Crystal structure of bis­[1,3-bis­(di­phenyl­phosphan­yl)propane-κ2P,P′]platinum(II) dichloride chloro­form penta­solvate

Anderson, B.G.; Hoyte, S.A.; Spencer, J.L.

doi:10.1107/S205698901500136X

metal-organic compounds

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Volume 71| Part 2| February 2015| Page m37

doi:10.1107/S205698901500136X

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Crystal structure of bis[1,3-bis(diphenylphosphanyl)propane-κ²P,P′]platinum(II) dichloride chloroform pentasolvate

Bradley G. Anderson,^a Sarah A. Hoyte ^a ^* and John L. Spencer ^a

^aSchool of Chemical and Physical Sciences, Victoria University of Wellington, Wellington, New Zealand
^*Correspondence e-mail: sarah.hoyte@vuw.ac.nz

Edited by J. F. Gallagher, Dublin City University, Ireland (Received 20 October 2014; accepted 21 January 2015; online 28 January 2015)

In the title compound, [Pt{Ph₂P(CH₂)₃PPh₂}₂]Cl₂·5CHCl₃, the Pt^II cations, located on a centre of inversion, is coordinated by two chelating diphosphane ligands in a geometry which is close to square-planar. The chelate rings adopt a chair conformation. The Pt^II cations are arranged in layers separated by Cl⁻ anions as well as CHCl₃ solvent molecules. While this complex has been reported previously [Anderson et al. (1983 ). Inorg. Chim. Acta, 76, L251–L252], this is the first time a structure has been determined.

Keywords: crystal structure; 1,3-bis(diphenylphosphanyl)propane; platinum(II) complex.

CCDC reference: 1044833

1. Related literature

For structures of related group 10 M²⁺ bis-diphosphane complexes, see: Pahor & Bruno (1977 ); Engelhardt et al. (1984 ); Ferguson et al. (1993 ); Berning et al. (1999 ); Raebiger et al. (2004 ); Fischer (2006 ). The corresponding Pt⁰ complex [Pt(dppp)₂] [dppp is 1,3-bis(diphenylphosphanyl)propane] has been reported by Asker et al. (1990 ). For a previous report of the title compound, see: Anderson et al. (1983).

2. Experimental

2.1. Crystal data

[Pt(C₂₇H₂₆P₂)₂]Cl₂·5CHCl₃
M_r = 1687.67
Orthorhombic, P c c n
a = 26.2042 (9) Å
b = 15.3120 (5) Å
c = 16.7930 (5) Å
V = 6738.0 (4) Å³
Z = 4
Mo Kα radiation
μ = 2.89 mm⁻¹
T = 160 K
0.60 × 0.38 × 0.28 mm

2.2. Data collection

Bruker APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2007 ) T_min = 0.562, T_max = 0.746
179974 measured reflections
10325 independent reflections
7580 reflections with I > 2σ(I)
R_int = 0.063

2.3. Refinement

R[F² > 2σ(F²)] = 0.037
wR(F²) = 0.073
S = 1.20
10325 reflections
385 parameters
H-atom parameters constrained
Δρ_max = 0.73 e Å⁻³
Δρ_min = −0.97 e Å⁻³

Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2015 ); molecular graphics: Mercury (Macrae et al., 2008 ); software used to prepare material for publication: SHELXL97.

Supporting information

CCDC reference: 1044833

Crystal structure: contains datablock I. DOI: 10.1107/S205698901500136X/gg2144sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S205698901500136X/gg2144Isup2.hkl

checkCIF report

Comment top

When [PtCl₂(SEt₂)₂] is reacted with bicyclopropylidene, this results in the formation of the β-chloroalkyl complex [Pt(C(CH₂)₂C(CH₂)₂Cl)Cl(SEt₂)₂] after 5 days. When dppp (Ph₂P(CH₂)₃PPh₂) was added in an attempt to make a phosphine β-chloroalkyl complex, the β-chloroalkyl ligand undergoes a β-chloride elimination to regenerate the alkene and [Pt(dppp)₂]Cl₂ is formed. While this complex has been reported previously (Anderson et al., 1983), this is the first time a structure has been obtained (Fig. 1).

