0.7466 (3)	0.9843 (3)	0.0742 (12)	0.664 (4)
O72	0.5754 (5)	0.6137 (4)	0.9427 (4)	0.0531 (13)	0.664 (4)
O73	0.5718 (3)	0.6816 (4)	0.8496 (3)	0.0636 (11)	0.664 (4)
O74	0.4604 (6)	0.6705 (7)	0.9322 (6)	0.073 (3)	0.336 (4)
O75	0.5564 (8)	0.5768 (6)	0.9192 (8)	0.049 (2)	0.336 (4)
O76	0.5349 (5)	0.6238 (5)	0.8146 (5)	0.0500 (17)	0.336 (4)
C71	0.7074 (4)	0.7719 (3)	0.9886 (3)	0.0447 (11)	0.664 (4)
C71B	0.6510 (10)	0.7499 (8)	0.9679 (7)	0.054 (2)*	0.336 (4)
C72	0.7250 (5)	0.8533 (4)	1.0635 (3)	0.0561 (13)	0.664 (4)
H72	0.674579	0.872546	1.083116	0.067*	0.664 (4)
C72B	0.6251 (10)	0.8216 (9)	1.0289 (9)	0.080 (3)*	0.336 (4)
H72B	0.560780	0.815774	1.026369	0.096*	0.336 (4)
C73	0.8188 (5)	0.9073 (3)	1.1103 (4)	0.0578 (13)	0.664 (4)
H73	0.830668	0.961914	1.162838	0.069*	0.664 (4)
C73B	0.6927 (14)	0.8963 (14)	1.0890 (13)	0.110 (5)*	0.336 (4)
H73B	0.677200	0.944309	1.131633	0.131*	0.336 (4)
C74	0.8897 (4)	0.8844 (3)	1.0836 (3)	0.0576 (13)	0.664 (4)
H74	0.952334	0.921716	1.116393	0.069*	0.664 (4)
C74B	0.7758 (12)	0.9040 (11)	1.0899 (9)	0.060 (3)*	0.336 (4)
H74B	0.823321	0.958885	1.133221	0.072*	0.336 (4)
C75	0.9479 (6)	0.7804 (5)	0.9779 (5)	0.0633 (17)	0.664 (4)
H75	1.009588	0.820294	1.011593	0.076*	0.664 (4)
C76	0.9361 (3)	0.7026 (4)	0.9042 (3)	0.0530 (12)	0.664 (4)
H76	0.989429	0.688286	0.886240	0.064*	0.664 (4)
C77	0.8433 (3)	0.6424 (3)	0.8539 (3)	0.0449 (10)	0.664 (4)
H77	0.835779	0.588437	0.802146	0.054*	0.664 (4)
C78	0.7667 (4)	0.6602 (4)	0.8777 (4)	0.0446 (13)	0.664 (4)
H78	0.705376	0.619185	0.844002	0.054*	0.664 (4)
C79	0.7796 (3)	0.7434 (3)	0.9560 (3)	0.0432 (10)	0.664 (4)
C79B	0.7344 (5)	0.7485 (6)	0.9584 (6)	0.055 (3)*	0.336 (4)
C80B	0.8068 (7)	0.8259 (6)	1.0218 (6)	0.093 (4)*	0.336 (4)
C75B	0.9001 (6)	0.8330 (7)	1.0213 (7)	0.084 (6)*	0.336 (4)
H75B	0.949546	0.885899	1.064682	0.101*	0.336 (4)
C76B	0.9210 (6)	0.7626 (9)	0.9574 (8)	0.096 (9)*	0.336 (4)
H76B	0.984748	0.767389	0.957056	0.116*	0.336 (4)
C77B	0.8486 (8)	0.6851 (7)	0.8940 (7)	0.079 (4)*	0.336 (4)
H77B	0.862866	0.637018	0.850270	0.095*	0.336 (4)
C78B	0.7553 (7)	0.6781 (6)	0.8945 (6)	0.054 (5)*	0.336 (4)
H78B	0.705780	0.625157	0.851110	0.064*	0.336 (4)
C80	0.8723 (5)	0.8017 (4)	1.0039 (4)	0.0542 (13)	0.664 (4)
S81	0.22980 (10)	0.15180 (13)	0.59209 (9)	0.0693 (5)	0.653 (3)
S82	0.23366 (18)	0.24064 (18)	0.62359 (17)	0.0589 (8)*	0.347 (3)
O81	0.2967 (2)	0.2151 (3)	0.5723 (2)	0.0979 (11)
O82	0.1992 (2)	0.1878 (2)	0.66559 (17)	0.0759 (7)
O83	0.2620 (4)	0.0730 (5)	0.5833 (3)	0.1042 (19)	0.653 (3)
O84	0.2782 (5)	0.3346 (5)	0.6928 (5)	0.0693 (19)*	0.347 (3)
C81	0.1281 (4)	0.0996 (4)	0.5068 (3)	0.0539 (12)	0.653 (3)
C81B	0.1368 (9)	0.2375 (9)	0.5622 (8)	0.059 (3)*	0.347 (3)
C82	0.0999 (4)	0.0089 (4)	0.4516 (4)	0.0617 (13)	0.653 (3)
H82	0.135095	−0.025865	0.459097	0.074*	0.653 (3)
C82B	0.1215 (8)	0.3201 (8)	0.5825 (7)	0.058 (2)*	0.347 (3)
H82B	0.164394	0.376013	0.628758	0.070*	0.347 (3)
C83	0.0246 (7)	−0.0345 (7)	0.3868 (5)	0.066 (2)	0.653 (3)
H83	0.009006	−0.098732	0.349413	0.079*	0.653 (3)
C83B	0.0435 (13)	0.3230 (13)	0.5359 (12)	0.073 (5)*	0.347 (3)
H83B	0.041471	0.382700	0.551213	0.088*	0.347 (3)
C84	−0.0307 (6)	0.0093 (6)	0.3720 (6)	0.064 (2)	0.653 (3)
H84	−0.084216	−0.022966	0.325424	0.077*	0.653 (3)
C84B	−0.0639 (11)	0.0783 (10)	0.3683 (10)	0.088 (4)*	0.347 (3)
H84B	−0.111151	0.081713	0.333282	0.105*	0.347 (3)
C85	−0.0606 (5)	0.1576 (5)	0.4190 (4)	0.0696 (16)	0.653 (3)
H85	−0.117371	0.126763	0.376046	0.084*	0.653 (3)
C85B	−0.0558 (17)	0.0051 (19)	0.3527 (16)	0.091 (8)*	0.347 (3)
H85B	−0.105630	−0.047911	0.309796	0.109*	0.347 (3)
C86	−0.0297 (4)	0.2490 (4)	0.4709 (3)	0.0921 (14)
H86A	−0.086967	0.251351	0.448352	0.111*	0.347 (3)
H86	−0.062676	0.283366	0.459217	0.111*	0.653 (3)
C86B	0.0122 (19)	−0.0123 (14)	0.3863 (15)	0.073 (6)*	0.347 (3)
H86B	0.015025	−0.072675	0.363851	0.088*	0.347 (3)
C87	0.0456 (7)	0.2968 (6)	0.5396 (5)	0.081 (3)	0.653 (3)
H87	0.059198	0.360505	0.577621	0.097*	0.653 (3)
C87B	0.0838 (11)	0.0688 (10)	0.4617 (10)	0.077 (3)*	0.347 (3)
H87B	0.135899	0.061259	0.486850	0.093*	0.347 (3)
C88	0.1018 (5)	0.2511 (4)	0.5530 (4)	0.0588 (14)	0.653 (3)
H88	0.155971	0.282653	0.598884	0.071*	0.653 (3)
C88B	−0.0008 (10)	0.1587 (10)	0.4405 (8)	0.065 (3)*	0.347 (3)
C89	0.0751 (2)	0.1547 (2)	0.4950 (2)	0.0564 (8)
C90	−0.0047 (4)	0.1089 (4)	0.4310 (3)	0.0504 (11)	0.653 (3)
S91	0.4483 (2)	0.98470 (17)	1.25004 (17)	0.0911 (7)	0.637 (4)
S92	0.46734 (18)	0.9573 (2)	1.22524 (18)	0.0452 (6)*	0.363 (4)
O14	0.4633 (7)	1.0402 (7)	1.2301 (7)	0.078 (3)*	0.363 (4)
O91	0.4769 (4)	0.9913 (5)	1.1749 (5)	0.119 (3)	0.637 (4)
O92	0.4912 (4)	0.9233 (4)	1.2675 (5)	0.099 (2)	0.637 (4)
O94	0.4644 (8)	0.9548 (7)	1.3043 (7)	0.085 (3)*	0.363 (4)
O95	0.5408 (7)	0.9298 (6)	1.1855 (6)	0.091 (3)*	0.363 (4)
O96	0.4717 (6)	1.0712 (4)	1.3178 (5)	0.173 (4)	0.637 (4)
C91B	0.3584 (7)	0.8652 (7)	1.1575 (6)	0.055 (2)*	0.363 (4)
C92B	0.3589 (9)	0.7862 (9)	1.0892 (9)	0.048 (3)*	0.363 (4)
H92B	0.420096	0.785727	1.082091	0.057*	0.363 (4)
C97	0.2844 (3)	0.7050 (3)	1.0273 (3)	0.0700 (10)
H97A	0.291636	0.652973	0.981989	0.084*	0.363 (4)
H97	0.320134	0.670889	0.995004	0.084*	0.637 (4)
C94B	0.1914 (10)	0.7155 (10)	1.0458 (9)	0.071 (3)*	0.363 (4)
H94B	0.134719	0.666133	1.009789	0.085*	0.363 (4)
C95	0.1381 (4)	0.7161 (4)	1.0478 (4)	0.0620 (16)	0.637 (4)
H95	0.071172	0.692417	1.031583	0.074*	0.637 (4)
C95B	0.1001 (16)	0.8013 (13)	1.1287 (12)	0.117 (6)*	0.363 (4)
H95B	0.044351	0.752010	1.090530	0.141*	0.363 (4)
C96	0.1879 (5)	0.6660 (4)	1.0004 (4)	0.0657 (17)	0.637 (4)
H96	0.157567	0.607265	0.951299	0.079*	0.637 (4)
C96B	0.0989 (12)	0.8769 (10)	1.1967 (10)	0.101 (5)*	0.363 (4)
H96B	0.038571	0.879009	1.205436	0.121*	0.363 (4)
C97B	0.2645 (10)	0.9494 (11)	1.2459 (10)	0.077 (4)*	0.363 (4)
H97B	0.319476	0.998395	1.285704	0.093*	0.363 (4)
C98	0.3316 (5)	0.7868 (5)	1.0950 (4)	0.0493 (16)	0.637 (4)
H98	0.398544	0.808904	1.109876	0.059*	0.637 (4)
C98B	0.2715 (9)	0.8734 (8)	1.1766 (8)	0.065 (3)*	0.363 (4)
C100	0.18446 (16)	0.80156 (19)	1.11953 (18)	0.0541 (8)
C94	0.1301 (2)	0.8492 (3)	1.1659 (3)	0.084 (2)	0.637 (4)
H94	0.063265	0.822719	1.148738	0.101*	0.637 (4)
C93	0.1735 (4)	0.9356 (3)	1.2374 (3)	0.102 (3)	0.637 (4)
H93	0.136294	0.968148	1.269154	0.122*	0.637 (4)
C92	0.2712 (4)	0.9743 (2)	1.2626 (2)	0.086 (3)	0.637 (4)
H92	0.300870	1.033374	1.311473	0.103*	0.637 (4)
C91	0.3256 (2)	0.9267 (2)	1.2162 (2)	0.0530 (12)	0.637 (4)
C99	0.28222 (15)	0.84030 (19)	1.14467 (18)	0.0359 (9)	0.637 (4)
O108	0.5310 (3)	0.9461 (4)	1.0261 (3)	0.174 (3)
O109	0.7018 (3)	0.9585 (3)	1.2768 (3)	0.1184 (13)
H10A	0.693679	0.940573	1.314920	0.178*
H10B	0.646507	0.956712	1.257750	0.178*
N1	0.00498 (14)	−0.09682 (14)	−0.11620 (13)	0.0342 (4)
N2	0.13738 (14)	0.01805 (15)	0.04811 (13)	0.0349 (4)
H2	0.078439	0.007940	0.027580	0.042*
N3	0.38210 (15)	−0.19078 (17)	−0.17920 (17)	0.0458 (6)
N4	0.35428 (18)	0.32939 (19)	0.43080 (16)	0.0523 (6)
C1	−0.06834 (17)	−0.15150 (18)	−0.18664 (16)	0.0359 (5)
C2	−0.0417 (2)	−0.2208 (2)	−0.25325 (19)	0.0460 (6)
H2A	−0.080172	−0.267205	−0.307906	0.055*
C3	0.04822 (19)	−0.2062 (2)	−0.22230 (19)	0.0457 (6)
H3	0.085817	−0.240133	−0.251301	0.055*
C4	0.07675 (17)	−0.12956 (18)	−0.13683 (16)	0.0350 (5)
C5	0.16521 (17)	−0.09594 (18)	−0.08191 (16)	0.0347 (5)
C6	0.19231 (17)	−0.02811 (19)	0.00377 (17)	0.0361 (5)
C7	0.28257 (17)	0.0083 (2)	0.06079 (18)	0.0410 (6)
H7	0.334951	−0.010537	0.047330	0.049*
C8	0.27982 (17)	0.0742 (2)	0.13708 (17)	0.0398 (6)
H8	0.329560	0.108961	0.186970	0.048*
C9	0.18848 (16)	0.08243 (18)	0.12942 (16)	0.0342 (5)
C10	0.15803 (17)	0.14413 (18)	0.19319 (16)	0.0352 (5)
C11	0.23765 (17)	−0.13397 (18)	−0.11892 (17)	0.0367 (5)
C12	0.2686 (2)	−0.1233 (2)	−0.18598 (19)	0.0448 (6)
H12	0.239804	−0.095851	−0.211677	0.054*
C13	0.3405 (2)	−0.1522 (2)	−0.2151 (2)	0.0485 (7)
H13	0.361088	−0.144919	−0.261162	0.058*
C14	0.3514 (2)	−0.2055 (2)	−0.1172 (2)	0.0522 (7)
H14	0.380116	−0.234744	−0.093724	0.063*
C15	0.2790 (2)	−0.1789 (2)	−0.0869 (2)	0.0487 (7)
H15	0.256878	−0.191155	−0.043690	0.058*
C16	0.4663 (2)	−0.2115 (3)	−0.2050 (3)	0.0681 (10)
H16A	0.453320	−0.246559	−0.267402	0.102*
H16B	0.481893	−0.248220	−0.180505	0.102*
H16C	0.519425	−0.153533	−0.184339	0.102*
C17	0.22757 (17)	0.20923 (19)	0.27671 (17)	0.0382 (6)
C18	0.3102 (2)	0.2748 (2)	0.28244 (19)	0.0476 (7)
H18	0.323403	0.278527	0.232921	0.057*
C19	0.3724 (2)	0.3341 (2)	0.3602 (2)	0.0559 (8)
H19	0.428817	0.378833	0.364229	0.067*
C20	0.2769 (2)	0.2655 (3)	0.4264 (2)	0.0571 (8)
H20	0.266450	0.261344	0.476314	0.069*
C21	0.2123 (2)	0.2059 (2)	0.35038 (19)	0.0512 (7)
H21	0.156525	0.161832	0.348286	0.061*
C22	0.4222 (3)	0.3943 (3)	0.5145 (2)	0.0765 (12)
H22A	0.486697	0.402045	0.506732	0.115*
H22B	0.410984	0.369313	0.553985	0.115*
H22C	0.413820	0.454385	0.537886	0.115*
N31	−0.01983 (14)	0.58834 (14)	1.11067 (13)	0.0321 (4)
N32	0.13443 (14)	0.52137 (14)	1.06377 (13)	0.0323 (4)
H32	0.077044	0.509769	1.037969	0.039*
N33	0.2909 (2)	0.8152 (3)	1.46135 (17)	0.0731 (10)
N34	0.40173 (18)	0.3243 (2)	0.85612 (18)	0.0514 (6)
C31	−0.09855 (17)	0.61123 (17)	1.12491 (16)	0.0327 (5)
C32	−0.08813 (19)	0.67293 (19)	1.21456 (17)	0.0398 (6)
H32A	−0.133520	0.697265	1.240105	0.048*
C33	−0.00096 (19)	0.68883 (19)	1.25441 (17)	0.0395 (6)
H33	0.027449	0.727228	1.313570	0.047*
C34	0.04086 (17)	0.63580 (17)	1.18920 (15)	0.0333 (5)
C35	0.13175 (17)	0.63437 (17)	1.20703 (15)	0.0336 (5)
C36	0.17406 (17)	0.58087 (17)	1.14865 (15)	0.0334 (5)
C37	0.26643 (17)	0.57766 (19)	1.16429 (17)	0.0380 (5)
H37	0.310929	0.611899	1.217652	0.046*
C38	0.27939 (17)	0.51735 (18)	1.08982 (17)	0.0366 (5)
H38	0.334072	0.501042	1.082191	0.044*
C39	0.19646 (16)	0.48239 (17)	1.02454 (16)	0.0329 (5)
C40	0.18079 (16)	0.42168 (17)	0.93809 (16)	0.0319 (5)
C41	0.18878 (18)	0.69690 (19)	1.29633 (16)	0.0380 (5)
C42	0.2087 (3)	0.6640 (3)	1.3497 (2)	0.0688 (10)
H42	0.187924	0.599196	1.329889	0.083*
C43	0.2590 (3)	0.7248 (4)	1.4325 (2)	0.0799 (13)
H43	0.271096	0.701316	1.469781	0.096*
C44	0.2684 (4)	0.8486 (3)	1.4119 (3)	0.0929 (16)
H44	0.288377	0.913703	1.433909	0.111*
C45	0.2173 (3)	0.7916 (3)	1.3297 (2)	0.0726 (11)
H45	0.201300	0.817205	1.295517	0.087*
C46	0.3478 (4)	0.8788 (4)	1.5499 (3)	0.118 (2)
H46A	0.305706	0.889834	1.589239	0.177*
H46B	0.385695	0.937711	1.554100	0.177*
H46C	0.389466	0.851050	1.564944	0.177*
C47	0.25891 (17)	0.38797 (18)	0.90922 (16)	0.0341 (5)
C48	0.24485 (19)	0.29423 (19)	0.87120 (17)	0.0391 (6)
H48	0.185397	0.251139	0.863903	0.047*
C49	0.3169 (2)	0.2636 (2)	0.8440 (2)	0.0463 (6)
H49	0.306574	0.199286	0.816653	0.056*
C50	0.4173 (2)	0.4150 (2)	0.8912 (2)	0.0478 (7)
H50	0.477407	0.456484	0.897517	0.057*
C51	0.34734 (18)	0.4485 (2)	0.91792 (18)	0.0395 (6)
H51	0.358894	0.512953	0.942445	0.047*
C52	0.4808 (3)	0.2911 (4)	0.8341 (4)	0.0919 (15)
H52A	0.507861	0.282822	0.880344	0.138*
H52B	0.529299	0.336592	0.826383	0.138*
H52C	0.457745	0.231909	0.781161	0.138*
C23	0.1762 (10)	0.9524 (12)	1.2558 (12)	0.088 (5)*	0.363 (4)
H23	0.168483	1.004107	1.301133	0.105*	0.363 (4)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
S61	0.0519 (5)	0.0947 (7)	0.0590 (5)	0.0258 (5)	0.0164 (4)	0.0358 (5)
O61	0.0742 (19)	0.123 (3)	0.0589 (17)	0.0228 (18)	0.0257 (15)	0.0237 (17)
O62	0.0605 (18)	0.152 (3)	0.107 (3)	0.049 (2)	0.0254 (18)	0.054 (2)
O63	0.0857 (19)	0.097 (2)	0.0792 (18)	0.0329 (16)	0.0307 (15)	0.0597 (17)
C61	0.075 (2)	0.061 (2)	0.0535 (19)	0.0203 (18)	0.0063 (17)	0.0284 (17)
C62	0.118 (4)	0.080 (3)	0.086 (3)	0.032 (3)	−0.008 (3)	0.046 (3)
C63	0.235 (9)	0.085 (4)	0.088 (4)	0.028 (5)	−0.023 (5)	0.056 (3)
C64	0.258 (10)	0.079 (4)	0.077 (4)	0.013 (5)	0.034 (6)	0.055 (3)
C65	0.193 (8)	0.050 (2)	0.100 (4)	0.005 (3)	0.100 (5)	0.023 (3)
C66	0.125 (5)	0.057 (3)	0.138 (6)	0.008 (3)	0.096 (5)	0.012 (3)
C67	0.065 (2)	0.056 (2)	0.096 (3)	0.0164 (18)	0.034 (2)	0.007 (2)
C68	0.060 (2)	0.059 (2)	0.056 (2)	0.0186 (16)	0.0206 (16)	0.0163 (16)
C69	0.079 (2)	0.0468 (17)	0.0489 (18)	0.0130 (16)	0.0239 (17)	0.0206 (15)
C70	0.151 (5)	0.051 (2)	0.061 (2)	0.008 (2)	0.043 (3)	0.0287 (19)
S71	0.0519 (10)	0.0656 (11)	0.0524 (8)	0.0327 (10)	0.0219 (8)	0.0393 (9)
S72	0.0329 (13)	0.0429 (15)	0.0523 (14)	0.0169 (12)	0.0060 (11)	0.0258 (13)
O71	0.065 (3)	0.087 (3)	0.088 (3)	0.044 (2)	0.035 (2)	0.044 (3)
O72	0.050 (3)	0.053 (3)	0.052 (3)	0.009 (3)	0.002 (2)	0.030 (3)
O73	0.057 (2)	0.101 (3)	0.057 (2)	0.037 (2)	0.0161 (19)	0.052 (3)
O74	0.071 (5)	0.110 (7)	0.088 (6)	0.067 (5)	0.039 (5)	0.065 (6)
O75	0.033 (5)	0.043 (5)	0.071 (7)	0.011 (4)	0.004 (4)	0.030 (5)
O76	0.044 (4)	0.044 (4)	0.044 (4)	0.014 (3)	−0.009 (3)	0.011 (3)
C71	0.051 (3)	0.051 (3)	0.052 (3)	0.024 (2)	0.017 (2)	0.036 (2)
C72	0.077 (4)	0.062 (3)	0.052 (3)	0.036 (3)	0.027 (3)	0.036 (3)
C73	0.059 (3)	0.041 (3)	0.074 (4)	0.011 (2)	0.003 (3)	0.035 (3)
C74	0.075 (3)	0.042 (2)	0.057 (3)	0.008 (2)	0.012 (2)	0.033 (2)
C75	0.072 (4)	0.059 (3)	0.055 (3)	−0.002 (3)	0.007 (3)	0.040 (3)
C76	0.044 (2)	0.062 (3)	0.058 (3)	0.010 (2)	0.010 (2)	0.039 (3)
C77	0.052 (3)	0.047 (2)	0.044 (2)	0.020 (2)	0.0171 (19)	0.026 (2)
C78	0.059 (3)	0.044 (2)	0.039 (2)	0.024 (3)	0.013 (2)	0.024 (2)
C79	0.059 (3)	0.050 (2)	0.047 (2)	0.030 (2)	0.026 (2)	0.037 (2)
C80	0.079 (4)	0.044 (3)	0.042 (3)	0.009 (3)	0.008 (3)	0.031 (2)
S81	0.0516 (7)	0.1105 (13)	0.0543 (8)	0.0227 (7)	0.0143 (6)	0.0498 (8)
O81	0.0653 (17)	0.150 (3)	0.085 (2)	0.0131 (18)	0.0155 (15)	0.078 (2)
O82	0.0868 (19)	0.0891 (19)	0.0577 (15)	0.0270 (15)	0.0183 (14)	0.0422 (14)
O83	0.079 (3)	0.173 (5)	0.060 (3)	0.070 (4)	0.022 (2)	0.039 (3)
C81	0.044 (3)	0.076 (3)	0.048 (3)	0.020 (2)	0.019 (2)	0.035 (3)
C82	0.065 (3)	0.078 (4)	0.058 (3)	0.038 (3)	0.030 (3)	0.035 (3)
C83	0.085 (6)	0.066 (4)	0.052 (4)	0.040 (4)	0.030 (3)	0.024 (3)
C84	0.041 (3)	0.081 (5)	0.070 (5)	0.010 (3)	0.013 (3)	0.042 (4)
C85	0.072 (4)	0.091 (5)	0.070 (4)	0.035 (3)	0.027 (3)	0.053 (4)
C86	0.120 (4)	0.085 (3)	0.081 (3)	0.035 (3)	0.018 (3)	0.049 (3)
C87	0.135 (8)	0.054 (4)	0.060 (4)	0.033 (5)	0.037 (4)	0.030 (4)
C88	0.078 (4)	0.055 (3)	0.046 (3)	0.015 (3)	0.022 (3)	0.030 (3)
C89	0.0597 (19)	0.0580 (18)	0.0471 (17)	0.0131 (15)	0.0230 (15)	0.0246 (15)
C90	0.054 (3)	0.065 (3)	0.048 (3)	0.026 (2)	0.024 (2)	0.036 (3)
S91	0.0849 (12)	0.0736 (11)	0.0747 (11)	−0.0061 (9)	−0.0378 (10)	0.0314 (10)
O91	0.065 (3)	0.142 (5)	0.144 (6)	−0.034 (3)	−0.030 (3)	0.114 (5)
O92	0.063 (3)	0.108 (4)	0.120 (5)	0.006 (3)	−0.027 (3)	0.072 (4)
O96	0.232 (9)	0.066 (3)	0.119 (5)	−0.034 (4)	−0.112 (6)	0.036 (3)
C97	0.105 (3)	0.061 (2)	0.060 (2)	0.033 (2)	0.018 (2)	0.0410 (19)
C95	0.046 (3)	0.075 (4)	0.070 (4)	−0.002 (3)	−0.001 (3)	0.056 (3)
C96	0.098 (5)	0.043 (3)	0.044 (3)	0.003 (3)	−0.004 (3)	0.027 (3)
C98	0.045 (3)	0.066 (4)	0.060 (4)	0.031 (3)	0.019 (3)	0.042 (3)
C100	0.0400 (14)	0.072 (2)	0.068 (2)	0.0146 (14)	0.0118 (13)	0.0514 (18)
C94	0.087 (5)	0.149 (6)	0.108 (5)	0.085 (5)	0.068 (4)	0.106 (5)
C93	0.156 (7)	0.142 (7)	0.110 (6)	0.115 (6)	0.098 (5)	0.098 (5)
C92	0.170 (7)	0.069 (5)	0.061 (4)	0.073 (5)	0.053 (4)	0.043 (4)
C91	0.072 (3)	0.049 (2)	0.039 (2)	0.020 (2)	0.001 (2)	0.0249 (19)
C99	0.0358 (19)	0.043 (2)	0.038 (2)	0.0116 (17)	0.0051 (17)	0.0289 (19)
O108	0.096 (3)	0.157 (4)	0.129 (4)	0.010 (3)	0.030 (3)	−0.028 (3)
O109	0.143 (4)	0.110 (3)	0.087 (3)	0.062 (3)	0.045 (3)	0.022 (2)
N1	0.0246 (9)	0.0396 (11)	0.0360 (11)	0.0060 (8)	0.0021 (8)	0.0200 (9)
N2	0.0239 (9)	0.0475 (12)	0.0330 (11)	0.0111 (8)	0.0021 (8)	0.0207 (9)
N3	0.0302 (11)	0.0464 (13)	0.0657 (16)	0.0178 (10)	0.0112 (11)	0.0283 (12)
N4	0.0421 (13)	0.0581 (15)	0.0360 (12)	0.0073 (11)	−0.0030 (10)	0.0134 (11)
C1	0.0276 (11)	0.0413 (13)	0.0349 (13)	0.0075 (10)	0.0031 (10)	0.0185 (11)
C2	0.0363 (14)	0.0477 (15)	0.0386 (14)	0.0125 (12)	0.0011 (11)	0.0106 (12)
C3	0.0344 (13)	0.0494 (16)	0.0425 (15)	0.0147 (12)	0.0049 (11)	0.0137 (13)
C4	0.0288 (11)	0.0393 (13)	0.0361 (13)	0.0095 (10)	0.0055 (10)	0.0192 (11)
C5	0.0275 (11)	0.0426 (13)	0.0377 (13)	0.0114 (10)	0.0063 (10)	0.0232 (11)
C6	0.0280 (11)	0.0473 (14)	0.0375 (13)	0.0120 (10)	0.0058 (10)	0.0253 (12)
C7	0.0262 (12)	0.0588 (16)	0.0417 (14)	0.0148 (11)	0.0057 (10)	0.0276 (13)
C8	0.0252 (11)	0.0555 (16)	0.0371 (13)	0.0107 (11)	0.0013 (10)	0.0240 (12)
C9	0.0257 (11)	0.0454 (14)	0.0325 (12)	0.0083 (10)	0.0032 (9)	0.0227 (11)
C10	0.0266 (11)	0.0433 (13)	0.0355 (13)	0.0059 (10)	0.0037 (10)	0.0230 (11)
C11	0.0283 (11)	0.0414 (13)	0.0402 (14)	0.0107 (10)	0.0044 (10)	0.0209 (11)
C12	0.0454 (15)	0.0570 (17)	0.0493 (16)	0.0297 (13)	0.0171 (12)	0.0321 (14)
C13	0.0453 (15)	0.0553 (17)	0.0594 (18)	0.0254 (13)	0.0209 (14)	0.0337 (15)
C14	0.0489 (16)	0.0554 (17)	0.066 (2)	0.0258 (14)	0.0103 (15)	0.0366 (16)
C15	0.0459 (15)	0.0579 (17)	0.0592 (18)	0.0231 (13)	0.0148 (13)	0.0390 (15)
C16	0.0379 (16)	0.070 (2)	0.106 (3)	0.0310 (16)	0.0270 (18)	0.042 (2)
C17	0.0274 (11)	0.0470 (14)	0.0352 (13)	0.0082 (10)	0.0006 (10)	0.0196 (11)
C18	0.0368 (14)	0.0550 (17)	0.0424 (15)	0.0024 (12)	0.0011 (11)	0.0257 (13)
C19	0.0416 (16)	0.0558 (18)	0.0491 (17)	−0.0044 (13)	−0.0025 (13)	0.0226 (15)
C20	0.0494 (17)	0.074 (2)	0.0371 (15)	0.0102 (15)	0.0055 (13)	0.0258 (15)
C21	0.0373 (14)	0.0658 (19)	0.0379 (15)	0.0026 (13)	0.0034 (12)	0.0246 (14)
C22	0.062 (2)	0.081 (3)	0.0401 (18)	0.0016 (19)	−0.0108 (16)	0.0087 (18)
N31	0.0278 (9)	0.0373 (10)	0.0312 (10)	0.0109 (8)	0.0051 (8)	0.0171 (9)
N32	0.0276 (9)	0.0392 (11)	0.0299 (10)	0.0134 (8)	0.0033 (8)	0.0160 (9)
N33	0.073 (2)	0.096 (2)	0.0300 (13)	0.0489 (19)	−0.0063 (13)	0.0044 (15)
N34	0.0441 (13)	0.0681 (17)	0.0643 (16)	0.0349 (12)	0.0267 (12)	0.0394 (14)
C31	0.0306 (11)	0.0373 (12)	0.0334 (12)	0.0125 (10)	0.0085 (9)	0.0193 (10)
C32	0.0361 (13)	0.0501 (15)	0.0343 (13)	0.0195 (11)	0.0107 (10)	0.0182 (12)
C33	0.0382 (13)	0.0496 (15)	0.0296 (12)	0.0183 (11)	0.0071 (10)	0.0164 (11)
C34	0.0311 (12)	0.0395 (13)	0.0302 (12)	0.0122 (10)	0.0067 (9)	0.0177 (10)
C35	0.0302 (11)	0.0396 (13)	0.0299 (12)	0.0114 (10)	0.0032 (9)	0.0169 (10)
C36	0.0291 (11)	0.0397 (13)	0.0306 (12)	0.0116 (10)	0.0028 (9)	0.0172 (10)
C37	0.0291 (12)	0.0481 (14)	0.0354 (13)	0.0129 (10)	0.0013 (10)	0.0201 (12)
C38	0.0291 (12)	0.0469 (14)	0.0382 (13)	0.0158 (10)	0.0051 (10)	0.0230 (12)
C39	0.0282 (11)	0.0390 (12)	0.0351 (12)	0.0136 (10)	0.0058 (9)	0.0201 (11)
C40	0.0277 (11)	0.0373 (12)	0.0358 (12)	0.0129 (9)	0.0073 (9)	0.0209 (10)
C41	0.0347 (12)	0.0495 (15)	0.0301 (12)	0.0185 (11)	0.0044 (10)	0.0176 (11)
C42	0.067 (2)	0.079 (2)	0.0498 (19)	0.0045 (18)	−0.0083 (16)	0.0391 (19)
C43	0.073 (3)	0.120 (4)	0.045 (2)	0.024 (2)	−0.0025 (18)	0.047 (2)
C44	0.107 (4)	0.065 (2)	0.065 (3)	0.033 (2)	−0.025 (2)	0.002 (2)
C45	0.083 (3)	0.059 (2)	0.054 (2)	0.0185 (19)	−0.0152 (18)	0.0173 (17)
C46	0.118 (4)	0.148 (5)	0.0343 (19)	0.075 (4)	−0.024 (2)	−0.012 (2)
C47	0.0317 (12)	0.0436 (13)	0.0336 (12)	0.0163 (10)	0.0077 (10)	0.0223 (11)
C48	0.0379 (13)	0.0438 (14)	0.0394 (14)	0.0171 (11)	0.0084 (11)	0.0215 (12)
C49	0.0501 (16)	0.0494 (16)	0.0490 (16)	0.0260 (13)	0.0151 (13)	0.0259 (14)
C50	0.0358 (14)	0.0623 (18)	0.0619 (18)	0.0220 (13)	0.0182 (13)	0.0399 (16)
C51	0.0347 (13)	0.0483 (15)	0.0444 (14)	0.0167 (11)	0.0105 (11)	0.0283 (13)
C52	0.071 (3)	0.103 (3)	0.144 (4)	0.063 (3)	0.064 (3)	0.070 (3)

Geometric parameters (Å, º)

