Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100007642/qa0303sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270100007642/qa0303Isup2.hkl |
CCDC reference: 147683
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.
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.
[PdCl2(C18H15O3P)2] | F(000) = 1616 |
Mr = 797.90 | Dx = 1.548 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 9.2007 (9) Å | Cell parameters from 5000 reflections |
b = 12.2973 (17) Å | θ = 2.1–26.1° |
c = 30.421 (3) Å | µ = 0.84 mm−1 |
β = 93.260 (12)° | T = 213 K |
V = 3436.4 (7) Å3 | Plate, colourless |
Z = 4 | 0.28 × 0.16 × 0.12 mm |
Stoe IPDS diffractometer | 6755 independent reflections |
Radiation source: fine-focus sealed tube | 4139 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.091 |
Detector resolution: 6.67 pixels mm-1 | θmax = 26.1°, θmin = 2.1° |
Image plate scans | h = −11→11 |
Absorption correction: numerical (X-SHAPE; Stoe, 1997) | k = −15→15 |
Tmin = 0.818, Tmax = 0.916 | l = −37→37 |
26396 measured reflections |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.044 | Calculated w = 1/[σ2(Fo2) + (0.0337P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.107 | (Δ/σ)max = 0.002 |
S = 0.86 | Δρmax = 0.97 e Å−3 |
6755 reflections | Δρmin = −1.30 e Å−3 |
424 parameters |
[PdCl2(C18H15O3P)2] | V = 3436.4 (7) Å3 |
Mr = 797.90 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 9.2007 (9) Å | µ = 0.84 mm−1 |
b = 12.2973 (17) Å | T = 213 K |
c = 30.421 (3) Å | 0.28 × 0.16 × 0.12 mm |
β = 93.260 (12)° |
Stoe IPDS diffractometer | 6755 independent reflections |
Absorption correction: numerical (X-SHAPE; Stoe, 1997) | 4139 reflections with I > 2σ(I) |
Tmin = 0.818, Tmax = 0.916 | Rint = 0.091 |
26396 measured reflections |
R[F2 > 2σ(F2)] = 0.044 | 0 restraints |
wR(F2) = 0.107 | H-atom parameters constrained |
S = 0.86 | Δρmax = 0.97 e Å−3 |
6755 reflections | Δρmin = −1.30 e Å−3 |
424 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
C1 | 1.2657 (4) | 0.0399 (4) | 0.88103 (14) | 0.0273 (10) | |
C2 | 1.1726 (5) | −0.0427 (4) | 0.88995 (17) | 0.0404 (12) | |
H2 | 1.0877 | −0.0548 | 0.8720 | 0.048* | |
C3 | 1.2066 (6) | −0.1083 (4) | 0.92620 (19) | 0.0503 (14) | |
H3 | 1.1443 | −0.1658 | 0.9329 | 0.060* | |
