The heterometallic one-dimensional solvated coordination polymer [NiPt2Cl6(TRIP-Py)4]n

Gildenast, H.; Gruszien, L.; Englert, U.

doi:10.1107/S2053229623001845

research papers

STRUCTURAL
CHEMISTRY

ISSN: 2053-2296

Volume 79| Part 4| April 2023| Pages 118-124

https://doi.org/10.1107/S2053229623001845

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The heterometallic one-dimensional solvated coordination polymer [NiPt₂Cl₆(TRIP-Py)₄]_n

Hans Gildenast,^a Lukas Gruszien ^a and Ulli Englert ^a ^*

^aInstitute of Inorganic Chemistry, RWTH Aachen University, Landoltweg 1, 52074 Aachen, Germany
^*Correspondence e-mail: ullrich.englert@ac.rwth-aachen.de

Edited by A. Lemmerer, University of the Witwatersrand, South Africa (Received 22 December 2022; accepted 28 February 2023; online 9 March 2023)

The ditopic ligand 10-[4-(pyridin-4-yl)phenyl]-9-phospha-10-silatriptycene (TRIP-Py, C₂₉H₂₀NPSi) binds as a pyridine donor to Ni^II and as a phosphatriptycene donor towards Pt^II. The selectivity relies entirely on the Pearson character of the donor sites and the matching hardness of the respective metal cations. The product is the one-dimensional coordination polymer catena-poly[[[dichloridonickel(II)]-bis{μ-10-[4-(pyridin-4-yl)phenyl]-9-phospha-10-silatriptycene}-bis[dichloridoplatinum(II)]-bis{μ-10-[4-(pyridin-4-yl)phenyl]-9-phospha-10-silatriptycene}] dichloromethane pentasolvate ethanol icosasolvate], {[NiPt₂Cl₆(TRIP-Py)₄]·5CH₂Cl₂·20EtOH}_n (1), which retains large pores due to the inherent rigidity of the ligand. This is enabled by the caged triptycene scaffold which fixes the direction of the phosphorus donor with respect to the remaining molecule and especially the pyridyl moiety. In its crystal structure, which was determined from synchrotron data, the pores of the polymer are filled with dichloromethane and ethanol molecules. Finding a suitable model for the pore content is complicated as it is too disordered to give a reasonable atomic model but too ordered to be described by an electron gas solvent mask. This article presents an in-depth description of this polymer, as well as a discussion on the use of the bypass algorithm for solvent masks.

Keywords: heterometallic; coordination polymer; synchrotron; platinum; nickel; crystal structure; bypass algorithm; solvent mask; caged triptycene.

CCDC reference: 2245178

1. Introduction

The research area of coordination polymers (CPs) has become an established field in modern inorganic and coordination chemistry over recent decades (Batten et al., 2008 ). CPs offer the possibility to adjust the material properties not just through the design of the ligand and the choice of the metal cation, but also through the dimensionality and topology of the CP. This allows a tailoring for a vast range of applications from catalysis, magnetism and optics to chemical separation, medicine and electrochemistry (Wang et al., 2020 ; Zhong et al., 2022 ; Yu et al., 2022 ; Zhou et al., 2022 ; Zhang et al., 2021 ; Indra et al., 2018 ). Controlling and understanding the properties of a CP requires information on its structure, making diffraction techniques indispensable for the field. As the growth of large single crystals of CPs can be quite challenging due to their inherent insolubility, the field profits heavily from high-flux X-ray sources like synchrotron facilities and modern techniques like electron diffraction (Balestri et al., 2019 ; Huang et al., 2021 ).

While the vast majority of CPs contains a single type of metal cation, interest in heterometallic CPs containing two or more different metal cations in an orderly fashion is steadily growing (Kremer & Englert, 2018 ; Kuwamura & Konno, 2021 ). This inherently increases the synthetic challenge but opens an even larger playground to tune and combine properties. Gaining control over the position of the two different cations is frequently achieved by using heterofunctional ligands with distinctly different coordination sites. These can, for example, differ in their Pearson hardness (Pearson, 1963 ) and preferably coordinate metal cations of matching Pearson character.

In this article, we address the selectivity of a soft phosphorus and a harder nitrogen donor. This combination has been demonstrated to give selective heterometallic coordination compounds for a long list of discrete metal complexes (Hara et al., 2021 ; Schroers et al., 2021 ). In CP chemistry, however, the same pair of donor sites has only very recently been used for a heterometallic CP (Gildenast et al., 2022a ). The ligand used in this previous report on heterometallic Zn^II/Hg^II polymers and also in the construction of the title compound is a rigid linear linker combining a pyridyl moiety with a phosphatriptycene, abbreviated as TRIP-Py (Fig. 1).

Figure 1
Reaction scheme for the synthesis of [NiPt₂Cl₆(TRIP-Py)₄]_n and a simplified structural formula of the product.

The phosphatriptycene belongs to the family of caged phosphines and has unique properties due to its special geometry (Shet et al., 2021 ; Tsuji et al., 2006 ). The introduction of the secondary bridgehead forces the phenylene propellers to be parallel to the phosphorus lone pair. Thus, the H atoms are pointing in the same direction increasing steric demand. Accordingly, until our recent publication (Gildenast et al., 2022b ), no metal complex with more than two phosphatriptycene ligands bound to a single metal cation had been reported. At the same time, the geometry forces acute C—P—C angles which increases the s-character of the lone pair, lowering its basicity and σ-donor strength while increasing the π acidity (Agou et al., 2004 ; Freijee & Stam, 1980 ; Jongsma et al., 1974 ; Drover et al., 2018 ; Hu et al., 2019 ; Mahaut et al., 2022 ). This strengthens the bond, especially towards electron-rich metal cations (Cao et al., 2019 ; Hu et al., 2021 ).

In this article, we present the crystallization and particularly challenging structural investigation of a desolvation-labile heterometallic CP in which TRIP-Py connects the softer Pt^II and the harder Ni^II cations. In contrast to our previously reported structures involving TRIP-Py, the halides coordinated at either metal cation are not engaged in polymer expansion and remain strictly terminal.

2. Experimental

Unless stated otherwise, all reagents and solvents were obtained from commercial sources and used without further purification. TRIP-Py and [PtCl₂(COD)] were prepared according to published procedures (Gildenast et al., 2022a; Brauer, 1981 ). For the single-crystal X-ray diffraction measurement, the κ goniometer at PETRA-III, P24, EH1, was used. The instrument was equipped with a Dectris CdTe area detector. For our experiment, synchrotron radiation (25 keV, λ = 0.500 Å) was used at a temperature of 100 (2) K (Oxford Cryostream 600 instrument, Oxfordshire, UK). Data were integrated with XDS (Kabsch, 2010 ) and corrected for absorption by multi-scan methods with SADABS (Bruker, 2014 ). The powder diffraction patterns were recorded at the Institute of Inorganic Chemistry, RWTH Aachen University, using a curved Stoe imaging-plate detector (IP-PSD). The diffractogram was recorded on a flat sample at ambient temperature in transmission using Cu Kα₁ radiation. The ATR FT–IR spectrum was measured with a Shimadzu IRSpirit with a QATR-S ATR unit equipped with a diamond prism and is shown in Fig. 2. It immediately shows the presence of the ditopic ligand in the solid. In the range between 1600 and 500 cm⁻¹, the spectrum reflects the pattern observed for uncoordinated TRIP-Py (Gildenast et al., 2022a). The elemental analysis (CHN) was measured using a HERAEUS CHNO-Rapid VarioEL. The thermogravimetric (TGA) measurements were carried out with a Netzsch STA 409 C/CD in a flux of air (60 ml min⁻¹) at a heating rate of 5 K min⁻¹ on a sample dried in air. The EDX measurement was performed in a Leo/ZeissFE-SEM Supra 35 VP instrument equipped with an OxfordINCA Energy 200 (SiLi crystal, 133 eV, 10 mm²).

Figure 2
Comparison of the IR spectra of uncoordinated TRIP-Py and [NiPt₂Cl₆(TRIP-Py)₄]_n. The wavenumber axis is stretched between 2000 and 400 cm⁻¹.

2.1. Synthesis and crystallization

TRIP-Py (17.6 mg, 0.04 mmol) and [PtCl₂(COD)] (7.5 mg, 0.02 mmol) were each dissolved in dichloromethane (1 ml each) and the solutions were combined. NiCl₂·6H₂O (2.4 mg, 0.01 mmol) was dissolved in ethanol (1 ml). The two solutions were layered with a layer of the mixed solvents (1 ml) in between. After several days, light-green crystals of 1 were obtained. For bulk analyses, they were isolated by filtration and washed with ethanol (yield: 14.6 mg, 60%).