The asymmetric unit contains only half of the molecule, consisting of a complete dppp ligand as well as one of the Cl^- counter ions and half of the five CDCl₃ solvent molecules. The platinum is close to square planar, with a P1—Pt—P2 angle of 87.23 (3)°. This is smaller than the corresponding angle in the Pt(0) complex [Pt(dppp)₂] (97.76 (4)°) (Asker et al., 1990). The Pt—P bond lengths are 2.3648 (7) and 2.3790 (8) Å, longer than those in [Pt(dppp)₂] (2.286 (1) Å). The chelate ring has a 'chair' conformation, typical for dppp complexes. In [Pt(dppp)₂]Cl₂, the chelate two rings are rotated by 180° relative to each other, while in [Pt(dppp)₂] the rings are rotated by 87.20 (2)° (according to the PtP1P2 planes). While [Pt(dppp)₂]Cl₂ crystallized as a CDCl₃ solvate in the orthorhombic Pccn space group, [Pt(dppp)₂] crystallized solvent-free from tetrahydrofuran in the monoclinic C2/c space group. The Cl^- counter ion is separated by 4.197 Å from the Pt, showing that it is not coordinated. The [Pt(dppp)₂]²⁺ ions are arranged in two-dimensional layers, with the Cl^- anions and solvent between the layers.

Related literature top

For structures of related group 10 M²⁺ bis-diphosphane complexes, see: Pahor & Bruno (1977); Engelhardt et al. (1984); Ferguson et al. (1993); Berning et al. (1999); Raebiger et al. (2004); Fischer (2006). The corresponding Pt⁰ complex [Pt(dppp)₂] [dppp is 1,3-bis(diphenylphosphanyl)propane] has been reported by Asker et al. (1990). For a previous report of the title compound, see: Anderson et al. (1983).

Experimental top

[PtCl₂(SEt₂)₂] (50 mg, 0.11 mmol) was dissolved in CDCl₃ (0.5 ml) in an NMR tube under Ar and 5 equiv. bicyclopropylidene added (50 µL, 0.54 mmol). The reaction was stirred for 5 days, resulting in the formation of trans-[Pt(C(CH₂)₂C(CH₂)₂Cl)Cl(SEt₂)₂]. The solution was frozen in liquid N₂, and a solution of dppp (90 mg, 0.22 mmol) in CDCl₃ (0.5 ml) added. Crystals of [Pt(dppp)₂]Cl₂ formed as the solution warmed to RT.

Computing details top

Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT (Bruker, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2015); molecular graphics: Mercury (Macrae et al., 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top

Fig. 1. : ORTEP diagram of [Pt(Ph₂P(C₂H₃)PPh₂)₂]Cl₂ showing 50% probability ellipsoids. H atoms have been omitted for clarity.

Bis[1,3-bis(diphenylphosphanyl)propane-κ²P,P']platinum(II) dichloride chloroform pentasolvate top

Crystal data top

[Pt(C₂₇H₂₆P₂)₂]Cl₂·5CHCl₃	F(000) = 3352.00
M_r = 1687.67	D_x = 1.664 Mg m⁻³
Orthorhombic, Pccn	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ab 2ac	Cell parameters from 9982 reflections
a = 26.2042 (9) Å	θ = 2.4–30.5°
b = 15.3120 (5) Å	µ = 2.89 mm⁻¹
c = 16.7930 (5) Å	T = 160 K
V = 6738.0 (4) Å³	Block, colourless
Z = 4	0.6 × 0.38 × 0.28 mm

