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Acta Crystallogr Sect E Struct Rep Online. 2009 November 1; 65(Pt 11): m1392.
Published online 2009 October 17. doi:  10.1107/S1600536809042226
PMCID: PMC2971432

cis-Dichloridobis(triisopropoxy­phosphine)­platinum(II)

Abstract

The title compound, [PtCl2(C9H21O3P)2], was obtained from a solution of PtCl2(COD) (COD = 1,5-cyclooctadiene) and triisopropyl­phosphite in dichloro­methane. The complex features a Pt(II) atom coordinated by two Cl and two P atoms, yielding a slightly distorted cis square-planar geometry.

Related literature

For the structure of cis-bis­(trimethoxy­phosphite)dichlorido­platinum, see: Bao et al. (1987 [triangle]), for cis-dichlorido­bis(di­meth­oxy­phenyl­phosphino)platinum(II), see: Slawin et al. (2007a [triangle]); for dichloridobis(methoxy­diphenyl­phosphino)platinum(II), see: Slawin et al. (2007b [triangle]) and for cis-bis­(trimethoxy­phos­phite)dichlorido­palladium(II), see Slawin et al. (2009 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-65-m1392-scheme1.jpg

Experimental

Crystal data

  • [PtCl2(C9H21O3P)2]
  • M r = 682.47
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-65-m1392-efi1.jpg
  • a = 10.8962 (4) Å
  • b = 18.9114 (8) Å
  • c = 14.2754 (6) Å
  • β = 104.7461 (10)°
  • V = 2844.7 (2) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 5.24 mm−1
  • T = 125 K
  • 0.22 × 0.22 × 0.13 mm

Data collection

  • Rigaku SCXmini diffractometer
  • Absorption correction: multi-scan (ABSCOR; Higashi, 1995 [triangle]) T min = 0.356, T max = 0.506
  • 24157 measured reflections
  • 4995 independent reflections
  • 4473 reflections with I > 2σ(I)
  • R int = 0.040

Refinement

  • R[F 2 > 2σ(F 2)] = 0.024
  • wR(F 2) = 0.038
  • S = 1.11
  • 4995 reflections
  • 275 parameters
  • H-atom parameters constrained
  • Δρmax = 0.57 e Å−3
  • Δρmin = −0.49 e Å−3

Data collection: SCXmini (Rigaku, 2006 [triangle]); cell refinement: PROCESS-AUTO (Rigaku, 1998 [triangle]); data reduction: PROCESS-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: CrystalStructure (Rigaku, 2006 [triangle]); software used to prepare material for publication: CrystalStructure.

Table 1
Selected geometric parameters (Å, °)

Supplementary Material

Crystal structure: contains datablocks General, I. DOI: 10.1107/S1600536809042226/fi2086sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809042226/fi2086Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

We are grateful to the EPSRC for support.

supplementary crystallographic information

Comment

The title complex can be compared to similar platinum dichloride complexes containing trimethoxy phosphite; [PtCl2(P(OMe)3)2] (Bao et al., 1987). When compared to the structure of [PtCl2(P(OMe)Ph2)2] and [PtCl2(P(OMe)2Ph)2] (Slawin et al., 2007a, 2007b) we note that the title compound has marginally shorter coordination bond lengths and significantly reduced Cl—Pt—Cl and P—Pt—P angles. Cl(1)—Pt(1)—Cl(2) 87.18?(2) , P(1)—Pt(1)—P(2) 96.99?(3) °

Experimental

0.5 g (1.34 mmol) of PtCl2(COD) was dissolved in the minimum volume of dichloromethane in a round-bottomed flask. To this 0.52 mL (2.67 mmol) of triisopropylphosphite was added. The solution was stirred for 0.5 h at room temperature. The product was precipitated via slow diffusion of hexane and the product was filtered off and dried under vacuum, [PtCl2(P(OiPr)3)2](0.82 mmol,ca 63%). 31P-{1H}NMR: δ 61.7 p.p.m.. J{Pt—P} 5812 Hz.

Refinement

All H atoms were included in calculated positions (C—H distances are 0.98 Å for methyl H atoms, 1.00 Å for methylene H atoms) and were refined as riding atoms with Uiso(H) = 1.2 Ueq(parent atom, methylene H atoms) or Uiso(H) = 1.5 Ueq(parent atom, methyl H atoms). The highest peak in the difference map is 1.23 Å from atom Pt1.

Figures

Fig. 1.
The structure of (1) with displacement ellipsoids drawn at the 50% probability level, hydrogen atoms omitted for clarity.

