Abstract
The title complex, [PtCl2(C18H40P2)], contains a PtII center in an approximately square-planar geometry [cis angle range = 88.09 (3)–91.39 (3)°; twist angle = 1.19 (5)°]. The Pt—P bond lengths of 2.2536 (8) and 2.2513 (8) Å and the Pt—Cl bond lengths of 2.3750 (8) and 2.3588 (8) Å are normal. This crystal form is a polymorph of a structure reported previously [Harada, Kai, Yasuoka & Kasai (1976 ▶). Bull. Chem. Soc. Jpn, 49, 3472–3477].
Related literature
For related literature, see: Crascall & Spencer (1990 ▶); Green et al. (1977 ▶); McDermott et al. (1976 ▶); Ogoshi et al. (2004 ▶).
Experimental
Crystal data
[PtCl2(C18H40P2)]
M r = 584.43
Monoclinic,
a = 11.0981 (10) Å
b = 15.3242 (13) Å
c = 14.5413 (13) Å
β = 109.287 (1)°
V = 2334.2 (4) Å3
Z = 4
Mo Kα radiation
μ = 6.38 mm−1
T = 100.0 (1) K
0.20 × 0.14 × 0.08 mm
Data collection
Bruker SMART APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 2007 ▶) T min = 0.342, T max = 0.600
20415 measured reflections
8022 independent reflections
6312 reflections with I > 2σ(I)
R int = 0.034
Refinement
R[F 2 > 2σ(F 2)] = 0.029
wR(F 2) = 0.060
S = 1.01
8022 reflections
208 parameters
H-atom parameters constrained
Δρmax = 1.11 e Å−3
Δρmin = −0.81 e Å−3
Data collection: APEX2 (Bruker, 2006 ▶); cell refinement: SAINT (Bruker, 2006 ▶); data reduction: SAINT; program(s) used to solve structure: SIR97 (Altomare et al., 1999 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Bruker, 2000 ▶); software used to prepare material for publication: SHELXTL.
Supplementary Material
Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808000603/pv2062sup1.cif
Structure factors: contains datablocks I. DOI: 10.1107/S1600536808000603/pv2062Isup2.hkl
Additional supplementary materials: crystallographic information; 3D view; checkCIF report
Table 1. Selected geometric parameters (Å, °).
| Pt1—P2 | 2.2513 (8) |
| Pt1—P1 | 2.2536 (8) |
| Pt1—Cl2 | 2.3588 (8) |
| Pt1—Cl1 | 2.3750 (8) |
| P2—Pt1—P1 | 89.70 (3) |
| P2—Pt1—Cl2 | 90.82 (3) |
| P1—Pt1—Cl2 | 178.77 (3) |
| P2—Pt1—Cl1 | 178.84 (3) |
| P1—Pt1—Cl1 | 91.39 (3) |
| Cl2—Pt1—Cl1 | 88.09 (3) |
Acknowledgments
We thank the US Department of Energy for support (grant FG02–86ER13569).
supplementary crystallographic information
Comment
One of the most commonly used Pt(0) precursors, Pt(COD)2, COD = 1,5-cyclooctadiene, is generally synthesized by the reduction of platinumdichlorides, like Pt(COD)Cl2, with Li2(COT), COT = cyclooctatetraene (Green et al., 1977; Crascall & Spencer, 1990), or with SmI2 (Ogoshi et al., 2004). The latter reduction with 20 equivalents of SmI2 afforded Pt(COD)2 in moderate yields (45% average). After addition of chelating ligand 1,2-bis(di-tert-butylphosphino)ethane (dtbpe) to the SmI2 reduction product, it was observed that some PtII remained, based on the formation of the title compound, Pt(dtbpe)Cl2 (I). An independent synthesis of (I) was performed to support these observations, in which dtbpe was added directly to Pt(COD)Cl2 (see experimental section). The resulting pure product in 88% yield was characterized by 1H, 13C, 31P NMR spectroscopies and by single-crystal X-ray diffraction.
Experimental
Pt(COD)Cl2, COD = 1,5-cyclooctadiene, was synthesized according to the published procedure (McDermott et al., 1976). Under an atmosphere of dinitrogen, bis(di-tert-butylphosphino)ethane (dtbpe) (212 mg, 0.67 mmol) was added to a light yellow suspension of Pt(COD)Cl2 (250 mg, 0.67 mmol) in THF (25 ml). The reaction mixture was heated with stirring for 12 h at 373 K. After complete conversion to (I) was verified by 31P NMR spectroscopy, the volatiles (THF, COD) were removed in vacuo, leaving the white powdery product (343.4 mg, 0.59 mmol) in 88% yield. Crystals of (I) were grown by vapor diffusion of hexanes into THF.