C4 | 1.3308 (6) | −0.0895 (5) | 0.95233 (19) | 0.0568 (16) | |
H4 | 1.3537 | −0.1343 | 0.9768 | 0.068* | |
C5 | 1.4216 (6) | −0.0050 (6) | 0.94258 (18) | 0.0581 (17) | |
H5 | 1.5064 | 0.0077 | 0.9606 | 0.070* | |
C6 | 1.3902 (5) | 0.0609 (4) | 0.90698 (16) | 0.0411 (13) | |
H6 | 1.4519 | 0.1189 | 0.9004 | 0.049* | |
C7 | 1.0520 (5) | 0.2469 (4) | 0.74996 (14) | 0.0284 (10) | |
C8 | 1.0908 (5) | 0.2190 (5) | 0.70793 (15) | 0.0421 (12) | |
H8 | 1.1458 | 0.1562 | 0.7029 | 0.051* | |
C9 | 1.0444 (6) | 0.2883 (6) | 0.67336 (17) | 0.0575 (16) | |
H9 | 1.0689 | 0.2719 | 0.6445 | 0.069* | |
C10 | 0.9642 (6) | 0.3791 (6) | 0.68083 (19) | 0.0568 (16) | |
H10 | 0.9345 | 0.4246 | 0.6572 | 0.068* | |
C11 | 0.9270 (5) | 0.4043 (5) | 0.72230 (18) | 0.0471 (14) | |
H11 | 0.8727 | 0.4675 | 0.7271 | 0.057* | |
C12 | 0.9689 (5) | 0.3367 (4) | 0.75768 (16) | 0.0361 (11) | |
H12 | 0.9408 | 0.3525 | 0.7862 | 0.043* | |
C13 | 1.3485 (4) | 0.3253 (4) | 0.80558 (14) | 0.0267 (10) | |
C14 | 1.4771 (5) | 0.2681 (4) | 0.81075 (15) | 0.0333 (11) | |
H14 | 1.4928 | 0.2183 | 0.8340 | 0.040* | |
C15 | 1.5830 (5) | 0.2860 (4) | 0.78079 (16) | 0.0389 (11) | |
H15 | 1.6719 | 0.2483 | 0.7837 | 0.047* | |
C16 | 1.5577 (5) | 0.3588 (4) | 0.74691 (16) | 0.0384 (12) | |
H16 | 1.6286 | 0.3691 | 0.7262 | 0.046* | |
C17 | 1.4303 (5) | 0.4164 (4) | 0.74304 (16) | 0.0364 (11) | |
H17 | 1.4151 | 0.4669 | 0.7200 | 0.044* | |
C18 | 1.3240 (5) | 0.4010 (4) | 0.77271 (15) | 0.0321 (11) | |
H18 | 1.2370 | 0.4412 | 0.7705 | 0.039* | |
C19 | 1.0823 (4) | 0.2468 (4) | 1.00593 (14) | 0.0274 (10) | |
C20 | 1.1209 (5) | 0.2895 (4) | 1.04674 (15) | 0.0392 (11) | |
H20 | 1.1069 | 0.3638 | 1.0524 | 0.047* | |
C21 | 1.1806 (6) | 0.2217 (5) | 1.07947 (17) | 0.0508 (14) | |
H21 | 1.2062 | 0.2496 | 1.1076 | 0.061* | |
C22 | 1.2023 (5) | 0.1131 (5) | 1.07056 (17) | 0.0439 (13) | |
H22 | 1.2426 | 0.0669 | 1.0927 | 0.053* | |
C23 | 1.1652 (6) | 0.0726 (4) | 1.02955 (17) | 0.0454 (13) | |
H23 | 1.1814 | −0.0012 | 1.0235 | 0.055* | |
C24 | 1.1040 (5) | 0.1397 (4) | 0.99692 (16) | 0.0380 (12) | |
H24 | 1.0777 | 0.1116 | 0.9688 | 0.046* | |
C25 | 0.9235 (5) | 0.4918 (4) | 0.87866 (15) | 0.0305 (11) | |
C26 | 1.0157 (6) | 0.5589 (5) | 0.85747 (18) | 0.0495 (14) | |
H26 | 1.1129 | 0.5676 | 0.8681 | 0.059* | |
C27 | 0.9630 (7) | 0.6138 (5) | 0.8201 (2) | 0.0662 (18) | |
