Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802018421/cv6153sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536802018421/cv6153Isup2.hkl |
CCDC reference: 200727
Data collection: SMART (Bruker, 1995); cell refinement: SAINT (Bruker, 1995); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXL97.
[Pt2Cl2(C6H5)2(C2H6OS)2] | Z = 1 |
Mr = 771.54 | F(000) = 356 |
Triclinic, P1 | Dx = 2.461 Mg m−3 |
a = 5.9625 (12) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 8.0026 (16) Å | Cell parameters from 3272 reflections |
c = 11.388 (2) Å | θ = 2.6–30.1° |
α = 99.24 (3)° | µ = 13.89 mm−1 |
β = 102.01 (3)° | T = 293 K |
γ = 94.91 (3)° | Plate, white |
V = 520.59 (18) Å3 | 0.14 × 0.10 × 0.06 mm |
Bruker SMART CCD diffractometer | 3170 independent reflections |
Radiation source: rotating anode | 2621 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.053 |
Detector resolution: 512 pixels mm-1 | θmax = 31.6°, θmin = 1.9° |
ω scans | h = −8→8 |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | k = −11→11 |
Tmin = 0.145, Tmax = 0.359 | l = −16→15 |
6421 measured reflections |
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)] = 0.047 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.120 | H-atom parameters constrained |
S = 1.00 | w = 1/[σ2(Fo2) + (0.0771P)2] where P = (Fo2 + 2Fc2)/3 |
3170 reflections | (Δ/σ)max = 0.001 |
109 parameters | Δρmax = 3.63 e Å−3 |
0 restraints | Δρmin = −2.58 e Å−3 |
Experimental. Data was collected with a SMART CCD system using ω-scan, -0.25° and 60 s per frame. The detector distance was set to 4.0 cm. The data have a completeness of more then 99% out to θ=28.5°. The structure was solved by direct methods and refined by full matrix least squares methods. Scattering factors, dispersion corrections and absorption coefficients were taken from International Tables for Crystallography, Vol. C. (1992), tables 6.1.1.4, 4.2.6.8 and 4.2.4.2 respectively. The crystallographic raw data frames were integrated, the reflections reduced and corrections were applied for Lorentz and polarization effects. |
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. |
x | y | z | Uiso*/Ueq | ||
Pt1 | −0.11587 (5) | 0.55821 (3) | 0.63114 (3) | 0.02870 (11) | |
Cl1 | −0.1138 (4) | 0.3042 (2) | 0.4928 (2) | 0.0402 (5) | |
S1 | −0.1308 (4) | 0.8007 (3) | 0.7485 (2) | 0.0375 (4) | |
O1 | 0.0865 (14) | 0.8859 (10) | 0.8282 (8) | 0.064 (2) | |
C1 | −0.344 (3) | 0.7931 (14) | 0.8371 (14) | 0.086 (5) | |
H1A | −0.3052 | 0.7193 | 0.8950 | 0.128* | |
H1B | −0.4924 | 0.7501 | 0.7842 | 0.128* | |
H1C | −0.3498 | 0.9057 | 0.8798 | 0.128* | |
C2 | −0.240 (2) | 0.9417 (12) | 0.6515 (10) | 0.053 (3) | |
H2A | −0.1388 | 0.9585 | 0.5981 | 0.080* | |
H2B | −0.2504 | 1.0494 | 0.7002 | 0.080* | |
H2C | −0.3912 | 0.8937 | 0.6039 | 0.080* | |
C11 | −0.2856 (13) | 0.4254 (9) | 0.7268 (7) | 0.0289 (15) | |
C12 | −0.5159 (15) | 0.3583 (12) | 0.6814 (9) | 0.0412 (19) | |
H12 | −0.5937 | 0.3760 | 0.6055 | 0.049* | |