Data collection top

Bruker APEXII CCD diffractometer	10325 independent reflections
Radiation source: fine-focus sealed tube	7580 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.063
ϕ and ω scans	θ_max = 30.6°, θ_min = 2.4°
Absorption correction: multi-scan (SADABS; Bruker, 2007)	h = −37→37
T_min = 0.562, T_max = 0.746	k = −21→21
179974 measured reflections	l = −23→24

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.037	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.073	H-atom parameters constrained
S = 1.20	w = 1/[σ²(F_o²) + (0.P)² + 21.821P] where P = (F_o² + 2F_c²)/3
10325 reflections	(Δ/σ)_max = 0.001
385 parameters	Δρ_max = 0.73 e Å⁻³
0 restraints	Δρ_min = −0.97 e Å⁻³

Crystal data top

[Pt(C₂₇H₂₆P₂)₂]Cl₂·5CHCl₃	V = 6738.0 (4) Å³
M_r = 1687.67	Z = 4
Orthorhombic, Pccn	Mo Kα radiation
a = 26.2042 (9) Å	µ = 2.89 mm⁻¹
b = 15.3120 (5) Å	T = 160 K
c = 16.7930 (5) Å	0.6 × 0.38 × 0.28 mm

Data collection top

Bruker APEXII CCD diffractometer	10325 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2007)	7580 reflections with I > 2σ(I)
T_min = 0.562, T_max = 0.746	R_int = 0.063
179974 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.037	0 restraints
wR(F²) = 0.073	H-atom parameters constrained
S = 1.20	w = 1/[σ²(F_o²) + (0.P)² + 21.821P] where P = (F_o² + 2F_c²)/3
10325 reflections	Δρ_max = 0.73 e Å⁻³
385 parameters	Δρ_min = −0.97 e Å⁻³