Crystal data

[PtCl2(C9H21O3P)2]F(000) = 1360.00
Mr = 682.47Dx = 1.593 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71075 Å
Hall symbol: -P 2ybcCell parameters from 27042 reflections
a = 10.8962 (4) Åθ = 3.0–27.5°
b = 18.9114 (8) ŵ = 5.24 mm1
c = 14.2754 (6) ÅT = 125 K
β = 104.7461 (10)°Chip, colourless
V = 2844.7 (2) Å30.22 × 0.22 × 0.13 mm
Z = 4

Data collection

Rigaku SCXmini diffractometer4995 independent reflections
Radiation source: fine-focus sealed tube4473 reflections with F2 > 2σ(F2)
Detector resolution: 6.85 pixels mm-1Rint = 0.040
ω scansθmax = 25.0°, θmin = 2.1°
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)h = −12→12
Tmin = 0.356, Tmax = 0.506k = −22→22
24157 measured reflectionsl = −16→16

Refinement

Refinement on F2H-atom parameters constrained
R[F2 > 2σ(F2)] = 0.024w = 1/[σ2(Fo2) + (0.0077P)2 + 2.3925P] where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.038(Δ/σ)max = 0.001
S = 1.11Δρmax = 0.57 e Å3
4995 reflectionsΔρmin = −0.49 e Å3
275 parameters

Special details

Geometry. ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY
Refinement. Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F2. R-factor (gt) are based on F. The threshold expression of F2 > 2.0 σ(F2) is used only for calculating R-factor (gt).