Refinement
The H-atoms were included in the refinements at geometrically idealized positions with C—H distances 0.98 and 0.99 Å for CH3 and CH2 type H-atoms, respectively; Uiso values were 1.5Ueq and 1.2Ueq of the carrier atoms for the methyl and CH2 groups, respectively. The final difference map showed a residual electron density in the vicinity of H31A atom and was chemically meaningless.
Figures
Fig. 1.
Displacement ellipsoid (50% probability) drawing of (I) with H atoms omitted.
Crystal data
| [PtCl2(C18H40P2)] | F000 = 1160 |
| Mr = 584.43 | Dx = 1.663 Mg m−3 |
| Monoclinic, P21/n | Mo Kα radiation λ = 0.71073 Å |
| Hall symbol: -P 2yn | Cell parameters from 4040 reflections |
| a = 11.0981 (10) Å | θ = 3.0–32.9º |
| b = 15.3242 (13) Å | µ = 6.38 mm−1 |
| c = 14.5413 (13) Å | T = 100.0 (1) K |
| β = 109.287 (1)º | Block, colorless |
| V = 2334.2 (4) Å3 | 0.20 × 0.14 × 0.08 mm |
| Z = 4 |
Data collection
| Bruker SMART APEXII CCD diffractometer | 8022 independent reflections |
| Radiation source: fine-focus sealed tube | 6312 reflections with I > 2σ(I) |
| Monochromator: graphite | Rint = 0.034 |
| T = 100.0(1) K | θmax = 32.0º |
| area detector, ω scans per φ | θmin = 2.0º |
| Absorption correction: multi-scan(SADABS; Sheldrick, 2007) | h = −15→16 |
| Tmin = 0.342, Tmax = 0.600 | k = −22→22 |
| 20415 measured reflections | l = −19→21 |
Refinement
| Refinement on F2 | Secondary atom site location: difference Fourier map |
| Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
| R[F2 > 2σ(F2)] = 0.029 | H-atom parameters constrained |
| wR(F2) = 0.060 | w = 1/[σ2(Fo2) + (0.0232P)2] where P = (Fo2 + 2Fc2)/3 |
| S = 1.02 | (Δ/σ)max = 0.002 |
| 8022 reflections | Δρmax = 1.11 e Å−3 |
| 208 parameters | Δρmin = −0.81 e Å−3 |
| Primary atom site location: structure-invariant direct methods | Extinction correction: none |
Special details
| Experimental. 1H NMR (CDCl3, 20 °C): δ 1.5 (d, 3JHP = 14.1 Hz, 36 H, -(CH3)3), 1.9 (d, 2JHP = 16 Hz, 4 H, -CH2-); 13C NMR (CDCl3, 20 °C): δ 24.5 (d, 1JCP = 33 Hz, -CH2-), 30.4 (s, -(CH3)3), 37.6 (d, 1JCP = 30 Hz, -C-); 31P NMR (CDCl3, 20 °C): δ 75.7 (s, with platinum satellites 1JPPt = 3643.2 Hz). |