Special details top

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

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Pt1	0.5000	0.0000	0.0000	0.01283 (4)
P2	0.49876 (3)	0.10087 (5)	0.10661 (4)	0.01623 (14)
P1	0.48568 (3)	−0.11136 (5)	0.09623 (4)	0.01524 (15)
C4	0.41837 (12)	−0.1208 (2)	0.11952 (18)	0.0178 (6)
C3	0.52924 (13)	0.0645 (2)	0.19883 (18)	0.0210 (6)
H3A	0.5648	0.0519	0.1875	0.025*
H3B	0.5284	0.1123	0.2367	0.025*
C18	0.53826 (15)	0.3596 (2)	0.1019 (2)	0.0278 (8)
H18	0.5219	0.4133	0.1061	0.033*
C1	0.51746 (13)	−0.0980 (2)	0.19268 (17)	0.0194 (6)
H1A	0.5082	−0.1472	0.2261	0.023*
H1B	0.5540	−0.1009	0.1841	0.023*
C21	0.58744 (13)	0.1990 (2)	0.0910 (2)	0.0234 (7)
H21	0.6040	0.1453	0.0886	0.028*
C2	0.50582 (13)	−0.0150 (2)	0.23790 (17)	0.0211 (7)
H2A	0.5188	−0.0202	0.2918	0.025*
H2B	0.4691	−0.0074	0.2410	0.025*
C9	0.40155 (13)	−0.1654 (2)	0.18772 (19)	0.0219 (7)
H9	0.4251	−0.1879	0.2237	0.026*
C22	0.43463 (13)	0.1321 (2)	0.13539 (19)	0.0203 (6)
C14	0.49389 (16)	−0.3787 (2)	0.0796 (2)	0.0299 (8)
H14	0.4719	−0.4262	0.0833	0.036*
C5	0.38263 (13)	−0.0870 (2)	0.0673 (2)	0.0239 (7)
H5	0.3934	−0.0568	0.0222	0.029*
C8	0.34994 (14)	−0.1758 (3)	0.2012 (2)	0.0294 (8)
H8	0.3389	−0.2057	0.2461	0.035*
C16	0.53416 (12)	0.2026 (2)	0.09712 (18)	0.0183 (6)
C19	0.59096 (16)	0.3563 (3)	0.0944 (2)	0.0316 (8)
H19	0.6099	0.4077	0.0932	0.038*
C17	0.50980 (13)	0.2833 (2)	0.10331 (18)	0.0217 (7)
H17	0.4745	0.2859	0.1084	0.026*
C11	0.56005 (14)	−0.2376 (2)	0.0705 (2)	0.0251 (7)
H11	0.5824	−0.1905	0.0679	0.030*
C10	0.50772 (13)	−0.22317 (19)	0.07887 (17)	0.0189 (6)
C6	0.33060 (14)	−0.0978 (3)	0.0817 (2)	0.0352 (9)
H6	0.3068	−0.0752	0.0463	0.042*
C12	0.57854 (16)	−0.3223 (3)	0.0660 (2)	0.0326 (9)
H12	0.6134	−0.3320	0.0598	0.039*
C15	0.47444 (14)	−0.2942 (2)	0.08337 (18)	0.0214 (7)
H15	0.4395	−0.2852	0.0888	0.026*
C23	0.39470 (13)	0.1199 (2)	0.0827 (2)	0.0236 (7)
H23	0.4008	0.0938	0.0336	0.028*
C20	0.61522 (15)	0.2762 (2)	0.0886 (2)	0.0291 (8)
H20	0.6505	0.2741	0.0830	0.035*
C7	0.31462 (15)	−0.1420 (3)	0.1484 (2)	0.0352 (9)
H7	0.2799	−0.1492	0.1581	0.042*
C13	0.54565 (17)	−0.3923 (3)	0.0706 (2)	0.0350 (9)
H13	0.5583	−0.4489	0.0676	0.042*
C26	0.37622 (16)	0.1975 (3)	0.2287 (3)	0.0365 (9)
H26	0.3698	0.2235	0.2778	0.044*
C24	0.34563 (15)	0.1462 (3)	0.1022 (3)	0.0343 (9)
H24	0.3189	0.1377	0.0665	0.041*
C27	0.42495 (15)	0.1714 (3)	0.2095 (2)	0.0288 (8)
H27	0.4515	0.1798	0.2455	0.035*
C25	0.33674 (16)	0.1853 (3)	0.1753 (3)	0.0414 (10)
H25	0.3039	0.2034	0.1885	0.050*
Cl1	0.35882 (4)	0.04388 (8)	−0.11105 (5)	0.0380 (2)
Cl3B	0.31059 (4)	0.01417 (7)	0.32358 (6)	0.0371 (2)
Cl2A	0.21666 (4)	0.05178 (8)	0.17673 (6)	0.0434 (3)
Cl2B	0.24294 (5)	−0.13417 (8)	0.34282 (7)	0.0475 (3)
Cl3A	0.14625 (5)	−0.09321 (7)	0.16878 (7)	0.0430 (2)
Cl1A	0.11366 (4)	0.07947 (8)	0.12128 (7)	0.0447 (3)
Cl1B	0.29044 (4)	−0.05640 (10)	0.48005 (6)	0.0523 (3)
C1B	0.26446 (14)	−0.0355 (3)	0.3849 (2)	0.0328 (8)
H1BA	0.2354	0.0042	0.3907	0.039*
C1A	0.15290 (14)	0.0195 (3)	0.1870 (2)	0.0304 (8)
H1AA	0.1420	0.0315	0.2417	0.036*
C1C	0.2657 (3)	0.2740 (5)	0.4313 (4)	0.0282 (15)	0.5
H1C	0.2954	0.3115	0.4218	0.034*	0.5
Cl3C	0.23595 (11)	0.2360 (3)	0.34548 (14)	0.0622 (9)	0.5
Cl1C	0.2171 (5)	0.3222 (11)	0.4886 (6)	0.076 (3)	0.5
Cl2C	0.2802 (3)	0.1693 (9)	0.4893 (3)	0.0494 (17)	0.5

