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The title compound, trans-[PdCl2(PhSCH2SPh)2], crystallizes with two half-mol­ecules in the asymmetric unit and each independent mol­ecule lies about a crystallographic inversion center. In each mol­ecule, one S atom of the bis­(phenyl­sulfan­yl)methane ligand is coordinated to the Pd atom while the second S atom of the same ligand is uncoordinated.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680502235X/lh6472sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680502235X/lh6472Isup2.hkl
Contains datablock I

CCDC reference: 282541

Key indicators

  • Single-crystal X-ray study
  • T = 100 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.040
  • wR factor = 0.106
  • Data-to-parameter ratio = 16.6

checkCIF/PLATON results

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Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98 PLAT213_ALERT_2_C Atom C11 has ADP max/min Ratio ............. 3.10 oblate PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 3.42 PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.67
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 1999); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: UdMX (Maris, 2004).

trans-Dichlorobis[(phenylsulfanyl)methane-κS]palladium(II) top
Crystal data top
[PdCl2(C13H12S2)2]Z = 2
Mr = 641.99F(000) = 648
Triclinic, P1Dx = 1.626 Mg m3
Hall symbol: -P 1Cu Kα radiation, λ = 1.54178 Å
a = 7.7798 (1) ÅCell parameters from 7199 reflections
b = 11.0645 (2) Åθ = 2.9–72.7°
c = 15.4006 (3) ŵ = 10.67 mm1
α = 85.256 (1)°T = 100 K
β = 82.988 (1)°Block, colourless
γ = 88.068 (1)°0.27 × 0.11 × 0.09 mm
V = 1310.88 (4) Å3
Data collection top
Bruker SMART2000
diffractometer
4986 independent reflections
Radiation source: Sealed Tube4749 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.037
Detector resolution: 5.5 pixels mm-1θmax = 72.9°, θmin = 2.9°
ω scansh = 99
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
k = 1313
Tmin = 0.176, Tmax = 0.383l = 1817
15821 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.040Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.106H-atom parameters constrained
S = 1.07 w = 1/[σ2(Fo2) + (0.0753P)2 + 1.085P]
where P = (Fo2 + 2Fc2)/3
4986 reflections(Δ/σ)max = 0.001
301 parametersΔρmax = 1.36 e Å3
0 restraintsΔρmin = 1.29 e Å3
Special details top

Experimental. X-ray crystallographic data for I were collected from a single-crystal sample, which was mounted on a loop fiber. Data were collected using a Bruker Platform diffractometer, equipped with a Bruker SMART 2 K Charged-Coupled Device (CCD) Area Detector using the program SMART and normal focus sealed tube source graphite monochromated Cu—Kα radiation. The crystal-to-detector distance was 4.908 cm, and the data collection was carried out in 512 x 512 pixel mode, utilizing 4 x 4 pixel binning. The initial unit-cell parameters were determined by a least-squares fit of the angular setting of strong reflections, collected by a 9.0 degree scan in 30 frames over four different parts of the reciprocal space (120 frames total). One complete sphere of data was collected, to better than 0.8 Å resolution. Upon completion of the data collection, the first 101 frames were recollected in order to improve the decay correction analysis.