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

xyzUiso*/Ueq
Pt(1)0.111011 (11)0.242171 (6)0.268469 (9)0.01376 (4)
Cl(1)0.15473 (8)0.36409 (4)0.26788 (6)0.02227 (18)
Cl(2)−0.09964 (8)0.27341 (4)0.26386 (7)0.0280 (2)
P(1)0.04057 (8)0.13168 (4)0.25627 (6)0.01632 (18)
P(2)0.31368 (8)0.21699 (4)0.28526 (6)0.01501 (17)
O(1)0.14345 (19)0.07376 (10)0.25384 (16)0.0175 (5)
O(2)−0.0612 (2)0.11456 (11)0.15873 (16)0.0234 (5)
O(3)−0.0298 (2)0.10821 (11)0.33539 (17)0.0221 (5)
O(4)0.4129 (2)0.27767 (10)0.32742 (15)0.0180 (5)
O(5)0.3566 (2)0.19463 (12)0.19174 (17)0.0256 (5)
O(6)0.3592 (2)0.15798 (11)0.36474 (16)0.0200 (5)
C(1)0.1080 (3)−0.00243 (16)0.2408 (2)0.0216 (8)
C(2)0.1982 (3)−0.04269 (17)0.3196 (2)0.0326 (9)
C(3)0.1142 (4)−0.02438 (18)0.1407 (2)0.0384 (10)
C(4)−0.1988 (3)0.12485 (18)0.1375 (2)0.0311 (9)
C(5)−0.2575 (3)0.0519 (2)0.1211 (3)0.0587 (14)
C(6)−0.2359 (4)0.1716 (2)0.0491 (3)0.0513 (12)
C(7)0.0033 (3)0.13724 (18)0.4343 (2)0.0279 (8)
C(8)0.1093 (3)0.0943 (2)0.4968 (2)0.0382 (10)
C(9)−0.1176 (3)0.1367 (2)0.4670 (3)0.0449 (11)
C(10)0.4641 (3)0.32852 (17)0.2685 (2)0.0228 (8)
C(11)0.5885 (3)0.29936 (19)0.2570 (2)0.0315 (9)
C(12)0.4805 (3)0.39815 (17)0.3221 (2)0.0321 (9)
C(13)0.2760 (3)0.16206 (17)0.1040 (2)0.0225 (8)
C(14)0.3629 (4)0.1203 (2)0.0582 (3)0.0442 (11)
C(15)0.2054 (4)0.2179 (2)0.0382 (2)0.0534 (12)
C(16)0.4941 (3)0.13800 (17)0.3989 (2)0.0253 (8)
C(17)0.5077 (3)0.0630 (2)0.3695 (3)0.0533 (13)
C(18)0.5323 (3)0.1501 (2)0.5057 (2)0.0466 (11)
H(1)0.0195−0.00890.24730.026*
H(2)0.2847−0.03770.31200.039*
H(3)0.1744−0.09280.31550.039*
H(4)0.1945−0.02390.38280.039*
H(5)0.05480.00430.09240.046*
H(6)0.0912−0.07440.13060.046*
H(7)0.2005−0.01730.13380.046*
H(8)−0.22170.14810.19370.037*
H(9)−0.23170.02880.06770.070*
H(10)−0.35010.05600.10490.070*
H(11)−0.22860.02370.18020.070*
H(12)−0.19120.21690.06270.062*
H(13)−0.32770.17990.03260.062*
H(14)−0.21280.1484−0.00540.062*
H(15)0.03240.18720.43220.034*
H(16)0.08350.04460.49550.046*
H(17)0.12830.11190.56360.046*
H(18)0.18500.09840.47210.046*
H(19)−0.18090.16670.42390.054*
H(20)−0.10070.15470.53340.054*
H(21)−0.15000.08820.46480.054*
H(22)0.40310.33420.20350.027*
H(23)0.64620.29180.32100.038*
H(24)0.62650.33310.22040.038*
H(25)0.57330.25430.22190.038*
H(26)0.39790.41460.32880.038*
H(27)0.51600.43320.28570.038*
H(28)0.53830.39180.38640.038*
H(29)0.21410.12930.12250.027*
H(30)0.42760.15180.04440.053*
H(31)0.31350.0991−0.00230.053*
H(32)0.40410.08290.10260.053*
H(33)0.15100.24410.07120.064*
H(34)0.15300.1959−0.02050.064*
H(35)0.26600.25050.02080.064*
H(36)0.54580.16930.36740.030*
H(37)0.45700.03210.40000.064*
H(38)0.59710.04900.39020.064*
H(39)0.47780.05890.29890.064*
H(40)0.52050.20010.51920.056*
H(41)0.62170.13730.53110.056*
H(42)0.47970.12090.53670.056*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Pt(1)0.01280 (7)0.01280 (7)0.01598 (7)0.00090 (6)0.00422 (5)0.00039 (6)
Cl(1)0.0217 (4)0.0136 (4)0.0319 (5)−0.0003 (3)0.0075 (4)0.0018 (3)
Cl(2)0.0155 (4)0.0193 (4)0.0505 (6)0.0030 (3)0.0111 (4)−0.0011 (3)
P(1)0.0143 (4)0.0152 (4)0.0197 (5)−0.0008 (3)0.0047 (3)0.0000 (3)
P(2)0.0131 (4)0.0171 (4)0.0152 (4)0.0002 (3)0.0043 (3)−0.0004 (3)
O(1)0.0145 (12)0.0139 (11)0.0237 (13)−0.0001 (8)0.0044 (10)−0.0013 (9)
O(2)0.0168 (12)0.0244 (12)0.0254 (14)−0.0020 (10)−0.0012 (11)−0.0037 (10)
O(3)0.0226 (13)0.0195 (12)0.0279 (14)−0.0059 (9)0.0131 (11)−0.0031 (10)
O(4)0.0178 (12)0.0175 (11)0.0187 (12)−0.0038 (9)0.0046 (10)0.0006 (9)
O(5)0.0174 (13)0.0394 (14)0.0214 (13)−0.0001 (10)0.0076 (11)−0.0091 (10)
O(6)0.0140 (12)0.0178 (11)0.0258 (14)0.0004 (9)0.0004 (10)0.0073 (9)
C(1)0.0244 (19)0.0115 (16)0.030 (2)−0.0046 (14)0.0082 (17)−0.0032 (13)
C(2)0.046 (2)0.0159 (18)0.034 (2)0.0017 (17)0.008 (2)0.0006 (16)
C(3)0.059 (2)0.023 (2)0.031 (2)−0.0006 (18)0.008 (2)−0.0051 (16)
C(4)0.017 (2)0.0241 (19)0.044 (2)0.0016 (15)−0.0071 (18)−0.0037 (17)
C(5)0.027 (2)0.035 (2)0.103 (4)−0.0081 (19)−0.005 (2)−0.005 (2)
C(6)0.046 (2)0.041 (2)0.052 (3)0.010 (2)−0.015 (2)0.002 (2)
C(7)0.040 (2)0.0227 (19)0.026 (2)−0.0053 (16)0.0177 (19)−0.0063 (15)
C(8)0.053 (2)0.036 (2)0.026 (2)−0.0003 (19)0.013 (2)−0.0005 (17)
C(9)0.057 (3)0.041 (2)0.052 (3)0.007 (2)0.042 (2)0.002 (2)
C(10)0.0162 (19)0.0271 (19)0.026 (2)−0.0051 (14)0.0073 (16)0.0091 (15)
C(11)0.017 (2)0.041 (2)0.038 (2)−0.0048 (16)0.0108 (18)0.0048 (18)
C(12)0.027 (2)0.024 (2)0.045 (2)−0.0072 (16)0.0079 (19)0.0070 (17)
C(13)0.027 (2)0.0254 (19)0.0166 (19)−0.0076 (15)0.0085 (16)−0.0053 (14)
C(14)0.054 (2)0.047 (2)0.036 (2)0.014 (2)0.019 (2)−0.011 (2)
C(15)0.074 (3)0.065 (3)0.021 (2)0.030 (2)0.012 (2)0.004 (2)
C(16)0.0150 (19)0.0242 (19)0.034 (2)0.0035 (14)0.0006 (17)0.0058 (15)
C(17)0.034 (2)0.039 (2)0.076 (3)0.014 (2)−0.004 (2)−0.009 (2)
C(18)0.030 (2)0.060 (2)0.041 (2)0.012 (2)−0.006 (2)0.003 (2)

