supplementary materials


Acta Cryst. (2009). E65, m1391    [ doi:10.1107/S1600536809041919 ]

cis-Dichloridobis(trimethoxyphosphine)palladium(II) at 125 K

A. M. Z. Slawin, P. G. Waddell and J. D. Woollins

Abstract top

The title compound, [PdCl2(C3H9O3P)2], which is isotypic with its platinum analogue, adopts a slightly distorted cis square-planar geometry for the Pd centre.

Comment top

[PdCl2(P(OMe)3)2] is isomorphous with its platinum analogue [PtCl2(P(OMe)3)2] (2) (Bao et al., 1987) and adopts a cis square planar geometry, Whereas the Pt complex was reported to have quite dissmilar bond lengths for Pt—P1/Pt—P2 and Pt—Cl1/PtCl2 bond lengths these pairs of bonds are equivalent in the title compound.

The Pd—Cl bond bonds in (1) ( Pd(1)—Cl(1) 2.356?(2), Pd(1)—Cl(2) 2.358?(2) Å ) are shorter than the Pt—Cl bonds in (2) whilst the Pd—P bonds ( Pd(1)—P(1) 2.241?(2), Pd(1)—P(2) 2.233?(2) Å ) are longer than the Pt—P bonds in (2). The P—M—P angle ( P(1)—Pd(1)—P(2) 92.38?(8) ° ) is reduced and the Cl—M—Cl angle is enlarged ( Cl(1)—Pd(1)—Cl(2) 89.71?(8) ° ) on going from Pt to Pd with the palladium compound reported here having angles which are closer to ideal square planar .

Related literature top

For the platinum analogue, see: Bao et al. (1987). For related platinum complexes, see: Slawin et al. (2007a,b). For the structure of cis-bis(triisopropoxyphosphino)platinum dichloride, see: Slawin et al. (2009).

Experimental top

0.5 g (1.75 mmol) of PdCl2(COD) was dissolved in dichloromethane (5 mL) in a round-bottomed flask. To this 0.41 mL (3.5 mmol) of trimethylphosphite was added. The solution was stirred for 0.5 h at room temperature. The product was precipitated via slow diffusion of hexane and was then filtered off and dried under vacuum, [PdCl2(P(OMe)3)2] (1.36 mmol, ca 77%). 31P-{1H}NMR: δ 97.9 p.p.m..

Refinement top

All H atoms were included in calculated positions and refined as riding atoms with Uĩso~(H) = 1.5 U~eq~. The highest peak in the difference map is 1.097 Å from atom Pd1.

Computing details top

Data collection: SCXmini (Rigaku, 2006); cell refinement: PROCESS-AUTO (Rigaku, 1998); data reduction: PROCESS-AUTO (Rigaku, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: Crystal Structure (Rigaku, 2006); software used to prepare material for publication: Crystal Structure (Rigaku, 2006).

