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Acta Crystallographica Section E: Structure Reports Online logoLink to Acta Crystallographica Section E: Structure Reports Online
. 2008 Feb 6;64(Pt 3):m454. doi: 10.1107/S1600536808000603

A second polymorph of [1,2-bis­(di-tert-butyl­phosphino)ethane]dichlorido­platinum(II)

Ahmet Gunay a, William W Brennessel a, William D Jones a,*
PMCID: PMC2960814  PMID: 21201850

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).graphic file with name e-64-0m454-scheme1.jpg

Experimental

Crystal data

  • [PtCl2(C18H40P2)]

  • M r = 584.43

  • Monoclinic, Inline graphic

  • 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

e-64-0m454-sup1.cif (22.5KB, cif)

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808000603/pv2062Isup2.hkl

e-64-0m454-Isup2.hkl (392.5KB, 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.

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 m3
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 mm1
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 Å3
208 parameters Δρmin = −0.81 e Å3
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

e-64-0m454-sup1.cif (22.5KB, cif)

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808000603/pv2062Isup2.hkl

e-64-0m454-Isup2.hkl (392.5KB, hkl)

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


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