S61—O61	1.440 (3)	C94B—H94B	0.9500
S61—O62	1.439 (3)	C94B—C100	1.529 (15)
S61—O63	1.436 (3)	C95—H95	0.9500
S61—C61	1.782 (4)	C95—C96	1.364 (10)
C61—C62	1.363 (6)	C95—C100	1.389 (7)
C61—C69	1.442 (6)	C95B—H95B	0.9500
C62—H62	0.9500	C95B—C96B	1.341 (16)
C62—C63	1.419 (10)	C95B—C100	1.30 (2)
C63—H63	0.9500	C96—H96	0.9500
C63—C64	1.351 (12)	C96B—H96B	0.9500
C64—H64	0.9500	C96B—C23	1.390 (15)
C64—C70	1.418 (11)	C97B—H97B	0.9500
C65—H65	0.9500	C97B—C98B	1.391 (15)
C65—C66	1.322 (10)	C97B—C23	1.379 (15)
C65—C70	1.465 (10)	C98—H98	0.9500
C66—H66	0.9500	C98—C99	1.405 (7)
C66—C67	1.377 (9)	C98B—C100	1.445 (13)
C67—H67	0.9500	C100—C94	1.3900
C67—C68	1.377 (5)	C100—C99	1.3900
C68—H68	0.9500	C94—H94	0.9500
C68—C69	1.417 (6)	C94—C93	1.3900
C69—C70	1.426 (5)	C93—H93	0.9500
S71—O71	1.448 (4)	C93—C92	1.3900
S71—O72	1.450 (6)	C92—H92	0.9500
S71—O73	1.450 (4)	C92—C91	1.3900
S71—C71	1.824 (6)	C91—C99	1.3900
S72—O74	1.455 (7)	O109—H10A	0.8694
S72—O75	1.442 (12)	O109—H10B	0.8697
S72—O76	1.432 (8)	N1—C1	1.369 (3)
S72—C71B	1.882 (15)	N1—C4	1.366 (3)
C71—C72	1.384 (8)	N2—H2	0.8800
C71—C79	1.391 (7)	N2—C6	1.370 (3)
C71B—C72B	1.422 (17)	N2—C9	1.371 (3)
C71B—C79B	1.296 (15)	N3—C13	1.343 (4)
C72—H72	0.9500	N3—C14	1.334 (4)
C72—C73	1.410 (9)	N3—C16	1.476 (4)
C72B—H72B	0.9500	N4—C19	1.348 (4)
C72B—C73B	1.32 (2)	N4—C20	1.334 (4)
C73—H73	0.9500	N4—C22	1.486 (4)
C73—C74	1.303 (8)	C1—C2	1.450 (4)
C73B—H73B	0.9500	C1—C10^i	1.405 (3)
C73B—C74B	1.23 (2)	C2—H2A	0.9500
C74—H74	0.9500	C2—C3	1.345 (4)
C74—C80	1.442 (8)	C3—H3	0.9500
C74B—H74B	0.9500	C3—C4	1.441 (4)
C74B—C80B	1.586 (16)	C4—C5	1.405 (3)
C75—H75	0.9500	C5—C6	1.396 (4)
C75—C76	1.358 (9)	C5—C11	1.488 (3)
C75—C80	1.356 (9)	C6—C7	1.435 (3)
C76—H76	0.9500	C7—H7	0.9500
C76—C77	1.428 (7)	C7—C8	1.353 (4)
C77—H77	0.9500	C8—H8	0.9500
C77—C78	1.339 (8)	C8—C9	1.437 (3)
C78—H78	0.9500	C9—C10	1.392 (4)
C78—C79	1.446 (8)	C10—C17	1.495 (3)
C79—C80	1.411 (9)	C11—C12	1.390 (4)
C79B—C80B	1.3900	C11—C15	1.388 (4)
C79B—C78B	1.3900	C12—H12	0.9500
C80B—C75B	1.3900	C12—C13	1.371 (4)
C75B—H75B	0.9500	C13—H13	0.9500
C75B—C76B	1.3900	C14—H14	0.9500
C76B—H76B	0.9500	C14—C15	1.367 (4)
C76B—C77B	1.3900	C15—H15	0.9500
C77B—H77B	0.9500	C16—H16A	0.9800
C77B—C78B	1.3900	C16—H16B	0.9800
C78B—H78B	0.9500	C16—H16C	0.9800
S81—O81	1.454 (3)	C17—C18	1.393 (4)
S81—O82	1.369 (3)	C17—C21	1.381 (4)
S81—O83	1.516 (6)	C18—H18	0.9500
S81—C81	1.786 (6)	C18—C19	1.373 (4)
S82—O81	1.404 (4)	C19—H19	0.9500
S82—O82	1.435 (4)	C20—H20	0.9500
S82—O84	1.450 (8)	C20—C21	1.369 (4)
S82—C81B	1.743 (13)	C21—H21	0.9500
C81—C82	1.340 (8)	C22—H22A	0.9800
C81—C89	1.472 (7)	C22—H22B	0.9800
C81B—C82B	1.395 (16)	C22—H22C	0.9800
C81B—C89	1.388 (13)	N31—C31	1.369 (3)
C82—H82	0.9500	N31—C34	1.367 (3)
C82—C83	1.331 (11)	N32—H32	0.8800
C82B—H82B	0.9500	N32—C36	1.368 (3)
C82B—C83B	1.42 (2)	N32—C39	1.369 (3)
C83—H83	0.9500	N33—C43	1.323 (6)
C83—C84	1.358 (14)	N33—C44	1.321 (6)
C83B—H83B	0.9500	N33—C46	1.483 (5)
C83B—C86	1.385 (19)	N34—C49	1.341 (4)
C84—H84	0.9500	N34—C50	1.338 (4)
C84—C90	1.473 (11)	N34—C52	1.479 (4)
C84B—H84B	0.9500	C31—C32	1.450 (4)
C84B—C85B	1.21 (3)	C31—C40^ii	1.409 (3)
C84B—C88B	1.41 (2)	C32—H32A	0.9500
C85—H85	0.9500	C32—C33	1.350 (4)
C85—C86	1.339 (8)	C33—H33	0.9500
C85—C90	1.413 (8)	C33—C34	1.451 (4)
C85B—H85B	0.9500	C34—C35	1.404 (3)
C85B—C86B	1.33 (3)	C35—C36	1.394 (4)
C86—H86A	0.9500	C35—C41	1.491 (3)
C86—H86	0.9500	C36—C37	1.432 (3)
C86—C87	1.367 (11)	C37—H37	0.9500
C86—C88B	1.605 (16)	C37—C38	1.355 (4)
C86B—H86B	0.9500	C38—H38	0.9500
C86B—C87B	1.49 (3)	C38—C39	1.432 (3)
C87—H87	0.9500	C39—C40	1.390 (4)
C87—C88	1.385 (13)	C40—C47	1.493 (3)
C87B—H87B	0.9500	C41—C42	1.364 (4)
C87B—C89	1.378 (15)	C41—C45	1.380 (5)
C88—H88	0.9500	C42—H42	0.9500
C88—C89	1.427 (7)	C42—C43	1.377 (5)
C88B—C89	1.492 (15)	C43—H43	0.9500
C89—C90	1.366 (6)	C44—H44	0.9500
S91—O91	1.488 (8)	C44—C45	1.365 (5)
S91—O92	1.512 (6)	C45—H45	0.9500
S91—O96	1.365 (7)	C46—H46A	0.9800
S91—C91	1.758 (4)	C46—H46B	0.9800
S92—O14	1.408 (10)	C46—H46C	0.9800
S92—O94	1.441 (11)	C47—C48	1.388 (4)
S92—O95	1.449 (10)	C47—C51	1.397 (4)
S92—C91B	1.803 (10)	C48—H48	0.9500
C91B—C92B	1.375 (16)	C48—C49	1.376 (4)
C91B—C98B	1.419 (15)	C49—H49	0.9500
C92B—H92B	0.9500	C50—H50	0.9500
C92B—C97	1.421 (14)	C50—C51	1.368 (4)
C97—H97A	0.9500	C51—H51	0.9500
C97—H97	0.9500	C52—H52A	0.9800
C97—C94B	1.517 (15)	C52—H52B	0.9800
C97—C96	1.374 (8)	C52—H52C	0.9800
C97—C98	1.329 (8)	C23—H23	0.9500
O61—S61—C61	105.68 (19)	C100—C95—H95	119.8
O62—S61—O61	113.4 (2)	C96B—C95B—H95B	123.0
O62—S61—C61	106.6 (2)	C100—C95B—H95B	123.0
O63—S61—O61	112.9 (2)	C100—C95B—C96B	114.1 (17)
O63—S61—O62	111.6 (2)	C97—C96—H96	121.8
O63—S61—C61	105.93 (17)	C95—C96—C97	116.5 (5)
C62—C61—S61	117.4 (4)	C95—C96—H96	121.8
C62—C61—C69	122.8 (4)	C95B—C96B—H96B	116.4
C69—C61—S61	119.8 (3)	C95B—C96B—C23	127.2 (18)
C61—C62—H62	120.8	C23—C96B—H96B	116.4
C61—C62—C63	118.4 (6)	C98B—C97B—H97B	120.6
C63—C62—H62	120.8	C23—C97B—H97B	120.6
C62—C63—H63	119.5	C23—C97B—C98B	118.8 (15)
C64—C63—C62	120.9 (6)	C97—C98—H98	120.1
C64—C63—H63	119.5	C97—C98—C99	119.8 (6)
C63—C64—H64	119.0	C99—C98—H98	120.1
C63—C64—C70	122.1 (5)	C91B—C98B—C100	119.1 (9)
C70—C64—H64	119.0	C97B—C98B—C91B	123.7 (12)
C66—C65—H65	119.2	C97B—C98B—C100	117.1 (11)
C66—C65—C70	121.5 (5)	C95—C100—C94	118.0 (4)
C70—C65—H65	119.2	C95—C100—C99	122.0 (4)
C65—C66—H66	119.1	C95B—C100—C94B	117.0 (10)
C65—C66—C67	121.8 (6)	C95B—C100—C98B	125.4 (9)
C67—C66—H66	119.1	C98B—C100—C94B	117.5 (7)
C66—C67—H67	120.0	C94—C100—C99	120.0
C66—C67—C68	120.1 (6)	C100—C94—H94	120.0
C68—C67—H67	120.0	C100—C94—C93	120.0
C67—C68—H68	119.3	C93—C94—H94	120.0
C67—C68—C69	121.3 (4)	C94—C93—H93	120.0
C69—C68—H68	119.3	C92—C93—C94	120.0
C68—C69—C61	124.4 (3)	C92—C93—H93	120.0
C68—C69—C70	118.4 (4)	C93—C92—H92	120.0
C70—C69—C61	117.2 (4)	C93—C92—C91	120.0
C64—C70—C65	124.5 (6)	C91—C92—H92	120.0
C64—C70—C69	118.6 (6)	C92—C91—S91	116.2 (3)
C69—C70—C65	116.9 (5)	C99—C91—S91	123.7 (3)
O71—S71—O72	112.5 (4)	C99—C91—C92	120.0
O71—S71—O73	112.6 (3)	C100—C99—C98	116.2 (4)
O71—S71—C71	106.2 (3)	C91—C99—C98	123.8 (4)
O72—S71—O73	113.6 (3)	C91—C99—C100	120.0
O72—S71—C71	105.1 (3)	H10A—O109—H10B	104.6
O73—S71—C71	106.0 (2)	C4—N1—C1	105.5 (2)
O74—S72—C71B	108.5 (6)	C6—N2—H2	125.3
O75—S72—O74	112.8 (6)	C6—N2—C9	109.5 (2)
O75—S72—C71B	102.6 (5)	C9—N2—H2	125.3
O76—S72—O74	112.5 (4)	C13—N3—C16	119.4 (3)
O76—S72—O75	111.9 (6)	C14—N3—C13	120.6 (2)
O76—S72—C71B	107.9 (5)	C14—N3—C16	119.9 (3)
C72—C71—S71	118.0 (4)	C19—N4—C22	120.0 (3)
C72—C71—C79	122.0 (5)	C20—N4—C19	120.8 (3)
C79—C71—S71	119.8 (4)	C20—N4—C22	119.2 (3)
C72B—C71B—S72	108.0 (10)	N1—C1—C2	110.5 (2)
C79B—C71B—S72	122.8 (8)	N1—C1—C10^i	125.2 (2)
C79B—C71B—C72B	129.1 (13)	C10^i—C1—C2	124.3 (2)
C71—C72—H72	120.4	C1—C2—H2A	126.8
C71—C72—C73	119.2 (5)	C3—C2—C1	106.4 (2)
C73—C72—H72	120.4	C3—C2—H2A	126.8
C71B—C72B—H72B	120.8	C2—C3—H3	126.5
C73B—C72B—C71B	118.3 (16)	C2—C3—C4	107.0 (3)
C73B—C72B—H72B	120.8	C4—C3—H3	126.5
C72—C73—H73	119.1	N1—C4—C3	110.6 (2)
C74—C73—C72	121.8 (6)	N1—C4—C5	125.2 (2)
C74—C73—H73	119.1	C5—C4—C3	124.2 (2)
C72B—C73B—H73B	120.0	C4—C5—C11	117.2 (2)
C74B—C73B—C72B	120 (2)	C6—C5—C4	125.9 (2)
C74B—C73B—H73B	120.0	C6—C5—C11	116.9 (2)
C73—C74—H74	120.3	N2—C6—C5	125.6 (2)
C73—C74—C80	119.4 (6)	N2—C6—C7	107.4 (2)
C80—C74—H74	120.3	C5—C6—C7	127.0 (2)
C73B—C74B—H74B	118.7	C6—C7—H7	126.1
C73B—C74B—C80B	122.7 (18)	C8—C7—C6	107.9 (2)
C80B—C74B—H74B	118.7	C8—C7—H7	126.1
C76—C75—H75	119.7	C7—C8—H8	126.0
C80—C75—H75	119.7	C7—C8—C9	108.0 (2)
C80—C75—C76	120.6 (8)	C9—C8—H8	126.0
C75—C76—H76	120.1	N2—C9—C8	107.2 (2)
C75—C76—C77	119.7 (6)	N2—C9—C10	126.8 (2)
C77—C76—H76	120.1	C10—C9—C8	126.0 (2)
C76—C77—H77	119.2	C1^i—C10—C17	116.7 (2)
C78—C77—C76	121.7 (5)	C9—C10—C1^i	126.4 (2)
C78—C77—H77	119.2	C9—C10—C17	116.9 (2)
C77—C78—H78	120.8	C12—C11—C5	120.7 (2)
C77—C78—C79	118.4 (5)	C15—C11—C5	122.0 (2)
C79—C78—H78	120.8	C15—C11—C12	117.3 (3)
C71—C79—C78	125.2 (5)	C11—C12—H12	119.9
C71—C79—C80	116.4 (5)	C13—C12—C11	120.2 (3)
C80—C79—C78	118.5 (5)	C13—C12—H12	119.9
C71B—C79B—C80B	113.5 (8)	N3—C13—C12	120.6 (3)
C71B—C79B—C78B	126.5 (8)	N3—C13—H13	119.7
C80B—C79B—C78B	120.0	C12—C13—H13	119.7
C79B—C80B—C74B	116.2 (9)	N3—C14—H14	119.6
C79B—C80B—C75B	120.0	N3—C14—C15	120.7 (3)
C75B—C80B—C74B	123.8 (9)	C15—C14—H14	119.6
C80B—C75B—H75B	120.0	C11—C15—H15	119.8
C76B—C75B—C80B	120.0	C14—C15—C11	120.5 (3)
C76B—C75B—H75B	120.0	C14—C15—H15	119.8
C75B—C76B—H76B	120.0	N3—C16—H16A	109.5
C75B—C76B—C77B	120.0	N3—C16—H16B	109.5
C77B—C76B—H76B	120.0	N3—C16—H16C	109.5
C76B—C77B—H77B	120.0	H16A—C16—H16B	109.5
C76B—C77B—C78B	120.0	H16A—C16—H16C	109.5
C78B—C77B—H77B	120.0	H16B—C16—H16C	109.5
C79B—C78B—H78B	120.0	C18—C17—C10	120.9 (2)
C77B—C78B—C79B	120.0	C21—C17—C10	121.1 (2)
C77B—C78B—H78B	120.0	C21—C17—C18	118.0 (2)
C75—C80—C74	117.7 (7)	C17—C18—H18	120.2
C75—C80—C79	121.2 (6)	C19—C18—C17	119.5 (3)
C79—C80—C74	121.1 (5)	C19—C18—H18	120.2
O81—S81—O83	111.1 (3)	N4—C19—C18	120.7 (3)
O81—S81—C81	103.5 (2)	N4—C19—H19	119.7
O82—S81—O81	118.5 (2)	C18—C19—H19	119.7
O82—S81—O83	111.6 (2)	N4—C20—H20	119.8
O82—S81—C81	105.8 (2)	N4—C20—C21	120.4 (3)
O83—S81—C81	105.0 (3)	C21—C20—H20	119.8
O81—S82—O82	117.4 (3)	C17—C21—H21	119.7
O81—S82—O84	110.3 (4)	C20—C21—C17	120.6 (3)
O81—S82—C81B	109.0 (5)	C20—C21—H21	119.7
O82—S82—O84	104.0 (4)	N4—C22—H22A	109.5
O82—S82—C81B	108.0 (5)	N4—C22—H22B	109.5
O84—S82—C81B	107.6 (6)	N4—C22—H22C	109.5
C82—C81—S81	119.7 (4)	H22A—C22—H22B	109.5
C82—C81—C89	119.1 (5)	H22A—C22—H22C	109.5
C89—C81—S81	121.2 (4)	H22B—C22—H22C	109.5
C82B—C81B—S82	118.7 (9)	C34—N31—C31	104.7 (2)
C89—C81B—S82	121.1 (9)	C36—N32—H32	124.7
C89—C81B—C82B	120.3 (10)	C36—N32—C39	110.58 (19)
C81—C82—H82	118.5	C39—N32—H32	124.7
C83—C82—C81	122.9 (6)	C43—N33—C46	120.2 (4)
C83—C82—H82	118.5	C44—N33—C43	119.5 (3)
C81B—C82B—H82B	119.0	C44—N33—C46	120.2 (4)
C81B—C82B—C83B	122.0 (13)	C49—N34—C52	119.5 (3)
C83B—C82B—H82B	119.0	C50—N34—C49	121.2 (2)
C82—C83—H83	118.7	C50—N34—C52	119.2 (3)
C82—C83—C84	122.6 (9)	N31—C31—C32	111.4 (2)
C84—C83—H83	118.7	N31—C31—C40^ii	125.2 (2)
C82B—C83B—H83B	116.1	C40^ii—C31—C32	123.4 (2)
C86—C83B—C82B	127.7 (15)	C31—C32—H32A	126.9
C86—C83B—H83B	116.1	C33—C32—C31	106.2 (2)
C83—C84—H84	121.3	C33—C32—H32A	126.9
C83—C84—C90	117.5 (9)	C32—C33—H33	126.7
C90—C84—H84	121.3	C32—C33—C34	106.6 (2)
C85B—C84B—H84B	121.0	C34—C33—H33	126.7
C85B—C84B—C88B	117.9 (18)	N31—C34—C33	111.2 (2)
C88B—C84B—H84B	121.0	N31—C34—C35	125.9 (2)
C86—C85—H85	121.5	C35—C34—C33	123.0 (2)
C86—C85—C90	116.9 (7)	C34—C35—C41	117.0 (2)
C90—C85—H85	121.5	C36—C35—C34	126.0 (2)
C84B—C85B—H85B	115.2	C36—C35—C41	117.1 (2)
C84B—C85B—C86B	130 (2)	N32—C36—C35	125.8 (2)
C86B—C85B—H85B	115.2	N32—C36—C37	106.5 (2)
C83B—C86—H86A	126.1	C35—C36—C37	127.6 (2)
C83B—C86—C88B	107.9 (10)	C36—C37—H37	125.9
C85—C86—H86	117.5	C38—C37—C36	108.2 (2)
C85—C86—C87	124.9 (6)	C38—C37—H37	125.9
C87—C86—H86	117.5	C37—C38—H38	125.9
C88B—C86—H86A	126.1	C37—C38—C39	108.2 (2)
C85B—C86B—H86B	122.1	C39—C38—H38	125.9
C85B—C86B—C87B	116 (2)	N32—C39—C38	106.4 (2)
C87B—C86B—H86B	122.1	N32—C39—C40	125.9 (2)
C86—C87—H87	120.4	C40—C39—C38	127.7 (2)
C86—C87—C88	119.2 (7)	C31^ii—C40—C47	116.8 (2)
C88—C87—H87	120.4	C39—C40—C31^ii	126.5 (2)
C86B—C87B—H87B	119.7	C39—C40—C47	116.7 (2)
C89—C87B—C86B	120.5 (15)	C42—C41—C35	122.1 (3)
C89—C87B—H87B	119.7	C42—C41—C45	117.5 (3)
C87—C88—H88	121.4	C45—C41—C35	120.2 (3)
C87—C88—C89	117.3 (6)	C41—C42—H42	120.1
C89—C88—H88	121.4	C41—C42—C43	119.8 (4)
C84B—C88B—C86	115.4 (12)	C43—C42—H42	120.1
C84B—C88B—C89	121.6 (13)	N33—C43—C42	121.4 (4)
C89—C88B—C86	121.8 (9)	N33—C43—H43	119.3
C81B—C89—C88B	117.8 (8)	C42—C43—H43	119.3
C87B—C89—C81B	127.9 (9)	N33—C44—H44	119.3
C87B—C89—C88B	113.2 (9)	N33—C44—C45	121.5 (4)
C88—C89—C81	121.0 (5)	C45—C44—H44	119.3
C90—C89—C81	117.7 (4)	C41—C45—H45	120.0
C90—C89—C88	121.1 (5)	C44—C45—C41	120.0 (4)
C85—C90—C84	119.7 (6)	C44—C45—H45	120.0
C89—C90—C84	120.1 (6)	N33—C46—H46A	109.5
C89—C90—C85	120.2 (6)	N33—C46—H46B	109.5
O91—S91—O92	109.1 (6)	N33—C46—H46C	109.5
O91—S91—C91	104.5 (2)	H46A—C46—H46B	109.5
O92—S91—C91	107.4 (3)	H46A—C46—H46C	109.5
O96—S91—O91	109.9 (5)	H46B—C46—H46C	109.5
O96—S91—O92	113.8 (4)	C48—C47—C40	120.4 (2)
O96—S91—C91	111.7 (5)	C48—C47—C51	117.8 (2)
O14—S92—O94	113.2 (7)	C51—C47—C40	121.8 (2)
O14—S92—O95	113.3 (6)	C47—C48—H48	120.0
O14—S92—C91B	108.3 (5)	C49—C48—C47	120.1 (3)
O94—S92—O95	114.7 (6)	C49—C48—H48	120.0
O94—S92—C91B	100.7 (6)	N34—C49—C48	120.3 (3)
O95—S92—C91B	105.3 (5)	N34—C49—H49	119.9
C92B—C91B—S92	120.7 (8)	C48—C49—H49	119.9
C92B—C91B—C98B	119.7 (10)	N34—C50—H50	119.7
C98B—C91B—S92	119.5 (8)	N34—C50—C51	120.5 (3)
C91B—C92B—H92B	114.2	C51—C50—H50	119.7
C91B—C92B—C97	131.7 (11)	C47—C51—H51	120.0
C97—C92B—H92B	114.2	C50—C51—C47	120.0 (3)
C92B—C97—H97A	125.8	C50—C51—H51	120.0
C92B—C97—C94B	108.5 (8)	N34—C52—H52A	109.5
C94B—C97—H97A	125.8	N34—C52—H52B	109.5
C96—C97—H97	117.5	N34—C52—H52C	109.5
C98—C97—H97	117.5	H52A—C52—H52B	109.5
C98—C97—C96	125.0 (6)	H52A—C52—H52C	109.5
C97—C94B—H94B	118.4	H52B—C52—H52C	109.5
C97—C94B—C100	123.3 (10)	C96B—C23—H23	121.3
C100—C94B—H94B	118.4	C97B—C23—C96B	117.4 (16)
C96—C95—H95	119.8	C97B—C23—H23	121.3
C96—C95—C100	120.4 (5)
S61—C61—C62—C63	−179.0 (4)	C91B—C98B—C100—C94B	5.8 (13)
S61—C61—C69—C68	−2.3 (5)	C91B—C98B—C100—C95B	−178.7 (14)
S61—C61—C69—C70	179.1 (3)	C92B—C91B—C98B—C97B	177.9 (14)
O61—S61—C61—C62	−117.7 (4)	C92B—C91B—C98B—C100	−5.1 (16)
O61—S61—C61—C69	61.7 (3)	C92B—C97—C94B—C100	0.5 (12)
O62—S61—C61—C62	3.3 (4)	C97—C94B—C100—C95B	−179.5 (13)
O62—S61—C61—C69	−177.3 (3)	C97—C94B—C100—C98B	−3.7 (13)
O63—S61—C61—C62	122.2 (4)	C97—C98—C99—C100	1.5 (6)
O63—S61—C61—C69	−58.4 (3)	C97—C98—C99—C91	−179.6 (4)
C61—C62—C63—C64	−1.2 (9)	C95—C100—C94—C93	−179.0 (3)
C61—C69—C70—C64	0.9 (6)	C95—C100—C99—C98	−2.1 (4)
C61—C69—C70—C65	178.3 (4)	C95—C100—C99—C91	179.0 (3)
C62—C61—C69—C68	177.0 (4)	C95B—C96B—C23—C97B	−2 (3)
C62—C61—C69—C70	−1.5 (6)	C96—C97—C98—C99	−0.4 (8)
C62—C63—C64—C70	0.6 (11)	C96—C95—C100—C94	−179.4 (4)
C63—C64—C70—C65	−177.7 (6)	C96—C95—C100—C99	1.6 (6)
C63—C64—C70—C69	−0.5 (9)	C96B—C95B—C100—C94B	177.1 (14)
C65—C66—C67—C68	0.7 (8)	C96B—C95B—C100—C98B	2 (2)
C66—C65—C70—C64	177.3 (6)	C97B—C98B—C100—C94B	−176.9 (11)
C66—C65—C70—C69	0.1 (7)	C97B—C98B—C100—C95B	−1.5 (19)
C66—C67—C68—C69	−0.9 (6)	C98—C97—C96—C95	−0.1 (7)
C67—C68—C69—C61	−177.8 (3)	C98B—C91B—C92B—C97	2 (2)
C67—C68—C69—C70	0.7 (5)	C98B—C97B—C23—C96B	2 (2)
C68—C69—C70—C64	−177.7 (4)	C100—C95—C96—C97	−0.4 (6)
C68—C69—C70—C65	−0.3 (5)	C100—C95B—C96B—C23	0 (3)
C69—C61—C62—C63	1.6 (7)	C100—C94—C93—C92	0.0
C70—C65—C66—C67	−0.3 (9)	C94—C100—C99—C98	178.9 (4)
S71—C71—C72—C73	172.6 (4)	C94—C100—C99—C91	0.0
S71—C71—C79—C78	5.7 (6)	C94—C93—C92—C91	0.0
S71—C71—C79—C80	−174.8 (3)	C93—C92—C91—S91	176.6 (3)
S72—C71B—C72B—C73B	171.4 (13)	C93—C92—C91—C99	0.0
S72—C71B—C79B—C80B	−170.2 (7)	C92—C91—C99—C98	−178.8 (4)
S72—C71B—C79B—C78B	8.0 (14)	C92—C91—C99—C100	0.0
O71—S71—C71—C72	5.6 (4)	C99—C100—C94—C93	0.0
O71—S71—C71—C79	−179.0 (3)	N1—C1—C2—C3	−0.7 (3)
O72—S71—C71—C72	−113.8 (4)	N1—C4—C5—C6	4.3 (4)
O72—S71—C71—C79	61.6 (4)	N1—C4—C5—C11	−173.8 (2)
O73—S71—C71—C72	125.6 (4)	N2—C6—C7—C8	0.3 (3)
O73—S71—C71—C79	−59.0 (4)	N2—C9—C10—C1^i	0.8 (4)
O74—S72—C71B—C72B	0.5 (9)	N2—C9—C10—C17	−178.9 (2)
O74—S72—C71B—C79B	177.1 (9)	N3—C14—C15—C11	−1.6 (5)
O75—S72—C71B—C72B	−119.1 (10)	N4—C20—C21—C17	1.8 (5)
O75—S72—C71B—C79B	57.5 (11)	C1—N1—C4—C3	0.3 (3)
O76—S72—C71B—C72B	122.6 (8)	C1—N1—C4—C5	−177.6 (2)
O76—S72—C71B—C79B	−60.8 (11)	C1—C2—C3—C4	0.8 (3)
C71—C72—C73—C74	2.3 (8)	C1^i—C10—C17—C18	−116.4 (3)
C71—C79—C80—C74	2.1 (6)	C1^i—C10—C17—C21	64.0 (4)
C71—C79—C80—C75	180.0 (4)	C2—C3—C4—N1	−0.7 (3)
C71B—C72B—C73B—C74B	2 (2)	C2—C3—C4—C5	177.2 (3)
C71B—C79B—C80B—C74B	−3.8 (11)	C3—C4—C5—C6	−173.3 (3)
C71B—C79B—C80B—C75B	178.3 (10)	C3—C4—C5—C11	8.6 (4)
C71B—C79B—C78B—C77B	−178.1 (12)	C4—N1—C1—C2	0.2 (3)
C72—C71—C79—C78	−179.0 (4)	C4—N1—C1—C10^i	178.3 (2)
C72—C71—C79—C80	0.4 (6)	C4—C5—C6—N2	−1.2 (4)
C72—C73—C74—C80	0.2 (7)	C4—C5—C6—C7	−179.0 (3)
C72B—C71B—C79B—C80B	5.6 (16)	C4—C5—C11—C12	60.6 (3)
C72B—C71B—C79B—C78B	−176.2 (10)	C4—C5—C11—C15	−121.3 (3)
C72B—C73B—C74B—C80B	−1 (3)	C5—C6—C7—C8	178.5 (3)
C73—C74—C80—C75	179.6 (5)	C5—C11—C12—C13	174.9 (3)
C73—C74—C80—C79	−2.5 (7)	C5—C11—C15—C14	−174.0 (3)
C73B—C74B—C80B—C79B	2.0 (19)	C6—N2—C9—C8	−1.7 (3)
C73B—C74B—C80B—C75B	179.8 (14)	C6—N2—C9—C10	178.6 (2)
C74B—C80B—C75B—C76B	−177.7 (11)	C6—C5—C11—C12	−117.7 (3)
C75—C76—C77—C78	−0.5 (7)	C6—C5—C11—C15	60.4 (3)
C76—C75—C80—C74	178.8 (4)	C6—C7—C8—C9	−1.3 (3)
C76—C75—C80—C79	0.8 (7)	C7—C8—C9—N2	1.9 (3)
C76—C77—C78—C79	0.9 (6)	C7—C8—C9—C10	−178.4 (2)
C77—C78—C79—C71	179.1 (4)	C8—C9—C10—C1^i	−178.8 (2)
C77—C78—C79—C80	−0.3 (6)	C8—C9—C10—C17	1.5 (4)
C78—C79—C80—C74	−178.3 (4)	C9—N2—C6—C5	−177.3 (2)
C78—C79—C80—C75	−0.5 (6)	C9—N2—C6—C7	0.9 (3)
C79—C71—C72—C73	−2.7 (7)	C9—C10—C17—C18	63.3 (4)
C79B—C71B—C72B—C73B	−5 (2)	C9—C10—C17—C21	−116.2 (3)
C79B—C80B—C75B—C76B	0.0	C10^i—C1—C2—C3	−178.8 (3)
C80B—C79B—C78B—C77B	0.0	C10—C17—C18—C19	179.6 (3)
C80B—C75B—C76B—C77B	0.0	C10—C17—C21—C20	179.6 (3)
C75B—C76B—C77B—C78B	0.0	C11—C5—C6—N2	176.9 (2)
C76B—C77B—C78B—C79B	0.0	C11—C5—C6—C7	−0.9 (4)
C78B—C79B—C80B—C74B	177.9 (10)	C11—C12—C13—N3	−0.3 (5)
C78B—C79B—C80B—C75B	0.0	C12—C11—C15—C14	4.2 (4)
C80—C75—C76—C77	−0.3 (7)	C13—N3—C14—C15	−2.2 (5)
S81—C81—C82—C83	179.7 (5)	C14—N3—C13—C12	3.1 (5)
S81—C81—C89—C88	−1.8 (5)	C15—C11—C12—C13	−3.3 (4)
S81—C81—C89—C90	−176.6 (3)	C16—N3—C13—C12	−173.0 (3)
S82—C81B—C82B—C83B	−179.4 (11)	C16—N3—C14—C15	173.9 (3)
S82—C81B—C89—C87B	−7.1 (15)	C17—C18—C19—N4	0.0 (5)
S82—C81B—C89—C88B	−174.4 (8)	C18—C17—C21—C20	0.0 (5)
O81—S81—C81—C82	114.6 (4)	C19—N4—C20—C21	−2.8 (5)
O81—S81—C81—C89	−64.7 (4)	C20—N4—C19—C18	1.9 (5)
O81—S82—C81B—C82B	−114.9 (10)	C21—C17—C18—C19	−0.9 (5)
O81—S82—C81B—C89	65.9 (10)	C22—N4—C19—C18	−179.8 (4)
O82—S81—C81—C82	−120.2 (4)	C22—N4—C20—C21	178.9 (4)
O82—S81—C81—C89	60.6 (4)	N31—C31—C32—C33	1.3 (3)
O82—S82—C81B—C82B	116.4 (10)	N31—C34—C35—C36	−3.4 (4)
O82—S82—C81B—C89	−62.8 (10)	N31—C34—C35—C41	175.6 (2)
O83—S81—C81—C82	−2.0 (5)	N32—C36—C37—C38	−0.1 (3)
O83—S81—C81—C89	178.8 (4)	N32—C39—C40—C31^ii	−0.3 (4)
O84—S82—C81B—C82B	4.7 (12)	N32—C39—C40—C47	179.8 (2)
O84—S82—C81B—C89	−174.5 (8)	N33—C44—C45—C41	−0.8 (8)
C81—C82—C83—C84	−1.1 (11)	N34—C50—C51—C47	0.4 (4)
C81—C89—C90—C84	−5.1 (6)	C31—N31—C34—C33	0.7 (3)
C81—C89—C90—C85	177.4 (4)	C31—N31—C34—C35	−179.9 (2)
C81B—C82B—C83B—C86	5 (2)	C31—C32—C33—C34	−0.8 (3)
C82—C81—C89—C88	179.0 (4)	C31^ii—C40—C47—C48	−60.4 (3)
C82—C81—C89—C90	4.1 (6)	C31^ii—C40—C47—C51	118.5 (3)
C82—C83—C84—C90	0.1 (11)	C32—C33—C34—N31	0.1 (3)
C82B—C81B—C89—C87B	173.8 (10)	C32—C33—C34—C35	−179.3 (2)
C82B—C81B—C89—C88B	6.4 (15)	C33—C34—C35—C36	175.9 (2)
C82B—C83B—C86—C88B	−13.1 (19)	C33—C34—C35—C41	−5.1 (4)
C83—C84—C90—C85	−179.3 (6)	C34—N31—C31—C32	−1.2 (3)
C83—C84—C90—C89	3.2 (9)	C34—N31—C31—C40^ii	−179.9 (2)
C83B—C86—C88B—C84B	−173.9 (12)	C34—C35—C36—N32	0.8 (4)
C83B—C86—C88B—C89	18.7 (14)	C34—C35—C36—C37	179.8 (3)
C84B—C85B—C86B—C87B	8 (4)	C34—C35—C41—C42	109.5 (3)
C84B—C88B—C89—C81B	176.9 (11)	C34—C35—C41—C45	−65.6 (4)
C84B—C88B—C89—C87B	7.7 (15)	C35—C36—C37—C38	−179.3 (3)
C85—C86—C87—C88	7.3 (11)	C35—C41—C42—C43	−177.8 (3)
C85B—C84B—C88B—C86	−166.0 (17)	C35—C41—C45—C44	179.2 (4)
C85B—C84B—C88B—C89	1 (2)	C36—N32—C39—C38	2.1 (3)
C85B—C86B—C87B—C89	3 (3)	C36—N32—C39—C40	−177.3 (2)
C86—C85—C90—C84	−175.5 (5)	C36—C35—C41—C42	−71.4 (4)
C86—C85—C90—C89	2.0 (7)	C36—C35—C41—C45	113.5 (3)
C86—C87—C88—C89	−2.2 (9)	C36—C37—C38—C39	1.4 (3)
C86—C88B—C89—C81B	−16.5 (13)	C37—C38—C39—N32	−2.1 (3)
C86—C88B—C89—C87B	174.3 (9)	C37—C38—C39—C40	177.3 (3)
C86B—C87B—C89—C81B	−177.2 (13)	C38—C39—C40—C31^ii	−179.6 (2)
C86B—C87B—C89—C88B	−9.4 (17)	C38—C39—C40—C47	0.5 (4)
C87—C88—C89—C81	−177.1 (5)	C39—N32—C36—C35	178.0 (2)
C87—C88—C89—C90	−2.4 (7)	C39—N32—C36—C37	−1.3 (3)
C88—C89—C90—C84	−180.0 (5)	C39—C40—C47—C48	119.5 (3)
C88—C89—C90—C85	2.5 (6)	C39—C40—C47—C51	−61.6 (3)
C88B—C84B—C85B—C86B	−10 (4)	C40^ii—C31—C32—C33	180.0 (2)
C89—C81—C82—C83	−1.0 (8)	C40—C47—C48—C49	179.4 (2)
C89—C81B—C82B—C83B	−0.2 (18)	C40—C47—C51—C50	179.6 (2)
C90—C85—C86—C87	−7.1 (9)	C41—C35—C36—N32	−178.2 (2)
S91—C91—C99—C98	4.8 (4)	C41—C35—C36—C37	0.8 (4)
S91—C91—C99—C100	−176.3 (3)	C41—C42—C43—N33	−1.7 (7)
S92—C91B—C92B—C97	179.9 (10)	C42—C41—C45—C44	3.9 (6)
S92—C91B—C98B—C97B	−0.3 (17)	C43—N33—C44—C45	−3.6 (8)
S92—C91B—C98B—C100	176.8 (7)	C44—N33—C43—C42	4.9 (7)
O14—S92—C91B—C92B	126.7 (10)	C45—C41—C42—C43	−2.7 (6)
O14—S92—C91B—C98B	−55.2 (10)	C46—N33—C43—C42	−177.8 (4)
O91—S91—C91—C92	−120.1 (4)	C46—N33—C44—C45	179.1 (5)
O91—S91—C91—C99	56.4 (5)	C47—C48—C49—N34	1.7 (4)
O92—S91—C91—C92	124.2 (4)	C48—C47—C51—C50	−1.5 (4)
O92—S91—C91—C99	−59.4 (5)	C49—N34—C50—C51	1.9 (5)
O94—S92—C91B—C92B	−114.3 (10)	C50—N34—C49—C48	−2.9 (5)
O94—S92—C91B—C98B	63.8 (10)	C51—C47—C48—C49	0.5 (4)
O95—S92—C91B—C92B	5.2 (11)	C52—N34—C49—C48	174.1 (3)
O95—S92—C91B—C98B	−176.7 (9)	C52—N34—C50—C51	−175.2 (3)
O96—S91—C91—C92	−1.3 (4)	C23—C97B—C98B—C91B	176.5 (13)
O96—S91—C91—C99	175.2 (4)	C23—C97B—C98B—C100	−1 (2)
C91B—C92B—C97—C94B	0.5 (17)

Symmetry codes: (i) −x, −y, −z; (ii) −x, −y+1, −z+2.

(TriMCNP)(p-tosylate)3(H2O)8.75

Crystal data

3(C7H7O3S)·6.5(H2O)·0.5(HO)·C45H35N8·0.25[]	F(000) = 5580
Mr = 1326.97	Dx = 1.308 Mg m^−3
Monoclinic, P21/c	Cu Kα radiation, λ = 1.54184 Å
a = 17.54006 (8) Å	Cell parameters from 134892 reflections
b = 25.99854 (12) Å	θ = 2.6–78.5°
c = 30.05455 (13) Å	µ = 1.61 mm^−1
β = 100.5017 (4)°	T = 160 K
V = 13475.78 (10) Å^3	Needle, red
Z = 8	0.27 × 0.15 × 0.14 mm

Data collection

XtaLAB Synergy, Dualflex, HyPix diffractometer	25118 reflections with I > 2σ(I)
Detector resolution: 10.0000 pixels mm^-1	Rint = 0.039
ω scans	θmax = 79.2°, θmin = 2.3°
Absorption correction: gaussian CrysAlisPro 1.171.43.130a (Rigaku Oxford Diffraction, 2024) 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 = −21→22
Tmin = 0.416, Tmax = 1.000	k = −32→31
275353 measured reflections	l = −38→37
28905 independent reflections

Refinement

Refinement on F^2	230 restraints
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.072	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.218	w = 1/[σ^2(Fo^2) + (0.126P)^2 + 11.3362P] where P = (Fo^2 + 2Fc^2)/3
S = 1.06	(Δ/σ)max = 0.003
28905 reflections	Δρmax = 1.82 e Å^−3
1761 parameters	Δρmin = −1.36 e Å^−3

