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The title compound, cis-[Pd2Cl3(C7H7S)(C6H15P)2], has bridging chloro and aryl­thiol­ato groups, with the phosphines being trans to the bridging chloro group. The four-membered metallocyclic Pd2ClS ring is unexpectedly non-planar, with a dihedral angle of 133.8 (1)° between the PdCl2SP coordination planes. Principal dimensions include Pd-Clt 2.316 (3) and 2.329 (3), Pd-Clb 2.442 (3) and 2.432 (3), Pd-S 2.280 (3) and 2.282 (3), and Pd-P 2.233 (3) and 2.236 (3) Å (where Clt and Clb are terminal and bridging chloro ligands, respectively).

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100013408/qa0405sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100013408/qa0405Isup2.hkl
Contains datablock I

CCDC reference: 153929

Computing details top

Data collection: CAD-4-PC (Enraf-Nonius, 1992); cell refinement: SET4 and CELDIM (Enraf-Nonius, 1992); data reduction: DATRD2 in NRCVAX96 (Gabe et al., 1989); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: NRCVAX96 and SHELXL97 (Sheldrick, 1997); software used to prepare material for publication: NRCVAX96, SHELXL97 and WORDPERFECT macro PREP8 (Ferguson, 1998).

cis-µ-Chloro-µ-p-toluenethiolato-bis[chloro(triethylphosphine)palladium] top
Crystal data top
[Pd2Cl3(C7H7S)(C6H15P)2]? #Insert any comments here.
Mr = 678.69Dx = 1.680 Mg m3
Monoclinic, P21Mo Kα radiation, λ = 0.71073 Å
a = 7.8564 (7) ÅCell parameters from 25 reflections
b = 17.4629 (16) Åθ = 10.0–18.3°
c = 9.7865 (16) ŵ = 1.84 mm1
β = 92.132 (9)°T = 294 K
V = 1341.7 (3) Å3Plate, colouless
Z = 20.43 × 0.16 × 0.07 mm
F(000) = 680
Data collection top
Enraf-Nonius CAD-4
diffractometer
1842 reflections with I > 2σ(I)
Radiation source: X-ray tubeRint = 0.016
Graphite monochromatorθmax = 25.0°, θmin = 2.1°
θ/2θ scansh = 99
Absorption correction: gaussian
(ABSO in NRCVAX; Gabe et al., 1989)
k = 020
Tmin = 0.746, Tmax = 0.883l = 011
2652 measured reflections3 standard reflections every 120 min
2457 independent reflections intensity decay: no decay, variation 1.0%
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.038H-atom parameters constrained
wR(F2) = 0.068 w = 1/[σ2(Fo2) + (0.027P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.98(Δ/σ)max < 0.001
2457 reflectionsΔρmax = 0.48 e Å3
245 parametersΔρmin = 0.55 e Å3