2.2. Refinement

Crystal data, data collection and structure refinement details for 1 are summarized in Table 1 and the asymmetric unit is shown in Fig. 3.

Table 1
Experimental details

Crystal data
Chemical formula	[NiPt₂Cl₆(C₂₉H₂₀NPSi)₄]·5CH₂Cl₂·20C₂H₆O
M_r	3773.65
Crystal system, space group	Triclinic, P $[\overline{1}]$
Temperature (K)	100
a, b, c (Å)	12.702 (7), 19.372 (10), 20.340 (7)
α, β, γ (°)	71.313 (7), 81.809 (13), 78.917 (19)
V (Å³)	4635 (4)
Z	1
Radiation type	Synchrotron, λ = 0.500 Å
μ (mm⁻¹)	0.78
Crystal size (mm)	0.20 × 0.20 × 0.10

Data collection
Diffractometer	Area-detector Dectris CdTe on a κ goniometer at EH1 P24, DESY
Absorption correction	Multi-scan (SADABS; Bruker, 2014)
T_min, T_max	0.775, 0.837
No. of measured, independent and observed [I > 2σ(I)] reflections	161591, 20869, 16117
R_int	0.063
(sin θ/λ)_max (Å⁻¹)	0.657

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.036, 0.108, 1.03
No. of reflections	20869
No. of parameters	691
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	1.58, −1.04
Computer programs: KAPPA (Paulmann, 2023 ), XDS2022 (Kabsch, 2010), SHELXT2018 (Sheldrick, 2015a ), SHELXL2018 (Sheldrick, 2015b ) and PLATON (Spek, 2020 ).

Figure 3
Displacement ellipsoid plot of the asymmetric unit of [NiPt₂Cl₆(TRIP-Py)₄]_n in 1 (40% probability level), with labels for the atom sites. H atoms and alternative conformations for the disordered pyridyl rings have been omitted for clarity.

H atoms attached to C atoms were introduced in calculated positions and treated as riding, with U_iso(H) = 1.2U_eq(C). For the pyridyl rings, split positions were refined for the C atoms in positions 2, 3, 5 and 6 with respect to the nitrogen. Only a site occupancy of 0.5 is compatible with reasonable interatomic distances between neighbouring pyridyl rings. The contribution of pore-contained solvent to the structure factors was treated with the bypass algorithm as implemented in SQUEEZE in PLATON (van der Sluis & Spek, 1990 ; Spek, 2015 ); a detailed discussion of alternative approaches is given in Section 3 (Results and discussion).

3. Results and discussion

The title compound, [NiPt₂Cl₆(TRIP-Py)₄]_n, was prepared by reactive diffusion crystallization of an in-situ-generated dichloromethane solution of the complex [PtCl₂(TRIP-Py)₂] with an ethanolic solution of NiCl₂. The insoluble product is a heterometallic coordination polymer connected via covalent and coordinative bonds in one spatial direction (Fig. 4).

Figure 4
Displacement ellipsoid plot of [NiPt₂Cl₆(TRIP-Py)₄]_n in 1 (50% probability level, space group P $[\overline{1}]$ , Z = 1) prepared with PLATON (Spek, 2020

). The two concerted local conformations for the pyridyl rings are coloured red and pink. Selected interatomic distances and angles (Å, °): Ni1—N1 2.100 (4), Ni1—N2 2.107 (3), Ni1—Cl3 2.4467 (18), τ₄(Pt1) = 0.19 and Var(X—Pt1—Y) = 1650.9°² (Yang et al., 2007

). [Symmetry codes: (a) x − 1, y, z − 1; (b) −x + 1, −y + 2, −z + 1.]

The Ni^II cation is located on a crystallographic centre of inversion and resides in pseudo-octahedral coordination by two chloride ligands and four pyridyl donors of TRIP-Py ligands. Steric repulsion between ortho H atoms of adjacent ligands and between pyridyl H atoms and the halide ligands requires a tilt of the heteroaromatic rings. As a continuous windmill arrangement is incompatible with the inversion symmetry, disorder with alternative ring conformations of exactly half site occupancy is enforced. Each [NiCl₂(TRIP-Py)₄] cross is connected to the next one via two PtCl₂ moieties with the P-atom donors in a cis configuration, resulting in a one-dimensional CP along [101]. Fig. 5 shows a scatter plot for the geometry of [PtX₂(PR₃)₂] complexes and clearly displays the expected binodal distribution of the Pt—P distances, with the trans complexes showing systematically larger values as two π acceptors are opposed and compete for backbonding from the same metal d orbital. The data for the examples with phosphatriptycenes are especially highlighted, including the data from this article.

Figure 5
Scatter plot for the geometry of [PtX₂(PR₃)₂] complexes (X = halide or methyl and PR₃ = tertiary phosphine). The P—Pt—P angle is plotted against the Pt—P distance. The data for the shown fragment were extracted from the CSD (Groom et al., 2016

). The search was limited to error-free data sets collected at T ≤ 200 K with R₁ ≤ 0.05. Polymers and disordered structures were excluded, as well as structures of chelating phosphines with a C₂ bridge. All Pt complexes of phosphatriptycenes are added to the plot with star-shaped data points, and their respective secondary heteroatom is noted as Y-TRIP, with Y being either B, N or Si. Additionally, the data from the structure presented in this article are noted with this article. The colours of the stars denote whether they are chloride or methyl complexes (Drover et al., 2018

; Tsuji et al., 2006

; Ube et al., 2017

The plot shows that the Pt—P distances for phosphatriptycenes are very comparable to those of regular uncaged phosphines. In contrast, the metal–ligand distances in Au^I complexes of phosphatriptycenes (Gildenast et al., 2022a) are among the shortest of all phosphines in the Cambridge Structural Database (CSD; Version 5.43, with updates from November 2022; Groom et al., 2016 ). We speculate that π backbonding may play a less pronounced role in the case of the Pt^II cation with its more positive formal charge. The P—Pt—P angle, however, is systematically at the larger end of the spectrum for phosphatriptycenes. The repulsion of the large triptycene moieties distorts the coordination sphere around the Pt^II cation increasing the P—Pt—P angle and compressing the three remaining cis angles. Additionally, a reduction in planarity of the coordination sphere occurs compared to the cis-PtCl₂ complex of the uncaged phosphine PPh₃ (Table 2).

Table 2
Selection of geometrical parameters of the Pt^II coordination sphere of 1 and two solvates of [PtCl₂(PPh₃)₂] (Miao et al., 2009 ; Al-Fawaz et al., 2004 ) representing the uncaged phosphines; discrepancies from planarity can be detected using the τ₄ parameter (Yang et al., 2007 ) and the dihedral angle φ between Pt1/P1/P2 and Pt1/Cl1/Cl2

	[NiPt₂Cl₆(TRIP-Py)₄]·5CH₂Cl₂·20EtOH	[PtCl₂(PPh₃)₂]·CHCl₃	[PtCl₂(PPh₃)₂]·3CHCl₃
Pt1—P1	2.2486 (17)	2.2481 (18)	2.2560 (19)
Pt1—P2	2.2563 (16)	2.266 (2)	2.2708 (19)
Pt1—Cl1	2.3428 (19)	2.324 (2)	2.353 (2)
Pt1—Cl2	2.3337 (17)	2.3548 (19)	2.350 (2)
P1—Pt1—P2	103.09 (5)	97.43 (7)	98.74 (7)
Cl1—Pt1—Cl2	86.88 (4)	86.48 (7)	85.24 (7)
P1—Pt1—Cl2	87.01 (4)	89.85 (7)	91.01 (7)
P2—Pt1—Cl1	84.85 (4)	86.26 (7)	85.11 (7)
τ₄	0.19	0.08	0.10
φ(PtCl₂, PtP₂)	14.04 (6)	2.01 (10)	3.69 (10)

There are very few contacts between individual polymer strands close to the sum of their van der Waals radii. This includes a contact between an aromatic H atom and a chloride ligand attached to the Ni centre [Cl3⋯H4^a = 2.92 Å; symmetry code: (a) −x, −y + 2, −z + 1], an aromatic H atom pointing towards the centre of an aromatic ring [C10⋯H39^b = 2.83 Å; symmetry code: (b) x, y, z − 1] and two aromatic C atoms around an inversion centre which puts them in a potential π-stacking position [C45⋯C45^c = 3.369 (9) Å; symmetry code: (c) −x + 2, −y + 1, −z + 2]. In none of these does the molecular arrangement suggest a strong interaction. Instead, there is a distinct packing feature with the PtCl₂ corner of each [Ni₂Pt₂(TRIP-Py)₄] parallelogram pointing roughly towards the re-entrant corner of the NiCl₂ vertex of a neighbouring strand. This results in a presumably weak offset π-stacking interaction [C16⋯C18^d = 3.620 (5) Å; symmetry code: (d) −x, −y + 1, −z + 1]. Fig. 6 shows how adjacent polymers are interdigitated.