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	Occ. (<1)
S1	0.53186 (4)	0.76049 (3)	0.52469 (2)	0.05164 (17)
O1	0.49363 (15)	0.79257 (10)	0.48831 (7)	0.0675 (6)
O2	0.60692 (15)	0.74289 (14)	0.51775 (9)	0.0867 (9)
O3	0.48248 (14)	0.71860 (9)	0.53551 (8)	0.0632 (6)
C1	0.54985 (14)	0.79917 (11)	0.57387 (8)	0.0421 (5)
C2	0.59267 (16)	0.77902 (12)	0.61378 (9)	0.0477 (6)
H2	0.613853	0.745351	0.614258	0.057*
C3	0.60386 (16)	0.80868 (12)	0.65259 (9)	0.0488 (6)
H3A	0.632680	0.794885	0.679806	0.059*
C4	0.57395 (15)	0.85826 (11)	0.65281 (8)	0.0439 (6)
C5	0.53287 (15)	0.87764 (11)	0.61263 (9)	0.0438 (5)
H5	0.512846	0.911641	0.611975	0.053*
C6	0.52032 (15)	0.84865 (11)	0.57341 (9)	0.0427 (5)
H6	0.491547	0.862589	0.546243	0.051*
C7	0.5840 (2)	0.88873 (14)	0.69596 (10)	0.0594 (8)
H7A	0.560284	0.870128	0.718303	0.089*
H7B	0.558959	0.922342	0.689972	0.089*
H7C	0.639434	0.893609	0.707753	0.089*
S2	0.25891 (4)	1.16160 (3)	0.82036 (2)	0.04608 (15)
O4	0.22584 (16)	1.11160 (9)	0.81247 (12)	0.0840 (9)
O5	0.32451 (14)	1.17040 (10)	0.79846 (8)	0.0672 (6)
O6	0.27660 (15)	1.17480 (10)	0.86789 (7)	0.0650 (6)
C8	0.18625 (16)	1.20624 (10)	0.79583 (9)	0.0449 (6)
C9	0.20576 (17)	1.24973 (11)	0.77407 (10)	0.0472 (6)
H9	0.258155	1.255567	0.771297	0.057*
C10	0.14951 (18)	1.28455 (11)	0.75645 (10)	0.0510 (6)
H10A	0.163716	1.313914	0.741006	0.061*
C11	0.07286 (18)	1.27821 (13)	0.76047 (10)	0.0543 (7)
C12	0.0541 (2)	1.23355 (14)	0.78177 (14)	0.0674 (9)
H12A	0.001662	1.227416	0.784216	0.081*
C13	0.10986 (19)	1.19810 (13)	0.79934 (13)	0.0610 (8)
H13G	0.095707	1.168047	0.813875	0.073*
C14	0.0132 (2)	1.31912 (16)	0.74432 (14)	0.0727 (10)
H14A	0.009061	1.342478	0.769365	0.109*
H14B	−0.037224	1.302860	0.733532	0.109*
H14C	0.028887	1.338587	0.719565	0.109*
S3	0.69437 (4)	0.88900 (3)	0.83806 (3)	0.04938 (16)
O7	0.64753 (15)	0.93317 (10)	0.84225 (10)	0.0761 (7)
O8	0.75279 (12)	0.89588 (8)	0.81033 (8)	0.0562 (5)
O9	0.72890 (16)	0.86845 (12)	0.88275 (8)	0.0782 (7)
C15	0.63121 (15)	0.84006 (9)	0.81198 (8)	0.0385 (5)
C16	0.55154 (15)	0.84341 (10)	0.80935 (9)	0.0412 (5)
H16	0.529541	0.872275	0.821728	0.049*
C17	0.50438 (15)	0.80436 (10)	0.78856 (9)	0.0441 (5)
H17	0.449910	0.806667	0.787006	0.053*
C18	0.53489 (16)	0.76189 (10)	0.76991 (9)	0.0434 (5)
C19	0.61523 (17)	0.75902 (10)	0.77348 (9)	0.0445 (6)
H19	0.637429	0.730154	0.761230	0.053*
C20	0.66302 (16)	0.79747 (10)	0.79454 (9)	0.0432 (5)
H20	0.717647	0.794699	0.797065	0.052*
C21	0.4838 (2)	0.71960 (13)	0.74680 (12)	0.0610 (8)
H21A	0.483020	0.690951	0.767908	0.092*
H21B	0.504031	0.707595	0.720317	0.092*
H21C	0.430968	0.732732	0.737136	0.092*
S4	0.33582 (4)	0.85231 (3)	0.86918 (3)	0.04993 (17)
O10	0.40391 (15)	0.87476 (12)	0.85730 (10)	0.0784 (7)
O11	0.35123 (19)	0.80527 (10)	0.89476 (9)	0.0808 (8)
O12	0.29201 (15)	0.88906 (11)	0.89051 (9)	0.0739 (7)
C22	0.27513 (16)	0.83596 (10)	0.81749 (10)	0.0460 (6)
C23	0.28192 (19)	0.78828 (11)	0.79753 (12)	0.0562 (7)
H23	0.316031	0.762944	0.812808	0.067*
C24	0.2385 (2)	0.77818 (13)	0.75525 (13)	0.0647 (8)
H24	0.242929	0.745516	0.741784	0.078*
C25	0.1889 (2)	0.81444 (15)	0.73207 (12)	0.0638 (8)
C26	0.1821 (2)	0.86131 (15)	0.75261 (12)	0.0634 (8)
H26	0.147824	0.886533	0.737333	0.076*
C27	0.22463 (18)	0.87219 (12)	0.79519 (11)	0.0547 (7)
H27	0.218970	0.904521	0.808959	0.066*
C28	0.1452 (3)	0.8047 (2)	0.68475 (14)	0.0959 (15)
H28A	0.175220	0.817876	0.662753	0.144*
H28B	0.094865	0.822157	0.680576	0.144*
H28C	0.136998	0.767602	0.680202	0.144*
S5	0.08495 (4)	1.25286 (3)	0.53743 (3)	0.05662 (19)
O13	0.0112 (11)	1.2450 (7)	0.5154 (6)	0.1038 (14)*	0.212 (2)
O14	0.0329 (3)	1.2897 (2)	0.54489 (17)	0.1141 (10)	0.788 (2)
O15	0.1541 (14)	1.2395 (8)	0.5179 (8)	0.1108 (14)*	0.212 (2)
O16	0.1549 (3)	1.2640 (2)	0.52543 (17)	0.1076 (10)	0.788 (2)
O17	0.0952 (12)	1.3075 (7)	0.5625 (6)	0.1067 (14)*	0.212 (2)
O18	0.0492 (3)	1.2191 (2)	0.49632 (17)	0.1186 (10)	0.788 (2)
C29	0.10040 (16)	1.21005 (12)	0.58400 (9)	0.0474 (6)
C30	0.06565 (16)	1.16222 (11)	0.58038 (9)	0.0478 (6)
H30	0.034247	1.151949	0.552641	0.057*
C31	0.0765 (2)	1.12926 (12)	0.61708 (10)	0.0558 (7)
H31	0.051576	1.096677	0.614624	0.067*
C32	0.1238 (2)	1.14351 (13)	0.65771 (10)	0.0646 (9)
C33	0.1577 (3)	1.19123 (14)	0.66037 (11)	0.0695 (10)
H33	0.189555	1.201491	0.687952	0.083*
C34	0.1468 (2)	1.22472 (13)	0.62426 (11)	0.0586 (7)
H34	0.170978	1.257562	0.626968	0.070*
C35	0.1362 (4)	1.10744 (19)	0.69811 (14)	0.1060 (18)
H35A	0.103203	1.077032	0.691105	0.159*
H35B	0.122808	1.125185	0.724394	0.159*
H35C	0.190727	1.096809	0.704902	0.159*
S6	−0.11125 (4)	1.15024 (3)	0.86308 (3)	0.0569 (2)
O19	−0.1593 (3)	1.12794 (13)	0.8908 (2)	0.177 (3)
O20	−0.1518 (2)	1.15976 (19)	0.81882 (13)	0.149 (2)
O21	−0.07218 (14)	1.19429 (9)	0.88325 (10)	0.0737 (7)
C36	−0.03834 (16)	1.10439 (11)	0.85876 (11)	0.0490 (6)
C37	−0.0063 (2)	1.07538 (14)	0.89554 (13)	0.0641 (8)
H37	−0.024258	1.078858	0.923375	0.077*
C38	0.0527 (2)	1.04075 (15)	0.89170 (16)	0.0750 (11)
H38	0.074870	1.020630	0.917183	0.090*
C39	0.0796 (2)	1.03509 (13)	0.85179 (17)	0.0722 (11)
C40	0.0466 (2)	1.06417 (12)	0.81565 (14)	0.0651 (9)
H40	0.064647	1.060515	0.787865	0.078*
C41	−0.01247 (18)	1.09898 (11)	0.81816 (12)	0.0531 (7)
H41	−0.034754	1.118738	0.792473	0.064*
C42	0.1433 (3)	0.99771 (18)	0.8477 (2)	0.115 (2)
H42A	0.175103	0.991817	0.877599	0.173*
H42B	0.175703	1.011844	0.827314	0.173*
H42C	0.120551	0.965069	0.835464	0.173*
O22	0.58662 (13)	1.09213 (10)	0.80864 (8)	0.0610 (5)
H22A	0.544031	1.104834	0.815131	0.091*
H22B	0.571073	1.071244	0.786214	0.091*
O23	0.63578 (14)	1.19827 (9)	0.58741 (8)	0.0623 (5)
H23A	0.640003	1.229868	0.596911	0.093*
H23B	0.600832	1.199445	0.562850	0.093*
O24	0.46644 (15)	1.13159 (12)	0.84568 (10)	0.0675 (6)
H24A	0.453 (3)	1.124 (2)	0.8672 (19)	0.101*
H24B	0.422 (3)	1.139 (2)	0.8316 (18)	0.101*
O25	0.07714 (14)	0.79025 (12)	0.57368 (10)	0.0789 (8)
H25A	0.039934	0.781767	0.551632	0.118*
H25B	0.090445	0.761507	0.587793	0.118*
O26	0.69112 (14)	1.15774 (12)	0.77223 (9)	0.0738 (7)
H26A	0.729128	1.162731	0.794776	0.111*
H26B	0.654023	1.145062	0.784462	0.111*
O27	0.09639 (16)	1.36066 (12)	0.64626 (11)	0.0789 (7)
H27A	0.144046	1.367828	0.658536	0.118*
H27B	0.096583	1.359886	0.617371	0.118*
O28	0.33071 (16)	0.70828 (13)	0.49152 (11)	0.0853 (8)
H28D	0.376576	0.715078	0.506929	0.128*
H28E	0.333932	0.676643	0.482675	0.128*
O29	0.52509 (18)	0.61952 (11)	0.56067 (11)	0.0781 (7)
H29A	0.507579	0.650279	0.553558	0.117*
H29B	0.575290	0.622802	0.565141	0.117*
O30	0.61416 (18)	1.15870 (16)	0.67537 (11)	0.0940 (10)
H30A	0.636379	1.165978	0.652553	0.141*
H30B	0.651297	1.160654	0.698863	0.141*
O31	0.5889 (2)	1.05145 (13)	0.97384 (13)	0.0982 (10)
H31A	0.548788	1.066878	0.958114	0.147*
H31B	0.592631	1.022810	0.959425	0.147*
O32	0.2497 (2)	1.05612 (16)	0.99534 (12)	0.1042 (11)
H32A	0.270036	1.067260	0.972875	0.156*
H32B	0.208189	1.039670	0.982573	0.156*
O33	0.6299 (2)	0.96391 (15)	0.93234 (13)	0.0984 (10)
H33A	0.639751	0.951018	0.907316	0.148*
H33B	0.665392	0.950903	0.953405	0.148*
O34	0.3185 (2)	1.09469 (16)	0.92875 (12)	0.1073 (12)
H34A	0.302 (4)	1.114 (2)	0.9047 (16)	0.161*
O35	0.0979 (3)	0.6725 (2)	0.5147 (2)	0.162 (2)
H35D	0.053521	0.660172	0.501365	0.243*
H35E	0.131663	0.647752	0.520148	0.243*
N1	0.18266 (17)	0.99360 (9)	0.15061 (7)	0.0510 (6)
N2	0.15817 (11)	1.03648 (7)	0.35706 (6)	0.0325 (4)
N3	0.15080 (12)	0.92559 (7)	0.35173 (6)	0.0348 (4)
H3	0.149397	0.948905	0.372792	0.042*
N4	0.15687 (11)	1.03307 (7)	0.45501 (6)	0.0317 (4)
H4	0.159713	1.009736	0.434170	0.038*
N5	0.14338 (11)	0.92261 (7)	0.44869 (6)	0.0320 (4)
N6	0.15395 (13)	1.27303 (8)	0.42017 (7)	0.0406 (4)
N7	0.10468 (13)	0.68667 (8)	0.39512 (8)	0.0457 (5)
N8	0.0423 (2)	0.96731 (14)	0.72831 (10)	0.0777 (9)
C43	0.17015 (15)	0.98727 (9)	0.24057 (8)	0.0371 (5)
C44	0.23330 (17)	0.96649 (10)	0.22473 (9)	0.0453 (6)
H44	0.273211	0.949542	0.245081	0.054*
C45	0.2380 (2)	0.97044 (11)	0.17969 (10)	0.0521 (7)
H45	0.281585	0.956394	0.169246	0.063*
C46	0.12130 (19)	1.01511 (11)	0.16459 (9)	0.0510 (7)
H46	0.082827	1.032259	0.143411	0.061*
C47	0.11390 (16)	1.01243 (10)	0.20940 (9)	0.0428 (5)
H47	0.070478	1.027726	0.219041	0.051*
C48	0.16390 (14)	0.98447 (9)	0.28922 (8)	0.0349 (5)
C49	0.16524 (13)	1.03132 (9)	0.31256 (8)	0.0337 (4)
C50	0.18024 (16)	1.08084 (9)	0.29414 (8)	0.0397 (5)
H50	0.188137	1.087591	0.264249	0.048*
C51	0.18091 (16)	1.11571 (9)	0.32751 (8)	0.0397 (5)
H51	0.189049	1.151701	0.325588	0.048*
C52	0.16681 (13)	1.08754 (9)	0.36680 (8)	0.0329 (4)
C53	0.1879 (3)	0.99629 (15)	0.10190 (10)	0.0746 (11)
H53A	0.242497	0.996357	0.098712	0.112*
H53B	0.162838	1.027880	0.088749	0.112*
H53C	0.161741	0.966400	0.086083	0.112*
C54	0.15833 (14)	0.93557 (9)	0.30782 (8)	0.0358 (5)
C55	0.15839 (16)	0.88726 (9)	0.28492 (9)	0.0422 (5)
H55	0.162705	0.882488	0.254135	0.051*
C56	0.15119 (16)	0.84953 (10)	0.31508 (9)	0.0423 (5)
H56	0.149923	0.813602	0.309219	0.051*
C57	0.14583 (14)	0.87352 (9)	0.35742 (8)	0.0359 (5)
C58	0.16497 (13)	1.11079 (8)	0.40871 (8)	0.0325 (4)
C59	0.15991 (13)	1.08523 (8)	0.44920 (7)	0.0321 (4)
C60	0.14865 (13)	1.02326 (9)	0.49871 (7)	0.0322 (4)
C61	0.14903 (15)	1.07140 (9)	0.52178 (8)	0.0379 (5)
H61	0.145522	1.076079	0.552689	0.045*
C62	0.15533 (15)	1.10927 (9)	0.49144 (8)	0.0382 (5)
H62	0.156472	1.145204	0.497257	0.046*
C63	0.13845 (14)	0.84803 (9)	0.39743 (8)	0.0349 (5)
C64	0.13690 (13)	0.87125 (9)	0.43956 (8)	0.0331 (4)
C65	0.12446 (14)	0.84353 (9)	0.47952 (8)	0.0371 (5)
H65	0.118423	0.807410	0.482131	0.044*
C66	0.12311 (14)	0.87873 (9)	0.51216 (8)	0.0361 (5)
H66	0.115640	0.872197	0.542168	0.043*
C67	0.13519 (12)	0.92844 (8)	0.49290 (7)	0.0318 (4)
C68	0.16376 (13)	1.16808 (8)	0.41077 (7)	0.0327 (4)
C69	0.22789 (15)	1.19692 (9)	0.42927 (9)	0.0415 (5)
H69	0.276422	1.180465	0.439007	0.050*
C70	0.22180 (16)	1.24947 (10)	0.43368 (9)	0.0442 (6)
H70	0.266187	1.269026	0.446418	0.053*
C71	0.09158 (16)	1.24655 (10)	0.40077 (11)	0.0507 (7)
H71	0.044129	1.264113	0.390508	0.061*
C72	0.09514 (15)	1.19416 (10)	0.39544 (11)	0.0486 (6)
H72	0.050467	1.175805	0.381218	0.058*
C73	0.13712 (12)	0.97484 (9)	0.51653 (7)	0.0317 (4)
C74	0.11960 (13)	0.97314 (9)	0.56359 (8)	0.0327 (4)
C75	0.04489 (19)	0.9716 (2)	0.56964 (11)	0.0935 (17)
H75	0.004386	0.971271	0.543906	0.112*
C76	0.02636 (19)	0.9704 (2)	0.61233 (11)	0.0930 (16)
H76	−0.026547	0.969962	0.615487	0.112*
C77	0.08224 (15)	0.96986 (10)	0.64956 (8)	0.0415 (5)
C78	0.1576 (2)	0.9707 (2)	0.64405 (11)	0.0933 (17)
H78	0.198139	0.969869	0.669766	0.112*
C79	0.17533 (18)	0.9727 (2)	0.60080 (10)	0.0816 (14)
H79	0.228135	0.973807	0.597472	0.098*
C80	0.12799 (14)	0.79131 (9)	0.39518 (8)	0.0357 (5)
C81	0.06172 (15)	0.76926 (10)	0.36969 (9)	0.0399 (5)
H81	0.023970	0.790427	0.351714	0.048*
C82	0.05095 (16)	0.71715 (10)	0.37051 (9)	0.0437 (5)
H82	0.005161	0.702394	0.353570	0.052*
C83	0.16890 (17)	0.70661 (10)	0.41994 (11)	0.0507 (6)
H83	0.205725	0.684427	0.437447	0.061*
C84	0.18245 (16)	0.75861 (10)	0.42052 (10)	0.0457 (6)
H84	0.228562	0.772276	0.438045	0.055*
C85	0.1458 (2)	1.32868 (10)	0.42798 (12)	0.0569 (7)
H85A	0.190264	1.340715	0.450169	0.085*
H85B	0.097888	1.334969	0.439497	0.085*
H85C	0.144004	1.347282	0.399440	0.085*
C86	0.06064 (19)	0.96860 (13)	0.69352 (10)	0.0549 (7)
C87	0.0924 (2)	0.63051 (11)	0.39532 (15)	0.0694 (10)
H87A	0.073495	0.620682	0.422845	0.104*
H87B	0.141578	0.612889	0.394541	0.104*
H87C	0.054154	0.620673	0.368710	0.104*
N9	0.41706 (14)	0.99415 (9)	0.86521 (7)	0.0456 (5)
N10	0.36110 (11)	1.04751 (7)	0.65230 (6)	0.0348 (4)
H10	0.356705	1.022426	0.632342	0.042*	0.5
N11	0.35920 (11)	0.93593 (7)	0.65610 (6)	0.0332 (4)
H11	0.358127	0.958783	0.634393	0.040*	0.5
N12	0.35214 (11)	1.04265 (7)	0.55401 (6)	0.0324 (4)
H12	0.343740	1.020191	0.574482	0.039*	0.5
N13	0.34355 (11)	0.93130 (7)	0.55806 (6)	0.0313 (4)
H13	0.348139	0.956189	0.578222	0.038*	0.5
N14	0.40448 (14)	1.28017 (8)	0.58402 (7)	0.0434 (5)
N15	0.32661 (13)	0.69527 (8)	0.59951 (8)	0.0415 (4)
N16	0.43887 (16)	0.96311 (12)	0.27675 (8)	0.0597 (7)
C88	0.39036 (15)	0.99671 (9)	0.77183 (8)	0.0380 (5)
C89	0.45949 (16)	0.97760 (10)	0.79657 (9)	0.0424 (5)
H89	0.498717	0.965336	0.781248	0.051*
C90	0.47117 (17)	0.97641 (11)	0.84288 (9)	0.0458 (6)
H90	0.518223	0.962841	0.859382	0.055*
C91	0.35190 (18)	1.01543 (12)	0.84274 (9)	0.0519 (7)
H91	0.315357	1.029519	0.859122	0.062*
C92	0.33708 (16)	1.01720 (12)	0.79632 (9)	0.0474 (6)
H92	0.290471	1.032397	0.780827	0.057*
C93	0.37540 (13)	0.99503 (9)	0.72146 (8)	0.0356 (5)
C94	0.36846 (14)	1.04209 (9)	0.69823 (8)	0.0361 (5)
C95	0.36182 (14)	1.09899 (9)	0.64313 (8)	0.0358 (5)
C96	0.36747 (17)	1.12720 (10)	0.68486 (9)	0.0441 (6)
H96	0.368090	1.163549	0.688107	0.053*
C97	0.37172 (17)	1.09228 (10)	0.71853 (8)	0.0444 (6)
H97	0.376064	1.099576	0.749864	0.053*
C98	0.4284 (2)	0.98801 (14)	0.91502 (10)	0.0608 (8)
H98A	0.409512	0.954094	0.922281	0.091*
H98B	0.399388	1.014815	0.927726	0.091*
H98C	0.483630	0.991044	0.927990	0.091*
C99	0.37006 (13)	0.94607 (9)	0.70158 (8)	0.0341 (4)
C100	0.36863 (15)	0.89828 (10)	0.72559 (8)	0.0396 (5)
H100	0.375188	0.894167	0.757466	0.048*
C101	0.35616 (15)	0.86020 (9)	0.69422 (8)	0.0387 (5)
H101	0.352039	0.824484	0.700044	0.046*
C102	0.35034 (13)	0.88396 (9)	0.65051 (8)	0.0334 (4)
C103	0.36153 (13)	1.12142 (9)	0.60088 (8)	0.0343 (4)
C104	0.35919 (13)	1.09447 (9)	0.55991 (8)	0.0335 (4)
C105	0.36043 (13)	1.03168 (9)	0.51062 (7)	0.0321 (4)
C106	0.37303 (15)	1.07918 (9)	0.48826 (8)	0.0376 (5)
H106	0.381025	1.082731	0.457991	0.045*
C107	0.37140 (15)	1.11782 (9)	0.51831 (8)	0.0382 (5)
H107	0.377193	1.153501	0.512964	0.046*
C108	0.33586 (12)	0.85781 (8)	0.60895 (8)	0.0325 (4)
C109	0.33251 (13)	0.88030 (8)	0.56600 (8)	0.0318 (4)
C110	0.32541 (14)	0.85265 (9)	0.52377 (8)	0.0361 (5)
H110	0.316337	0.816818	0.519466	0.043*
C111	0.33404 (14)	0.88718 (9)	0.49158 (8)	0.0358 (5)
H111	0.332420	0.880148	0.460399	0.043*
C112	0.34616 (12)	0.93659 (9)	0.51316 (7)	0.0312 (4)
C113	0.37400 (14)	1.17813 (9)	0.59837 (8)	0.0362 (5)
C114	0.31661 (16)	1.21052 (10)	0.57614 (9)	0.0425 (5)
H114	0.265908	1.197573	0.565524	0.051*
C115	0.33298 (17)	1.26131 (10)	0.56947 (10)	0.0469 (6)
H115	0.293308	1.283339	0.554393	0.056*
C116	0.45989 (16)	1.25037 (10)	0.60729 (10)	0.0458 (6)
H116	0.509669	1.264560	0.618276	0.055*
C117	0.44609 (15)	1.19950 (10)	0.61562 (9)	0.0426 (5)
H117	0.485530	1.179083	0.633043	0.051*
C118	0.35914 (12)	0.98260 (9)	0.49122 (7)	0.0311 (4)
C119	0.37530 (12)	0.97823 (8)	0.44438 (7)	0.0313 (4)
C120	0.43586 (17)	0.94755 (12)	0.43608 (10)	0.0356 (4)	0.788 (2)
H120	0.466258	0.929105	0.460293	0.043*	0.788 (2)
C121	0.45256 (17)	0.94348 (12)	0.39300 (10)	0.0362 (4)	0.788 (2)
H121	0.494262	0.922334	0.387849	0.043*	0.788 (2)
C122	0.40915 (14)	0.96984 (10)	0.35765 (8)	0.0388 (5)
C123	0.34749 (17)	1.00172 (12)	0.36528 (10)	0.0354 (4)	0.788 (2)
H123	0.317857	1.020566	0.341048	0.042*	0.788 (2)
C124	0.33088 (17)	1.00514 (11)	0.40823 (10)	0.0343 (4)	0.788 (2)
H124	0.288874	1.025962	0.413442	0.041*	0.788 (2)
C125	0.33058 (13)	0.80067 (9)	0.60911 (8)	0.0341 (4)
C126	0.39374 (14)	0.77053 (9)	0.62707 (8)	0.0370 (5)
H126	0.439514	0.786274	0.643068	0.044*
C127	0.39077 (15)	0.71818 (10)	0.62197 (9)	0.0402 (5)
H127	0.434535	0.697911	0.634444	0.048*
C128	0.26261 (15)	0.72319 (10)	0.58316 (10)	0.0442 (6)
H128	0.216970	0.706297	0.568320	0.053*
C129	0.26292 (14)	0.77559 (9)	0.58779 (9)	0.0408 (5)
H129	0.217478	0.794883	0.576590	0.049*
C130	0.4230 (2)	1.33331 (10)	0.57164 (11)	0.0582 (8)
H13A	0.432427	1.333737	0.540478	0.087*
H13B	0.469556	1.345272	0.592196	0.087*
H13C	0.379418	1.356041	0.574055	0.087*
C131	0.42579 (15)	0.96555 (11)	0.31283 (9)	0.0452 (6)
C132	0.3264 (2)	0.63915 (11)	0.59137 (12)	0.0570 (7)
H13D	0.360007	0.631261	0.569559	0.085*
H13E	0.273417	0.627758	0.579249	0.085*
H13F	0.345600	0.621259	0.619912	0.085*
C220	0.4487 (7)	0.9888 (4)	0.4359 (4)	0.0374 (6)*	0.212 (2)
H220	0.487902	1.000734	0.459800	0.045*	0.212 (2)
C221	0.4656 (7)	0.9822 (4)	0.3930 (4)	0.0377 (6)*	0.212 (2)
H221	0.517368	0.986486	0.388369	0.045*	0.212 (2)
C223	0.3392 (7)	0.9482 (4)	0.3667 (4)	0.0375 (6)*	0.212 (2)
H223	0.305519	0.929127	0.344316	0.045*	0.212 (2)
C224	0.3216 (7)	0.9557 (4)	0.4094 (4)	0.0375 (6)*	0.212 (2)
H224	0.272345	0.945413	0.415173	0.045*	0.212 (2)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
S1	0.0442 (3)	0.0695 (5)	0.0416 (3)	−0.0099 (3)	0.0087 (3)	−0.0112 (3)
O1	0.0790 (15)	0.0830 (16)	0.0370 (10)	−0.0255 (13)	0.0012 (10)	0.0003 (10)
O2	0.0545 (13)	0.139 (3)	0.0679 (15)	0.0012 (15)	0.0138 (11)	−0.0500 (17)
O3	0.0675 (14)	0.0580 (13)	0.0615 (13)	−0.0154 (11)	0.0049 (10)	−0.0061 (10)
C1	0.0347 (11)	0.0566 (15)	0.0362 (11)	−0.0077 (10)	0.0094 (9)	0.0015 (10)
C2	0.0450 (14)	0.0551 (16)	0.0434 (13)	0.0030 (12)	0.0090 (11)	0.0017 (11)
C3	0.0462 (14)	0.0625 (17)	0.0366 (12)	0.0000 (12)	0.0046 (10)	0.0046 (11)
C4	0.0429 (13)	0.0551 (15)	0.0357 (12)	−0.0097 (11)	0.0121 (10)	0.0012 (11)
C5	0.0418 (13)	0.0465 (14)	0.0452 (13)	−0.0067 (11)	0.0129 (10)	0.0055 (11)
C6	0.0369 (12)	0.0529 (15)	0.0381 (12)	−0.0075 (10)	0.0061 (9)	0.0082 (10)
C7	0.072 (2)	0.0642 (19)	0.0432 (14)	−0.0138 (16)	0.0146 (14)	−0.0062 (13)
S2	0.0493 (3)	0.0411 (3)	0.0499 (3)	−0.0017 (3)	0.0147 (3)	−0.0053 (3)
O4	0.0742 (16)	0.0372 (11)	0.132 (2)	−0.0006 (11)	−0.0048 (16)	−0.0077 (13)
O5	0.0589 (13)	0.0852 (17)	0.0638 (13)	0.0211 (12)	0.0283 (11)	0.0160 (12)
O6	0.0783 (15)	0.0730 (15)	0.0459 (11)	0.0096 (12)	0.0170 (10)	−0.0019 (10)
C8	0.0480 (14)	0.0418 (13)	0.0475 (14)	−0.0035 (11)	0.0159 (11)	−0.0115 (11)
C9	0.0498 (14)	0.0439 (14)	0.0511 (15)	−0.0046 (11)	0.0175 (12)	−0.0084 (11)
C10	0.0574 (16)	0.0448 (14)	0.0534 (15)	0.0009 (12)	0.0170 (13)	−0.0112 (12)
C11	0.0541 (16)	0.0568 (17)	0.0527 (15)	0.0054 (13)	0.0117 (13)	−0.0148 (13)
C12	0.0472 (16)	0.066 (2)	0.094 (3)	−0.0036 (15)	0.0243 (17)	−0.0078 (18)
C13	0.0557 (17)	0.0530 (17)	0.080 (2)	−0.0052 (14)	0.0265 (16)	−0.0003 (15)
C14	0.066 (2)	0.080 (2)	0.072 (2)	0.0217 (18)	0.0099 (17)	−0.0103 (19)
S3	0.0458 (3)	0.0467 (4)	0.0576 (4)	−0.0084 (3)	0.0148 (3)	−0.0085 (3)
O7	0.0642 (14)	0.0548 (13)	0.111 (2)	−0.0031 (11)	0.0191 (14)	−0.0274 (13)
O8	0.0517 (11)	0.0543 (12)	0.0658 (13)	−0.0137 (9)	0.0191 (10)	0.0003 (10)
O9	0.0783 (17)	0.098 (2)	0.0531 (13)	−0.0247 (15)	−0.0018 (12)	0.0017 (13)
C15	0.0424 (12)	0.0363 (12)	0.0383 (12)	−0.0023 (9)	0.0115 (9)	0.0038 (9)
C16	0.0432 (13)	0.0375 (12)	0.0450 (13)	0.0018 (10)	0.0133 (10)	0.0049 (10)
C17	0.0404 (12)	0.0450 (14)	0.0472 (13)	−0.0019 (10)	0.0088 (10)	0.0087 (11)
C18	0.0514 (14)	0.0393 (13)	0.0391 (12)	−0.0076 (11)	0.0074 (10)	0.0075 (10)
C19	0.0555 (15)	0.0363 (12)	0.0450 (13)	−0.0016 (11)	0.0178 (11)	0.0025 (10)
C20	0.0431 (13)	0.0382 (13)	0.0508 (14)	−0.0003 (10)	0.0154 (11)	0.0030 (10)
C21	0.0676 (19)	0.0530 (17)	0.0597 (18)	−0.0186 (15)	0.0044 (15)	−0.0009 (14)
S4	0.0469 (3)	0.0415 (3)	0.0631 (4)	−0.0005 (3)	0.0145 (3)	0.0013 (3)
O10	0.0588 (14)	0.0865 (18)	0.0943 (19)	−0.0242 (13)	0.0254 (13)	−0.0118 (15)
O11	0.105 (2)	0.0519 (13)	0.0761 (16)	0.0016 (13)	−0.0072 (15)	0.0117 (12)
O12	0.0691 (15)	0.0803 (17)	0.0721 (15)	0.0115 (13)	0.0125 (12)	−0.0224 (13)
C22	0.0441 (13)	0.0369 (13)	0.0609 (16)	−0.0010 (10)	0.0199 (12)	0.0003 (11)
C23	0.0620 (18)	0.0369 (14)	0.073 (2)	−0.0001 (12)	0.0212 (15)	−0.0009 (13)
C24	0.076 (2)	0.0504 (17)	0.074 (2)	−0.0104 (16)	0.0287 (18)	−0.0121 (15)
C25	0.0562 (17)	0.078 (2)	0.0610 (18)	−0.0147 (16)	0.0201 (15)	−0.0067 (16)
C26	0.0525 (17)	0.070 (2)	0.067 (2)	0.0065 (15)	0.0106 (15)	0.0030 (16)
C27	0.0503 (15)	0.0463 (15)	0.0697 (19)	0.0076 (12)	0.0168 (14)	−0.0004 (13)
C28	0.090 (3)	0.135 (4)	0.062 (2)	−0.024 (3)	0.012 (2)	−0.015 (3)
S5	0.0495 (4)	0.0648 (5)	0.0563 (4)	0.0080 (3)	0.0115 (3)	0.0158 (3)
O14	0.1238 (17)	0.1199 (17)	0.1107 (17)	0.0584 (15)	0.0534 (15)	0.0509 (15)
O16	0.1037 (16)	0.1274 (18)	0.1071 (16)	0.0487 (15)	0.0601 (14)	0.0760 (15)
O18	0.1257 (17)	0.1273 (17)	0.1147 (17)	0.0605 (15)	0.0535 (15)	0.0720 (15)
C29	0.0428 (13)	0.0565 (16)	0.0439 (13)	0.0079 (12)	0.0105 (11)	0.0002 (12)
C30	0.0455 (14)	0.0543 (16)	0.0438 (13)	0.0073 (12)	0.0086 (11)	−0.0052 (11)
C31	0.0709 (19)	0.0474 (15)	0.0513 (16)	0.0061 (14)	0.0172 (14)	−0.0063 (12)
C32	0.103 (3)	0.0507 (17)	0.0400 (14)	0.0149 (17)	0.0133 (16)	−0.0025 (12)
C33	0.102 (3)	0.062 (2)	0.0396 (15)	0.0025 (18)	−0.0006 (16)	−0.0111 (14)
C34	0.0682 (19)	0.0528 (17)	0.0527 (16)	0.0004 (14)	0.0058 (14)	−0.0057 (13)
C35	0.186 (6)	0.074 (3)	0.053 (2)	0.007 (3)	0.011 (3)	0.0122 (19)
S6	0.0446 (4)	0.0489 (4)	0.0796 (5)	−0.0063 (3)	0.0178 (3)	−0.0272 (4)
O19	0.183 (4)	0.0647 (19)	0.345 (7)	0.010 (2)	0.213 (5)	0.004 (3)
O20	0.102 (2)	0.201 (4)	0.116 (3)	0.094 (3)	−0.056 (2)	−0.102 (3)
O21	0.0611 (13)	0.0430 (11)	0.109 (2)	−0.0005 (10)	−0.0055 (13)	−0.0250 (12)
C36	0.0423 (13)	0.0417 (14)	0.0648 (17)	−0.0067 (11)	0.0142 (12)	−0.0120 (12)
C37	0.0615 (19)	0.0622 (19)	0.070 (2)	−0.0155 (15)	0.0159 (16)	−0.0029 (16)
C38	0.062 (2)	0.057 (2)	0.103 (3)	−0.0069 (16)	0.006 (2)	0.0242 (19)
C39	0.0519 (17)	0.0449 (16)	0.126 (3)	0.0000 (13)	0.033 (2)	0.0145 (19)
C40	0.0595 (18)	0.0453 (16)	0.101 (3)	−0.0021 (14)	0.0418 (18)	−0.0036 (16)
C41	0.0501 (15)	0.0421 (14)	0.0705 (19)	−0.0030 (12)	0.0198 (13)	−0.0023 (13)
C42	0.081 (3)	0.068 (3)	0.210 (7)	0.024 (2)	0.063 (4)	0.037 (3)
O22	0.0550 (12)	0.0731 (15)	0.0574 (12)	−0.0026 (11)	0.0174 (10)	−0.0185 (11)
O23	0.0659 (14)	0.0577 (13)	0.0615 (13)	−0.0008 (11)	0.0068 (10)	−0.0063 (10)
O24	0.0514 (12)	0.0867 (18)	0.0673 (15)	0.0051 (12)	0.0189 (11)	−0.0091 (13)
O25	0.0537 (13)	0.0935 (19)	0.0849 (18)	−0.0161 (13)	0.0008 (12)	0.0472 (15)
O26	0.0513 (13)	0.0848 (18)	0.0815 (17)	−0.0022 (12)	0.0017 (11)	0.0222 (14)
O27	0.0598 (14)	0.0734 (17)	0.102 (2)	−0.0140 (13)	0.0106 (14)	−0.0053 (16)
O28	0.0626 (15)	0.101 (2)	0.087 (2)	−0.0117 (14)	−0.0001 (13)	0.0235 (17)
O29	0.0787 (17)	0.0675 (16)	0.0871 (18)	−0.0067 (13)	0.0125 (15)	0.0054 (14)
O30	0.0711 (17)	0.141 (3)	0.0702 (17)	−0.0089 (18)	0.0132 (14)	0.0076 (19)
O31	0.090 (2)	0.0703 (18)	0.123 (3)	0.0016 (16)	−0.0107 (19)	0.0030 (18)
O32	0.120 (3)	0.101 (3)	0.094 (2)	0.007 (2)	0.026 (2)	0.0338 (19)
O33	0.092 (2)	0.107 (3)	0.095 (2)	0.0095 (18)	0.0146 (18)	−0.022 (2)
O34	0.101 (2)	0.132 (3)	0.096 (2)	0.034 (2)	0.0365 (19)	0.048 (2)
O35	0.102 (3)	0.224 (6)	0.147 (4)	0.028 (4)	−0.011 (3)	0.041 (4)
N1	0.0804 (17)	0.0397 (11)	0.0370 (11)	−0.0234 (11)	0.0216 (11)	−0.0056 (9)
N2	0.0370 (9)	0.0287 (9)	0.0331 (9)	0.0006 (7)	0.0102 (7)	0.0008 (7)
N3	0.0456 (11)	0.0283 (9)	0.0326 (9)	0.0002 (8)	0.0128 (8)	−0.0002 (7)
N4	0.0388 (9)	0.0269 (9)	0.0313 (9)	−0.0008 (7)	0.0113 (7)	0.0013 (7)
N5	0.0371 (9)	0.0281 (9)	0.0324 (9)	−0.0015 (7)	0.0102 (7)	0.0014 (7)
N6	0.0523 (12)	0.0273 (9)	0.0463 (11)	0.0025 (8)	0.0202 (9)	0.0038 (8)
N7	0.0495 (12)	0.0292 (10)	0.0606 (13)	−0.0018 (9)	0.0161 (10)	−0.0021 (9)
N8	0.094 (2)	0.097 (2)	0.0519 (15)	0.0238 (19)	0.0389 (16)	0.0097 (15)
C43	0.0483 (13)	0.0301 (11)	0.0346 (11)	−0.0057 (9)	0.0118 (9)	−0.0012 (9)
C44	0.0586 (15)	0.0395 (13)	0.0419 (13)	−0.0001 (11)	0.0198 (11)	−0.0012 (10)
C45	0.0747 (19)	0.0411 (14)	0.0479 (15)	−0.0082 (13)	0.0307 (14)	−0.0062 (11)
C46	0.0686 (18)	0.0436 (14)	0.0383 (13)	−0.0172 (13)	0.0032 (12)	0.0064 (11)
C47	0.0517 (14)	0.0370 (12)	0.0400 (12)	−0.0069 (10)	0.0094 (10)	0.0034 (10)
C48	0.0393 (11)	0.0328 (11)	0.0339 (11)	0.0002 (9)	0.0102 (9)	0.0022 (9)
C49	0.0376 (11)	0.0315 (11)	0.0334 (10)	−0.0001 (9)	0.0101 (9)	0.0026 (8)
C50	0.0541 (14)	0.0328 (11)	0.0349 (11)	−0.0012 (10)	0.0148 (10)	0.0044 (9)
C51	0.0548 (14)	0.0301 (11)	0.0361 (11)	−0.0032 (10)	0.0129 (10)	0.0040 (9)
C52	0.0366 (11)	0.0290 (10)	0.0344 (11)	−0.0002 (8)	0.0095 (8)	0.0033 (8)
C53	0.118 (3)	0.074 (2)	0.0370 (14)	−0.042 (2)	0.0290 (17)	−0.0083 (14)
C54	0.0443 (12)	0.0304 (11)	0.0344 (11)	−0.0007 (9)	0.0115 (9)	0.0000 (9)
C55	0.0578 (15)	0.0340 (12)	0.0376 (12)	−0.0005 (10)	0.0162 (11)	−0.0033 (9)
C56	0.0578 (15)	0.0310 (11)	0.0414 (12)	−0.0011 (10)	0.0173 (11)	−0.0021 (9)
C57	0.0425 (12)	0.0309 (11)	0.0361 (11)	−0.0006 (9)	0.0116 (9)	−0.0002 (9)
C58	0.0348 (11)	0.0291 (10)	0.0348 (11)	0.0002 (8)	0.0097 (8)	0.0021 (8)
C59	0.0362 (11)	0.0277 (10)	0.0335 (10)	0.0003 (8)	0.0090 (8)	0.0015 (8)
C60	0.0345 (10)	0.0299 (10)	0.0333 (10)	0.0013 (8)	0.0093 (8)	0.0010 (8)
C61	0.0484 (13)	0.0339 (11)	0.0339 (11)	0.0001 (10)	0.0145 (9)	−0.0019 (9)
C62	0.0510 (13)	0.0291 (11)	0.0366 (11)	0.0012 (9)	0.0139 (10)	−0.0008 (9)
C63	0.0376 (11)	0.0292 (11)	0.0391 (11)	0.0003 (8)	0.0106 (9)	0.0008 (9)
C64	0.0347 (11)	0.0300 (10)	0.0355 (11)	−0.0014 (8)	0.0086 (8)	0.0030 (8)
C65	0.0424 (12)	0.0298 (11)	0.0398 (12)	−0.0046 (9)	0.0098 (9)	0.0054 (9)
C66	0.0416 (12)	0.0340 (11)	0.0337 (11)	−0.0027 (9)	0.0094 (9)	0.0053 (9)
C67	0.0315 (10)	0.0307 (11)	0.0335 (10)	−0.0009 (8)	0.0070 (8)	0.0040 (8)
C68	0.0381 (11)	0.0296 (10)	0.0322 (10)	0.0014 (8)	0.0115 (8)	0.0032 (8)
C69	0.0378 (12)	0.0333 (12)	0.0513 (14)	0.0017 (9)	0.0031 (10)	0.0031 (10)
C70	0.0489 (14)	0.0328 (12)	0.0490 (14)	−0.0039 (10)	0.0038 (11)	0.0024 (10)
C71	0.0419 (13)	0.0350 (13)	0.0774 (19)	0.0083 (10)	0.0166 (13)	0.0129 (12)
C72	0.0374 (12)	0.0356 (13)	0.0714 (18)	0.0001 (10)	0.0063 (12)	0.0056 (12)
C73	0.0302 (10)	0.0339 (11)	0.0315 (10)	0.0001 (8)	0.0073 (8)	0.0027 (8)
C74	0.0348 (11)	0.0311 (10)	0.0339 (11)	−0.0006 (8)	0.0107 (8)	0.0018 (8)
C75	0.0348 (15)	0.210 (6)	0.0360 (15)	−0.012 (2)	0.0081 (12)	0.005 (2)
C76	0.0373 (15)	0.202 (5)	0.0435 (16)	−0.015 (2)	0.0178 (13)	0.005 (2)
C77	0.0470 (13)	0.0444 (13)	0.0365 (12)	0.0058 (10)	0.0165 (10)	0.0035 (10)
C78	0.0441 (16)	0.204 (5)	0.0323 (14)	0.033 (2)	0.0079 (12)	0.004 (2)
C79	0.0368 (14)	0.174 (4)	0.0357 (14)	0.021 (2)	0.0115 (11)	0.0034 (19)
C80	0.0395 (11)	0.0306 (11)	0.0395 (11)	0.0003 (9)	0.0138 (9)	−0.0003 (9)
C81	0.0442 (13)	0.0338 (12)	0.0422 (12)	0.0002 (10)	0.0091 (10)	−0.0018 (9)
C82	0.0441 (13)	0.0373 (13)	0.0505 (14)	−0.0027 (10)	0.0105 (11)	−0.0061 (10)
C83	0.0477 (14)	0.0332 (13)	0.0696 (18)	0.0061 (11)	0.0069 (13)	0.0047 (12)
C84	0.0408 (13)	0.0338 (12)	0.0610 (16)	−0.0004 (10)	0.0049 (11)	0.0006 (11)
C85	0.077 (2)	0.0290 (12)	0.0711 (19)	0.0051 (12)	0.0316 (16)	0.0017 (12)
C86	0.0629 (17)	0.0625 (18)	0.0440 (14)	0.0150 (14)	0.0223 (13)	0.0054 (13)
C87	0.072 (2)	0.0288 (14)	0.105 (3)	−0.0038 (13)	0.0101 (19)	−0.0006 (15)
N9	0.0573 (13)	0.0442 (12)	0.0366 (10)	−0.0089 (10)	0.0117 (9)	−0.0025 (9)
N10	0.0410 (10)	0.0319 (9)	0.0328 (9)	0.0021 (8)	0.0101 (8)	−0.0010 (7)
N11	0.0362 (9)	0.0323 (9)	0.0327 (9)	0.0016 (7)	0.0107 (7)	0.0007 (7)
N12	0.0372 (9)	0.0294 (9)	0.0317 (9)	−0.0002 (7)	0.0097 (7)	−0.0011 (7)
N13	0.0340 (9)	0.0288 (9)	0.0325 (9)	0.0009 (7)	0.0101 (7)	0.0009 (7)
N14	0.0598 (13)	0.0309 (10)	0.0437 (11)	−0.0040 (9)	0.0202 (10)	−0.0070 (8)
N15	0.0461 (11)	0.0316 (10)	0.0476 (11)	−0.0019 (8)	0.0109 (9)	0.0044 (8)
N16	0.0605 (15)	0.0810 (19)	0.0422 (12)	−0.0055 (13)	0.0215 (11)	−0.0090 (12)
C88	0.0425 (12)	0.0373 (12)	0.0364 (11)	−0.0015 (9)	0.0134 (9)	−0.0002 (9)
C89	0.0457 (13)	0.0437 (13)	0.0394 (12)	0.0024 (10)	0.0117 (10)	0.0010 (10)
C90	0.0523 (15)	0.0445 (14)	0.0399 (13)	−0.0008 (11)	0.0063 (11)	0.0014 (10)
C91	0.0549 (16)	0.0634 (18)	0.0418 (14)	−0.0030 (13)	0.0202 (12)	−0.0097 (12)
C92	0.0459 (14)	0.0584 (16)	0.0401 (13)	0.0059 (12)	0.0139 (11)	−0.0026 (11)
C93	0.0355 (11)	0.0385 (12)	0.0351 (11)	0.0028 (9)	0.0123 (9)	−0.0004 (9)
C94	0.0384 (11)	0.0364 (12)	0.0351 (11)	0.0027 (9)	0.0110 (9)	−0.0029 (9)
C95	0.0411 (12)	0.0323 (11)	0.0354 (11)	0.0034 (9)	0.0106 (9)	−0.0029 (9)
C96	0.0624 (16)	0.0326 (12)	0.0395 (12)	0.0046 (11)	0.0149 (11)	−0.0063 (10)
C97	0.0602 (16)	0.0398 (13)	0.0348 (12)	0.0061 (11)	0.0129 (11)	−0.0045 (10)
C98	0.083 (2)	0.0639 (19)	0.0352 (13)	−0.0098 (16)	0.0098 (14)	−0.0034 (12)
C99	0.0338 (10)	0.0354 (11)	0.0354 (11)	0.0016 (9)	0.0124 (8)	0.0032 (9)
C100	0.0472 (13)	0.0394 (12)	0.0349 (11)	−0.0004 (10)	0.0147 (10)	0.0043 (9)
C101	0.0447 (13)	0.0348 (12)	0.0391 (12)	−0.0015 (9)	0.0141 (10)	0.0051 (9)
C102	0.0333 (10)	0.0326 (11)	0.0360 (11)	0.0002 (8)	0.0109 (9)	0.0029 (8)
C103	0.0366 (11)	0.0305 (11)	0.0361 (11)	0.0025 (8)	0.0076 (9)	−0.0020 (8)
C104	0.0361 (11)	0.0308 (11)	0.0341 (11)	0.0008 (8)	0.0078 (8)	−0.0002 (8)
C105	0.0327 (10)	0.0316 (11)	0.0332 (10)	0.0003 (8)	0.0087 (8)	0.0009 (8)
C106	0.0467 (13)	0.0340 (11)	0.0334 (11)	−0.0021 (9)	0.0110 (9)	0.0032 (9)
C107	0.0485 (13)	0.0299 (11)	0.0370 (11)	−0.0027 (9)	0.0103 (10)	0.0020 (9)
C108	0.0308 (10)	0.0304 (10)	0.0376 (11)	−0.0005 (8)	0.0098 (8)	0.0017 (8)
C109	0.0314 (10)	0.0291 (10)	0.0359 (11)	0.0007 (8)	0.0083 (8)	−0.0002 (8)
C110	0.0409 (12)	0.0301 (11)	0.0379 (11)	−0.0029 (9)	0.0087 (9)	−0.0043 (9)
C111	0.0400 (12)	0.0344 (11)	0.0339 (11)	−0.0018 (9)	0.0088 (9)	−0.0041 (9)
C112	0.0295 (10)	0.0322 (11)	0.0327 (10)	0.0021 (8)	0.0078 (8)	−0.0005 (8)
C113	0.0432 (12)	0.0316 (11)	0.0352 (11)	0.0011 (9)	0.0107 (9)	−0.0032 (9)
C114	0.0439 (13)	0.0326 (12)	0.0505 (14)	0.0022 (10)	0.0072 (11)	−0.0020 (10)
C115	0.0557 (15)	0.0324 (12)	0.0523 (15)	0.0055 (11)	0.0093 (12)	−0.0016 (10)
C116	0.0471 (14)	0.0404 (13)	0.0517 (14)	−0.0070 (11)	0.0142 (11)	−0.0120 (11)
C117	0.0445 (13)	0.0390 (13)	0.0438 (13)	0.0011 (10)	0.0067 (10)	−0.0040 (10)
C118	0.0294 (10)	0.0327 (11)	0.0319 (10)	0.0015 (8)	0.0073 (8)	−0.0007 (8)
C119	0.0311 (10)	0.0326 (10)	0.0309 (10)	−0.0013 (8)	0.0080 (8)	−0.0012 (8)
C120	0.0347 (7)	0.0383 (7)	0.0347 (7)	0.0040 (7)	0.0085 (6)	0.0002 (6)
C121	0.0351 (7)	0.0389 (7)	0.0360 (7)	0.0043 (7)	0.0098 (6)	−0.0013 (7)
C122	0.0362 (11)	0.0484 (13)	0.0338 (11)	−0.0037 (10)	0.0115 (9)	−0.0042 (10)
C123	0.0351 (7)	0.0378 (7)	0.0340 (7)	0.0022 (7)	0.0084 (6)	0.0011 (6)
C124	0.0335 (7)	0.0365 (7)	0.0339 (7)	0.0031 (6)	0.0089 (6)	0.0003 (6)
C125	0.0351 (11)	0.0320 (11)	0.0372 (11)	−0.0010 (8)	0.0117 (9)	0.0036 (9)
C126	0.0359 (11)	0.0357 (12)	0.0398 (12)	−0.0024 (9)	0.0080 (9)	0.0029 (9)
C127	0.0399 (12)	0.0359 (12)	0.0453 (13)	0.0031 (9)	0.0095 (10)	0.0051 (10)
C128	0.0375 (12)	0.0371 (12)	0.0567 (15)	−0.0062 (10)	0.0055 (11)	0.0035 (11)
C129	0.0343 (11)	0.0348 (12)	0.0529 (14)	−0.0018 (9)	0.0069 (10)	0.0058 (10)
C130	0.087 (2)	0.0308 (13)	0.0631 (18)	−0.0093 (13)	0.0312 (16)	−0.0071 (12)
C131	0.0421 (13)	0.0566 (16)	0.0395 (13)	−0.0033 (11)	0.0144 (10)	−0.0034 (11)
C132	0.0635 (18)	0.0318 (13)	0.074 (2)	−0.0009 (12)	0.0089 (15)	−0.0012 (13)

Geometric parameters (Å, º)