Figures top
[Figure 1] Fig. 1. The structure of the title compound with displacement ellipsoids drawn at the 50% probability level, hydrogen atoms omitted for clarity.
cis-Dichloridobis(trimethoxyphosphine)palladium(II) top
Crystal data top
[PdCl2(C3H9O3P)2]F(000) = 848.00
Mr = 425.46Dx = 1.866 Mg m3
Monoclinic, CcMo Kα radiation, λ = 0.71075 Å
Hall symbol: C -2ycCell parameters from 7139 reflections
a = 6.8059 (19) Åθ = 3.1–27.7°
b = 16.897 (5) ŵ = 1.80 mm1
c = 13.374 (4) ÅT = 125 K
β = 100.086 (7)°Chunk, yellow
V = 1514.2 (7) Å30.22 × 0.16 × 0.13 mm
Z = 4
Data collection top
Rigaku SCXmini
diffractometer
2639 independent reflections
Radiation source: fine-focus sealed tube2338 reflections with F2 > 2.0σ(F2)
graphiteRint = 0.072
Detector resolution: 6.85 pixels mm-1θmax = 25.4°, θmin = 2.1°
ω scansh = 88
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
k = 2020
Tmin = 0.662, Tmax = 0.791l = 1616
6333 measured reflections
Refinement top
Refinement on F2H-atom parameters constrained
R[F2 > 2σ(F2)] = 0.054 w = 1/[σ^2^(Fo^2^) + (0.0247P)^2^]
where P = (Fo^2^ + 2Fc^2^)/3
wR(F2) = 0.090(Δ/σ)max < 0.001
S = 1.07Δρmax = 1.26 e Å3
2639 reflectionsΔρmin = 0.71 e Å3
161 parametersAbsolute structure: Flack,(1983), 1308 Friedel pairs
Primary atom site location: structure-invariant direct methodsFlack parameter: 0.01 (5)
Hydrogen site location: inferred from neighbouring sites
Crystal data top
[PdCl2(C3H9O3P)2]V = 1514.2 (7) Å3
Mr = 425.46Z = 4
Monoclinic, CcMo Kα radiation
a = 6.8059 (19) ŵ = 1.80 mm1
b = 16.897 (5) ÅT = 125 K
c = 13.374 (4) Å0.22 × 0.16 × 0.13 mm
β = 100.086 (7)°
Data collection top
Rigaku SCXmini
diffractometer
2639 independent reflections
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
2338 reflections with F2 > 2.0σ(F2)
Tmin = 0.662, Tmax = 0.791Rint = 0.072
6333 measured reflectionsθmax = 25.4°
Refinement top
R[F2 > 2σ(F2)] = 0.054H-atom parameters constrained
wR(F2) = 0.090Δρmax = 1.26 e Å3
S = 1.07Δρmin = 0.71 e Å3
2639 reflectionsAbsolute structure: Flack,(1983), 1308 Friedel pairs
161 parametersFlack parameter: 0.01 (5)
? restraints
Special details top