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Pd10.00000.50000.00000.01033 (11)
Pd20.00001.00000.50000.01128 (11)
Cl20.24307 (8)1.07525 (6)0.54448 (5)0.01733 (16)
Cl10.26197 (8)0.59025 (6)0.03969 (5)0.01757 (16)
S10.10940 (8)0.30300 (6)0.01333 (5)0.01190 (15)
S20.44174 (8)0.15432 (6)0.01706 (5)0.01475 (16)
S30.46529 (9)0.67160 (6)0.45418 (5)0.01764 (17)
S40.12173 (8)0.80903 (6)0.47574 (5)0.01323 (16)
C110.0706 (3)0.2342 (2)0.08300 (19)0.0138 (5)
C120.1453 (4)0.2773 (3)0.1670 (2)0.0173 (6)
H120.21460.34510.17430.021*
C130.1148 (4)0.2177 (3)0.2385 (2)0.0212 (6)
H130.16290.24590.29440.025*
C140.0122 (4)0.1156 (3)0.2274 (2)0.0247 (7)
H140.00580.07480.27590.030*
C150.0634 (4)0.0742 (3)0.1445 (2)0.0227 (6)
H150.13310.00660.13760.027*
C160.0347 (4)0.1343 (3)0.0714 (2)0.0185 (6)
H160.08580.10750.01570.022*
C170.3459 (4)0.3028 (3)0.0003 (2)0.0147 (6)
H17A0.38700.33700.05820.018*
H17B0.38370.35450.04190.018*
C210.4396 (3)0.1351 (2)0.13261 (19)0.0136 (5)
C220.3254 (4)0.1970 (3)0.1913 (2)0.0196 (6)
H220.24640.25360.17020.023*
C230.3289 (4)0.1746 (3)0.2812 (2)0.0198 (6)
H230.25240.21640.32000.024*
C240.4458 (4)0.0905 (3)0.3133 (2)0.0180 (6)
H240.44870.07580.37350.022*
C250.5587 (4)0.0283 (3)0.2547 (2)0.0241 (7)
H250.63650.02900.27610.029*
C260.5576 (4)0.0500 (3)0.1652 (2)0.0184 (6)
H260.63490.00830.12680.022*
C310.4389 (3)0.6340 (3)0.3472 (2)0.0157 (6)
C320.3567 (4)0.7067 (3)0.2860 (2)0.0167 (6)
H320.31270.78310.29930.020*
C330.3404 (4)0.6645 (3)0.2045 (2)0.0175 (6)
H330.28520.71290.16350.021*
C340.4060 (4)0.5510 (3)0.1843 (2)0.0192 (6)
H340.39260.52250.13040.023*
C350.4915 (4)0.4800 (3)0.2445 (2)0.0204 (7)
H350.53760.40450.23030.025*
C360.5091 (4)0.5200 (3)0.3255 (2)0.0177 (6)
H360.56710.47180.36560.021*
C370.3587 (4)0.8166 (3)0.4627 (2)0.0176 (6)
H37A0.39590.86860.41040.021*
H37B0.39400.85340.51250.021*
C410.0842 (3)0.7254 (2)0.5805 (2)0.0160 (6)
C420.1433 (4)0.7656 (3)0.6544 (2)0.0175 (6)
H420.20160.83820.65070.021*
C430.1140 (4)0.6958 (3)0.7343 (2)0.0226 (6)
H430.15310.72130.78440.027*
C440.0253 (4)0.5872 (3)0.7382 (2)0.0258 (7)
H440.00750.53970.79110.031*
C450.0359 (4)0.5495 (3)0.6649 (2)0.0240 (7)
H450.09700.47810.66880.029*
C460.0063 (4)0.6185 (3)0.5848 (2)0.0208 (6)