1 restraintAbsolute structure: Flack (1983), no Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.01 (5)
Special details top

Experimental. ? #Insert any special details here.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Pd10.57138 (9)0.00001 (4)0.58569 (7)0.0417 (2)
Pd20.41466 (10)0.09317 (4)0.32653 (8)0.0434 (2)
S10.3062 (3)0.01285 (15)0.4850 (2)0.0423 (6)
Cl10.8433 (3)0.0031 (3)0.6854 (3)0.0786 (9)
Cl20.5263 (4)0.1698 (2)0.1568 (3)0.0738 (9)
Cl120.6746 (3)0.01835 (15)0.3557 (3)0.0556 (8)
P10.4450 (4)0.01369 (18)0.7852 (3)0.0515 (8)
P20.1798 (4)0.16526 (16)0.3146 (3)0.0498 (7)
C110.3036 (16)0.0981 (8)0.7788 (12)0.075 (4)
C120.1981 (18)0.1087 (9)0.9010 (14)0.109 (5)
C130.5725 (15)0.0205 (7)0.9409 (10)0.070 (4)
C140.6676 (17)0.0924 (8)0.9655 (13)0.095 (4)
C150.3101 (15)0.0677 (7)0.8128 (12)0.066 (4)
C160.4005 (16)0.1435 (7)0.7913 (13)0.077 (4)
C210.0698 (17)0.1543 (8)0.1514 (12)0.076 (4)
C220.0183 (15)0.0720 (8)0.1187 (11)0.083 (4)
C230.2310 (17)0.2660 (7)0.3273 (14)0.078 (4)
C240.3412 (18)0.2869 (7)0.4485 (16)0.103 (5)
C250.0273 (12)0.1479 (7)0.4428 (11)0.061 (3)
C260.1285 (14)0.1997 (7)0.4373 (12)0.077 (4)
C310.2507 (13)0.0716 (6)0.3901 (10)0.043 (3)
C320.3665 (15)0.1158 (7)0.3259 (11)0.063 (4)
C330.3083 (17)0.1825 (7)0.2537 (12)0.076 (4)
C340.140 (2)0.1988 (9)0.2418 (15)0.082 (4)
C350.0285 (18)0.1521 (9)0.3015 (14)0.083 (4)
C360.0801 (15)0.0898 (7)0.3773 (12)0.072 (4)
C370.085 (2)0.2698 (9)0.1633 (15)0.124 (6)
H11A0.37290.14350.76790.090*
H11B0.22810.09400.69840.090*
H12A0.12870.15360.88900.163*
H12B0.27130.11450.98100.163*
H12C0.12630.06470.91150.163*
H13A0.49840.01271.01680.084*
H13B0.65370.02130.94240.084*
H14A0.73050.08911.05130.143*
H14B0.58910.13450.96790.143*
H14C0.74510.10030.89320.143*
H15A0.27030.06590.90540.079*
H15B0.21130.06470.75060.079*
H16A0.32340.18490.80720.116*
H16B0.49710.14720.85390.116*
H16C0.43790.14610.69920.116*
H21A0.14250.17280.08060.092*
H21B0.03170.18590.14970.092*
H22A0.03960.07010.03060.124*
H22B0.11820.04030.11790.124*
H22C0.05620.05350.18700.124*
H23A0.12560.29490.33040.094*
H23B0.28780.28140.24530.094*
H24A0.36260.34100.44800.154*
H24B0.28490.27330.53050.154*
H24C0.44730.25970.44530.154*
H25A0.08410.15350.53190.073*
H25B0.01090.09520.43460.073*
H26A0.20220.18610.50940.115*
H26B0.09320.25200.44830.115*
H26C0.18830.19370.35060.115*
H320.48140.10270.32900.075*
H330.38670.21500.21460.091*
