Acta Cryst. (2009). E65, m1391 [ doi:10.1107/S1600536809041919 ]
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.
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..
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.
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).
| Fig. 1. The structure of the title compound with displacement ellipsoids drawn at the 50% probability level, hydrogen atoms omitted for clarity. |
| [PdCl2(C3H9O3P)2] | F(000) = 848.00 |
| Mr = 425.46 | Dx = 1.866 Mg m−3 |
| Monoclinic, Cc | Mo Kα radiation, λ = 0.71075 Å |
| Hall symbol: C -2yc | Cell parameters from 7139 reflections |
| a = 6.8059 (19) Å | θ = 3.1–27.7° |
| b = 16.897 (5) Å | µ = 1.80 mm−1 |
| c = 13.374 (4) Å | T = 125 K |
| β = 100.086 (7)° | Chunk, yellow |
| V = 1514.2 (7) Å3 | 0.22 × 0.16 × 0.13 mm |
| Z = 4 |
| Rigaku SCXmini diffractometer | 2639 independent reflections |
| Radiation source: fine-focus sealed tube | 2338 reflections with F2 > 2.0σ(F2) |
| graphite | Rint = 0.072 |
| Detector resolution: 6.85 pixels mm-1 | θmax = 25.4°, θmin = 2.1° |
| ω scans | h = −8→8 |
| Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −20→20 |
| Tmin = 0.662, Tmax = 0.791 | l = −16→16 |
| 6333 measured reflections |
| Refinement on F2 | H-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 = 1.07 | Δρmax = 1.26 e Å−3 |
| 2639 reflections | Δρmin = −0.71 e Å−3 |
| 161 parameters | Absolute structure: Flack,(1983), 1308 Friedel pairs |
| Primary atom site location: structure-invariant direct methods | Flack parameter: −0.01 (5) |
| Hydrogen site location: inferred from neighbouring sites |
| [PdCl2(C3H9O3P)2] | V = 1514.2 (7) Å3 |
| Mr = 425.46 | Z = 4 |
| Monoclinic, Cc | Mo Kα radiation |
| a = 6.8059 (19) Å | µ = 1.80 mm−1 |
| b = 16.897 (5) Å | T = 125 K |
| c = 13.374 (4) Å | 0.22 × 0.16 × 0.13 mm |
| β = 100.086 (7)° |
| Rigaku SCXmini diffractometer | 2639 independent reflections |
| Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | 2338 reflections with F2 > 2.0σ(F2) |
| Tmin = 0.662, Tmax = 0.791 | Rint = 0.072 |
| 6333 measured reflections | θmax = 25.4° |
| R[F2 > 2σ(F2)] = 0.054 | H-atom parameters constrained |
| wR(F2) = 0.090 | Δρmax = 1.26 e Å−3 |
| S = 1.07 | Δρmin = −0.71 e Å−3 |
| 2639 reflections | Absolute structure: Flack,(1983), 1308 Friedel pairs |
| 161 parameters | Flack parameter: −0.01 (5) |
| ? restraints |
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). |
| x | y | z | Uiso*/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) | 0.7662 | −0.1183 | 0.3459 | 0.041* | |
| H(2) | 0.8233 | −0.0265 | 0.3455 | 0.041* | |
