Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807059636/si2052sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807059636/si2052Isup2.hkl |
CCDC reference: 672721
The title compound was prepared by literature methods and subsequently isolated from dichloromethane/hexane as as a few small irregular red crystals following crystallization of the residue of its reaction mixture with SbPh3 in refluxing tetrachloroethane (Boag & Ravetz, 1995).
The hydrogen atoms were placed in calculated positions and allowed to ride on their respective atoms, with C—H = 0.97 Å and Uiso(H) = 1.2 Ueq(C).
Data collection: P3 Diffractometer Control Program (Siemens, 1990); cell refinement: XSCANS (Siemens, 1996); data reduction: XSCANS (Siemens, 1996); program(s) used to solve structure: SHELXTL-Plus (Sheldrick, 1995); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL-Plus (Sheldrick, 1995); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).
[Pt2Cl4(C2H4)2] | Z = 3 |
Mr = 588.06 | F(000) = 768 |
Triclinic, P1 | Dx = 3.845 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 6.6413 (8) Å | Cell parameters from 49 reflections |
b = 10.1222 (13) Å | θ = 7.3–15.3° |
c = 12.2397 (15) Å | µ = 28.49 mm−1 |
α = 87.23 (1)° | T = 293 K |
β = 75.462 (9)° | Irregular block, red |
γ = 73.142 (10)° | 0.20 × 0.10 × 0.10 mm |
V = 761.97 (16) Å3 |
Nicolet R3m/V diffractometer | 2740 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.039 |
Graphite monochromator | θmax = 27.6°, θmin = 2.1° |
intensity fitting of θ/2θ scans | h = 0→8 |
Absorption correction: ψ scan (XPREP; Siemens, 1995) | k = −12→13 |
Tmin = 0.150, Tmax = 0.954 | l = −15→15 |
3804 measured reflections | 3 standard reflections every 100 reflections |
3502 independent reflections | intensity decay: none |
Refinement on F2 | H-atom parameters constrained |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0717P)2 + 15.2811P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.054 | (Δ/σ)max < 0.001 |
wR(F2) = 0.140 | Δρmax = 3.86 e Å−3 |
S = 1.08 | Δρmin = −3.24 e Å−3 |
3502 reflections | Extinction correction: SHELXL97 (Sheldrick, 1997) |
137 parameters | Extinction coefficient: 0.0030 (3) |
0 restraints |
[Pt2Cl4(C2H4)2] | γ = 73.142 (10)° |
Mr = 588.06 | V = 761.97 (16) Å3 |
Triclinic, P1 | Z = 3 |
a = 6.6413 (8) Å | Mo Kα radiation |
b = 10.1222 (13) Å | µ = 28.49 mm−1 |
c = 12.2397 (15) Å | T = 293 K |
α = 87.23 (1)° | 0.20 × 0.10 × 0.10 mm |
β = 75.462 (9)° |
Nicolet R3m/V diffractometer | 2740 reflections with I > 2σ(I) |
Absorption correction: ψ scan (XPREP; Siemens, 1995) | Rint = 0.039 |
Tmin = 0.150, Tmax = 0.954 | 3 standard reflections every 100 reflections |
3804 measured reflections | intensity decay: none |
3502 independent reflections |
R[F2 > 2σ(F2)] = 0.054 | 0 restraints |
wR(F2) = 0.140 | H-atom parameters constrained |