Geometric parameters (Å, °)

Pt(1)—Cl(1)2.3548 (7)C(4)—H(8)1.000
Pt(1)—Cl(2)2.3547 (9)C(5)—H(9)0.980
Pt(1)—P(1)2.2176 (7)C(5)—H(10)0.980
Pt(1)—P(2)2.2117 (8)C(5)—H(11)0.980
P(1)—O(1)1.574 (2)C(6)—H(12)0.980
P(1)—O(2)1.577 (2)C(6)—H(13)0.980
P(1)—O(3)1.582 (2)C(6)—H(14)0.980
P(2)—O(4)1.587 (2)C(7)—H(15)1.000
P(2)—O(5)1.580 (2)C(8)—H(16)0.980
P(2)—O(6)1.579 (2)C(8)—H(17)0.980
O(1)—C(1)1.491 (3)C(8)—H(18)0.980
O(2)—C(4)1.466 (4)C(9)—H(19)0.980
O(3)—C(7)1.472 (4)C(9)—H(20)0.980
O(4)—C(10)1.477 (4)C(9)—H(21)0.980
O(5)—C(13)1.470 (3)C(10)—H(22)1.000
O(6)—C(16)1.475 (3)C(11)—H(23)0.980
C(1)—C(2)1.500 (4)C(11)—H(24)0.980
C(1)—C(3)1.506 (5)C(11)—H(25)0.980
C(4)—C(5)1.513 (5)C(12)—H(26)0.980
C(4)—C(6)1.509 (5)C(12)—H(27)0.980
C(7)—C(8)1.505 (4)C(12)—H(28)0.980
C(7)—C(9)1.505 (6)C(13)—H(29)1.000
C(10)—C(11)1.510 (5)C(14)—H(30)0.980
C(10)—C(12)1.510 (4)C(14)—H(31)0.980
C(13)—C(14)1.504 (5)C(14)—H(32)0.980
C(13)—C(15)1.490 (5)C(15)—H(33)0.980
C(16)—C(17)1.497 (5)C(15)—H(34)0.980
C(16)—C(18)1.491 (5)C(15)—H(35)0.980
C(1)—H(1)1.000C(16)—H(36)1.000
C(2)—H(2)0.980C(17)—H(37)0.980
C(2)—H(3)0.980C(17)—H(38)0.980
C(2)—H(4)0.980C(17)—H(39)0.980
C(3)—H(5)0.980C(18)—H(40)0.980
C(3)—H(6)0.980C(18)—H(41)0.980
C(3)—H(7)0.980C(18)—H(42)0.980
Cl(2)···C(11)i3.410 (3)H(19)···H(12)ii2.981
C(7)···C(15)ii3.591 (5)H(19)···H(23)i3.144
C(11)···Cl(2)iii3.410 (3)H(19)···H(36)i2.880
C(15)···C(7)iv3.591 (5)H(19)···H(38)i3.233
Pt(1)···H(34)ii3.155H(19)···H(41)i2.992
Pt(1)···H(35)ii3.571H(20)···Cl(2)ii3.557
Cl(1)···H(1)v3.035H(20)···C(2)vi3.340
Cl(1)···H(3)v3.574H(20)···H(3)vi2.748
Cl(1)···H(6)v3.551H(20)···H(4)vi3.036
Cl(1)···H(11)v3.162H(20)···H(12)ii2.693
Cl(1)···H(17)iv2.893H(20)···H(33)ii3.275
Cl(1)···H(31)ii3.369H(20)···H(41)i3.034
Cl(1)···H(34)ii3.231H(21)···C(2)vi3.364
Cl(2)···H(3)v2.807H(21)···C(8)vi3.505
Cl(2)···H(6)v3.238H(21)···H(3)vi3.215
Cl(2)···H(20)iv3.557H(21)···H(4)vi2.643
Cl(2)···H(23)i3.099H(21)···H(16)vi2.635
Cl(2)···H(24)i3.101H(21)···H(36)i3.595
Cl(2)···H(25)i3.479H(21)···H(38)i2.791
P(2)···H(35)ii3.584H(21)···H(41)i3.024
O(4)···H(30)ii3.339H(22)···C(18)iv3.473
O(4)···H(35)ii3.567H(22)···H(17)iv3.309
O(6)···H(35)ii3.185H(22)···H(40)iv3.269
C(2)···H(20)vi3.340H(22)···H(42)iv2.845
C(2)···H(21)vi3.364H(23)···Cl(2)iii3.099
C(2)···H(24)vii3.170H(23)···C(6)xii3.256
C(2)···H(41)viii3.076H(23)···H(12)xii3.457
C(3)···H(5)ix3.389H(23)···H(13)xii3.010
C(3)···H(9)ix3.526H(23)···H(14)xii2.801
C(3)···H(14)ix3.383H(23)···H(19)iii3.144
C(5)···H(26)x3.186H(24)···Cl(2)iii3.101