H350.08730.16250.29080.100*
H360.00000.05990.42010.087*
H37A0.16300.27950.09220.186*
H37B0.08400.31280.22440.186*
H37C0.02740.26220.12360.186*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pd10.0316 (4)0.0482 (5)0.0453 (4)0.0003 (4)0.0000 (3)0.0007 (4)
Pd20.0402 (4)0.0490 (5)0.0409 (4)0.0037 (5)0.0015 (3)0.0032 (4)
S10.0341 (13)0.0462 (17)0.0464 (14)0.0041 (12)0.0003 (11)0.0027 (12)
Cl10.0396 (15)0.121 (3)0.0737 (19)0.008 (2)0.0120 (13)0.011 (2)
Cl20.072 (2)0.090 (2)0.0595 (19)0.0133 (19)0.0061 (16)0.0229 (18)
Cl120.0419 (15)0.067 (2)0.0590 (16)0.0009 (14)0.0112 (12)0.0023 (14)
P10.0532 (17)0.058 (2)0.0430 (15)0.0028 (16)0.0003 (12)0.0022 (15)
P20.0487 (18)0.0538 (18)0.0464 (17)0.0060 (15)0.0045 (14)0.0057 (14)
C110.082 (9)0.082 (9)0.063 (8)0.021 (8)0.015 (7)0.017 (7)
C120.094 (11)0.113 (13)0.118 (13)0.040 (10)0.007 (10)0.021 (10)
C130.068 (8)0.087 (10)0.056 (7)0.005 (7)0.004 (6)0.017 (7)
C140.106 (12)0.083 (10)0.097 (11)0.011 (10)0.010 (9)0.008 (9)
C150.062 (8)0.082 (9)0.056 (7)0.001 (7)0.019 (6)0.007 (6)
C160.094 (11)0.053 (8)0.085 (10)0.019 (8)0.022 (8)0.004 (7)
C210.073 (9)0.097 (11)0.058 (8)0.031 (9)0.010 (7)0.009 (7)
C220.072 (9)0.134 (13)0.041 (6)0.036 (9)0.005 (6)0.014 (7)
C230.083 (10)0.059 (8)0.092 (10)0.008 (7)0.015 (8)0.016 (8)
C240.125 (13)0.053 (9)0.129 (15)0.025 (10)0.021 (12)0.016 (8)
C250.035 (6)0.070 (8)0.078 (9)0.009 (6)0.001 (6)0.008 (7)
C260.060 (8)0.076 (9)0.095 (10)0.015 (7)0.009 (7)0.008 (8)
C310.039 (6)0.049 (7)0.040 (6)0.007 (5)0.004 (5)0.017 (5)
C320.057 (8)0.088 (9)0.043 (6)0.016 (7)0.005 (6)0.010 (7)
C330.084 (10)0.083 (10)0.060 (8)0.018 (8)0.011 (8)0.023 (8)
C340.085 (11)0.095 (11)0.063 (9)0.035 (10)0.016 (9)0.001 (7)
C350.055 (9)0.104 (12)0.089 (11)0.037 (9)0.017 (8)0.013 (9)
C360.048 (7)0.077 (9)0.091 (9)0.031 (7)0.007 (7)0.006 (7)
C370.155 (16)0.116 (13)0.099 (11)0.080 (12)0.002 (11)0.051 (10)
Geometric parameters (Å, º) top
Pd1—P12.236 (3)C21—C221.524 (18)
Pd1—S12.282 (3)C21—H21A0.97
Pd1—Cl12.316 (3)C21—H21B0.97
Pd1—Cl122.442 (3)C22—H22A0.96
Pd2—P22.233 (3)C22—H22B0.96
Pd2—S12.280 (3)C22—H22C0.96
Pd2—Cl22.329 (3)C23—C241.488 (16)
Pd2—Cl122.432 (3)C23—H23A0.97
S1—C311.788 (11)C23—H23B0.97
P1—C131.796 (10)C24—H24A0.96
P1—C151.799 (11)C24—H24B0.96
P1—C111.845 (12)C24—H24C0.96
P2—C251.793 (11)C25—C261.521 (13)
P2—C211.797 (11)C25—H25A0.97
P2—C231.809 (12)C25—H25B0.97