S = 1.08 | w = 1/[σ2(Fo2) + (0.0717P)2 + 15.2811P] where P = (Fo2 + 2Fc2)/3 |
3502 reflections | Δρmax = 3.86 e Å−3 |
137 parameters | Δρmin = −3.24 e Å−3 |
Experimental. The few crystals isolated were not particularly well formed and showed evidence of not being single- a few spurious diffactions peaks and peaks showing shoulders. The final structure exhibits multiple unassigned electron density features within 1 Å of both the platinum and chlorine atoms. 10 reflections having 2θ between 12.82 and 32.77 degrees giving 360 ψ scans for parameter estimation |
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. Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) - 0.2484 (0.0142) x - 0.7140 (0.0203) y + 11.7169 (0.0078) z = 3.3733 (0.0090) * 0.0000 (0.0000) Pt2 * 0.0000 (0.0000) Cl23 * 0.0000 (0.0000) Cl32 Rms deviation of fitted atoms = 0.0000 0.1666 (0.0141) x + 2.7437 (0.0193) y + 11.3718 (0.0094) z = 3.7927 (0.0059) Angle to previous plane (with approximate e.s.d.) = 19.90 (0.13) * 0.0000 (0.0000) Pt3 * 0.0000 (0.0000) Cl23 * 0.0000 (0.0000) Cl32 Rms deviation of fitted atoms = 0.0000 - 0.0376 (0.0125) x + 1.0741 (0.0106) y + 11.7155 (0.0076) z = 3.9458 (0.0050) Angle to previous plane (with approximate e.s.d.) = 9.70 (0.14) * 0.0028 (0.0027) Pt2 * -0.0109 (0.0028) Pt3 * 0.3044 (0.0033) Cl2 * 0.3102 (0.0034) Cl3 * -0.3029 (0.0030) Cl23 * -0.3036 (0.0031) Cl32 Rms deviation of fitted atoms = 0.2493 - 0.1017 (0.0209) x + 0.7141 (0.0035) y + 11.7343 (0.0116) z = 11.6834 (0.0220) Angle to previous plane (with approximate e.s.d.) = 2.05 (0.16) * 0.0000 (0.0000) Pt1 * 0.0000 (0.0000) Cl11 * 0.0000 (0.0000) Cl11_$1 Rms deviation of fitted atoms = 0.0000 - 0.1017 (0.0209) x + 0.7141 (0.0035) y + 11.7343 (0.0116) z = 11.6834 (0.0220) Angle to previous plane (with approximate e.s.d.) = 0.00 (0.19) * 0.0000 (0.0000) Pt1_$1 * 0.0000 (0.0000) Cl11 * 0.0000 (0.0000) Cl11_$1 Rms deviation of fitted atoms = 0.0000 - 0.1032 (0.0192) x + 0.7215 (0.0147) y + 11.7325 (0.0097) z = 11.6810 (0.0192) Angle to previous plane (with approximate e.s.d.) = 0.05 (0.18) * 0.0013 (0.0025) Pt1 * -0.0013 (0.0025) Pt1_$1 * -0.0007 (0.0013) Cl1 * 0.0007 (0.0014) Cl11 * 0.0007 (0.0013) Cl1_$1 * -0.0007 (0.0014) Cl11_$1 Rms deviation of fitted atoms = 0.0009 3.2046 (0.0430) x - 7.0595 (0.0521) y + 2.2326 (0.2470) z = 2.6178 (0.2425) Angle to previous plane (with approximate e.s.d.) = 87.90 (1.21) * 0.0000 (0.0000) Pt1 * 0.0000 (0.0000) C11 * 0.0000 (0.0000) C12 Rms deviation of fitted atoms = 0.0000 - 0.1015 (0.0212) x + 0.7235 (0.0186) y + 11.7332 (0.0103) z = 11.6828 (0.0211) Angle to previous plane (with approximate e.s.d.) = 87.90 (1.21) * 0.0013 (0.0026) Pt1 * -0.0007 (0.0013) Cl1 * 0.0000 (0.0001) Cl11 * -0.0007 (0.0013) Cl11_$1 Rms deviation of fitted atoms = 0.0008 5.4046 (0.0316) x + 8.0081 (0.0511) y + 2.7407 (0.2779) z = 4.2011 (0.0831) Angle to previous plane (with approximate