H27 | 1.0241 | 0.6613 | 0.8054 | 0.079* | |
C28 | 0.8204 (7) | 0.5986 (5) | 0.8044 (2) | 0.0601 (17) | |
H28 | 0.7846 | 0.6362 | 0.7792 | 0.072* | |
C29 | 0.7311 (6) | 0.5292 (4) | 0.82538 (19) | 0.0495 (14) | |
H29 | 0.6348 | 0.5185 | 0.8142 | 0.059* | |
C30 | 0.7817 (5) | 0.4752 (4) | 0.86260 (17) | 0.0387 (12) | |
H30 | 0.7205 | 0.4274 | 0.8771 | 0.046* | |
C31 | 1.2912 (4) | 0.4462 (4) | 0.93906 (15) | 0.0286 (10) | |
C32 | 1.4124 (5) | 0.4696 (4) | 0.91597 (18) | 0.0450 (13) | |
H32 | 1.4400 | 0.4245 | 0.8929 | 0.054* | |
C33 | 1.4920 (6) | 0.5616 (5) | 0.9279 (2) | 0.0580 (17) | |
H33 | 1.5740 | 0.5797 | 0.9123 | 0.070* | |
C34 | 1.4537 (6) | 0.6266 (4) | 0.9618 (2) | 0.0500 (14) | |
H34 | 1.5096 | 0.6884 | 0.9696 | 0.060* | |
C35 | 1.3332 (5) | 0.6013 (4) | 0.98436 (18) | 0.0432 (13) | |
H35 | 1.3066 | 0.6458 | 1.0077 | 0.052* | |
C36 | 1.2512 (5) | 0.5107 (4) | 0.97289 (16) | 0.0383 (12) | |
H36 | 1.1683 | 0.4935 | 0.9882 | 0.046* | |
O1 | 1.2429 (3) | 0.0997 (2) | 0.84164 (10) | 0.0315 (7) | |
O2 | 1.1065 (3) | 0.1769 (2) | 0.78323 (9) | 0.0293 (7) | |
O3 | 1.2360 (3) | 0.3082 (2) | 0.83514 (9) | 0.0289 (7) | |
O4 | 1.0118 (3) | 0.3188 (2) | 0.97574 (9) | 0.0274 (7) | |
O5 | 0.9685 (3) | 0.4469 (2) | 0.92002 (10) | 0.0299 (7) | |
O6 | 1.2143 (3) | 0.3506 (2) | 0.92510 (10) | 0.0293 (7) | |
P1 | 1.13885 (11) | 0.20135 (9) | 0.83398 (3) | 0.0222 (2) | |
P2 | 1.04409 (12) | 0.33164 (9) | 0.92555 (4) | 0.0232 (2) | |
Cl1 | 0.84326 (12) | 0.08008 (9) | 0.83039 (4) | 0.0334 (3) | |
Cl2 | 0.74995 (11) | 0.20810 (10) | 0.92057 (4) | 0.0348 (3) | |
Pd1 | 0.95339 (3) | 0.20752 (3) | 0.878026 (10) | 0.02092 (10) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.028 (2) | 0.033 (2) | 0.021 (2) | 0.0047 (19) | 0.0048 (18) | 0.006 (2) |
C2 | 0.037 (3) | 0.039 (3) | 0.045 (3) | −0.006 (2) | 0.005 (2) | 0.005 (3) |
C3 | 0.068 (4) | 0.033 (3) | 0.052 (4) | 0.004 (3) | 0.021 (3) | 0.014 (3) |
C4 | 0.067 (4) | 0.061 (4) | 0.043 (4) | 0.026 (3) | 0.010 (3) | 0.021 (3) |
C5 | 0.045 (3) | 0.095 (5) | 0.034 (3) | 0.004 (3) | −0.003 (3) | 0.013 (3) |
C6 | 0.039 (3) | 0.056 (3) | 0.028 (3) | −0.012 (2) | 0.001 (2) | 0.007 (2) |
C7 | 0.028 (2) | 0.037 (2) | 0.020 (2) | −0.007 (2) | −0.0018 (18) | 0.007 (2) |