C11—C121.492 (16)C26—H26A0.96
C11—H11A0.97C26—H26B0.96
C11—H11B0.97C26—H26C0.96
C12—H12A0.96C31—C321.364 (14)
C12—H12B0.96C31—C361.379 (13)
C12—H12C0.96C32—C331.430 (15)
C13—C141.476 (15)C32—H320.93
C13—H13A0.97C33—C341.353 (16)
C13—H13B0.97C33—H330.93
C14—H14A0.96C34—C351.346 (18)
C14—H14B0.96C34—C371.513 (17)
C14—H14C0.96C35—C361.369 (17)
C15—C161.520 (15)C35—H350.93
C15—H15A0.97C36—H360.93
C15—H15B0.97C37—H37A0.96
C16—H16A0.96C37—H37B0.96
C16—H16B0.96C37—H37C0.96
C16—H16C0.96
P1—Pd1—S187.69 (10)H16A—C16—H16C109.5
P1—Pd1—Cl193.84 (10)H16B—C16—H16C109.5
S1—Pd1—Cl1172.99 (14)C22—C21—P2113.7 (9)
P1—Pd1—Cl12172.96 (10)C22—C21—H21A108.8
S1—Pd1—Cl1285.31 (9)P2—C21—H21A108.8
Cl1—Pd1—Cl1293.02 (10)C22—C21—H21B108.8
P2—Pd2—S193.07 (10)P2—C21—H21B108.8
P2—Pd2—Cl288.36 (12)H21A—C21—H21B107.7
S1—Pd2—Cl2176.97 (12)C21—C22—H22A109.5
P2—Pd2—Cl12175.93 (11)C21—C22—H22B109.5
S1—Pd2—Cl1285.59 (9)H22A—C22—H22B109.5
Cl2—Pd2—Cl1293.16 (11)C21—C22—H22C109.5
C31—S1—Pd2104.1 (3)H22A—C22—H22C109.5
C31—S1—Pd1110.1 (3)H22B—C22—H22C109.5
Pd2—S1—Pd189.78 (9)C24—C23—P2114.5 (9)
Pd2—Cl12—Pd182.67 (8)C24—C23—H23A108.6
C13—P1—C15103.8 (6)P2—C23—H23A108.6
C13—P1—C11107.0 (6)C24—C23—H23B108.6
C15—P1—C11106.2 (6)P2—C23—H23B108.6
C13—P1—Pd1119.7 (4)H23A—C23—H23B107.6
C15—P1—Pd1109.3 (4)C23—C24—H24A109.5
C11—P1—Pd1110.0 (4)C23—C24—H24B109.5
C25—P2—C21106.9 (6)H24A—C24—H24B109.5
C25—P2—C23105.6 (6)C23—C24—H24C109.5
C21—P2—C23105.3 (6)H24A—C24—H24C109.5
C25—P2—Pd2116.2 (4)H24B—C24—H24C109.5
C21—P2—Pd2110.8 (4)C26—C25—P2115.6 (8)
C23—P2—Pd2111.4 (4)C26—C25—H25A108.4
C12—C11—P1115.0 (10)P2—C25—H25A108.4
C12—C11—H11A108.5C26—C25—H25B108.4
P1—C11—H11A108.5P2—C25—H25B108.4
C12—C11—H11B108.5H25A—C25—H25B107.4
P1—C11—H11B108.5C25—C26—H26A109.5
H11A—C11—H11B107.5C25—C26—H26B109.5
C11—C12—H12A109.5H26A—C26—H26B109.5
C11—C12—H12B109.5C25—C26—H26C109.5
H12A—C12—H12B109.5H26A—C26—H26C109.5
C11—C12—H12C109.5H26B—C26—H26C109.5
H12A—C12—H12C109.5C32—C31—C36119.3 (11)
H12B—C12—H12C109.5C32—C31—S1123.5 (9)
C14—C13—P1117.2 (9)C36—C31—S1117.1 (9)
C14—C13—H13A108.0C31—C32—C33118.8 (12)
P1—C13—H13A108.0C31—C32—H32120.6
C14—C13—H13B108.0C33—C32—H32120.6
P1—C13—H13B108.0C34—C33—C32120.5 (13)
H13A—C13—H13B107.2C34—C33—H33119.7
C13—C14—H14A109.5C32—C33—H33119.7
C13—C14—H14B109.5C35—C34—C33119.0 (14)
H14A—C14—H14B109.5C35—C34—C37122.6 (14)
C13—C14—H14C109.5C33—C34—C37118.4 (15)