C(5)···H(31)ix3.298H(24)···C(2)xiii3.170
C(6)···H(23)xi3.256H(24)···C(18)iv2.992
C(6)···H(28)xi3.159H(24)···H(2)xiii2.711
C(6)···H(40)xi3.542H(24)···H(3)xiii2.739
C(7)···H(33)ii3.138H(24)···H(40)iv2.879
C(7)···H(34)ii3.535H(24)···H(41)iv2.747
C(7)···H(35)ii3.525H(24)···H(42)iv2.839
C(8)···H(16)vi3.382H(25)···Cl(2)iii3.479
C(8)···H(21)vi3.505H(25)···C(18)iv3.507
C(8)···H(33)ii3.230H(25)···H(8)iii3.106
C(8)···H(35)ii3.369H(25)···H(13)iii3.455
C(9)···H(3)vi3.420H(25)···H(40)iv2.933
C(9)···H(4)vi3.281H(25)···H(41)iv3.554
C(9)···H(12)ii3.277H(25)···H(42)iv3.497
C(9)···H(16)vi3.475H(26)···C(5)v3.186
C(9)···H(38)i3.447H(26)···C(14)ii3.456
C(9)···H(41)i3.199H(26)···H(9)v3.390
C(10)···H(42)iv3.489H(26)···H(10)v2.928
C(11)···H(40)iv3.285H(26)···H(11)v2.748
C(11)···H(41)iv3.543H(26)···H(30)ii3.263
C(11)···H(42)iv3.416H(26)···H(31)ii2.802
C(12)···H(10)v3.574H(27)···C(17)xiii3.273
C(12)···H(13)xii3.519H(27)···H(2)xiii2.916
C(12)···H(30)ii3.497H(27)···H(7)xiii3.151
C(12)···H(31)ii3.453H(27)···H(10)v3.541
C(12)···H(39)xiii3.582H(27)···H(32)xiii3.257
C(14)···H(9)ix3.453H(27)···H(37)xiii3.318
C(14)···H(10)iii3.262H(27)···H(38)xiii3.323
C(14)···H(26)iv3.456H(27)···H(39)xiii2.675
C(14)···H(28)iv3.479H(28)···C(6)xii3.159
C(15)···H(15)iv2.759H(28)···C(14)ii3.479
C(15)···H(17)iv3.369H(28)···H(7)xiii3.399
C(15)···H(18)iv3.591H(28)···H(9)xii3.454
C(16)···H(19)iii3.510H(28)···H(10)xii3.201
C(17)···H(27)vii3.273H(28)···H(13)xii2.603
C(18)···H(2)viii3.554H(28)···H(14)xii2.862
C(18)···H(13)xii3.538H(28)···H(30)ii2.934
C(18)···H(22)ii3.473H(28)···H(31)ii3.245
C(18)···H(24)ii2.992H(30)···O(4)iv3.339
C(18)···H(25)ii3.507H(30)···C(12)iv3.497
C(18)···H(35)ii3.510H(30)···H(10)iii2.971
H(1)···Cl(1)x3.035H(30)···H(13)iii2.766
H(2)···C(18)viii3.554H(30)···H(26)iv3.263
H(2)···H(24)vii2.711H(30)···H(28)iv2.934
H(2)···H(27)vii2.916H(30)···H(40)iv3.031
H(2)···H(41)viii2.905H(31)···Cl(1)iv3.369
H(2)···H(42)viii3.302H(31)···C(5)ix3.298
H(3)···Cl(1)x3.574H(31)···C(12)iv3.453
H(3)···Cl(2)x2.807H(31)···H(9)ix2.663
H(3)···C(9)vi3.420H(31)···H(10)ix3.348
H(3)···H(20)vi2.748H(31)···H(11)ix3.390
H(3)···H(21)vi3.215H(31)···H(26)iv2.802
H(3)···H(24)vii2.739H(31)···H(28)iv3.245
H(3)···H(41)viii2.821H(32)···H(9)ix3.403
H(4)···C(9)vi3.281H(32)···H(10)iii2.718
H(4)···H(20)vi3.036H(32)···H(27)vii3.257
H(4)···H(21)vi2.643H(33)···C(7)iv3.138
H(4)···H(38)viii3.484H(33)···C(8)iv3.230
H(4)···H(41)viii2.978H(33)···H(15)iv2.448
H(5)···C(3)ix3.389H(33)···H(17)iv2.734
