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The title complex, trans-[PdCl2(PPh3)]2, in the crystal structure of its benzene disolvate, [Pd2Cl4(C18H15P)2]·2C6H6,occupies a special position in the inversion centre. The Pd atom has a distorted square-planar coordination environment formed by a tri­phenyl­phosphine [Pd—P 2.2278 (6) Å], a terminal chloride [Pd–Cl 2.2722 (7) Å], and two bridging chloride ligands. The Pd—μ-Cl bond in the trans-position to the phosphine ligand [2.4128 (6) Å] is considerably longer than the Pd—μ-Cl bond in the trans-position to the terminal chloride [2.3228 (6) Å].

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803015502/ya6169sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803015502/ya6169Isup2.hkl
Contains datablock I

CCDC reference: 221638

Key indicators

  • Single-crystal X-ray study
  • T = 220 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.034
  • wR factor = 0.089
  • Data-to-parameter ratio = 17.3

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry








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: SHELXL97.

(I) top
Crystal data top
[Pd2Cl4(C18H15P)2]·2C6H6F(000) = 1040
Mr = 1035.40Dx = 1.542 Mg m3
Monoclinic, P21/cCu Kα radiation, λ = 1.54178 Å
Hall symbol: -P 2ybcCell parameters from 7164 reflections
a = 9.6895 (2) Åθ = 2.3–72.8°
b = 18.9619 (3) ŵ = 9.64 mm1
c = 12.8905 (2) ÅT = 220 K
β = 109.743 (1)°Block, dark orange–red
V = 2229.17 (7) Å30.27 × 0.14 × 0.10 mm
Z = 2
Data collection top
Bruker AXS SMART 2K/Platform
diffractometer
4387 independent reflections
Radiation source: normal-focus X-ray tube3992 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.059
Detector resolution: 5.5 pixels mm-1θmax = 72.8°, θmin = 4.3°
ω scansh = 1011
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
k = 2323
Tmin = 0.238, Tmax = 0.382l = 1515
26449 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)] = 0.034Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.089H-atom parameters constrained
S = 1.05 w = 1/[σ2(Fo2) + (0.0666P)2]
where P = (Fo2 + 2Fc2)/3
4387 reflections(Δ/σ)max = 0.001
253 parametersΔρmax = 1.41 e Å3
0 restraintsΔρmin = 0.49 e Å3
Special details top