| 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 takeninto account individually in the estimation of e.s.d.'s in distances, anglesand torsion angles; correlations between e.s.d.'s in cell parameters are onlyused 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 andgoodness of fit S are based on F2, conventional R-factors R are basedon F, with F set to zero for negative F2. The threshold expression ofF2 > σ(F2) is used only for calculating R-factors(gt) etc. and isnot relevant to the choice of reflections for refinement. R-factors basedon 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)
| x | y | z | Uiso*/Ueq | ||
| Pt1 | 0.268368 (10) | 0.706474 (7) | 0.781256 (8) | 0.01505 (3) | |
| Cl1 | 0.17379 (7) | 0.80168 (5) | 0.86681 (6) | 0.02422 (16) | |
| Cl2 | 0.44219 (8) | 0.80401 (5) | 0.81687 (6) | 0.02415 (16) | |
| P1 | 0.09956 (7) | 0.61552 (5) | 0.74524 (5) | 0.01603 (14) | |
| P2 | 0.36188 (7) | 0.61746 (5) | 0.70173 (6) | 0.01776 (15) | |
| C1 | 0.0577 (3) | 0.5718 (2) | 0.8529 (2) | 0.0227 (6) | |
| C2 | −0.0053 (4) | 0.4814 (2) | 0.8323 (3) | 0.0323 (8) | |
| H2A | −0.0253 | 0.4613 | 0.8896 | 0.048* | |
| H2B | 0.0533 | 0.4400 | 0.8177 | 0.048* | |
| H2C | −0.0842 | 0.4851 | 0.7763 | 0.048* | |
| C3 | −0.0326 (3) | 0.6333 (2) | 0.8823 (3) | 0.0287 (7) | |
| H3A | −0.0520 | 0.6085 | 0.9380 | 0.043* | |
| H3B | −0.1120 | 0.6402 | 0.8273 | 0.043* | |
| H3C | 0.0083 | 0.6903 | 0.9002 | 0.043* | |
| C4 | 0.1821 (3) | 0.5634 (2) | 0.9392 (2) | 0.0308 (8) | |
| H4A | 0.1632 | 0.5409 | 0.9960 | 0.046* | |
| H4B | 0.2227 | 0.6208 | 0.9547 | 0.046* | |
| H4C | 0.2400 | 0.5231 | 0.9221 | 0.046* | |
| C5 | −0.0478 (3) | 0.6578 (2) | 0.6491 (2) | 0.0232 (7) | |
| C6 | −0.1592 (3) | 0.5927 (2) | 0.6247 (3) | 0.0302 (8) | |
| H6A | −0.2334 | 0.6177 | 0.5744 | 0.045* | |
| H6B | −0.1812 | 0.5807 | 0.6834 | 0.045* | |
| H6C | −0.1342 | 0.5383 | 0.6006 | 0.045* | |
| C7 | −0.0919 (3) | 0.7459 (2) | 0.6749 (3) | 0.0316 (8) | |
| H7A | −0.1686 | 0.7645 | 0.6224 | 0.047* | |
| H7B | −0.0240 | 0.7891 | 0.6833 | 0.047* | |
| H7C | −0.1113 | 0.7406 | 0.7357 | 0.047* | |
| C8 | −0.0127 (3) | 0.6711 (3) | 0.5569 (3) | 0.0388 (9) | |
| H8A | −0.0871 | 0.6932 | 0.5046 | 0.058* | |
| H8B | 0.0143 | 0.6154 | 0.5370 | 0.058* | |
| H8C | 0.0573 | 0.7133 | 0.5700 | 0.058* | |
| C9 | 0.5007 (3) | 0.5527 (2) | 0.7849 (2) | 0.0246 (7) | |
| C10 | 0.5670 (4) | 0.4957 (2) | 0.7285 (3) | 0.0349 (9) | |
| H10A | 0.6377 | 0.4637 | 0.7747 | 0.052* | |
| H10B | 0.5999 | 0.5329 | 0.6874 | 0.052* | |
| H10C | 0.5053 | 0.4541 | 0.6874 | 0.052* | |
| C11 | 0.5985 (3) | 0.6126 (2) | 0.8564 (3) | 0.0340 (8) | |
| H11A | 0.6690 | 0.5774 | 0.8984 | 0.051* | |
| H11B | 0.5573 | 0.6440 | 0.8967 | 0.051* | |
| H11C | 0.6317 | 0.6546 | 0.8199 | 0.051* | |
