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In the title compound, [PdCl2{P(OPh)3}2], the PdII centre shows slightly distorted square-planar geometry, with the two chloro ligands in cis positions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100007642/qa0303sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100007642/qa0303Isup2.hkl
Contains datablock I

CCDC reference: 147683

Comment top

During a study of the substitution reactions of [PdCl2{P(OPh)3}2], we noticed that there is no reported X-ray structure determination of this complex. This was due to difficulty experienced in crystallizing the compound from the ethanol reaction solution (Ahmed et al., 1973). IR and NMR data of the compound are in agreement with an earlier conclusion (Allen et al., 1970). With new X-ray data, it is now clear that PdII adopts a distorted four-coordinate geometry involving two chloro ligands and two phosphite groups. Evidently, the Cl1—Pd—Cl2 [90.74 (4)°] and P1—Pd—P2 [98.15 (4)°] angles are wider than their ideal values of 90° due to bulky phosphite ligands. The Cl1—Pd—Cl2 angle is also narrower than the P1—Pd—P2 angle, and this is apparently due to steric effects of the phosphite ligands. The Pd—P and Pd—Cl bonds are approximately within the same range of other phosphine complexes (Kitano et al., 1983; Ferguson et al., 1982).

Experimental top

The title complex was prepared by refluxing [PdCl4]2− and P(OPh3) in a molar ratio of 1:2 in toluene for 6 h. The yellow precipitate was extracted from the resultant suspension and colourless crystals suitable for X-ray diffraction analysis were obtained by slow addition of methanol into a solution of the compound in chloroform. Since our values of δp and 1J(Pd—P) are in excellent agreement with those in the literature (Ahmed et al., 1970), they are not reproduced here.

Computing details top

Data collection: EXPOSE (Stoe, 1997); cell refinement: CELL (Stoe, 1997); data reduction: INTEGRATE (Stoe, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97.

(I) top
Crystal data top
[PdCl2(C18H15O3P)2]F(000) = 1616
Mr = 797.90Dx = 1.548 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 9.2007 (9) ÅCell parameters from 5000 reflections
b = 12.2973 (17) Åθ = 2.1–26.1°
c = 30.421 (3) ŵ = 0.84 mm1
β = 93.260 (12)°T = 213 K
V = 3436.4 (7) Å3Plate, colourless
Z = 40.28 × 0.16 × 0.12 mm
Data collection top
Stoe IPDS
diffractometer
6755 independent reflections
Radiation source: fine-focus sealed tube4139 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.091
Detector resolution: 6.67 pixels mm-1θmax = 26.1°, θmin = 2.1°
Image plate scansh = 1111
Absorption correction: numerical
(X-SHAPE; Stoe, 1997)
k = 1515
Tmin = 0.818, Tmax = 0.916l = 3737
26396 measured reflections
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.044Calculated w = 1/[σ2(Fo2) + (0.0337P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.107(Δ/σ)max = 0.002
S = 0.86Δρmax = 0.97 e Å3
6755 reflectionsΔρmin = 1.30 e Å3
424 parameters
Crystal data top
[PdCl2(C18H15O3P)2]V = 3436.4 (7) Å3
Mr = 797.90Z = 4
Monoclinic, P21/nMo Kα radiation
a = 9.2007 (9) ŵ = 0.84 mm1
b = 12.2973 (17) ÅT = 213 K
c = 30.421 (3) Å0.28 × 0.16 × 0.12 mm
β = 93.260 (12)°
Data collection top
Stoe IPDS
diffractometer
6755 independent reflections
Absorption correction: numerical
(X-SHAPE; Stoe, 1997)
4139 reflections with I > 2σ(I)
Tmin = 0.818, Tmax = 0.916Rint = 0.091
26396 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0440 restraints
wR(F2) = 0.107H-atom parameters constrained
S = 0.86Δρmax = 0.97 e Å3
6755 reflectionsΔρmin = 1.30 e Å3
424 parameters
Special details top