e.s.d.) = 86.04 (1.36) * 0.0000 (0.0001) Pt2 * 0.0000 (0.0001) C21 * 0.0000 (0.0000) C22 Rms deviation of fitted atoms = 0.0000 - 0.2622 (0.0125) x - 0.7660 (0.0207) y + 11.7074 (0.0068) z = 3.3593 (0.0073) Angle to previous plane (with approximate e.s.d.) = 87.96 (1.36) * -0.0070 (0.0027) Pt2 * 0.0036 (0.0014) Cl2 * 0.0036 (0.0014) Cl23 * -0.0002 (0.0001) Cl32 Rms deviation of fitted atoms = 0.0043 5.3896 (0.0286) x + 7.8027 (0.0677) y + 0.3253 (0.2328) z = 1.0068 (0.0793) Angle to previous plane (with approximate e.s.d.) = 76.27 (1.17) * 0.0000 (0.0001) Pt3 * 0.0000 (0.0000) C31 * 0.0000 (0.0000) C32 Rms deviation of fitted atoms = 0.0000 0.2017 (0.0123) x + 2.8713 (0.0199) y + 11.3424 (0.0108) z = 3.8031 (0.0057) Angle to previous plane (with approximate e.s.d.) = 88.61 (1.10) * -0.0179 (0.0027) Pt3 * 0.0093 (0.0014) Cl3 * -0.0005 (0.0001) Cl23 * 0.0091 (0.0014) Cl32 Rms deviation of fitted atoms = 0.0111 |
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. |
x | y | z | Uiso*/Ueq | ||
Pt1 | 0.50253 (10) | 0.17030 (6) | 0.98966 (5) | 0.03098 (19) | |
Cl1 | 0.2485 (8) | 0.3697 (5) | 0.9750 (5) | 0.0527 (12) | |
Cl11 | 0.2524 (7) | 0.0431 (5) | 0.9952 (4) | 0.0445 (10) | |
C11 | 0.752 (3) | 0.263 (2) | 0.9248 (19) | 0.056 (5) | |
H11A | 0.8938 | 0.2015 | 0.8895 | 0.067* | |
H11B | 0.7140 | 0.3476 | 0.8840 | 0.067* | |
C12 | 0.701 (3) | 0.2771 (19) | 1.0430 (17) | 0.046 (5) | |
H12A | 0.6282 | 0.3695 | 1.0753 | 0.056* | |
H12B | 0.8085 | 0.2229 | 1.0808 | 0.056* | |
Pt2 | 0.17340 (10) | 0.30150 (7) | 0.30995 (5) | 0.0318 (2) | |
Pt3 | 0.22859 (10) | −0.04306 (7) | 0.34055 (5) | 0.0315 (2) | |
Cl2 | 0.3916 (8) | 0.4329 (6) | 0.3243 (5) | 0.0574 (13) | |
Cl3 | −0.0144 (8) | −0.1663 (6) | 0.3785 (5) | 0.0573 (13) | |
Cl23 | −0.0320 (7) | 0.1547 (5) | 0.2967 (4) | 0.0423 (10) | |
Cl32 | 0.4598 (6) | 0.0964 (5) | 0.3035 (4) | 0.0406 (9) | |
C21 | −0.108 (3) | 0.471 (2) | 0.3702 (18) | 0.052 (5) | |
H21A | −0.2419 | 0.4481 | 0.4044 | 0.062* | |
H21B | −0.0883 | 0.5454 | 0.4093 | 0.062* | |
C22 | −0.048 (3) | 0.470 (2) | 0.2542 (17) | 0.051 (5) | |
H22A | 0.0087 | 0.5446 | 0.2203 | 0.062* | |
H22B | −0.1447 | 0.4473 | 0.2154 | 0.062* | |
C31 | 0.493 (3) | −0.225 (2) | 0.3172 (17) | 0.046 (4) | |
H31A | 0.4656 | −0.3089 | 0.2983 | 0.055* | |
H31B | 0.6333 | −0.2160 | 0.2752 | 0.055* | |
C32 | 0.430 (3) | −0.186 (2) | 0.4305 (16) | 0.046 (4) | |
H32A | 0.5294 | −0.1518 | 0.4592 | 0.055* | |
H32B | 0.3615 | −0.2448 | 0.4823 | 0.055* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pt1 | 0.0319 (3) | 0.0189 (3) | 0.0421 (3) | −0.0048 (2) | −0.0128 (2) | 0.0047 (2) |
Cl1 | 0.047 (3) | 0.026 (2) | 0.081 (3) | 0.001 (2) | −0.025 (2) | 0.013 (2) |
Cl11 | 0.0291 (19) | 0.023 (2) | 0.082 (3) | −0.0028 (17) | −0.0217 (19) | 0.006 (2) |
C11 | 0.038 (10) | 0.056 (14) | 0.086 (15) | −0.033 (10) | −0.019 (10) | 0.020 (11) |