| C12 | 0.4469 (3) | 0.4907 (2) | 0.8451 (3) | 0.0298 (8) | |
| H12A | 0.5166 | 0.4561 | 0.8890 | 0.045* | |
| H12B | 0.3840 | 0.4516 | 0.8011 | 0.045* | |
| H12C | 0.4058 | 0.5249 | 0.8834 | 0.045* | |
| C13 | 0.4076 (3) | 0.6704 (2) | 0.5996 (2) | 0.0241 (7) | |
| C14 | 0.5394 (3) | 0.7143 (2) | 0.6356 (3) | 0.0292 (7) | |
| H14A | 0.5579 | 0.7404 | 0.5802 | 0.044* | |
| H14B | 0.6046 | 0.6707 | 0.6667 | 0.044* | |
| H14C | 0.5396 | 0.7600 | 0.6829 | 0.044* | |
| C15 | 0.4083 (4) | 0.6035 (2) | 0.5199 (3) | 0.0374 (9) | |
| H15A | 0.4322 | 0.6329 | 0.4687 | 0.056* | |
| H15B | 0.3230 | 0.5780 | 0.4919 | 0.056* | |
| H15C | 0.4702 | 0.5572 | 0.5489 | 0.056* | |
| C16 | 0.3071 (3) | 0.7402 (2) | 0.5518 (3) | 0.0286 (7) | |
| H16A | 0.3286 | 0.7684 | 0.4988 | 0.043* | |
| H16B | 0.3055 | 0.7839 | 0.6006 | 0.043* | |
| H16C | 0.2229 | 0.7126 | 0.5256 | 0.043* | |
| C31 | 0.1465 (3) | 0.5180 (2) | 0.6924 (2) | 0.0216 (6) | |
| H31A | 0.1853 | 0.4755 | 0.7452 | 0.026* | |
| H31B | 0.0690 | 0.4908 | 0.6465 | 0.026* | |
| C32 | 0.2411 (3) | 0.5363 (2) | 0.6385 (2) | 0.0211 (6) | |
| H32A | 0.1938 | 0.5577 | 0.5721 | 0.025* | |
| H32B | 0.2842 | 0.4813 | 0.6320 | 0.025* |
Atomic displacement parameters (Å2)
| U11 | U22 | U33 | U12 | U13 | U23 | |
| Pt1 | 0.01739 (5) | 0.01316 (5) | 0.01369 (5) | 0.00118 (5) | 0.00389 (4) | −0.00008 (4) |
| Cl1 | 0.0232 (4) | 0.0226 (4) | 0.0254 (4) | 0.0034 (3) | 0.0061 (3) | −0.0079 (3) |
| Cl2 | 0.0275 (4) | 0.0195 (4) | 0.0271 (4) | −0.0052 (3) | 0.0112 (3) | −0.0035 (3) |
| P1 | 0.0182 (4) | 0.0177 (4) | 0.0132 (3) | −0.0006 (3) | 0.0066 (3) | −0.0002 (3) |
| P2 | 0.0202 (4) | 0.0158 (4) | 0.0199 (4) | −0.0004 (3) | 0.0102 (3) | −0.0011 (3) |
| C1 | 0.0277 (16) | 0.0264 (16) | 0.0185 (15) | 0.0043 (13) | 0.0137 (13) | 0.0043 (12) |
| C2 | 0.046 (2) | 0.0275 (18) | 0.0333 (19) | −0.0032 (16) | 0.0261 (17) | 0.0057 (15) |
| C3 | 0.0365 (19) | 0.0297 (18) | 0.0269 (17) | 0.0024 (15) | 0.0201 (15) | 0.0022 (14) |
| C4 | 0.0348 (19) | 0.041 (2) | 0.0186 (16) | 0.0045 (16) | 0.0116 (14) | 0.0099 (15) |
| C5 | 0.0185 (15) | 0.0330 (18) | 0.0165 (15) | −0.0029 (13) | 0.0034 (12) | 0.0040 (13) |
| C6 | 0.0208 (16) | 0.037 (2) | 0.0302 (19) | −0.0070 (14) | 0.0053 (14) | −0.0058 (15) |
| C7 | 0.0222 (17) | 0.0323 (19) | 0.034 (2) | 0.0028 (14) | 0.0009 (15) | 0.0085 (16) |
| C8 | 0.0208 (17) | 0.071 (3) | 0.0212 (18) | −0.0038 (17) | 0.0018 (14) | 0.0117 (18) |