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
C11.2657 (4)0.0399 (4)0.88103 (14)0.0273 (10)
C21.1726 (5)0.0427 (4)0.88995 (17)0.0404 (12)
H21.08770.05480.87200.048*
C31.2066 (6)0.1083 (4)0.92620 (19)0.0503 (14)
H31.14430.16580.93290.060*
C41.3308 (6)0.0895 (5)0.95233 (19)0.0568 (16)
H41.35370.13430.97680.068*
C51.4216 (6)0.0050 (6)0.94258 (18)0.0581 (17)
H51.50640.00770.96060.070*
C61.3902 (5)0.0609 (4)0.90698 (16)0.0411 (13)
H61.45190.11890.90040.049*
C71.0520 (5)0.2469 (4)0.74996 (14)0.0284 (10)
C81.0908 (5)0.2190 (5)0.70793 (15)0.0421 (12)
H81.14580.15620.70290.051*
C91.0444 (6)0.2883 (6)0.67336 (17)0.0575 (16)
H91.06890.27190.64450.069*
C100.9642 (6)0.3791 (6)0.68083 (19)0.0568 (16)
H100.93450.42460.65720.068*
C110.9270 (5)0.4043 (5)0.72230 (18)0.0471 (14)
H110.87270.46750.72710.057*
C120.9689 (5)0.3367 (4)0.75768 (16)0.0361 (11)
H120.94080.35250.78620.043*
C131.3485 (4)0.3253 (4)0.80558 (14)0.0267 (10)
C141.4771 (5)0.2681 (4)0.81075 (15)0.0333 (11)
H141.49280.21830.83400.040*
C151.5830 (5)0.2860 (4)0.78079 (16)0.0389 (11)
H151.67190.24830.78370.047*
C161.5577 (5)0.3588 (4)0.74691 (16)0.0384 (12)
H161.62860.36910.72620.046*
C171.4303 (5)0.4164 (4)0.74304 (16)0.0364 (11)
H171.41510.46690.72000.044*
C181.3240 (5)0.4010 (4)0.77271 (15)0.0321 (11)
H181.23700.44120.77050.039*
C191.0823 (4)0.2468 (4)1.00593 (14)0.0274 (10)
C201.1209 (5)0.2895 (4)1.04674 (15)0.0392 (11)
H201.10690.36381.05240.047*
C211.1806 (6)0.2217 (5)1.07947 (17)0.0508 (14)
H211.20620.24961.10760.061*
C221.2023 (5)0.1131 (5)1.07056 (17)0.0439 (13)
H221.24260.06691.09270.053*
C231.1652 (6)0.0726 (4)1.02955 (17)0.0454 (13)
H231.18140.00121.02350.055*
C241.1040 (5)0.1397 (4)0.99692 (16)0.0380 (12)
H241.07770.11160.96880.046*
C250.9235 (5)0.4918 (4)0.87866 (15)0.0305 (11)
C261.0157 (6)0.5589 (5)0.85747 (18)0.0495 (14)
H261.11290.56760.86810.059*
C270.9630 (7)0.6138 (5)0.8201 (2)0.0662 (18)
H271.02410.66130.80540.079*
C280.8204 (7)0.5986 (5)0.8044 (2)0.0601 (17)
H280.78460.63620.77920.072*
C290.7311 (6)0.5292 (4)0.82538 (19)0.0495 (14)
H290.63480.51850.81420.059*
C300.7817 (5)0.4752 (4)0.86260 (17)0.0387 (12)
H300.72050.42740.87710.046*
C311.2912 (4)0.4462 (4)0.93906 (15)0.0286 (10)
C321.4124 (5)0.4696 (4)0.91597 (18)0.0450 (13)
H321.44000.42450.89290.054*
C331.4920 (6)0.5616 (5)0.9279 (2)0.0580 (17)
H331.57400.57970.91230.070*
C341.4537 (6)0.6266 (4)0.9618 (2)0.0500 (14)
H341.50960.68840.96960.060*
C351.3332 (5)0.6013 (4)0.98436 (18)0.0432 (13)
H351.30660.64581.00770.052*
C361.2512 (5)0.5107 (4)0.97289 (16)0.0383 (12)
H361.16830.49350.98820.046*