| H(3) | 0.5939 | −0.0527 | 0.3281 | 0.041* | |
| H(4) | 0.2211 | −0.0723 | 0.5972 | 0.037* | |
| H(5) | 0.1031 | −0.1090 | 0.4935 | 0.037* | |
| H(6) | 0.1394 | −0.0155 | 0.5034 | 0.037* | |
| H(7) | 0.6000 | −0.1045 | 0.7417 | 0.040* | |
| H(8) | 0.8152 | −0.1028 | 0.7089 | 0.040* | |
| H(9) | 0.6298 | −0.1419 | 0.6354 | 0.040* | |
| H(10) | 1.2047 | 0.1387 | 0.6388 | 0.043* | |
| H(11) | 1.1716 | 0.0681 | 0.7138 | 0.043* | |
| H(12) | 1.0774 | 0.1534 | 0.7269 | 0.043* | |
| H(13) | 0.6614 | 0.2980 | 0.6975 | 0.038* | |
| H(14) | 0.4874 | 0.2454 | 0.7298 | 0.038* | |
| H(15) | 0.4901 | 0.2621 | 0.6123 | 0.038* | |
| H(16) | 1.0930 | 0.2546 | 0.4672 | 0.038* | |
| H(17) | 0.8764 | 0.2575 | 0.3977 | 0.038* | |
| H(18) | 0.9775 | 0.1740 | 0.4321 | 0.038* |
| U11 | U22 | U33 | U12 | U13 | U23 | |
| 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) |
| 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) | 0.980 | C(6)—H(18) | 0.980 |
| Cl(1)···O(5)i | 3.473 (5) | H(4)···O(6)iii | 3.594 |
| Cl(1)···C(5)i | 3.563 (8) | H(4)···C(4)viii | 3.466 |
| O(1)···C(2)ii | 3.121 (11) | H(4)···C(5)iii | 3.367 |
| O(2)···O(6)iii | 3.352 (7) | H(4)···H(8)viii | 3.402 |
| O(2)···C(6)iii | 3.367 (10) | H(4)···H(11)viii | 2.891 |
| O(3)···C(1)iv | 3.369 (10) | H(4)···H(13)iii | 2.636 |
| O(4)···C(2)ii | 3.550 (11) | H(4)···H(15)iii | 3.232 |
| O(5)···Cl(1)v | 3.473 (5) | H(5)···Cl(1)iii | 2.989 |
| O(5)···C(1)iv | 3.194 (11) | H(5)···O(1)viii | 2.624 |
| O(6)···O(2)vi | 3.352 (7) | H(5)···O(6)iii | 3.271 |
| C(1)···O(3)vii | 3.369 (10) | H(5)···C(1)viii | 2.915 |
| C(1)···O(5)vii | 3.194 (11) | H(5)···C(5)iii | 3.440 |
| C(1)···C(2)ii | 3.506 (13) | H(5)···H(1)viii | 2.756 |
| C(2)···O(1)viii | 3.121 (11) | H(5)···H(2)viii | 2.858 |
| C(2)···O(4)viii | 3.550 (11) | H(5)···H(13)iii | 3.113 |
| C(2)···C(1)viii | 3.506 (13) | H(5)···H(15)iii | 2.879 |
| C(5)···Cl(1)v | 3.563 (8) | H(5)···H(17)iii | 3.321 |
| C(6)···O(2)vi | 3.367 (10) | H(6)···O(1)viii | 2.842 |
| Pd(1)···H(7)vii | 3.060 | H(6)···O(4)viii | 2.832 |
| Pd(1)···H(10)viii | 3.493 | H(6)···C(1)viii | 3.188 |
| Cl(1)···H(1)ix | 2.793 | H(6)···C(4)viii | 3.238 |
| Cl(1)···H(5)vi | 2.989 | H(6)···H(1)viii | 3.469 |
| Cl(1)···H(7)vii | 3.300 | H(6)···H(2)viii | 2.745 |
| Cl(1)···H(12)i | 3.121 | H(6)···H(10)viii | 3.158 |
| Cl(1)···H(13)i | 3.103 | H(6)···H(11)viii | 3.121 |
| Cl(1)···H(14)i | 3.585 | H(6)···H(18)viii | 3.466 |
| Cl(1)···H(16)viii | 2.843 | H(7)···Pd(1)iv | 3.060 |
| Cl(1)···H(18)viii | 3.571 | H(7)···Cl(1)iv | 3.300 |
| Cl(2)···H(2)viii | 3.255 | H(7)···Cl(2)iv | 3.005 |