| C9 | 0.0239 (16) | 0.0186 (15) | 0.0326 (18) | 0.0045 (12) | 0.0109 (14) | 0.0015 (13) |
| C10 | 0.0326 (19) | 0.0228 (17) | 0.056 (2) | 0.0042 (15) | 0.0233 (18) | −0.0002 (16) |
| C11 | 0.0236 (17) | 0.0309 (18) | 0.041 (2) | 0.0022 (15) | 0.0021 (15) | 0.0048 (16) |
| C12 | 0.0287 (18) | 0.0263 (17) | 0.036 (2) | 0.0079 (14) | 0.0126 (15) | 0.0104 (15) |
| C13 | 0.0296 (17) | 0.0250 (16) | 0.0238 (17) | −0.0025 (14) | 0.0172 (14) | −0.0011 (13) |
| C14 | 0.0272 (17) | 0.0292 (18) | 0.0363 (19) | 0.0001 (14) | 0.0173 (15) | 0.0008 (15) |
| C15 | 0.050 (2) | 0.042 (2) | 0.0306 (19) | −0.0120 (19) | 0.0282 (18) | −0.0071 (17) |
| C16 | 0.0315 (18) | 0.0327 (18) | 0.0255 (18) | −0.0035 (15) | 0.0148 (15) | 0.0084 (14) |
| C31 | 0.0270 (16) | 0.0180 (15) | 0.0243 (16) | −0.0022 (12) | 0.0144 (13) | −0.0048 (12) |
| C32 | 0.0244 (15) | 0.0202 (15) | 0.0221 (15) | −0.0033 (12) | 0.0125 (12) | −0.0046 (12) |
Geometric parameters (Å, °)
| Pt1—P2 | 2.2513 (8) | C8—H8B | 0.9800 |
| Pt1—P1 | 2.2536 (8) | C8—H8C | 0.9800 |
| Pt1—Cl2 | 2.3588 (8) | C9—C11 | 1.535 (5) |
| Pt1—Cl1 | 2.3750 (8) | C9—C10 | 1.542 (5) |
| P1—C31 | 1.833 (3) | C9—C12 | 1.540 (5) |
| P1—C5 | 1.881 (3) | C10—H10A | 0.9800 |
| P1—C1 | 1.897 (3) | C10—H10B | 0.9800 |
| P2—C32 | 1.837 (3) | C10—H10C | 0.9800 |
| P2—C9 | 1.895 (3) | C11—H11A | 0.9800 |
| P2—C13 | 1.903 (3) | C11—H11B | 0.9800 |
| C1—C4 | 1.534 (5) | C11—H11C | 0.9800 |
| C1—C3 | 1.535 (4) | C12—H12A | 0.9800 |
| C1—C2 | 1.537 (5) | C12—H12B | 0.9800 |
| C2—H2A | 0.9800 | C12—H12C | 0.9800 |
| C2—H2B | 0.9800 | C13—C16 | 1.536 (5) |
| C2—H2C | 0.9800 | C13—C14 | 1.536 (5) |
| C3—H3A | 0.9800 | C13—C15 | 1.549 (5) |
| C3—H3B | 0.9800 | C14—H14A | 0.9800 |
| C3—H3C | 0.9800 | C14—H14B | 0.9800 |
| C4—H4A | 0.9800 | C14—H14C | 0.9800 |
| C4—H4B | 0.9800 | C15—H15A | 0.9800 |
| C4—H4C | 0.9800 | C15—H15B | 0.9800 |
| C5—C7 | 1.525 (5) | C15—H15C | 0.9800 |
| C5—C8 | 1.528 (5) | C16—H16A | 0.9800 |
| C5—C6 | 1.536 (4) | C16—H16B | 0.9800 |
| C6—H6A | 0.9800 | C16—H16C | 0.9800 |
| C6—H6B | 0.9800 | C31—C32 | 1.529 (4) |
| C6—H6C | 0.9800 | C31—H31A | 0.9900 |
| C7—H7A | 0.9800 | C31—H31B | 0.9900 |
| C7—H7B | 0.9800 | C32—H32A | 0.9900 |
| C7—H7C | 0.9800 | C32—H32B | 0.9900 |
| C8—H8A | 0.9800 | ||
| P2—Pt1—P1 | 89.70 (3) | C5—C8—H8C | 109.5 |
| P2—Pt1—Cl2 | 90.82 (3) | H8A—C8—H8C | 109.5 |
| P1—Pt1—Cl2 | 178.77 (3) | H8B—C8—H8C | 109.5 |
| P2—Pt1—Cl1 | 178.84 (3) | C11—C9—C10 | 110.2 (3) |
| P1—Pt1—Cl1 | 91.39 (3) | C11—C9—C12 | 107.7 (3) |