O11.2429 (3)0.0997 (2)0.84164 (10)0.0315 (7)
O21.1065 (3)0.1769 (2)0.78323 (9)0.0293 (7)
O31.2360 (3)0.3082 (2)0.83514 (9)0.0289 (7)
O41.0118 (3)0.3188 (2)0.97574 (9)0.0274 (7)
O50.9685 (3)0.4469 (2)0.92002 (10)0.0299 (7)
O61.2143 (3)0.3506 (2)0.92510 (10)0.0293 (7)
P11.13885 (11)0.20135 (9)0.83398 (3)0.0222 (2)
P21.04409 (12)0.33164 (9)0.92555 (4)0.0232 (2)
Cl10.84326 (12)0.08008 (9)0.83039 (4)0.0334 (3)
Cl20.74995 (11)0.20810 (10)0.92057 (4)0.0348 (3)
Pd10.95339 (3)0.20752 (3)0.878026 (10)0.02092 (10)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.028 (2)0.033 (2)0.021 (2)0.0047 (19)0.0048 (18)0.006 (2)
C20.037 (3)0.039 (3)0.045 (3)0.006 (2)0.005 (2)0.005 (3)
C30.068 (4)0.033 (3)0.052 (4)0.004 (3)0.021 (3)0.014 (3)
C40.067 (4)0.061 (4)0.043 (4)0.026 (3)0.010 (3)0.021 (3)
C50.045 (3)0.095 (5)0.034 (3)0.004 (3)0.003 (3)0.013 (3)
C60.039 (3)0.056 (3)0.028 (3)0.012 (2)0.001 (2)0.007 (2)
C70.028 (2)0.037 (2)0.020 (2)0.007 (2)0.0018 (18)0.007 (2)
C80.048 (3)0.052 (3)0.026 (3)0.007 (3)0.004 (2)0.003 (3)
C90.065 (4)0.086 (5)0.021 (3)0.012 (4)0.001 (2)0.006 (3)
C100.048 (3)0.078 (4)0.043 (4)0.004 (3)0.011 (3)0.027 (3)
C110.031 (3)0.063 (4)0.047 (3)0.003 (2)0.004 (2)0.018 (3)
C120.032 (3)0.048 (3)0.028 (3)0.001 (2)0.002 (2)0.009 (2)
C130.028 (2)0.032 (2)0.021 (2)0.0071 (18)0.0059 (18)0.0040 (19)
C140.031 (2)0.040 (3)0.028 (3)0.002 (2)0.0010 (19)0.008 (2)
C150.032 (2)0.041 (3)0.044 (3)0.001 (2)0.006 (2)0.004 (3)
C160.040 (3)0.041 (3)0.035 (3)0.008 (2)0.009 (2)0.003 (2)
C170.041 (3)0.038 (3)0.030 (3)0.013 (2)0.001 (2)0.011 (2)
C180.030 (2)0.030 (3)0.036 (3)0.0037 (19)0.003 (2)0.005 (2)
C190.028 (2)0.031 (2)0.024 (2)0.0028 (19)0.0013 (18)0.003 (2)
C200.057 (3)0.031 (3)0.028 (3)0.004 (2)0.010 (2)0.005 (2)
C210.070 (4)0.055 (4)0.026 (3)0.006 (3)0.013 (2)0.001 (3)
C220.044 (3)0.050 (3)0.037 (3)0.003 (2)0.002 (2)0.006 (3)
C230.062 (3)0.036 (3)0.040 (3)0.011 (3)0.009 (3)0.003 (2)
C240.060 (3)0.031 (3)0.022 (3)0.004 (2)0.000 (2)0.001 (2)
C250.038 (3)0.028 (2)0.024 (2)0.0062 (19)0.001 (2)0.002 (2)
C260.044 (3)0.057 (4)0.048 (3)0.005 (3)0.003 (3)0.019 (3)
C270.071 (4)0.073 (5)0.055 (4)0.010 (3)0.012 (3)0.035 (4)
C280.075 (4)0.063 (4)0.041 (3)0.022 (3)0.007 (3)0.014 (3)
C290.051 (3)0.043 (3)0.052 (4)0.013 (3)0.021 (3)0.005 (3)
C300.042 (3)0.033 (3)0.041 (3)0.004 (2)0.003 (2)0.007 (2)
C310.026 (2)0.030 (3)0.029 (3)0.0030 (19)0.0029 (19)0.003 (2)
C320.037 (3)0.051 (3)0.047 (3)0.011 (2)0.013 (2)0.018 (3)
C330.040 (3)0.057 (4)0.079 (5)0.020 (3)0.016 (3)0.020 (3)
C340.047 (3)0.039 (3)0.064 (4)0.011 (2)0.003 (3)0.017 (3)
C350.046 (3)0.037 (3)0.047 (3)0.005 (2)0.006 (2)0.015 (3)