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pt1	0.01516 (6)	0.01052 (6)	0.01280 (6)	0.00000 (7)	0.00067 (6)	0.00078 (6)
P2	0.0207 (4)	0.0126 (3)	0.0154 (3)	−0.0020 (3)	0.0032 (3)	−0.0003 (3)
P1	0.0192 (4)	0.0124 (3)	0.0141 (3)	0.0011 (3)	0.0022 (3)	0.0021 (3)
C4	0.0193 (15)	0.0149 (15)	0.0190 (14)	−0.0017 (12)	0.0029 (11)	−0.0026 (11)
C3	0.0254 (17)	0.0203 (16)	0.0174 (14)	−0.0028 (13)	−0.0029 (12)	0.0006 (12)
C18	0.044 (2)	0.0149 (16)	0.0248 (17)	−0.0045 (15)	0.0073 (15)	−0.0037 (13)
C1	0.0232 (15)	0.0188 (15)	0.0163 (13)	0.0000 (13)	−0.0023 (11)	0.0029 (11)
C21	0.0261 (17)	0.0215 (17)	0.0227 (15)	−0.0029 (14)	−0.0008 (13)	0.0006 (13)
C2	0.0278 (18)	0.0213 (17)	0.0141 (12)	−0.0034 (13)	−0.0035 (12)	0.0021 (10)
C9	0.0237 (17)	0.0212 (16)	0.0208 (15)	0.0015 (13)	0.0028 (12)	0.0020 (12)
C22	0.0258 (17)	0.0141 (15)	0.0211 (15)	−0.0009 (13)	0.0056 (12)	0.0026 (12)
C14	0.049 (2)	0.0157 (15)	0.0253 (16)	−0.0002 (16)	0.0086 (16)	0.0042 (12)
C5	0.0250 (17)	0.0251 (18)	0.0216 (15)	−0.0006 (14)	−0.0015 (13)	0.0039 (13)
C8	0.0276 (19)	0.033 (2)	0.0280 (17)	−0.0057 (16)	0.0099 (14)	−0.0017 (15)
C16	0.0240 (16)	0.0164 (15)	0.0146 (13)	−0.0049 (12)	0.0009 (11)	−0.0003 (11)
C19	0.043 (2)	0.0238 (18)	0.0276 (17)	−0.0149 (17)	0.0017 (16)	−0.0028 (15)
C17	0.0293 (19)	0.0170 (15)	0.0188 (14)	0.0002 (13)	0.0070 (12)	0.0005 (11)
C11	0.0303 (19)	0.0194 (17)	0.0255 (16)	0.0025 (14)	0.0090 (14)	0.0037 (13)
C10	0.0283 (19)	0.0106 (13)	0.0179 (13)	0.0016 (12)	0.0056 (12)	0.0030 (10)
C6	0.0229 (18)	0.046 (2)	0.036 (2)	0.0016 (17)	−0.0060 (15)	0.0019 (18)
C12	0.034 (2)	0.0257 (19)	0.038 (2)	0.0122 (16)	0.0134 (16)	0.0076 (16)
C15	0.0292 (18)	0.0194 (16)	0.0156 (14)	0.0002 (13)	0.0032 (12)	0.0016 (12)
C23	0.0254 (17)	0.0175 (16)	0.0280 (17)	0.0003 (13)	0.0041 (13)	0.0015 (13)
C20	0.0284 (19)	0.0282 (19)	0.0307 (18)	−0.0084 (15)	−0.0007 (15)	0.0007 (15)
C7	0.0206 (18)	0.043 (2)	0.042 (2)	−0.0021 (17)	0.0045 (16)	−0.0016 (18)
C13	0.053 (3)	0.0189 (18)	0.0335 (19)	0.0140 (18)	0.0129 (17)	0.0048 (15)
C26	0.037 (2)	0.033 (2)	0.039 (2)	0.0013 (18)	0.0192 (18)	−0.0097 (17)
C24	0.0241 (19)	0.031 (2)	0.047 (2)	−0.0007 (16)	0.0024 (17)	0.0015 (18)
C27	0.031 (2)	0.031 (2)	0.0245 (16)	−0.0018 (16)	0.0088 (14)	−0.0058 (14)
C25	0.027 (2)	0.035 (2)	0.063 (3)	0.0041 (17)	0.018 (2)	−0.001 (2)
Cl1	0.0287 (5)	0.0622 (7)	0.0231 (4)	−0.0202 (5)	−0.0050 (3)	0.0069 (4)
Cl3B	0.0336 (5)	0.0431 (6)	0.0346 (5)	0.0032 (4)	0.0003 (4)	0.0038 (4)
Cl2A	0.0321 (5)	0.0565 (7)	0.0417 (5)	−0.0104 (5)	−0.0056 (4)	0.0056 (5)
Cl2B	0.0446 (6)	0.0378 (6)	0.0602 (7)	−0.0017 (5)	0.0086 (5)	−0.0088 (5)
Cl3A	0.0497 (6)	0.0355 (6)	0.0437 (5)	−0.0053 (5)	−0.0016 (5)	0.0020 (4)
Cl1A	0.0346 (5)	0.0484 (7)	0.0510 (6)	0.0033 (5)	−0.0021 (5)	0.0146 (5)
Cl1B	0.0340 (5)	0.0915 (10)	0.0314 (5)	0.0023 (6)	0.0049 (4)	0.0052 (5)
C1B	0.0246 (19)	0.038 (2)	0.0358 (19)	0.0078 (16)	0.0004 (15)	−0.0033 (17)
C1A	0.031 (2)	0.038 (2)	0.0219 (16)	−0.0022 (16)	0.0035 (14)	0.0008 (14)
C1C	0.024 (4)	0.030 (4)	0.030 (3)	0.000 (3)	−0.004 (3)	−0.001 (3)
Cl3C	0.071 (3)	0.073 (3)	0.0421 (11)	0.0157 (19)	−0.0230 (11)	−0.0151 (14)
Cl1C	0.079 (6)	0.076 (5)	0.074 (5)	0.046 (4)	0.006 (4)	−0.009 (3)
Cl2C	0.045 (3)	0.076 (4)	0.027 (2)	0.041 (3)	0.0020 (18)	0.005 (2)