Experimental. X-ray crystallographic data for I were collected from a single-crystal sample, which was mounted on a glass 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. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating R-factor_obs 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
Pd10.059522 (19)0.077817 (9)0.574033 (14)0.02316 (9)
Cl10.10130 (7)0.01308 (3)0.42624 (5)0.03129 (15)
Cl20.22125 (8)0.16325 (4)0.56831 (6)0.04067 (18)
P10.02311 (7)0.13824 (3)0.71075 (5)0.02407 (15)
C110.1258 (3)0.10080 (14)0.7488 (2)0.0286 (5)
C120.0943 (4)0.04479 (16)0.8241 (3)0.0383 (6)
H120.00350.03110.86030.046*
C130.2066 (4)0.00979 (17)0.8451 (3)0.0477 (8)
H130.18530.02740.89630.057*
C140.3514 (4)0.02930 (19)0.7907 (3)0.0522 (9)
H140.42800.00480.80410.063*
C150.3822 (4)0.0841 (2)0.7177 (4)0.0529 (9)
H150.48020.09770.68220.063*
C160.2702 (3)0.11998 (17)0.6953 (3)0.0397 (7)
H160.29250.15710.64400.048*
C210.0252 (3)0.22907 (13)0.6715 (2)0.0266 (5)
C220.0329 (3)0.28559 (15)0.7409 (2)0.0361 (6)
H220.10080.27760.81180.043*
C230.0092 (4)0.35396 (16)0.7056 (3)0.0456 (8)
H230.03080.39210.75260.055*
C240.1091 (4)0.36628 (17)0.6020 (3)0.0466 (8)
H240.13760.41270.57880.056*
C250.1673 (4)0.31029 (17)0.5323 (3)0.0444 (7)
H250.23590.31850.46180.053*
C260.1248 (3)0.24255 (15)0.5664 (2)0.0369 (6)
H260.16340.20470.51810.044*
C310.1784 (3)0.13582 (14)0.8376 (2)0.0283 (5)
C320.1653 (4)0.16284 (15)0.9344 (2)0.0355 (6)
H320.07680.18380.93310.043*
C330.2819 (4)0.15895 (17)1.0323 (2)0.0437 (7)
H330.27360.17821.09710.052*
C340.4099 (4)0.12685 (19)1.0346 (3)0.0505 (8)
H340.48840.12381.10150.061*
C350.4249 (4)0.0992 (2)0.9406 (3)0.0563 (9)
H350.51330.07750.94330.068*
C360.3087 (3)0.10341 (19)0.8411 (3)0.0419 (7)
H360.31830.08440.77650.050*
C410.3147 (4)0.8808 (3)0.6636 (3)0.0656 (12)
H410.23620.90740.67020.079*
C420.4027 (6)0.9086 (3)0.6116 (4)0.0743 (13)
H420.38560.95460.58260.089*
C430.5179 (5)0.8691 (3)0.6013 (4)0.0837 (15)
H430.57920.88770.56500.100*
C440.5408 (5)0.8022 (3)0.6453 (4)0.0803 (15)
H440.61880.77490.63930.096*
C450.4524 (5)0.7754 (2)0.6969 (4)0.0699 (12)
H450.46910.72960.72650.084*
C460.3404 (5)0.8139 (3)0.7064 (3)0.0648 (11)
H460.27940.79490.74270.078*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pd10.03141 (13)0.01733 (13)0.02153 (13)0.00016 (6)0.00996 (8)0.00179 (6)
Cl10.0483 (4)0.0214 (3)0.0309 (3)0.0055 (2)0.0222 (3)0.0057 (2)
Cl20.0472 (4)0.0329 (4)0.0486 (4)0.0126 (3)0.0249 (3)0.0071 (3)
P10.0294 (3)0.0203 (3)0.0224 (3)0.0005 (2)0.0087 (2)0.0041 (2)
C110.0357 (14)0.0242 (13)0.0291 (13)0.0032 (10)0.0150 (11)0.0081 (10)
C120.0471 (17)0.0303 (15)0.0402 (16)0.0017 (12)0.0182 (13)0.0003 (12)