C8 | 0.048 (3) | 0.052 (3) | 0.026 (3) | −0.007 (3) | 0.004 (2) | −0.003 (3) |
C9 | 0.065 (4) | 0.086 (5) | 0.021 (3) | −0.012 (4) | −0.001 (2) | 0.006 (3) |
C10 | 0.048 (3) | 0.078 (4) | 0.043 (4) | −0.004 (3) | −0.011 (3) | 0.027 (3) |
C11 | 0.031 (3) | 0.063 (4) | 0.047 (3) | 0.003 (2) | −0.004 (2) | 0.018 (3) |
C12 | 0.032 (3) | 0.048 (3) | 0.028 (3) | 0.001 (2) | 0.002 (2) | 0.009 (2) |
C13 | 0.028 (2) | 0.032 (2) | 0.021 (2) | −0.0071 (18) | 0.0059 (18) | −0.0040 (19) |
C14 | 0.031 (2) | 0.040 (3) | 0.028 (3) | −0.002 (2) | −0.0010 (19) | 0.008 (2) |
C15 | 0.032 (2) | 0.041 (3) | 0.044 (3) | −0.001 (2) | 0.006 (2) | 0.004 (3) |
C16 | 0.040 (3) | 0.041 (3) | 0.035 (3) | −0.008 (2) | 0.009 (2) | 0.003 (2) |
C17 | 0.041 (3) | 0.038 (3) | 0.030 (3) | −0.013 (2) | 0.001 (2) | 0.011 (2) |
C18 | 0.030 (2) | 0.030 (3) | 0.036 (3) | −0.0037 (19) | −0.003 (2) | 0.005 (2) |
C19 | 0.028 (2) | 0.031 (2) | 0.024 (2) | −0.0028 (19) | 0.0013 (18) | 0.003 (2) |
C20 | 0.057 (3) | 0.031 (3) | 0.028 (3) | −0.004 (2) | −0.010 (2) | −0.005 (2) |
C21 | 0.070 (4) | 0.055 (4) | 0.026 (3) | −0.006 (3) | −0.013 (2) | 0.001 (3) |
C22 | 0.044 (3) | 0.050 (3) | 0.037 (3) | 0.003 (2) | −0.002 (2) | 0.006 (3) |
C23 | 0.062 (3) | 0.036 (3) | 0.040 (3) | 0.011 (3) | 0.009 (3) | 0.003 (2) |
C24 | 0.060 (3) | 0.031 (3) | 0.022 (3) | 0.004 (2) | 0.000 (2) | −0.001 (2) |
C25 | 0.038 (3) | 0.028 (2) | 0.024 (2) | 0.0062 (19) | −0.001 (2) | −0.002 (2) |
C26 | 0.044 (3) | 0.057 (4) | 0.048 (3) | 0.005 (3) | 0.003 (3) | 0.019 (3) |
C27 | 0.071 (4) | 0.073 (5) | 0.055 (4) | 0.010 (3) | 0.012 (3) | 0.035 (4) |
C28 | 0.075 (4) | 0.063 (4) | 0.041 (3) | 0.022 (3) | −0.007 (3) | 0.014 (3) |
C29 | 0.051 (3) | 0.043 (3) | 0.052 (4) | 0.013 (3) | −0.021 (3) | −0.005 (3) |
C30 | 0.042 (3) | 0.033 (3) | 0.041 (3) | 0.004 (2) | −0.003 (2) | −0.007 (2) |
C31 | 0.026 (2) | 0.030 (3) | 0.029 (3) | −0.0030 (19) | −0.0029 (19) | −0.003 (2) |
C32 | 0.037 (3) | 0.051 (3) | 0.047 (3) | −0.011 (2) | 0.013 (2) | −0.018 (3) |
C33 | 0.040 (3) | 0.057 (4) | 0.079 (5) | −0.020 (3) | 0.016 (3) | −0.020 (3) |
C34 | 0.047 (3) | 0.039 (3) | 0.064 (4) | −0.011 (2) | 0.003 (3) | −0.017 (3) |
C35 | 0.046 (3) | 0.037 (3) | 0.047 (3) | −0.005 (2) | 0.006 (2) | −0.015 (3) |
C36 | 0.045 (3) | 0.038 (3) | 0.033 (3) | −0.009 (2) | 0.006 (2) | −0.009 (2) |