Geometric parameters (Å, º) top

Pt1—P2	2.3648 (7)	C5—C6	1.395 (5)
Pt1—P2ⁱ	2.3648 (7)	C8—C7	1.381 (6)
Pt1—P1	2.3790 (8)	C16—C17	1.395 (4)
Pt1—P1ⁱ	2.3790 (8)	C19—C20	1.385 (5)
P2—C3	1.829 (3)	C11—C10	1.396 (5)
P2—C22	1.813 (3)	C11—C12	1.387 (5)
P2—C16	1.820 (3)	C10—C15	1.396 (4)
P1—C4	1.812 (3)	C6—C7	1.374 (6)
P1—C1	1.833 (3)	C12—C13	1.377 (6)
P1—C10	1.830 (3)	C23—C24	1.386 (5)
C4—C9	1.404 (4)	C26—C27	1.376 (5)
C4—C5	1.384 (5)	C26—C25	1.382 (6)
C3—C2	1.513 (4)	C24—C25	1.386 (6)
C18—C19	1.388 (5)	Cl3B—C1B	1.761 (4)
C18—C17	1.387 (5)	Cl2A—C1A	1.751 (4)
C1—C2	1.512 (4)	Cl2B—C1B	1.760 (4)
C21—C16	1.401 (5)	Cl3A—C1A	1.761 (4)
C21—C20	1.390 (5)	Cl1A—C1A	1.766 (4)
C9—C8	1.380 (5)	Cl1B—C1B	1.765 (4)
C22—C23	1.382 (5)	C1C—Cl3C	1.739 (7)
C22—C27	1.405 (5)	C1C—Cl1C	1.759 (13)
C14—C15	1.391 (5)	C1C—Cl2C	1.914 (14)
C14—C13	1.381 (6)