H(5)···H(5)ix2.610H(33)···H(18)iv3.358
H(5)···H(6)ix3.442H(33)···H(20)iv3.275
H(5)···H(9)ix3.402H(34)···Pt(1)iv3.155
H(6)···Cl(1)x3.551H(34)···Cl(1)iv3.231
H(6)···Cl(2)x3.238H(34)···C(7)iv3.535
H(6)···H(5)ix3.442H(34)···H(6)ix3.563
H(6)···H(14)ix2.849H(34)···H(15)iv2.572
H(6)···H(34)ix3.563H(35)···Pt(1)iv3.571
H(7)···H(9)ix2.989H(35)···P(2)iv3.584
H(7)···H(14)ix3.107H(35)···O(4)iv3.567
H(7)···H(27)vii3.151H(35)···O(6)iv3.185
H(7)···H(28)vii3.399H(35)···C(7)iv3.525
H(8)···H(25)i3.106H(35)···C(8)iv3.369
H(9)···C(3)ix3.526H(35)···C(18)iv3.510
H(9)···C(14)ix3.453H(35)···H(15)iv2.797
H(9)···H(5)ix3.402H(35)···H(17)iv3.139
H(9)···H(7)ix2.989H(35)···H(18)iv3.018
H(9)···H(26)x3.390H(35)···H(40)iv2.932
H(9)···H(28)xi3.454H(35)···H(42)iv3.335
H(9)···H(31)ix2.663H(36)···H(19)iii2.880
H(9)···H(32)ix3.403H(36)···H(21)iii3.595
H(10)···C(12)x3.574H(37)···H(27)vii3.318
H(10)···C(14)i3.262H(37)···H(37)viii3.023
H(10)···H(26)x2.928H(37)···H(38)viii3.544
H(10)···H(27)x3.541H(37)···H(41)viii3.520
H(10)···H(28)xi3.201H(37)···H(42)viii3.056
H(10)···H(30)i2.971H(38)···C(9)iii3.447
H(10)···H(31)ix3.348H(38)···H(4)viii3.484
H(10)···H(32)i2.718H(38)···H(19)iii3.233
H(11)···Cl(1)x3.162H(38)···H(21)iii2.791
H(11)···H(26)x2.748H(38)···H(27)vii3.323
H(11)···H(31)ix3.390H(38)···H(37)viii3.544
H(12)···C(9)iv3.277H(38)···H(42)viii3.542
H(12)···H(19)iv2.981H(39)···C(12)vii3.582
H(12)···H(20)iv2.693H(39)···H(27)vii2.675
H(12)···H(23)xi3.457H(40)···C(6)xii3.542
H(12)···H(40)xi3.425H(40)···C(11)ii3.285
H(12)···H(41)xi3.390H(40)···H(12)xii3.425
H(13)···C(12)xi3.519H(40)···H(13)xii2.787
H(13)···C(18)xi3.538H(40)···H(22)ii3.269
H(13)···H(23)xi3.010H(40)···H(24)ii2.879
H(13)···H(25)i3.455H(40)···H(25)ii2.933
H(13)···H(28)xi2.603H(40)···H(30)ii3.031
H(13)···H(30)i2.766H(40)···H(35)ii2.932
H(13)···H(40)xi2.787H(41)···C(2)viii3.076
H(13)···H(41)xi3.501H(41)···C(9)iii3.199
H(14)···C(3)ix3.383H(41)···C(11)ii3.543
H(14)···H(6)ix2.849H(41)···H(2)viii2.905
H(14)···H(7)ix3.107H(41)···H(3)viii2.821
H(14)···H(23)xi2.801H(41)···H(4)viii2.978
H(14)···H(28)xi2.862H(41)···H(12)xii3.390
H(15)···C(15)ii2.759H(41)···H(13)xii3.501
H(15)···H(33)ii2.448H(41)···H(19)iii2.992
H(15)···H(34)ii2.572H(41)···H(20)iii3.034
H(15)···H(35)ii2.797H(41)···H(21)iii3.024
H(16)···C(8)vi3.382H(41)···H(24)ii2.747
H(16)···C(9)vi3.475H(41)···H(25)ii3.554
H(16)···H(16)vi2.508H(41)···H(37)viii3.520
H(16)···H(21)vi2.635H(42)···C(10)ii3.489
H(17)···Cl(1)ii2.893H(42)···C(11)ii3.416
H(17)···C(15)ii3.369H(42)···H(2)viii3.302