C130.068 (2)0.0353 (17)0.0481 (19)0.0081 (15)0.0309 (17)0.0005 (14)
C140.056 (2)0.047 (2)0.065 (2)0.0154 (16)0.0357 (18)0.0128 (17)
C150.0383 (18)0.055 (2)0.072 (3)0.0037 (14)0.0270 (18)0.0054 (18)
C160.0374 (15)0.0366 (16)0.0464 (18)0.0007 (12)0.0160 (13)0.0009 (13)
C210.0327 (13)0.0208 (12)0.0272 (13)0.0017 (10)0.0112 (10)0.0035 (10)
C220.0459 (16)0.0271 (14)0.0309 (15)0.0074 (12)0.0073 (12)0.0054 (11)
C230.067 (2)0.0234 (14)0.0443 (18)0.0091 (14)0.0164 (15)0.0090 (13)
C240.064 (2)0.0225 (15)0.053 (2)0.0020 (13)0.0187 (16)0.0049 (13)
C250.0536 (19)0.0338 (16)0.0393 (17)0.0019 (13)0.0073 (14)0.0055 (13)
C260.0482 (17)0.0258 (14)0.0299 (14)0.0012 (12)0.0045 (12)0.0038 (11)
C310.0331 (13)0.0248 (13)0.0248 (13)0.0017 (10)0.0067 (10)0.0025 (10)
C320.0468 (17)0.0314 (15)0.0286 (14)0.0011 (12)0.0132 (12)0.0028 (11)
C330.065 (2)0.0340 (16)0.0264 (15)0.0057 (14)0.0079 (14)0.0037 (12)
C340.054 (2)0.051 (2)0.0330 (17)0.0033 (15)0.0041 (14)0.0006 (14)
C350.0410 (19)0.070 (3)0.047 (2)0.0113 (17)0.0012 (15)0.0042 (18)
C360.0388 (16)0.0519 (19)0.0327 (16)0.0052 (14)0.0091 (13)0.0040 (14)
C410.052 (2)0.079 (3)0.050 (2)0.009 (2)0.0028 (17)0.027 (2)
C420.074 (3)0.063 (3)0.065 (3)0.006 (2)0.004 (2)0.005 (2)
C430.063 (3)0.116 (5)0.073 (3)0.022 (3)0.023 (2)0.005 (3)
C440.052 (2)0.090 (4)0.086 (3)0.015 (2)0.006 (2)0.028 (3)
C450.065 (3)0.060 (3)0.064 (3)0.002 (2)0.005 (2)0.006 (2)
C460.060 (2)0.080 (3)0.045 (2)0.010 (2)0.0051 (17)0.009 (2)
Geometric parameters (Å, º) top
Pd1—P12.2278 (6)C25—C261.375 (4)
Pd1—Cl22.2722 (7)C25—H250.9400
Pd1—Cl1i2.3228 (6)C26—H260.9400
Pd1—Cl12.4128 (6)C31—C361.391 (4)
Cl1—Pd1i2.3228 (6)C31—C321.393 (4)
P1—C311.810 (3)C32—C331.383 (4)
P1—C211.811 (3)C32—H320.9400
P1—C111.818 (3)C33—C341.373 (5)
C11—C161.383 (4)C33—H330.9400
C11—C121.401 (4)C34—C351.372 (5)
C12—C131.377 (4)C34—H340.9400
C12—H120.9400C35—C361.394 (4)
C13—C141.390 (5)C35—H350.9400
C13—H130.9400C36—H360.9400
C14—C151.365 (5)C41—C421.356 (7)
C14—H140.9400C41—C461.372 (6)
C15—C161.392 (5)C41—H410.9400
C15—H150.9400C42—C431.388 (8)
C16—H160.9400C42—H420.9400
C21—C221.387 (4)C43—C441.376 (7)
C21—C261.397 (4)C43—H430.9400
C22—C231.389 (4)C44—C451.349 (7)
C22—H220.9400C44—H440.9400
C23—C241.379 (5)C45—C461.348 (6)
C23—H230.9400C45—H450.9400
C24—C251.382 (5)C46—H460.9400
C24—H240.9400
P1—Pd1—Cl287.38 (2)C26—C25—C24119.9 (3)
P1—Pd1—Cl1i95.59 (2)C26—C25—H25120.0
Cl2—Pd1—Cl1i176.98 (2)C24—C25—H25120.0
P1—Pd1—Cl1179.39 (2)C25—C26—C21121.0 (3)
Cl2—Pd1—Cl192.04 (2)C25—C26—H26119.5
Cl1i—Pd1—Cl184.99 (2)C21—C26—H26119.5
Pd1i—Cl1—Pd195.01 (2)C36—C31—C32119.3 (3)
C31—P1—C21109.49 (12)C36—C31—P1120.6 (2)