Geometry. ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY

Refinement. Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F2. R-factor (gt) are based on F. The threshold expression of F2 > 2.0 σ(F2) is used only for calculating R-factor (gt).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Pd(1)0.50973 (10)0.10743 (4)0.45788 (7)0.01777 (16)
Cl(1)0.4602 (3)0.23766 (14)0.39555 (17)0.0298 (6)
Cl(2)0.2407 (3)0.06430 (14)0.33413 (17)0.0277 (6)
P(1)0.5605 (3)0.01677 (14)0.51540 (16)0.0183 (5)
P(2)0.7614 (3)0.15409 (14)0.57243 (17)0.0201 (5)
O(1)0.7314 (8)0.0612 (3)0.4734 (4)0.0215 (14)
O(2)0.3841 (8)0.0766 (3)0.4858 (4)0.0210 (14)
O(3)0.6237 (9)0.0227 (3)0.6348 (4)0.0252 (15)
O(4)0.9294 (8)0.0917 (3)0.6089 (4)0.0259 (15)
O(5)0.6928 (8)0.1816 (3)0.6740 (4)0.0267 (15)
O(6)0.8710 (8)0.2305 (3)0.5430 (4)0.0202 (14)
C(1)0.7285 (16)0.0650 (6)0.3643 (6)0.034 (2)
C(2)0.1966 (14)0.0676 (5)0.5230 (7)0.030 (2)
C(3)0.6711 (15)0.0993 (5)0.6843 (7)0.033 (2)
C(4)1.1106 (14)0.1149 (5)0.6777 (7)0.036 (2)
C(5)0.5731 (15)0.2526 (5)0.6788 (6)0.032 (2)
C(6)0.9618 (13)0.2290 (5)0.4527 (8)0.032 (2)
H(1)0.76620.11830.34590.041*
H(2)0.82330.02650.34550.041*
H(3)0.59390.05270.32810.041*
H(4)0.22110.07230.59720.037*
H(5)0.10310.10900.49350.037*
H(6)0.13940.01550.50340.037*
H(7)0.60000.10450.74170.040*
H(8)0.81520.10280.70890.040*
H(9)0.62980.14190.63540.040*
H(10)1.20470.13870.63880.043*
H(11)1.17160.06810.71380.043*
H(12)1.07740.15340.72690.043*
H(13)0.66140.29800.69750.038*
H(14)0.48740.24540.72980.038*
H(15)0.49010.26210.61230.038*
H(16)1.09300.25460.46720.038*
H(17)0.87640.25750.39770.038*
H(18)0.97750.17400.43210.038*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pd(1)0.0217 (3)0.0152 (3)0.0159 (3)0.0006 (3)0.0018 (2)0.0001 (3)
Cl(1)0.0375 (15)0.0183 (13)0.0301 (14)0.0010 (12)0.0040 (11)0.0048 (10)
Cl(2)0.0321 (14)0.0253 (14)0.0223 (13)0.0027 (12)0.0050 (11)0.0006 (10)
P(1)0.0228 (14)0.0171 (13)0.0157 (13)0.0017 (11)0.0056 (10)0.0012 (9)
P(2)0.0234 (15)0.0173 (14)0.0193 (13)0.0010 (11)0.0031 (11)0.0002 (10)
O(1)0.031 (3)0.019 (3)0.014 (3)0.013 (3)0.003 (2)0.002 (2)
O(2)0.024 (3)0.019 (3)0.020 (3)0.001 (2)0.004 (2)0.004 (2)
O(3)0.038 (4)0.019 (3)0.016 (3)0.005 (3)0.002 (2)0.002 (2)
O(4)0.021 (3)0.017 (3)0.037 (3)0.000 (2)0.003 (3)0.001 (2)
O(5)0.036 (4)0.026 (3)0.019 (3)0.000 (3)0.006 (2)0.002 (2)