C360.045 (3)0.038 (3)0.033 (3)0.009 (2)0.006 (2)0.009 (2)
O10.0333 (16)0.0343 (18)0.0276 (18)0.0113 (14)0.0085 (13)0.0100 (15)
O20.0379 (17)0.0332 (17)0.0167 (15)0.0010 (13)0.0000 (13)0.0016 (13)
O30.0295 (15)0.0323 (18)0.0257 (16)0.0090 (13)0.0087 (12)0.0047 (14)
O40.0353 (16)0.0330 (18)0.0137 (15)0.0031 (13)0.0012 (12)0.0006 (13)
O50.0409 (17)0.0230 (16)0.0256 (17)0.0049 (14)0.0009 (14)0.0007 (13)
O60.0246 (15)0.0329 (17)0.0309 (18)0.0072 (13)0.0046 (13)0.0120 (14)
P10.0264 (5)0.0229 (6)0.0172 (5)0.0007 (5)0.0010 (4)0.0004 (5)
P20.0262 (6)0.0236 (6)0.0199 (6)0.0005 (4)0.0017 (4)0.0008 (5)
Cl10.0332 (6)0.0346 (6)0.0318 (6)0.0066 (5)0.0031 (5)0.0099 (5)
Cl20.0295 (5)0.0389 (6)0.0370 (7)0.0048 (5)0.0109 (5)0.0057 (6)
Pd10.02192 (16)0.02207 (17)0.01869 (17)0.00056 (14)0.00047 (11)0.00133 (15)
Geometric parameters (Å, º) top
C1—C21.365 (6)C22—C231.368 (7)
C1—C61.378 (6)C23—C241.385 (7)
C1—O11.412 (5)C25—C261.371 (7)
C2—C31.388 (7)C25—C301.381 (6)
C3—C41.374 (8)C25—O51.414 (5)
C4—C51.376 (8)C26—C271.386 (7)
C5—C61.370 (7)C27—C281.383 (8)
C7—C121.371 (6)C28—C291.367 (8)
C7—C81.390 (6)C29—C301.371 (7)
C7—O21.400 (5)C31—C361.367 (6)
C8—C91.401 (7)C31—C321.382 (6)
C9—C101.365 (8)C31—O61.424 (5)
C10—C111.362 (8)C32—C331.384 (7)
C11—C121.397 (7)C33—C341.367 (8)
C13—C181.376 (6)C34—C351.372 (7)
C13—C141.378 (6)C35—C361.379 (6)
C13—O31.425 (5)O1—P11.583 (3)
C14—C151.389 (6)O2—P11.585 (3)
C15—C161.375 (7)O3—P11.588 (3)
C16—C171.369 (7)O4—P21.580 (3)
C17—C181.381 (6)O5—P21.584 (3)
C19—C241.363 (6)O6—P21.584 (3)
C19—C201.376 (6)P1—Pd12.2299 (11)
C19—O41.408 (5)P2—Pd12.2314 (12)
C20—C211.388 (7)Cl1—Pd12.3273 (11)
C21—C221.379 (7)Cl2—Pd12.3354 (11)
C2—C1—C6122.4 (4)C28—C27—C26119.8 (6)
C2—C1—O1119.5 (4)C29—C28—C27120.5 (5)
C6—C1—O1117.8 (4)C28—C29—C30120.2 (5)
C1—C2—C3118.4 (5)C29—C30—C25119.4 (5)
C4—C3—C2120.3 (5)C36—C31—C32121.5 (4)
C3—C4—C5119.8 (5)C36—C31—O6123.6 (4)
C6—C5—C4120.9 (5)C32—C31—O6115.0 (4)
C5—C6—C1118.2 (5)C31—C32—C33117.9 (5)
C12—C7—C8122.1 (4)C34—C33—C32121.4 (5)
C12—C7—O2123.5 (4)C33—C34—C35119.7 (5)
C8—C7—O2114.4 (4)C34—C35—C36120.2 (5)
C7—C8—C9117.2 (5)C31—C36—C35119.5 (5)
C10—C9—C8121.2 (5)C1—O1—P1126.6 (3)
C11—C10—C9120.5 (5)C7—O2—P1128.9 (3)
C10—C11—C12120.3 (5)C13—O3—P1122.4 (3)
C7—C12—C11118.7 (5)C19—O4—P2126.0 (3)
C18—C13—C14122.2 (4)C25—O5—P2123.2 (3)
C18—C13—O3117.6 (4)C31—O6—P2126.4 (3)
C14—C13—O3120.2 (4)O1—P1—O294.12 (16)
C13—C14—C15118.3 (4)O1—P1—O3108.35 (16)
C16—C15—C14120.0 (4)O2—P1—O3104.66 (16)
C17—C16—C15120.6 (4)O1—P1—Pd1114.54 (12)
C16—C17—C18120.5 (4)O2—P1—Pd1118.95 (12)
C13—C18—C17118.4 (4)O3—P1—Pd1114.05 (12)