Figure 6
Packing of two neighbouring polymer strands of [NiPt₂Cl₆(TRIP-Py)₄]_n in 1 shown along [311]. H atoms have been omitted and the triptycene wings simplified for clarity. The yellow ellipse shows how adjacent polymers are interdigitated.

The centre of the parallelogram also corresponds to the largest pore along [100] (Fig. 7). The diameter of the largest possible sphere that can pass through this pore has been determined with Zeo++ (Willems et al., 2012 ) and amounts to 5.02 Å. The pores along [010] and [001] are slightly more narrow with limiting diameters of 3.86 and 4.15 Å, respectively, and have much more contorted pathways. Depending on which size is used for the probe radius, the three-dimensional pore system comprises between 52 and 56% of the unit-cell volume (SQUEEZE in PLATON, 1.5 and 1.0 Å probe radius, electron count remains roughly the same, <4% discrepancy).

Figure 7
Packing of 1 × 3 × 2 unit cells of 1 with a void contact surface calculated with Mercury (Macrae et al., 2020

) (1.2 Å probe radius, 0.3 Å grid spacing). The spheres represent the diameter of the largest possible sphere that can pass through the pore along the given unit-cell vectors (Willems et al., 2012

The pore contains strongly disordered solvent molecules. Based on preliminary distances between residual electron-density peaks and in agreement with the solvents employed in the synthesis, both dichloromethane and ethanol molecules are present. A tentative refinement of solvent molecules was performed, and 5.6 dichloromethane and 10.8 ethanol molecules per unit cell could be assigned in this model A (Fig. 8).

Figure 8
The asymmetric unit of 1, with a partial molecular model of the solvent-filled pore. H atoms have been omited for clarity. The dichloromethane molecule shown as dashed is only partially occupied and overlaps with the position of the adjacent ethanol molecule.

On the one hand, the above-mentioned solvent model A is not fully satisfactory: it did not account for the complete pore space but left a discrete void and a thin solvent-accessible channel, with a combined volume of 871 Å per unit cell. Despite the combined use of rigid fragments and hard geometry restraints for the solvent part, this partial solvent model A did not converge without damping, most probably because of high correlation between refinement variables describing the solvent. On the other hand, the graphical synopsis of the solvent-masking process in Fig. 9 indicates that `squeezing out' the entire solvent-filled pore according to model B is an equally crude approximation.

Figure 9
Plot for 1 of the agreement factor R₁ against the diffraction resolution for the original data and the data modified with the bypass algorithm as implemented in PLATON (van der Sluis & Spek, 1990

; Spek, 2015

Fig. 9 shows that the contribution of the solvent molecules to the structure factors extends up to a resolution of 0.4 Å⁻¹, i.e. almost into atomic resolution. The solvent part is at least in part associated with long-range order and cannot be well modelled by an electron gas. This explains why the solvent-squeezed structure model B retains a significant number of disagreeable intensities in the intermediate resolution range. These unsatisfactory intensity data show better agreement with the calculated structure factors from the partial solvent model A. In conclusion, we decided to report the more straightforward model B because localization of individual solvent molecules is not a crucial feature for the title structure. The overall content of the pore can be estimated from the results of the bypass algorithm as summarized in Table 3.

Table 3
Void volume (V) and electron content (e⁻) according to the program SQUEEZE (Spek, 2015) as implemented in PLATON (Spek, 2020), and the average electron count per volume in the void ρ for the pore treated with the bypass algorithm

The values for V for dichloromethane and ethanol were taken from their crystal structures (Kawaguchi et al., 1973 ; Jönsson, 1976 ) and multiplied by 1.3 (Mecozzi & Rebek, 1998).

	V (Å³)	e⁻	ρ (e⁻ Å⁻³)
Void	2528	740	0.29
CH₂Cl₂	107	42	0.39
EtOH	97	26	0.27
5CH₂Cl₂ + 20EtOH	2475	730	0.29

For the estimation of the spatial demand of a disordered solvent molecule, we followed the suggestion of Mecozzi & Rebek (1998 ) and assumed a 1.3-fold of the volume of the molecules in their own crystal structure. A combination of 5 dichloromethane (DCM) and 20 ethanol molecules per unit cell represents a good fit to pore volume and electron count. This amount of dichloromethane molecules is slightly lower than in our tentative molecular solvent model A, but we recall that this model is rather unstable. The large number of volatile solvent molecules also makes the compound prone to rapid desolvation. This impairs a reasonable validation of the structure by powder diffraction. We measured powder patterns of both wet crystals taken directly from the mother liquor, as well as dried samples. Both of them look quite similar but do not match the phase characterized by single crystal X-ray diffraction. The loss of solvent molecules is also reflected in the elemental analysis which matches more closely the expected values of the desolvated polymer with small amounts of residual solvent (Table 4). The best match for the experimentally determined values is achieved for two dichloromethane molecules per unit cell.

Table 4
CHN elemental analysis (%) for the bulk material of [NiPt₂Cl₆(TRIP-Py)₄]_n (the sample was prepared by drying in air)

	C	H	N
Analysis calculated for desolvated (C₁₁₆H₈₀Cl₆N₄NiP₄Pt₂Si₄)	57.39	3.32	2.31
Analysis calculated for ·5DCM·20EtOH (C₁₆₁H₂₁₀Cl₁₆N₄NiO₂₀P₄Pt₂Si₄)	51.24	5.61	1.48
Analysis calculated for ·2DCM (C₁₁₈H₈₄Cl₁₀N₄NiP₄Pt₂Si₄)	54.56	3.26	2.16
Found	53.98	3.37	2.15

The elemental analysis matches the results obtained in the thermogravimetric analysis (Fig. 10). {[NiPt₂Cl₆(TRIP-Py)₄]·2DCM}_n loses weight in two well-separated steps. First, a gradual loss of 6.7% of mass until 160 °C is observed, which agrees with the desolvation of two dichloromethane molecules. The second step begins at 350 °C and ends at 520 °C, after which 37.5% of the original sample weight is left. The identity of the remaining black powder could not be identified unambiguously. Its diffraction pattern displays merely reflections for elemental Pt. These are very broad, indicating a small average particle size. Using energy-dispersive X-ray spectroscopy (EDX), the elements Pt, Ni, Si and P were detected in a ratio of 2.0 (3):1.3 (4):4.1 (5):4.0 (5), in acceptable match with the composition in the original CP. From this we propose that Ni and Si stay in their oxidation states Ni^II and Si^IV, that phosphorus is oxidized to phosphate anions and oxide anions balance the remaining positive charge. The total sum formula of this mixture has a molecular weight of 38.1% of the original CP and two molecules of dichloromethane, matching the experimental weight loss from the TGA measurement. The EDX measurement does however reveal a higher than expected value for oxygen. Our suggested composition would require a Pt:O ratio of 2:19; the EDX analysis yields 2.0 (3):34 (3). This discrepancy may be caused by a contribution to the oxygen signal from the material used for fixing the sample.

Figure 10
Thermogravimetric analysis of [NiPt₂Cl₆(TRIP-Py)₄]_n, with a heating rate of 5 K min⁻¹ in a stream of air.

4. Conclusion

The structural characterization of 1 proved challenging but also rewarding. The PtCl₂ moieties in the heterometallic polymer are exposed towards the periphery and therefore potentially useful for follow-up reactions. They might, for example, represent analytically active sites which could be tested in future experiments. The unique electronic properties of the phosphatriptycene can lead to interesting reactivities, and the very low solubility of the coordination polymer enables a simple separation of the catalyst from potential products.