C13 | −0.630 (2) | 0.2648 (14) | 0.7488 (11) | 0.055 (3) | |
H13 | −0.7856 | 0.2227 | 0.7188 | 0.066* | |
C14 | −0.516 (2) | 0.2344 (12) | 0.8592 (10) | 0.056 (3) | |
H14 | −0.5936 | 0.1684 | 0.9020 | 0.068* | |
C15 | −0.294 (2) | 0.2979 (12) | 0.9068 (9) | 0.052 (3) | |
H15 | −0.2195 | 0.2793 | 0.9831 | 0.062* | |
C16 | −0.1762 (17) | 0.3921 (11) | 0.8405 (8) | 0.0402 (19) | |
H16 | −0.0213 | 0.4339 | 0.8724 | 0.048* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pt1 | 0.02807 (17) | 0.02633 (15) | 0.03420 (18) | 0.00095 (10) | 0.01042 (11) | 0.00972 (11) |
Cl1 | 0.0492 (12) | 0.0282 (8) | 0.0473 (12) | −0.0029 (8) | 0.0227 (10) | 0.0079 (8) |
S1 | 0.0460 (12) | 0.0296 (9) | 0.0393 (11) | 0.0033 (8) | 0.0141 (9) | 0.0081 (8) |
O1 | 0.056 (5) | 0.053 (4) | 0.065 (5) | −0.003 (3) | −0.006 (4) | −0.007 (4) |
C1 | 0.139 (14) | 0.040 (5) | 0.107 (11) | 0.011 (7) | 0.102 (11) | 0.005 (6) |
C2 | 0.079 (8) | 0.034 (4) | 0.053 (6) | 0.017 (5) | 0.019 (5) | 0.017 (4) |
C11 | 0.027 (4) | 0.029 (3) | 0.034 (4) | 0.002 (3) | 0.013 (3) | 0.010 (3) |
C12 | 0.028 (4) | 0.051 (5) | 0.045 (5) | −0.003 (3) | 0.007 (3) | 0.015 (4) |
C13 | 0.048 (6) | 0.057 (6) | 0.068 (7) | −0.003 (5) | 0.032 (5) | 0.015 (5) |
C14 | 0.085 (8) | 0.040 (4) | 0.048 (6) | −0.017 (5) | 0.030 (6) | 0.013 (4) |
C15 | 0.080 (8) | 0.045 (5) | 0.032 (5) | −0.003 (5) | 0.015 (5) | 0.013 (4) |
C16 | 0.050 (5) | 0.037 (4) | 0.032 (4) | −0.006 (4) | 0.006 (4) | 0.010 (3) |
Pt1—C11 | 1.997 (7) | C15—C16 | 1.395 (13) |
Pt1—S1 | 2.192 (2) | C1—H1A | 0.9600 |
Pt1—Cl1 | 2.366 (2) | C1—H1B | 0.9600 |
Pt1—Cl1i | 2.475 (2) | C1—H1C | 0.9600 |
Cl1—Pt1i | 2.475 (2) | C2—H2A | 0.9600 |
S1—O1 | 1.459 (8) | C2—H2B | 0.9600 |
S1—C2 | 1.773 (10) | C2—H2C | 0.9600 |
S1—C1 | 1.784 (11) | C12—H12 | 0.9300 |
C11—C12 | 1.389 (12) | C13—H13 | 0.9300 |
C11—C16 | 1.400 (12) | C14—H14 | 0.9300 |
C12—C13 | 1.390 (13) | C15—H15 | 0.9300 |
C13—C14 | 1.369 (17) | C16—H16 | 0.9300 |
C14—C15 | 1.343 (17) | ||
C11—Pt1—S1 | 92.2 (2) | S1—C1—H1B | 109.5 |
C11—Pt1—Cl1 | 89.9 (2) | H1A—C1—H1B | 109.5 |
S1—Pt1—Cl1 | 175.98 (8) | S1—C1—H1C | 109.5 |
C11—Pt1—Cl1i | 174.0 (2) | H1A—C1—H1C | 109.5 |
S1—Pt1—Cl1i | 93.10 (8) | H1B—C1—H1C | 109.5 |
Cl1—Pt1—Cl1i | 85.02 (7) | S1—C2—H2A | 109.5 |
Pt1—Cl1—Pt1i | 94.98 (7) | S1—C2—H2B | 109.5 |
O1—S1—C2 | 107.7 (5) | H2A—C2—H2B | 109.5 |
O1—S1—C1 | 108.5 (7) | S1—C2—H2C | 109.5 |
C2—S1—C1 | 100.6 (7) | H2A—C2—H2C | 109.5 |
O1—S1—Pt1 | 116.7 (4) | H2B—C2—H2C | 109.5 |
C2—S1—Pt1 | 107.3 (4) | C11—C12—H12 | 119.9 |
C1—S1—Pt1 | 114.6 (4) | C13—C12—H12 | 119.9 |
C12—C11—C16 | 117.4 (7) | C14—C13—H13 | 119.8 |
C12—C11—Pt1 | 121.1 (6) | C12—C13—H13 | 119.8 |
C16—C11—Pt1 | 121.5 (6) | C15—C14—H14 | 119.4 |
C11—C12—C13 | 120.2 (9) | C13—C14—H14 | 119.4 |
C14—C13—C12 | 120.4 (10) | CC14—C15—H15 | 120.4 |
C15—C14—C13 | 121.3 (9) | C16—C15—H15 | 120.4 |
C14—C15—C16 | 119.1 (9) | C15—C16—H16 | 119.2 |
C15—C16—C11 | 121.6 (9) | C11—C16—H16 | 119.2 |
S1—C1—H1A | 109.5 |
Symmetry code: (i) −x, −y+1, −z+1. |