O1 | 0.0333 (16) | 0.0343 (18) | 0.0276 (18) | 0.0113 (14) | 0.0085 (13) | 0.0100 (15) |
O2 | 0.0379 (17) | 0.0332 (17) | 0.0167 (15) | 0.0010 (13) | 0.0000 (13) | −0.0016 (13) |
O3 | 0.0295 (15) | 0.0323 (18) | 0.0257 (16) | −0.0090 (13) | 0.0087 (12) | −0.0047 (14) |
O4 | 0.0353 (16) | 0.0330 (18) | 0.0137 (15) | 0.0031 (13) | 0.0012 (12) | −0.0006 (13) |
O5 | 0.0409 (17) | 0.0230 (16) | 0.0256 (17) | 0.0049 (14) | −0.0009 (14) | −0.0007 (13) |
O6 | 0.0246 (15) | 0.0329 (17) | 0.0309 (18) | −0.0072 (13) | 0.0046 (13) | −0.0120 (14) |
P1 | 0.0264 (5) | 0.0229 (6) | 0.0172 (5) | 0.0007 (5) | 0.0010 (4) | 0.0004 (5) |
P2 | 0.0262 (6) | 0.0236 (6) | 0.0199 (6) | 0.0005 (4) | 0.0017 (4) | −0.0008 (5) |
Cl1 | 0.0332 (6) | 0.0346 (6) | 0.0318 (6) | −0.0066 (5) | −0.0031 (5) | −0.0099 (5) |
Cl2 | 0.0295 (5) | 0.0389 (6) | 0.0370 (7) | −0.0048 (5) | 0.0109 (5) | −0.0057 (6) |
Pd1 | 0.02192 (16) | 0.02207 (17) | 0.01869 (17) | −0.00056 (14) | 0.00047 (11) | −0.00133 (15) |
C1—C2 | 1.365 (6) | C22—C23 | 1.368 (7) |
C1—C6 | 1.378 (6) | C23—C24 | 1.385 (7) |
C1—O1 | 1.412 (5) | C25—C26 | 1.371 (7) |
C2—C3 | 1.388 (7) | C25—C30 | 1.381 (6) |
C3—C4 | 1.374 (8) | C25—O5 | 1.414 (5) |
C4—C5 | 1.376 (8) | C26—C27 | 1.386 (7) |
C5—C6 | 1.370 (7) | C27—C28 | 1.383 (8) |
C7—C12 | 1.371 (6) | C28—C29 | 1.367 (8) |
C7—C8 | 1.390 (6) | C29—C30 | 1.371 (7) |
C7—O2 | 1.400 (5) | C31—C36 | 1.367 (6) |
C8—C9 | 1.401 (7) | C31—C32 | 1.382 (6) |
C9—C10 | 1.365 (8) | C31—O6 | 1.424 (5) |
C10—C11 | 1.362 (8) | C32—C33 | 1.384 (7) |
C11—C12 | 1.397 (7) | C33—C34 | 1.367 (8) |
C13—C18 | 1.376 (6) | C34—C35 | 1.372 (7) |
C13—C14 | 1.378 (6) | C35—C36 | 1.379 (6) |
C13—O3 | 1.425 (5) | O1—P1 | 1.583 (3) |
C14—C15 | 1.389 (6) | O2—P1 | 1.585 (3) |
C15—C16 | 1.375 (7) | O3—P1 | 1.588 (3) |
C16—C17 | 1.369 (7) | O4—P2 | 1.580 (3) |
C17—C18 | 1.381 (6) | O5—P2 | 1.584 (3) |
C19—C24 | 1.363 (6) | O6—P2 | 1.584 (3) |
C19—C20 | 1.376 (6) | P1—Pd1 | 2.2299 (11) |
C19—O4 | 1.408 (5) | P2—Pd1 | 2.2314 (12) |
C20—C21 | 1.388 (7) | Cl1—Pd1 | 2.3273 (11) |
C21—C22 | 1.379 (7) | Cl2—Pd1 | 2.3354 (11) |
C2—C1—C6 | 122.4 (4) | C28—C27—C26 | 119.8 (6) |
C2—C1—O1 | 119.5 (4) | C29—C28—C27 | 120.5 (5) |
C6—C1—O1 | 117.8 (4) | C28—C29—C30 | 120.2 (5) |
C1—C2—C3 | 118.4 (5) | C29—C30—C25 | 119.4 (5) |