Supporting information

CCDC reference: 2245178

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S2053229623001845/ef3041sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S2053229623001845/ef3041Isup2.hkl

Computing details top

Data collection: KAPPA (Paulmann, 2023); cell refinement: XDS2022 (Kabsch 2010); data reduction: XDS2022 (Kabsch 2010); program(s) used to solve structure: SHELXT2018 (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2018 (Sheldrick, 2015b); molecular graphics: PLATON (Spek, 2020); software used to prepare material for publication: SHELXL2018 (Sheldrick, 2015b).

catena-Poly[[[dichloridonickel(II)]-bis{µ-10-[4-(pyridin-4-yl)phenyl]-9-phospha-10-silatriptycene}-bis[dichloridoplatinum(II)]-bis{µ-10-[4-(pyridin-4-yl)phenyl]-9-phospha-10-silatriptycene}] dichloromethane pentasolvate ethanol icosasolvate] top

Crystal data top

[NiPt₂Cl₆(C₂₉H₂₀NPSi)₄]·5CH₂Cl₂·20C₂H₆O	Z = 1
M_r = 3773.65	F(000) = 1936
Triclinic, P1	D_x = 1.352 Mg m⁻³
a = 12.702 (7) Å	Synchrotron radiation, λ = 0.500 Å
b = 19.372 (10) Å	Cell parameters from 18294 reflections
c = 20.340 (7) Å	θ = 1.2–19.2°
α = 71.313 (7)°	µ = 0.78 mm⁻¹
β = 81.809 (13)°	T = 100 K
γ = 78.917 (19)°	Block, colourless
V = 4635 (4) Å³	0.20 × 0.20 × 0.10 mm

Data collection top

Area detector Dectris CdTe on kappa goniometer at EH1 P24, DESY diffractometer	16117 reflections with I > 2σ(I)
Radiation source: synchrotron	R_int = 0.063
rotation method, ω scans	θ_max = 19.2°, θ_min = 1.3°
Absorption correction: multi-scan (SADABS; Bruker, 2003)	h = −15→16
T_min = 0.775, T_max = 0.837	k = −24→25
161591 measured reflections	l = −26→25
20869 independent reflections

Refinement top

Refinement on F²	Primary atom site location: dual
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.036	H-atom parameters constrained
wR(F²) = 0.108	w = 1/[σ²(F_o²) + (0.0595P)² + 1.5152P] where P = (F_o² + 2F_c²)/3
S = 1.03	(Δ/σ)_max = 0.002
20869 reflections	Δρ_max = 1.58 e Å⁻³
691 parameters	Δρ_min = −1.04 e Å⁻³
0 restraints

Special details top

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 (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Pt1	−0.24780 (2)	0.51481 (2)	0.29402 (2)	0.06157 (6)
Ni1	0.500000	1.000000	0.500000	0.06009 (16)
Cl1	−0.34139 (10)	0.42920 (5)	0.27793 (5)	0.0881 (3)
Cl2	−0.25151 (9)	0.44541 (5)	0.41140 (4)	0.0804 (3)
Cl3	0.33746 (8)	1.07104 (4)	0.54048 (4)	0.0707 (2)
P1	−0.13199 (8)	0.57662 (4)	0.31726 (4)	0.0579 (2)
P2	0.71054 (8)	0.58261 (4)	1.18539 (4)	0.0594 (2)
Si1	0.00870 (9)	0.66614 (5)	0.35694 (5)	0.0662 (3)
Si2	0.65048 (11)	0.65298 (6)	1.03559 (5)	0.0747 (3)
N1	0.4055 (2)	0.93354 (13)	0.47811 (13)	0.0615 (7)
N2	0.5147 (3)	0.92798 (14)	0.60204 (14)	0.0638 (7)
C1	−0.1996 (3)	0.64304 (17)	0.36154 (15)	0.0616 (8)
C2	−0.3107 (3)	0.6512 (2)	0.37812 (18)	0.0726 (10)
H2	−0.352297	0.621783	0.366180	0.087*
C3	−0.3602 (4)	0.7016 (2)	0.4117 (2)	0.0857 (12)
H3	−0.435817	0.706440	0.423534	0.103*
C4	−0.3009 (4)	0.7455 (2)	0.4285 (2)	0.0839 (12)
H4	−0.335952	0.781279	0.450499	0.101*
C5	−0.1910 (4)	0.73726 (19)	0.41323 (18)	0.0747 (11)
H5	−0.150370	0.766687	0.425910	0.090*
C6	−0.1384 (3)	0.68638 (17)	0.37947 (16)	0.0655 (9)
C7	−0.0430 (3)	0.62890 (17)	0.24603 (16)	0.0610 (8)
C8	−0.0325 (3)	0.62007 (18)	0.18006 (17)	0.0663 (9)
H8	−0.071849	0.587614	0.170933	0.080*
C9	0.0353 (3)	0.6585 (2)	0.12800 (19)	0.0740 (10)
H9	0.043503	0.652042	0.083080	0.089*
C10	0.0912 (4)	0.7064 (2)	0.1412 (2)	0.0796 (11)
H10	0.134011	0.735560	0.104559	0.096*
C11	0.0850 (3)	0.7122 (2)	0.2087 (2)	0.0742 (10)
H11	0.127244	0.742822	0.218113	0.089*
C12	0.0177 (3)	0.67359 (18)	0.26177 (17)	0.0645 (9)
C13	−0.0241 (3)	0.52234 (17)	0.37306 (15)	0.0610 (8)
C14	0.0016 (3)	0.44582 (18)	0.39028 (16)	0.0653 (9)
H14	−0.039708	0.418773	0.374996	0.078*
C15	0.0870 (3)	0.40926 (19)	0.42954 (18)	0.0701 (9)
H15	0.104350	0.357076	0.441135	0.084*
C16	0.1475 (3)	0.4481 (2)	0.45208 (18)	0.0716 (10)
H16	0.204700	0.422437	0.480352	0.086*
C17	0.1250 (3)	0.5241 (2)	0.43358 (17)	0.0714 (10)
H17	0.168677	0.550287	0.448018	0.086*
C18	0.0390 (3)	0.56327 (18)	0.39400 (16)	0.0634 (9)
C19	0.0894 (3)	0.72160 (18)	0.38298 (18)	0.0682 (9)
C20	0.1114 (4)	0.78951 (19)	0.33846 (19)	0.0802 (12)
H20	0.084450	0.807822	0.293826	0.096*
C21	0.1715 (4)	0.83071 (19)	0.35790 (19)	0.0772 (11)
H21	0.186567	0.876448	0.326142	0.093*
C22	0.2105 (3)	0.80613 (17)	0.42370 (17)	0.0648 (9)
C23	0.1863 (3)	0.74037 (19)	0.46922 (18)	0.0727 (10)
H23	0.210780	0.723180	0.514544	0.087*
C24	0.1257 (4)	0.69867 (19)	0.44891 (18)	0.0767 (11)
H24	0.109036	0.653538	0.481077	0.092*
C25	0.2772 (3)	0.84978 (17)	0.44334 (16)	0.0626 (9)
C30	0.7227 (3)	0.68090 (17)	1.14695 (16)	0.0638 (9)
C31	0.7421 (4)	0.72430 (18)	1.18428 (18)	0.0741 (10)
H31	0.750653	0.703499	1.232681	0.089*
C32	0.7495 (4)	0.7982 (2)	1.1519 (2)	0.0935 (14)
H32	0.764497	0.827659	1.177804	0.112*
C33	0.7350 (5)	0.8287 (2)	1.0821 (2)	0.1035 (16)
H33	0.742610	0.878863	1.059253	0.124*
C34	0.7091 (5)	0.7860 (2)	1.0448 (2)	0.0946 (15)
H34	0.696578	0.807868	0.997051	0.114*
C35	0.7013 (4)	0.71205 (19)	1.07634 (17)	0.0731 (10)
C36	0.5675 (3)	0.5910 (2)	1.17181 (18)	0.0722 (10)
C37	0.4903 (4)	0.5728 (3)	1.2269 (2)	0.0894 (12)
H37	0.510360	0.555013	1.273340	0.107*
C38	0.3836 (4)	0.5804 (3)	1.2145 (3)	0.1151 (17)
H38	0.329718	0.569134	1.252141	0.138*
C39	0.3568 (5)	0.6050 (4)	1.1452 (4)	0.126 (2)
H39	0.284802	0.607087	1.135954	0.152*
C40	0.4325 (5)	0.6260 (3)	1.0907 (3)	0.1032 (15)
H40	0.411884	0.644376	1.044364	0.124*
C41	0.5400 (4)	0.6208 (2)	1.10275 (19)	0.0783 (11)
C42	0.7794 (3)	0.53983 (17)	1.11977 (16)	0.0640 (9)
C43	0.8554 (4)	0.47551 (19)	1.1399 (2)	0.0762 (11)
H43	0.872652	0.455985	1.186972	0.091*
C44	0.9048 (5)	0.4409 (2)	1.0920 (3)	0.0990 (15)
H44	0.955830	0.397246	1.106035	0.119*
C45	0.8809 (5)	0.4690 (3)	1.0234 (3)	0.1097 (17)
H45	0.917069	0.445621	0.990063	0.132*
C46	0.8034 (5)	0.5319 (2)	1.0029 (2)	0.0953 (15)
H46	0.784897	0.549482	0.956098	0.114*
C47	0.7530 (4)	0.56904 (19)	1.05017 (17)	0.0722 (10)
C48	0.6162 (4)	0.7046 (2)	0.94515 (19)	0.0813 (12)
C49	0.5188 (5)	0.7547 (2)	0.9328 (2)	0.0978 (15)
H49	0.468475	0.759504	0.970978	0.117*
C50	0.4963 (4)	0.7965 (2)	0.8663 (2)	0.0922 (14)
H50	0.429898	0.829047	0.858803	0.111*
C51	0.5695 (4)	0.79157 (19)	0.81019 (18)	0.0743 (10)
C52	0.6650 (4)	0.7436 (2)	0.8214 (2)	0.0825 (11)
H52	0.715192	0.739650	0.782915	0.099*
C53	0.6886 (4)	0.7008 (2)	0.88831 (19)	0.0824 (11)
H53	0.755289	0.668589	0.895160	0.099*
C54	0.5486 (3)	0.83811 (18)	0.73752 (17)	0.0700 (10)
C26A	0.3650 (7)	0.8758 (4)	0.4001 (3)	0.073 (2)	0.5
H26A	0.380745	0.866694	0.356212	0.087*	0.5
C27A	0.4301 (7)	0.9145 (4)	0.4191 (3)	0.0663 (19)	0.5
H27A	0.493055	0.927869	0.390011	0.080*	0.5
C28A	0.3258 (6)	0.9065 (3)	0.5224 (3)	0.0679 (19)	0.5
H28A	0.313484	0.915232	0.566382	0.081*	0.5
C29A	0.2598 (6)	0.8658 (4)	0.5067 (4)	0.0683 (19)	0.5
H29A	0.201977	0.848688	0.539272	0.082*	0.5
C55A	0.5044 (8)	0.9117 (4)	0.7252 (4)	0.078 (2)	0.5
H55A	0.484230	0.932357	0.762474	0.094*	0.5
C56A	0.4906 (7)	0.9535 (4)	0.6584 (4)	0.073 (2)	0.5
H56A	0.462178	1.004310	0.650280	0.087*	0.5
C57A	0.5517 (7)	0.8554 (3)	0.6161 (3)	0.072 (2)	0.5
H57A	0.565383	0.834537	0.578783	0.086*	0.5
C58A	0.5705 (7)	0.8100 (4)	0.6824 (3)	0.075 (2)	0.5
H58A	0.598700	0.759225	0.689796	0.090*	0.5
C26B	0.2508 (6)	0.9263 (3)	0.4242 (4)	0.069 (2)	0.5
H26B	0.189854	0.950550	0.398971	0.082*	0.5
C27B	0.3145 (7)	0.9664 (3)	0.4426 (4)	0.071 (2)	0.5
H27B	0.295274	1.018489	0.430316	0.085*	0.5
C28B	0.4274 (6)	0.8613 (3)	0.4950 (3)	0.0590 (16)	0.5
H28B	0.489230	0.837510	0.519544	0.071*	0.5
C29B	0.3656 (6)	0.8171 (3)	0.4793 (3)	0.0588 (16)	0.5
H29B	0.384981	0.764966	0.493557	0.071*	0.5
C55B	0.4445 (7)	0.8586 (4)	0.7133 (3)	0.0690 (19)	0.5
H55B	0.383869	0.842161	0.743340	0.083*	0.5
C56B	0.4322 (7)	0.9030 (3)	0.6450 (3)	0.0677 (19)	0.5
H56B	0.362450	0.915862	0.628661	0.081*	0.5
C57B	0.6140 (6)	0.9090 (4)	0.6241 (3)	0.0689 (19)	0.5
H57B	0.673096	0.925594	0.592533	0.083*	0.5
C58B	0.6323 (7)	0.8659 (4)	0.6913 (4)	0.073 (2)	0.5
H58B	0.702983	0.855229	0.705945	0.087*	0.5