O(6)0.025 (3)0.019 (3)0.017 (3)0.000 (2)0.005 (2)0.004 (2)
C(1)0.050 (7)0.038 (6)0.014 (5)0.015 (5)0.006 (5)0.010 (4)
C(2)0.030 (6)0.026 (5)0.036 (6)0.002 (5)0.008 (4)0.002 (5)
C(3)0.046 (6)0.024 (5)0.030 (5)0.006 (5)0.006 (4)0.002 (4)
C(4)0.026 (5)0.029 (6)0.047 (6)0.006 (4)0.007 (4)0.007 (5)
C(5)0.045 (6)0.036 (6)0.016 (5)0.003 (5)0.011 (4)0.009 (4)
C(6)0.037 (8)0.028 (5)0.033 (5)0.005 (4)0.013 (5)0.008 (5)
Geometric parameters (Å, °) top
Pd(1)—Cl(1)2.356 (2)C(1)—H(2)0.980
Pd(1)—Cl(2)2.358 (2)C(1)—H(3)0.980
Pd(1)—P(1)2.241 (2)C(2)—H(4)0.980
Pd(1)—P(2)2.233 (2)C(2)—H(5)0.980
P(1)—O(1)1.568 (6)C(2)—H(6)0.980
P(1)—O(2)1.567 (6)C(3)—H(7)0.980
P(1)—O(3)1.583 (5)C(3)—H(8)0.980
P(2)—O(4)1.568 (6)C(3)—H(9)0.980
P(2)—O(5)1.582 (6)C(4)—H(10)0.980
P(2)—O(6)1.575 (6)C(4)—H(11)0.980
O(1)—C(1)1.457 (10)C(4)—H(12)0.980
O(2)—C(2)1.457 (12)C(5)—H(13)0.980
O(3)—C(3)1.464 (10)C(5)—H(14)0.980
O(4)—C(4)1.458 (10)C(5)—H(15)0.980
O(5)—C(5)1.458 (11)C(6)—H(16)0.980
O(6)—C(6)1.451 (12)C(6)—H(17)0.980
C(1)—H(1)0.980C(6)—H(18)0.980
Cl(1)···O(5)i3.473 (5)H(4)···O(6)iii3.594
Cl(1)···C(5)i3.563 (8)H(4)···C(4)viii3.466
O(1)···C(2)ii3.121 (11)H(4)···C(5)iii3.367
O(2)···O(6)iii3.352 (7)H(4)···H(8)viii3.402
O(2)···C(6)iii3.367 (10)H(4)···H(11)viii2.891
O(3)···C(1)iv3.369 (10)H(4)···H(13)iii2.636
O(4)···C(2)ii3.550 (11)H(4)···H(15)iii3.232
O(5)···Cl(1)v3.473 (5)H(5)···Cl(1)iii2.989
O(5)···C(1)iv3.194 (11)H(5)···O(1)viii2.624
O(6)···O(2)vi3.352 (7)H(5)···O(6)iii3.271
C(1)···O(3)vii3.369 (10)H(5)···C(1)viii2.915
C(1)···O(5)vii3.194 (11)H(5)···C(5)iii3.440
C(1)···C(2)ii3.506 (13)H(5)···H(1)viii2.756
C(2)···O(1)viii3.121 (11)H(5)···H(2)viii2.858
C(2)···O(4)viii3.550 (11)H(5)···H(13)iii3.113
C(2)···C(1)viii3.506 (13)H(5)···H(15)iii2.879
C(5)···Cl(1)v3.563 (8)H(5)···H(17)iii3.321
C(6)···O(2)vi3.367 (10)H(6)···O(1)viii2.842
Pd(1)···H(7)vii3.060H(6)···O(4)viii2.832
Pd(1)···H(10)viii3.493H(6)···C(1)viii3.188
Cl(1)···H(1)ix2.793H(6)···C(4)viii3.238
Cl(1)···H(5)vi2.989H(6)···H(1)viii3.469
Cl(1)···H(7)vii3.300H(6)···H(2)viii2.745
Cl(1)···H(12)i3.121H(6)···H(10)viii3.158
Cl(1)···H(13)i3.103H(6)···H(11)viii3.121
Cl(1)···H(14)i3.585H(6)···H(18)viii3.466
Cl(1)···H(16)viii2.843H(7)···Pd(1)iv3.060
Cl(1)···H(18)viii3.571H(7)···Cl(1)iv3.300
Cl(2)···H(2)viii3.255H(7)···Cl(2)iv3.005
Cl(2)···H(4)vii3.151H(7)···C(1)iv3.339