S1—O1	1.440 (3)	C50—C51	1.350 (3)
S1—O2	1.444 (3)	C51—H51	0.9500
S1—O3	1.464 (2)	C51—C52	1.449 (3)
S1—C1	1.768 (3)	C52—C58	1.403 (3)
C1—C2	1.396 (4)	C53—H53A	0.9800
C1—C6	1.386 (4)	C53—H53B	0.9800
C2—H2	0.9500	C53—H53C	0.9800
C2—C3	1.382 (4)	C54—C55	1.432 (3)
C3—H3A	0.9500	C55—H55	0.9500
C3—C4	1.392 (4)	C55—C56	1.357 (4)
C4—C5	1.384 (4)	C56—H56	0.9500
C4—C7	1.502 (4)	C56—C57	1.435 (3)
C5—H5	0.9500	C57—C63	1.400 (3)
C5—C6	1.383 (4)	C58—C59	1.403 (3)
C6—H6	0.9500	C58—C68	1.491 (3)
C7—H7A	0.9800	C59—C62	1.431 (3)
C7—H7B	0.9800	C60—C61	1.430 (3)
C7—H7C	0.9800	C60—C73	1.397 (3)
S2—O4	1.426 (2)	C61—H61	0.9500
S2—O5	1.444 (2)	C61—C62	1.360 (3)
S2—O6	1.447 (2)	C62—H62	0.9500
S2—C8	1.781 (3)	C63—C64	1.407 (3)
C8—C9	1.380 (4)	C63—C80	1.486 (3)
C8—C13	1.379 (4)	C64—C65	1.451 (3)
C9—H9	0.9500	C65—H65	0.9500
C9—C10	1.372 (4)	C65—C66	1.345 (3)
C10—H10A	0.9500	C66—H66	0.9500
C10—C11	1.382 (4)	C66—C67	1.448 (3)
C11—C12	1.394 (5)	C67—C73	1.397 (3)
C11—C14	1.509 (5)	C68—C69	1.382 (3)
C12—H12A	0.9500	C68—C72	1.385 (3)
C12—C13	1.377 (5)	C69—H69	0.9500
C13—H13G	0.9500	C69—C70	1.379 (3)
C14—H14A	0.9800	C70—H70	0.9500
C14—H14B	0.9800	C71—H71	0.9500
C14—H14C	0.9800	C71—C72	1.374 (4)
S3—O7	1.431 (3)	C72—H72	0.9500
S3—O8	1.445 (2)	C73—C74	1.502 (3)
S3—O9	1.469 (3)	C74—C75	1.356 (4)
S3—C15	1.773 (3)	C74—C79	1.345 (4)
C15—C16	1.388 (4)	C75—H75	0.9500
C15—C20	1.385 (4)	C75—C76	1.380 (4)
C16—H16	0.9500	C76—H76	0.9500
C16—C17	1.385 (4)	C76—C77	1.347 (4)
C17—H17	0.9500	C77—C78	1.362 (4)
C17—C18	1.389 (4)	C77—C86	1.440 (3)
C18—C19	1.396 (4)	C78—H78	0.9500
C18—C21	1.506 (4)	C78—C79	1.392 (4)
C19—H19	0.9500	C79—H79	0.9500
C19—C20	1.382 (4)	C80—C81	1.394 (3)
C20—H20	0.9500	C80—C84	1.396 (4)
C21—H21A	0.9800	C81—H81	0.9500
C21—H21B	0.9800	C81—C82	1.369 (4)
C21—H21C	0.9800	C82—H82	0.9500
S4—O10	1.432 (2)	C83—H83	0.9500
S4—O11	1.443 (3)	C83—C84	1.372 (4)
S4—O12	1.447 (2)	C84—H84	0.9500
S4—C22	1.768 (3)	C85—H85A	0.9800
C22—C23	1.392 (4)	C85—H85B	0.9800
C22—C27	1.380 (4)	C85—H85C	0.9800
C23—H23	0.9500	C87—H87A	0.9800
C23—C24	1.382 (5)	C87—H87B	0.9800
C24—H24	0.9500	C87—H87C	0.9800
C24—C25	1.383 (5)	N9—C90	1.340 (4)
C25—C26	1.381 (5)	N9—C91	1.337 (4)
C25—C28	1.509 (5)	N9—C98	1.482 (3)
C26—H26	0.9500	N10—H10	0.8800
C26—C27	1.388 (5)	N10—C94	1.370 (3)
C27—H27	0.9500	N10—C95	1.367 (3)
C28—H28A	0.9800	N11—H11	0.8800
C28—H28B	0.9800	N11—C99	1.371 (3)
C28—H28C	0.9800	N11—C102	1.367 (3)
S5—O13	1.357 (19)	N12—H12	0.8800
S5—O14	1.370 (4)	N12—C104	1.361 (3)
S5—O15	1.48 (2)	N12—C105	1.368 (3)
S5—O16	1.371 (5)	N13—H13	0.8800
S5—O17	1.603 (19)	N13—C109	1.367 (3)
S5—O18	1.552 (7)	N13—C112	1.366 (3)
S5—C29	1.770 (3)	N14—C115	1.343 (4)
C29—C30	1.380 (4)	N14—C116	1.337 (4)
C29—C34	1.383 (4)	N14—C130	1.482 (3)
C30—H30	0.9500	N15—C127	1.342 (3)
C30—C31	1.382 (4)	N15—C128	1.352 (3)
C31—H31	0.9500	N15—C132	1.479 (3)
C31—C32	1.395 (5)	N16—C131	1.150 (3)
C32—C33	1.372 (5)	C88—C89	1.393 (4)
C32—C35	1.518 (5)	C88—C92	1.396 (3)
C33—H33	0.9500	C88—C93	1.489 (3)
C33—C34	1.377 (5)	C89—H89	0.9500
C34—H34	0.9500	C89—C90	1.370 (4)
C35—H35A	0.9800	C90—H90	0.9500
C35—H35B	0.9800	C91—H91	0.9500
C35—H35C	0.9800	C91—C92	1.372 (4)
S6—O19	1.414 (4)	C92—H92	0.9500
S6—O20	1.411 (4)	C93—C94	1.403 (3)
S6—O21	1.413 (2)	C93—C99	1.402 (3)
S6—C36	1.770 (3)	C94—C97	1.437 (3)
C36—C37	1.371 (5)	C95—C96	1.441 (3)
C36—C41	1.384 (4)	C95—C103	1.397 (3)
C37—H37	0.9500	C96—H96	0.9500
C37—C38	1.393 (6)	C96—C97	1.351 (4)
C38—H38	0.9500	C97—H97	0.9500
C38—C39	1.374 (6)	C98—H98A	0.9800
C39—C40	1.363 (6)	C98—H98B	0.9800
C39—C42	1.502 (5)	C98—H98C	0.9800
C40—H40	0.9500	C99—C100	1.439 (3)
C40—C41	1.389 (4)	C100—H100	0.9500
C41—H41	0.9500	C100—C101	1.357 (4)
C42—H42A	0.9800	C101—H101	0.9500
C42—H42B	0.9800	C101—C102	1.438 (3)
C42—H42C	0.9800	C102—C108	1.404 (3)
O22—H22A	0.8707	C103—C104	1.411 (3)
O22—H22B	0.8698	C103—C113	1.494 (3)
O23—H23A	0.8685	C104—C107	1.441 (3)
O23—H23B	0.8698	C105—C106	1.442 (3)
O24—H24A	0.75 (5)	C105—C118	1.401 (3)
O24—H24B	0.84 (6)	C106—H106	0.9500
O25—H25A	0.8695	C106—C107	1.354 (3)
O25—H25B	0.8699	C107—H107	0.9500
O26—H26A	0.8694	C108—C109	1.408 (3)
O26—H26B	0.8686	C108—C125	1.489 (3)
O27—H27A	0.8701	C109—C110	1.444 (3)
O27—H27B	0.8693	C110—H110	0.9500
O28—H28D	0.8701	C110—C111	1.348 (3)
O28—H28E	0.8695	C111—H111	0.9500
O29—H29A	0.8693	C111—C112	1.437 (3)
O29—H29B	0.8704	C112—C118	1.405 (3)
O30—H30A	0.8691	C113—C114	1.387 (4)
O30—H30B	0.8704	C113—C117	1.392 (4)
O31—H31A	0.8706	C114—H114	0.9500
O31—H31B	0.8699	C114—C115	1.374 (4)
O32—H32A	0.8689	C115—H115	0.9500
O32—H32B	0.8708	C116—H116	0.9500
O33—H33A	0.8689	C116—C117	1.375 (4)
O33—H33B	0.8707	C117—H117	0.9500
O34—H34A	0.88 (2)	C118—C119	1.490 (3)
O35—H35D	0.8698	C119—C120	1.387 (4)
O35—H35E	0.8694	C119—C124	1.403 (4)
N1—C45	1.327 (4)	C119—C220	1.385 (12)
N1—C46	1.346 (4)	C119—C224	1.404 (11)
N1—C53	1.485 (3)	C120—H120	0.9500
N2—C49	1.372 (3)	C120—C121	1.382 (4)
N2—C52	1.362 (3)	C121—H121	0.9500
N3—H3	0.8800	C121—C122	1.372 (4)
N3—C54	1.375 (3)	C122—C123	1.414 (4)
N3—C57	1.369 (3)	C122—C131	1.434 (3)
N4—H4	0.8800	C122—C221	1.353 (12)
N4—C59	1.370 (3)	C122—C223	1.422 (12)
N4—C60	1.371 (3)	C123—H123	0.9500
N5—C64	1.364 (3)	C123—C124	1.377 (4)
N5—C67	1.371 (3)	C124—H124	0.9500
N6—C70	1.334 (4)	C125—C126	1.384 (3)
N6—C71	1.334 (4)	C125—C129	1.402 (3)
N6—C85	1.477 (3)	C126—H126	0.9500
N7—C82	1.345 (4)	C126—C127	1.370 (3)
N7—C83	1.337 (4)	C127—H127	0.9500
N7—C87	1.476 (3)	C128—H128	0.9500
N8—C86	1.149 (4)	C128—C129	1.369 (4)
C43—C44	1.392 (4)	C129—H129	0.9500
C43—C47	1.393 (4)	C130—H13A	0.9800
C43—C48	1.488 (3)	C130—H13B	0.9800
C44—H44	0.9500	C130—H13C	0.9800
C44—C45	1.375 (4)	C132—H13D	0.9800
C45—H45	0.9500	C132—H13E	0.9800
C46—H46	0.9500	C132—H13F	0.9800
C46—C47	1.378 (4)	C220—H220	0.9500
C47—H47	0.9500	C220—C221	1.386 (16)
C48—C49	1.404 (3)	C221—H221	0.9500
C48—C54	1.399 (3)	C223—H223	0.9500
C49—C50	1.444 (3)	C223—C224	1.387 (16)
C50—H50	0.9500	C224—H224	0.9500
O1—S1—O2	112.60 (18)	N4—C60—C61	108.03 (19)
O1—S1—O3	112.77 (14)	N4—C60—C73	125.6 (2)
O1—S1—C1	107.03 (14)	C73—C60—C61	126.2 (2)
O2—S1—O3	112.83 (19)	C60—C61—H61	126.2
O2—S1—C1	105.81 (13)	C62—C61—C60	107.6 (2)
O3—S1—C1	105.08 (13)	C62—C61—H61	126.2
C2—C1—S1	119.4 (2)	C59—C62—H62	126.2
C6—C1—S1	120.7 (2)	C61—C62—C59	107.7 (2)
C6—C1—C2	119.9 (2)	C61—C62—H62	126.2
C1—C2—H2	120.4	C57—C63—C64	126.2 (2)
C3—C2—C1	119.2 (3)	C57—C63—C80	117.4 (2)
C3—C2—H2	120.4	C64—C63—C80	116.4 (2)
C2—C3—H3A	119.2	N5—C64—C63	125.9 (2)
C2—C3—C4	121.7 (3)	N5—C64—C65	109.85 (19)
C4—C3—H3A	119.2	C63—C64—C65	124.2 (2)
C3—C4—C7	120.5 (3)	C64—C65—H65	126.5
C5—C4—C3	118.0 (2)	C66—C65—C64	106.9 (2)
C5—C4—C7	121.5 (3)	C66—C65—H65	126.5
C4—C5—H5	119.3	C65—C66—H66	126.5
C6—C5—C4	121.5 (3)	C65—C66—C67	107.0 (2)
C6—C5—H5	119.3	C67—C66—H66	126.5
C1—C6—H6	120.1	N5—C67—C66	109.74 (19)
C5—C6—C1	119.8 (2)	N5—C67—C73	126.2 (2)
C5—C6—H6	120.1	C73—C67—C66	124.0 (2)
C4—C7—H7A	109.5	C69—C68—C58	122.8 (2)
C4—C7—H7B	109.5	C69—C68—C72	117.5 (2)
C4—C7—H7C	109.5	C72—C68—C58	119.6 (2)
H7A—C7—H7B	109.5	C68—C69—H69	119.8
H7A—C7—H7C	109.5	C70—C69—C68	120.3 (2)
H7B—C7—H7C	109.5	C70—C69—H69	119.8
O4—S2—O5	113.73 (18)	N6—C70—C69	120.4 (2)
O4—S2—O6	112.83 (18)	N6—C70—H70	119.8
O4—S2—C8	106.66 (15)	C69—C70—H70	119.8
O5—S2—O6	111.53 (16)	N6—C71—H71	119.6
O5—S2—C8	106.11 (13)	N6—C71—C72	120.8 (2)
O6—S2—C8	105.23 (13)	C72—C71—H71	119.6
C9—C8—S2	120.6 (2)	C68—C72—H72	119.9
C13—C8—S2	120.0 (2)	C71—C72—C68	120.1 (3)
C13—C8—C9	119.3 (3)	C71—C72—H72	119.9
C8—C9—H9	120.0	C60—C73—C74	117.1 (2)
C10—C9—C8	120.0 (3)	C67—C73—C60	125.1 (2)
C10—C9—H9	120.0	C67—C73—C74	117.60 (19)
C9—C10—H10A	119.0	C75—C74—C73	119.7 (2)
C9—C10—C11	122.0 (3)	C79—C74—C73	122.8 (2)
C11—C10—H10A	119.0	C79—C74—C75	117.5 (2)
C10—C11—C12	117.0 (3)	C74—C75—H75	119.3
C10—C11—C14	121.1 (3)	C74—C75—C76	121.5 (3)
C12—C11—C14	121.8 (3)	C76—C75—H75	119.3
C11—C12—H12A	119.2	C75—C76—H76	119.5
C13—C12—C11	121.6 (3)	C77—C76—C75	120.9 (3)
C13—C12—H12A	119.2	C77—C76—H76	119.5
C8—C13—H13G	120.0	C76—C77—C78	118.3 (3)
C12—C13—C8	120.0 (3)	C76—C77—C86	119.3 (3)
C12—C13—H13G	120.0	C78—C77—C86	122.4 (3)
C11—C14—H14A	109.5	C77—C78—H78	120.0
C11—C14—H14B	109.5	C77—C78—C79	120.1 (3)
C11—C14—H14C	109.5	C79—C78—H78	120.0
H14A—C14—H14B	109.5	C74—C79—C78	121.7 (3)
H14A—C14—H14C	109.5	C74—C79—H79	119.2
H14B—C14—H14C	109.5	C78—C79—H79	119.2
O7—S3—O8	115.48 (16)	C81—C80—C63	121.1 (2)
O7—S3—O9	111.04 (19)	C81—C80—C84	117.9 (2)
O7—S3—C15	107.00 (14)	C84—C80—C63	120.8 (2)
O8—S3—O9	110.78 (16)	C80—C81—H81	120.0
O8—S3—C15	106.58 (12)	C82—C81—C80	120.1 (2)
O9—S3—C15	105.27 (14)	C82—C81—H81	120.0
C16—C15—S3	121.4 (2)	N7—C82—C81	120.5 (2)
C20—C15—S3	118.6 (2)	N7—C82—H82	119.7
C20—C15—C16	120.0 (2)	C81—C82—H82	119.7
C15—C16—H16	120.3	N7—C83—H83	119.5
C17—C16—C15	119.5 (2)	N7—C83—C84	121.0 (3)
C17—C16—H16	120.3	C84—C83—H83	119.5
C16—C17—H17	119.2	C80—C84—H84	120.2
C16—C17—C18	121.5 (2)	C83—C84—C80	119.6 (3)
C18—C17—H17	119.2	C83—C84—H84	120.2
C17—C18—C19	118.0 (2)	N6—C85—H85A	109.5
C17—C18—C21	121.7 (3)	N6—C85—H85B	109.5
C19—C18—C21	120.3 (3)	N6—C85—H85C	109.5
C18—C19—H19	119.5	H85A—C85—H85B	109.5
C20—C19—C18	121.1 (3)	H85A—C85—H85C	109.5
C20—C19—H19	119.5	H85B—C85—H85C	109.5
C15—C20—H20	120.0	N8—C86—C77	178.9 (4)
C19—C20—C15	119.9 (2)	N7—C87—H87A	109.5
C19—C20—H20	120.0	N7—C87—H87B	109.5
C18—C21—H21A	109.5	N7—C87—H87C	109.5
C18—C21—H21B	109.5	H87A—C87—H87B	109.5
C18—C21—H21C	109.5	H87A—C87—H87C	109.5
H21A—C21—H21B	109.5	H87B—C87—H87C	109.5
H21A—C21—H21C	109.5	C90—N9—C98	119.5 (3)
H21B—C21—H21C	109.5	C91—N9—C90	120.5 (2)
O10—S4—O11	113.24 (19)	C91—N9—C98	120.0 (3)
O10—S4—O12	112.07 (17)	C94—N10—H10	126.2
O10—S4—C22	105.95 (15)	C95—N10—H10	126.2
O11—S4—O12	112.74 (18)	C95—N10—C94	107.54 (19)
O11—S4—C22	106.78 (15)	C99—N11—H11	126.1
O12—S4—C22	105.35 (14)	C102—N11—H11	126.1
C23—C22—S4	120.5 (2)	C102—N11—C99	107.73 (19)
C27—C22—S4	119.5 (2)	C104—N12—H12	126.0
C27—C22—C23	119.8 (3)	C104—N12—C105	107.91 (18)
C22—C23—H23	120.3	C105—N12—H12	126.0
C24—C23—C22	119.3 (3)	C109—N13—H13	126.2
C24—C23—H23	120.3	C112—N13—H13	126.2
C23—C24—H24	119.2	C112—N13—C109	107.54 (18)
C23—C24—C25	121.6 (3)	C115—N14—C130	119.5 (3)
C25—C24—H24	119.2	C116—N14—C115	120.4 (2)
C24—C25—C28	121.7 (4)	C116—N14—C130	120.0 (3)
C26—C25—C24	118.3 (3)	C127—N15—C128	120.6 (2)
C26—C25—C28	120.0 (4)	C127—N15—C132	119.9 (2)
C25—C26—H26	119.4	C128—N15—C132	119.5 (2)
C25—C26—C27	121.1 (3)	C89—C88—C92	117.1 (2)
C27—C26—H26	119.4	C89—C88—C93	120.5 (2)
C22—C27—C26	119.9 (3)	C92—C88—C93	122.4 (2)
C22—C27—H27	120.1	C88—C89—H89	119.8
C26—C27—H27	120.1	C90—C89—C88	120.3 (2)
C25—C28—H28A	109.5	C90—C89—H89	119.8
C25—C28—H28B	109.5	N9—C90—C89	120.9 (3)
C25—C28—H28C	109.5	N9—C90—H90	119.6
H28A—C28—H28B	109.5	C89—C90—H90	119.6
H28A—C28—H28C	109.5	N9—C91—H91	119.5
H28B—C28—H28C	109.5	N9—C91—C92	120.9 (3)
O13—S5—O15	123.2 (12)	C92—C91—H91	119.5
O13—S5—O17	112.2 (11)	C88—C92—H92	119.9
O13—S5—C29	106.7 (8)	C91—C92—C88	120.1 (3)
O14—S5—O16	123.4 (3)	C91—C92—H92	119.9
O14—S5—O18	110.0 (3)	C94—C93—C88	117.6 (2)
O14—S5—C29	108.7 (2)	C99—C93—C88	116.5 (2)
O15—S5—O17	111.3 (11)	C99—C93—C94	125.9 (2)
O15—S5—C29	98.5 (9)	N10—C94—C93	125.1 (2)
O16—S5—O18	99.2 (3)	N10—C94—C97	108.9 (2)
O16—S5—C29	108.95 (19)	C93—C94—C97	126.0 (2)
O17—S5—C29	101.5 (7)	N10—C95—C96	108.9 (2)
O18—S5—C29	104.80 (18)	N10—C95—C103	126.4 (2)
C30—C29—S5	120.2 (2)	C103—C95—C96	124.6 (2)
C30—C29—C34	119.9 (3)	C95—C96—H96	126.4
C34—C29—S5	119.9 (2)	C97—C96—C95	107.2 (2)
C29—C30—H30	120.0	C97—C96—H96	126.4
C29—C30—C31	120.1 (3)	C94—C97—H97	126.3
C31—C30—H30	120.0	C96—C97—C94	107.4 (2)
C30—C31—H31	119.8	C96—C97—H97	126.3
C30—C31—C32	120.5 (3)	N9—C98—H98A	109.5
C32—C31—H31	119.8	N9—C98—H98B	109.5
C31—C32—C35	120.8 (4)	N9—C98—H98C	109.5
C33—C32—C31	118.2 (3)	H98A—C98—H98B	109.5
C33—C32—C35	121.0 (4)	H98A—C98—H98C	109.5
C32—C33—H33	119.0	H98B—C98—H98C	109.5
C32—C33—C34	122.0 (3)	N11—C99—C93	125.9 (2)
C34—C33—H33	119.0	N11—C99—C100	108.8 (2)
C29—C34—H34	120.3	C93—C99—C100	125.2 (2)
C33—C34—C29	119.3 (3)	C99—C100—H100	126.4
C33—C34—H34	120.3	C101—C100—C99	107.3 (2)
C32—C35—H35A	109.5	C101—C100—H100	126.4
C32—C35—H35B	109.5	C100—C101—H101	126.4
C32—C35—H35C	109.5	C100—C101—C102	107.3 (2)
H35A—C35—H35B	109.5	C102—C101—H101	126.4
H35A—C35—H35C	109.5	N11—C102—C101	109.0 (2)
H35B—C35—H35C	109.5	N11—C102—C108	125.9 (2)
O19—S6—C36	106.47 (19)	C108—C102—C101	125.2 (2)
O20—S6—O19	112.0 (4)	C95—C103—C104	125.5 (2)
O20—S6—O21	112.6 (3)	C95—C103—C113	118.8 (2)
O20—S6—C36	107.22 (16)	C104—C103—C113	115.3 (2)
O21—S6—O19	112.0 (3)	N12—C104—C103	126.3 (2)
O21—S6—C36	106.07 (14)	N12—C104—C107	109.16 (19)
C37—C36—S6	120.4 (3)	C103—C104—C107	124.3 (2)
C37—C36—C41	120.2 (3)	N12—C105—C106	108.50 (19)
C41—C36—S6	119.4 (2)	N12—C105—C118	126.1 (2)
C36—C37—H37	120.3	C118—C105—C106	125.3 (2)
C36—C37—C38	119.3 (3)	C105—C106—H106	126.2
C38—C37—H37	120.3	C107—C106—C105	107.5 (2)
C37—C38—H38	119.3	C107—C106—H106	126.2
C39—C38—C37	121.3 (4)	C104—C107—H107	126.6
C39—C38—H38	119.3	C106—C107—C104	106.9 (2)
C38—C39—C42	121.3 (4)	C106—C107—H107	126.6
C40—C39—C38	118.2 (3)	C102—C108—C109	125.8 (2)
C40—C39—C42	120.5 (4)	C102—C108—C125	118.8 (2)
C39—C40—H40	119.0	C109—C108—C125	115.2 (2)
C39—C40—C41	122.1 (3)	N13—C109—C108	125.4 (2)
C41—C40—H40	119.0	N13—C109—C110	108.76 (19)
C36—C41—C40	118.8 (3)	C108—C109—C110	125.5 (2)
C36—C41—H41	120.6	C109—C110—H110	126.4
C40—C41—H41	120.6	C111—C110—C109	107.2 (2)
C39—C42—H42A	109.5	C111—C110—H110	126.4
C39—C42—H42B	109.5	C110—C111—H111	126.3
C39—C42—H42C	109.5	C110—C111—C112	107.3 (2)
H42A—C42—H42B	109.5	C112—C111—H111	126.3
H42A—C42—H42C	109.5	N13—C112—C111	109.11 (19)
H42B—C42—H42C	109.5	N13—C112—C118	126.0 (2)
H22A—O22—H22B	104.5	C118—C112—C111	124.9 (2)
H23A—O23—H23B	104.5	C114—C113—C103	121.6 (2)
H24A—O24—H24B	96 (5)	C114—C113—C117	117.9 (2)
H25A—O25—H25B	104.5	C117—C113—C103	120.4 (2)
H26A—O26—H26B	104.7	C113—C114—H114	120.0
H27A—O27—H27B	104.5	C115—C114—C113	120.1 (3)
H28D—O28—H28E	104.5	C115—C114—H114	120.0
H29A—O29—H29B	104.5	N14—C115—C114	120.7 (3)
H30A—O30—H30B	104.5	N14—C115—H115	119.6
H31A—O31—H31B	104.5	C114—C115—H115	119.6
H32A—O32—H32B	104.5	N14—C116—H116	119.4
H33A—O33—H33B	104.6	N14—C116—C117	121.2 (3)
H35D—O35—H35E	109.6	C117—C116—H116	119.4
C45—N1—C46	120.9 (2)	C113—C117—H117	120.2
C45—N1—C53	120.1 (3)	C116—C117—C113	119.6 (3)
C46—N1—C53	119.0 (3)	C116—C117—H117	120.2
C52—N2—C49	106.18 (18)	C105—C118—C112	124.9 (2)
C54—N3—H3	125.5	C105—C118—C119	118.11 (19)
C57—N3—H3	125.5	C112—C118—C119	116.97 (19)
C57—N3—C54	109.03 (19)	C120—C119—C118	119.9 (2)
C59—N4—H4	125.7	C120—C119—C124	118.9 (2)
C59—N4—C60	108.66 (18)	C124—C119—C118	121.3 (2)
C60—N4—H4	125.7	C220—C119—C118	120.1 (5)
C64—N5—C67	106.48 (18)	C220—C119—C224	117.7 (7)
C70—N6—C85	120.5 (2)	C224—C119—C118	121.4 (5)
C71—N6—C70	120.8 (2)	C119—C120—H120	119.6
C71—N6—C85	118.7 (2)	C121—C120—C119	120.8 (3)
C82—N7—C87	119.8 (3)	C121—C120—H120	119.6
C83—N7—C82	120.9 (2)	C120—C121—H121	119.9
C83—N7—C87	119.3 (3)	C122—C121—C120	120.3 (3)
C44—C43—C47	117.5 (2)	C122—C121—H121	119.9
C44—C43—C48	121.5 (2)	C121—C122—C123	120.0 (2)
C47—C43—C48	120.9 (2)	C121—C122—C131	120.6 (2)
C43—C44—H44	119.9	C123—C122—C131	119.4 (2)
C45—C44—C43	120.2 (3)	C221—C122—C131	120.8 (5)
C45—C44—H44	119.9	C221—C122—C223	118.5 (7)
N1—C45—C44	120.9 (3)	C223—C122—C131	118.7 (5)
N1—C45—H45	119.5	C122—C123—H123	120.4
C44—C45—H45	119.5	C124—C123—C122	119.2 (3)
N1—C46—H46	119.8	C124—C123—H123	120.4
N1—C46—C47	120.5 (3)	C119—C124—H124	119.6
C47—C46—H46	119.8	C123—C124—C119	120.7 (3)
C43—C47—H47	120.0	C123—C124—H124	119.6
C46—C47—C43	120.0 (3)	C126—C125—C108	121.4 (2)
C46—C47—H47	120.0	C126—C125—C129	117.7 (2)
C49—C48—C43	116.8 (2)	C129—C125—C108	120.7 (2)
C54—C48—C43	117.4 (2)	C125—C126—H126	119.7
C54—C48—C49	125.8 (2)	C127—C126—C125	120.5 (2)
N2—C49—C48	125.1 (2)	C127—C126—H126	119.7
N2—C49—C50	110.0 (2)	N15—C127—C126	120.6 (2)
C48—C49—C50	124.7 (2)	N15—C127—H127	119.7
C49—C50—H50	126.5	C126—C127—H127	119.7
C51—C50—C49	106.9 (2)	N15—C128—H128	119.7
C51—C50—H50	126.5	N15—C128—C129	120.6 (2)
C50—C51—H51	126.7	C129—C128—H128	119.7
C50—C51—C52	106.6 (2)	C125—C129—H129	120.1
C52—C51—H51	126.7	C128—C129—C125	119.8 (2)
N2—C52—C51	110.3 (2)	C128—C129—H129	120.1
N2—C52—C58	126.4 (2)	N14—C130—H13A	109.5
C58—C52—C51	123.3 (2)	N14—C130—H13B	109.5
N1—C53—H53A	109.5	N14—C130—H13C	109.5
N1—C53—H53B	109.5	H13A—C130—H13B	109.5
N1—C53—H53C	109.5	H13A—C130—H13C	109.5
H53A—C53—H53B	109.5	H13B—C130—H13C	109.5
H53A—C53—H53C	109.5	N16—C131—C122	178.7 (3)
H53B—C53—H53C	109.5	N15—C132—H13D	109.5
N3—C54—C48	125.5 (2)	N15—C132—H13E	109.5
N3—C54—C55	107.7 (2)	N15—C132—H13F	109.5
C48—C54—C55	126.7 (2)	H13D—C132—H13E	109.5
C54—C55—H55	126.1	H13D—C132—H13F	109.5
C56—C55—C54	107.7 (2)	H13E—C132—H13F	109.5
C56—C55—H55	126.1	C119—C220—H220	119.7
C55—C56—H56	126.1	C119—C220—C221	120.6 (10)
C55—C56—C57	107.9 (2)	C221—C220—H220	119.7
C57—C56—H56	126.1	C122—C221—C220	120.7 (10)
N3—C57—C56	107.6 (2)	C122—C221—H221	119.6
N3—C57—C63	126.4 (2)	C220—C221—H221	119.6
C63—C57—C56	126.0 (2)	C122—C223—H223	121.1
C52—C58—C59	126.2 (2)	C224—C223—C122	117.8 (9)
C52—C58—C68	118.07 (19)	C224—C223—H223	121.1
C59—C58—C68	115.69 (19)	C119—C224—H224	119.4
N4—C59—C58	126.1 (2)	C223—C224—C119	121.3 (10)
N4—C59—C62	108.03 (19)	C223—C224—H224	119.4
C58—C59—C62	125.8 (2)
S1—C1—C2—C3	−177.4 (2)	C63—C80—C81—C82	−175.7 (2)
S1—C1—C6—C5	177.84 (19)	C63—C80—C84—C83	176.0 (3)
O1—S1—C1—C2	−174.5 (2)	C64—N5—C67—C66	0.0 (2)
O1—S1—C1—C6	7.1 (2)	C64—N5—C67—C73	−179.4 (2)
O2—S1—C1—C2	−54.2 (3)	C64—C63—C80—C81	112.3 (3)
O2—S1—C1—C6	127.4 (2)	C64—C63—C80—C84	−64.3 (3)
O3—S1—C1—C2	65.4 (2)	C64—C65—C66—C67	−0.4 (3)
O3—S1—C1—C6	−113.0 (2)	C65—C66—C67—N5	0.3 (3)
C1—C2—C3—C4	−0.4 (4)	C65—C66—C67—C73	179.6 (2)
C2—C1—C6—C5	−0.6 (4)	C66—C67—C73—C60	−180.0 (2)
C2—C3—C4—C5	−0.7 (4)	C66—C67—C73—C74	−4.8 (3)
C2—C3—C4—C7	177.3 (3)	C67—N5—C64—C63	177.2 (2)
C3—C4—C5—C6	1.2 (4)	C67—N5—C64—C65	−0.2 (3)
C4—C5—C6—C1	−0.6 (4)	C67—C73—C74—C75	−80.9 (4)
C6—C1—C2—C3	1.1 (4)	C67—C73—C74—C79	98.6 (4)
C7—C4—C5—C6	−176.8 (3)	C68—C58—C59—N4	177.3 (2)
S2—C8—C9—C10	−178.2 (2)	C68—C58—C59—C62	−1.3 (3)
S2—C8—C13—C12	177.7 (3)	C68—C69—C70—N6	0.1 (4)
O4—S2—C8—C9	−142.1 (3)	C69—C68—C72—C71	−3.0 (4)
O4—S2—C8—C13	39.3 (3)	C70—N6—C71—C72	1.9 (4)
O5—S2—C8—C9	−20.5 (3)	C71—N6—C70—C69	−2.4 (4)
O5—S2—C8—C13	160.9 (3)	C72—C68—C69—C70	2.5 (4)
O6—S2—C8—C9	97.8 (2)	C73—C60—C61—C62	−174.8 (2)
O6—S2—C8—C13	−80.8 (3)	C73—C74—C75—C76	−179.5 (4)
C8—C9—C10—C11	1.3 (4)	C73—C74—C79—C78	−179.4 (4)
C9—C8—C13—C12	−0.9 (5)	C74—C75—C76—C77	−1.2 (9)
C9—C10—C11—C12	−2.5 (4)	C75—C74—C79—C78	0.0 (7)
C9—C10—C11—C14	174.8 (3)	C75—C76—C77—C78	0.2 (8)
C10—C11—C12—C13	2.1 (5)	C75—C76—C77—C86	−180.0 (5)
C11—C12—C13—C8	−0.4 (6)	C76—C77—C78—C79	0.8 (7)
C13—C8—C9—C10	0.4 (4)	C77—C78—C79—C74	−1.0 (8)
C14—C11—C12—C13	−175.3 (3)	C79—C74—C75—C76	1.0 (7)
S3—C15—C16—C17	179.81 (19)	C80—C63—C64—N5	−178.3 (2)
S3—C15—C20—C19	−179.1 (2)	C80—C63—C64—C65	−1.2 (3)
O7—S3—C15—C16	−15.5 (3)	C80—C81—C82—N7	−1.3 (4)
O7—S3—C15—C20	165.3 (2)	C81—C80—C84—C83	−0.7 (4)
O8—S3—C15—C16	−139.6 (2)	C82—N7—C83—C84	−1.0 (4)
O8—S3—C15—C20	41.2 (2)	C83—N7—C82—C81	1.3 (4)
O9—S3—C15—C16	102.7 (2)	C84—C80—C81—C82	1.0 (4)
O9—S3—C15—C20	−76.5 (2)	C85—N6—C70—C69	175.4 (3)
C15—C16—C17—C18	−0.4 (4)	C85—N6—C71—C72	−175.8 (3)
C16—C15—C20—C19	1.7 (4)	C86—C77—C78—C79	−179.0 (4)
C16—C17—C18—C19	1.3 (4)	C87—N7—C82—C81	−179.5 (3)
C16—C17—C18—C21	−179.3 (3)	C87—N7—C83—C84	179.8 (3)
C17—C18—C19—C20	−0.6 (4)	N9—C91—C92—C88	−0.1 (5)
C18—C19—C20—C15	−0.9 (4)	N10—C94—C97—C96	−0.9 (3)
C20—C15—C16—C17	−1.1 (4)	N10—C95—C96—C97	1.3 (3)
C21—C18—C19—C20	180.0 (3)	N10—C95—C103—C104	1.1 (4)
S4—C22—C23—C24	−174.4 (2)	N10—C95—C103—C113	−171.2 (2)
S4—C22—C27—C26	173.9 (2)	N11—C99—C100—C101	−0.6 (3)
O10—S4—C22—C23	88.3 (3)	N11—C102—C108—C109	4.0 (4)
O10—S4—C22—C27	−87.0 (3)	N11—C102—C108—C125	177.8 (2)
O11—S4—C22—C23	−32.7 (3)	N12—C104—C107—C106	−1.2 (3)
O11—S4—C22—C27	152.1 (3)	N12—C105—C106—C107	−0.6 (3)
O12—S4—C22—C23	−152.8 (3)	N12—C105—C118—C112	2.5 (4)
O12—S4—C22—C27	32.0 (3)	N12—C105—C118—C119	−175.4 (2)
C22—C23—C24—C25	0.5 (5)	N13—C109—C110—C111	1.4 (3)
C23—C22—C27—C26	−1.3 (5)	N13—C112—C118—C105	−9.7 (4)
C23—C24—C25—C26	−1.3 (5)	N13—C112—C118—C119	168.2 (2)
C23—C24—C25—C28	176.2 (4)	N14—C116—C117—C113	2.0 (4)
C24—C25—C26—C27	0.7 (5)	N15—C128—C129—C125	0.9 (4)
C25—C26—C27—C22	0.6 (5)	C88—C89—C90—N9	−0.9 (4)
C27—C22—C23—C24	0.8 (4)	C88—C93—C94—N10	174.3 (2)
C28—C25—C26—C27	−176.8 (3)	C88—C93—C94—C97	−2.4 (4)
S5—C29—C30—C31	−178.7 (2)	C88—C93—C99—N11	−177.7 (2)
S5—C29—C34—C33	179.3 (3)	C88—C93—C99—C100	7.8 (3)
O13—S5—C29—C30	34.1 (9)	C89—C88—C92—C91	−3.5 (4)
O13—S5—C29—C34	−145.3 (9)	C89—C88—C93—C94	−115.6 (3)
O14—S5—C29—C30	103.0 (4)	C89—C88—C93—C99	64.0 (3)
O14—S5—C29—C34	−76.4 (4)	C90—N9—C91—C92	3.4 (4)
O15—S5—C29—C30	−94.4 (8)	C91—N9—C90—C89	−2.9 (4)
O15—S5—C29—C34	86.2 (9)	C92—C88—C89—C90	4.0 (4)
O16—S5—C29—C30	−120.0 (4)	C92—C88—C93—C94	64.3 (3)
O16—S5—C29—C34	60.6 (4)	C92—C88—C93—C99	−116.1 (3)
O17—S5—C29—C30	151.7 (8)	C93—C88—C89—C90	−176.1 (2)
O17—S5—C29—C34	−27.7 (8)	C93—C88—C92—C91	176.6 (3)
O18—S5—C29—C30	−14.6 (3)	C93—C94—C97—C96	176.3 (3)
O18—S5—C29—C34	166.0 (3)	C93—C99—C100—C101	174.7 (2)
C29—C30—C31—C32	−1.3 (5)	C94—N10—C95—C96	−1.8 (3)
C30—C29—C34—C33	−0.1 (5)	C94—N10—C95—C103	174.9 (2)
C30—C31—C32—C33	1.3 (5)	C94—C93—C99—N11	1.8 (4)
C30—C31—C32—C35	−179.8 (4)	C94—C93—C99—C100	−172.6 (2)
C31—C32—C33—C34	−0.6 (6)	C95—N10—C94—C93	−175.5 (2)
C32—C33—C34—C29	0.1 (6)	C95—N10—C94—C97	1.7 (3)
C34—C29—C30—C31	0.7 (4)	C95—C96—C97—C94	−0.2 (3)
C35—C32—C33—C34	−179.6 (4)	C95—C103—C104—N12	4.2 (4)
S6—C36—C37—C38	−177.9 (3)	C95—C103—C104—C107	−169.6 (2)
S6—C36—C41—C40	177.8 (2)	C95—C103—C113—C114	−115.5 (3)
O19—S6—C36—C37	−38.8 (4)	C95—C103—C113—C117	69.2 (3)
O19—S6—C36—C41	142.8 (4)	C96—C95—C103—C104	177.3 (2)
O20—S6—C36—C37	−158.9 (3)	C96—C95—C103—C113	5.0 (4)
O20—S6—C36—C41	22.7 (4)	C98—N9—C90—C89	174.5 (3)
O21—S6—C36—C37	80.6 (3)	C98—N9—C91—C92	−174.0 (3)
O21—S6—C36—C41	−97.8 (3)	C99—N11—C102—C101	−0.3 (3)
C36—C37—C38—C39	0.0 (5)	C99—N11—C102—C108	178.2 (2)
C37—C36—C41—C40	−0.6 (4)	C99—C93—C94—N10	−5.2 (4)
C37—C38—C39—C40	−0.4 (6)	C99—C93—C94—C97	178.1 (2)
C37—C38—C39—C42	−180.0 (4)	C99—C100—C101—C102	0.4 (3)
C38—C39—C40—C41	0.2 (5)	C100—C101—C102—N11	−0.1 (3)
C39—C40—C41—C36	0.3 (5)	C100—C101—C102—C108	−178.6 (2)
C41—C36—C37—C38	0.4 (5)	C101—C102—C108—C109	−177.8 (2)
C42—C39—C40—C41	179.8 (4)	C101—C102—C108—C125	−3.9 (3)
N1—C46—C47—C43	−0.1 (4)	C102—N11—C99—C93	−174.7 (2)
N2—C49—C50—C51	−0.9 (3)	C102—N11—C99—C100	0.5 (3)
N2—C52—C58—C59	5.3 (4)	C102—C108—C109—N13	0.6 (4)
N2—C52—C58—C68	−171.0 (2)	C102—C108—C109—C110	173.4 (2)
N3—C54—C55—C56	−0.2 (3)	C102—C108—C125—C126	−64.2 (3)
N3—C57—C63—C64	−1.8 (4)	C102—C108—C125—C129	120.9 (3)
N3—C57—C63—C80	175.5 (2)	C103—C95—C96—C97	−175.5 (2)
N4—C59—C62—C61	−0.5 (3)	C103—C104—C107—C106	173.5 (2)
N4—C60—C61—C62	1.6 (3)	C103—C113—C114—C115	−171.8 (2)
N4—C60—C73—C67	2.7 (4)	C103—C113—C117—C116	170.6 (2)
N4—C60—C73—C74	−172.5 (2)	C104—N12—C105—C106	−0.2 (3)
N5—C64—C65—C66	0.4 (3)	C104—N12—C105—C118	178.2 (2)
N5—C67—C73—C60	−0.7 (4)	C104—C103—C113—C114	71.4 (3)
N5—C67—C73—C74	174.5 (2)	C104—C103—C113—C117	−103.9 (3)
N6—C71—C72—C68	0.8 (5)	C105—N12—C104—C103	−173.7 (2)
N7—C83—C84—C80	0.7 (5)	C105—N12—C104—C107	0.9 (3)
C43—C44—C45—N1	−0.5 (4)	C105—C106—C107—C104	1.1 (3)
C43—C48—C49—N2	178.2 (2)	C105—C118—C119—C120	122.3 (3)
C43—C48—C49—C50	−6.8 (4)	C105—C118—C119—C124	−56.9 (3)
C43—C48—C54—N3	−178.8 (2)	C105—C118—C119—C220	68.0 (6)
C43—C48—C54—C55	0.4 (4)	C105—C118—C119—C224	−122.4 (6)
C44—C43—C47—C46	1.3 (4)	C106—C105—C118—C112	−179.4 (2)
C44—C43—C48—C49	115.7 (3)	C106—C105—C118—C119	2.7 (3)
C44—C43—C48—C54	−63.4 (3)	C108—C109—C110—C111	−172.4 (2)
C45—N1—C46—C47	−1.5 (4)	C108—C125—C126—C127	−171.9 (2)
C46—N1—C45—C44	1.8 (4)	C108—C125—C129—C128	171.5 (2)
C47—C43—C44—C45	−1.0 (4)	C109—N13—C112—C111	1.7 (2)
C47—C43—C48—C49	−62.1 (3)	C109—N13—C112—C118	−177.8 (2)
C47—C43—C48—C54	118.7 (3)	C109—C108—C125—C126	110.3 (3)
C48—C43—C44—C45	−178.9 (2)	C109—C108—C125—C129	−64.6 (3)
C48—C43—C47—C46	179.2 (2)	C109—C110—C111—C112	−0.3 (3)
C48—C49—C50—C51	−176.6 (2)	C110—C111—C112—N13	−0.9 (3)
C48—C54—C55—C56	−179.4 (3)	C110—C111—C112—C118	178.7 (2)
C49—N2—C52—C51	−0.8 (3)	C111—C112—C118—C105	170.8 (2)
C49—N2—C52—C58	−179.1 (2)	C111—C112—C118—C119	−11.3 (3)
C49—C48—C54—N3	2.2 (4)	C112—N13—C109—C108	171.9 (2)
C49—C48—C54—C55	−178.7 (3)	C112—N13—C109—C110	−1.9 (2)
C49—C50—C51—C52	0.4 (3)	C112—C118—C119—C120	−55.7 (3)
C50—C51—C52—N2	0.3 (3)	C112—C118—C119—C124	125.1 (2)
C50—C51—C52—C58	178.6 (2)	C112—C118—C119—C220	−110.0 (6)
C51—C52—C58—C59	−172.7 (2)	C112—C118—C119—C224	59.6 (6)
C51—C52—C58—C68	10.9 (3)	C113—C103—C104—N12	176.8 (2)
C52—N2—C49—C48	176.7 (2)	C113—C103—C104—C107	3.0 (3)
C52—N2—C49—C50	1.1 (3)	C113—C114—C115—N14	0.4 (4)
C52—C58—C59—N4	0.9 (4)	C114—C113—C117—C116	−4.8 (4)
C52—C58—C59—C62	−177.7 (2)	C115—N14—C116—C117	2.2 (4)
C52—C58—C68—C69	−104.8 (3)	C116—N14—C115—C114	−3.4 (4)
C52—C58—C68—C72	78.0 (3)	C117—C113—C114—C115	3.7 (4)
C53—N1—C45—C44	−178.4 (3)	C118—C105—C106—C107	−179.0 (2)
C53—N1—C46—C47	178.7 (3)	C118—C119—C120—C121	−179.1 (3)
C54—N3—C57—C56	0.5 (3)	C118—C119—C124—C123	178.5 (2)
C54—N3—C57—C63	179.3 (2)	C118—C119—C220—C221	176.5 (8)
C54—C48—C49—N2	−2.7 (4)	C118—C119—C224—C223	−175.1 (8)
C54—C48—C49—C50	172.3 (2)	C119—C120—C121—C122	−0.1 (5)
C54—C55—C56—C57	0.5 (3)	C119—C220—C221—C122	6.0 (16)
C55—C56—C57—N3	−0.6 (3)	C120—C119—C124—C123	−0.7 (4)
C55—C56—C57—C63	−179.4 (3)	C120—C121—C122—C123	0.6 (4)
C56—C57—C63—C64	176.7 (2)	C120—C121—C122—C131	−179.6 (3)
C56—C57—C63—C80	−6.0 (4)	C121—C122—C123—C124	−1.2 (4)
C57—N3—C54—C48	179.0 (2)	C122—C123—C124—C119	1.2 (4)
C57—N3—C54—C55	−0.2 (3)	C122—C223—C224—C119	−7.9 (15)
C57—C63—C64—N5	−0.9 (4)	C124—C119—C120—C121	0.1 (4)
C57—C63—C64—C65	176.1 (2)	C125—C108—C109—N13	−173.4 (2)
C57—C63—C80—C81	−65.3 (3)	C125—C108—C109—C110	−0.7 (3)
C57—C63—C80—C84	118.1 (3)	C125—C126—C127—N15	0.0 (4)
C58—C59—C62—C61	178.3 (2)	C126—C125—C129—C128	−3.6 (4)
C58—C68—C69—C70	−174.6 (2)	C127—N15—C128—C129	2.4 (4)
C58—C68—C72—C71	174.3 (3)	C128—N15—C127—C126	−2.8 (4)
C59—N4—C60—C61	−1.9 (3)	C129—C125—C126—C127	3.2 (3)
C59—N4—C60—C73	174.5 (2)	C130—N14—C115—C114	172.8 (3)
C59—C58—C68—C69	78.5 (3)	C130—N14—C116—C117	−174.0 (2)
C59—C58—C68—C72	−98.7 (3)	C131—C122—C123—C124	179.0 (3)
C60—N4—C59—C58	−177.3 (2)	C131—C122—C221—C220	176.8 (8)
C60—N4—C59—C62	1.5 (3)	C131—C122—C223—C224	−175.8 (8)
C60—C61—C62—C59	−0.7 (3)	C132—N15—C127—C126	175.5 (3)
C60—C73—C74—C75	94.7 (4)	C132—N15—C128—C129	−175.9 (3)
C60—C73—C74—C79	−85.8 (4)	C220—C119—C224—C223	−5.2 (13)
C61—C60—C73—C67	178.4 (2)	C221—C122—C223—C224	20.2 (13)
C61—C60—C73—C74	3.2 (3)	C223—C122—C221—C220	−19.5 (14)
C63—C64—C65—C66	−177.1 (2)	C224—C119—C220—C221	6.5 (13)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O22—H22A···O24	0.87	1.91	2.755 (3)	164
O22—H22B···N16^i	0.87	2.07	2.904 (3)	160
O23—H23A···O11^ii	0.87	1.98	2.834 (3)	168
O23—H23B···O1^i	0.87	2.06	2.916 (3)	170
O24—H24A···O29^ii	0.75 (5)	2.13 (5)	2.809 (4)	149 (6)
O24—H24B···O5	0.84 (6)	1.99 (6)	2.818 (4)	170 (5)
O25—H25A···O13^iii	0.87	2.16	2.982 (19)	156
O25—H25A···O18^iii	0.87	1.92	2.774 (6)	166
O25—H25B···O21^iv	0.87	2.00	2.819 (3)	156
O26—H26A···O20^v	0.87	2.08	2.854 (4)	147
O26—H26B···O22	0.87	2.03	2.863 (4)	160
O27—H27A···O8^ii	0.87	2.02	2.878 (4)	170
O27—H27B···O17	0.87	2.14	2.869 (19)	142
O28—H28D···O3	0.87	1.90	2.761 (4)	169
O29—H29A···O3	0.87	1.89	2.749 (4)	172
O29—H29B···O34^vi	0.87	1.98	2.779 (5)	153
O30—H30A···O23	0.87	2.13	2.925 (4)	152
O30—H30B···O26	0.87	2.19	2.977 (4)	150
O31—H31A···O29^ii	0.87	1.90	2.729 (4)	159
O31—H31B···O33	0.87	1.91	2.753 (5)	165
O32—H32A···O34	0.87	1.84	2.711 (5)	175
O33—H33A···O7	0.87	2.04	2.893 (5)	168
O33—H33B···O32^vii	0.87	1.95	2.789 (5)	163
O34—H34A···O6	0.88 (2)	1.93 (3)	2.781 (4)	160 (7)
O35—H35D···O14^iii	0.87	2.27	2.818 (7)	121
N3—H3···N2	0.88	2.34	2.889 (3)	121
N4—H4···N5	0.88	2.33	2.885 (3)	121
N10—H10···N11	0.88	2.36	2.904 (3)	120

Symmetry codes: (i) −x+1, −y+2, −z+1; (ii) −x+1, y+1/2, −z+3/2; (iii) −x, −y+2, −z+1; (iv) −x, y−1/2, −z+3/2; (v) x+1, y, z; (vi) −x+1, y−1/2, −z+3/2; (vii) −x+1, −y+2, −z+2.