P2—Pt1—P2ⁱ	180.0	C4—C5—C6	120.5 (3)
P2ⁱ—Pt1—P1	92.77 (3)	C9—C8—C7	120.6 (3)
P2—Pt1—P1	87.23 (3)	C21—C16—P2	118.7 (3)
P2—Pt1—P1ⁱ	92.77 (3)	C17—C16—P2	121.2 (2)
P2ⁱ—Pt1—P1ⁱ	87.23 (3)	C17—C16—C21	119.8 (3)
P1ⁱ—Pt1—P1	180.0	C20—C19—C18	119.7 (3)
C3—P2—Pt1	115.85 (11)	C18—C17—C16	119.9 (3)
C22—P2—Pt1	112.76 (11)	C12—C11—C10	119.8 (3)
C22—P2—C3	105.04 (15)	C11—C10—P1	118.3 (2)
C22—P2—C16	105.67 (15)	C11—C10—C15	119.7 (3)
C16—P2—Pt1	119.06 (10)	C15—C10—P1	121.5 (3)
C16—P2—C3	96.45 (15)	C7—C6—C5	119.9 (4)
C4—P1—Pt1	110.94 (11)	C13—C12—C11	120.4 (4)
C4—P1—C1	105.09 (15)	C14—C15—C10	119.5 (3)
C4—P1—C10	105.47 (15)	C22—C23—C24	120.8 (3)
C1—P1—Pt1	116.67 (11)	C19—C20—C21	120.8 (3)
C10—P1—Pt1	120.83 (10)	C6—C7—C8	120.2 (4)
C10—P1—C1	95.82 (15)	C12—C13—C14	120.2 (3)
C9—C4—P1	121.3 (3)	C27—C26—C25	120.2 (4)
C5—C4—P1	119.5 (2)	C25—C24—C23	119.3 (4)
C5—C4—C9	119.1 (3)	C26—C27—C22	120.0 (4)
C2—C3—P2	115.8 (2)	C26—C25—C24	120.5 (4)
C17—C18—C19	120.4 (3)	Cl3B—C1B—Cl1B	110.0 (2)
C2—C1—P1	116.5 (2)	Cl2B—C1B—Cl3B	110.8 (2)
C20—C21—C16	119.4 (3)	Cl2B—C1B—Cl1B	109.4 (2)
C1—C2—C3	112.1 (3)	Cl2A—C1A—Cl3A	110.8 (2)
C8—C9—C4	119.8 (3)	Cl2A—C1A—Cl1A	110.3 (2)
C23—C22—P2	119.7 (2)	Cl3A—C1A—Cl1A	110.1 (2)
C23—C22—C27	119.2 (3)	Cl3C—C1C—Cl1C	105.6 (5)
C27—C22—P2	121.1 (3)	Cl3C—C1C—Cl2C	103.3 (5)
C13—C14—C15	120.3 (3)	Cl1C—C1C—Cl2C	102.5 (6)