C31—P1—C11103.85 (12)C32—C31—P1120.0 (2)
C21—P1—C11107.04 (12)C33—C32—C31120.3 (3)
C31—P1—Pd1113.34 (9)C33—C32—H32119.9
C21—P1—Pd1111.30 (8)C31—C32—H32119.9
C11—P1—Pd1111.40 (8)C34—C33—C32119.8 (3)
C16—C11—C12119.4 (3)C34—C33—H33120.1
C16—C11—P1121.6 (2)C32—C33—H33120.1
C12—C11—P1118.4 (2)C35—C34—C33121.0 (3)
C13—C12—C11120.0 (3)C35—C34—H34119.5
C13—C12—H12120.0C33—C34—H34119.5
C11—C12—H12120.0C34—C35—C36119.8 (3)
C12—C13—C14120.2 (3)C34—C35—H35120.1
C12—C13—H13119.9C36—C35—H35120.1
C14—C13—H13119.9C31—C36—C35119.8 (3)
C15—C14—C13119.9 (3)C31—C36—H36120.1
C15—C14—H14120.0C35—C36—H36120.1
C13—C14—H14120.0C42—C41—C46120.0 (4)
C14—C15—C16120.7 (4)C42—C41—H41120.0
C14—C15—H15119.6C46—C41—H41120.0
C16—C15—H15119.6C41—C42—C43119.8 (5)
C11—C16—C15119.8 (3)C41—C42—H42120.1
C11—C16—H16120.1C43—C42—H42120.1
C15—C16—H16120.1C44—C43—C42118.8 (5)
C22—C21—C26118.8 (3)C44—C43—H43120.6
C22—C21—P1123.0 (2)C42—C43—H43120.6
C26—C21—P1118.3 (2)C45—C44—C43120.6 (5)
C21—C22—C23119.9 (3)C45—C44—H44119.7
C21—C22—H22120.0C43—C44—H44119.7
C23—C22—H22120.0C46—C45—C44120.4 (5)
C24—C23—C22120.5 (3)C46—C45—H45119.8
C24—C23—H23119.7C44—C45—H45119.8
C22—C23—H23119.7C45—C46—C41120.4 (4)
C23—C24—C25119.9 (3)C45—C46—H46119.8
C23—C24—H24120.0C41—C46—H46119.8
C25—C24—H24120.0
Cl2—Pd1—Cl1—Pd1i179.43 (3)C26—C21—C22—C230.5 (4)
Cl1i—Pd1—Cl1—Pd1i0.0P1—C21—C22—C23179.9 (2)
Cl2—Pd1—P1—C3170.50 (10)C21—C22—C23—C240.3 (5)
Cl1i—Pd1—P1—C31108.92 (10)C22—C23—C24—C250.4 (6)
Cl2—Pd1—P1—C2153.44 (9)C23—C24—C25—C260.3 (5)
Cl1i—Pd1—P1—C21127.14 (9)C24—C25—C26—C211.2 (5)
Cl2—Pd1—P1—C11172.82 (10)C22—C21—C26—C251.2 (5)
Cl1i—Pd1—P1—C117.77 (10)P1—C21—C26—C25179.1 (3)
C31—P1—C11—C16151.0 (2)C21—P1—C31—C36120.0 (3)
C21—P1—C11—C1635.2 (3)C11—P1—C31—C36126.0 (3)
Pd1—P1—C11—C1686.6 (2)Pd1—P1—C31—C365.0 (3)
C31—P1—C11—C1237.3 (2)C21—P1—C31—C3263.9 (3)
C21—P1—C11—C12153.1 (2)C11—P1—C31—C3250.2 (3)
Pd1—P1—C11—C1285.0 (2)Pd1—P1—C31—C32171.2 (2)
C16—C11—C12—C130.6 (4)C36—C31—C32—C331.5 (4)
P1—C11—C12—C13172.5 (2)P1—C31—C32—C33177.8 (2)
C11—C12—C13—C140.8 (5)C31—C32—C33—C341.5 (5)
C12—C13—C14—C151.2 (5)C32—C33—C34—C350.8 (5)
C13—C14—C15—C161.3 (6)C33—C34—C35—C360.2 (6)
C12—C11—C16—C150.8 (5)C32—C31—C36—C350.9 (5)
P1—C11—C16—C15172.3 (3)P1—C31—C36—C35177.1 (3)
C14—C15—C16—C111.1 (5)C34—C35—C36—C310.2 (6)
C31—P1—C21—C2210.9 (3)C46—C41—C42—C430.4 (7)
C11—P1—C21—C22101.1 (3)C41—C42—C43—C440.5 (7)
Pd1—P1—C21—C22137.0 (2)C42—C43—C44—C450.3 (7)
C31—P1—C21—C26168.8 (2)C43—C44—C45—C460.1 (7)
C11—P1—C21—C2679.3 (2)C44—C45—C46—C410.1 (6)
Pd1—P1—C21—C2642.7 (2)C42—C41—C46—C450.2 (6)
Symmetry code: (i) x, y, z+1.
 

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