(TriMCNP)(p-tosylate)3(H2O)7

Crystal data

3(C7H7O3S)·6(H2O)·2.75(O)·C45H35N8	F(000) = 5768
Mr = 1364.55	Dx = 1.347 Mg m^−3
Monoclinic, P21/c	Cu Kα radiation, λ = 1.54184 Å
a = 17.50074 (18) Å	Cell parameters from 39011 reflections
b = 25.9751 (3) Å	θ = 2.3–47.6°
c = 30.1002 (4) Å	µ = 1.65 mm^−1
β = 100.4228 (12)°	T = 160 K
V = 13457.2 (3) Å^3	Needle, red
Z = 8	0.44 × 0.03 × 0.03 mm

Data collection

XtaLAB Synergy, Dualflex, HyPix diffractometer	12390 independent reflections
Radiation source: micro-focus sealed X-ray tube, PhotonJet (Cu) X-ray Source	10103 reflections with I > 2σ(I)
Mirror monochromator	Rint = 0.047
Detector resolution: 10.0000 pixels mm^-1	θmax = 47.7°, θmin = 2.3°
ω scans	h = −16→13
Absorption correction: gaussian CrysAlisPro 1.171.43.130a (Rigaku Oxford Diffraction, 2024) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	k = −24→24
Tmin = 0.915, Tmax = 1.000	l = −28→28
99768 measured reflections

Refinement

Refinement on F^2	Primary atom site location: dual
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.078	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.228	w = 1/[σ^2(Fo^2) + (0.1267P)^2 + 57.4028P] where P = (Fo^2 + 2Fc^2)/3
S = 1.03	(Δ/σ)max = 0.001
12390 reflections	Δρmax = 1.62 e Å^−3
1812 parameters	Δρmin = −0.59 e Å^−3
13 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	Occ. (<1)
S1	0.75711 (10)	0.33844 (7)	−0.17952 (6)	0.0443 (5)
S2	0.83572 (11)	0.64807 (7)	−0.13174 (7)	0.0505 (6)
S3	0.80688 (11)	0.38918 (7)	0.16264 (7)	0.0512 (6)
S4	1.03311 (11)	0.75918 (8)	0.02471 (6)	0.0504 (6)
S5	0.58466 (12)	0.25184 (8)	0.03645 (7)	0.0564 (6)
S6	0.38823 (11)	0.35004 (7)	−0.13712 (8)	0.0545 (6)
O1	0.7237 (3)	0.38850 (19)	−0.1872 (2)	0.0818 (19)
O2	0.7750 (3)	0.3251 (2)	−0.13232 (16)	0.0585 (14)
O3	0.8233 (3)	0.3301 (2)	−0.20132 (17)	0.0628 (15)
O4	0.9033 (3)	0.6256 (2)	−0.1439 (2)	0.0732 (17)
O5	0.8518 (3)	0.6953 (2)	−0.1064 (2)	0.0767 (17)
O6	0.7912 (3)	0.6118 (2)	−0.10999 (19)	0.0692 (16)
O7	0.8544 (3)	0.4332 (2)	0.1588 (2)	0.086 (2)
O8	0.7473 (3)	0.39589 (18)	0.18985 (17)	0.0516 (13)
O9	0.7725 (3)	0.3683 (2)	0.11757 (18)	0.0798 (18)
O10	0.9956 (3)	0.7910 (2)	−0.01165 (16)	0.0631 (15)
O11	1.1082 (3)	0.7414 (3)	0.01828 (19)	0.084 (2)
O12	0.9829 (3)	0.71784 (19)	0.03523 (17)	0.0603 (14)
O13	0.5372 (7)	0.2892 (4)	0.0444 (3)	0.176 (4)
O14	0.6538 (4)	0.2619 (3)	0.0246 (2)	0.119 (3)
O15	0.5442 (6)	0.2209 (4)	−0.0022 (3)	0.155 (4)
O16	0.3466 (4)	0.3405 (3)	−0.1811 (3)	0.134 (4)
O17	0.4277 (3)	0.30580 (19)	−0.1169 (2)	0.0729 (17)
O18	0.3405 (5)	0.3723 (3)	−0.1088 (4)	0.170 (5)
O19	0.9151 (3)	0.5918 (2)	0.19215 (18)	0.0570 (14)
H19A	0.959364	0.604897	0.188457	0.085*
H19B	0.927142	0.571101	0.215076	0.085*
O20	0.8650 (3)	0.80160 (19)	−0.08712 (19)	0.0599 (14)
H20A	0.856618	0.769045	−0.092682	0.090*
H20B	0.901700	0.802202	−0.063421	0.090*
O21	1.0353 (3)	0.6317 (2)	0.1553 (2)	0.0661 (15)
H21D	1.042258	0.624582	0.128123	0.099*
H21E	1.079531	0.644302	0.168712	0.099*
O22	0.1910 (3)	0.3426 (2)	−0.22802 (19)	0.0697 (16)
H22A	0.236423	0.343425	−0.210659	0.105*
H22B	0.159622	0.355571	−0.211527	0.105*
O23	0.4219 (3)	0.2107 (2)	−0.0734 (2)	0.0783 (19)
H23A	0.453371	0.220518	−0.049142	0.117*
H23B	0.413782	0.238411	−0.089922	0.117*
O24	0.5959 (3)	0.3615 (2)	0.1469 (2)	0.0754 (17)
H24A	0.643085	0.371181	0.158121	0.113*
H24B	0.597100	0.354782	0.118739	0.113*
O25	0.8317 (4)	0.7092 (3)	−0.0081 (3)	0.089 (2)
H25A	0.785607	0.704282	−0.001757	0.133*
H25B	0.847836	0.680912	−0.018784	0.133*
O26	1.0273 (4)	0.6195 (2)	0.0625 (2)	0.0830 (18)
H26A	1.014039	0.651602	0.058492	0.125*
H26B	0.985358	0.602363	0.051717	0.125*
O27	0.8859 (3)	0.8410 (3)	−0.1754 (2)	0.0871 (19)
H27A	0.863326	0.838739	−0.151924	0.131*
H27B	0.847844	0.839913	−0.198364	0.131*
O28	0.9137 (4)	0.5507 (3)	0.0274 (3)	0.104 (2)
H28D	0.866124	0.561857	0.020496	0.157*
H28E	0.909110	0.518329	0.033852	0.157*
O29	0.7491 (5)	0.4426 (3)	−0.0048 (2)	0.112 (2)
O30	0.8162 (4)	0.4053 (3)	−0.0721 (3)	0.119 (3)
O31	0.8705 (4)	0.4640 (3)	0.0674 (3)	0.113 (2)
H31A	0.833029	0.445599	0.052243	0.169*
H31B	0.854129	0.472253	0.092051	0.169*
O32	0.4014 (5)	0.3299 (6)	−0.0127 (4)	0.158 (4)
H32A	0.439352	0.347921	0.002383	0.238*
H32B	0.413345	0.326155	−0.039317	0.238*
O33	0.6693 (8)	0.3778 (5)	0.0416 (4)	0.207 (5)*
O34	0.6790 (8)	0.5361 (6)	−0.0091 (5)	0.104 (4)*	0.5
O35	0.7883 (5)	0.5989 (5)	−0.0229 (3)	0.186 (5)
O36	0.5241 (11)	0.5388 (7)	−0.0159 (6)	0.143 (6)*	0.5
O37	0.4485 (11)	0.5703 (8)	−0.0693 (6)	0.147 (6)*	0.5
N1	0.9151 (4)	0.5058 (2)	0.8642 (2)	0.0448 (15)
N2	0.8590 (3)	0.5640 (2)	0.65594 (19)	0.0304 (13)
H2	0.857878	0.541021	0.634361	0.01 (3)*	0.5
N3	0.8604 (3)	0.45254 (19)	0.65176 (18)	0.0325 (13)
H3	0.855584	0.477729	0.631904	0.039*	0.5
N4	0.8441 (3)	0.56875 (19)	0.55789 (17)	0.0285 (13)
H4	0.849032	0.543810	0.578001	0.034*	0.5
N5	0.8518 (3)	0.45713 (19)	0.55363 (18)	0.0288 (13)
H5	0.842864	0.479509	0.574024	0.035*	0.5
N6	0.8271 (3)	0.8046 (2)	0.59943 (19)	0.0407 (15)
N7	0.9056 (4)	0.2197 (2)	0.5845 (2)	0.0413 (15)
N8	0.9391 (4)	0.5367 (3)	0.2768 (3)	0.0595 (18)
N9	0.6827 (5)	−0.0062 (2)	−0.3489 (2)	0.0515 (17)
N10	0.6512 (3)	−0.0748 (2)	−0.14817 (18)	0.0329 (13)
H10	0.649741	−0.051501	−0.127129	0.034 (19)*
N11	0.6581 (3)	0.03611 (19)	−0.14290 (18)	0.0307 (13)
N12	0.6437 (3)	−0.07740 (19)	−0.05116 (17)	0.0295 (13)
N13	0.6571 (3)	0.03313 (19)	−0.04481 (18)	0.0287 (13)
H13	0.659893	0.009680	−0.065550	0.05 (2)*
N14	0.6053 (4)	−0.3139 (2)	−0.1045 (2)	0.0440 (15)
N15	0.6532 (4)	0.2727 (2)	−0.07997 (19)	0.0374 (14)
N16	0.5415 (4)	−0.0326 (3)	0.2276 (3)	0.077 (2)
C1	0.6849 (4)	0.2937 (3)	−0.2042 (2)	0.0401 (18)
C2	0.6085 (5)	0.3015 (3)	−0.2008 (3)	0.058 (2)
H2A	0.594027	0.331318	−0.186127	0.05 (2)*
C3	0.5528 (5)	0.2659 (3)	−0.2189 (3)	0.064 (2)
H3A	0.500093	0.271942	−0.216664	0.076*
C4	0.5719 (4)	0.2215 (3)	−0.2401 (2)	0.048 (2)
C5	0.6486 (4)	0.2152 (3)	−0.2437 (2)	0.0450 (19)
H5A	0.663375	0.185863	−0.259019	0.06 (2)*
C6	0.7048 (4)	0.2506 (3)	−0.2256 (2)	0.0442 (19)
H6	0.757473	0.244908	−0.228038	0.053*
C7	0.5117 (5)	0.1811 (4)	−0.2566 (3)	0.073 (3)
H7A	0.505919	0.158207	−0.231493	0.110*
H7B	0.528264	0.160915	−0.280698	0.10 (4)*
H7C	0.461915	0.197723	−0.268226	0.153*
C8	0.7749 (4)	0.6644 (3)	−0.1830 (3)	0.0444 (19)
C9	0.7245 (4)	0.6281 (3)	−0.2052 (3)	0.053 (2)
H9	0.719100	0.595756	−0.191461	0.034 (18)*
C10	0.6817 (5)	0.6387 (3)	−0.2477 (3)	0.060 (2)
H10D	0.647108	0.613490	−0.262836	0.072*
C11	0.6890 (5)	0.6857 (4)	−0.2681 (3)	0.060 (2)
C12	0.7387 (5)	0.7223 (3)	−0.2448 (3)	0.066 (2)
H12	0.742929	0.755204	−0.257943	0.05 (2)*
C13	0.7819 (4)	0.7115 (3)	−0.2028 (3)	0.053 (2)
H13G	0.816573	0.736572	−0.187588	0.064*
C14	0.6445 (6)	0.6954 (5)	−0.3161 (3)	0.091 (3)
H14A	0.678347	0.687966	−0.337906	0.136*
H14B	0.627929	0.731472	−0.319001	0.16 (6)*
H14C	0.598780	0.672968	−0.322003	0.242*
C15	0.8699 (4)	0.3401 (3)	0.1888 (2)	0.0362 (17)
C16	0.9489 (4)	0.3428 (3)	0.1917 (2)	0.0365 (17)
H16	0.971378	0.371704	0.179582	0.035 (18)*
C17	0.9960 (4)	0.3037 (3)	0.2121 (2)	0.0408 (18)
H17	1.050500	0.306014	0.213422	0.049*
C18	0.9660 (4)	0.2616 (3)	0.2306 (2)	0.0374 (18)
C19	0.8851 (4)	0.2590 (3)	0.2266 (2)	0.0425 (19)
H19	0.862411	0.230009	0.238517	0.040 (19)*
C20	0.8379 (4)	0.2977 (3)	0.2058 (2)	0.0389 (18)
H20	0.783073	0.295026	0.203111	0.047*
C21	1.0162 (5)	0.2190 (3)	0.2531 (3)	0.057 (2)
H21A	1.018361	0.191194	0.231307	0.086*
H21B	0.994435	0.205746	0.278608	0.07 (2)*
H21C	1.068766	0.232096	0.263998	0.099*
C22	1.0507 (4)	0.7982 (3)	0.0737 (2)	0.0382 (18)
C23	1.0932 (4)	0.7784 (3)	0.1135 (2)	0.0434 (19)
H23	1.114333	0.744668	0.114178	0.06 (2)*
C24	1.1043 (4)	0.8084 (3)	0.1519 (2)	0.0441 (19)
H24	1.133889	0.794963	0.179014	0.053*
C25	1.0734 (4)	0.8577 (3)	0.1522 (2)	0.0415 (19)
C26	1.0329 (4)	0.8768 (3)	0.1119 (2)	0.0393 (18)
H26	1.012766	0.910836	0.110889	0.041 (19)*
C27	1.0210 (4)	0.8473 (3)	0.0730 (2)	0.0389 (18)
H27	0.992301	0.860968	0.045711	0.047*
C28	1.0845 (5)	0.8883 (3)	0.1957 (2)	0.055 (2)
H28A	1.062371	0.869242	0.218424	0.082*
H28B	1.058283	0.921654	0.190145	0.13 (4)*
H28C	1.140122	0.893884	0.206657	0.197*
C29	0.5996 (4)	0.2095 (3)	0.0831 (2)	0.0439 (19)
C30	0.6455 (5)	0.2247 (3)	0.1235 (3)	0.056 (2)
H30	0.668963	0.257772	0.126028	0.05 (2)*
C31	0.6567 (5)	0.1919 (3)	0.1596 (3)	0.063 (2)
H31	0.688940	0.202392	0.186955	0.076*
C32	0.6221 (5)	0.1437 (3)	0.1572 (3)	0.060 (2)
C33	0.5764 (4)	0.1294 (3)	0.1169 (3)	0.050 (2)
H33	0.552091	0.096601	0.114455	0.06 (2)*
C34	0.5653 (4)	0.1619 (3)	0.0801 (2)	0.0424 (18)
H34	0.533915	0.151224	0.052485	0.051*
C35	0.6357 (8)	0.1076 (4)	0.1977 (3)	0.097 (4)
H35A	0.668659	0.078922	0.191662	0.146*
H35B	0.585704	0.094293	0.202953	0.15 (6)*
H35C	0.661382	0.126457	0.224464	0.232*
C36	0.4604 (4)	0.3960 (3)	−0.1415 (3)	0.0446 (19)
C37	0.4862 (4)	0.4014 (3)	−0.1821 (3)	0.049 (2)
H37	0.463459	0.381510	−0.207574	0.05 (2)*
C38	0.5449 (5)	0.4357 (3)	−0.1855 (3)	0.067 (3)
H38	0.562736	0.438565	−0.213377	0.080*
C39	0.5780 (5)	0.4655 (3)	−0.1502 (4)	0.072 (3)
C40	0.5529 (5)	0.4606 (3)	−0.1097 (4)	0.074 (3)
H40	0.575866	0.480952	−0.084653	0.08 (3)*
C41	0.4929 (5)	0.4253 (3)	−0.1051 (3)	0.063 (2)
H41	0.475435	0.422134	−0.077073	0.076*
C42	0.6412 (7)	0.5043 (4)	−0.1556 (6)	0.117 (5)
H42A	0.670636	0.491590	−0.178136	0.176*
H42B	0.676365	0.508838	−0.126597	0.21 (8)*
H42C	0.617225	0.537423	−0.165599	0.312*
C43	0.8892 (4)	0.5033 (2)	0.7712 (2)	0.0348 (17)
C44	0.8363 (4)	0.4827 (3)	0.7952 (2)	0.0447 (19)
H44	0.789916	0.467187	0.779588	0.06 (2)*
C45	0.8503 (5)	0.4845 (3)	0.8414 (3)	0.051 (2)
H45	0.813384	0.470341	0.857520	0.062*
C46	0.9685 (5)	0.5235 (3)	0.8419 (3)	0.047 (2)
H46	1.015445	0.537219	0.858541	0.057*
C47	0.9580 (4)	0.5226 (3)	0.7960 (2)	0.0401 (18)
H47	0.997536	0.535142	0.780969	0.048*
C48	0.8747 (4)	0.5049 (3)	0.7212 (2)	0.0337 (17)
C49	0.8696 (3)	0.5542 (3)	0.7011 (2)	0.0318 (17)
C50	0.8504 (3)	0.6163 (3)	0.6501 (2)	0.0323 (17)
C51	0.8561 (4)	0.6394 (3)	0.6936 (2)	0.0374 (18)
H51	0.851692	0.675095	0.699526	0.042 (19)*
C52	0.8685 (4)	0.6021 (3)	0.7246 (2)	0.0373 (17)
H52	0.875400	0.606468	0.756387	0.045*
C53	0.9260 (6)	0.5116 (3)	0.9141 (2)	0.065 (2)
H53A	0.916782	0.547527	0.921587	0.097*
H53B	0.979165	0.501845	0.927664	0.12 (4)*
H53C	0.889130	0.489297	0.925865	0.184*
C54	0.8680 (4)	0.4577 (3)	0.6978 (2)	0.0334 (17)
C55	0.8706 (4)	0.4076 (3)	0.7176 (3)	0.0407 (18)
H55	0.874368	0.400174	0.748870	0.05 (2)*
C56	0.8667 (4)	0.3729 (3)	0.6843 (2)	0.0398 (18)
H56	0.867129	0.336534	0.687661	0.048*
C57	0.8617 (4)	0.4008 (3)	0.6425 (2)	0.0339 (17)
C58	0.8360 (3)	0.6423 (2)	0.6085 (2)	0.0309 (17)
C59	0.8328 (3)	0.6198 (2)	0.5660 (2)	0.0299 (16)
C60	0.8462 (3)	0.5634 (2)	0.5131 (2)	0.0294 (16)
C61	0.8344 (3)	0.6128 (3)	0.4917 (2)	0.0330 (17)
H61	0.833184	0.619787	0.460646	0.024 (16)*
C62	0.8254 (4)	0.6474 (3)	0.5237 (2)	0.0358 (17)
H62	0.815973	0.683214	0.519248	0.043*
C63	0.8615 (3)	0.3784 (2)	0.6006 (2)	0.0306 (16)
C64	0.8593 (3)	0.4052 (3)	0.5596 (2)	0.0322 (17)
C65	0.8716 (4)	0.3822 (3)	0.5185 (2)	0.0352 (17)
H65	0.877686	0.346501	0.513217	0.05 (2)*
C66	0.8730 (4)	0.4208 (3)	0.4884 (2)	0.0369 (17)
H66	0.880771	0.417221	0.458077	0.044*
C67	0.8606 (3)	0.4684 (2)	0.5109 (2)	0.0307 (17)
C68	0.8308 (4)	0.6992 (2)	0.6090 (2)	0.0293 (16)
C69	0.7638 (4)	0.7246 (3)	0.5878 (2)	0.0379 (18)
H69	0.718230	0.705454	0.576549	0.032 (17)*
C70	0.7634 (4)	0.7769 (3)	0.5832 (2)	0.0438 (19)
H70	0.717698	0.793766	0.568451	0.053*
C71	0.8910 (4)	0.7818 (3)	0.6218 (2)	0.0394 (18)
H71	0.934738	0.802091	0.634291	0.047*
C72	0.8940 (4)	0.7294 (3)	0.6268 (2)	0.0355 (17)
H72	0.939886	0.713663	0.642719	0.043*
C73	0.8593 (3)	0.5176 (2)	0.4908 (2)	0.0278 (16)
C74	0.8755 (3)	0.5217 (2)	0.4444 (2)	0.0283 (16)
C75	0.948 (3)	0.507 (2)	0.4348 (17)	0.032 (15)*	0.126 (10)
H75	0.983830	0.489796	0.457088	0.039*	0.126 (10)
C76	0.967 (3)	0.518 (3)	0.3965 (19)	0.041 (17)*	0.126 (10)
H76	1.020517	0.516985	0.393851	0.049*	0.126 (10)
C77	0.9098 (4)	0.5303 (3)	0.3576 (2)	0.0337 (17)
C78	0.9525 (5)	0.5563 (4)	0.3927 (3)	0.040 (2)	0.874 (10)
H78	0.993870	0.577852	0.387592	0.04 (2)*	0.874 (10)
C79	0.9363 (4)	0.5518 (3)	0.4357 (3)	0.038 (2)	0.874 (10)
H79	0.967656	0.569697	0.459926	0.046*	0.874 (10)
C80	0.8738 (4)	0.3218 (2)	0.5982 (2)	0.0326 (17)
C81	0.9454 (4)	0.3003 (3)	0.6158 (2)	0.0399 (18)
H81	0.984433	0.320894	0.633404	0.05 (2)*
C82	0.9604 (4)	0.2498 (3)	0.6079 (2)	0.0429 (19)
H82	1.010410	0.236002	0.619224	0.051*
C83	0.8344 (5)	0.2384 (3)	0.5693 (2)	0.0443 (19)
H83	0.795033	0.216277	0.553991	0.053*
C84	0.8177 (4)	0.2891 (3)	0.5758 (2)	0.0400 (18)
H84	0.767007	0.301846	0.564628	0.048*
C85	0.8271 (5)	0.8614 (3)	0.5912 (3)	0.057 (2)
H85A	0.852965	0.868629	0.565614	0.085*
H85B	0.854777	0.878829	0.618228	0.11 (4)*
H85C	0.773365	0.873849	0.584346	0.172*
C86	0.8319 (4)	0.4948 (3)	0.4081 (3)	0.033 (2)	0.874 (10)
H86	0.790157	0.473618	0.413348	0.039*	0.874 (10)
C87	0.8480 (4)	0.4981 (3)	0.3655 (3)	0.038 (2)	0.874 (10)
H87	0.818135	0.479218	0.341464	0.046*	0.874 (10)
C88	0.824 (4)	0.543 (3)	0.409 (2)	0.059 (19)*	0.126 (10)
H88	0.773479	0.551121	0.414558	0.070*	0.126 (10)
C89	0.837 (3)	0.553 (2)	0.3651 (18)	0.039 (16)*	0.126 (10)
H89	0.802467	0.572627	0.343254	0.047*	0.126 (10)
C90	0.9259 (4)	0.5344 (3)	0.3130 (3)	0.0451 (19)
C91	0.9245 (5)	0.1660 (3)	0.5723 (3)	0.058 (2)
H91A	0.929818	0.164841	0.540487	0.09 (3)*
H91B	0.882753	0.142804	0.577259	0.13 (4)*
H91C	0.973471	0.155265	0.591288	0.197*
C92	0.6707 (4)	−0.0130 (2)	−0.2586 (2)	0.0354 (17)
C93	0.7337 (5)	−0.0342 (3)	−0.2750 (3)	0.0458 (19)
H93	0.773466	−0.051633	−0.254916	0.05 (2)*
C94	0.7382 (5)	−0.0300 (3)	−0.3196 (3)	0.055 (2)
H94	0.781729	−0.044199	−0.330098	0.067*
C95	0.6221 (5)	0.0151 (3)	−0.3345 (3)	0.049 (2)
H95	0.583570	0.032402	−0.355519	0.059*
C96	0.6144 (4)	0.0125 (3)	−0.2897 (2)	0.0425 (19)
H96	0.570930	0.027913	−0.280122	0.051*
C97	0.6644 (4)	−0.0159 (2)	−0.2105 (2)	0.0322 (17)
C98	0.6588 (4)	−0.0646 (2)	−0.1917 (2)	0.0328 (17)
C99	0.6591 (4)	−0.1132 (3)	−0.2142 (2)	0.0412 (18)
H99	0.663696	−0.118204	−0.244846	0.036 (18)*
C100	0.6518 (4)	−0.1503 (3)	−0.1846 (2)	0.0412 (18)
H100	0.650542	−0.186261	−0.190529	0.049*
C101	0.6463 (4)	−0.1268 (2)	−0.1423 (2)	0.0333 (17)
C102	0.6875 (7)	−0.0034 (4)	−0.3975 (3)	0.079 (3)
H10A	0.741992	−0.005734	−0.400997	0.11 (4)*
H10B	0.665593	0.029363	−0.409978	0.14 (5)*
H10C	0.658121	−0.031959	−0.413621	0.210*
C103	0.6657 (4)	0.0312 (2)	−0.1870 (2)	0.0319 (17)
C104	0.6804 (4)	0.0810 (3)	−0.2051 (2)	0.0372 (17)
H104	0.688425	0.088080	−0.234905	0.040 (19)*
C105	0.6807 (4)	0.1149 (3)	−0.1722 (2)	0.0343 (17)
H105	0.688655	0.150974	−0.174142	0.041*
C106	0.6668 (3)	0.0875 (2)	−0.1332 (2)	0.0316 (17)
C107	0.6390 (4)	−0.1525 (2)	−0.1023 (2)	0.0328 (17)
C108	0.6374 (3)	−0.1292 (2)	−0.0602 (2)	0.0299 (16)
C109	0.6248 (3)	−0.1562 (3)	−0.0203 (2)	0.0352 (17)
H109	0.618755	−0.192332	−0.017698	0.05 (2)*
C110	0.6233 (4)	−0.1217 (2)	0.0121 (2)	0.0322 (16)
H110	0.615825	−0.128415	0.042095	0.039*
C111	0.6352 (3)	−0.0716 (2)	−0.0072 (2)	0.0289 (16)
C112	0.6649 (3)	0.1107 (2)	−0.0912 (2)	0.0287 (16)
C113	0.6603 (3)	0.0850 (2)	−0.0509 (2)	0.0304 (16)
C114	0.6488 (3)	0.0233 (2)	−0.0012 (2)	0.0301 (16)
C115	0.6489 (4)	0.0711 (3)	0.0215 (2)	0.0346 (17)
H115	0.645461	0.075937	0.052313	0.010 (14)*
C116	0.6550 (4)	0.1087 (3)	−0.0088 (2)	0.0352 (17)
H116	0.655556	0.144676	−0.002986	0.042*
C117	0.6290 (4)	−0.2089 (2)	−0.1044 (2)	0.0326 (17)
C118	0.5623 (4)	−0.2315 (3)	−0.1296 (2)	0.0367 (17)
H118	0.524120	−0.210364	−0.147304	0.022 (16)*
C119	0.5517 (4)	−0.2832 (3)	−0.1289 (2)	0.0415 (18)
H119	0.505919	−0.297876	−0.145971	0.050*
C120	0.6704 (4)	−0.2936 (3)	−0.0799 (3)	0.051 (2)
H120	0.707764	−0.315637	−0.062643	0.061*
C121	0.6833 (4)	−0.2415 (3)	−0.0794 (3)	0.0432 (19)
H121	0.729422	−0.227704	−0.061903	0.052*
C122	0.6374 (3)	−0.0254 (2)	0.0166 (2)	0.0277 (16)
C123	0.6195 (4)	−0.0271 (2)	0.0635 (2)	0.0296 (16)
C124	0.5456 (5)	−0.0292 (5)	0.0698 (3)	0.086 (3)
H124	0.505096	−0.030154	0.044099	0.11 (3)*
C125	0.5266 (5)	−0.0300 (5)	0.1115 (3)	0.089 (3)
H125	0.473433	−0.030229	0.114370	0.106*
C126	0.5821 (4)	−0.0303 (3)	0.1493 (2)	0.0392 (18)
C127	0.6570 (5)	−0.0287 (5)	0.1436 (3)	0.088 (4)
H127	0.697498	−0.028766	0.169271	0.09 (3)*
C128	0.6751 (5)	−0.0270 (4)	0.1007 (3)	0.075 (3)
H128	0.728106	−0.025612	0.097543	0.090*
C129	0.6630 (4)	0.1678 (2)	−0.0892 (2)	0.0299 (16)
C130	0.7266 (4)	0.1969 (3)	−0.0702 (2)	0.0385 (18)
H130	0.775087	0.180553	−0.059910	0.06 (2)*
C131	0.7203 (4)	0.2493 (3)	−0.0661 (2)	0.0412 (18)
H131	0.764654	0.268873	−0.053256	0.049*
C132	0.5913 (4)	0.2463 (3)	−0.0996 (3)	0.048 (2)
H132	0.544011	0.263872	−0.110296	0.058*
C133	0.5948 (4)	0.1936 (3)	−0.1046 (3)	0.0451 (19)
H133	0.550069	0.175208	−0.118710	0.054*
C134	0.5935 (5)	−0.3705 (3)	−0.1038 (3)	0.066 (2)
H13A	0.578683	−0.380512	−0.075171	0.099*
H13B	0.641912	−0.387982	−0.106965	0.10 (3)*
H13C	0.552288	−0.380368	−0.128927	0.146*
C135	0.5599 (5)	−0.0318 (3)	0.1927 (3)	0.053 (2)
C136	0.6440 (5)	0.3288 (3)	−0.0724 (3)	0.055 (2)
H13D	0.690111	0.341756	−0.052096	0.11 (4)*
H13E	0.597913	0.334559	−0.058845	0.08 (3)*
H13F	0.638019	0.346949	−0.101386	0.115*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
S1	0.0459 (12)	0.0374 (12)	0.0513 (13)	0.0033 (9)	0.0134 (9)	0.0064 (9)
S2	0.0423 (12)	0.0403 (12)	0.0704 (14)	−0.0001 (9)	0.0146 (10)	−0.0007 (10)
S3	0.0440 (12)	0.0436 (12)	0.0679 (15)	0.0093 (10)	0.0148 (11)	0.0104 (10)
S4	0.0422 (12)	0.0640 (14)	0.0449 (12)	−0.0086 (10)	0.0071 (10)	−0.0117 (11)
S5	0.0472 (13)	0.0554 (13)	0.0679 (15)	0.0114 (10)	0.0138 (11)	0.0146 (11)
S6	0.0442 (12)	0.0443 (12)	0.0779 (16)	0.0061 (10)	0.0191 (12)	0.0204 (11)
O1	0.067 (4)	0.033 (3)	0.136 (6)	0.008 (3)	−0.008 (4)	0.008 (3)
O2	0.067 (4)	0.065 (4)	0.045 (3)	−0.004 (3)	0.016 (3)	0.005 (3)
O3	0.052 (3)	0.080 (4)	0.063 (4)	−0.020 (3)	0.028 (3)	−0.016 (3)
O4	0.046 (3)	0.081 (4)	0.098 (5)	0.024 (3)	0.027 (3)	0.013 (3)
O5	0.093 (4)	0.044 (3)	0.085 (4)	−0.001 (3)	−0.007 (3)	−0.014 (3)
O6	0.064 (4)	0.070 (4)	0.074 (4)	−0.014 (3)	0.017 (3)	0.018 (3)
O7	0.060 (4)	0.049 (4)	0.147 (6)	0.002 (3)	0.019 (4)	0.033 (4)
O8	0.044 (3)	0.050 (3)	0.064 (3)	0.013 (2)	0.019 (3)	0.001 (3)
O9	0.086 (4)	0.101 (5)	0.048 (4)	0.029 (4)	−0.001 (3)	−0.001 (3)
O10	0.072 (4)	0.074 (4)	0.039 (3)	−0.024 (3)	0.001 (3)	0.001 (3)
O11	0.047 (4)	0.134 (6)	0.072 (4)	0.003 (3)	0.017 (3)	−0.049 (4)
O12	0.064 (3)	0.053 (3)	0.062 (4)	−0.017 (3)	0.007 (3)	−0.008 (3)
O13	0.234 (8)	0.169 (7)	0.156 (7)	0.106 (6)	0.114 (6)	0.093 (6)
O14	0.052 (4)	0.209 (9)	0.100 (5)	0.020 (4)	0.027 (4)	0.088 (6)
O15	0.155 (6)	0.158 (7)	0.126 (6)	−0.056 (5)	−0.041 (5)	0.062 (5)
O16	0.094 (5)	0.169 (8)	0.114 (6)	−0.081 (5)	−0.051 (5)	0.083 (6)
O17	0.058 (3)	0.036 (3)	0.114 (5)	0.006 (3)	−0.010 (3)	0.030 (3)
O18	0.181 (8)	0.059 (4)	0.334 (14)	−0.014 (5)	0.212 (10)	−0.012 (6)
O19	0.049 (3)	0.063 (4)	0.061 (4)	0.001 (3)	0.016 (3)	0.017 (3)
O20	0.059 (4)	0.050 (3)	0.069 (4)	−0.002 (3)	0.008 (3)	−0.007 (3)
O21	0.048 (3)	0.080 (4)	0.074 (4)	−0.003 (3)	0.019 (3)	0.007 (3)
O22	0.048 (3)	0.077 (4)	0.082 (4)	0.003 (3)	0.003 (3)	−0.019 (3)
O23	0.050 (4)	0.093 (5)	0.088 (5)	−0.014 (3)	0.002 (3)	0.046 (4)
O24	0.055 (4)	0.064 (4)	0.104 (5)	−0.015 (3)	0.006 (3)	−0.006 (4)
O25	0.056 (4)	0.099 (5)	0.105 (5)	−0.008 (3)	−0.003 (4)	0.033 (4)
O26	0.089 (5)	0.063 (4)	0.094 (5)	−0.005 (3)	0.009 (4)	0.002 (4)
O27	0.066 (4)	0.123 (5)	0.071 (4)	−0.004 (4)	0.012 (3)	0.008 (4)
O28	0.086 (5)	0.080 (5)	0.133 (6)	0.009 (4)	−0.015 (5)	−0.020 (5)
O29	0.131 (6)	0.103 (6)	0.103 (6)	−0.017 (5)	0.027 (5)	−0.030 (4)
O30	0.115 (6)	0.139 (7)	0.114 (6)	−0.048 (5)	0.050 (5)	−0.047 (5)
O31	0.096 (5)	0.109 (6)	0.131 (7)	−0.005 (4)	0.018 (5)	0.006 (5)
O32	0.108 (7)	0.224 (12)	0.136 (8)	0.023 (7)	0.001 (6)	0.027 (8)
O35	0.118 (7)	0.347 (16)	0.092 (6)	0.112 (9)	0.014 (5)	0.035 (8)
N1	0.056 (4)	0.038 (4)	0.043 (4)	0.008 (3)	0.017 (4)	0.004 (3)
N2	0.031 (3)	0.026 (4)	0.036 (4)	−0.002 (2)	0.012 (3)	−0.005 (3)
N3	0.035 (3)	0.023 (4)	0.040 (4)	−0.002 (2)	0.009 (3)	0.002 (3)
N4	0.030 (3)	0.027 (4)	0.030 (4)	−0.001 (2)	0.009 (2)	0.000 (3)
N5	0.032 (3)	0.025 (4)	0.032 (4)	0.003 (2)	0.012 (2)	0.001 (3)
N6	0.037 (4)	0.034 (4)	0.052 (4)	0.001 (3)	0.009 (3)	−0.005 (3)
N7	0.051 (4)	0.028 (4)	0.050 (4)	0.006 (4)	0.020 (3)	0.010 (3)
N8	0.056 (4)	0.075 (5)	0.051 (5)	0.004 (3)	0.018 (4)	0.005 (4)
N9	0.082 (5)	0.034 (4)	0.041 (4)	−0.026 (4)	0.018 (4)	−0.007 (3)
N10	0.042 (3)	0.024 (4)	0.034 (4)	−0.001 (2)	0.010 (3)	−0.002 (3)
N11	0.029 (3)	0.023 (4)	0.041 (4)	−0.001 (2)	0.009 (3)	−0.001 (3)
N12	0.030 (3)	0.025 (4)	0.035 (4)	−0.002 (2)	0.009 (2)	−0.001 (3)
N13	0.037 (3)	0.019 (3)	0.032 (4)	0.000 (2)	0.010 (3)	−0.001 (3)
N14	0.045 (4)	0.023 (4)	0.066 (4)	−0.003 (3)	0.017 (3)	−0.004 (3)
N15	0.048 (4)	0.022 (3)	0.046 (4)	−0.003 (3)	0.021 (3)	0.002 (3)
N16	0.082 (5)	0.095 (6)	0.062 (5)	0.025 (4)	0.036 (4)	0.013 (4)
C1	0.045 (5)	0.035 (5)	0.042 (4)	0.004 (4)	0.014 (4)	0.012 (4)
C2	0.045 (6)	0.046 (5)	0.088 (6)	0.002 (5)	0.027 (5)	0.001 (5)
C3	0.040 (5)	0.067 (6)	0.088 (7)	0.000 (5)	0.022 (5)	0.014 (5)
C4	0.050 (6)	0.044 (5)	0.051 (5)	−0.005 (4)	0.013 (4)	0.011 (4)
C5	0.048 (5)	0.039 (5)	0.052 (5)	−0.002 (4)	0.019 (4)	0.009 (4)
C6	0.046 (5)	0.038 (5)	0.051 (5)	0.003 (4)	0.015 (4)	0.012 (4)
C7	0.069 (6)	0.076 (6)	0.073 (6)	−0.024 (5)	0.007 (5)	0.011 (5)
C8	0.043 (5)	0.028 (4)	0.069 (5)	0.001 (4)	0.025 (4)	0.003 (4)
C9	0.043 (5)	0.034 (5)	0.084 (7)	−0.002 (4)	0.022 (5)	0.007 (5)
C10	0.048 (5)	0.063 (6)	0.068 (6)	−0.002 (4)	0.010 (5)	0.004 (5)
C11	0.055 (5)	0.068 (7)	0.061 (6)	0.022 (5)	0.023 (5)	0.008 (5)
C12	0.072 (6)	0.043 (6)	0.090 (8)	0.005 (5)	0.034 (6)	0.008 (5)
C13	0.050 (5)	0.043 (5)	0.067 (6)	0.002 (4)	0.011 (5)	0.000 (4)
C14	0.086 (7)	0.122 (10)	0.067 (7)	0.022 (7)	0.023 (6)	0.019 (6)
C15	0.039 (5)	0.031 (4)	0.039 (4)	0.003 (3)	0.012 (3)	−0.003 (3)
C16	0.039 (5)	0.033 (4)	0.040 (4)	−0.003 (4)	0.014 (3)	−0.007 (4)
C17	0.034 (4)	0.040 (5)	0.049 (5)	0.001 (4)	0.008 (4)	−0.008 (4)
C18	0.041 (5)	0.033 (4)	0.038 (4)	0.009 (4)	0.008 (3)	−0.003 (3)
C19	0.054 (6)	0.030 (4)	0.048 (5)	−0.003 (4)	0.020 (4)	−0.005 (4)
C20	0.032 (4)	0.038 (5)	0.048 (5)	0.003 (4)	0.012 (4)	−0.004 (4)
C21	0.062 (5)	0.049 (5)	0.061 (5)	0.015 (4)	0.010 (4)	0.004 (4)
C22	0.030 (4)	0.048 (5)	0.038 (5)	−0.008 (4)	0.010 (4)	0.000 (4)
C23	0.040 (4)	0.046 (5)	0.044 (5)	0.003 (4)	0.010 (4)	0.006 (4)
C24	0.038 (4)	0.056 (5)	0.037 (5)	−0.001 (4)	0.004 (3)	0.003 (4)
C25	0.035 (4)	0.047 (5)	0.044 (5)	−0.012 (4)	0.012 (4)	−0.001 (4)
C26	0.031 (4)	0.041 (5)	0.047 (5)	−0.003 (4)	0.010 (4)	0.010 (4)
C27	0.028 (4)	0.049 (5)	0.040 (5)	−0.006 (4)	0.006 (3)	0.006 (4)
C28	0.068 (5)	0.053 (5)	0.046 (5)	−0.010 (4)	0.018 (4)	−0.007 (4)
C29	0.034 (4)	0.053 (5)	0.046 (5)	0.009 (4)	0.012 (4)	0.002 (4)
C30	0.064 (5)	0.040 (5)	0.064 (6)	0.000 (4)	0.011 (5)	−0.009 (5)
C31	0.089 (7)	0.056 (6)	0.042 (5)	0.002 (5)	0.003 (4)	−0.009 (5)
C32	0.091 (6)	0.046 (6)	0.044 (6)	0.018 (5)	0.016 (5)	−0.004 (4)
C33	0.058 (5)	0.042 (5)	0.053 (6)	0.002 (4)	0.014 (4)	−0.010 (5)
C34	0.042 (4)	0.044 (5)	0.042 (5)	0.003 (4)	0.008 (3)	0.000 (4)
C35	0.164 (12)	0.069 (7)	0.057 (7)	0.007 (7)	0.015 (6)	0.017 (5)
C36	0.039 (4)	0.036 (4)	0.062 (6)	0.009 (4)	0.018 (4)	0.007 (4)
C37	0.040 (5)	0.029 (4)	0.081 (7)	0.004 (4)	0.016 (4)	0.005 (4)
C38	0.069 (6)	0.038 (5)	0.105 (8)	0.004 (5)	0.044 (6)	−0.005 (5)
C39	0.056 (6)	0.043 (5)	0.125 (9)	0.001 (5)	0.039 (6)	−0.021 (6)
C40	0.052 (6)	0.052 (6)	0.112 (9)	0.007 (5)	0.000 (6)	−0.029 (6)
C41	0.061 (6)	0.058 (6)	0.070 (6)	0.016 (5)	0.012 (5)	−0.004 (5)
C42	0.076 (7)	0.071 (7)	0.219 (15)	−0.027 (6)	0.067 (9)	−0.042 (8)
C43	0.043 (5)	0.030 (4)	0.035 (5)	0.003 (3)	0.018 (4)	−0.002 (3)
C44	0.048 (5)	0.053 (5)	0.034 (5)	−0.004 (4)	0.010 (4)	0.003 (4)
C45	0.046 (5)	0.052 (5)	0.061 (6)	0.004 (4)	0.023 (5)	0.009 (4)
C46	0.054 (5)	0.038 (4)	0.047 (6)	0.002 (4)	0.001 (4)	−0.001 (4)
C47	0.045 (5)	0.036 (4)	0.040 (5)	−0.003 (4)	0.010 (4)	0.000 (4)
C48	0.029 (4)	0.032 (5)	0.044 (5)	−0.004 (3)	0.016 (3)	0.000 (4)
C49	0.022 (4)	0.036 (5)	0.040 (5)	−0.004 (3)	0.013 (3)	−0.007 (4)
C50	0.024 (4)	0.036 (5)	0.039 (5)	−0.003 (3)	0.010 (3)	−0.007 (4)
C51	0.035 (4)	0.031 (5)	0.048 (5)	0.001 (3)	0.013 (3)	−0.004 (4)
C52	0.035 (4)	0.037 (5)	0.042 (4)	−0.002 (3)	0.013 (3)	−0.003 (4)
C53	0.104 (8)	0.058 (5)	0.032 (5)	0.010 (5)	0.011 (5)	0.005 (4)
C54	0.029 (4)	0.037 (5)	0.036 (5)	−0.005 (3)	0.011 (3)	0.004 (4)
C55	0.046 (5)	0.037 (5)	0.040 (5)	−0.003 (3)	0.011 (3)	0.007 (4)
C56	0.051 (5)	0.028 (4)	0.042 (5)	−0.004 (3)	0.012 (4)	0.000 (4)
C57	0.030 (4)	0.033 (5)	0.039 (5)	−0.006 (3)	0.009 (3)	0.003 (4)
C58	0.022 (4)	0.030 (4)	0.043 (5)	0.002 (3)	0.011 (3)	−0.001 (4)
C59	0.021 (4)	0.027 (4)	0.042 (5)	−0.002 (3)	0.009 (3)	0.002 (4)
C60	0.021 (4)	0.028 (5)	0.039 (5)	−0.005 (3)	0.006 (3)	0.005 (4)
C61	0.030 (4)	0.036 (4)	0.033 (5)	0.001 (3)	0.004 (3)	0.004 (4)
C62	0.034 (4)	0.030 (4)	0.044 (5)	0.005 (3)	0.010 (3)	0.001 (4)
C63	0.027 (4)	0.032 (4)	0.034 (5)	−0.003 (3)	0.007 (3)	0.004 (4)
C64	0.022 (4)	0.036 (5)	0.039 (5)	0.000 (3)	0.007 (3)	−0.006 (4)
C65	0.040 (4)	0.027 (4)	0.039 (5)	0.002 (3)	0.006 (3)	−0.001 (4)
C66	0.035 (4)	0.036 (5)	0.040 (4)	0.003 (3)	0.009 (3)	−0.006 (4)
C67	0.022 (4)	0.033 (5)	0.036 (5)	−0.002 (3)	0.004 (3)	−0.004 (4)
C68	0.029 (4)	0.024 (4)	0.038 (4)	0.000 (3)	0.014 (3)	−0.004 (3)
C69	0.027 (4)	0.030 (5)	0.056 (5)	−0.003 (4)	0.008 (4)	−0.007 (4)
C70	0.029 (5)	0.039 (5)	0.061 (5)	0.009 (4)	0.002 (4)	−0.007 (4)
C71	0.032 (5)	0.038 (5)	0.049 (5)	−0.001 (4)	0.008 (4)	−0.006 (4)
C72	0.033 (4)	0.031 (5)	0.042 (4)	0.004 (4)	0.004 (3)	−0.005 (3)
C73	0.018 (4)	0.027 (4)	0.038 (4)	−0.001 (3)	0.004 (3)	0.001 (4)
C74	0.023 (4)	0.028 (4)	0.034 (4)	0.002 (3)	0.006 (3)	0.004 (3)
C77	0.031 (4)	0.043 (4)	0.030 (5)	0.002 (4)	0.012 (4)	0.004 (4)
C78	0.031 (5)	0.043 (6)	0.050 (7)	−0.007 (4)	0.014 (5)	0.004 (5)
C79	0.031 (5)	0.046 (6)	0.038 (6)	−0.012 (4)	0.010 (4)	−0.003 (4)
C80	0.031 (4)	0.031 (4)	0.037 (4)	−0.004 (4)	0.009 (3)	0.001 (3)
C81	0.036 (5)	0.034 (5)	0.050 (5)	−0.006 (4)	0.009 (4)	0.001 (4)
C82	0.039 (5)	0.039 (5)	0.053 (5)	0.004 (4)	0.014 (4)	0.013 (4)
C83	0.050 (5)	0.033 (5)	0.050 (5)	−0.004 (4)	0.009 (4)	0.001 (4)
C84	0.038 (4)	0.030 (5)	0.050 (5)	0.001 (4)	0.005 (4)	0.002 (4)
C85	0.063 (5)	0.025 (4)	0.080 (6)	0.001 (4)	0.007 (5)	0.002 (4)
C86	0.027 (5)	0.033 (5)	0.040 (6)	−0.005 (4)	0.012 (4)	0.000 (4)
C87	0.033 (5)	0.047 (6)	0.036 (6)	0.000 (4)	0.007 (4)	−0.006 (4)
C90	0.037 (5)	0.046 (5)	0.054 (6)	0.001 (3)	0.013 (4)	0.000 (4)
C91	0.087 (6)	0.024 (4)	0.069 (6)	0.008 (4)	0.034 (5)	0.002 (4)
C92	0.044 (5)	0.025 (4)	0.037 (5)	−0.005 (3)	0.007 (4)	0.000 (3)
C93	0.059 (5)	0.041 (5)	0.042 (5)	0.000 (4)	0.021 (4)	0.005 (4)
C94	0.079 (6)	0.034 (5)	0.061 (6)	−0.006 (4)	0.033 (5)	−0.006 (4)
C95	0.060 (6)	0.037 (5)	0.048 (6)	−0.017 (4)	0.000 (4)	0.006 (4)
C96	0.055 (5)	0.030 (4)	0.043 (5)	−0.009 (4)	0.011 (4)	0.000 (4)
C97	0.031 (4)	0.032 (5)	0.034 (4)	0.000 (3)	0.009 (3)	0.000 (4)
C98	0.039 (4)	0.028 (5)	0.032 (5)	−0.003 (3)	0.008 (3)	−0.003 (4)
C99	0.055 (5)	0.034 (5)	0.037 (5)	−0.001 (3)	0.014 (4)	−0.002 (4)
C100	0.054 (5)	0.025 (4)	0.047 (5)	0.000 (3)	0.015 (4)	0.000 (4)
C101	0.034 (4)	0.027 (5)	0.040 (5)	0.000 (3)	0.009 (3)	−0.002 (4)
C102	0.123 (9)	0.086 (8)	0.033 (5)	−0.049 (6)	0.029 (5)	−0.007 (5)
C103	0.032 (4)	0.033 (5)	0.031 (5)	−0.002 (3)	0.007 (3)	0.004 (4)
C104	0.048 (5)	0.031 (4)	0.036 (5)	−0.001 (3)	0.015 (3)	0.003 (4)
C105	0.042 (4)	0.024 (4)	0.037 (4)	−0.004 (3)	0.008 (3)	0.005 (4)
C106	0.029 (4)	0.030 (5)	0.036 (5)	0.002 (3)	0.006 (3)	0.004 (4)
C107	0.031 (4)	0.027 (4)	0.041 (5)	0.000 (3)	0.009 (3)	0.003 (4)
C108	0.025 (4)	0.030 (5)	0.034 (5)	0.003 (3)	0.005 (3)	0.006 (4)
C109	0.030 (4)	0.026 (4)	0.049 (5)	−0.003 (3)	0.005 (3)	0.006 (4)
C110	0.036 (4)	0.030 (4)	0.030 (4)	−0.004 (3)	0.007 (3)	0.002 (4)
C111	0.023 (4)	0.029 (5)	0.035 (5)	0.002 (3)	0.006 (3)	0.005 (4)
C112	0.025 (4)	0.027 (4)	0.036 (5)	0.001 (3)	0.010 (3)	0.002 (4)
C113	0.023 (4)	0.030 (5)	0.037 (5)	−0.001 (3)	0.004 (3)	−0.001 (4)
C114	0.025 (4)	0.026 (5)	0.040 (5)	−0.002 (3)	0.008 (3)	−0.001 (4)
C115	0.041 (4)	0.035 (5)	0.031 (4)	0.000 (3)	0.013 (3)	−0.001 (4)
C116	0.040 (4)	0.025 (4)	0.042 (5)	−0.002 (3)	0.010 (3)	−0.003 (4)
C117	0.033 (4)	0.029 (4)	0.040 (4)	0.000 (4)	0.017 (3)	−0.001 (3)
C118	0.042 (5)	0.026 (5)	0.042 (4)	0.001 (4)	0.005 (4)	0.000 (3)
C119	0.036 (4)	0.036 (5)	0.052 (5)	0.001 (4)	0.008 (4)	−0.003 (4)
C120	0.036 (5)	0.037 (5)	0.080 (6)	0.004 (4)	0.010 (4)	0.002 (4)
C121	0.036 (4)	0.030 (5)	0.063 (5)	−0.001 (4)	0.009 (4)	0.001 (4)
C122	0.016 (3)	0.030 (5)	0.037 (4)	0.003 (3)	0.007 (3)	0.004 (4)
C123	0.027 (4)	0.028 (4)	0.035 (5)	0.000 (3)	0.008 (4)	0.004 (3)
C124	0.028 (5)	0.200 (12)	0.031 (5)	−0.017 (6)	0.005 (4)	0.007 (6)
C125	0.038 (5)	0.177 (11)	0.054 (6)	−0.014 (6)	0.017 (5)	0.012 (6)
C126	0.043 (5)	0.037 (4)	0.040 (5)	0.007 (3)	0.013 (4)	0.006 (3)
C127	0.028 (5)	0.197 (12)	0.038 (6)	0.028 (6)	0.001 (4)	−0.001 (6)
C128	0.029 (5)	0.160 (10)	0.039 (6)	0.026 (5)	0.013 (4)	0.003 (5)
C129	0.032 (4)	0.025 (4)	0.035 (4)	0.002 (4)	0.012 (3)	0.004 (3)
C130	0.033 (5)	0.023 (5)	0.058 (5)	0.002 (4)	0.004 (4)	0.005 (3)
C131	0.035 (5)	0.036 (5)	0.051 (5)	−0.002 (4)	0.000 (4)	0.004 (4)
C132	0.036 (5)	0.037 (5)	0.075 (6)	0.010 (4)	0.017 (4)	0.017 (4)
C133	0.030 (5)	0.031 (5)	0.072 (5)	−0.001 (4)	0.003 (4)	0.005 (4)
C134	0.069 (6)	0.027 (5)	0.099 (7)	−0.001 (4)	0.008 (5)	−0.005 (4)
C135	0.057 (5)	0.058 (5)	0.047 (6)	0.015 (4)	0.021 (5)	0.009 (4)
C136	0.078 (6)	0.026 (5)	0.068 (6)	0.001 (4)	0.032 (5)	−0.003 (4)