C12 | 0.044 (10) | 0.024 (9) | 0.076 (13) | 0.000 (8) | −0.033 (9) | −0.008 (9) |
Pt2 | 0.0305 (3) | 0.0243 (3) | 0.0434 (4) | −0.0096 (3) | −0.0127 (2) | 0.0061 (2) |
Pt3 | 0.0302 (3) | 0.0240 (3) | 0.0420 (3) | −0.0095 (3) | −0.0102 (2) | 0.0022 (2) |
Cl2 | 0.046 (3) | 0.036 (3) | 0.096 (4) | −0.018 (2) | −0.020 (3) | −0.003 (3) |
Cl3 | 0.042 (2) | 0.037 (3) | 0.100 (4) | −0.024 (2) | −0.018 (2) | 0.014 (3) |
Cl23 | 0.037 (2) | 0.032 (2) | 0.067 (3) | −0.0145 (18) | −0.0242 (19) | 0.0080 (19) |
Cl32 | 0.0276 (18) | 0.028 (2) | 0.069 (3) | −0.0107 (17) | −0.0158 (17) | 0.0055 (19) |
C21 | 0.038 (9) | 0.031 (11) | 0.073 (13) | 0.014 (8) | −0.016 (9) | −0.011 (9) |
C22 | 0.050 (11) | 0.048 (13) | 0.059 (11) | −0.015 (10) | −0.022 (9) | 0.031 (9) |
C31 | 0.034 (9) | 0.025 (10) | 0.077 (13) | −0.003 (8) | −0.016 (9) | −0.001 (9) |
C32 | 0.041 (10) | 0.037 (11) | 0.063 (11) | −0.012 (8) | −0.023 (8) | 0.024 (9) |
Pt1—C11 | 2.108 (18) | Pt3—Cl3 | 2.261 (5) |
Pt1—C12 | 2.157 (18) | Pt3—Cl32 | 2.324 (4) |
Pt1—Cl1 | 2.257 (5) | Pt3—Cl23 | 2.376 (4) |
Pt1—Cl11i | 2.328 (4) | C21—C22 | 1.38 (3) |
Pt1—Cl11 | 2.366 (5) | C21—H21A | 0.9700 |
Cl11—Pt1i | 2.328 (4) | C21—H21B | 0.9700 |
C11—C12 | 1.41 (3) | C22—H22A | 0.9700 |
C11—H11A | 0.9700 | C22—H22B | 0.9700 |
C11—H11B | 0.9700 | C31—C32 | 1.39 (3) |
C12—H12A | 0.9700 | C31—H31A | 0.9700 |
C12—H12B | 0.9700 | C31—H31B | 0.9700 |
Pt2—C22 | 2.114 (19) | C32—H32A | 0.9700 |
Pt2—C21 | 2.132 (17) | C32—H32B | 0.9700 |
Pt2—Cl2 | 2.274 (5) | Pt1—Pt1i | 3.4539 (14) |
Pt2—Cl23 | 2.325 (4) | Pt2—Pt3 | 3.4117 (10) |
Pt2—Cl32 | 2.363 (4) | Pt1—Pt2ii | 4.0531 (10) |
Pt3—C31 | 2.118 (18) | Pt1—Pt3iii | 4.0901 (10) |
Pt3—C32 | 2.133 (17) | Pt3—Pt3iv | 4.2494 (14) |
C11—Pt1—C12 | 38.5 (8) | C31—Pt3—Cl32 | 91.9 (6) |
C11—Pt1—Cl1 | 90.9 (7) | C32—Pt3—Cl32 | 92.4 (6) |
C12—Pt1—Cl1 | 92.3 (5) | Cl3—Pt3—Cl32 | 176.35 (17) |
C11—Pt1—Cl11i | 92.7 (7) | C31—Pt3—Cl23 | 159.9 (6) |
C12—Pt1—Cl11i | 91.3 (5) | C32—Pt3—Cl23 | 161.6 (6) |
Cl1—Pt1—Cl11i | 176.20 (18) | Cl3—Pt3—Cl23 | 91.83 (18) |
C11—Pt1—Cl11 | 159.9 (7) | Cl32—Pt3—Cl23 | 84.76 (15) |
C12—Pt1—Cl11 | 161.3 (6) | Pt2—Cl23—Pt3 | 93.05 (14) |
Cl1—Pt1—Cl11 | 90.94 (17) | Pt3—Cl32—Pt2 | 93.42 (14) |
Cl11i—Pt1—Cl11 | 85.26 (15) | C22—C21—Pt2 | 70.4 (11) |
Pt1i—Cl11—Pt1 | 94.74 (15) | C22—C21—H21A | 116.6 |
C12—C11—Pt1 | 72.7 (11) | Pt2—C21—H21A | 116.6 |
C12—C11—H11A | 116.3 | C22—C21—H21B | 116.6 |
Pt1—C11—H11A | 116.3 | Pt2—C21—H21B | 116.6 |
C12—C11—H11B | 116.3 | H21A—C21—H21B | 113.6 |
Pt1—C11—H11B | 116.3 | C21—C22—Pt2 | 71.8 (10) |
H11A—C11—H11B | 113.3 | C21—C22—H22A | 116.4 |
C11—C12—Pt1 | 68.9 (10) | Pt2—C22—H22A | 116.4 |
C11—C12—H12A | 116.8 | C21—C22—H22B | 116.4 |
Pt1—C12—H12A | 116.8 | Pt2—C22—H22B | 116.4 |
C11—C12—H12B | 116.8 | H22A—C22—H22B | 113.4 |
Pt1—C12—H12B | 116.8 | C32—C31—Pt3 | 71.5 (10) |
H12A—C12—H12B | 113.8 | C32—C31—H31A | 116.4 |