H460.04660.59330.53500.025*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pd10.01045 (16)0.00778 (16)0.01231 (17)0.00599 (10)0.00063 (11)0.00174 (10)
Pd20.01164 (16)0.00978 (16)0.01187 (17)0.00479 (11)0.00010 (11)0.00165 (11)
Cl20.0144 (3)0.0168 (3)0.0214 (4)0.0037 (2)0.0026 (3)0.0063 (3)
Cl10.0128 (3)0.0137 (3)0.0251 (4)0.0042 (2)0.0002 (3)0.0004 (3)
S10.0122 (3)0.0075 (3)0.0154 (3)0.0068 (2)0.0015 (3)0.0008 (2)
S20.0179 (3)0.0118 (3)0.0141 (4)0.0106 (2)0.0015 (3)0.0029 (2)
S30.0193 (3)0.0170 (3)0.0164 (4)0.0102 (3)0.0023 (3)0.0036 (3)
S40.0137 (3)0.0102 (3)0.0151 (3)0.0050 (2)0.0004 (3)0.0029 (2)
C110.0143 (12)0.0098 (12)0.0176 (14)0.0092 (10)0.0050 (11)0.0020 (10)
C120.0168 (13)0.0153 (13)0.0189 (15)0.0064 (10)0.0004 (11)0.0018 (11)
C130.0191 (14)0.0275 (16)0.0165 (15)0.0121 (12)0.0008 (12)0.0056 (12)
C140.0232 (15)0.0244 (15)0.0286 (17)0.0147 (12)0.0087 (13)0.0119 (13)
C150.0210 (14)0.0140 (13)0.0342 (18)0.0056 (11)0.0063 (13)0.0073 (12)
C160.0166 (13)0.0136 (13)0.0249 (16)0.0060 (10)0.0032 (12)0.0006 (11)
C170.0134 (12)0.0119 (12)0.0188 (15)0.0064 (10)0.0034 (11)0.0011 (11)
C210.0145 (12)0.0100 (12)0.0163 (14)0.0036 (10)0.0016 (11)0.0024 (10)
C220.0189 (13)0.0196 (14)0.0199 (15)0.0144 (11)0.0035 (12)0.0042 (12)
C230.0192 (13)0.0226 (15)0.0165 (15)0.0090 (11)0.0008 (12)0.0030 (12)
C240.0237 (14)0.0163 (13)0.0136 (14)0.0039 (11)0.0023 (12)0.0010 (11)
C250.0283 (16)0.0200 (15)0.0243 (17)0.0154 (13)0.0097 (14)0.0006 (13)
C260.0196 (14)0.0176 (14)0.0175 (15)0.0139 (11)0.0011 (12)0.0053 (11)
C310.0140 (12)0.0150 (13)0.0168 (14)0.0041 (10)0.0018 (11)0.0010 (11)
C320.0176 (13)0.0139 (13)0.0172 (14)0.0089 (10)0.0018 (11)0.0027 (11)
C330.0169 (13)0.0181 (14)0.0162 (14)0.0067 (10)0.0001 (11)0.0009 (11)
C340.0199 (13)0.0207 (14)0.0160 (14)0.0019 (11)0.0024 (12)0.0043 (11)
C350.0200 (14)0.0139 (13)0.0263 (17)0.0055 (11)0.0030 (13)0.0057 (12)
C360.0191 (13)0.0136 (13)0.0189 (15)0.0083 (11)0.0008 (12)0.0004 (11)
C370.0147 (13)0.0185 (14)0.0193 (15)0.0023 (11)0.0007 (12)0.0044 (12)
C410.0142 (12)0.0112 (12)0.0207 (15)0.0077 (10)0.0015 (11)0.0015 (11)
C420.0167 (13)0.0166 (13)0.0182 (15)0.0050 (10)0.0005 (11)0.0009 (11)
C430.0217 (14)0.0265 (16)0.0180 (15)0.0132 (12)0.0018 (12)0.0003 (12)
C440.0235 (15)0.0197 (15)0.0289 (18)0.0120 (12)0.0064 (13)0.0097 (13)