Geometric parameters (Å, º)

S1—O1	1.427 (5)	C40—H40	0.9500
S1—O2	1.441 (5)	C40—C41	1.419 (12)
S1—O3	1.447 (5)	C41—H41	0.9500
S1—C1	1.778 (7)	C42—H42A	0.9800
S2—O4	1.424 (5)	C42—H42B	0.9800
S2—O5	1.444 (6)	C42—H42C	0.9800
S2—O6	1.451 (5)	C43—C44	1.381 (9)
S2—C8	1.760 (8)	C43—C47	1.392 (9)
S3—O7	1.431 (6)	C43—C48	1.481 (9)
S3—O8	1.448 (5)	C44—H44	0.9500
S3—O9	1.484 (6)	C44—C45	1.368 (10)
S3—C15	1.773 (7)	C45—H45	0.9500
S4—O10	1.432 (5)	C46—H46	0.9500
S4—O11	1.439 (6)	C46—C47	1.361 (10)
S4—O12	1.458 (5)	C47—H47	0.9500
S4—C22	1.768 (7)	C48—C49	1.413 (9)
S5—O13	1.326 (9)	C48—C54	1.409 (9)
S5—O14	1.347 (6)	C49—C52	1.433 (9)
S5—O15	1.483 (9)	C50—C51	1.428 (9)
S5—C29	1.767 (8)	C50—C58	1.407 (9)
S6—O16	1.412 (7)	C51—H51	0.9500
S6—O17	1.420 (5)	C51—C52	1.334 (9)
S6—O18	1.422 (7)	C52—H52	0.9500
S6—C36	1.759 (8)	C53—H53A	0.9800
O19—H19A	0.8716	C53—H53B	0.9800
O19—H19B	0.8704	C53—H53C	0.9800
O20—H20A	0.8694	C54—C55	1.429 (9)
O20—H20B	0.8697	C55—H55	0.9500
O21—H21D	0.8692	C55—C56	1.341 (9)
O21—H21E	0.8700	C56—H56	0.9500
O22—H22A	0.8696	C56—C57	1.441 (9)
O22—H22B	0.8708	C57—C63	1.387 (9)
O23—H23A	0.8704	C58—C59	1.396 (9)
O23—H23B	0.8724	C58—C68	1.483 (9)
O24—H24A	0.8703	C59—C62	1.448 (9)
O24—H24B	0.8687	C60—C61	1.432 (9)
O25—H25A	0.8714	C60—C73	1.406 (9)
O25—H25B	0.8696	C61—H61	0.9500
O26—H26A	0.8690	C61—C62	1.347 (9)
O26—H26B	0.8698	C62—H62	0.9500
O27—H27A	0.8702	C63—C64	1.411 (9)
O27—H27B	0.8695	C63—C80	1.490 (9)
O28—H28D	0.8704	C64—C65	1.426 (9)
O28—H28E	0.8710	C65—H65	0.9500
O31—H31A	0.8707	C65—C66	1.355 (9)
O31—H31B	0.8695	C66—H66	0.9500
O32—H32A	0.8701	C66—C67	1.444 (9)
O32—H32B	0.8704	C67—C73	1.413 (9)
N1—C45	1.334 (9)	C68—C69	1.395 (9)
N1—C46	1.327 (9)	C68—C72	1.382 (9)
N1—C53	1.487 (9)	C69—H69	0.9500
N2—H2	0.8800	C69—C70	1.363 (9)
N2—C49	1.362 (8)	C70—H70	0.9500
N2—C50	1.373 (8)	C71—H71	0.9500
N3—H3	0.8800	C71—C72	1.369 (9)
N3—C54	1.375 (8)	C72—H72	0.9500
N3—C57	1.374 (8)	C73—C74	1.479 (9)
N4—H4	0.8800	C74—C75	1.40 (5)
N4—C59	1.370 (8)	C74—C79	1.383 (10)
N4—C60	1.363 (8)	C74—C86	1.400 (10)
N5—H5	0.8800	C74—C88	1.39 (7)
N5—C64	1.363 (8)	C75—H75	0.9500
N5—C67	1.356 (8)	C75—C76	1.29 (7)
N6—C70	1.343 (9)	C76—H76	0.9500
N6—C71	1.334 (8)	C76—C77	1.44 (6)
N6—C85	1.496 (9)	C77—C78	1.359 (10)
N7—C82	1.336 (9)	C77—C87	1.420 (10)
N7—C83	1.338 (9)	C77—C89	1.47 (5)
N7—C91	1.494 (9)	C77—C90	1.425 (11)
N8—C90	1.157 (9)	C78—H78	0.9500
N9—C94	1.339 (10)	C78—C79	1.379 (11)
N9—C95	1.336 (10)	C79—H79	0.9500
N9—C102	1.482 (10)	C80—C81	1.386 (9)
N10—H10	0.8800	C80—C84	1.379 (9)
N10—C98	1.367 (8)	C81—H81	0.9500
N10—C101	1.366 (8)	C81—C82	1.366 (10)
N11—C103	1.363 (8)	C82—H82	0.9500
N11—C106	1.368 (8)	C83—H83	0.9500
N12—C108	1.373 (8)	C83—C84	1.370 (10)
N12—C111	1.367 (8)	C84—H84	0.9500
N13—H13	0.8800	C85—H85A	0.9800
N13—C113	1.362 (8)	C85—H85B	0.9800
N13—C114	1.372 (8)	C85—H85C	0.9800
N14—C119	1.345 (9)	C86—H86	0.9500
N14—C120	1.349 (9)	C86—C87	1.364 (10)
N14—C134	1.485 (9)	C87—H87	0.9500
N15—C131	1.322 (8)	C88—H88	0.9500
N15—C132	1.326 (9)	C88—C89	1.40 (8)
N15—C136	1.487 (9)	C89—H89	0.9500
N16—C135	1.153 (9)	C91—H91A	0.9800
C1—C2	1.372 (10)	C91—H91B	0.9800
C1—C6	1.369 (10)	C91—H91C	0.9800
C2—H2A	0.9500	C92—C93	1.400 (10)
C2—C3	1.381 (11)	C92—C96	1.396 (10)
C3—H3A	0.9500	C92—C97	1.474 (9)
C3—C4	1.389 (11)	C93—H93	0.9500
C4—C5	1.376 (10)	C93—C94	1.364 (10)
C4—C7	1.507 (11)	C94—H94	0.9500
C5—H5A	0.9500	C95—H95	0.9500
C5—C6	1.383 (10)	C95—C96	1.380 (10)
C6—H6	0.9500	C96—H96	0.9500
C7—H7A	0.9800	C97—C98	1.397 (9)
C7—H7B	0.9800	C97—C103	1.411 (9)
C7—H7C	0.9800	C98—C99	1.434 (9)
C8—C9	1.379 (10)	C99—H99	0.9500
C8—C13	1.377 (10)	C99—C100	1.334 (9)
C9—H9	0.9500	C100—H100	0.9500
C9—C10	1.387 (11)	C100—C101	1.429 (9)
C10—H10D	0.9500	C101—C107	1.404 (9)
C10—C11	1.385 (11)	C102—H10A	0.9800
C11—C12	1.390 (12)	C102—H10B	0.9800
C11—C14	1.531 (12)	C102—H10C	0.9800
C12—H12	0.9500	C103—C104	1.445 (9)
C12—C13	1.379 (11)	C104—H104	0.9500
C13—H13G	0.9500	C104—C105	1.325 (9)
C14—H14A	0.9800	C105—H105	0.9500
C14—H14B	0.9800	C105—C106	1.432 (9)
C14—H14C	0.9800	C106—C112	1.406 (9)
C15—C16	1.372 (9)	C107—C108	1.410 (9)
C15—C20	1.377 (9)	C107—C117	1.477 (9)
C16—H16	0.9500	C108—C109	1.440 (9)
C16—C17	1.379 (9)	C109—H109	0.9500
C17—H17	0.9500	C109—C110	1.330 (9)
C17—C18	1.375 (9)	C110—H110	0.9500
C18—C19	1.400 (10)	C110—C111	1.455 (9)
C18—C21	1.496 (10)	C111—C122	1.395 (9)
C19—H19	0.9500	C112—C113	1.402 (9)
C19—C20	1.379 (10)	C112—C129	1.484 (9)
C20—H20	0.9500	C113—C116	1.428 (9)
C21—H21A	0.9800	C114—C115	1.416 (9)
C21—H21B	0.9800	C114—C122	1.401 (9)
C21—H21C	0.9800	C115—H115	0.9500
C22—C23	1.389 (10)	C115—C116	1.351 (9)
C22—C27	1.377 (10)	C116—H116	0.9500
C23—H23	0.9500	C117—C118	1.400 (9)
C23—C24	1.380 (10)	C117—C121	1.389 (9)
C24—H24	0.9500	C118—H118	0.9500
C24—C25	1.392 (10)	C118—C119	1.357 (9)
C25—C26	1.381 (10)	C119—H119	0.9500
C25—C28	1.514 (10)	C120—H120	0.9500
C26—H26	0.9500	C120—C121	1.371 (10)
C26—C27	1.384 (10)	C121—H121	0.9500
C27—H27	0.9500	C122—C123	1.503 (9)
C28—H28A	0.9800	C123—C124	1.342 (10)
C28—H28B	0.9800	C123—C128	1.344 (10)
C28—H28C	0.9800	C124—H124	0.9500
C29—C30	1.387 (10)	C124—C125	1.357 (11)
C29—C34	1.369 (10)	C125—H125	0.9500
C30—H30	0.9500	C125—C126	1.354 (11)
C30—C31	1.366 (11)	C126—C127	1.352 (10)
C31—H31	0.9500	C126—C135	1.431 (11)
C31—C32	1.387 (12)	C127—H127	0.9500
C32—C33	1.378 (11)	C127—C128	1.384 (11)
C32—C35	1.520 (12)	C128—H128	0.9500
C33—H33	0.9500	C129—C130	1.381 (9)
C33—C34	1.379 (10)	C129—C133	1.374 (9)
C34—H34	0.9500	C130—H130	0.9500
C35—H35A	0.9800	C130—C131	1.371 (9)
C35—H35B	0.9800	C131—H131	0.9500
C35—H35C	0.9800	C132—H132	0.9500
C36—C37	1.385 (10)	C132—C133	1.378 (10)
C36—C41	1.372 (11)	C133—H133	0.9500
C37—H37	0.9500	C134—H13A	0.9800
C37—C38	1.377 (11)	C134—H13B	0.9800
C38—H38	0.9500	C134—H13C	0.9800
C38—C39	1.358 (12)	C136—H13D	0.9800
C39—C40	1.372 (13)	C136—H13E	0.9800
C39—C42	1.527 (13)	C136—H13F	0.9800
O1—S1—O2	112.9 (4)	N3—C54—C48	124.9 (6)
O1—S1—O3	113.6 (4)	N3—C54—C55	108.8 (6)
O1—S1—C1	106.7 (3)	C48—C54—C55	126.2 (6)
O2—S1—O3	111.2 (3)	C54—C55—H55	126.1
O2—S1—C1	105.4 (3)	C56—C55—C54	107.8 (6)
O3—S1—C1	106.3 (3)	C56—C55—H55	126.1
O4—S2—O5	113.0 (4)	C55—C56—H56	126.2
O4—S2—O6	112.9 (3)	C55—C56—C57	107.6 (6)
O4—S2—C8	105.8 (3)	C57—C56—H56	126.2
O5—S2—O6	112.4 (4)	N3—C57—C56	108.3 (6)
O5—S2—C8	106.7 (3)	N3—C57—C63	126.6 (6)
O6—S2—C8	105.2 (3)	C63—C57—C56	125.0 (6)
O7—S3—O8	116.0 (3)	C50—C58—C68	118.1 (6)
O7—S3—O9	111.3 (4)	C59—C58—C50	125.8 (6)
O7—S3—C15	106.7 (3)	C59—C58—C68	115.8 (6)
O8—S3—O9	110.3 (3)	N4—C59—C58	125.9 (6)
O8—S3—C15	106.8 (3)	N4—C59—C62	108.3 (6)
O9—S3—C15	105.0 (3)	C58—C59—C62	125.5 (6)
O10—S4—O11	112.7 (4)	N4—C60—C61	109.0 (6)
O10—S4—O12	112.3 (3)	N4—C60—C73	126.5 (6)
O10—S4—C22	107.0 (3)	C73—C60—C61	124.5 (6)
O11—S4—O12	113.2 (4)	C60—C61—H61	126.2
O11—S4—C22	105.7 (3)	C62—C61—C60	107.7 (6)
O12—S4—C22	105.2 (3)	C62—C61—H61	126.2
O13—S5—O14	121.9 (6)	C59—C62—H62	126.4
O13—S5—O15	108.1 (7)	C61—C62—C59	107.1 (6)
O13—S5—C29	108.6 (4)	C61—C62—H62	126.4
O14—S5—O15	102.9 (6)	C57—C63—C64	125.7 (6)
O14—S5—C29	108.6 (4)	C57—C63—C80	118.7 (6)
O15—S5—C29	105.5 (4)	C64—C63—C80	115.2 (6)
O16—S6—O17	112.8 (5)	N5—C64—C63	126.2 (6)
O16—S6—O18	112.0 (7)	N5—C64—C65	109.0 (6)
O16—S6—C36	107.7 (4)	C63—C64—C65	124.6 (6)
O17—S6—O18	111.5 (5)	C64—C65—H65	126.4
O17—S6—C36	106.3 (3)	C66—C65—C64	107.1 (6)
O18—S6—C36	106.1 (4)	C66—C65—H65	126.4
H19A—O19—H19B	104.4	C65—C66—H66	126.4
H20A—O20—H20B	104.4	C65—C66—C67	107.2 (6)
H21D—O21—H21E	104.5	C67—C66—H66	126.4
H22A—O22—H22B	104.5	N5—C67—C66	108.3 (6)
H23A—O23—H23B	104.3	N5—C67—C73	127.2 (6)
H24A—O24—H24B	104.4	C73—C67—C66	124.5 (6)
H25A—O25—H25B	109.4	C69—C68—C58	121.0 (6)
H26A—O26—H26B	104.6	C72—C68—C58	121.6 (6)
H27A—O27—H27B	104.5	C72—C68—C69	117.2 (6)
H28D—O28—H28E	104.5	C68—C69—H69	119.8
H31A—O31—H31B	104.4	C70—C69—C68	120.4 (6)
H32A—O32—H32B	104.6	C70—C69—H69	119.8
C45—N1—C53	120.2 (7)	N6—C70—C69	120.5 (6)
C46—N1—C45	119.7 (6)	N6—C70—H70	119.7
C46—N1—C53	120.1 (7)	C69—C70—H70	119.7
C49—N2—H2	126.1	N6—C71—H71	119.7
C49—N2—C50	107.7 (5)	N6—C71—C72	120.6 (6)
C50—N2—H2	126.1	C72—C71—H71	119.7
C54—N3—H3	126.3	C68—C72—H72	119.7
C57—N3—H3	126.3	C71—C72—C68	120.6 (6)
C57—N3—C54	107.3 (5)	C71—C72—H72	119.7
C59—N4—H4	126.1	C60—C73—C67	123.7 (6)
C60—N4—H4	126.1	C60—C73—C74	117.8 (5)
C60—N4—C59	107.8 (5)	C67—C73—C74	118.5 (6)
C64—N5—H5	125.8	C75—C74—C73	121 (2)
C67—N5—H5	125.8	C79—C74—C73	120.3 (6)
C67—N5—C64	108.3 (5)	C79—C74—C86	117.7 (6)
C70—N6—C85	119.5 (6)	C86—C74—C73	122.0 (6)
C71—N6—C70	120.7 (6)	C88—C74—C73	123 (3)
C71—N6—C85	119.8 (6)	C88—C74—C75	116 (4)
C82—N7—C83	120.2 (6)	C74—C75—H75	119.2
C82—N7—C91	120.4 (6)	C76—C75—C74	122 (5)
C83—N7—C91	119.3 (7)	C76—C75—H75	119.2
C94—N9—C102	120.6 (8)	C75—C76—H76	119.4
C95—N9—C94	120.1 (7)	C75—C76—C77	121 (5)
C95—N9—C102	119.3 (9)	C77—C76—H76	119.4
C98—N10—H10	125.2	C76—C77—C89	118 (3)
C101—N10—H10	125.2	C78—C77—C87	119.4 (7)
C101—N10—C98	109.6 (5)	C78—C77—C90	121.4 (7)
C103—N11—C106	105.8 (5)	C87—C77—C90	119.2 (7)
C111—N12—C108	106.3 (5)	C90—C77—C76	124 (2)
C113—N13—H13	125.5	C90—C77—C89	116 (2)
C113—N13—C114	109.0 (5)	C77—C78—H78	119.7
C114—N13—H13	125.5	C77—C78—C79	120.7 (7)
C119—N14—C120	120.3 (6)	C79—C78—H78	119.7
C119—N14—C134	120.7 (6)	C74—C79—H79	119.3
C120—N14—C134	119.0 (6)	C78—C79—C74	121.3 (7)
C131—N15—C132	120.6 (6)	C78—C79—H79	119.3
C131—N15—C136	121.1 (6)	C81—C80—C63	120.5 (6)
C132—N15—C136	118.2 (6)	C84—C80—C63	122.4 (6)
C2—C1—S1	120.1 (6)	C84—C80—C81	116.9 (6)
C6—C1—S1	120.6 (6)	C80—C81—H81	119.7
C6—C1—C2	119.3 (7)	C82—C81—C80	120.6 (7)
C1—C2—H2A	120.0	C82—C81—H81	119.7
C1—C2—C3	120.0 (8)	N7—C82—C81	120.7 (7)
C3—C2—H2A	120.0	N7—C82—H82	119.6
C2—C3—H3A	119.2	C81—C82—H82	119.6
C2—C3—C4	121.6 (7)	N7—C83—H83	119.7
C4—C3—H3A	119.2	N7—C83—C84	120.6 (7)
C3—C4—C7	121.2 (8)	C84—C83—H83	119.7
C5—C4—C3	117.1 (7)	C80—C84—H84	119.6
C5—C4—C7	121.7 (8)	C83—C84—C80	120.7 (7)
C4—C5—H5A	119.2	C83—C84—H84	119.6
C4—C5—C6	121.6 (7)	N6—C85—H85A	109.5
C6—C5—H5A	119.2	N6—C85—H85B	109.5
C1—C6—C5	120.4 (7)	N6—C85—H85C	109.5
C1—C6—H6	119.8	H85A—C85—H85B	109.5
C5—C6—H6	119.8	H85A—C85—H85C	109.5
C4—C7—H7A	109.5	H85B—C85—H85C	109.5
C4—C7—H7B	109.5	C74—C86—H86	119.2
C4—C7—H7C	109.5	C87—C86—C74	121.7 (7)
H7A—C7—H7B	109.5	C87—C86—H86	119.2
H7A—C7—H7C	109.5	C77—C87—H87	120.4
H7B—C7—H7C	109.5	C86—C87—C77	119.2 (7)
C9—C8—S2	119.6 (6)	C86—C87—H87	120.4
C13—C8—S2	120.5 (6)	C74—C88—H88	116.3
C13—C8—C9	119.7 (7)	C74—C88—C89	127 (6)
C8—C9—H9	119.8	C89—C88—H88	116.3
C8—C9—C10	120.3 (7)	C77—C89—H89	124.4
C10—C9—H9	119.8	C88—C89—C77	111 (5)
C9—C10—H10D	119.8	C88—C89—H89	124.4
C11—C10—C9	120.4 (8)	N8—C90—C77	178.8 (8)
C11—C10—H10D	119.8	N7—C91—H91A	109.5
C10—C11—C12	118.6 (8)	N7—C91—H91B	109.5
C10—C11—C14	119.4 (9)	N7—C91—H91C	109.5
C12—C11—C14	122.0 (9)	H91A—C91—H91B	109.5
C11—C12—H12	119.6	H91A—C91—H91C	109.5
C13—C12—C11	120.9 (8)	H91B—C91—H91C	109.5
C13—C12—H12	119.6	C93—C92—C97	121.9 (6)
C8—C13—C12	120.1 (8)	C96—C92—C93	117.1 (6)
C8—C13—H13G	119.9	C96—C92—C97	121.0 (6)
C12—C13—H13G	119.9	C92—C93—H93	119.8
C11—C14—H14A	109.5	C94—C93—C92	120.3 (7)
C11—C14—H14B	109.5	C94—C93—H93	119.8
C11—C14—H14C	109.5	N9—C94—C93	121.4 (7)
H14A—C14—H14B	109.5	N9—C94—H94	119.3
H14A—C14—H14C	109.5	C93—C94—H94	119.3
H14B—C14—H14C	109.5	N9—C95—H95	119.3
C16—C15—S3	122.0 (5)	N9—C95—C96	121.3 (7)
C16—C15—C20	119.4 (6)	C96—C95—H95	119.3
C20—C15—S3	118.6 (5)	C92—C96—H96	120.1
C15—C16—H16	119.9	C95—C96—C92	119.7 (7)
C15—C16—C17	120.3 (6)	C95—C96—H96	120.1
C17—C16—H16	119.9	C98—C97—C92	117.9 (6)
C16—C17—H17	119.1	C98—C97—C103	125.2 (6)
C18—C17—C16	121.7 (6)	C103—C97—C92	116.9 (6)
C18—C17—H17	119.1	N10—C98—C97	126.3 (6)
C17—C18—C19	117.2 (6)	N10—C98—C99	106.8 (6)
C17—C18—C21	122.4 (7)	C97—C98—C99	126.9 (6)
C19—C18—C21	120.3 (7)	C98—C99—H99	125.9
C18—C19—H19	119.4	C100—C99—C98	108.2 (6)
C20—C19—C18	121.2 (7)	C100—C99—H99	125.9
C20—C19—H19	119.4	C99—C100—H100	125.8
C15—C20—C19	120.2 (6)	C99—C100—C101	108.3 (6)
C15—C20—H20	119.9	C101—C100—H100	125.8
C19—C20—H20	119.9	N10—C101—C100	107.0 (6)
C18—C21—H21A	109.5	N10—C101—C107	126.7 (6)
C18—C21—H21B	109.5	C107—C101—C100	126.2 (6)
C18—C21—H21C	109.5	N9—C102—H10A	109.5
H21A—C21—H21B	109.5	N9—C102—H10B	109.5
H21A—C21—H21C	109.5	N9—C102—H10C	109.5
H21B—C21—H21C	109.5	H10A—C102—H10B	109.5
C23—C22—S4	119.5 (6)	H10A—C102—H10C	109.5
C27—C22—S4	120.7 (6)	H10B—C102—H10C	109.5
C27—C22—C23	119.8 (7)	N11—C103—C97	125.0 (6)
C22—C23—H23	120.4	N11—C103—C104	109.8 (6)
C24—C23—C22	119.2 (7)	C97—C103—C104	125.0 (6)
C24—C23—H23	120.4	C103—C104—H104	126.6
C23—C24—H24	119.0	C105—C104—C103	106.8 (6)
C23—C24—C25	121.9 (7)	C105—C104—H104	126.6
C25—C24—H24	119.0	C104—C105—H105	126.2
C24—C25—C28	119.9 (7)	C104—C105—C106	107.7 (6)
C26—C25—C24	117.6 (7)	C106—C105—H105	126.2
C26—C25—C28	122.4 (7)	N11—C106—C105	109.8 (6)
C25—C26—H26	119.4	N11—C106—C112	126.3 (6)
C25—C26—C27	121.3 (7)	C112—C106—C105	123.9 (6)
C27—C26—H26	119.4	C101—C107—C108	126.0 (6)
C22—C27—C26	120.1 (7)	C101—C107—C117	117.7 (6)
C22—C27—H27	119.9	C108—C107—C117	116.2 (6)
C26—C27—H27	119.9	N12—C108—C107	125.8 (6)
C25—C28—H28A	109.5	N12—C108—C109	109.3 (6)
C25—C28—H28B	109.5	C107—C108—C109	124.8 (6)
C25—C28—H28C	109.5	C108—C109—H109	125.9
H28A—C28—H28B	109.5	C110—C109—C108	108.1 (6)
H28A—C28—H28C	109.5	C110—C109—H109	125.9
H28B—C28—H28C	109.5	C109—C110—H110	126.7
C30—C29—S5	119.9 (6)	C109—C110—C111	106.5 (6)
C34—C29—S5	120.5 (6)	C111—C110—H110	126.7
C34—C29—C30	119.6 (7)	N12—C111—C110	109.7 (5)
C29—C30—H30	120.1	N12—C111—C122	126.4 (6)
C31—C30—C29	119.8 (8)	C122—C111—C110	123.9 (6)
C31—C30—H30	120.1	C106—C112—C129	118.1 (6)
C30—C31—H31	119.2	C113—C112—C106	126.0 (6)
C30—C31—C32	121.5 (8)	C113—C112—C129	115.9 (6)
C32—C31—H31	119.2	N13—C113—C112	126.8 (6)
C31—C32—C35	120.8 (8)	N13—C113—C116	107.3 (6)
C33—C32—C31	117.8 (7)	C112—C113—C116	125.9 (6)
C33—C32—C35	121.4 (8)	N13—C114—C115	107.8 (5)
C32—C33—H33	119.4	N13—C114—C122	125.4 (6)
C32—C33—C34	121.2 (7)	C122—C114—C115	126.7 (6)
C34—C33—H33	119.4	C114—C115—H115	126.2
C29—C34—C33	120.1 (7)	C116—C115—C114	107.7 (6)
C29—C34—H34	120.0	C116—C115—H115	126.2
C33—C34—H34	120.0	C113—C116—H116	125.9
C32—C35—H35A	109.5	C115—C116—C113	108.2 (6)
C32—C35—H35B	109.5	C115—C116—H116	125.9
C32—C35—H35C	109.5	C118—C117—C107	121.3 (6)
H35A—C35—H35B	109.5	C121—C117—C107	121.2 (6)
H35A—C35—H35C	109.5	C121—C117—C118	117.4 (6)
H35B—C35—H35C	109.5	C117—C118—H118	119.7
C37—C36—S6	119.2 (6)	C119—C118—C117	120.6 (6)
C41—C36—S6	121.1 (6)	C119—C118—H118	119.7
C41—C36—C37	119.7 (7)	N14—C119—C118	120.8 (6)
C36—C37—H37	120.1	N14—C119—H119	119.6
C38—C37—C36	119.9 (8)	C118—C119—H119	119.6
C38—C37—H37	120.1	N14—C120—H120	119.6
C37—C38—H38	119.0	N14—C120—C121	120.9 (7)
C39—C38—C37	122.0 (9)	C121—C120—H120	119.6
C39—C38—H38	119.0	C117—C121—H121	120.0
C38—C39—C40	118.7 (8)	C120—C121—C117	120.0 (7)
C38—C39—C42	120.5 (11)	C120—C121—H121	120.0
C40—C39—C42	120.8 (11)	C111—C122—C114	125.1 (6)
C39—C40—H40	119.7	C111—C122—C123	117.7 (5)
C39—C40—C41	120.7 (9)	C114—C122—C123	117.0 (6)
C41—C40—H40	119.7	C124—C123—C122	120.2 (6)
C36—C41—C40	119.1 (8)	C124—C123—C128	117.0 (7)
C36—C41—H41	120.5	C128—C123—C122	122.8 (6)
C40—C41—H41	120.5	C123—C124—H124	118.9
C39—C42—H42A	109.5	C123—C124—C125	122.3 (8)
C39—C42—H42B	109.5	C125—C124—H124	118.9
C39—C42—H42C	109.5	C124—C125—H125	119.4
H42A—C42—H42B	109.5	C126—C125—C124	121.2 (8)
H42A—C42—H42C	109.5	C126—C125—H125	119.4
H42B—C42—H42C	109.5	C125—C126—C135	119.7 (7)
C44—C43—C47	117.2 (6)	C127—C126—C125	117.2 (7)
C44—C43—C48	122.4 (6)	C127—C126—C135	123.1 (7)
C47—C43—C48	120.4 (6)	C126—C127—H127	119.7
C43—C44—H44	119.9	C126—C127—C128	120.7 (7)
C45—C44—C43	120.2 (7)	C128—C127—H127	119.7
C45—C44—H44	119.9	C123—C128—C127	121.5 (7)
N1—C45—C44	121.1 (7)	C123—C128—H128	119.2
N1—C45—H45	119.4	C127—C128—H128	119.2
C44—C45—H45	119.4	C130—C129—C112	122.7 (6)
N1—C46—H46	119.0	C133—C129—C112	119.9 (6)
N1—C46—C47	121.9 (7)	C133—C129—C130	117.3 (6)
C47—C46—H46	119.0	C129—C130—H130	119.7
C43—C47—H47	120.2	C131—C130—C129	120.6 (6)
C46—C47—C43	119.7 (7)	C131—C130—H130	119.7
C46—C47—H47	120.2	N15—C131—C130	120.6 (6)
C49—C48—C43	116.6 (6)	N15—C131—H131	119.7
C54—C48—C43	117.8 (6)	C130—C131—H131	119.7
C54—C48—C49	125.5 (6)	N15—C132—H132	119.5
N2—C49—C48	125.8 (6)	N15—C132—C133	120.9 (6)
N2—C49—C52	108.6 (6)	C133—C132—H132	119.5
C48—C49—C52	125.5 (6)	C129—C133—C132	120.0 (7)
N2—C50—C51	108.1 (6)	C129—C133—H133	120.0
N2—C50—C58	125.9 (6)	C132—C133—H133	120.0
C58—C50—C51	125.9 (6)	N14—C134—H13A	109.5
C50—C51—H51	126.0	N14—C134—H13B	109.5
C52—C51—C50	108.1 (6)	N14—C134—H13C	109.5
C52—C51—H51	126.0	H13A—C134—H13B	109.5
C49—C52—H52	126.2	H13A—C134—H13C	109.5
C51—C52—C49	107.5 (6)	H13B—C134—H13C	109.5
C51—C52—H52	126.2	N16—C135—C126	179.4 (9)
N1—C53—H53A	109.5	N15—C136—H13D	109.5
N1—C53—H53B	109.5	N15—C136—H13E	109.5
N1—C53—H53C	109.5	N15—C136—H13F	109.5
H53A—C53—H53B	109.5	H13D—C136—H13E	109.5
H53A—C53—H53C	109.5	H13D—C136—H13F	109.5
H53B—C53—H53C	109.5	H13E—C136—H13F	109.5
S1—C1—C2—C3	−178.1 (6)	C58—C68—C72—C71	171.5 (6)
S1—C1—C6—C5	178.3 (5)	C59—N4—C60—C61	−1.1 (6)
S2—C8—C9—C10	−173.7 (6)	C59—N4—C60—C73	177.7 (6)
S2—C8—C13—C12	174.4 (6)	C59—C58—C68—C69	64.2 (8)
S3—C15—C16—C17	−179.7 (5)	C59—C58—C68—C72	−109.9 (7)
S3—C15—C20—C19	−179.5 (5)	C60—N4—C59—C58	−172.2 (6)
S4—C22—C23—C24	−177.7 (5)	C60—N4—C59—C62	1.6 (6)
S4—C22—C27—C26	177.8 (5)	C60—C61—C62—C59	0.9 (7)
S5—C29—C30—C31	179.8 (6)	C60—C73—C74—C75	114 (3)
S5—C29—C34—C33	−179.0 (5)	C60—C73—C74—C79	56.0 (8)
S6—C36—C37—C38	−177.3 (6)	C60—C73—C74—C86	−125.4 (7)
S6—C36—C41—C40	177.7 (6)	C60—C73—C74—C88	−61 (3)
O1—S1—C1—C2	−39.2 (7)	C61—C60—C73—C67	−171.3 (6)
O1—S1—C1—C6	142.6 (6)	C61—C60—C73—C74	11.1 (9)
O2—S1—C1—C2	81.1 (6)	C63—C64—C65—C66	−173.7 (6)
O2—S1—C1—C6	−97.2 (6)	C63—C80—C81—C82	−170.4 (6)
O3—S1—C1—C2	−160.8 (6)	C63—C80—C84—C83	171.7 (6)
O3—S1—C1—C6	21.0 (6)	C64—N5—C67—C66	1.0 (7)
O4—S2—C8—C9	86.5 (6)	C64—N5—C67—C73	−178.2 (6)
O4—S2—C8—C13	−87.9 (6)	C64—C63—C80—C81	104.5 (7)
O5—S2—C8—C9	−152.9 (6)	C64—C63—C80—C84	−70.4 (8)
O5—S2—C8—C13	32.7 (7)	C64—C65—C66—C67	−0.6 (7)
O6—S2—C8—C9	−33.3 (7)	C65—C66—C67—N5	−0.2 (7)
O6—S2—C8—C13	152.3 (6)	C65—C66—C67—C73	179.0 (6)
O7—S3—C15—C16	−15.7 (7)	C66—C67—C73—C60	179.2 (6)
O7—S3—C15—C20	165.6 (6)	C66—C67—C73—C74	−3.2 (9)
O8—S3—C15—C16	−140.4 (5)	C67—N5—C64—C63	173.5 (6)
O8—S3—C15—C20	40.9 (6)	C67—N5—C64—C65	−1.4 (7)
O9—S3—C15—C16	102.5 (6)	C67—C73—C74—C75	−63 (3)
O9—S3—C15—C20	−76.2 (6)	C67—C73—C74—C79	−121.7 (7)
O10—S4—C22—C23	−174.1 (5)	C67—C73—C74—C86	56.9 (8)
O10—S4—C22—C27	7.6 (6)	C67—C73—C74—C88	122 (3)
O11—S4—C22—C23	−53.7 (6)	C68—C58—C59—N4	173.2 (5)
O11—S4—C22—C27	127.9 (6)	C68—C58—C59—C62	0.4 (9)
O12—S4—C22—C23	66.3 (6)	C68—C69—C70—N6	−0.7 (10)
O12—S4—C22—C27	−112.1 (6)	C69—C68—C72—C71	−2.9 (9)
O13—S5—C29—C30	−72.8 (9)	C70—N6—C71—C72	3.0 (10)
O13—S5—C29—C34	106.3 (8)	C71—N6—C70—C69	−2.5 (10)
O14—S5—C29—C30	61.8 (8)	C72—C68—C69—C70	3.3 (9)
O14—S5—C29—C34	−119.1 (7)	C73—C60—C61—C62	−178.7 (6)
O15—S5—C29—C30	171.5 (7)	C73—C74—C75—C76	−170 (4)
O15—S5—C29—C34	−9.4 (8)	C73—C74—C79—C78	−179.8 (7)
O16—S6—C36—C37	−23.4 (7)	C73—C74—C86—C87	−179.1 (6)
O16—S6—C36—C41	158.4 (7)	C73—C74—C88—C89	173 (5)
O17—S6—C36—C37	97.7 (6)	C74—C75—C76—C77	−18 (9)
O17—S6—C36—C41	−80.5 (7)	C74—C86—C87—C77	−0.9 (11)
O18—S6—C36—C37	−143.5 (7)	C74—C88—C89—C77	10 (8)
O18—S6—C36—C41	38.3 (8)	C75—C74—C88—C89	−3 (8)
N1—C46—C47—C43	0.8 (10)	C75—C76—C77—C89	27 (8)
N2—C49—C52—C51	1.1 (7)	C75—C76—C77—C90	−170 (5)
N2—C50—C51—C52	0.6 (7)	C76—C77—C89—C88	−21 (6)
N2—C50—C58—C59	−4.3 (10)	C77—C78—C79—C74	−1.4 (12)
N2—C50—C58—C68	−178.1 (5)	C78—C77—C87—C86	1.1 (11)
N3—C54—C55—C56	1.6 (7)	C79—C74—C86—C87	−0.5 (10)
N3—C57—C63—C64	−0.4 (10)	C80—C63—C64—N5	−177.3 (6)
N3—C57—C63—C80	171.9 (6)	C80—C63—C64—C65	−3.1 (9)
N4—C59—C62—C61	−1.6 (7)	C80—C81—C82—N7	−2.3 (10)
N4—C60—C61—C62	0.1 (7)	C81—C80—C84—C83	−3.4 (10)
N4—C60—C73—C67	10.0 (9)	C82—N7—C83—C84	3.1 (10)
N4—C60—C73—C74	−167.5 (5)	C83—N7—C82—C81	−1.7 (10)
N5—C64—C65—C66	1.3 (7)	C84—C80—C81—C82	4.7 (9)
N5—C67—C73—C60	−1.8 (10)	C85—N6—C70—C69	175.8 (7)
N5—C67—C73—C74	175.8 (6)	C85—N6—C71—C72	−175.3 (6)
N6—C71—C72—C68	−0.2 (10)	C86—C74—C79—C78	1.6 (11)
N7—C83—C84—C80	−0.4 (10)	C87—C77—C78—C79	0.0 (12)
N9—C95—C96—C92	−0.1 (10)	C88—C74—C75—C76	6 (7)
N10—C98—C99—C100	0.1 (7)	C90—C77—C78—C79	−179.7 (7)
N10—C101—C107—C108	−1.8 (10)	C90—C77—C87—C86	−179.2 (7)
N10—C101—C107—C117	175.7 (6)	C90—C77—C89—C88	175 (4)
N11—C103—C104—C105	−0.6 (7)	C91—N7—C82—C81	174.3 (6)
N11—C106—C112—C113	5.7 (10)	C91—N7—C83—C84	−172.9 (6)
N11—C106—C112—C129	−170.4 (6)	C92—C93—C94—N9	−0.8 (11)
N12—C108—C109—C110	0.2 (7)	C92—C97—C98—N10	−178.7 (6)
N12—C111—C122—C114	0.2 (10)	C92—C97—C98—C99	0.6 (10)
N12—C111—C122—C123	174.6 (5)	C92—C97—C103—N11	177.8 (6)
N13—C113—C116—C115	0.2 (7)	C92—C97—C103—C104	−6.6 (9)
N13—C114—C115—C116	1.8 (7)	C93—C92—C96—C95	0.9 (9)
N13—C114—C122—C111	2.0 (10)	C93—C92—C97—C98	−62.7 (8)
N13—C114—C122—C123	−172.4 (5)	C93—C92—C97—C103	116.4 (7)
N14—C120—C121—C117	0.1 (11)	C94—N9—C95—C96	−1.2 (10)
N15—C132—C133—C129	0.0 (11)	C95—N9—C94—C93	1.6 (10)
C1—C2—C3—C4	0.8 (12)	C96—C92—C93—C94	−0.4 (10)
C2—C1—C6—C5	0.1 (10)	C96—C92—C97—C98	119.0 (7)
C2—C3—C4—C5	−1.9 (11)	C96—C92—C97—C103	−61.9 (8)
C2—C3—C4—C7	175.4 (7)	C97—C92—C93—C94	−178.8 (6)
C3—C4—C5—C6	2.2 (10)	C97—C92—C96—C95	179.3 (6)
C4—C5—C6—C1	−1.3 (10)	C97—C98—C99—C100	−179.3 (6)
C6—C1—C2—C3	0.2 (11)	C97—C103—C104—C105	−176.8 (6)
C7—C4—C5—C6	−175.1 (7)	C98—N10—C101—C100	0.5 (7)
C8—C9—C10—C11	0.0 (11)	C98—N10—C101—C107	179.3 (6)
C9—C8—C13—C12	0.1 (11)	C98—C97—C103—N11	−3.2 (10)
C9—C10—C11—C12	−1.4 (11)	C98—C97—C103—C104	172.5 (6)
C9—C10—C11—C14	176.7 (7)	C98—C99—C100—C101	0.2 (8)
C10—C11—C12—C13	2.2 (12)	C99—C100—C101—N10	−0.5 (7)
C11—C12—C13—C8	−1.6 (12)	C99—C100—C101—C107	−179.2 (6)
C13—C8—C9—C10	0.7 (11)	C100—C101—C107—C108	176.7 (6)
C14—C11—C12—C13	−175.8 (8)	C100—C101—C107—C117	−5.8 (10)
C15—C16—C17—C18	−0.9 (10)	C101—N10—C98—C97	179.1 (6)
C16—C15—C20—C19	1.8 (10)	C101—N10—C98—C99	−0.4 (7)
C16—C17—C18—C19	2.1 (10)	C101—C107—C108—N12	−0.8 (10)
C16—C17—C18—C21	−179.8 (6)	C101—C107—C108—C109	175.9 (6)
C17—C18—C19—C20	−1.3 (10)	C101—C107—C117—C118	−65.8 (8)
C18—C19—C20—C15	−0.6 (10)	C101—C107—C117—C121	117.9 (7)
C20—C15—C16—C17	−1.0 (10)	C102—N9—C94—C93	−178.1 (7)
C21—C18—C19—C20	−179.5 (6)	C102—N9—C95—C96	178.6 (6)
C22—C23—C24—C25	0.7 (10)	C103—N11—C106—C105	−0.4 (7)
C23—C22—C27—C26	−0.6 (9)	C103—N11—C106—C112	−178.7 (6)
C23—C24—C25—C26	−2.1 (10)	C103—C97—C98—N10	2.2 (10)
C23—C24—C25—C28	177.6 (6)	C103—C97—C98—C99	−178.5 (6)
C24—C25—C26—C27	2.2 (9)	C103—C104—C105—C106	0.4 (7)
C25—C26—C27—C22	−0.9 (9)	C104—C105—C106—N11	0.0 (7)
C27—C22—C23—C24	0.7 (10)	C104—C105—C106—C112	178.4 (6)
C28—C25—C26—C27	−177.5 (6)	C105—C106—C112—C113	−172.4 (6)
C29—C30—C31—C32	−1.1 (12)	C105—C106—C112—C129	11.5 (9)
C30—C29—C34—C33	0.1 (10)	C106—N11—C103—C97	176.8 (6)
C30—C31—C32—C33	0.8 (12)	C106—N11—C103—C104	0.6 (7)
C30—C31—C32—C35	179.6 (9)	C106—C112—C113—N13	0.3 (10)
C31—C32—C33—C34	0.0 (11)	C106—C112—C113—C116	−177.1 (6)
C32—C33—C34—C29	−0.4 (11)	C106—C112—C129—C130	−106.0 (7)
C34—C29—C30—C31	0.7 (11)	C106—C112—C129—C133	77.4 (8)
C35—C32—C33—C34	−178.8 (8)	C107—C108—C109—C110	−176.9 (6)
C36—C37—C38—C39	−1.2 (12)	C107—C117—C118—C119	−175.9 (6)
C37—C36—C41—C40	−0.4 (11)	C107—C117—C121—C120	176.2 (6)
C37—C38—C39—C40	1.1 (13)	C108—N12—C111—C110	0.2 (6)
C37—C38—C39—C42	−178.1 (8)	C108—N12—C111—C122	−180.0 (6)
C38—C39—C40—C41	−0.6 (13)	C108—C107—C117—C118	112.0 (7)
C39—C40—C41—C36	0.3 (12)	C108—C107—C117—C121	−64.3 (8)
C41—C36—C37—C38	0.9 (10)	C108—C109—C110—C111	−0.1 (7)
C42—C39—C40—C41	178.6 (8)	C109—C110—C111—N12	0.0 (7)
C43—C44—C45—N1	−0.3 (11)	C109—C110—C111—C122	−179.9 (6)
C43—C48—C49—N2	177.9 (5)	C110—C111—C122—C114	−180.0 (6)
C43—C48—C49—C52	−7.4 (9)	C110—C111—C122—C123	−5.5 (9)
C43—C48—C54—N3	−174.9 (6)	C111—N12—C108—C107	176.9 (6)
C43—C48—C54—C55	2.7 (9)	C111—N12—C108—C109	−0.3 (6)
C44—C43—C47—C46	−4.0 (9)	C111—C122—C123—C124	−79.8 (9)
C44—C43—C48—C49	116.7 (7)	C111—C122—C123—C128	99.8 (8)
C44—C43—C48—C54	−63.9 (8)	C112—C113—C116—C115	177.9 (6)
C45—N1—C46—C47	2.8 (10)	C112—C129—C130—C131	−175.1 (6)
C46—N1—C45—C44	−3.0 (10)	C112—C129—C133—C132	175.0 (6)
C47—C43—C44—C45	3.8 (10)	C113—N13—C114—C115	−1.7 (7)
C47—C43—C48—C49	−63.6 (8)	C113—N13—C114—C122	174.8 (6)
C47—C43—C48—C54	115.8 (7)	C113—C112—C129—C130	77.4 (8)
C48—C43—C44—C45	−176.5 (6)	C113—C112—C129—C133	−99.2 (7)
C48—C43—C47—C46	176.3 (6)	C114—N13—C113—C112	−176.8 (6)
C48—C49—C52—C51	−174.3 (6)	C114—N13—C113—C116	1.0 (7)
C48—C54—C55—C56	−176.4 (6)	C114—C115—C116—C113	−1.2 (7)
C49—N2—C50—C51	0.0 (6)	C114—C122—C123—C124	95.1 (9)
C49—N2—C50—C58	−178.1 (6)	C114—C122—C123—C128	−85.3 (9)
C49—C48—C54—N3	4.4 (10)	C115—C114—C122—C111	177.9 (6)
C49—C48—C54—C55	−177.9 (6)	C115—C114—C122—C123	3.4 (9)
C50—N2—C49—C48	174.7 (6)	C117—C107—C108—N12	−178.4 (6)
C50—N2—C49—C52	−0.6 (6)	C117—C107—C108—C109	−1.7 (9)
C50—C51—C52—C49	−1.0 (7)	C117—C118—C119—N14	−0.7 (10)
C50—C58—C59—N4	−0.8 (10)	C118—C117—C121—C120	−0.3 (10)
C50—C58—C59—C62	−173.7 (6)	C119—N14—C120—C121	−0.2 (11)
C50—C58—C68—C69	−121.3 (7)	C120—N14—C119—C118	0.4 (10)
C50—C58—C68—C72	64.6 (8)	C121—C117—C118—C119	0.5 (9)
C51—C50—C58—C59	178.0 (6)	C122—C114—C115—C116	−174.7 (6)
C51—C50—C58—C68	4.1 (9)	C122—C123—C124—C125	−178.9 (9)
C53—N1—C45—C44	174.5 (7)	C122—C123—C128—C127	−179.8 (9)
C53—N1—C46—C47	−174.7 (6)	C123—C124—C125—C126	−2.2 (18)
C54—N3—C57—C56	2.8 (7)	C124—C123—C128—C127	−0.2 (14)
C54—N3—C57—C63	−174.9 (6)	C124—C125—C126—C127	1.5 (16)
C54—C48—C49—N2	−1.4 (10)	C124—C125—C126—C135	−179.3 (10)
C54—C48—C49—C52	173.2 (6)	C125—C126—C127—C128	−0.3 (15)
C54—C55—C56—C57	0.1 (7)	C126—C127—C128—C123	−0.4 (16)
C55—C56—C57—N3	−1.8 (7)	C128—C123—C124—C125	1.4 (15)
C55—C56—C57—C63	175.9 (6)	C129—C112—C113—N13	176.5 (6)
C56—C57—C63—C64	−177.7 (6)	C129—C112—C113—C116	−0.8 (9)
C56—C57—C63—C80	−5.4 (9)	C129—C130—C131—N15	0.6 (10)
C57—N3—C54—C48	175.3 (6)	C130—C129—C133—C132	−1.8 (10)
C57—N3—C54—C55	−2.7 (7)	C131—N15—C132—C133	2.3 (10)
C57—C63—C64—N5	−4.7 (10)	C132—N15—C131—C130	−2.5 (10)
C57—C63—C64—C65	169.4 (6)	C133—C129—C130—C131	1.6 (10)
C57—C63—C80—C81	−68.6 (8)	C134—N14—C119—C118	−180.0 (7)
C57—C63—C80—C84	116.5 (7)	C134—N14—C120—C121	−179.7 (7)
C58—C50—C51—C52	178.7 (6)	C135—C126—C127—C128	−179.5 (9)
C58—C59—C62—C61	172.3 (6)	C136—N15—C131—C130	175.1 (6)
C58—C68—C69—C70	−171.1 (6)	C136—N15—C132—C133	−175.4 (7)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O19—H19A···O21	0.87	1.93	2.751 (7)	157
O19—H19B···N8	0.87	2.04	2.885 (9)	165
O20—H20A···O5	0.87	1.96	2.824 (7)	173
O20—H20B···O10	0.87	2.07	2.930 (7)	169
O21—H21D···O26	0.87	1.95	2.789 (9)	162
O21—H21E···O3^i	0.87	1.92	2.791 (8)	177
O22—H22A···O16	0.87	1.97	2.834 (8)	170
O22—H22B···O19^ii	0.87	2.05	2.869 (8)	157
O23—H23A···O15	0.87	1.93	2.755 (10)	159
O23—H23B···O17	0.87	1.96	2.807 (7)	162
O24—H24A···O8	0.87	2.01	2.872 (7)	174
O25—H25B···O35	0.87	2.37	2.977 (16)	128
O26—H26A···O12	0.87	1.90	2.753 (8)	167
O26—H26B···O28	0.87	1.89	2.738 (9)	165
O27—H27A···O20	0.87	2.17	2.930 (9)	146
O27—H27B···O22^iii	0.87	2.20	2.975 (9)	149
O28—H28D···O35	0.87	1.96	2.734 (11)	147
O28—H28E···O31	0.87	1.93	2.726 (11)	152
O31—H31A···O29	0.87	2.05	2.807 (11)	145
O31—H31B···O7	0.87	2.25	2.926 (11)	135
N2—H2···N3	0.88	2.36	2.899 (7)	120
N3—H3···N2	0.88	2.35	2.899 (7)	120
N10—H10···N11	0.88	2.33	2.887 (7)	121
N10—H10···N12	0.88	2.40	2.948 (7)	120
N13—H13···N12	0.88	2.33	2.884 (7)	121

Symmetry codes: (i) −x+2, −y+1, −z; (ii) −x+1, −y+1, −z; (iii) −x+1, y+1/2, −z−1/2.