H(17)···H(22)ii3.309H(42)···H(22)ii2.845
H(17)···H(33)ii2.734H(42)···H(24)ii2.839
H(17)···H(35)ii3.139H(42)···H(25)ii3.497
H(18)···C(15)ii3.591H(42)···H(35)ii3.335
H(18)···H(33)ii3.358H(42)···H(37)viii3.056
H(18)···H(35)ii3.018H(42)···H(38)viii3.542
H(19)···C(16)i3.510
Cl(1)—Pt(1)—Cl(2)87.18 (2)C(4)—C(6)—H(12)109.5
Cl(1)—Pt(1)—P(1)171.35 (2)C(4)—C(6)—H(13)109.5
Cl(1)—Pt(1)—P(2)90.80 (2)C(4)—C(6)—H(14)109.5
Cl(2)—Pt(1)—P(1)85.34 (2)H(12)—C(6)—H(13)109.5
Cl(2)—Pt(1)—P(2)175.09 (3)H(12)—C(6)—H(14)109.5
P(1)—Pt(1)—P(2)96.99 (3)H(13)—C(6)—H(14)109.5
Pt(1)—P(1)—O(1)115.04 (8)O(3)—C(7)—H(15)109.0
Pt(1)—P(1)—O(2)114.47 (8)C(8)—C(7)—H(15)109.0
Pt(1)—P(1)—O(3)115.43 (8)C(9)—C(7)—H(15)109.0
O(1)—P(1)—O(2)100.50 (11)C(7)—C(8)—H(16)109.5
O(1)—P(1)—O(3)107.34 (12)C(7)—C(8)—H(17)109.5
O(2)—P(1)—O(3)102.31 (12)C(7)—C(8)—H(18)109.5
Pt(1)—P(2)—O(4)116.80 (8)H(16)—C(8)—H(17)109.5
Pt(1)—P(2)—O(5)117.90 (8)H(16)—C(8)—H(18)109.5
Pt(1)—P(2)—O(6)110.65 (9)H(17)—C(8)—H(18)109.5
O(4)—P(2)—O(5)101.20 (12)C(7)—C(9)—H(19)109.5
O(4)—P(2)—O(6)100.33 (10)C(7)—C(9)—H(20)109.5
O(5)—P(2)—O(6)108.15 (12)C(7)—C(9)—H(21)109.5
P(1)—O(1)—C(1)120.80 (19)H(19)—C(9)—H(20)109.5
P(1)—O(2)—C(4)127.4 (2)H(19)—C(9)—H(21)109.5
P(1)—O(3)—C(7)122.4 (2)H(20)—C(9)—H(21)109.5
P(2)—O(4)—C(10)125.05 (18)O(4)—C(10)—H(22)109.9
P(2)—O(5)—C(13)126.2 (2)C(11)—C(10)—H(22)109.9
P(2)—O(6)—C(16)121.6 (2)C(12)—C(10)—H(22)109.9
O(1)—C(1)—C(2)107.3 (2)C(10)—C(11)—H(23)109.5
O(1)—C(1)—C(3)108.2 (2)C(10)—C(11)—H(24)109.5
C(2)—C(1)—C(3)113.1 (3)C(10)—C(11)—H(25)109.5
O(2)—C(4)—C(5)106.3 (2)H(23)—C(11)—H(24)109.5
O(2)—C(4)—C(6)107.0 (3)H(23)—C(11)—H(25)109.5
C(5)—C(4)—C(6)113.1 (3)H(24)—C(11)—H(25)109.5
O(3)—C(7)—C(8)109.3 (2)C(10)—C(12)—H(26)109.5
O(3)—C(7)—C(9)105.9 (2)C(10)—C(12)—H(27)109.5
C(8)—C(7)—C(9)114.4 (3)C(10)—C(12)—H(28)109.5
O(4)—C(10)—C(11)107.7 (2)H(26)—C(12)—H(27)109.5
O(4)—C(10)—C(12)107.0 (2)H(26)—C(12)—H(28)109.5
C(11)—C(10)—C(12)112.3 (2)H(27)—C(12)—H(28)109.5
O(5)—C(13)—C(14)106.6 (2)O(5)—C(13)—H(29)109.3
O(5)—C(13)—C(15)109.9 (2)C(14)—C(13)—H(29)109.4
C(14)—C(13)—C(15)112.3 (3)C(15)—C(13)—H(29)109.3
O(6)—C(16)—C(17)108.1 (2)C(13)—C(14)—H(30)109.5
O(6)—C(16)—C(18)107.1 (3)C(13)—C(14)—H(31)109.5
C(17)—C(16)—C(18)114.2 (3)C(13)—C(14)—H(32)109.5
O(1)—C(1)—H(1)109.4H(30)—C(14)—H(31)109.5
C(2)—C(1)—H(1)109.4H(30)—C(14)—H(32)109.5
C(3)—C(1)—H(1)109.4H(31)—C(14)—H(32)109.5
C(1)—C(2)—H(2)109.5C(13)—C(15)—H(33)109.5
C(1)—C(2)—H(3)109.5C(13)—C(15)—H(34)109.5
C(1)—C(2)—H(4)109.5C(13)—C(15)—H(35)109.5