| Cl(2)···H(4)vii | 3.151 | H(7)···C(1)iv | 3.339 |
| Cl(2)···H(7)vii | 3.005 | H(7)···H(2)iv | 2.897 |
| Cl(2)···H(8)x | 3.149 | H(7)···H(3)iv | 2.900 |
| Cl(2)···H(11)x | 2.747 | H(7)···H(13)iii | 3.370 |
| Cl(2)···H(13)i | 2.949 | H(7)···H(18)iv | 3.489 |
| Cl(2)···H(18)viii | 3.031 | H(8)···Cl(2)xiv | 3.149 |
| O(1)···H(4)ii | 3.457 | H(8)···C(5)xi | 3.076 |
| O(1)···H(5)ii | 2.624 | H(8)···H(2)iv | 2.842 |
| O(1)···H(6)ii | 2.842 | H(8)···H(3)iv | 3.543 |
| O(1)···H(16)iii | 3.250 | H(8)···H(4)ii | 3.402 |
| O(2)···H(16)iii | 3.216 | H(8)···H(13)xi | 2.917 |
| O(2)···H(17)iii | 3.038 | H(8)···H(14)xi | 2.814 |
| O(3)···H(2)iv | 3.022 | H(8)···H(15)xi | 2.973 |
| O(3)···H(3)iv | 2.920 | H(8)···H(18)iv | 3.229 |
| O(4)···H(1)iv | 3.567 | H(9)···O(6)iii | 2.917 |
| O(4)···H(2)iv | 3.543 | H(9)···C(5)xi | 3.465 |
| O(4)···H(4)ii | 3.429 | H(9)···C(6)iii | 3.325 |
| O(4)···H(6)ii | 2.832 | H(9)···H(13)iii | 3.578 |
| O(5)···H(1)iv | 2.506 | H(9)···H(14)xi | 3.173 |
| O(5)···H(2)iv | 3.494 | H(9)···H(15)xi | 3.001 |
| O(5)···H(3)iv | 3.151 | H(9)···H(16)iii | 2.826 |
| O(5)···H(10)viii | 3.352 | H(10)···Pd(1)ii | 3.493 |
| O(6)···H(4)vi | 3.594 | H(10)···O(5)ii | 3.352 |
| O(6)···H(5)vi | 3.271 | H(10)···C(5)ii | 3.132 |
| O(6)···H(9)vi | 2.917 | H(10)···H(6)ii | 3.158 |
| C(1)···H(5)ii | 2.915 | H(10)···H(14)ii | 2.759 |
| C(1)···H(6)ii | 3.188 | H(10)···H(15)ii | 2.914 |
| C(1)···H(7)vii | 3.339 | H(11)···Cl(2)xiv | 2.747 |
| C(1)···H(12)vii | 3.575 | H(11)···C(2)ii | 3.457 |
| C(1)···H(16)iii | 3.534 | H(11)···H(2)iv | 3.268 |
| C(2)···H(1)viii | 3.535 | H(11)···H(3)xiv | 3.021 |
| C(2)···H(2)viii | 3.235 | H(11)···H(4)ii | 2.891 |
| C(2)···H(11)viii | 3.457 | H(11)···H(6)ii | 3.121 |
| C(2)···H(13)iii | 3.293 | H(12)···Cl(1)v | 3.121 |
| C(2)···H(15)iii | 3.502 | H(12)···C(1)iv | 3.575 |
| C(3)···H(2)iv | 3.075 | H(12)···H(1)iv | 2.925 |
| C(3)···H(3)iv | 3.305 | H(12)···H(2)iv | 3.327 |
| C(3)···H(14)xi | 3.381 | H(12)···H(14)ii | 3.188 |
| C(3)···H(15)xi | 3.443 | H(12)···H(17)v | 3.161 |
| C(4)···H(1)iv | 3.522 | H(13)···Cl(1)v | 3.103 |
| C(4)···H(2)iv | 3.554 | H(13)···Cl(2)v | 2.949 |
| C(4)···H(4)ii | 3.466 | H(13)···C(2)vi | 3.293 |
| C(4)···H(6)ii | 3.238 | H(13)···H(4)vi | 2.636 |
| C(4)···H(14)ii | 3.361 | H(13)···H(5)vi | 3.113 |
| C(5)···H(1)iv | 3.293 | H(13)···H(7)vi | 3.370 |
| C(5)···H(4)vi | 3.367 | H(13)···H(8)ix | 2.917 |
| C(5)···H(5)vi | 3.440 | H(13)···H(9)vi | 3.578 |
| C(5)···H(8)ix | 3.076 | H(14)···Cl(1)v | 3.585 |
| C(5)···H(9)ix | 3.465 | H(14)···C(3)ix | 3.381 |
| C(5)···H(10)viii | 3.132 | H(14)···C(4)viii | 3.361 |