C4—C3—C2 | 120.3 (5) | C36—C31—C32 | 121.5 (4) |
C3—C4—C5 | 119.8 (5) | C36—C31—O6 | 123.6 (4) |
C6—C5—C4 | 120.9 (5) | C32—C31—O6 | 115.0 (4) |
C5—C6—C1 | 118.2 (5) | C31—C32—C33 | 117.9 (5) |
C12—C7—C8 | 122.1 (4) | C34—C33—C32 | 121.4 (5) |
C12—C7—O2 | 123.5 (4) | C33—C34—C35 | 119.7 (5) |
C8—C7—O2 | 114.4 (4) | C34—C35—C36 | 120.2 (5) |
C7—C8—C9 | 117.2 (5) | C31—C36—C35 | 119.5 (5) |
C10—C9—C8 | 121.2 (5) | C1—O1—P1 | 126.6 (3) |
C11—C10—C9 | 120.5 (5) | C7—O2—P1 | 128.9 (3) |
C10—C11—C12 | 120.3 (5) | C13—O3—P1 | 122.4 (3) |
C7—C12—C11 | 118.7 (5) | C19—O4—P2 | 126.0 (3) |
C18—C13—C14 | 122.2 (4) | C25—O5—P2 | 123.2 (3) |
C18—C13—O3 | 117.6 (4) | C31—O6—P2 | 126.4 (3) |
C14—C13—O3 | 120.2 (4) | O1—P1—O2 | 94.12 (16) |
C13—C14—C15 | 118.3 (4) | O1—P1—O3 | 108.35 (16) |
C16—C15—C14 | 120.0 (4) | O2—P1—O3 | 104.66 (16) |
C17—C16—C15 | 120.6 (4) | O1—P1—Pd1 | 114.54 (12) |
C16—C17—C18 | 120.5 (4) | O2—P1—Pd1 | 118.95 (12) |
C13—C18—C17 | 118.4 (4) | O3—P1—Pd1 | 114.05 (12) |
C24—C19—C20 | 121.1 (4) | O4—P2—O5 | 94.95 (16) |
C24—C19—O4 | 123.0 (4) | O4—P2—O6 | 105.28 (16) |
C20—C19—O4 | 115.8 (4) | O5—P2—O6 | 107.18 (17) |
C19—C20—C21 | 119.3 (5) | O4—P2—Pd1 | 118.29 (12) |
C22—C21—C20 | 119.8 (5) | O5—P2—Pd1 | 113.44 (12) |
C23—C22—C21 | 120.0 (5) | O6—P2—Pd1 | 115.38 (12) |
C22—C23—C24 | 120.5 (5) | P1—Pd1—P2 | 98.15 (4) |
C19—C24—C23 | 119.3 (4) | P1—Pd1—Cl1 | 85.63 (4) |
C26—C25—C30 | 121.3 (5) | P2—Pd1—Cl1 | 176.07 (4) |
C26—C25—O5 | 119.7 (4) | P1—Pd1—Cl2 | 176.26 (4) |
C30—C25—O5 | 118.7 (4) | P2—Pd1—Cl2 | 85.46 (4) |
C25—C26—C27 | 118.8 (5) | Cl1—Pd1—Cl2 | 90.74 (4) |
C6—C1—C2—C3 | −0.9 (7) | C2—C1—O1—P1 | 85.3 (5) |
O1—C1—C2—C3 | 172.7 (4) | C6—C1—O1—P1 | −100.9 (5) |
C1—C2—C3—C4 | 0.3 (8) | C12—C7—O2—P1 | −24.6 (6) |
C2—C3—C4—C5 | 0.3 (9) | C8—C7—O2—P1 | 154.5 (3) |
C3—C4—C5—C6 | −0.2 (9) | C18—C13—O3—P1 | 107.6 (4) |
C4—C5—C6—C1 | −0.4 (8) | C14—C13—O3—P1 | −73.2 (5) |
C2—C1—C6—C5 | 1.0 (8) | C24—C19—O4—P2 | −47.8 (6) |
O1—C1—C6—C5 | −172.7 (5) | C20—C19—O4—P2 | 136.2 (4) |
C12—C7—C8—C9 | 1.5 (7) | C26—C25—O5—P2 | −93.0 (5) |
O2—C7—C8—C9 | −177.6 (4) | C30—C25—O5—P2 | 93.3 (4) |
C7—C8—C9—C10 | −0.2 (8) | C36—C31—O6—P2 | 33.6 (6) |
C8—C9—C10—C11 | −0.2 (9) | C32—C31—O6—P2 | −147.0 (4) |
C9—C10—C11—C12 | −0.8 (8) | C1—O1—P1—O2 | −150.3 (3) |