H14A—C14—H14C109.5C34—C35—C36122.2 (13)
H14B—C14—H14C109.5C34—C35—H35118.9
C16—C15—P1112.7 (8)C36—C35—H35118.9
C16—C15—H15A109.0C35—C36—C31120.0 (13)
P1—C15—H15A109.0C35—C36—H36120.0
C16—C15—H15B109.0C31—C36—H36120.0
P1—C15—H15B109.0C34—C37—H37A109.5
H15A—C15—H15B107.8C34—C37—H37B109.5
C15—C16—H16A109.5H37A—C37—H37B109.5
C15—C16—H16B109.5C34—C37—H37C109.5
H16A—C16—H16B109.5H37A—C37—H37C109.5
C15—C16—H16C109.5H37B—C37—H37C109.5
P1—Pd1—Pd2—P26.80 (15)Pd1—Pd2—P2—C2520.2 (5)
S1—Pd1—Pd2—P246.80 (14)S1—Pd2—P2—C21111.4 (5)
Cl1—Pd1—Pd2—P2126.70 (16)Cl2—Pd2—P2—C2166.0 (5)
Cl12—Pd1—Pd2—P2176.56 (15)Pd1—Pd2—P2—C21142.5 (5)
P1—Pd1—Pd2—S140.00 (14)S1—Pd2—P2—C23131.8 (5)
Cl1—Pd1—Pd2—S1173.50 (17)Cl2—Pd2—P2—C2350.8 (5)
Cl12—Pd1—Pd2—S1136.64 (13)Pd1—Pd2—P2—C23100.7 (5)
P1—Pd1—Pd2—Cl2144.26 (16)C13—P1—C11—C1254.5 (11)
S1—Pd1—Pd2—Cl2175.74 (17)C15—P1—C11—C1255.8 (11)
Cl1—Pd1—Pd2—Cl210.76 (19)Pd1—P1—C11—C12173.9 (9)
Cl12—Pd1—Pd2—Cl239.10 (15)C15—P1—C13—C14165.5 (10)
P1—Pd1—Pd2—Cl12176.63 (14)C11—P1—C13—C1453.4 (11)
S1—Pd1—Pd2—Cl12136.64 (13)Pd1—P1—C13—C1472.5 (11)
Cl1—Pd1—Pd2—Cl1249.86 (16)C13—P1—C15—C1679.4 (10)
P2—Pd2—S1—C31104.3 (3)C11—P1—C15—C16168.0 (9)
Cl12—Pd2—S1—C3179.5 (3)Pd1—P1—C15—C1649.4 (10)
Pd1—Pd2—S1—C31110.7 (3)C25—P2—C21—C2269.4 (11)
P2—Pd2—S1—Pd1144.94 (10)C23—P2—C21—C22178.6 (10)
Cl12—Pd2—S1—Pd131.21 (9)Pd2—P2—C21—C2258.1 (11)
P1—Pd1—S1—C31106.8 (3)C25—P2—C23—C2473.9 (12)
Cl12—Pd1—S1—C3173.9 (3)C21—P2—C23—C24173.2 (11)
Pd2—Pd1—S1—C31105.0 (3)Pd2—P2—C23—C2453.0 (12)
P1—Pd1—S1—Pd2148.17 (11)C21—P2—C25—C2658.2 (10)
Cl12—Pd1—S1—Pd231.08 (9)C23—P2—C25—C2653.5 (10)
S1—Pd2—Cl12—Pd129.22 (9)Pd2—P2—C25—C26177.5 (7)
Cl2—Pd2—Cl12—Pd1153.54 (10)Pd2—S1—C31—C3262.6 (9)
S1—Pd1—Cl12—Pd229.20 (9)Pd1—S1—C31—C3232.5 (10)
Cl1—Pd1—Cl12—Pd2143.97 (13)Pd2—S1—C31—C36114.3 (8)
S1—Pd1—P1—C13174.9 (5)Pd1—S1—C31—C36150.6 (7)
Cl1—Pd1—P1—C131.8 (5)C36—C31—C32—C333.7 (16)
Pd2—Pd1—P1—C13147.8 (5)S1—C31—C32—C33179.4 (8)
S1—Pd1—P1—C1555.6 (4)C31—C32—C33—C344.3 (18)
Cl1—Pd1—P1—C15117.5 (4)C32—C33—C34—C351 (2)
Pd2—Pd1—P1—C1528.5 (4)C32—C33—C34—C37179.5 (13)
S1—Pd1—P1—C1160.6 (5)C33—C34—C35—C362 (2)
Cl1—Pd1—P1—C11126.3 (5)C37—C34—C35—C36177.1 (13)
Pd2—Pd1—P1—C1187.7 (5)C34—C35—C36—C313 (2)
S1—Pd2—P2—C2510.9 (4)C32—C31—C36—C350.5 (17)
Cl2—Pd2—P2—C25171.7 (4)S1—C31—C36—C35177.5 (9)
 

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