(TriMCOOP)(besylate)3(H2O)4

Crystal data

3(C6H5O3S)·C45H36N7O2·4(H2O)·1[]	F(000) = 2616
Mr = 1250.35	Dx = 1.345 Mg m^−3
Monoclinic, P21/n	Cu Kα radiation, λ = 1.54184 Å
a = 20.92834 (15) Å	Cell parameters from 44580 reflections
b = 9.39850 (8) Å	θ = 4.3–78.4°
c = 32.2135 (2) Å	µ = 1.71 mm^−1
β = 102.9338 (7)°	T = 160 K
V = 6175.48 (8) Å^3	Plate, red
Z = 4	0.18 × 0.09 × 0.05 mm

Data collection

XtaLAB Synergy, Dualflex, Pilatus 200K diffractometer	13115 independent reflections
Radiation source: micro-focus sealed X-ray tube, PhotonJet (Cu) X-ray Source	11510 reflections with I > 2σ(I)
Mirror monochromator	Rint = 0.042
ω scans	θmax = 78.9°, θmin = 4.3°
Absorption correction: gaussian CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) 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 = −24→26
Tmin = 0.571, Tmax = 1.000	k = −11→11
87383 measured reflections	l = −40→40

Refinement

Refinement on F^2	54 restraints
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.073	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.200	w = 1/[σ^2(Fo^2) + (0.0746P)^2 + 10.9969P] where P = (Fo^2 + 2Fc^2)/3
S = 1.06	(Δ/σ)max = 0.006
13115 reflections	Δρmax = 0.80 e Å^−3
863 parameters	Δρmin = −0.66 e Å^−3

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	Occ. (<1)
S1	0.64698 (4)	0.17660 (9)	0.83726 (2)	0.0448 (2)
S2	0.40589 (5)	0.62089 (13)	0.83352 (3)	0.0630 (3)
S3	0.21354 (4)	0.76090 (10)	0.49927 (3)	0.0498 (2)
O1	0.53335 (16)	0.5194 (3)	0.70621 (8)	0.0620 (7)
H1	0.534 (3)	0.513 (6)	0.7312 (17)	0.093*
O2	0.54050 (15)	0.7492 (3)	0.72254 (7)	0.0591 (7)
O11	0.5867 (2)	0.1077 (5)	0.83299 (18)	0.0693 (17)	0.624 (6)
O11B	0.6203 (4)	0.0732 (9)	0.8680 (3)	0.073 (3)	0.376 (6)
O12	0.6876 (3)	0.1916 (7)	0.87787 (13)	0.0650 (16)	0.624 (6)
O12B	0.6880 (4)	0.2768 (13)	0.8633 (3)	0.075 (3)	0.376 (6)
O13	0.63924 (18)	0.3120 (4)	0.81224 (11)	0.0467 (11)	0.624 (6)
O13B	0.5877 (3)	0.2254 (7)	0.81075 (18)	0.050 (2)	0.376 (6)
O14	0.46764 (13)	0.6476 (3)	0.82199 (10)	0.0665 (7)
O15	0.40851 (19)	0.4957 (5)	0.86029 (10)	0.0982 (11)
O16	0.37973 (15)	0.7458 (4)	0.84908 (13)	0.0972 (11)
O17	0.15800 (12)	0.7904 (4)	0.51759 (9)	0.0656 (7)
O18	0.20769 (18)	0.6279 (3)	0.47600 (9)	0.0805 (9)
O19	0.22994 (13)	0.8790 (3)	0.47481 (10)	0.0691 (8)
O21	0.5229 (3)	0.4483 (6)	0.77937 (14)	0.0502 (11)	0.624 (6)
H21A	0.559 (3)	0.407 (2)	0.7932 (16)	0.080 (16)*
H21B	0.516 (3)	0.522 (6)	0.7967 (17)	0.088 (17)*
O21B	0.5568 (4)	0.4979 (9)	0.7909 (2)	0.0464 (17)	0.376 (6)
O22	1.01107 (19)	1.0736 (6)	0.43213 (13)	0.1109 (15)
H22A	0.988 (3)	1.043 (9)	0.4076 (13)	0.166*
H22B	1.048 (2)	1.113 (8)	0.430 (2)	0.166*
O25	0.13948 (13)	1.0561 (4)	0.42099 (9)	0.0635 (7)
H25A	0.169 (3)	1.014 (5)	0.4412 (14)	0.095*
O26	0.1554 (3)	0.7661 (6)	0.60640 (16)	0.1291 (18)
H26A	0.117 (3)	0.815 (9)	0.598 (2)	0.194*
H26B	0.170 (4)	0.755 (10)	0.5826 (15)	0.194*
N1	0.63479 (11)	0.7585 (3)	0.47359 (7)	0.0324 (5)
H1A	0.604717	0.772197	0.450041	0.039*	0.5
N2	0.49164 (11)	0.7806 (3)	0.45220 (7)	0.0314 (5)
H2	0.521775	0.779735	0.437027	0.038*	0.5
N3	0.49035 (11)	0.8152 (3)	0.36333 (7)	0.0320 (5)
H3	0.520399	0.810485	0.387252	0.038*	0.5
N4	0.63336 (11)	0.7855 (3)	0.38407 (7)	0.0330 (5)
H4	0.602800	0.779060	0.398821	0.040*	0.5
N5	0.18576 (13)	0.7835 (4)	0.36650 (10)	0.0556 (8)
N6	0.55813 (14)	0.9197 (4)	0.18339 (8)	0.0506 (7)
N7	0.93767 (15)	0.7329 (4)	0.46184 (14)	0.0750 (11)
C1	0.70102 (13)	0.7484 (3)	0.47644 (8)	0.0322 (6)
C2	0.73265 (14)	0.7273 (3)	0.52039 (9)	0.0366 (6)
H2A	0.778442	0.717232	0.531549	0.044*
C3	0.68565 (14)	0.7243 (3)	0.54292 (9)	0.0369 (6)
H3A	0.692426	0.711645	0.572848	0.044*
C4	0.62341 (13)	0.7437 (3)	0.51367 (8)	0.0317 (5)
C5	0.56223 (13)	0.7482 (3)	0.52400 (8)	0.0326 (6)
C6	0.50188 (13)	0.7701 (3)	0.49557 (9)	0.0337 (6)
C7	0.43996 (14)	0.7800 (4)	0.50824 (10)	0.0427 (7)
H7	0.433658	0.776456	0.536522	0.051*
C8	0.39287 (14)	0.7952 (4)	0.47237 (9)	0.0409 (7)
H8	0.347178	0.805488	0.470606	0.049*
C9	0.42521 (13)	0.7929 (3)	0.43702 (9)	0.0331 (6)
C10	0.39313 (13)	0.8020 (3)	0.39405 (9)	0.0322 (5)
C11	0.42384 (13)	0.8124 (3)	0.35983 (8)	0.0318 (5)
C12	0.39248 (14)	0.8202 (3)	0.31533 (9)	0.0353 (6)
H12	0.346589	0.819004	0.303623	0.042*
C13	0.43998 (14)	0.8295 (3)	0.29322 (9)	0.0376 (6)
H13	0.433538	0.836737	0.263153	0.045*
C14	0.50210 (14)	0.8266 (3)	0.32333 (8)	0.0335 (6)
C15	0.56325 (14)	0.8297 (3)	0.31302 (8)	0.0352 (6)
C16	0.62407 (14)	0.8092 (3)	0.34124 (9)	0.0354 (6)
C17	0.68665 (15)	0.8126 (4)	0.32941 (9)	0.0427 (7)
H17	0.693684	0.828180	0.301637	0.051*
C18	0.73311 (14)	0.7896 (4)	0.36498 (9)	0.0414 (7)
H18	0.779069	0.784686	0.367104	0.050*
C19	0.69960 (13)	0.7738 (3)	0.39943 (9)	0.0343 (6)
C20	0.73147 (13)	0.7552 (3)	0.44216 (9)	0.0333 (6)
C21	0.56004 (13)	0.7234 (3)	0.56978 (8)	0.0327 (6)
C22	0.55299 (18)	0.5878 (3)	0.58393 (10)	0.0455 (7)
H22	0.551862	0.509764	0.565047	0.055*
C23	0.54749 (18)	0.5634 (3)	0.62546 (10)	0.0463 (7)
H23	0.542397	0.469028	0.634784	0.056*
C24	0.54942 (13)	0.6761 (3)	0.65330 (8)	0.0323 (6)
C25	0.5574 (2)	0.8112 (4)	0.63934 (10)	0.0521 (9)
H25	0.559307	0.889201	0.658324	0.063*
C26	0.5626 (2)	0.8352 (4)	0.59780 (10)	0.0559 (10)
H26	0.568050	0.929476	0.588555	0.067*
C27	0.54053 (14)	0.6535 (3)	0.69767 (9)	0.0375 (6)
C28	0.32012 (13)	0.7972 (3)	0.38404 (9)	0.0356 (6)
C29	0.28821 (14)	0.6787 (4)	0.39503 (10)	0.0414 (7)
H29	0.312863	0.600390	0.408804	0.050*
C30	0.22105 (16)	0.6745 (4)	0.38604 (11)	0.0506 (8)
H30	0.199389	0.593185	0.393800	0.061*
C31	0.21502 (18)	0.9002 (5)	0.35547 (12)	0.0601 (10)
H31	0.189157	0.977103	0.341780	0.072*
C32	0.28195 (16)	0.9090 (4)	0.36388 (11)	0.0475 (7)
H32	0.302385	0.991685	0.355901	0.057*
C33	0.11291 (17)	0.7777 (6)	0.35714 (18)	0.0885 (17)
H33A	0.096584	0.846585	0.375129	0.133*
H33B	0.098832	0.681791	0.363033	0.133*
H33C	0.095328	0.800910	0.327094	0.133*
C34	0.56336 (14)	0.8608 (4)	0.26751 (9)	0.0388 (6)
C35	0.54119 (15)	0.9917 (4)	0.25013 (9)	0.0427 (7)
H35	0.527443	1.062269	0.267360	0.051*
C36	0.53915 (16)	1.0190 (4)	0.20800 (10)	0.0487 (8)
H36	0.524193	1.108879	0.196198	0.058*
C37	0.58081 (19)	0.7941 (5)	0.19947 (10)	0.0583 (10)
H37	0.594473	0.725571	0.181571	0.070*
C38	0.58468 (18)	0.7625 (4)	0.24162 (10)	0.0507 (8)
H38	0.601894	0.673528	0.252931	0.061*
C39	0.5499 (2)	0.9492 (6)	0.13734 (11)	0.0711 (12)
H39A	0.579118	0.887232	0.125572	0.107*
H39B	0.560863	1.048947	0.133324	0.107*
H39C	0.504356	0.931121	0.122643	0.107*
C40	0.80460 (13)	0.7443 (3)	0.45136 (9)	0.0358 (6)
C41	0.83595 (15)	0.6200 (4)	0.44459 (10)	0.0453 (7)
H41	0.810994	0.536919	0.435280	0.054*
C42	0.90322 (17)	0.6161 (5)	0.45127 (12)	0.0548 (9)
H42	0.924791	0.529039	0.448244	0.066*
C43	0.90929 (19)	0.8536 (5)	0.4691 (2)	0.098 (2)
H43	0.935400	0.935957	0.477261	0.118*
C44	0.84278 (17)	0.8611 (4)	0.46513 (16)	0.0662 (12)
H44	0.823220	0.946747	0.471849	0.079*
C45	1.0103 (2)	0.7273 (8)	0.4667 (3)	0.163 (4)
H45A	1.031130	0.699757	0.495977	0.244*
H45B	1.026358	0.821251	0.460607	0.244*
H45C	1.021153	0.657314	0.446831	0.244*
C51	0.69163 (14)	0.0699 (3)	0.80843 (9)	0.0385 (6)
C52	0.65947 (15)	−0.0356 (4)	0.78146 (10)	0.0441 (7)
H52	0.614077	−0.052458	0.779247	0.053*
C53	0.69385 (17)	−0.1159 (4)	0.75786 (11)	0.0516 (8)
H53	0.671848	−0.188162	0.739478	0.062*
C54	0.75954 (18)	−0.0923 (4)	0.76069 (12)	0.0549 (9)
H54	0.782652	−0.146410	0.743891	0.066*
C55	0.79154 (17)	0.0107 (4)	0.78814 (12)	0.0559 (9)
H55	0.837180	0.025467	0.790803	0.067*
C56	0.75791 (16)	0.0925 (4)	0.81180 (11)	0.0494 (8)
H56	0.780236	0.164131	0.830334	0.059*
C57	0.34983 (19)	0.5756 (5)	0.78589 (14)	0.0611 (8)
C58	0.3572 (3)	0.6272 (6)	0.74681 (15)	0.0854 (14)
H58	0.394104	0.684451	0.745361	0.102*
C59	0.3111 (4)	0.5956 (8)	0.71003 (18)	0.110 (2)
H59	0.315930	0.633368	0.683551	0.132*
C60	0.2582 (3)	0.5097 (8)	0.7114 (2)	0.110 (2)
H60	0.226627	0.488377	0.686015	0.132*
C61	0.2518 (2)	0.4565 (6)	0.7491 (2)	0.0904 (17)
H61	0.215821	0.395954	0.750072	0.108*
C62	0.2971 (2)	0.4891 (5)	0.78654 (16)	0.0713 (11)
H62	0.291592	0.451063	0.812831	0.086*
C63	0.28114 (16)	0.7392 (4)	0.54321 (11)	0.0454 (7)
C64	0.3020 (3)	0.8513 (5)	0.56992 (17)	0.0952 (19)
H64	0.282147	0.942048	0.563795	0.114*
C65	0.3517 (3)	0.8329 (6)	0.60580 (18)	0.102 (2)
H65	0.366101	0.910909	0.624286	0.123*
C66	0.38004 (19)	0.7032 (5)	0.61456 (14)	0.0686 (11)
H66	0.413138	0.689283	0.639712	0.082*
C67	0.3608 (2)	0.5936 (5)	0.58722 (17)	0.0755 (13)
H67	0.381390	0.503318	0.592920	0.091*
C68	0.31141 (18)	0.6125 (4)	0.55103 (15)	0.0612 (10)
H68	0.298872	0.535824	0.531692	0.073*
H25B	0.159 (2)	1.119 (5)	0.4079 (16)	0.10 (2)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
S1	0.0444 (4)	0.0463 (4)	0.0389 (4)	0.0063 (3)	−0.0007 (3)	−0.0023 (3)
S2	0.0499 (5)	0.0867 (7)	0.0601 (5)	−0.0084 (5)	0.0285 (4)	−0.0106 (5)
S3	0.0499 (5)	0.0528 (5)	0.0472 (4)	0.0050 (4)	0.0117 (3)	−0.0039 (4)
O1	0.101 (2)	0.0470 (14)	0.0467 (13)	0.0090 (14)	0.0352 (14)	0.0129 (11)
O2	0.0912 (19)	0.0519 (15)	0.0400 (12)	0.0006 (13)	0.0269 (12)	−0.0016 (11)
O11	0.064 (3)	0.065 (3)	0.092 (4)	−0.015 (2)	0.046 (3)	−0.016 (3)
O11B	0.084 (6)	0.062 (5)	0.090 (7)	0.021 (4)	0.055 (5)	0.014 (4)
O12	0.078 (3)	0.082 (4)	0.025 (2)	0.031 (3)	−0.0069 (19)	−0.004 (2)
O12B	0.068 (5)	0.091 (7)	0.060 (6)	−0.008 (5)	0.003 (4)	−0.039 (5)
O13	0.052 (2)	0.046 (2)	0.0407 (19)	0.0099 (17)	0.0077 (16)	0.0055 (15)
O13B	0.051 (4)	0.056 (4)	0.037 (3)	0.021 (3)	−0.002 (3)	−0.004 (3)
O14	0.0482 (13)	0.0794 (19)	0.0792 (18)	0.0073 (12)	0.0296 (12)	0.0028 (15)
O15	0.111 (3)	0.123 (3)	0.0621 (18)	−0.035 (2)	0.0225 (17)	0.0124 (19)
O16	0.0533 (16)	0.121 (2)	0.127 (3)	−0.0133 (17)	0.0414 (18)	−0.063 (2)
O17	0.0424 (13)	0.094 (2)	0.0602 (15)	−0.0039 (13)	0.0118 (11)	−0.0162 (15)
O18	0.106 (2)	0.069 (2)	0.0586 (17)	0.0117 (17)	0.0036 (16)	−0.0210 (15)
O19	0.0568 (15)	0.0741 (19)	0.0760 (18)	0.0144 (14)	0.0138 (13)	0.0267 (15)
O21	0.048 (3)	0.064 (3)	0.040 (2)	0.013 (2)	0.0125 (19)	0.014 (2)
O21B	0.046 (4)	0.056 (5)	0.042 (4)	0.011 (4)	0.020 (3)	0.013 (3)
O22	0.070 (2)	0.170 (5)	0.094 (3)	0.006 (3)	0.022 (2)	−0.023 (3)
O25	0.0557 (15)	0.0734 (19)	0.0582 (16)	0.0096 (14)	0.0060 (12)	0.0166 (14)
O26	0.148 (4)	0.141 (4)	0.124 (4)	0.032 (3)	0.086 (3)	0.044 (3)
N1	0.0275 (11)	0.0405 (13)	0.0289 (11)	0.0008 (9)	0.0056 (9)	0.0030 (9)
N2	0.0276 (11)	0.0369 (12)	0.0291 (11)	−0.0019 (9)	0.0049 (8)	0.0013 (9)
N3	0.0306 (11)	0.0364 (12)	0.0283 (11)	0.0001 (9)	0.0050 (9)	−0.0007 (9)
N4	0.0293 (11)	0.0410 (13)	0.0286 (11)	0.0010 (9)	0.0066 (9)	0.0027 (9)
N5	0.0275 (13)	0.076 (2)	0.0594 (18)	0.0081 (13)	0.0023 (12)	−0.0211 (16)
N6	0.0484 (15)	0.075 (2)	0.0284 (12)	0.0090 (14)	0.0086 (11)	0.0049 (13)
N7	0.0281 (14)	0.075 (2)	0.118 (3)	0.0033 (15)	0.0084 (17)	−0.011 (2)
C1	0.0284 (13)	0.0354 (14)	0.0317 (13)	0.0010 (10)	0.0040 (10)	0.0006 (11)
C2	0.0293 (13)	0.0464 (17)	0.0311 (13)	0.0025 (12)	0.0004 (10)	0.0014 (12)
C3	0.0328 (14)	0.0465 (17)	0.0292 (13)	0.0021 (12)	0.0027 (11)	0.0030 (12)
C4	0.0326 (13)	0.0339 (14)	0.0275 (12)	−0.0014 (11)	0.0044 (10)	0.0016 (10)
C5	0.0330 (13)	0.0351 (14)	0.0293 (13)	−0.0027 (11)	0.0060 (10)	0.0013 (11)
C6	0.0299 (13)	0.0402 (15)	0.0309 (13)	−0.0027 (11)	0.0069 (10)	0.0034 (11)
C7	0.0333 (14)	0.062 (2)	0.0343 (14)	−0.0015 (13)	0.0106 (12)	0.0042 (14)
C8	0.0277 (13)	0.0575 (19)	0.0384 (15)	−0.0008 (12)	0.0091 (11)	0.0050 (13)
C9	0.0286 (13)	0.0361 (14)	0.0343 (13)	−0.0017 (11)	0.0067 (10)	0.0017 (11)
C10	0.0286 (13)	0.0311 (14)	0.0354 (13)	0.0010 (10)	0.0041 (10)	0.0006 (11)
C11	0.0307 (13)	0.0318 (14)	0.0308 (13)	0.0000 (10)	0.0022 (10)	−0.0012 (10)
C12	0.0312 (13)	0.0403 (15)	0.0304 (13)	0.0022 (11)	−0.0018 (10)	−0.0024 (11)
C13	0.0377 (15)	0.0447 (17)	0.0271 (13)	0.0029 (12)	0.0005 (11)	0.0001 (11)
C14	0.0370 (14)	0.0357 (14)	0.0262 (12)	0.0021 (11)	0.0034 (10)	−0.0020 (10)
C15	0.0402 (15)	0.0385 (15)	0.0264 (12)	0.0035 (12)	0.0067 (11)	0.0004 (11)
C16	0.0342 (14)	0.0435 (16)	0.0285 (13)	0.0020 (12)	0.0067 (11)	0.0007 (11)
C17	0.0387 (15)	0.061 (2)	0.0310 (14)	0.0009 (14)	0.0125 (12)	0.0026 (13)
C18	0.0318 (14)	0.0581 (19)	0.0364 (14)	0.0026 (13)	0.0118 (12)	0.0020 (13)
C19	0.0300 (13)	0.0395 (15)	0.0339 (13)	0.0012 (11)	0.0085 (11)	0.0007 (11)
C20	0.0292 (13)	0.0363 (15)	0.0341 (13)	0.0015 (11)	0.0064 (10)	0.0004 (11)
C21	0.0289 (13)	0.0381 (15)	0.0308 (13)	−0.0016 (11)	0.0059 (10)	0.0022 (11)
C22	0.069 (2)	0.0342 (16)	0.0360 (15)	0.0075 (14)	0.0166 (14)	−0.0017 (12)
C23	0.069 (2)	0.0325 (15)	0.0408 (16)	0.0080 (14)	0.0199 (15)	0.0075 (12)
C24	0.0299 (13)	0.0361 (14)	0.0302 (13)	0.0032 (11)	0.0056 (10)	0.0030 (11)
C25	0.087 (3)	0.0373 (17)	0.0343 (15)	−0.0149 (17)	0.0192 (16)	−0.0060 (13)
C26	0.098 (3)	0.0356 (17)	0.0367 (16)	−0.0226 (18)	0.0214 (17)	−0.0017 (13)
C27	0.0331 (14)	0.0439 (17)	0.0367 (14)	0.0055 (12)	0.0106 (11)	0.0061 (12)
C28	0.0303 (13)	0.0412 (16)	0.0339 (13)	0.0029 (11)	0.0044 (11)	−0.0026 (12)
C29	0.0329 (14)	0.0450 (17)	0.0444 (16)	−0.0026 (12)	0.0048 (12)	−0.0034 (13)
C30	0.0343 (16)	0.067 (2)	0.0505 (18)	−0.0090 (15)	0.0087 (14)	−0.0160 (16)
C31	0.0415 (18)	0.074 (3)	0.059 (2)	0.0203 (18)	−0.0007 (16)	−0.0074 (19)
C32	0.0417 (16)	0.0493 (19)	0.0503 (18)	0.0106 (14)	0.0074 (14)	0.0030 (15)
C33	0.0243 (17)	0.122 (4)	0.113 (4)	0.006 (2)	0.003 (2)	−0.047 (3)
C34	0.0367 (14)	0.0516 (18)	0.0280 (13)	0.0055 (13)	0.0067 (11)	0.0015 (12)
C35	0.0422 (16)	0.0519 (19)	0.0348 (14)	0.0058 (14)	0.0105 (12)	0.0035 (13)
C36	0.0462 (17)	0.063 (2)	0.0370 (15)	0.0098 (15)	0.0102 (13)	0.0107 (15)
C37	0.063 (2)	0.080 (3)	0.0321 (16)	0.018 (2)	0.0129 (15)	−0.0045 (16)
C38	0.061 (2)	0.058 (2)	0.0344 (15)	0.0171 (17)	0.0127 (14)	0.0015 (14)
C39	0.077 (3)	0.107 (4)	0.0279 (16)	0.005 (2)	0.0081 (16)	0.0105 (19)
C40	0.0299 (13)	0.0461 (17)	0.0308 (13)	0.0022 (11)	0.0057 (10)	0.0018 (12)
C41	0.0381 (16)	0.0530 (19)	0.0453 (17)	0.0042 (14)	0.0105 (13)	−0.0037 (14)
C42	0.0424 (18)	0.067 (2)	0.056 (2)	0.0164 (17)	0.0129 (15)	−0.0004 (17)
C43	0.0315 (19)	0.067 (3)	0.184 (6)	−0.0057 (19)	0.001 (3)	−0.030 (3)
C44	0.0316 (16)	0.051 (2)	0.110 (3)	0.0018 (15)	0.0023 (18)	−0.019 (2)
C45	0.029 (2)	0.119 (6)	0.333 (13)	0.011 (3)	0.026 (4)	−0.032 (7)
C51	0.0391 (15)	0.0387 (15)	0.0323 (14)	0.0053 (12)	−0.0033 (11)	0.0057 (12)
C52	0.0367 (15)	0.0514 (19)	0.0391 (15)	0.0026 (13)	−0.0025 (12)	−0.0001 (14)
C53	0.0505 (19)	0.052 (2)	0.0461 (18)	0.0069 (15)	−0.0023 (14)	−0.0091 (15)
C54	0.0496 (19)	0.062 (2)	0.0518 (19)	0.0162 (17)	0.0080 (15)	−0.0009 (17)
C55	0.0400 (17)	0.063 (2)	0.063 (2)	0.0013 (16)	0.0093 (15)	0.0009 (18)
C56	0.0422 (17)	0.0494 (19)	0.0529 (19)	−0.0034 (14)	0.0028 (14)	−0.0009 (15)
C57	0.0548 (17)	0.065 (2)	0.0706 (18)	0.0088 (15)	0.0278 (15)	−0.0033 (16)
C58	0.113 (4)	0.086 (3)	0.062 (2)	−0.008 (3)	0.030 (2)	−0.009 (2)
C59	0.145 (6)	0.117 (5)	0.064 (3)	0.014 (5)	0.017 (4)	−0.003 (3)
C60	0.099 (4)	0.122 (6)	0.098 (5)	0.021 (4)	−0.001 (4)	−0.043 (4)
C61	0.058 (3)	0.094 (4)	0.119 (4)	0.004 (2)	0.020 (3)	−0.039 (4)
C62	0.054 (2)	0.073 (3)	0.091 (3)	0.0036 (17)	0.026 (2)	−0.014 (2)
C63	0.0462 (17)	0.0443 (18)	0.0485 (17)	0.0022 (14)	0.0165 (14)	0.0012 (14)
C64	0.111 (4)	0.062 (3)	0.088 (3)	0.036 (3)	−0.029 (3)	−0.026 (2)
C65	0.107 (4)	0.087 (4)	0.088 (4)	0.031 (3)	−0.030 (3)	−0.032 (3)
C66	0.044 (2)	0.089 (3)	0.068 (3)	0.002 (2)	0.0047 (18)	0.014 (2)
C67	0.048 (2)	0.056 (2)	0.116 (4)	0.0033 (18)	0.005 (2)	0.028 (3)
C68	0.0488 (19)	0.0418 (19)	0.092 (3)	−0.0023 (15)	0.0148 (19)	0.0046 (19)

Geometric parameters (Å, º)

S1—O11	1.397 (4)	C19—C20	1.400 (4)
S1—O11B	1.576 (8)	C20—C40	1.496 (4)
S1—O12	1.399 (4)	C21—C22	1.372 (4)
S1—O12B	1.417 (8)	C21—C26	1.378 (4)
S1—O13	1.496 (4)	C22—H22	0.9500
S1—O13B	1.415 (6)	C22—C23	1.387 (4)
S1—C51	1.769 (3)	C23—H23	0.9500
S2—O14	1.444 (3)	C23—C24	1.383 (4)
S2—O15	1.453 (4)	C24—C25	1.369 (4)
S2—O16	1.432 (3)	C24—C27	1.497 (4)
S2—C57	1.762 (5)	C25—H25	0.9500
S3—O17	1.443 (3)	C25—C26	1.385 (4)
S3—O18	1.449 (3)	C26—H26	0.9500
S3—O19	1.446 (3)	C28—C29	1.385 (4)
S3—C63	1.775 (4)	C28—C32	1.389 (4)
O1—H1	0.80 (5)	C29—H29	0.9500
O1—C27	1.306 (4)	C29—C30	1.371 (4)
O2—C27	1.204 (4)	C30—H30	0.9500
O21—H21A	0.88 (5)	C31—H31	0.9500
O21—H21B	0.92 (6)	C31—C32	1.368 (5)
O21B—H21A	0.86 (2)	C32—H32	0.9500
O21B—H21B	0.95 (5)	C33—H33A	0.9800
O22—H22A	0.88 (2)	C33—H33B	0.9800
O22—H22B	0.87 (2)	C33—H33C	0.9800
O25—H25A	0.88 (4)	C34—C35	1.388 (4)
O25—H25B	0.87 (2)	C34—C38	1.384 (4)
O26—H26A	0.91 (2)	C35—H35	0.9500
O26—H26B	0.89 (2)	C35—C36	1.372 (4)
N1—H1A	0.8800	C36—H36	0.9500
N1—C1	1.372 (3)	C37—H37	0.9500
N1—C4	1.371 (3)	C37—C38	1.375 (4)
N2—H2	0.8800	C38—H38	0.9500
N2—C6	1.369 (3)	C39—H39A	0.9800
N2—C9	1.372 (3)	C39—H39B	0.9800
N3—H3	0.8800	C39—H39C	0.9800
N3—C11	1.371 (3)	C40—C41	1.381 (4)
N3—C14	1.369 (3)	C40—C44	1.371 (5)
N4—H4	0.8800	C41—H41	0.9500
N4—C16	1.368 (3)	C41—C42	1.376 (5)
N4—C19	1.368 (3)	C42—H42	0.9500
N5—C30	1.335 (5)	C43—H43	0.9500
N5—C31	1.343 (6)	C43—C44	1.371 (5)
N5—C33	1.487 (4)	C44—H44	0.9500
N6—C36	1.341 (5)	C45—H45A	0.9800
N6—C37	1.333 (5)	C45—H45B	0.9800
N6—C39	1.481 (4)	C45—H45C	0.9800
N7—C42	1.316 (5)	C51—C52	1.389 (4)
N7—C43	1.325 (6)	C51—C56	1.383 (4)
N7—C45	1.494 (5)	C52—H52	0.9500
C1—C2	1.436 (4)	C52—C53	1.382 (5)
C1—C20	1.394 (4)	C53—H53	0.9500
C2—H2A	0.9500	C53—C54	1.375 (5)
C2—C3	1.347 (4)	C54—H54	0.9500
C3—H3A	0.9500	C54—C55	1.379 (5)
C3—C4	1.438 (4)	C55—H55	0.9500
C4—C5	1.394 (4)	C55—C56	1.381 (5)
C5—C6	1.399 (4)	C56—H56	0.9500
C5—C21	1.504 (4)	C57—C58	1.390 (6)
C6—C7	1.446 (4)	C57—C62	1.374 (6)
C7—H7	0.9500	C58—H58	0.9500
C7—C8	1.348 (4)	C58—C59	1.383 (8)
C8—H8	0.9500	C59—H59	0.9500
C8—C9	1.449 (4)	C59—C60	1.378 (10)
C9—C10	1.399 (4)	C60—H60	0.9500
C10—C11	1.398 (4)	C60—C61	1.347 (9)
C10—C28	1.490 (4)	C61—H61	0.9500
C11—C12	1.439 (4)	C61—C62	1.393 (7)
C12—H12	0.9500	C62—H62	0.9500
C12—C13	1.349 (4)	C63—C64	1.368 (5)
C13—H13	0.9500	C63—C68	1.346 (5)
C13—C14	1.438 (4)	C64—H64	0.9500
C14—C15	1.393 (4)	C64—C65	1.383 (6)
C15—C16	1.402 (4)	C65—H65	0.9500
C15—C34	1.495 (4)	C65—C66	1.357 (7)
C16—C17	1.444 (4)	C66—H66	0.9500
C17—H17	0.9500	C66—C67	1.357 (6)
C17—C18	1.344 (4)	C67—H67	0.9500
C18—H18	0.9500	C67—C68	1.386 (6)
C18—C19	1.447 (4)	C68—H68	0.9500
O11—S1—O12	119.0 (4)	C26—C25—H25	119.7
O11—S1—O13	110.8 (3)	C21—C26—C25	120.6 (3)
O11—S1—C51	104.9 (2)	C21—C26—H26	119.7
O11B—S1—C51	106.5 (3)	C25—C26—H26	119.7
O12—S1—O13	112.8 (3)	O1—C27—C24	112.5 (3)
O12—S1—C51	105.4 (2)	O2—C27—O1	124.2 (3)
O12B—S1—O11B	106.9 (6)	O2—C27—C24	123.2 (3)
O12B—S1—C51	111.5 (4)	C29—C28—C10	119.9 (3)
O13—S1—C51	101.85 (17)	C29—C28—C32	117.9 (3)
O13B—S1—O11B	101.1 (5)	C32—C28—C10	122.2 (3)
O13B—S1—O12B	118.4 (6)	C28—C29—H29	120.0
O13B—S1—C51	111.2 (3)	C30—C29—C28	120.0 (3)
O14—S2—O15	112.1 (2)	C30—C29—H29	120.0
O14—S2—C57	106.12 (18)	N5—C30—C29	120.7 (3)
O15—S2—C57	104.5 (2)	N5—C30—H30	119.7
O16—S2—O14	112.4 (2)	C29—C30—H30	119.7
O16—S2—O15	115.0 (2)	N5—C31—H31	119.9
O16—S2—C57	105.7 (2)	N5—C31—C32	120.3 (4)
O17—S3—O18	113.3 (2)	C32—C31—H31	119.9
O17—S3—O19	112.71 (18)	C28—C32—H32	119.9
O17—S3—C63	105.50 (16)	C31—C32—C28	120.2 (4)
O18—S3—C63	105.87 (18)	C31—C32—H32	119.9
O19—S3—O18	112.5 (2)	N5—C33—H33A	109.5
O19—S3—C63	106.17 (17)	N5—C33—H33B	109.5
C27—O1—H1	108 (4)	N5—C33—H33C	109.5
H21A—O21—H21B	105 (4)	H33A—C33—H33B	109.5
H21A—O21B—H21B	105 (5)	H33A—C33—H33C	109.5
H22A—O22—H22B	112 (3)	H33B—C33—H33C	109.5
H25A—O25—H25B	110 (4)	C35—C34—C15	119.7 (3)
H26A—O26—H26B	105 (3)	C38—C34—C15	122.1 (3)
C1—N1—H1A	125.8	C38—C34—C35	118.2 (3)
C4—N1—H1A	125.8	C34—C35—H35	120.0
C4—N1—C1	108.4 (2)	C36—C35—C34	119.9 (3)
C6—N2—H2	126.7	C36—C35—H35	120.0
C6—N2—C9	106.5 (2)	N6—C36—C35	120.4 (3)
C9—N2—H2	126.7	N6—C36—H36	119.8
C11—N3—H3	125.8	C35—C36—H36	119.8
C14—N3—H3	125.8	N6—C37—H37	119.6
C14—N3—C11	108.5 (2)	N6—C37—C38	120.8 (3)
C16—N4—H4	126.8	C38—C37—H37	119.6
C16—N4—C19	106.4 (2)	C34—C38—H38	120.2
C19—N4—H4	126.8	C37—C38—C34	119.7 (3)
C30—N5—C31	121.0 (3)	C37—C38—H38	120.2
C30—N5—C33	120.1 (4)	N6—C39—H39A	109.5
C31—N5—C33	118.9 (4)	N6—C39—H39B	109.5
C36—N6—C39	118.6 (3)	N6—C39—H39C	109.5
C37—N6—C36	120.9 (3)	H39A—C39—H39B	109.5
C37—N6—C39	120.4 (3)	H39A—C39—H39C	109.5
C42—N7—C43	121.2 (3)	H39B—C39—H39C	109.5
C42—N7—C45	118.9 (4)	C41—C40—C20	121.9 (3)
C43—N7—C45	119.8 (4)	C44—C40—C20	120.4 (3)
N1—C1—C2	108.2 (2)	C44—C40—C41	117.7 (3)
N1—C1—C20	125.3 (2)	C40—C41—H41	119.9
C20—C1—C2	126.5 (3)	C42—C41—C40	120.2 (3)
C1—C2—H2A	126.2	C42—C41—H41	119.9
C3—C2—C1	107.6 (2)	N7—C42—C41	120.0 (3)
C3—C2—H2A	126.2	N7—C42—H42	120.0
C2—C3—H3A	126.0	C41—C42—H42	120.0
C2—C3—C4	107.9 (2)	N7—C43—H43	119.6
C4—C3—H3A	126.0	N7—C43—C44	120.9 (4)
N1—C4—C3	107.9 (2)	C44—C43—H43	119.6
N1—C4—C5	125.7 (2)	C40—C44—H44	120.2
C5—C4—C3	126.4 (2)	C43—C44—C40	119.7 (4)
C4—C5—C6	126.2 (2)	C43—C44—H44	120.2
C4—C5—C21	117.4 (2)	N7—C45—H45A	109.5
C6—C5—C21	116.3 (2)	N7—C45—H45B	109.5
N2—C6—C5	126.2 (2)	N7—C45—H45C	109.5
N2—C6—C7	109.8 (2)	H45A—C45—H45B	109.5
C5—C6—C7	124.0 (3)	H45A—C45—H45C	109.5
C6—C7—H7	126.4	H45B—C45—H45C	109.5
C8—C7—C6	107.1 (3)	C52—C51—S1	119.6 (2)
C8—C7—H7	126.4	C56—C51—S1	120.7 (3)
C7—C8—H8	126.5	C56—C51—C52	119.7 (3)
C7—C8—C9	106.9 (3)	C51—C52—H52	120.2
C9—C8—H8	126.5	C53—C52—C51	119.7 (3)
N2—C9—C8	109.6 (2)	C53—C52—H52	120.2
N2—C9—C10	125.5 (2)	C52—C53—H53	119.6
C10—C9—C8	124.8 (3)	C54—C53—C52	120.8 (3)
C9—C10—C28	117.0 (2)	C54—C53—H53	119.6
C11—C10—C9	125.5 (2)	C53—C54—H54	120.3
C11—C10—C28	117.5 (2)	C53—C54—C55	119.3 (3)
N3—C11—C10	125.0 (2)	C55—C54—H54	120.3
N3—C11—C12	108.0 (2)	C54—C55—H55	119.7
C10—C11—C12	127.0 (3)	C54—C55—C56	120.7 (3)
C11—C12—H12	126.2	C56—C55—H55	119.7
C13—C12—C11	107.7 (2)	C51—C56—H56	120.1
C13—C12—H12	126.2	C55—C56—C51	119.8 (3)
C12—C13—H13	126.1	C55—C56—H56	120.1
C12—C13—C14	107.7 (2)	C58—C57—S2	121.1 (4)
C14—C13—H13	126.1	C62—C57—S2	120.6 (4)
N3—C14—C13	108.1 (2)	C62—C57—C58	118.2 (5)
N3—C14—C15	126.5 (2)	C57—C58—H58	119.9
C15—C14—C13	125.4 (2)	C59—C58—C57	120.2 (6)
C14—C15—C16	126.3 (2)	C59—C58—H58	119.9
C14—C15—C34	116.2 (2)	C58—C59—H59	119.6
C16—C15—C34	117.5 (3)	C60—C59—C58	120.7 (6)
N4—C16—C15	125.4 (3)	C60—C59—H59	119.6
N4—C16—C17	109.7 (2)	C59—C60—H60	120.4
C15—C16—C17	124.8 (3)	C61—C60—C59	119.2 (6)
C16—C17—H17	126.4	C61—C60—H60	120.4
C18—C17—C16	107.3 (2)	C60—C61—H61	119.5
C18—C17—H17	126.4	C60—C61—C62	120.9 (6)
C17—C18—H18	126.6	C62—C61—H61	119.5
C17—C18—C19	106.7 (3)	C57—C62—C61	120.7 (5)
C19—C18—H18	126.6	C57—C62—H62	119.7
N4—C19—C18	109.9 (2)	C61—C62—H62	119.7
N4—C19—C20	125.9 (2)	C64—C63—S3	119.9 (3)
C20—C19—C18	124.1 (3)	C68—C63—S3	120.6 (3)
C1—C20—C19	125.7 (3)	C68—C63—C64	119.5 (4)
C1—C20—C40	118.0 (2)	C63—C64—H64	119.9
C19—C20—C40	116.4 (2)	C63—C64—C65	120.3 (4)
C22—C21—C5	119.9 (3)	C65—C64—H64	119.9
C22—C21—C26	118.8 (3)	C64—C65—H65	120.1
C26—C21—C5	121.3 (3)	C66—C65—C64	119.9 (5)
C21—C22—H22	119.6	C66—C65—H65	120.1
C21—C22—C23	120.8 (3)	C65—C66—H66	120.1
C23—C22—H22	119.6	C65—C66—C67	119.7 (4)
C22—C23—H23	119.9	C67—C66—H66	120.1
C24—C23—C22	120.1 (3)	C66—C67—H67	119.8
C24—C23—H23	119.9	C66—C67—C68	120.3 (4)
C23—C24—C27	121.2 (3)	C68—C67—H67	119.8
C25—C24—C23	119.0 (3)	C63—C68—C67	120.1 (4)
C25—C24—C27	119.7 (3)	C63—C68—H68	119.9
C24—C25—H25	119.7	C67—C68—H68	119.9
C24—C25—C26	120.7 (3)
S1—C51—C52—C53	177.9 (3)	C11—C10—C28—C32	−62.2 (4)
S1—C51—C56—C55	−178.2 (3)	C11—C12—C13—C14	0.5 (3)
S2—C57—C58—C59	−177.1 (5)	C12—C13—C14—N3	0.1 (3)
S2—C57—C62—C61	178.2 (4)	C12—C13—C14—C15	178.0 (3)
S3—C63—C64—C65	175.7 (5)	C13—C14—C15—C16	−171.5 (3)
S3—C63—C68—C67	−175.0 (3)	C13—C14—C15—C34	9.8 (4)
O11—S1—C51—C52	12.6 (4)	C14—N3—C11—C10	−179.8 (3)
O11—S1—C51—C56	−168.7 (4)	C14—N3—C11—C12	0.9 (3)
O11B—S1—C51—C52	63.1 (5)	C14—C15—C16—N4	−1.5 (5)
O11B—S1—C51—C56	−118.3 (5)	C14—C15—C16—C17	179.7 (3)
O12—S1—C51—C52	139.1 (4)	C14—C15—C34—C35	63.7 (4)
O12—S1—C51—C56	−42.2 (4)	C14—C15—C34—C38	−115.9 (3)
O12B—S1—C51—C52	179.3 (6)	C15—C16—C17—C18	179.6 (3)
O12B—S1—C51—C56	−2.0 (6)	C15—C34—C35—C36	−177.8 (3)
O13—S1—C51—C52	−102.9 (3)	C15—C34—C38—C37	176.9 (3)
O13—S1—C51—C56	75.7 (3)	C16—N4—C19—C18	−0.5 (3)
O13B—S1—C51—C52	−46.2 (4)	C16—N4—C19—C20	177.1 (3)
O13B—S1—C51—C56	132.4 (4)	C16—C15—C34—C35	−115.2 (3)
O14—S2—C57—C58	−28.2 (4)	C16—C15—C34—C38	65.2 (4)
O14—S2—C57—C62	152.4 (3)	C16—C17—C18—C19	−0.8 (4)
O15—S2—C57—C58	−146.9 (4)	C17—C18—C19—N4	0.8 (4)
O15—S2—C57—C62	33.8 (4)	C17—C18—C19—C20	−176.8 (3)
O16—S2—C57—C58	91.4 (4)	C18—C19—C20—C1	175.8 (3)
O16—S2—C57—C62	−88.0 (4)	C18—C19—C20—C40	−3.1 (4)
O17—S3—C63—C64	−64.0 (4)	C19—N4—C16—C15	−179.0 (3)
O17—S3—C63—C68	114.7 (3)	C19—N4—C16—C17	−0.1 (3)
O18—S3—C63—C64	175.6 (4)	C19—C20—C40—C41	−79.0 (4)
O18—S3—C63—C68	−5.7 (4)	C19—C20—C40—C44	98.1 (4)
O19—S3—C63—C64	55.8 (4)	C20—C1—C2—C3	−178.7 (3)
O19—S3—C63—C68	−125.5 (3)	C20—C40—C41—C42	176.5 (3)
N1—C1—C2—C3	0.3 (3)	C20—C40—C44—C43	−173.2 (5)
N1—C1—C20—C19	0.2 (5)	C21—C5—C6—N2	−173.2 (3)
N1—C1—C20—C40	179.1 (3)	C21—C5—C6—C7	4.6 (4)
N1—C4—C5—C6	−0.7 (5)	C21—C22—C23—C24	−0.3 (5)
N1—C4—C5—C21	177.5 (3)	C22—C21—C26—C25	−0.8 (6)
N2—C6—C7—C8	0.5 (4)	C22—C23—C24—C25	−0.6 (5)
N2—C9—C10—C11	−5.9 (5)	C22—C23—C24—C27	177.2 (3)
N2—C9—C10—C28	172.8 (3)	C23—C24—C25—C26	0.8 (6)
N3—C11—C12—C13	−0.9 (3)	C23—C24—C27—O1	2.1 (4)
N3—C14—C15—C16	6.0 (5)	C23—C24—C27—O2	−178.4 (3)
N3—C14—C15—C34	−172.7 (3)	C24—C25—C26—C21	−0.1 (6)
N4—C16—C17—C18	0.6 (4)	C25—C24—C27—O1	179.8 (3)
N4—C19—C20—C1	−1.4 (5)	C25—C24—C27—O2	−0.7 (5)
N4—C19—C20—C40	179.7 (3)	C26—C21—C22—C23	1.0 (5)
N5—C31—C32—C28	−0.3 (5)	C27—C24—C25—C26	−177.0 (3)
N6—C37—C38—C34	1.5 (6)	C28—C10—C11—N3	−178.7 (3)
N7—C43—C44—C40	−3.2 (9)	C28—C10—C11—C12	0.5 (4)
C1—N1—C4—C3	0.4 (3)	C28—C29—C30—N5	0.4 (5)
C1—N1—C4—C5	179.8 (3)	C29—C28—C32—C31	0.1 (5)
C1—C2—C3—C4	−0.1 (3)	C30—N5—C31—C32	0.5 (5)
C1—C20—C40—C41	102.0 (3)	C31—N5—C30—C29	−0.5 (5)
C1—C20—C40—C44	−81.0 (4)	C32—C28—C29—C30	−0.1 (5)
C2—C1—C20—C19	179.0 (3)	C33—N5—C30—C29	−179.7 (3)
C2—C1—C20—C40	−2.1 (5)	C33—N5—C31—C32	179.6 (4)
C2—C3—C4—N1	−0.2 (3)	C34—C15—C16—N4	177.3 (3)
C2—C3—C4—C5	−179.5 (3)	C34—C15—C16—C17	−1.5 (5)
C3—C4—C5—C6	178.6 (3)	C34—C35—C36—N6	0.4 (5)
C3—C4—C5—C21	−3.3 (4)	C35—C34—C38—C37	−2.7 (5)
C4—N1—C1—C2	−0.4 (3)	C36—N6—C37—C38	0.7 (6)
C4—N1—C1—C20	178.6 (3)	C37—N6—C36—C35	−1.7 (5)
C4—C5—C6—N2	5.0 (5)	C38—C34—C35—C36	1.8 (5)
C4—C5—C6—C7	−177.2 (3)	C39—N6—C36—C35	175.0 (3)
C4—C5—C21—C22	−89.5 (4)	C39—N6—C37—C38	−175.9 (4)
C4—C5—C21—C26	92.8 (4)	C40—C41—C42—N7	−3.8 (6)
C5—C6—C7—C8	−177.6 (3)	C41—C40—C44—C43	4.0 (7)
C5—C21—C22—C23	−176.7 (3)	C42—N7—C43—C44	−1.2 (9)
C5—C21—C26—C25	176.9 (3)	C43—N7—C42—C41	4.7 (7)
C6—N2—C9—C8	2.1 (3)	C44—C40—C41—C42	−0.5 (5)
C6—N2—C9—C10	−177.9 (3)	C45—N7—C42—C41	−176.9 (6)
C6—C5—C21—C22	88.8 (4)	C45—N7—C43—C44	−179.6 (7)
C6—C5—C21—C26	−88.8 (4)	C51—C52—C53—C54	−0.2 (5)
C6—C7—C8—C9	0.7 (4)	C52—C51—C56—C55	0.4 (5)
C7—C8—C9—N2	−1.8 (4)	C52—C53—C54—C55	1.4 (6)
C7—C8—C9—C10	178.2 (3)	C53—C54—C55—C56	−1.8 (6)
C8—C9—C10—C11	174.1 (3)	C54—C55—C56—C51	0.9 (6)
C8—C9—C10—C28	−7.2 (4)	C56—C51—C52—C53	−0.8 (5)
C9—N2—C6—C5	176.4 (3)	C57—C58—C59—C60	−1.7 (10)
C9—N2—C6—C7	−1.6 (3)	C58—C57—C62—C61	−1.2 (7)
C9—C10—C11—N3	0.0 (5)	C58—C59—C60—C61	−0.1 (10)
C9—C10—C11—C12	179.2 (3)	C59—C60—C61—C62	1.1 (9)
C9—C10—C28—C29	−60.8 (4)	C60—C61—C62—C57	−0.5 (8)
C9—C10—C28—C32	119.0 (3)	C62—C57—C58—C59	2.3 (8)
C10—C11—C12—C13	179.8 (3)	C63—C64—C65—C66	0.0 (10)
C10—C28—C29—C30	179.7 (3)	C64—C63—C68—C67	3.7 (7)
C10—C28—C32—C31	−179.7 (3)	C64—C65—C66—C67	2.3 (9)
C11—N3—C14—C13	−0.7 (3)	C65—C66—C67—C68	−1.6 (8)
C11—N3—C14—C15	−178.5 (3)	C66—C67—C68—C63	−1.4 (7)
C11—C10—C28—C29	118.0 (3)	C68—C63—C64—C65	−3.0 (9)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1···O21	0.80 (5)	1.73 (5)	2.506 (5)	161 (6)
O1—H1···O21B	0.80 (5)	1.88 (5)	2.669 (8)	168 (5)
O21—H21A···O13	0.88 (5)	1.87 (5)	2.746 (6)	169 (5)
O21B—H21A···O13B	0.86 (2)	1.85 (3)	2.684 (10)	162 (6)
O21—H21B···O14	0.92 (6)	1.85 (6)	2.727 (6)	157 (5)
O21B—H21B···O14	0.95 (5)	1.85 (6)	2.701 (7)	148 (5)
O22—H22A···O15^i	0.88 (2)	2.02 (3)	2.857 (6)	159 (7)
O22—H22B···O25^ii	0.87 (2)	2.07 (6)	2.795 (5)	140 (8)
O25—H25A···O19	0.88 (4)	1.95 (4)	2.809 (4)	165 (5)
O26—H26A···O15^iii	0.91 (2)	2.29 (8)	2.870 (6)	121 (7)
O26—H26B···O17	0.89 (2)	2.08 (5)	2.883 (5)	149 (7)
N1—H1A···N2	0.88	2.38	2.927 (3)	120
N1—H1A···N4	0.88	2.34	2.888 (3)	121
N3—H3···N2	0.88	2.32	2.875 (3)	121
O25—H25B···O12B^iv	0.87 (2)	1.95 (3)	2.792 (9)	162 (5)