Cl(2)···H(7)vii3.005H(7)···H(2)iv2.897
Cl(2)···H(8)x3.149H(7)···H(3)iv2.900
Cl(2)···H(11)x2.747H(7)···H(13)iii3.370
Cl(2)···H(13)i2.949H(7)···H(18)iv3.489
Cl(2)···H(18)viii3.031H(8)···Cl(2)xiv3.149
O(1)···H(4)ii3.457H(8)···C(5)xi3.076
O(1)···H(5)ii2.624H(8)···H(2)iv2.842
O(1)···H(6)ii2.842H(8)···H(3)iv3.543
O(1)···H(16)iii3.250H(8)···H(4)ii3.402
O(2)···H(16)iii3.216H(8)···H(13)xi2.917
O(2)···H(17)iii3.038H(8)···H(14)xi2.814
O(3)···H(2)iv3.022H(8)···H(15)xi2.973
O(3)···H(3)iv2.920H(8)···H(18)iv3.229
O(4)···H(1)iv3.567H(9)···O(6)iii2.917
O(4)···H(2)iv3.543H(9)···C(5)xi3.465
O(4)···H(4)ii3.429H(9)···C(6)iii3.325
O(4)···H(6)ii2.832H(9)···H(13)iii3.578
O(5)···H(1)iv2.506H(9)···H(14)xi3.173
O(5)···H(2)iv3.494H(9)···H(15)xi3.001
O(5)···H(3)iv3.151H(9)···H(16)iii2.826
O(5)···H(10)viii3.352H(10)···Pd(1)ii3.493
O(6)···H(4)vi3.594H(10)···O(5)ii3.352
O(6)···H(5)vi3.271H(10)···C(5)ii3.132
O(6)···H(9)vi2.917H(10)···H(6)ii3.158
C(1)···H(5)ii2.915H(10)···H(14)ii2.759
C(1)···H(6)ii3.188H(10)···H(15)ii2.914
C(1)···H(7)vii3.339H(11)···Cl(2)xiv2.747
C(1)···H(12)vii3.575H(11)···C(2)ii3.457
C(1)···H(16)iii3.534H(11)···H(2)iv3.268
C(2)···H(1)viii3.535H(11)···H(3)xiv3.021
C(2)···H(2)viii3.235H(11)···H(4)ii2.891
C(2)···H(11)viii3.457H(11)···H(6)ii3.121
C(2)···H(13)iii3.293H(12)···Cl(1)v3.121
C(2)···H(15)iii3.502H(12)···C(1)iv3.575
C(3)···H(2)iv3.075H(12)···H(1)iv2.925
C(3)···H(3)iv3.305H(12)···H(2)iv3.327
C(3)···H(14)xi3.381H(12)···H(14)ii3.188
C(3)···H(15)xi3.443H(12)···H(17)v3.161
C(4)···H(1)iv3.522H(13)···Cl(1)v3.103
C(4)···H(2)iv3.554H(13)···Cl(2)v2.949
C(4)···H(4)ii3.466H(13)···C(2)vi3.293
C(4)···H(6)ii3.238H(13)···H(4)vi2.636
C(4)···H(14)ii3.361H(13)···H(5)vi3.113
C(5)···H(1)iv3.293H(13)···H(7)vi3.370
C(5)···H(4)vi3.367H(13)···H(8)ix2.917
C(5)···H(5)vi3.440H(13)···H(9)vi3.578
C(5)···H(8)ix3.076H(14)···Cl(1)v3.585
C(5)···H(9)ix3.465H(14)···C(3)ix3.381
C(5)···H(10)viii3.132H(14)···C(4)viii3.361
C(5)···H(17)xii3.430H(14)···C(6)xii3.047
C(6)···H(9)vi3.325H(14)···H(1)iv3.097
C(6)···H(14)xiii3.047H(14)···H(3)iv3.538
H(1)···Cl(1)xi2.793H(14)···H(8)ix2.814
H(1)···O(4)vii3.567H(14)···H(9)ix3.173
H(1)···O(5)vii2.506H(14)···H(10)viii2.759
H(1)···C(2)ii3.535H(14)···H(12)viii3.188
H(1)···C(4)vii3.522H(14)···H(16)xii3.131
H(1)···C(5)vii3.293H(14)···H(17)xii2.492
H(1)···H(5)ii2.756H(14)···H(18)xii3.040