C24—C19—C20121.1 (4)O4—P2—O594.95 (16)
C24—C19—O4123.0 (4)O4—P2—O6105.28 (16)
C20—C19—O4115.8 (4)O5—P2—O6107.18 (17)
C19—C20—C21119.3 (5)O4—P2—Pd1118.29 (12)
C22—C21—C20119.8 (5)O5—P2—Pd1113.44 (12)
C23—C22—C21120.0 (5)O6—P2—Pd1115.38 (12)
C22—C23—C24120.5 (5)P1—Pd1—P298.15 (4)
C19—C24—C23119.3 (4)P1—Pd1—Cl185.63 (4)
C26—C25—C30121.3 (5)P2—Pd1—Cl1176.07 (4)
C26—C25—O5119.7 (4)P1—Pd1—Cl2176.26 (4)
C30—C25—O5118.7 (4)P2—Pd1—Cl285.46 (4)
C25—C26—C27118.8 (5)Cl1—Pd1—Cl290.74 (4)
C6—C1—C2—C30.9 (7)C2—C1—O1—P185.3 (5)
O1—C1—C2—C3172.7 (4)C6—C1—O1—P1100.9 (5)
C1—C2—C3—C40.3 (8)C12—C7—O2—P124.6 (6)
C2—C3—C4—C50.3 (9)C8—C7—O2—P1154.5 (3)
C3—C4—C5—C60.2 (9)C18—C13—O3—P1107.6 (4)
C4—C5—C6—C10.4 (8)C14—C13—O3—P173.2 (5)
C2—C1—C6—C51.0 (8)C24—C19—O4—P247.8 (6)
O1—C1—C6—C5172.7 (5)C20—C19—O4—P2136.2 (4)
C12—C7—C8—C91.5 (7)C26—C25—O5—P293.0 (5)
O2—C7—C8—C9177.6 (4)C30—C25—O5—P293.3 (4)
C7—C8—C9—C100.2 (8)C36—C31—O6—P233.6 (6)
C8—C9—C10—C110.2 (9)C32—C31—O6—P2147.0 (4)
C9—C10—C11—C120.8 (8)C1—O1—P1—O2150.3 (3)
C8—C7—C12—C112.5 (7)C1—O1—P1—O3102.8 (3)
O2—C7—C12—C11176.5 (4)C1—O1—P1—Pd125.8 (4)
C10—C11—C12—C72.1 (7)C7—O2—P1—O1161.2 (3)
C18—C13—C14—C151.9 (7)C7—O2—P1—O351.1 (4)
O3—C13—C14—C15179.0 (4)C7—O2—P1—Pd177.7 (3)
C13—C14—C15—C160.3 (7)C13—O3—P1—O158.8 (3)
C14—C15—C16—C171.8 (7)C13—O3—P1—O240.7 (3)
C15—C16—C17—C181.1 (7)C13—O3—P1—Pd1172.3 (3)
C14—C13—C18—C172.6 (7)C19—O4—P2—O5161.7 (3)
O3—C13—C18—C17178.3 (4)C19—O4—P2—O652.4 (3)
C16—C17—C18—C131.1 (7)C19—O4—P2—Pd178.3 (3)
C24—C19—C20—C211.1 (8)C25—O5—P2—O4161.4 (3)
O4—C19—C20—C21175.0 (4)C25—O5—P2—O690.9 (3)
C19—C20—C21—C220.9 (8)C25—O5—P2—Pd137.6 (3)
C20—C21—C22—C230.1 (8)C31—O6—P2—O471.6 (4)
C21—C22—C23—C240.8 (8)C31—O6—P2—O528.6 (4)
C20—C19—C24—C230.3 (7)C31—O6—P2—Pd1156.0 (3)
O4—C19—C24—C23175.5 (4)O1—P1—Pd1—P2101.86 (14)
C22—C23—C24—C190.6 (8)O2—P1—Pd1—P2148.09 (14)
C30—C25—C26—C272.2 (8)O3—P1—Pd1—P223.79 (13)
O5—C25—C26—C27171.3 (5)O1—P1—Pd1—Cl179.19 (14)
C25—C26—C27—C281.2 (9)O2—P1—Pd1—Cl130.87 (14)
C26—C27—C28—C290.4 (10)O3—P1—Pd1—Cl1155.17 (13)
C27—C28—C29—C301.0 (9)O1—P1—Pd1—Cl293.2 (7)
C28—C29—C30—C250.0 (8)O2—P1—Pd1—Cl216.8 (8)
C26—C25—C30—C291.7 (7)O3—P1—Pd1—Cl2141.1 (7)
O5—C25—C30—C29171.9 (4)O4—P2—Pd1—P1143.71 (13)
C36—C31—C32—C330.7 (8)O5—P2—Pd1—P1106.41 (13)
O6—C31—C32—C33179.9 (5)O6—P2—Pd1—P117.79 (14)
C31—C32—C33—C341.0 (9)O4—P2—Pd1—Cl151.7 (7)
C32—C33—C34—C350.6 (9)O5—P2—Pd1—Cl158.2 (7)
C33—C34—C35—C360.1 (9)O6—P2—Pd1—Cl1178 (15)
C32—C31—C36—C350.0 (7)O4—P2—Pd1—Cl237.27 (13)
O6—C31—C36—C35179.4 (4)O5—P2—Pd1—Cl272.61 (14)
C34—C35—C36—C310.4 (8)O6—P2—Pd1—Cl2163.18 (14)