H(2)—C(2)—H(3)109.5H(33)—C(15)—H(34)109.5
H(2)—C(2)—H(4)109.5H(33)—C(15)—H(35)109.5
H(3)—C(2)—H(4)109.5H(34)—C(15)—H(35)109.5
C(1)—C(3)—H(5)109.5O(6)—C(16)—H(36)109.1
C(1)—C(3)—H(6)109.5C(17)—C(16)—H(36)109.1
C(1)—C(3)—H(7)109.5C(18)—C(16)—H(36)109.1
H(5)—C(3)—H(6)109.5C(16)—C(17)—H(37)109.5
H(5)—C(3)—H(7)109.5C(16)—C(17)—H(38)109.5
H(6)—C(3)—H(7)109.5C(16)—C(17)—H(39)109.5
O(2)—C(4)—H(8)110.1H(37)—C(17)—H(38)109.5
C(5)—C(4)—H(8)110.1H(37)—C(17)—H(39)109.5
C(6)—C(4)—H(8)110.1H(38)—C(17)—H(39)109.5
C(4)—C(5)—H(9)109.5C(16)—C(18)—H(40)109.5
C(4)—C(5)—H(10)109.5C(16)—C(18)—H(41)109.5
C(4)—C(5)—H(11)109.5C(16)—C(18)—H(42)109.5
H(9)—C(5)—H(10)109.5H(40)—C(18)—H(41)109.5
H(9)—C(5)—H(11)109.5H(40)—C(18)—H(42)109.5
H(10)—C(5)—H(11)109.5H(41)—C(18)—H(42)109.5
Cl(1)—Pt(1)—P(2)—O(4)21.21 (10)Pt(1)—P(2)—O(4)—C(10)−93.9 (2)
Cl(1)—Pt(1)—P(2)—O(5)−99.70 (10)Pt(1)—P(2)—O(5)—C(13)−25.7 (2)
Cl(1)—Pt(1)—P(2)—O(6)135.11 (9)Pt(1)—P(2)—O(6)—C(16)−172.06 (19)
Cl(2)—Pt(1)—P(1)—O(1)179.48 (10)O(4)—P(2)—O(5)—C(13)−154.4 (2)
Cl(2)—Pt(1)—P(1)—O(2)63.79 (11)O(5)—P(2)—O(4)—C(10)35.4 (2)
Cl(2)—Pt(1)—P(1)—O(3)−54.62 (9)O(4)—P(2)—O(6)—C(16)−48.1 (2)
P(1)—Pt(1)—P(2)—O(4)−162.57 (9)O(6)—P(2)—O(4)—C(10)146.5 (2)
P(1)—Pt(1)—P(2)—O(5)76.52 (10)O(5)—P(2)—O(6)—C(16)57.4 (2)
P(1)—Pt(1)—P(2)—O(6)−48.67 (9)O(6)—P(2)—O(5)—C(13)100.7 (2)
P(2)—Pt(1)—P(1)—O(1)−4.85 (10)P(1)—O(1)—C(1)—C(2)−129.3 (2)
P(2)—Pt(1)—P(1)—O(2)−120.55 (11)P(1)—O(1)—C(1)—C(3)108.3 (2)
P(2)—Pt(1)—P(1)—O(3)121.04 (9)P(1)—O(2)—C(4)—C(5)−115.5 (3)
Pt(1)—P(1)—O(1)—C(1)−176.87 (19)P(1)—O(2)—C(4)—C(6)123.5 (2)
Pt(1)—P(1)—O(2)—C(4)−86.4 (2)P(1)—O(3)—C(7)—C(8)−87.0 (3)
Pt(1)—P(1)—O(3)—C(7)−31.2 (2)P(1)—O(3)—C(7)—C(9)149.3 (2)
O(1)—P(1)—O(2)—C(4)149.7 (2)P(2)—O(4)—C(10)—C(11)−94.7 (2)
O(2)—P(1)—O(1)—C(1)−53.4 (2)P(2)—O(4)—C(10)—C(12)144.3 (2)
O(1)—P(1)—O(3)—C(7)98.5 (2)P(2)—O(5)—C(13)—C(14)−153.8 (2)
O(3)—P(1)—O(1)—C(1)53.2 (2)P(2)—O(5)—C(13)—C(15)84.3 (3)
O(2)—P(1)—O(3)—C(7)−156.2 (2)P(2)—O(6)—C(16)—C(17)−114.9 (3)
O(3)—P(1)—O(2)—C(4)39.2 (2)P(2)—O(6)—C(16)—C(18)121.6 (2)

Symmetry codes: (i) x−1, y, z; (ii) x, −y+1/2, z+1/2; (iii) x+1, y, z; (iv) x, −y+1/2, z−1/2; (v) −x, y+1/2, −z+1/2; (vi) −x, −y, −z+1; (vii) −x+1, y−1/2, −z+1/2; (viii) −x+1, −y, −z+1; (ix) −x, −y, −z; (x) −x, y−1/2, −z+1/2; (xi) x−1, −y+1/2, z−1/2; (xii) x+1, −y+1/2, z+1/2; (xiii) −x+1, y+1/2, −z+1/2.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: FI2086).

References

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