| Cl2—Pt1—Cl1 | 88.09 (3) | C10—C9—C12 | 107.1 (3) |
| C31—P1—C5 | 105.46 (15) | C11—C9—P2 | 111.3 (2) |
| C31—P1—C1 | 103.85 (14) | C10—C9—P2 | 112.8 (2) |
| C5—P1—C1 | 110.23 (14) | C12—C9—P2 | 107.4 (2) |
| C31—P1—Pt1 | 105.77 (10) | C9—C10—H10A | 109.5 |
| C5—P1—Pt1 | 114.31 (11) | C9—C10—H10B | 109.5 |
| C1—P1—Pt1 | 115.98 (11) | H10A—C10—H10B | 109.5 |
| C32—P2—C9 | 105.70 (15) | C9—C10—H10C | 109.5 |
| C32—P2—C13 | 103.69 (14) | H10A—C10—H10C | 109.5 |
| C9—P2—C13 | 110.56 (15) | H10B—C10—H10C | 109.5 |
| C32—P2—Pt1 | 106.44 (10) | C9—C11—H11A | 109.5 |
| C9—P2—Pt1 | 113.88 (11) | C9—C11—H11B | 109.5 |
| C13—P2—Pt1 | 115.45 (11) | H11A—C11—H11B | 109.5 |
| C4—C1—C3 | 108.6 (3) | C9—C11—H11C | 109.5 |
| C4—C1—C2 | 108.2 (3) | H11A—C11—H11C | 109.5 |
| C3—C1—C2 | 108.1 (3) | H11B—C11—H11C | 109.5 |
| C4—C1—P1 | 107.8 (2) | C9—C12—H12A | 109.5 |
| C3—C1—P1 | 111.9 (2) | C9—C12—H12B | 109.5 |
| C2—C1—P1 | 112.1 (2) | H12A—C12—H12B | 109.5 |
| C1—C2—H2A | 109.5 | C9—C12—H12C | 109.5 |
| C1—C2—H2B | 109.5 | H12A—C12—H12C | 109.5 |
| H2A—C2—H2B | 109.5 | H12B—C12—H12C | 109.5 |
| C1—C2—H2C | 109.5 | C16—C13—C14 | 108.5 (3) |
| H2A—C2—H2C | 109.5 | C16—C13—C15 | 107.8 (3) |
| H2B—C2—H2C | 109.5 | C14—C13—C15 | 107.8 (3) |
| C1—C3—H3A | 109.5 | C16—C13—P2 | 107.9 (2) |
| C1—C3—H3B | 109.5 | C14—C13—P2 | 113.0 (2) |
| H3A—C3—H3B | 109.5 | C15—C13—P2 | 111.7 (2) |
| C1—C3—H3C | 109.5 | C13—C14—H14A | 109.5 |
| H3A—C3—H3C | 109.5 | C13—C14—H14B | 109.5 |
| H3B—C3—H3C | 109.5 | H14A—C14—H14B | 109.5 |
| C1—C4—H4A | 109.5 | C13—C14—H14C | 109.5 |
| C1—C4—H4B | 109.5 | H14A—C14—H14C | 109.5 |
| H4A—C4—H4B | 109.5 | H14B—C14—H14C | 109.5 |
| C1—C4—H4C | 109.5 | C13—C15—H15A | 109.5 |
| H4A—C4—H4C | 109.5 | C13—C15—H15B | 109.5 |
| H4B—C4—H4C | 109.5 | H15A—C15—H15B | 109.5 |
| C7—C5—C8 | 107.0 (3) | C13—C15—H15C | 109.5 |
| C7—C5—C6 | 109.4 (3) | H15A—C15—H15C | 109.5 |
| C8—C5—C6 | 107.7 (3) | H15B—C15—H15C | 109.5 |
| C7—C5—P1 | 113.1 (2) | C13—C16—H16A | 109.5 |
| C8—C5—P1 | 106.7 (2) | C13—C16—H16B | 109.5 |
| C6—C5—P1 | 112.6 (2) | H16A—C16—H16B | 109.5 |
| C5—C6—H6A | 109.5 | C13—C16—H16C | 109.5 |
| C5—C6—H6B | 109.5 | H16A—C16—H16C | 109.5 |
| H6A—C6—H6B | 109.5 | H16B—C16—H16C | 109.5 |
| C5—C6—H6C | 109.5 | C32—C31—P1 | 113.8 (2) |
| H6A—C6—H6C | 109.5 | C32—C31—H31A | 108.8 |
| H6B—C6—H6C | 109.5 | P1—C31—H31A | 108.8 |
| C5—C7—H7A | 109.5 | C32—C31—H31B | 108.8 |
| C5—C7—H7B | 109.5 | P1—C31—H31B | 108.8 |