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pt1	0.09865 (11)	0.05017 (7)	0.04435 (7)	−0.03446 (6)	−0.03229 (6)	−0.00160 (5)
Ni1	0.1002 (4)	0.0404 (3)	0.0481 (3)	−0.0289 (3)	−0.0364 (3)	−0.0020 (2)
Cl1	0.1367 (9)	0.0675 (5)	0.0747 (5)	−0.0557 (6)	−0.0507 (6)	−0.0010 (4)
Cl2	0.1125 (7)	0.0818 (6)	0.0483 (4)	−0.0517 (5)	−0.0360 (4)	0.0119 (4)
Cl3	0.1054 (7)	0.0512 (4)	0.0618 (4)	−0.0257 (4)	−0.0339 (4)	−0.0068 (3)
P1	0.0903 (6)	0.0504 (4)	0.0427 (4)	−0.0317 (4)	−0.0256 (4)	−0.0068 (3)
P2	0.0948 (6)	0.0476 (4)	0.0424 (4)	−0.0224 (4)	−0.0292 (4)	−0.0066 (3)
Si1	0.1010 (7)	0.0525 (5)	0.0573 (5)	−0.0340 (5)	−0.0358 (5)	−0.0081 (4)
Si2	0.1235 (9)	0.0595 (5)	0.0453 (5)	−0.0151 (5)	−0.0395 (5)	−0.0076 (4)
N1	0.097 (2)	0.0448 (13)	0.0529 (14)	−0.0290 (13)	−0.0341 (14)	−0.0061 (11)
N2	0.103 (2)	0.0424 (12)	0.0525 (14)	−0.0273 (13)	−0.0369 (14)	−0.0018 (10)
C1	0.093 (3)	0.0568 (17)	0.0433 (15)	−0.0290 (17)	−0.0262 (15)	−0.0082 (12)
C2	0.103 (3)	0.070 (2)	0.0556 (18)	−0.031 (2)	−0.0213 (18)	−0.0174 (16)
C3	0.109 (3)	0.087 (3)	0.071 (2)	−0.026 (2)	−0.014 (2)	−0.029 (2)
C4	0.121 (4)	0.071 (2)	0.072 (2)	−0.022 (2)	−0.018 (2)	−0.0293 (19)
C5	0.119 (3)	0.0572 (19)	0.0580 (19)	−0.029 (2)	−0.030 (2)	−0.0134 (15)
C6	0.106 (3)	0.0485 (16)	0.0505 (16)	−0.0274 (17)	−0.0306 (17)	−0.0072 (13)
C7	0.086 (2)	0.0540 (16)	0.0491 (16)	−0.0299 (16)	−0.0242 (15)	−0.0048 (13)
C8	0.096 (3)	0.0584 (18)	0.0518 (17)	−0.0300 (17)	−0.0240 (17)	−0.0084 (14)
C9	0.101 (3)	0.068 (2)	0.0564 (19)	−0.030 (2)	−0.0150 (18)	−0.0105 (16)
C10	0.104 (3)	0.070 (2)	0.067 (2)	−0.038 (2)	−0.013 (2)	−0.0062 (17)
C11	0.098 (3)	0.0598 (19)	0.072 (2)	−0.0384 (19)	−0.0207 (19)	−0.0079 (16)
C12	0.089 (2)	0.0543 (17)	0.0561 (17)	−0.0273 (16)	−0.0264 (16)	−0.0067 (14)
C13	0.092 (2)	0.0543 (16)	0.0441 (15)	−0.0274 (16)	−0.0245 (15)	−0.0079 (12)
C14	0.102 (3)	0.0543 (17)	0.0478 (16)	−0.0322 (17)	−0.0195 (16)	−0.0092 (13)
C15	0.100 (3)	0.0560 (18)	0.0567 (18)	−0.0253 (18)	−0.0241 (18)	−0.0057 (14)
C16	0.094 (3)	0.066 (2)	0.0565 (18)	−0.0243 (19)	−0.0305 (18)	−0.0030 (15)
C17	0.097 (3)	0.069 (2)	0.0567 (18)	−0.0313 (19)	−0.0318 (18)	−0.0096 (15)
C18	0.093 (2)	0.0546 (17)	0.0519 (16)	−0.0282 (16)	−0.0287 (16)	−0.0092 (13)
C19	0.099 (3)	0.0543 (17)	0.0624 (19)	−0.0296 (17)	−0.0377 (18)	−0.0094 (14)
C20	0.134 (3)	0.0553 (18)	0.065 (2)	−0.039 (2)	−0.053 (2)	−0.0030 (15)
C21	0.126 (3)	0.0550 (18)	0.0624 (19)	−0.044 (2)	−0.042 (2)	−0.0019 (15)
C22	0.096 (2)	0.0507 (16)	0.0579 (18)	−0.0317 (16)	−0.0320 (17)	−0.0085 (13)
C23	0.115 (3)	0.0582 (18)	0.0563 (18)	−0.0412 (19)	−0.0393 (19)	−0.0035 (14)
C24	0.122 (3)	0.0588 (19)	0.0600 (19)	−0.045 (2)	−0.036 (2)	−0.0035 (15)
C25	0.096 (2)	0.0484 (16)	0.0519 (16)	−0.0294 (16)	−0.0295 (16)	−0.0067 (13)
C30	0.098 (3)	0.0501 (16)	0.0466 (16)	−0.0183 (16)	−0.0235 (16)	−0.0079 (13)
C31	0.124 (3)	0.0514 (17)	0.0530 (18)	−0.0167 (19)	−0.0322 (19)	−0.0113 (14)
C32	0.168 (5)	0.0524 (19)	0.070 (2)	−0.028 (2)	−0.040 (3)	−0.0137 (17)
C33	0.185 (5)	0.051 (2)	0.074 (3)	−0.031 (3)	−0.037 (3)	−0.0001 (18)
C34	0.173 (5)	0.054 (2)	0.055 (2)	−0.022 (2)	−0.034 (2)	−0.0021 (16)
C35	0.122 (3)	0.0527 (17)	0.0455 (16)	−0.0140 (19)	−0.0269 (18)	−0.0072 (13)
C36	0.099 (3)	0.066 (2)	0.0568 (19)	−0.0221 (19)	−0.0289 (19)	−0.0117 (16)
C37	0.105 (3)	0.092 (3)	0.074 (3)	−0.029 (2)	−0.029 (2)	−0.013 (2)
C38	0.096 (4)	0.134 (5)	0.113 (4)	−0.026 (3)	−0.022 (3)	−0.025 (4)
C39	0.098 (4)	0.145 (5)	0.140 (5)	−0.005 (4)	−0.054 (4)	−0.038 (4)
C40	0.117 (4)	0.108 (4)	0.088 (3)	−0.013 (3)	−0.048 (3)	−0.019 (3)
C41	0.104 (3)	0.075 (2)	0.062 (2)	−0.016 (2)	−0.038 (2)	−0.0143 (17)
C42	0.100 (3)	0.0487 (16)	0.0520 (16)	−0.0234 (16)	−0.0264 (17)	−0.0124 (13)
C43	0.118 (3)	0.0528 (18)	0.065 (2)	−0.0174 (19)	−0.035 (2)	−0.0138 (15)
C44	0.141 (4)	0.068 (2)	0.094 (3)	0.002 (3)	−0.032 (3)	−0.034 (2)
C45	0.176 (5)	0.079 (3)	0.081 (3)	0.003 (3)	−0.024 (3)	−0.041 (2)
C46	0.169 (5)	0.067 (2)	0.056 (2)	−0.015 (3)	−0.030 (3)	−0.0206 (18)
C47	0.117 (3)	0.0587 (18)	0.0476 (17)	−0.0232 (19)	−0.0292 (18)	−0.0107 (14)
C48	0.134 (4)	0.062 (2)	0.0510 (19)	−0.011 (2)	−0.039 (2)	−0.0107 (15)
C49	0.157 (4)	0.077 (3)	0.0485 (19)	0.008 (3)	−0.029 (2)	−0.0111 (18)
C50	0.136 (4)	0.074 (2)	0.055 (2)	0.017 (2)	−0.032 (2)	−0.0119 (18)
C51	0.118 (3)	0.0559 (18)	0.0539 (19)	−0.014 (2)	−0.037 (2)	−0.0099 (15)
C52	0.112 (3)	0.074 (2)	0.056 (2)	−0.011 (2)	−0.030 (2)	−0.0045 (17)
C53	0.107 (3)	0.079 (2)	0.056 (2)	−0.010 (2)	−0.033 (2)	−0.0046 (17)
C54	0.112 (3)	0.0520 (17)	0.0515 (17)	−0.0182 (18)	−0.0361 (19)	−0.0072 (14)
C26A	0.121 (6)	0.059 (4)	0.051 (3)	−0.041 (4)	−0.033 (4)	−0.009 (3)
C27A	0.104 (5)	0.057 (3)	0.051 (3)	−0.043 (4)	−0.023 (3)	−0.009 (3)
C28A	0.107 (6)	0.052 (3)	0.056 (3)	−0.034 (4)	−0.031 (4)	−0.008 (3)
C29A	0.093 (5)	0.051 (3)	0.066 (4)	−0.029 (3)	−0.030 (4)	−0.006 (3)
C55A	0.130 (7)	0.058 (4)	0.052 (4)	−0.013 (4)	−0.040 (4)	−0.010 (3)
C56A	0.118 (6)	0.047 (3)	0.061 (4)	−0.013 (4)	−0.040 (4)	−0.012 (3)
C57A	0.132 (6)	0.040 (3)	0.049 (3)	−0.025 (4)	−0.039 (4)	−0.003 (2)
C58A	0.133 (7)	0.047 (3)	0.048 (3)	−0.016 (4)	−0.029 (4)	−0.007 (3)
C26B	0.102 (5)	0.048 (3)	0.067 (4)	−0.027 (3)	−0.048 (4)	−0.008 (3)
C27B	0.110 (6)	0.045 (3)	0.067 (4)	−0.022 (3)	−0.051 (4)	−0.004 (3)
C28B	0.092 (5)	0.040 (3)	0.053 (3)	−0.020 (3)	−0.037 (3)	−0.006 (2)
C29B	0.092 (5)	0.042 (3)	0.049 (3)	−0.027 (3)	−0.033 (3)	−0.002 (2)
C55B	0.109 (6)	0.053 (3)	0.047 (3)	−0.025 (4)	−0.028 (3)	−0.002 (3)
C56B	0.109 (6)	0.048 (3)	0.054 (3)	−0.024 (4)	−0.036 (4)	−0.008 (3)
C57B	0.095 (5)	0.066 (4)	0.054 (3)	−0.036 (4)	−0.035 (3)	−0.004 (3)
C58B	0.097 (5)	0.066 (4)	0.060 (4)	−0.029 (4)	−0.040 (4)	−0.001 (3)