C22—Pt2—C21 | 37.8 (8) | Pt3—C31—H31A | 116.4 |
C22—Pt2—Cl2 | 92.1 (6) | C32—C31—H31B | 116.4 |
C21—Pt2—Cl2 | 90.6 (6) | Pt3—C31—H31B | 116.4 |
C22—Pt2—Cl23 | 91.5 (6) | H31A—C31—H31B | 113.4 |
C21—Pt2—Cl23 | 92.7 (6) | C31—C32—Pt3 | 70.4 (10) |
Cl2—Pt2—Cl23 | 176.34 (18) | C31—C32—H32A | 116.6 |
C22—Pt2—Cl32 | 159.9 (6) | Pt3—C32—H32A | 116.6 |
C21—Pt2—Cl32 | 162.0 (6) | C31—C32—H32B | 116.6 |
Cl2—Pt2—Cl32 | 91.34 (17) | Pt3—C32—H32B | 116.6 |
Cl23—Pt2—Cl32 | 85.03 (15) | H32A—C32—H32B | 113.6 |
C31—Pt3—C32 | 38.1 (8) | Pt2ii—Pt1—Pt3iii | 173.87 (2) |
C31—Pt3—Cl3 | 91.8 (6) | Pt1iii—Pt3—Pt3iv | 159.86 (3) |
C32—Pt3—Cl3 | 90.5 (6) | ||
C11—Pt1—Cl11—Pt1i | 84.8 (19) | C32—Pt3—Cl32—Pt2 | −147.4 (6) |
C12—Pt1—Cl11—Pt1i | −80.1 (15) | Cl23—Pt3—Cl32—Pt2 | 14.44 (16) |
Cl1—Pt1—Cl11—Pt1i | 179.90 (19) | C22—Pt2—Cl32—Pt3 | −95.5 (18) |
Cl11i—Pt1—Cl11—Pt1i | 0.0 | C21—Pt2—Cl32—Pt3 | 69 (2) |
Cl1—Pt1—C11—C12 | 92.6 (11) | Cl2—Pt2—Cl32—Pt3 | 164.7 (2) |
Cl11i—Pt1—C11—C12 | −88.8 (11) | Cl23—Pt2—Cl32—Pt3 | −14.76 (17) |
Cl11—Pt1—C11—C12 | −172.3 (13) | Cl2—Pt2—C21—C22 | 92.6 (13) |
Cl1—Pt1—C12—C11 | −88.5 (12) | Cl23—Pt2—C21—C22 | −89.0 (13) |
Cl11i—Pt1—C12—C11 | 92.6 (12) | Cl32—Pt2—C21—C22 | −171.2 (15) |
Cl11—Pt1—C12—C11 | 171.7 (14) | Cl2—Pt2—C22—C21 | −88.3 (13) |
C22—Pt2—Cl23—Pt3 | 174.6 (6) | Cl23—Pt2—C22—C21 | 92.4 (13) |
C21—Pt2—Cl23—Pt3 | −147.7 (6) | Cl32—Pt2—C22—C21 | 172.1 (14) |
Cl32—Pt2—Cl23—Pt3 | 14.42 (16) | Cl3—Pt3—C31—C32 | −88.4 (11) |
C31—Pt3—Cl23—Pt2 | −95.7 (16) | Cl32—Pt3—C31—C32 | 91.5 (11) |
C32—Pt3—Cl23—Pt2 | 67.0 (18) | Cl23—Pt3—C31—C32 | 171.3 (13) |
Cl3—Pt3—Cl23—Pt2 | 164.0 (2) | Cl3—Pt3—C32—C31 | 92.3 (11) |
Cl32—Pt3—Cl23—Pt2 | −14.67 (17) | Cl32—Pt3—C32—C31 | −90.0 (11) |
C31—Pt3—Cl32—Pt2 | 174.5 (6) | Cl23—Pt3—C32—C31 | −170.4 (14) |
Symmetry codes: (i) −x+1, −y, −z+2; (ii) x, y, z+1; (iii) −x+1, −y, −z+1; (iv) −x, −y, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
C31—H31A···Cl2v | 0.97 | 2.79 | 3.71 (2) | 159 |
Symmetry code: (v) x, y−1, z. |
Experimental details
Crystal data | |
Chemical formula | [Pt2Cl4(C2H4)2] |
Mr | 588.06 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 293 |
a, b, c (Å) | 6.6413 (8), 10.1222 (13), 12.2397 (15) |
α, β, γ (°) | 87.23 (1), 75.462 (9), 73.142 (10) |
V (Å3) | 761.97 (16) |
Z | 3 |
Radiation type | Mo Kα |
µ (mm−1) | 28.49 |
Crystal size (mm) | 0.20 × 0.10 × 0.10 |
Data collection | |
Diffractometer | Nicolet R3m/V diffractometer |
Absorption correction | ψ scan (XPREP; Siemens, 1995) |
Tmin, Tmax | 0.150, 0.954 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 3804, 3502, 2740 |
Rint | 0.039 |
(sin θ/λ)max (Å−1) | 0.651 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.054, 0.140, 1.08 |
No. of reflections | 3502 |
No. of parameters | 137 |
H-atom treatment | H-atom parameters constrained |
w = 1/[σ2(Fo2) + (0.0717P)2 + 15.2811P] where P = (Fo2 + 2Fc2)/3 | |