| H7A—C7—H7B | 109.5 | H31A—C31—H31B | 107.7 |
| C5—C7—H7C | 109.5 | C31—C32—P2 | 112.3 (2) |
| H7A—C7—H7C | 109.5 | C31—C32—H32A | 109.2 |
| H7B—C7—H7C | 109.5 | P2—C32—H32A | 109.2 |
| C5—C8—H8A | 109.5 | C31—C32—H32B | 109.2 |
| C5—C8—H8B | 109.5 | P2—C32—H32B | 109.2 |
| H8A—C8—H8B | 109.5 | H32A—C32—H32B | 107.9 |
| P2—Pt1—P1—C31 | 8.74 (11) | C1—P1—C5—C6 | −48.9 (3) |
| Cl1—Pt1—P1—C31 | −170.88 (11) | Pt1—P1—C5—C6 | 178.4 (2) |
| P2—Pt1—P1—C5 | −106.82 (12) | C32—P2—C9—C11 | −169.3 (2) |
| Cl1—Pt1—P1—C5 | 73.55 (12) | C13—P2—C9—C11 | 79.1 (3) |
| P2—Pt1—P1—C1 | 123.22 (11) | Pt1—P2—C9—C11 | −52.8 (3) |
| Cl1—Pt1—P1—C1 | −56.40 (11) | C32—P2—C9—C10 | 66.3 (3) |
| P1—Pt1—P2—C32 | 9.20 (11) | C13—P2—C9—C10 | −45.3 (3) |
| Cl2—Pt1—P2—C32 | −169.68 (11) | Pt1—P2—C9—C10 | −177.3 (2) |
| P1—Pt1—P2—C9 | −106.85 (12) | C32—P2—C9—C12 | −51.6 (2) |
| Cl2—Pt1—P2—C9 | 74.27 (12) | C13—P2—C9—C12 | −163.2 (2) |
| P1—Pt1—P2—C13 | 123.65 (12) | Pt1—P2—C9—C12 | 64.9 (2) |
| Cl2—Pt1—P2—C13 | −55.24 (12) | C32—P2—C13—C16 | 81.9 (2) |
| C31—P1—C1—C4 | 83.6 (2) | C9—P2—C13—C16 | −165.2 (2) |
| C5—P1—C1—C4 | −163.8 (2) | Pt1—P2—C13—C16 | −34.1 (3) |
| Pt1—P1—C1—C4 | −31.9 (3) | C32—P2—C13—C14 | −158.1 (2) |
| C31—P1—C1—C3 | −157.1 (2) | C9—P2—C13—C14 | −45.2 (3) |
| C5—P1—C1—C3 | −44.5 (3) | Pt1—P2—C13—C14 | 85.9 (2) |
| Pt1—P1—C1—C3 | 87.4 (2) | C32—P2—C13—C15 | −36.4 (3) |
| C31—P1—C1—C2 | −35.4 (3) | C9—P2—C13—C15 | 76.5 (3) |
| C5—P1—C1—C2 | 77.2 (3) | Pt1—P2—C13—C15 | −152.4 (2) |
| Pt1—P1—C1—C2 | −151.0 (2) | C5—P1—C31—C32 | 91.5 (2) |
| C31—P1—C5—C7 | −172.7 (2) | C1—P1—C31—C32 | −152.5 (2) |
| C1—P1—C5—C7 | 75.7 (3) | Pt1—P1—C31—C32 | −30.0 (2) |
| Pt1—P1—C5—C7 | −57.0 (3) | P1—C31—C32—P2 | 39.6 (3) |
| C31—P1—C5—C8 | −55.3 (3) | C9—P2—C32—C31 | 91.6 (2) |
| C1—P1—C5—C8 | −166.8 (2) | C13—P2—C32—C31 | −152.0 (2) |
| Pt1—P1—C5—C8 | 60.4 (3) | Pt1—P2—C32—C31 | −29.8 (2) |
| C31—P1—C5—C6 | 62.6 (3) |
Footnotes
Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: PV2062).
References
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Associated Data
This section collects any data citations, data availability statements, or supplementary materials included in this article.
Supplementary Materials
Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808000603/pv2062sup1.cif
Structure factors: contains datablocks I. DOI: 10.1107/S1600536808000603/pv2062Isup2.hkl
Additional supplementary materials: crystallographic information; 3D view; checkCIF report