Geometric parameters (Å, º) top

Pt1—P1	2.2493 (11)	C25—C29B	1.364 (7)
Pt1—P2ⁱ	2.2567 (10)	C25—C26A	1.386 (9)
Pt1—Cl2	2.3335 (11)	C25—C26B	1.391 (7)
Pt1—Cl1	2.3426 (12)	C25—C29A	1.398 (8)
Ni1—N1ⁱⁱ	2.100 (2)	C30—C31	1.374 (5)
Ni1—N1	2.100 (2)	C30—C35	1.412 (4)
Ni1—N2ⁱⁱ	2.108 (2)	C31—C32	1.386 (5)
Ni1—N2	2.108 (3)	C31—H31	0.9500
Ni1—Cl3	2.4461 (14)	C32—C33	1.377 (6)
Ni1—Cl3ⁱⁱ	2.4461 (14)	C32—H32	0.9500
P1—C1	1.817 (4)	C33—C34	1.395 (6)
P1—C13	1.842 (3)	C33—H33	0.9500
P1—C7	1.853 (3)	C34—C35	1.385 (5)
P2—C42	1.825 (4)	C34—H34	0.9500
P2—C30	1.840 (3)	C36—C37	1.382 (6)
P2—C36	1.845 (4)	C36—C41	1.404 (5)
Si1—C19	1.852 (3)	C37—C38	1.384 (7)
Si1—C6	1.856 (4)	C37—H37	0.9500
Si1—C18	1.874 (3)	C38—C39	1.406 (8)
Si1—C12	1.883 (4)	C38—H38	0.9500
Si2—C47	1.848 (4)	C39—C40	1.370 (8)
Si2—C48	1.859 (4)	C39—H39	0.9500
Si2—C35	1.860 (4)	C40—C41	1.401 (7)
Si2—C41	1.862 (5)	C40—H40	0.9500
N1—C28B	1.313 (6)	C42—C43	1.406 (5)
N1—C28A	1.324 (8)	C42—C47	1.409 (4)
N1—C27A	1.345 (7)	C43—C44	1.371 (6)
N1—C27B	1.387 (7)	C43—H43	0.9500
N2—C56B	1.326 (8)	C44—C45	1.381 (7)
N2—C57B	1.343 (8)	C44—H44	0.9500
N2—C57A	1.344 (7)	C45—C46	1.399 (7)
N2—C56A	1.362 (8)	C45—H45	0.9500
C1—C2	1.394 (5)	C46—C47	1.395 (6)
C1—C6	1.404 (4)	C46—H46	0.9500
C2—C3	1.374 (6)	C48—C53	1.383 (6)
C2—H2	0.9500	C48—C49	1.416 (7)
C3—C4	1.382 (6)	C49—C50	1.374 (5)
C3—H3	0.9500	C49—H49	0.9500
C4—C5	1.376 (6)	C50—C51	1.382 (6)
C4—H4	0.9500	C50—H50	0.9500
C5—C6	1.392 (5)	C51—C52	1.377 (6)
C5—H5	0.9500	C51—C54	1.495 (4)
C7—C8	1.391 (5)	C52—C53	1.388 (5)
C7—C12	1.397 (4)	C52—H52	0.9500
C8—C9	1.377 (5)	C53—H53	0.9500
C8—H8	0.9500	C54—C58A	1.370 (8)
C9—C10	1.382 (5)	C54—C55A	1.382 (8)
C9—H9	0.9500	C54—C58B	1.384 (9)
C10—C11	1.402 (5)	C54—C55B	1.416 (9)
C10—H10	0.9500	C26A—C27A	1.383 (8)
C11—C12	1.386 (5)	C26A—H26A	0.9500
C11—H11	0.9500	C27A—H27A	0.9500
C13—C14	1.393 (5)	C28A—C29A	1.384 (9)
C13—C18	1.419 (4)	C28A—H28A	0.9500
C14—C15	1.381 (5)	C29A—H29A	0.9500
C14—H14	0.9500	C55A—C56A	1.357 (9)
C15—C16	1.382 (5)	C55A—H55A	0.9500
C15—H15	0.9500	C56A—H56A	0.9500
C16—C17	1.380 (5)	C57A—C58A	1.378 (8)
C16—H16	0.9500	C57A—H57A	0.9500
C17—C18	1.398 (5)	C58A—H58A	0.9500
C17—H17	0.9500	C26B—C27B	1.383 (8)
C19—C24	1.387 (4)	C26B—H26B	0.9500
C19—C20	1.391 (4)	C27B—H27B	0.9500
C20—C21	1.378 (4)	C28B—C29B	1.398 (7)
C20—H20	0.9500	C28B—H28B	0.9500
C21—C22	1.398 (4)	C29B—H29B	0.9500
C21—H21	0.9500	C55B—C56B	1.394 (8)
C22—C23	1.374 (4)	C55B—H55B	0.9500
C22—C25	1.477 (4)	C56B—H56B	0.9500
C23—C24	1.400 (4)	C57B—C58B	1.381 (9)
C23—H23	0.9500	C57B—H57B	0.9500
C24—H24	0.9500	C58B—H58B	0.9500

P1—Pt1—P2ⁱ	103.07 (4)	C29B—C25—C22	121.7 (3)
P1—Pt1—Cl2	87.07 (4)	C26A—C25—C22	121.3 (4)
P2ⁱ—Pt1—Cl2	165.56 (4)	C26B—C25—C22	119.7 (4)
P1—Pt1—Cl1	168.18 (4)	C29A—C25—C22	123.4 (4)
P2ⁱ—Pt1—Cl1	84.82 (4)	C31—C30—C35	120.5 (3)
Cl2—Pt1—Cl1	86.88 (4)	C31—C30—P2	123.7 (2)
N1ⁱⁱ—Ni1—N1	180.0	C35—C30—P2	115.6 (2)
N1ⁱⁱ—Ni1—N2ⁱⁱ	91.30 (10)	C30—C31—C32	120.5 (3)
N1—Ni1—N2ⁱⁱ	88.71 (10)	C30—C31—H31	119.7
N1ⁱⁱ—Ni1—N2	88.70 (10)	C32—C31—H31	119.7
N1—Ni1—N2	91.29 (10)	C33—C32—C31	119.7 (4)
N2ⁱⁱ—Ni1—N2	180.0	C33—C32—H32	120.1
N1ⁱⁱ—Ni1—Cl3	89.86 (10)	C31—C32—H32	120.1
N1—Ni1—Cl3	90.14 (10)	C32—C33—C34	119.9 (4)
N2ⁱⁱ—Ni1—Cl3	89.62 (10)	C32—C33—H33	120.0
N2—Ni1—Cl3	90.39 (10)	C34—C33—H33	120.0
N1ⁱⁱ—Ni1—Cl3ⁱⁱ	90.14 (10)	C35—C34—C33	121.0 (3)
N1—Ni1—Cl3ⁱⁱ	89.86 (10)	C35—C34—H34	119.5
N2ⁱⁱ—Ni1—Cl3ⁱⁱ	90.39 (10)	C33—C34—H34	119.5
N2—Ni1—Cl3ⁱⁱ	89.61 (10)	C34—C35—C30	118.0 (3)
Cl3—Ni1—Cl3ⁱⁱ	180.00 (3)	C34—C35—Si2	124.7 (3)
C1—P1—C13	103.73 (15)	C30—C35—Si2	117.0 (3)
C1—P1—C7	104.51 (15)	C37—C36—C41	121.5 (4)
C13—P1—C7	96.17 (16)	C37—C36—P2	121.9 (3)
C1—P1—Pt1	112.13 (12)	C41—C36—P2	116.5 (3)
C13—P1—Pt1	117.55 (10)	C36—C37—C38	120.1 (4)
C7—P1—Pt1	120.35 (10)	C36—C37—H37	119.9
C42—P2—C30	104.44 (16)	C38—C37—H37	119.9
C42—P2—C36	102.41 (17)	C37—C38—C39	118.6 (5)
C30—P2—C36	97.21 (17)	C37—C38—H38	120.7
C42—P2—Pt1ⁱⁱⁱ	112.15 (11)	C39—C38—H38	120.7
C30—P2—Pt1ⁱⁱⁱ	124.07 (10)	C40—C39—C38	121.2 (5)
C36—P2—Pt1ⁱⁱⁱ	113.67 (12)	C40—C39—H39	119.4