Symmetry codes: (i) x+1/2, −y+3/2, z−1/2; (ii) x+1, y, z; (iii) −x+1/2, y+1/2, −z+3/2; (iv) x−1/2, −y+3/2, z−1/2.

(TMPyP)Br4(H2O)6

Crystal data

C44H38N8·4(Br)·5(H2O)·HO	Z = 2
Mr = 1106.56	F(000) = 1116
Triclinic, P1	Dx = 1.597 Mg m^−3
a = 10.15908 (14) Å	Cu Kα radiation, λ = 1.54184 Å
b = 14.97284 (18) Å	Cell parameters from 23732 reflections
c = 15.76491 (13) Å	θ = 2.9–78.5°
α = 81.1416 (8)°	µ = 4.73 mm^−1
β = 76.1519 (9)°	T = 160 K
γ = 88.1501 (11)°	Needle, red
V = 2300.51 (5) Å^3	0.15 × 0.06 × 0.04 mm

Data collection

XtaLAB Synergy, Dualflex, HyPix diffractometer	9864 independent reflections
Radiation source: micro-focus sealed X-ray tube, PhotonJet (Cu) X-ray Source	8634 reflections with I > 2σ(I)
Mirror monochromator	Rint = 0.035
Detector resolution: 10.0000 pixels mm^-1	θmax = 79.2°, θmin = 2.9°
ω scans	h = −12→12
Absorption correction: analytical CrysAlisPro 1.171.43.130a (Rigaku Oxford Diffraction, 2024) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	k = −18→19
Tmin = 0.624, Tmax = 0.852	l = −13→19
45971 measured reflections

Refinement

Refinement on F^2	Primary atom site location: dual
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.038	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.110	w = 1/[σ^2(Fo^2) + (0.0603P)^2 + 1.9207P] where P = (Fo^2 + 2Fc^2)/3
S = 1.09	(Δ/σ)max = 0.001
9864 reflections	Δρmax = 0.70 e Å^−3
590 parameters	Δρmin = −0.66 e Å^−3
4 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	Occ. (<1)
N1	0.6248 (2)	0.39307 (13)	0.55419 (13)	0.0244 (4)
H1	0.682901	0.437994	0.533096	0.029*	0.5
N2	0.7912 (2)	0.49877 (13)	0.63171 (13)	0.0227 (4)
H2	0.786781	0.494895	0.577335	0.027*	0.5
N3	0.8859 (2)	0.60714 (13)	0.46070 (13)	0.0236 (4)
H3	0.825019	0.563963	0.482420	0.028*	0.5
N4	0.7179 (2)	0.50311 (13)	0.38260 (13)	0.0232 (4)
H4	0.727196	0.504471	0.436467	0.028*	0.5
N5	0.3956 (2)	0.17388 (14)	0.30645 (13)	0.0248 (4)
N6	0.5161 (2)	0.18784 (15)	0.94852 (14)	0.0289 (4)
N7	1.1205 (2)	0.82633 (14)	0.70703 (13)	0.0256 (4)
N8	1.0295 (2)	0.81096 (15)	0.06941 (14)	0.0302 (5)
C1	0.5536 (3)	0.35247 (16)	0.50668 (15)	0.0243 (5)
C2	0.4655 (3)	0.28484 (17)	0.56662 (16)	0.0271 (5)
H2A	0.402953	0.247774	0.551674	0.033*
C3	0.4880 (3)	0.28364 (17)	0.64800 (16)	0.0278 (5)
H3A	0.444883	0.245261	0.700456	0.033*
C4	0.5896 (3)	0.35143 (16)	0.64028 (15)	0.0245 (5)
C5	0.6395 (3)	0.37217 (16)	0.71040 (15)	0.0251 (5)
C6	0.7269 (3)	0.44376 (16)	0.70714 (15)	0.0232 (4)
C7	0.7599 (3)	0.47231 (17)	0.78308 (16)	0.0269 (5)
H7	0.729604	0.444938	0.842915	0.032*
C8	0.8423 (3)	0.54561 (17)	0.75275 (15)	0.0254 (5)
H8	0.878939	0.580256	0.787370	0.031*
C9	0.8637 (3)	0.56093 (16)	0.65743 (15)	0.0229 (4)
C10	0.9423 (2)	0.63086 (15)	0.59962 (15)	0.0228 (4)
C11	0.9578 (2)	0.64717 (16)	0.50773 (15)	0.0233 (4)
C12	1.0518 (3)	0.71106 (16)	0.44724 (16)	0.0257 (5)
H12	1.115963	0.747089	0.461895	0.031*
C13	1.0315 (3)	0.71005 (16)	0.36583 (16)	0.0258 (5)
H13	1.079083	0.745483	0.312708	0.031*
C14	0.9252 (3)	0.64598 (16)	0.37354 (15)	0.0238 (4)
C15	0.8727 (3)	0.62735 (16)	0.30343 (15)	0.0237 (4)
C16	0.7791 (3)	0.55985 (16)	0.30770 (15)	0.0234 (4)
C17	0.7348 (3)	0.53681 (16)	0.23307 (16)	0.0256 (5)
H17	0.759773	0.566962	0.173908	0.031*
C18	0.6508 (3)	0.46413 (17)	0.26321 (15)	0.0255 (5)
H18	0.607885	0.432695	0.229156	0.031*
C19	0.6395 (3)	0.44394 (15)	0.35789 (15)	0.0233 (4)
C20	0.5653 (2)	0.37196 (16)	0.41542 (15)	0.0233 (4)
C21	0.5972 (3)	0.30969 (17)	0.79555 (16)	0.0256 (5)
C22	0.6436 (3)	0.22040 (17)	0.80091 (17)	0.0300 (5)
H22	0.703740	0.200769	0.751267	0.036*
C23	0.6022 (3)	0.16129 (18)	0.87786 (18)	0.0310 (5)
H23	0.634591	0.100930	0.881325	0.037*
C24	0.4705 (3)	0.27325 (18)	0.94578 (16)	0.0290 (5)
H24	0.410526	0.290963	0.996487	0.035*
C25	0.5098 (3)	0.33539 (18)	0.87028 (16)	0.0283 (5)
H25	0.477355	0.395680	0.869158	0.034*
C26	0.4673 (3)	0.12111 (19)	1.02809 (18)	0.0373 (6)
H26A	0.419567	0.152292	1.076801	0.056*
H26B	0.544629	0.088072	1.044434	0.056*
H26C	0.405280	0.078538	1.016033	0.056*
C27	1.0064 (2)	0.69788 (16)	0.63790 (15)	0.0233 (4)
C28	1.0890 (3)	0.67328 (16)	0.69641 (15)	0.0243 (5)
H28	1.107493	0.611274	0.712882	0.029*
C29	1.1442 (3)	0.73869 (17)	0.73063 (16)	0.0269 (5)
H29	1.199338	0.721335	0.771231	0.032*
C30	1.0405 (3)	0.85266 (16)	0.65125 (16)	0.0269 (5)
H30	1.024182	0.915191	0.635852	0.032*
C31	0.9820 (3)	0.78994 (16)	0.61613 (16)	0.0262 (5)
H31	0.925039	0.809262	0.577089	0.031*
C32	1.1764 (3)	0.89593 (18)	0.74619 (17)	0.0310 (5)
H32A	1.217721	0.944710	0.699354	0.047*
H32B	1.245203	0.868605	0.776222	0.047*
H32C	1.103248	0.920505	0.788919	0.047*
C33	0.9221 (3)	0.68919 (16)	0.21825 (15)	0.0244 (5)
C34	0.9964 (3)	0.65956 (17)	0.14137 (16)	0.0280 (5)
H34	1.010644	0.596777	0.139660	0.034*
C35	1.0495 (3)	0.72200 (18)	0.06744 (16)	0.0312 (5)
H35	1.100404	0.701857	0.015047	0.037*
C36	0.9531 (3)	0.84111 (18)	0.14104 (18)	0.0335 (6)
H36	0.936442	0.904036	0.139899	0.040*
C37	0.8984 (3)	0.78170 (17)	0.21635 (17)	0.0309 (5)
H37	0.844712	0.803720	0.266896	0.037*
C38	1.0912 (4)	0.8776 (2)	−0.00865 (18)	0.0391 (6)
H38A	1.168629	0.850083	−0.045512	0.059*
H38B	1.122006	0.930552	0.010988	0.059*
H38C	1.023734	0.896239	−0.043040	0.059*
C39	0.5034 (2)	0.30438 (16)	0.37622 (15)	0.0235 (4)
C40	0.4150 (3)	0.32727 (16)	0.32116 (16)	0.0261 (5)
H40	0.389934	0.388569	0.307871	0.031*
C41	0.3638 (3)	0.26095 (17)	0.28578 (16)	0.0275 (5)
H41	0.305806	0.277037	0.246722	0.033*
C42	0.4804 (3)	0.14922 (16)	0.35910 (16)	0.0269 (5)
H42	0.501923	0.087215	0.372351	0.032*
C43	0.5366 (3)	0.21323 (16)	0.39414 (16)	0.0261 (5)
H43	0.597939	0.195368	0.430533	0.031*
C44	0.3377 (3)	0.10242 (18)	0.27048 (18)	0.0345 (6)
H44A	0.411241	0.066175	0.240472	0.052*
H44B	0.286078	0.130452	0.228276	0.052*
H44C	0.277476	0.063413	0.318913	0.052*
Br1	0.35968 (3)	0.71925 (2)	0.88652 (2)	0.03654 (9)
Br4	0.79636 (3)	−0.08879 (2)	0.45769 (2)	0.04446 (10)
Br2	0.85815 (3)	0.75992 (2)	0.88759 (2)	0.04015 (9)
Br3	0.65164 (3)	−0.04655 (2)	0.16073 (2)	0.04107 (9)
O1	0.1012 (7)	0.4625 (3)	1.0401 (4)	0.1132 (17)
H1A	0.042429	0.418849	1.061207	0.170*
H1B	0.171721	0.437023	1.010341	0.170*
O2	0.3799 (6)	0.5085 (2)	0.9673 (3)	0.1050 (16)
H2B	0.383 (9)	0.5660 (16)	0.952 (6)	0.157*
O4	0.1096 (3)	−0.07262 (17)	0.32419 (17)	0.0494 (6)
H4A	0.032 (6)	−0.077 (4)	0.355 (4)	0.074*
H4B	0.156 (5)	−0.083 (4)	0.363 (3)	0.074*
O6	0.2667 (3)	−0.10383 (19)	0.45203 (18)	0.0512 (6)
H6A	0.349 (2)	−0.103 (4)	0.428 (3)	0.077*
H6B	0.264 (6)	−0.067 (4)	0.483 (4)	0.077*
O3	0.1578 (3)	0.00567 (18)	0.14507 (16)	0.0468 (5)
H3B	0.154 (5)	0.0617 (14)	0.134 (3)	0.070*
H3C	0.145 (6)	−0.024 (4)	0.186 (3)	0.070*
O5	0.5319 (2)	−0.06126 (14)	0.37185 (15)	0.0406 (5)
H5A	0.563086	−0.060369	0.315312	0.061*
H5B	0.602807	−0.071871	0.393852	0.061*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
N1	0.0312 (11)	0.0214 (9)	0.0207 (9)	−0.0079 (8)	−0.0048 (8)	−0.0045 (7)
N2	0.0296 (10)	0.0198 (9)	0.0184 (9)	−0.0068 (8)	−0.0039 (7)	−0.0037 (7)
N3	0.0315 (11)	0.0212 (9)	0.0183 (9)	−0.0065 (8)	−0.0049 (8)	−0.0035 (7)
N4	0.0296 (10)	0.0197 (9)	0.0203 (9)	−0.0060 (8)	−0.0047 (7)	−0.0035 (7)
N5	0.0319 (11)	0.0211 (9)	0.0214 (9)	−0.0068 (8)	−0.0041 (8)	−0.0053 (7)
N6	0.0387 (12)	0.0267 (10)	0.0212 (10)	−0.0088 (9)	−0.0077 (8)	−0.0002 (8)
N7	0.0314 (11)	0.0218 (9)	0.0240 (9)	−0.0076 (8)	−0.0050 (8)	−0.0059 (7)
N8	0.0412 (13)	0.0245 (10)	0.0223 (10)	−0.0066 (9)	−0.0053 (9)	0.0024 (8)
C1	0.0290 (12)	0.0209 (10)	0.0230 (11)	−0.0055 (9)	−0.0045 (9)	−0.0049 (8)
C2	0.0328 (13)	0.0247 (11)	0.0226 (11)	−0.0105 (10)	−0.0018 (9)	−0.0050 (9)
C3	0.0336 (13)	0.0257 (11)	0.0224 (11)	−0.0118 (10)	−0.0014 (9)	−0.0039 (9)
C4	0.0305 (12)	0.0201 (10)	0.0214 (11)	−0.0075 (9)	−0.0016 (9)	−0.0041 (8)
C5	0.0322 (13)	0.0225 (11)	0.0194 (10)	−0.0043 (9)	−0.0036 (9)	−0.0027 (8)
C6	0.0307 (12)	0.0198 (10)	0.0188 (10)	−0.0030 (9)	−0.0051 (9)	−0.0027 (8)
C7	0.0345 (13)	0.0264 (11)	0.0197 (11)	−0.0066 (10)	−0.0074 (9)	−0.0002 (9)
C8	0.0311 (12)	0.0255 (11)	0.0209 (11)	−0.0051 (9)	−0.0089 (9)	−0.0016 (9)
C9	0.0284 (12)	0.0199 (10)	0.0207 (11)	−0.0034 (9)	−0.0047 (9)	−0.0045 (8)
C10	0.0265 (12)	0.0194 (10)	0.0231 (11)	−0.0023 (8)	−0.0059 (9)	−0.0046 (8)
C11	0.0280 (12)	0.0200 (10)	0.0214 (11)	−0.0056 (9)	−0.0035 (9)	−0.0041 (8)
C12	0.0292 (12)	0.0230 (11)	0.0234 (11)	−0.0075 (9)	−0.0015 (9)	−0.0044 (9)
C13	0.0312 (13)	0.0218 (11)	0.0232 (11)	−0.0077 (9)	−0.0034 (9)	−0.0030 (8)
C14	0.0305 (12)	0.0200 (10)	0.0196 (10)	−0.0062 (9)	−0.0027 (9)	−0.0027 (8)
C15	0.0305 (12)	0.0206 (10)	0.0196 (10)	−0.0033 (9)	−0.0042 (9)	−0.0034 (8)
C16	0.0295 (12)	0.0200 (10)	0.0209 (10)	−0.0022 (9)	−0.0067 (9)	−0.0025 (8)
C17	0.0316 (13)	0.0229 (11)	0.0231 (11)	−0.0038 (9)	−0.0083 (9)	−0.0021 (9)
C18	0.0319 (13)	0.0253 (11)	0.0210 (11)	−0.0045 (9)	−0.0088 (9)	−0.0035 (9)
C19	0.0301 (12)	0.0187 (10)	0.0219 (11)	−0.0014 (9)	−0.0068 (9)	−0.0040 (8)
C20	0.0271 (12)	0.0208 (10)	0.0225 (11)	−0.0033 (9)	−0.0047 (9)	−0.0062 (8)
C21	0.0306 (12)	0.0239 (11)	0.0221 (11)	−0.0081 (9)	−0.0059 (9)	−0.0017 (9)
C22	0.0348 (14)	0.0235 (11)	0.0280 (12)	−0.0060 (10)	0.0003 (10)	−0.0037 (9)
C23	0.0370 (14)	0.0228 (11)	0.0312 (13)	−0.0037 (10)	−0.0055 (10)	−0.0017 (9)
C24	0.0360 (14)	0.0294 (12)	0.0199 (11)	−0.0046 (10)	−0.0027 (9)	−0.0036 (9)
C25	0.0347 (13)	0.0265 (12)	0.0234 (11)	−0.0026 (10)	−0.0059 (10)	−0.0041 (9)
C26	0.0516 (17)	0.0307 (13)	0.0254 (12)	−0.0080 (12)	−0.0055 (11)	0.0044 (10)
C27	0.0260 (11)	0.0236 (11)	0.0202 (10)	−0.0047 (9)	−0.0035 (8)	−0.0049 (8)
C28	0.0285 (12)	0.0208 (10)	0.0240 (11)	−0.0027 (9)	−0.0061 (9)	−0.0042 (8)
C29	0.0310 (13)	0.0268 (12)	0.0241 (11)	−0.0037 (9)	−0.0082 (9)	−0.0043 (9)
C30	0.0379 (14)	0.0198 (11)	0.0230 (11)	−0.0052 (9)	−0.0070 (9)	−0.0023 (8)
C31	0.0351 (13)	0.0227 (11)	0.0220 (11)	−0.0033 (9)	−0.0097 (9)	−0.0021 (8)
C32	0.0408 (15)	0.0271 (12)	0.0284 (12)	−0.0101 (10)	−0.0105 (10)	−0.0081 (10)
C33	0.0303 (12)	0.0220 (11)	0.0213 (11)	−0.0048 (9)	−0.0072 (9)	−0.0014 (8)
C34	0.0400 (14)	0.0224 (11)	0.0219 (11)	−0.0031 (10)	−0.0083 (10)	−0.0021 (9)
C35	0.0428 (15)	0.0291 (12)	0.0199 (11)	−0.0042 (11)	−0.0037 (10)	−0.0030 (9)
C36	0.0426 (15)	0.0240 (12)	0.0298 (13)	−0.0026 (10)	−0.0028 (11)	−0.0002 (10)
C37	0.0388 (14)	0.0239 (12)	0.0264 (12)	−0.0014 (10)	−0.0007 (10)	−0.0038 (9)
C38	0.0552 (18)	0.0313 (14)	0.0235 (12)	−0.0078 (12)	−0.0013 (12)	0.0071 (10)
C39	0.0276 (12)	0.0211 (11)	0.0211 (10)	−0.0060 (9)	−0.0035 (9)	−0.0038 (8)
C40	0.0291 (12)	0.0208 (11)	0.0283 (12)	−0.0028 (9)	−0.0062 (9)	−0.0042 (9)
C41	0.0297 (12)	0.0272 (12)	0.0270 (12)	−0.0056 (9)	−0.0081 (9)	−0.0052 (9)
C42	0.0353 (13)	0.0203 (11)	0.0248 (11)	−0.0040 (9)	−0.0058 (9)	−0.0040 (9)
C43	0.0333 (13)	0.0230 (11)	0.0224 (11)	−0.0035 (9)	−0.0074 (9)	−0.0031 (9)
C44	0.0482 (16)	0.0275 (12)	0.0323 (13)	−0.0090 (11)	−0.0145 (12)	−0.0087 (10)
Br1	0.04255 (17)	0.03953 (16)	0.02976 (15)	−0.00152 (12)	−0.01157 (12)	−0.00701 (11)
Br4	0.04078 (18)	0.0533 (2)	0.03576 (16)	0.00008 (14)	−0.01001 (13)	0.00575 (13)
Br2	0.04020 (17)	0.04306 (17)	0.03410 (16)	−0.00398 (12)	−0.00353 (12)	−0.00381 (12)
Br3	0.04608 (19)	0.03864 (16)	0.04304 (17)	−0.00279 (13)	−0.01875 (14)	−0.00664 (12)
O1	0.197 (5)	0.058 (2)	0.112 (3)	0.009 (3)	−0.095 (4)	−0.006 (2)
O2	0.190 (5)	0.0543 (19)	0.071 (2)	0.035 (3)	−0.035 (3)	−0.0112 (17)
O4	0.0548 (15)	0.0403 (12)	0.0476 (13)	−0.0141 (11)	−0.0050 (11)	0.0023 (10)
O6	0.0428 (13)	0.0503 (14)	0.0548 (15)	−0.0066 (11)	−0.0047 (11)	0.0006 (11)
O3	0.0574 (15)	0.0442 (13)	0.0410 (12)	−0.0118 (11)	−0.0122 (11)	−0.0101 (10)
O5	0.0419 (12)	0.0305 (10)	0.0484 (12)	−0.0022 (9)	−0.0108 (9)	−0.0019 (9)

Geometric parameters (Å, º)

N1—H1	0.8800	C21—C22	1.400 (4)
N1—C1	1.372 (3)	C21—C25	1.393 (4)
N1—C4	1.371 (3)	C22—H22	0.9500
N2—H2	0.8800	C22—C23	1.372 (4)
N2—C6	1.371 (3)	C23—H23	0.9500
N2—C9	1.370 (3)	C24—H24	0.9500
N3—H3	0.8800	C24—C25	1.377 (3)
N3—C11	1.366 (3)	C25—H25	0.9500
N3—C14	1.375 (3)	C26—H26A	0.9800
N4—H4	0.8800	C26—H26B	0.9800
N4—C16	1.370 (3)	C26—H26C	0.9800
N4—C19	1.368 (3)	C27—C28	1.391 (3)
N5—C41	1.343 (3)	C27—C31	1.397 (3)
N5—C42	1.340 (3)	C28—H28	0.9500
N5—C44	1.483 (3)	C28—C29	1.381 (3)
N6—C23	1.346 (4)	C29—H29	0.9500
N6—C24	1.344 (4)	C30—H30	0.9500
N6—C26	1.472 (3)	C30—C31	1.377 (3)
N7—C29	1.338 (3)	C31—H31	0.9500
N7—C30	1.343 (3)	C32—H32A	0.9800
N7—C32	1.481 (3)	C32—H32B	0.9800
N8—C35	1.345 (4)	C32—H32C	0.9800
N8—C36	1.340 (4)	C33—C34	1.393 (4)
N8—C38	1.482 (3)	C33—C37	1.395 (3)
C1—C2	1.441 (3)	C34—H34	0.9500
C1—C20	1.400 (3)	C34—C35	1.385 (3)
C2—H2A	0.9500	C35—H35	0.9500
C2—C3	1.353 (4)	C36—H36	0.9500
C3—H3A	0.9500	C36—C37	1.379 (4)
C3—C4	1.442 (3)	C37—H37	0.9500
C4—C5	1.400 (3)	C38—H38A	0.9800
C5—C6	1.401 (3)	C38—H38B	0.9800
C5—C21	1.492 (3)	C38—H38C	0.9800
C6—C7	1.445 (3)	C39—C40	1.392 (3)
C7—H7	0.9500	C39—C43	1.398 (3)
C7—C8	1.357 (3)	C40—H40	0.9500
C8—H8	0.9500	C40—C41	1.383 (3)
C8—C9	1.449 (3)	C41—H41	0.9500
C9—C10	1.406 (3)	C42—H42	0.9500
C10—C11	1.403 (3)	C42—C43	1.378 (3)
C10—C27	1.487 (3)	C43—H43	0.9500
C11—C12	1.442 (3)	C44—H44A	0.9800
C12—H12	0.9500	C44—H44B	0.9800
C12—C13	1.350 (4)	C44—H44C	0.9800
C13—H13	0.9500	O1—H1A	0.8705
C13—C14	1.438 (3)	O1—H1B	0.8698
C14—C15	1.404 (3)	O2—H2B	0.86 (2)
C15—C16	1.393 (3)	O4—H4A	0.82 (6)
C15—C33	1.496 (3)	O4—H4B	0.849 (19)
C16—C17	1.448 (3)	O6—H6A	0.83 (2)
C17—H17	0.9500	O6—H6B	0.79 (6)
C17—C18	1.358 (3)	O3—H3B	0.832 (19)
C18—H18	0.9500	O3—H3C	0.71 (5)
C18—C19	1.454 (3)	O5—H5A	0.8697
C19—C20	1.406 (3)	O5—H5B	0.8712
C20—C39	1.490 (3)
C1—N1—H1	126.0	C21—C22—H22	120.0
C4—N1—H1	126.0	C23—C22—C21	120.0 (2)
C4—N1—C1	108.06 (19)	C23—C22—H22	120.0
C6—N2—H2	126.7	N6—C23—C22	120.7 (2)
C9—N2—H2	126.7	N6—C23—H23	119.6
C9—N2—C6	106.70 (18)	C22—C23—H23	119.6
C11—N3—H3	125.9	N6—C24—H24	119.6
C11—N3—C14	108.22 (19)	N6—C24—C25	120.7 (2)
C14—N3—H3	125.9	C25—C24—H24	119.6
C16—N4—H4	126.5	C21—C25—H25	120.1
C19—N4—H4	126.5	C24—C25—C21	119.9 (2)
C19—N4—C16	107.09 (19)	C24—C25—H25	120.1
C41—N5—C44	120.3 (2)	N6—C26—H26A	109.5
C42—N5—C41	121.4 (2)	N6—C26—H26B	109.5
C42—N5—C44	118.3 (2)	N6—C26—H26C	109.5
C23—N6—C26	119.2 (2)	H26A—C26—H26B	109.5
C24—N6—C23	120.8 (2)	H26A—C26—H26C	109.5
C24—N6—C26	120.0 (2)	H26B—C26—H26C	109.5
C29—N7—C30	121.0 (2)	C28—C27—C10	123.0 (2)
C29—N7—C32	120.2 (2)	C28—C27—C31	117.6 (2)
C30—N7—C32	118.8 (2)	C31—C27—C10	119.4 (2)
C35—N8—C38	120.1 (2)	C27—C28—H28	119.9
C36—N8—C35	121.1 (2)	C29—C28—C27	120.2 (2)
C36—N8—C38	118.8 (2)	C29—C28—H28	119.9
N1—C1—C2	108.3 (2)	N7—C29—C28	120.5 (2)
N1—C1—C20	126.2 (2)	N7—C29—H29	119.8
C20—C1—C2	125.5 (2)	C28—C29—H29	119.8
C1—C2—H2A	126.1	N7—C30—H30	119.7
C3—C2—C1	107.7 (2)	N7—C30—C31	120.7 (2)
C3—C2—H2A	126.1	C31—C30—H30	119.7
C2—C3—H3A	126.4	C27—C31—H31	120.0
C2—C3—C4	107.3 (2)	C30—C31—C27	120.0 (2)
C4—C3—H3A	126.4	C30—C31—H31	120.0
N1—C4—C3	108.6 (2)	N7—C32—H32A	109.5
N1—C4—C5	126.4 (2)	N7—C32—H32B	109.5
C5—C4—C3	125.0 (2)	N7—C32—H32C	109.5
C4—C5—C6	126.3 (2)	H32A—C32—H32B	109.5
C4—C5—C21	115.8 (2)	H32A—C32—H32C	109.5
C6—C5—C21	117.8 (2)	H32B—C32—H32C	109.5
N2—C6—C5	125.2 (2)	C34—C33—C15	123.2 (2)
N2—C6—C7	109.7 (2)	C34—C33—C37	118.1 (2)
C5—C6—C7	125.1 (2)	C37—C33—C15	118.6 (2)
C6—C7—H7	126.5	C33—C34—H34	120.1
C8—C7—C6	107.0 (2)	C35—C34—C33	119.8 (2)
C8—C7—H7	126.5	C35—C34—H34	120.1
C7—C8—H8	126.6	N8—C35—C34	120.4 (2)
C7—C8—C9	106.8 (2)	N8—C35—H35	119.8
C9—C8—H8	126.6	C34—C35—H35	119.8
N2—C9—C8	109.7 (2)	N8—C36—H36	119.7
N2—C9—C10	124.6 (2)	N8—C36—C37	120.6 (2)
C10—C9—C8	125.7 (2)	C37—C36—H36	119.7
C9—C10—C27	118.5 (2)	C33—C37—H37	120.0
C11—C10—C9	125.1 (2)	C36—C37—C33	119.9 (2)
C11—C10—C27	116.2 (2)	C36—C37—H37	120.0
N3—C11—C10	126.3 (2)	N8—C38—H38A	109.5
N3—C11—C12	108.6 (2)	N8—C38—H38B	109.5
C10—C11—C12	125.0 (2)	N8—C38—H38C	109.5
C11—C12—H12	126.4	H38A—C38—H38B	109.5
C13—C12—C11	107.1 (2)	H38A—C38—H38C	109.5
C13—C12—H12	126.4	H38B—C38—H38C	109.5
C12—C13—H13	126.0	C40—C39—C20	123.4 (2)
C12—C13—C14	108.1 (2)	C40—C39—C43	117.7 (2)
C14—C13—H13	126.0	C43—C39—C20	118.9 (2)
N3—C14—C13	107.9 (2)	C39—C40—H40	119.9
N3—C14—C15	126.9 (2)	C41—C40—C39	120.1 (2)
C15—C14—C13	125.2 (2)	C41—C40—H40	119.9
C14—C15—C33	114.7 (2)	N5—C41—C40	120.2 (2)
C16—C15—C14	126.1 (2)	N5—C41—H41	119.9
C16—C15—C33	119.2 (2)	C40—C41—H41	119.9
N4—C16—C15	125.4 (2)	N5—C42—H42	119.8
N4—C16—C17	109.4 (2)	N5—C42—C43	120.4 (2)
C15—C16—C17	125.2 (2)	C43—C42—H42	119.8
C16—C17—H17	126.3	C39—C43—H43	120.0
C18—C17—C16	107.4 (2)	C42—C43—C39	120.1 (2)
C18—C17—H17	126.3	C42—C43—H43	120.0
C17—C18—H18	126.8	N5—C44—H44A	109.5
C17—C18—C19	106.4 (2)	N5—C44—H44B	109.5
C19—C18—H18	126.8	N5—C44—H44C	109.5
N4—C19—C18	109.7 (2)	H44A—C44—H44B	109.5
N4—C19—C20	124.5 (2)	H44A—C44—H44C	109.5
C20—C19—C18	125.7 (2)	H44B—C44—H44C	109.5
C1—C20—C19	125.9 (2)	H1A—O1—H1B	104.5
C1—C20—C39	115.7 (2)	H4A—O4—H4B	102 (5)
C19—C20—C39	118.1 (2)	H6A—O6—H6B	100 (5)
C22—C21—C5	119.2 (2)	H3B—O3—H3C	131 (5)
C25—C21—C5	122.9 (2)	H5A—O5—H5B	104.5
C25—C21—C22	117.9 (2)
N1—C1—C2—C3	−2.0 (3)	C12—C13—C14—C15	178.4 (2)
N1—C1—C20—C19	−8.4 (4)	C13—C14—C15—C16	173.5 (2)
N1—C1—C20—C39	165.5 (2)	C13—C14—C15—C33	−8.2 (4)
N1—C4—C5—C6	5.2 (4)	C14—N3—C11—C10	175.9 (2)
N1—C4—C5—C21	−173.1 (2)	C14—N3—C11—C12	−3.0 (3)
N2—C6—C7—C8	1.0 (3)	C14—C15—C16—N4	3.3 (4)
N2—C9—C10—C11	0.1 (4)	C14—C15—C16—C17	−174.5 (2)
N2—C9—C10—C27	175.0 (2)	C14—C15—C33—C34	117.9 (3)
N3—C11—C12—C13	1.9 (3)	C14—C15—C33—C37	−59.0 (3)
N3—C14—C15—C16	−6.3 (4)	C15—C16—C17—C18	176.0 (2)
N3—C14—C15—C33	172.0 (2)	C15—C33—C34—C35	−173.9 (2)
N4—C16—C17—C18	−2.2 (3)	C15—C33—C37—C36	174.3 (3)
N4—C19—C20—C1	3.8 (4)	C16—N4—C19—C18	−0.3 (3)
N4—C19—C20—C39	−170.0 (2)	C16—N4—C19—C20	176.7 (2)
N5—C42—C43—C39	1.2 (4)	C16—C15—C33—C34	−63.7 (3)
N6—C24—C25—C21	0.3 (4)	C16—C15—C33—C37	119.4 (3)
N7—C30—C31—C27	−0.5 (4)	C16—C17—C18—C19	1.9 (3)
N8—C36—C37—C33	−0.3 (4)	C17—C18—C19—N4	−1.1 (3)
C1—N1—C4—C3	−2.1 (3)	C17—C18—C19—C20	−178.0 (2)
C1—N1—C4—C5	179.7 (2)	C18—C19—C20—C1	−179.7 (2)
C1—C2—C3—C4	0.7 (3)	C18—C19—C20—C39	6.5 (4)
C1—C20—C39—C40	129.8 (3)	C19—N4—C16—C15	−176.7 (2)
C1—C20—C39—C43	−51.1 (3)	C19—N4—C16—C17	1.5 (3)
C2—C1—C20—C19	172.7 (3)	C19—C20—C39—C40	−55.8 (3)
C2—C1—C20—C39	−13.4 (4)	C19—C20—C39—C43	123.3 (3)
C2—C3—C4—N1	0.9 (3)	C20—C1—C2—C3	177.1 (3)
C2—C3—C4—C5	179.1 (3)	C20—C39—C40—C41	178.7 (2)
C3—C4—C5—C6	−172.7 (3)	C20—C39—C43—C42	179.7 (2)
C3—C4—C5—C21	9.0 (4)	C21—C5—C6—N2	169.8 (2)
C4—N1—C1—C2	2.5 (3)	C21—C5—C6—C7	−12.1 (4)
C4—N1—C1—C20	−176.6 (2)	C21—C22—C23—N6	0.6 (4)
C4—C5—C6—N2	−8.5 (4)	C22—C21—C25—C24	−0.8 (4)
C4—C5—C6—C7	169.7 (3)	C23—N6—C24—C25	0.6 (4)
C4—C5—C21—C22	66.9 (3)	C24—N6—C23—C22	−1.1 (4)
C4—C5—C21—C25	−111.4 (3)	C25—C21—C22—C23	0.4 (4)
C5—C6—C7—C8	−177.4 (2)	C26—N6—C23—C22	176.3 (3)
C5—C21—C22—C23	−177.9 (2)	C26—N6—C24—C25	−176.7 (3)
C5—C21—C25—C24	177.4 (2)	C27—C10—C11—N3	−165.3 (2)
C6—N2—C9—C8	−1.1 (3)	C27—C10—C11—C12	13.5 (4)
C6—N2—C9—C10	−178.8 (2)	C27—C28—C29—N7	−0.9 (4)
C6—C5—C21—C22	−111.6 (3)	C28—C27—C31—C30	1.0 (4)
C6—C5—C21—C25	70.2 (3)	C29—N7—C30—C31	−0.7 (4)
C6—C7—C8—C9	−1.7 (3)	C30—N7—C29—C28	1.4 (4)
C7—C8—C9—N2	1.8 (3)	C31—C27—C28—C29	−0.3 (4)
C7—C8—C9—C10	179.5 (2)	C32—N7—C29—C28	178.0 (2)
C8—C9—C10—C11	−177.3 (2)	C32—N7—C30—C31	−177.4 (2)
C8—C9—C10—C27	−2.3 (4)	C33—C15—C16—N4	−174.9 (2)
C9—N2—C6—C5	178.5 (2)	C33—C15—C16—C17	7.3 (4)
C9—N2—C6—C7	0.1 (3)	C33—C34—C35—N8	−0.2 (4)
C9—C10—C11—N3	9.8 (4)	C34—C33—C37—C36	−2.8 (4)
C9—C10—C11—C12	−171.5 (2)	C35—N8—C36—C37	3.2 (4)
C9—C10—C27—C28	53.8 (3)	C36—N8—C35—C34	−3.0 (4)
C9—C10—C27—C31	−125.1 (3)	C37—C33—C34—C35	3.0 (4)
C10—C11—C12—C13	−177.1 (2)	C38—N8—C35—C34	177.5 (3)
C10—C27—C28—C29	−179.1 (2)	C38—N8—C36—C37	−177.3 (3)
C10—C27—C31—C30	179.9 (2)	C39—C40—C41—N5	2.0 (4)
C11—N3—C14—C13	2.9 (3)	C40—C39—C43—C42	−1.2 (4)
C11—N3—C14—C15	−177.2 (2)	C41—N5—C42—C43	0.5 (4)
C11—C10—C27—C28	−130.8 (3)	C42—N5—C41—C40	−2.1 (4)
C11—C10—C27—C31	50.3 (3)	C43—C39—C40—C41	−0.4 (4)
C11—C12—C13—C14	0.0 (3)	C44—N5—C41—C40	178.3 (2)
C12—C13—C14—N3	−1.8 (3)	C44—N5—C42—C43	−179.9 (2)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1B···O2	0.87	2.31	2.852 (10)	121
O4—H4B···O6	0.85 (2)	1.98 (2)	2.833 (4)	179 (5)
O6—H6A···O5	0.83 (2)	1.94 (3)	2.738 (3)	162 (6)
O3—H3C···O4	0.71 (5)	2.14 (5)	2.818 (4)	162 (6)