C450.0229 (14)0.0135 (13)0.0319 (18)0.0045 (11)0.0077 (13)0.0022 (12)
C460.0203 (14)0.0173 (14)0.0241 (16)0.0040 (11)0.0017 (12)0.0060 (12)
Geometric parameters (Å, º) top
Pd1—Cl1i2.2927 (6)C22—H220.93
Pd1—Cl12.2927 (6)C23—C241.383 (4)
Pd1—S1i2.3155 (6)C23—H230.93
Pd1—S12.3155 (6)C24—C251.389 (5)
Pd2—Cl2ii2.2924 (6)C24—H240.93
Pd2—Cl22.2925 (6)C25—C261.380 (5)
Pd2—S42.3261 (6)C25—H250.93
Pd2—S4ii2.3261 (6)C26—H260.93
S1—C111.784 (3)C31—C321.390 (4)
S1—C171.826 (3)C31—C361.407 (4)
S2—C211.773 (3)C32—C331.397 (4)
S2—C171.794 (3)C32—H320.93
S3—C311.770 (3)C33—C341.384 (4)
S3—C371.788 (3)C33—H330.93
S4—C411.789 (3)C34—C351.384 (5)
S4—C371.834 (3)C34—H340.93
C11—C161.385 (4)C35—C361.382 (5)
C11—C121.405 (4)C35—H350.93
C12—C131.377 (4)C36—H360.93
C12—H120.93C37—H37a0.97
C13—C141.393 (5)C37—H37b0.97
C13—H130.93C41—C461.389 (4)
C14—C151.386 (5)C41—C421.389 (4)
C14—H140.93C42—C431.396 (4)
C15—C161.398 (5)C42—H420.93
C15—H150.93C43—C441.400 (5)
C16—H160.93C43—H430.93
C17—H17a0.97C44—C451.378 (5)
C17—H17b0.97C44—H440.93
C21—C221.393 (4)C45—C461.394 (4)
C21—C261.399 (4)C45—H450.93
C22—C231.390 (4)C46—H460.93
CL1i—PD1—CL1180C22—C23—H23119.9
CL1i—PD1—S1i96.21 (2)C23—C24—C25119.2 (3)
CL1—PD1—S1i83.79 (2)C23—C24—H24120.4
CL1i—PD1—S183.79 (2)C25—C24—H24120.4
CL1—PD1—S196.21 (2)C26—C25—C24121.2 (3)
S1i—PD1—S1180C26—C25—H25119.4
CL2ii—PD2—CL2180C24—C25—H25119.4
CL2ii—PD2—S484.78 (2)C25—C26—C21119.7 (3)
CL2—PD2—S495.22 (2)C25—C26—H26120.2
CL2ii—PD2—S4ii95.22 (2)C21—C26—H26120.2
CL2—PD2—S4ii84.78 (2)C32—C31—C36119.7 (3)
S4—PD2—S4ii180C32—C31—S3125.5 (2)
C11—S1—C17100.94 (13)C36—C31—S3114.8 (2)
C11—S1—PD1106.74 (9)C31—C32—C33119.6 (3)
C17—S1—PD1110.12 (9)C31—C32—H32120.2
C21—S2—C17102.81 (14)C33—C32—H32120.2
C31—S3—C37104.13 (14)C34—C33—C32120.4 (3)
C41—S4—C37100.59 (14)C34—C33—H33119.8
C41—S4—PD2104.10 (9)C32—C33—H33119.8
C37—S4—PD2109.73 (10)C35—C34—C33119.8 (3)
C16—C11—C12121.0 (3)C35—C34—H34120.1
C16—C11—S1117.0 (2)C33—C34—H34120.1
C12—C11—S1122.0 (2)C36—C35—C34120.7 (3)
C13—C12—C11119.1 (3)C36—C35—H35119.6
C13—C12—H12120.4C34—C35—H35119.6
C11—C12—H12120.4C35—C36—C31119.7 (3)
C12—C13—C14120.4 (3)C35—C36—H36120.2
C12—C13—H13119.8C31—C36—H36120.2
C14—C13—H13119.8S3—C37—S4113.33 (16)
C15—C14—C13120.4 (3)S3—C37—H37A108.9