| C(5)···H(17)xii | 3.430 | H(14)···C(6)xii | 3.047 |
| C(6)···H(9)vi | 3.325 | H(14)···H(1)iv | 3.097 |
| C(6)···H(14)xiii | 3.047 | H(14)···H(3)iv | 3.538 |
| H(1)···Cl(1)xi | 2.793 | H(14)···H(8)ix | 2.814 |
| H(1)···O(4)vii | 3.567 | H(14)···H(9)ix | 3.173 |
| H(1)···O(5)vii | 2.506 | H(14)···H(10)viii | 2.759 |
| H(1)···C(2)ii | 3.535 | H(14)···H(12)viii | 3.188 |
| H(1)···C(4)vii | 3.522 | H(14)···H(16)xii | 3.131 |
| H(1)···C(5)vii | 3.293 | H(14)···H(17)xii | 2.492 |
| H(1)···H(5)ii | 2.756 | H(14)···H(18)xii | 3.040 |
| H(1)···H(6)ii | 3.469 | H(15)···C(2)vi | 3.502 |
| H(1)···H(12)vii | 2.925 | H(15)···C(3)ix | 3.443 |
| H(1)···H(14)vii | 3.097 | H(15)···H(4)vi | 3.232 |
| H(1)···H(16)iii | 3.050 | H(15)···H(5)vi | 2.879 |
| H(1)···H(17)iii | 3.545 | H(15)···H(8)ix | 2.973 |
| H(2)···Cl(2)ii | 3.255 | H(15)···H(9)ix | 3.001 |
| H(2)···O(3)vii | 3.022 | H(15)···H(10)viii | 2.914 |
| H(2)···O(4)vii | 3.543 | H(15)···H(16)viii | 3.041 |
| H(2)···O(5)vii | 3.494 | H(16)···Cl(1)ii | 2.843 |
| H(2)···C(2)ii | 3.235 | H(16)···O(1)vi | 3.250 |
| H(2)···C(3)vii | 3.075 | H(16)···O(2)vi | 3.216 |
| H(2)···C(4)vii | 3.554 | H(16)···C(1)vi | 3.534 |
| H(2)···H(5)ii | 2.858 | H(16)···H(1)vi | 3.050 |
| H(2)···H(6)ii | 2.745 | H(16)···H(9)vi | 2.826 |
| H(2)···H(7)vii | 2.897 | H(16)···H(14)xiii | 3.131 |
| H(2)···H(8)vii | 2.842 | H(16)···H(15)ii | 3.041 |
| H(2)···H(11)vii | 3.268 | H(17)···O(2)vi | 3.038 |
| H(2)···H(12)vii | 3.327 | H(17)···C(5)xiii | 3.430 |
| H(3)···O(3)vii | 2.920 | H(17)···H(1)vi | 3.545 |
| H(3)···O(5)vii | 3.151 | H(17)···H(5)vi | 3.321 |
| H(3)···C(3)vii | 3.305 | H(17)···H(12)i | 3.161 |
| H(3)···H(7)vii | 2.900 | H(17)···H(14)xiii | 2.492 |
| H(3)···H(8)vii | 3.543 | H(18)···Cl(1)ii | 3.571 |
| H(3)···H(11)x | 3.021 | H(18)···Cl(2)ii | 3.031 |
| H(3)···H(14)vii | 3.538 | H(18)···H(6)ii | 3.466 |
| H(4)···Cl(2)iv | 3.151 | H(18)···H(7)vii | 3.489 |
| H(4)···O(1)viii | 3.457 | H(18)···H(8)vii | 3.229 |
| H(4)···O(4)viii | 3.429 | H(18)···H(14)xiii | 3.040 |
| 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) | 109.5 | O(6)—C(6)—H(16) | 109.5 |
| O(1)—C(1)—H(2) | 109.5 | O(6)—C(6)—H(17) | 109.5 |
| O(1)—C(1)—H(3) | 109.5 | O(6)—C(6)—H(18) | 109.5 |
| H(1)—C(1)—H(2) | 109.5 | H(16)—C(6)—H(17) | 109.5 |
| H(1)—C(1)—H(3) | 109.5 | H(16)—C(6)—H(18) | 109.5 |
| H(2)—C(1)—H(3) | 109.5 | H(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. |
| 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) |
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[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 .