H(1)···H(6)ii3.469H(15)···C(2)vi3.502
H(1)···H(12)vii2.925H(15)···C(3)ix3.443
H(1)···H(14)vii3.097H(15)···H(4)vi3.232
H(1)···H(16)iii3.050H(15)···H(5)vi2.879
H(1)···H(17)iii3.545H(15)···H(8)ix2.973
H(2)···Cl(2)ii3.255H(15)···H(9)ix3.001
H(2)···O(3)vii3.022H(15)···H(10)viii2.914
H(2)···O(4)vii3.543H(15)···H(16)viii3.041
H(2)···O(5)vii3.494H(16)···Cl(1)ii2.843
H(2)···C(2)ii3.235H(16)···O(1)vi3.250
H(2)···C(3)vii3.075H(16)···O(2)vi3.216
H(2)···C(4)vii3.554H(16)···C(1)vi3.534
H(2)···H(5)ii2.858H(16)···H(1)vi3.050
H(2)···H(6)ii2.745H(16)···H(9)vi2.826
H(2)···H(7)vii2.897H(16)···H(14)xiii3.131
H(2)···H(8)vii2.842H(16)···H(15)ii3.041
H(2)···H(11)vii3.268H(17)···O(2)vi3.038
H(2)···H(12)vii3.327H(17)···C(5)xiii3.430
H(3)···O(3)vii2.920H(17)···H(1)vi3.545
H(3)···O(5)vii3.151H(17)···H(5)vi3.321
H(3)···C(3)vii3.305H(17)···H(12)i3.161
H(3)···H(7)vii2.900H(17)···H(14)xiii2.492
H(3)···H(8)vii3.543H(18)···Cl(1)ii3.571
H(3)···H(11)x3.021H(18)···Cl(2)ii3.031
H(3)···H(14)vii3.538H(18)···H(6)ii3.466
H(4)···Cl(2)iv3.151H(18)···H(7)vii3.489
H(4)···O(1)viii3.457H(18)···H(8)vii3.229
H(4)···O(4)viii3.429H(18)···H(14)xiii3.040
Cl(1)—Pd(1)—Cl(2)89.71 (8)O(2)—C(2)—H(4)109.5
Cl(1)—Pd(1)—P(1)179.04 (9)O(2)—C(2)—H(5)109.5
Cl(1)—Pd(1)—P(2)87.59 (8)O(2)—C(2)—H(6)109.5
Cl(2)—Pd(1)—P(1)90.32 (8)H(4)—C(2)—H(5)109.5
Cl(2)—Pd(1)—P(2)177.30 (8)H(4)—C(2)—H(6)109.5
P(1)—Pd(1)—P(2)92.38 (8)H(5)—C(2)—H(6)109.5
Pd(1)—P(1)—O(1)113.9 (2)O(3)—C(3)—H(7)109.5
Pd(1)—P(1)—O(2)116.9 (2)O(3)—C(3)—H(8)109.5
Pd(1)—P(1)—O(3)113.8 (2)O(3)—C(3)—H(9)109.5
O(1)—P(1)—O(2)100.6 (3)H(7)—C(3)—H(8)109.5
O(1)—P(1)—O(3)104.1 (3)H(7)—C(3)—H(9)109.5
O(2)—P(1)—O(3)106.0 (3)H(8)—C(3)—H(9)109.5
Pd(1)—P(2)—O(4)113.9 (2)O(4)—C(4)—H(10)109.5
Pd(1)—P(2)—O(5)112.8 (2)O(4)—C(4)—H(11)109.5
Pd(1)—P(2)—O(6)117.3 (2)O(4)—C(4)—H(12)109.5
O(4)—P(2)—O(5)103.9 (3)H(10)—C(4)—H(11)109.5
O(4)—P(2)—O(6)106.1 (3)H(10)—C(4)—H(12)109.5
O(5)—P(2)—O(6)101.4 (3)H(11)—C(4)—H(12)109.5
P(1)—O(1)—C(1)119.9 (5)O(5)—C(5)—H(13)109.5
P(1)—O(2)—C(2)121.6 (5)O(5)—C(5)—H(14)109.5
P(1)—O(3)—C(3)120.7 (5)O(5)—C(5)—H(15)109.5
P(2)—O(4)—C(4)120.4 (5)H(13)—C(5)—H(14)109.5
P(2)—O(5)—C(5)122.1 (5)H(13)—C(5)—H(15)109.5
P(2)—O(6)—C(6)118.9 (5)H(14)—C(5)—H(15)109.5
O(1)—C(1)—H(1)109.5O(6)—C(6)—H(16)109.5
O(1)—C(1)—H(2)109.5O(6)—C(6)—H(17)109.5
O(1)—C(1)—H(3)109.5O(6)—C(6)—H(18)109.5
H(1)—C(1)—H(2)109.5H(16)—C(6)—H(17)109.5