Experimental details

Crystal data
Chemical formula[PdCl2(C18H15O3P)2]
Mr797.90
Crystal system, space groupMonoclinic, P21/n
Temperature (K)213
a, b, c (Å)9.2007 (9), 12.2973 (17), 30.421 (3)
β (°) 93.260 (12)
V3)3436.4 (7)
Z4
Radiation typeMo Kα
µ (mm1)0.84
Crystal size (mm)0.28 × 0.16 × 0.12
Data collection
DiffractometerStoe IPDS
diffractometer
Absorption correctionNumerical
(X-SHAPE; Stoe, 1997)
Tmin, Tmax0.818, 0.916
No. of measured, independent and
observed [I > 2σ(I)] reflections
26396, 6755, 4139
Rint0.091
(sin θ/λ)max1)0.620
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.044, 0.107, 0.86
No. of reflections6755
No. of parameters424
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.97, 1.30

Computer programs: EXPOSE (Stoe, 1997), CELL (Stoe, 1997), INTEGRATE (Stoe, 1997), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), ORTEP-3 (Farrugia, 1997), SHELXL97.

Selected geometric parameters (Å, º) top
O1—P11.583 (3)O6—P21.584 (3)
O2—P11.585 (3)P1—Pd12.2299 (11)
O3—P11.588 (3)P2—Pd12.2314 (12)
O4—P21.580 (3)Cl1—Pd12.3273 (11)
O5—P21.584 (3)Cl2—Pd12.3354 (11)
O1—P1—O294.12 (16)O4—P2—Pd1118.29 (12)
O1—P1—O3108.35 (16)O5—P2—Pd1113.44 (12)
O2—P1—O3104.66 (16)O6—P2—Pd1115.38 (12)
O1—P1—Pd1114.54 (12)P1—Pd1—P298.15 (4)
O2—P1—Pd1118.95 (12)P1—Pd1—Cl185.63 (4)
O3—P1—Pd1114.05 (12)P2—Pd1—Cl1176.07 (4)
O4—P2—O594.95 (16)P1—Pd1—Cl2176.26 (4)
O4—P2—O6105.28 (16)P2—Pd1—Cl285.46 (4)
O5—P2—O6107.18 (17)Cl1—Pd1—Cl290.74 (4)
 

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