Pt1—P2—C3—C2	−61.9 (3)	C21—C16—C17—C18	1.2 (5)
Pt1—P2—C22—C23	−19.8 (3)	C9—C4—C5—C6	−0.7 (5)
Pt1—P2—C22—C27	162.4 (3)	C9—C8—C7—C6	0.2 (6)
Pt1—P2—C16—C21	−64.6 (3)	C22—P2—C3—C2	63.2 (3)
Pt1—P2—C16—C17	121.4 (2)	C22—P2—C16—C21	167.4 (3)
Pt1—P1—C4—C9	−163.8 (2)	C22—P2—C16—C17	−6.6 (3)
Pt1—P1—C4—C5	19.2 (3)	C22—C23—C24—C25	0.2 (6)
Pt1—P1—C1—C2	57.5 (3)	C5—C4—C9—C8	0.8 (5)
Pt1—P1—C10—C11	62.2 (3)	C5—C6—C7—C8	−0.1 (6)
Pt1—P1—C10—C15	−125.6 (2)	C16—P2—C3—C2	171.3 (3)
P2—C3—C2—C1	72.9 (3)	C16—P2—C22—C23	111.8 (3)
P2—C22—C23—C24	−177.6 (3)	C16—P2—C22—C27	−65.9 (3)
P2—C22—C27—C26	177.6 (3)	C16—C21—C20—C19	1.8 (5)
P2—C16—C17—C18	175.1 (2)	C19—C18—C17—C16	0.0 (5)
P1—C4—C9—C8	−176.2 (3)	C17—C18—C19—C20	−0.3 (5)
P1—C4—C5—C6	176.4 (3)	C11—C10—C15—C14	0.2 (5)
P1—C1—C2—C3	−70.5 (3)	C11—C12—C13—C14	0.1 (6)
P1—C10—C15—C14	−172.0 (2)	C10—P1—C4—C9	63.7 (3)
C4—P1—C1—C2	−65.8 (3)	C10—P1—C4—C5	−113.3 (3)
C4—P1—C10—C11	−171.2 (2)	C10—P1—C1—C2	−173.6 (3)
C4—P1—C10—C15	1.1 (3)	C10—C11—C12—C13	−0.7 (6)
C4—C9—C8—C7	−0.6 (6)	C12—C11—C10—P1	173.0 (3)
C4—C5—C6—C7	0.3 (6)	C12—C11—C10—C15	0.6 (5)
C3—P2—C22—C23	−146.9 (3)	C15—C14—C13—C12	0.7 (6)
C3—P2—C22—C27	35.4 (3)	C23—C22—C27—C26	−0.2 (5)
C3—P2—C16—C21	59.8 (3)	C23—C24—C25—C26	−0.5 (6)
C3—P2—C16—C17	−114.2 (3)	C20—C21—C16—P2	−176.1 (3)
C18—C19—C20—C21	−0.6 (6)	C20—C21—C16—C17	−2.1 (5)
C1—P1—C4—C9	−36.9 (3)	C13—C14—C15—C10	−0.8 (5)
C1—P1—C4—C5	146.2 (3)	C27—C22—C23—C24	0.2 (5)
C1—P1—C10—C11	−63.7 (3)	C27—C26—C25—C24	0.4 (7)
C1—P1—C10—C15	108.5 (3)	C25—C26—C27—C22	−0.1 (6)

Symmetry code: (i) −x+1, −y, −z.

Experimental details

Crystal data
Chemical formula	[Pt(C₂₇H₂₆P₂)₂]Cl₂·5CHCl₃
M_r	1687.67
Crystal system, space group	Orthorhombic, Pccn
Temperature (K)	160
a, b, c (Å)	26.2042 (9), 15.3120 (5), 16.7930 (5)
V (Å³)	6738.0 (4)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	2.89
Crystal size (mm)	0.6 × 0.38 × 0.28

Data collection
Diffractometer	Bruker APEXII CCD diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 2007)
T_min, T_max	0.562, 0.746
No. of measured, independent and observed [I > 2σ(I)] reflections	179974, 10325, 7580
R_int	0.063
(sin θ/λ)_max (Å⁻¹)	0.716

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.037, 0.073, 1.20
No. of reflections	10325
No. of parameters	385
H-atom treatment	H-atom parameters constrained
	w = 1/[σ²(F_o²) + (0.P)² + 21.821P] where P = (F_o² + 2F_c²)/3
Δρ_max, Δρ_min (e Å⁻³)	0.73, −0.97

Computer programs: APEX2 (Bruker, 2007), SAINT (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2015), Mercury (Macrae et al., 2008), SHELXL97 (Sheldrick, 2008).

Acknowledgements

We thank Dr Jan Wikaira at the University of Canterbury, New Zealand, for collection of the single-crystal X-ray data.

References

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