C15—C14—H14119.8S4—C37—H37A108.9
C13—C14—H14119.8S3—C37—H37B108.9
C14—C15—C16119.9 (3)S4—C37—H37B108.9
C14—C15—H15120H37A—C37—H37B107.7
C16—C15—H15120C46—C41—C42121.4 (3)
C11—C16—C15119.2 (3)C46—C41—S4117.2 (2)
C11—C16—H16120.4C42—C41—S4121.4 (2)
C15—C16—H16120.4C41—C42—C43119.2 (3)
S2—C17—S1113.15 (15)C41—C42—H42120.4
S2—C17—H17A108.9C43—C42—H42120.4
S1—C17—H17A108.9C42—C43—C44119.3 (3)
S2—C17—H17B108.9C42—C43—H43120.4
S1—C17—H17B108.9C44—C43—H43120.4
H17A—C17—H17B107.8C45—C44—C43121.0 (3)
C22—C21—C26119.2 (3)C45—C44—H44119.5
C22—C21—S2123.8 (2)C43—C44—H44119.5
C26—C21—S2116.9 (2)C44—C45—C46120.0 (3)
C23—C22—C21120.4 (3)C44—C45—H45120
C23—C22—H22119.8C46—C45—H45120
C21—C22—H22119.8C41—C46—C45119.1 (3)
C24—C23—C22120.3 (3)C41—C46—H46120.5
C24—C23—H23119.9C45—C46—H46120.5
CL1i—PD1—S1—C1177.63 (10)C23—C24—C25—C260.8 (5)
CL1—PD1—S1—C11102.37 (10)C24—C25—C26—C210.7 (5)
CL1i—PD1—S1—C17173.63 (11)C22—C21—C26—C250.3 (5)
CL1—PD1—S1—C176.37 (11)S2—C21—C26—C25178.1 (3)
CL2ii—PD2—S4—C4193.07 (10)C37—S3—C31—C321.6 (3)
CL2—PD2—S4—C4186.93 (10)C37—S3—C31—C36178.3 (2)
CL2ii—PD2—S4—C37160.00 (11)C36—C31—C32—C331.7 (4)
CL2—PD2—S4—C3720.00 (11)S3—C31—C32—C33178.2 (2)
C17—S1—C11—C16126.4 (2)C31—C32—C33—C340.1 (4)
PD1—S1—C11—C16118.49 (19)C32—C33—C34—C351.4 (4)
C17—S1—C11—C1252.4 (2)C33—C34—C35—C361.4 (5)
PD1—S1—C11—C1262.7 (2)C34—C35—C36—C310.2 (5)
C16—C11—C12—C130.9 (4)C32—C31—C36—C351.8 (4)
S1—C11—C12—C13177.9 (2)S3—C31—C36—C35178.2 (2)
C11—C12—C13—C140.5 (4)C31—S3—C37—S474.09 (19)
C12—C13—C14—C151.4 (4)C41—S4—C37—S365.05 (19)
C13—C14—C15—C160.9 (4)PD2—S4—C37—S3174.33 (12)
C12—C11—C16—C151.4 (4)C37—S4—C41—C46123.2 (2)
S1—C11—C16—C15177.4 (2)PD2—S4—C41—C46123.1 (2)
C14—C15—C16—C110.5 (4)C37—S4—C41—C4256.7 (2)
C21—S2—C17—S184.50 (18)PD2—S4—C41—C4256.9 (2)
C11—S1—C17—S271.42 (18)C46—C41—C42—C431.3 (4)
PD1—S1—C17—S2176.05 (12)S4—C41—C42—C43178.6 (2)
C17—S2—C21—C2223.9 (3)C41—C42—C43—C440.2 (4)
C17—S2—C21—C26157.8 (2)C42—C43—C44—C451.2 (4)
C26—C21—C22—C230.1 (5)C43—C44—C45—C461.5 (5)
S2—C21—C22—C23178.3 (2)C42—C41—C46—C451.0 (4)
C21—C22—C23—C240.1 (5)S4—C41—C46—C45179.0 (2)
C22—C23—C24—C250.4 (5)C44—C45—C46—C410.4 (4)
Symmetry codes: (i) x, y+1, z; (ii) x, y+2, z+1.
 

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