Δρmax, Δρmin (e Å−3) | 3.86, −3.24 |
Computer programs: P3 Diffractometer Control Program (Siemens, 1990), XSCANS (Siemens, 1996), SHELXTL-Plus (Sheldrick, 1995), SHELXL97 (Sheldrick, 1997).
Pt1—Pt2i | 4.0531 (10) | Pt3—Pt3iii | 4.2494 (14) |
Pt1—Pt3ii | 4.0901 (10) | ||
Pt2i—Pt1—Pt3ii | 173.87 (2) | Pt1ii—Pt3—Pt3iii | 159.86 (3) |
Symmetry codes: (i) x, y, z+1; (ii) −x+1, −y, −z+1; (iii) −x, −y, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
C31—H31A···Cl2iv | 0.97 | 2.79 | 3.71 (2) | 159.3 |
Symmetry code: (iv) x, y−1, z. |
Bis(µ2-chloro)dichlorobis(η2-ethene)diplatinum(II) (Zeize's dimer) consists of two independent dimeric molecules in the unit cell, one of which is crystallographically centrosymmetric (Fig. 1). All platinum atoms are essentially square planar with bridging and terminal chloride groups. The ethylene groups are trans to each other across the dimeric unit in both molecules and are essentially orthogonal to the square plane geometry of their coordinated platinum atom. The non-centrosymmetric molecule exhibits a small hinge angle of 160.10 (13)° at the bridging chlorides. The overall geometry and molecular dimensions are comparable to related palladium and platinum structures, (Jain & Jain, 2005; Otto et al., 2003) including the palladium analogue (Dempsey & Baenziger, 1955). Amongst these, however, only bis(µ2-chloro)dichlorobis(η2-1,3-di-tert-butyl-2,2-dimethyl-1,3-diaza-2-sila-4- cyclopentene)dipalladium(II) is not rigorously planar (hinge angle = 150.9°) (Zettlitzer et al., 1986).
The title compound exhibits a layered structure running approximately parallel to the (0 0 1) face with a layer of the centrosymmetric dimer directly stacked between two layers of the non-centrosymmetric molecules (Pt(1)···Pt(2) 4.053 (1) Å and Pt(1')···Pt(3) 4.090 (1) Å). Within this stack, the ethylene groups of the central molecule are located between two terminal chloride groups of the adjacent molecules (τ ~90° (Aullón & Alvarez, 1997)). Adjacent three layer sandwiches are staggered from each other so that stacking occurs for only one square plane, disrupting any further interaction by Pt(2), but allowing a weaker Pt(3)···Pt(3) interaction (4.249 (1) Å). The direct Pt···Pt interaction thus extends for only five layers (Fig. 2). The Pt···Pt distances are comparable to those in K2[PtCl4] in which the electronic effects of any interaction are classified as minimal (Aullón & Alvarez, 1997). By contrast, in the palladium analogue, the molecules stack directly above each other, but with a 90° twist between adjacent Pd2(µ2-Cl)2 units leading to parallel Pd···Cl···Pd chains (3.76 Å) (Dempsey & Baenziger, 1955).
Within the presented structure, the non-centrosymmetric molecule layer exhibits a weak hydrogen bond between one terminal chloride and an ethylene hydrogen on an adjacent molecule (Fig. 2).