C19—Si1—C6	114.22 (17)	C38—C39—H39	119.4
C19—Si1—C18	117.44 (15)	C39—C40—C41	120.5 (5)
C6—Si1—C18	103.04 (16)	C39—C40—H40	119.7
C19—Si1—C12	117.64 (16)	C41—C40—H40	119.7
C6—Si1—C12	102.99 (16)	C40—C41—C36	117.8 (4)
C18—Si1—C12	99.12 (15)	C40—C41—Si2	125.9 (3)
C47—Si2—C48	118.87 (18)	C36—C41—Si2	116.2 (3)
C47—Si2—C35	103.99 (18)	C43—C42—C47	120.3 (3)
C48—Si2—C35	111.43 (17)	C43—C42—P2	119.4 (3)
C47—Si2—C41	101.77 (18)	C47—C42—P2	120.3 (3)
C48—Si2—C41	118.6 (2)	C44—C43—C42	120.3 (4)
C35—Si2—C41	99.62 (18)	C44—C43—H43	119.9
C28A—N1—C27A	118.7 (4)	C42—C43—H43	119.9
C28B—N1—C27B	116.3 (4)	C43—C44—C45	120.4 (4)
C28B—N1—Ni1	124.2 (3)	C43—C44—H44	119.8
C28A—N1—Ni1	122.0 (3)	C45—C44—H44	119.8
C27A—N1—Ni1	119.1 (3)	C44—C45—C46	120.0 (4)
C27B—N1—Ni1	119.5 (3)	C44—C45—H45	120.0
C56B—N2—C57B	119.5 (5)	C46—C45—H45	120.0
C57A—N2—C56A	115.6 (4)	C47—C46—C45	120.9 (4)
C56B—N2—Ni1	123.9 (3)	C47—C46—H46	119.5
C57B—N2—Ni1	116.6 (3)	C45—C46—H46	119.5
C57A—N2—Ni1	123.2 (3)	C46—C47—C42	118.1 (4)
C56A—N2—Ni1	121.2 (3)	C46—C47—Si2	129.0 (3)
C2—C1—C6	119.8 (3)	C42—C47—Si2	112.9 (3)
C2—C1—P1	121.1 (2)	C53—C48—C49	117.7 (3)
C6—C1—P1	119.1 (3)	C53—C48—Si2	121.4 (3)
C3—C2—C1	120.1 (4)	C49—C48—Si2	120.6 (3)
C3—C2—H2	120.0	C50—C49—C48	120.8 (4)
C1—C2—H2	120.0	C50—C49—H49	119.6
C2—C3—C4	120.5 (5)	C48—C49—H49	119.6
C2—C3—H3	119.7	C49—C50—C51	120.5 (4)
C4—C3—H3	119.7	C49—C50—H50	119.8
C5—C4—C3	119.9 (4)	C51—C50—H50	119.8
C5—C4—H4	120.1	C52—C51—C50	119.4 (3)
C3—C4—H4	120.1	C52—C51—C54	119.0 (4)
C4—C5—C6	120.9 (3)	C50—C51—C54	121.6 (4)
C4—C5—H5	119.5	C51—C52—C53	120.7 (4)
C6—C5—H5	119.5	C51—C52—H52	119.7
C5—C6—C1	118.7 (4)	C53—C52—H52	119.7
C5—C6—Si1	126.8 (3)	C48—C53—C52	120.9 (4)
C1—C6—Si1	114.4 (3)	C48—C53—H53	119.6
C8—C7—C12	121.3 (3)	C52—C53—H53	119.6
C8—C7—P1	120.6 (2)	C58A—C54—C55A	118.5 (5)
C12—C7—P1	118.0 (2)	C58B—C54—C55B	116.9 (4)
C9—C8—C7	119.8 (3)	C58A—C54—C51	122.0 (4)
C9—C8—H8	120.1	C55A—C54—C51	119.4 (4)
C7—C8—H8	120.1	C58B—C54—C51	120.0 (4)
C8—C9—C10	119.9 (4)	C55B—C54—C51	123.0 (4)
C8—C9—H9	120.1	C27A—C26A—C25	121.7 (6)
C10—C9—H9	120.1	C27A—C26A—H26A	119.1
C9—C10—C11	120.1 (3)	C25—C26A—H26A	119.1
C9—C10—H10	120.0	N1—C27A—C26A	120.9 (7)
C11—C10—H10	120.0	N1—C27A—H27A	119.6
C12—C11—C10	120.6 (3)	C26A—C27A—H27A	119.6
C12—C11—H11	119.7	N1—C28A—C29A	122.3 (6)
C10—C11—H11	119.7	N1—C28A—H28A	118.9
C11—C12—C7	118.1 (3)	C29A—C28A—H28A	118.9
C11—C12—Si1	126.9 (3)	C28A—C29A—C25	120.7 (7)
C7—C12—Si1	114.6 (2)	C28A—C29A—H29A	119.7
C14—C13—C18	120.3 (3)	C25—C29A—H29A	119.7
C14—C13—P1	123.4 (2)	C56A—C55A—C54	118.3 (7)
C18—C13—P1	116.2 (2)	C56A—C55A—H55A	120.9
C15—C14—C13	120.0 (3)	C54—C55A—H55A	120.9
C15—C14—H14	120.0	C55A—C56A—N2	124.7 (6)
C13—C14—H14	120.0	C55A—C56A—H56A	117.6
C14—C15—C16	120.4 (3)	N2—C56A—H56A	117.6
C14—C15—H15	119.8	N2—C57A—C58A	122.8 (6)
C16—C15—H15	119.8	N2—C57A—H57A	118.6
C17—C16—C15	120.1 (3)	C58A—C57A—H57A	118.6
C17—C16—H16	119.9	C54—C58A—C57A	119.9 (6)
C15—C16—H16	119.9	C54—C58A—H58A	120.1
C16—C17—C18	121.3 (3)	C57A—C58A—H58A	120.1
C16—C17—H17	119.3	C27B—C26B—C25	119.0 (6)
C18—C17—H17	119.3	C27B—C26B—H26B	120.5
C17—C18—C13	117.8 (3)	C25—C26B—H26B	120.5
C17—C18—Si1	125.7 (2)	C26B—C27B—N1	122.6 (6)
C13—C18—Si1	116.1 (2)	C26B—C27B—H27B	118.7
C24—C19—C20	117.4 (3)	N1—C27B—H27B	118.7
C24—C19—Si1	121.2 (2)	N1—C28B—C29B	124.2 (5)
C20—C19—Si1	121.3 (2)	N1—C28B—H28B	117.9
C21—C20—C19	121.2 (3)	C29B—C28B—H28B	117.9
C21—C20—H20	119.4	C25—C29B—C28B	119.2 (5)
C19—C20—H20	119.4	C25—C29B—H29B	120.4
C20—C21—C22	120.9 (3)	C28B—C29B—H29B	120.4
C20—C21—H21	119.5	C56B—C55B—C54	119.2 (7)
C22—C21—H21	119.5	C56B—C55B—H55B	120.4
C23—C22—C21	118.6 (3)	C54—C55B—H55B	120.4
C23—C22—C25	120.9 (3)	N2—C56B—C55B	122.1 (7)
C21—C22—C25	120.5 (3)	N2—C56B—H56B	119.0
C22—C23—C24	120.1 (3)	C55B—C56B—H56B	119.0
C22—C23—H23	119.9	N2—C57B—C58B	121.7 (7)
C24—C23—H23	119.9	N2—C57B—H57B	119.1
C19—C24—C23	121.6 (3)	C58B—C57B—H57B	119.1
C19—C24—H24	119.2	C57B—C58B—C54	120.5 (6)
C23—C24—H24	119.2	C57B—C58B—H58B	119.8
C29B—C25—C26B	118.6 (4)	C54—C58B—H58B	119.8
C26A—C25—C29A	115.3 (4)