H(1)—C(1)—H(3)109.5H(16)—C(6)—H(18)109.5
H(2)—C(1)—H(3)109.5H(17)—C(6)—H(18)109.5
Cl(1)—Pd(1)—P(2)—O(4)151.9 (2)O(1)—P(1)—O(2)—C(2)170.3 (5)
Cl(1)—Pd(1)—P(2)—O(5)90.0 (2)O(2)—P(1)—O(1)—C(1)73.0 (6)
Cl(1)—Pd(1)—P(2)—O(6)27.2 (2)O(1)—P(1)—O(3)—C(3)52.8 (7)
Cl(2)—Pd(1)—P(1)—O(1)98.3 (2)O(3)—P(1)—O(1)—C(1)177.4 (6)
Cl(2)—Pd(1)—P(1)—O(2)18.5 (2)O(2)—P(1)—O(3)—C(3)52.8 (7)
Cl(2)—Pd(1)—P(1)—O(3)142.6 (2)O(3)—P(1)—O(2)—C(2)62.1 (6)
P(1)—Pd(1)—P(2)—O(4)27.1 (2)Pd(1)—P(2)—O(4)—C(4)175.4 (5)
P(1)—Pd(1)—P(2)—O(5)91.0 (2)Pd(1)—P(2)—O(5)—C(5)71.2 (6)
P(1)—Pd(1)—P(2)—O(6)151.9 (2)Pd(1)—P(2)—O(6)—C(6)58.1 (5)
P(2)—Pd(1)—P(1)—O(1)81.8 (2)O(4)—P(2)—O(5)—C(5)165.0 (6)
P(2)—Pd(1)—P(1)—O(2)161.4 (2)O(5)—P(2)—O(4)—C(4)61.6 (7)
P(2)—Pd(1)—P(1)—O(3)37.3 (2)O(4)—P(2)—O(6)—C(6)70.5 (5)
Pd(1)—P(1)—O(1)—C(1)52.9 (6)O(6)—P(2)—O(4)—C(4)44.8 (7)
Pd(1)—P(1)—O(2)—C(2)65.9 (6)O(5)—P(2)—O(6)—C(6)178.7 (5)
Pd(1)—P(1)—O(3)—C(3)177.3 (5)O(6)—P(2)—O(5)—C(5)55.1 (6)
Symmetry codes: (i) x−1/2, −y+1/2, z−1/2; (ii) x+1, y, z; (iii) x−1/2, y−1/2, z; (iv) x, −y, z+1/2; (v) x+1/2, −y+1/2, z+1/2; (vi) x+1/2, y+1/2, z; (vii) x, −y, z−1/2; (viii) x−1, y, z; (ix) x−1/2, y+1/2, z; (x) x−1, −y, z−1/2; (xi) x+1/2, y−1/2, z; (xii) x−1/2, −y+1/2, z+1/2; (xiii) x+1/2, −y+1/2, z−1/2; (xiv) x+1, −y, z+1/2.
Table 1
Selected geometric parameters (Å, °)
top
Pd(1)—Cl(1)2.356 (2)Pd(1)—P(1)2.241 (2)
Pd(1)—Cl(2)2.358 (2)Pd(1)—P(2)2.233 (2)
Cl(1)—Pd(1)—Cl(2)89.71 (8)Cl(2)—Pd(1)—P(1)90.32 (8)
Cl(1)—Pd(1)—P(1)179.04 (9)Cl(2)—Pd(1)—P(2)177.30 (8)
Cl(1)—Pd(1)—P(2)87.59 (8)P(1)—Pd(1)—P(2)92.38 (8)
references
References top

Bao, Q.-B., Geib, S. J., Rheingold, A. L. & Brill, T. B. (1987). Inorg. Chem. 26, 3453-3458.

Flack, H. D. (1983). Acta Cryst. A39, 876–881.

Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan.

Rigaku (1998). PROCESS-AUTO. Rigaku Corporation, Tokyo, Japan.

Rigaku (2006). Crystal Structure and SCXmini Benchtop Crystallography System Software. Rigaku Americas Corporation, The Woodlands, Texas, USA.

Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122.

Slawin, A. M. Z., Waddell, P. G. & Woollins, J. D. (2007a). Acta Cryst. E63, m2017.

Slawin, A. M. Z., Waddell, P. G. & Woollins, J. D. (2007b). Acta Cryst. E63, m2018.

Slawin, A. M. Z., Waddell, P. G. & Woollins, J. D. (2009). Acta Cryst. E65, m????. [FI2086]