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

Selection of geometrical parameters of the Pt^II coordination sphere of 1 and two solvates of [PtCl₂(PPh₃)₂] (Miao et al., 2009; Al-Fawaz et al., 2004) representing the uncaged phosphines. Discrepancies from planarity can be detected using the τ₄ parameter (Yang et al., 2007) and the dihedral angle φ between Pt1/P1/P2 and Pt1/Cl1/Cl2. top

	[NiPt₂Cl₆(TRIP-Py)₄]·5CH₂Cl₂·20EtOH	[PtCl₂(PPh₃)₂]·CHCl₃	[PtCl₂(PPh₃)₂]·3CHCl₃
Pt1—P1	2.2486 (17)	2.2481 (18)	2.2560 (19)
Pt1—P2	2.2563 (16)	2.266 (2)	2.2708 (19)
Pt1—Cl1	2.3428 (19)	2.324 (2)	2.353 (2)
Pt1—Cl2	2.3337 (17)	2.3548 (19)	2.350 (2)
P1—Pt1—P2	103.09 (5)	97.43 (7)	98.74 (7)
Cl1—Pt1—Cl2	86.88 (4)	86.48 (7)	85.24 (7)
P1—Pt1—Cl2	87.01 (4)	89.85 (7)	91.01 (7)
P2—Pt1—Cl1	84.85 (4)	86.26 (7)	85.11 (7)
τ₄	0.19	0.08	0.10
φ(PtCl₂, PtP₂)	14.04 (6)	2.01 (10)	3.69 (10)

Void volume (V) and electron content (e^-) according to the program SQUEEZE (Spek, 2015) as implemented in PLATON (Spek, 2020), and average electron count per volume in the void ρ for the pore treated with the bypass algorithm. The values for V for dichloromethane and ethanol were taken from their crystal structures (Kawaguchi et al., 1973; Jönsson, 1976) and multiplied by 1.3 (Mecozzi & Rebek, 1998). top

	V (Å³)	e^-	ρ (e^- Å^-3)
Void	2528	740	0.29
CH₂Cl₂	107	42	0.39
EtOH	97	26	0.27
5CH₂Cl₂ + 20EtOH	2475	730	0.29

CHN elemental analysis (%)for the bulk material of [NiPt₂Cl₆(TRIPPy)₄]_n. The sample was prepared by drying in air. top

	C	H	N
Analysis calculated for desolvated (C₁₁₆H₈₀Cl₆N₄NiP₄Pt₂Si₄)	57.39	3.32	2.31
Analysis calculated for ·5DCM·20EtOH (C₁₆₁H₂₁₀Cl₁₆N₄NiO₂₀P₄Pt₂Si₄)	51.24	5.61	1.48
Analysis calculated for ·2DCM (C₁₁₈H₈₄Cl₁₀N₄NiP₄Pt₂Si₄)	54.56	3.26	2.16
Found	53.98	3.37	2.15

Acknowledgements

We thank Dr Carsten Paulmann for help with the single-crystal X-ray diffraction measurement at the synchrotron beamline P24, PETRA III, DESY. The EDX analysis was carried out by Anne Frommelius, which is gratefully acknowledged. Open access funding enabled and organized by Projekt DEAL.

Funding information

Funding for this research was provided by: Studienstiftung des Deutschen Volkes (scholarship to HG); One Hundred-Talent Program of Shanxi Province (grant to UE).

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