C8—C7—C12—C11 | −2.5 (7) | C1—O1—P1—O3 | 102.8 (3) |
O2—C7—C12—C11 | 176.5 (4) | C1—O1—P1—Pd1 | −25.8 (4) |
C10—C11—C12—C7 | 2.1 (7) | C7—O2—P1—O1 | −161.2 (3) |
C18—C13—C14—C15 | −1.9 (7) | C7—O2—P1—O3 | −51.1 (4) |
O3—C13—C14—C15 | 179.0 (4) | C7—O2—P1—Pd1 | 77.7 (3) |
C13—C14—C15—C16 | −0.3 (7) | C13—O3—P1—O1 | 58.8 (3) |
C14—C15—C16—C17 | 1.8 (7) | C13—O3—P1—O2 | −40.7 (3) |
C15—C16—C17—C18 | −1.1 (7) | C13—O3—P1—Pd1 | −172.3 (3) |
C14—C13—C18—C17 | 2.6 (7) | C19—O4—P2—O5 | −161.7 (3) |
O3—C13—C18—C17 | −178.3 (4) | C19—O4—P2—O6 | −52.4 (3) |
C16—C17—C18—C13 | −1.1 (7) | C19—O4—P2—Pd1 | 78.3 (3) |
C24—C19—C20—C21 | −1.1 (8) | C25—O5—P2—O4 | −161.4 (3) |
O4—C19—C20—C21 | 175.0 (4) | C25—O5—P2—O6 | 90.9 (3) |
C19—C20—C21—C22 | 0.9 (8) | C25—O5—P2—Pd1 | −37.6 (3) |
C20—C21—C22—C23 | 0.1 (8) | C31—O6—P2—O4 | −71.6 (4) |
C21—C22—C23—C24 | −0.8 (8) | C31—O6—P2—O5 | 28.6 (4) |
C20—C19—C24—C23 | 0.3 (7) | C31—O6—P2—Pd1 | 156.0 (3) |
O4—C19—C24—C23 | −175.5 (4) | O1—P1—Pd1—P2 | 101.86 (14) |
C22—C23—C24—C19 | 0.6 (8) | O2—P1—Pd1—P2 | −148.09 (14) |
C30—C25—C26—C27 | 2.2 (8) | O3—P1—Pd1—P2 | −23.79 (13) |
O5—C25—C26—C27 | −171.3 (5) | O1—P1—Pd1—Cl1 | −79.19 (14) |
C25—C26—C27—C28 | −1.2 (9) | O2—P1—Pd1—Cl1 | 30.87 (14) |
C26—C27—C28—C29 | −0.4 (10) | O3—P1—Pd1—Cl1 | 155.17 (13) |
C27—C28—C29—C30 | 1.0 (9) | O1—P1—Pd1—Cl2 | −93.2 (7) |
C28—C29—C30—C25 | 0.0 (8) | O2—P1—Pd1—Cl2 | 16.8 (8) |
C26—C25—C30—C29 | −1.7 (7) | O3—P1—Pd1—Cl2 | 141.1 (7) |
O5—C25—C30—C29 | 171.9 (4) | O4—P2—Pd1—P1 | −143.71 (13) |
C36—C31—C32—C33 | −0.7 (8) | O5—P2—Pd1—P1 | 106.41 (13) |
O6—C31—C32—C33 | 179.9 (5) | O6—P2—Pd1—P1 | −17.79 (14) |
C31—C32—C33—C34 | 1.0 (9) | O4—P2—Pd1—Cl1 | 51.7 (7) |
C32—C33—C34—C35 | −0.6 (9) | O5—P2—Pd1—Cl1 | −58.2 (7) |
C33—C34—C35—C36 | −0.1 (9) | O6—P2—Pd1—Cl1 | 178 (15) |
C32—C31—C36—C35 | 0.0 (7) | O4—P2—Pd1—Cl2 | 37.27 (13) |
O6—C31—C36—C35 | 179.4 (4) | O5—P2—Pd1—Cl2 | −72.61 (14) |
C34—C35—C36—C31 | 0.4 (8) | O6—P2—Pd1—Cl2 | 163.18 (14) |
Experimental details
Crystal data | |
Chemical formula | [PdCl2(C18H15O3P)2] |
Mr | 797.90 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 213 |
a, b, c (Å) | 9.2007 (9), 12.2973 (17), 30.421 (3) |
β (°) | 93.260 (12) |
V (Å3) | 3436.4 (7) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.84 |
Crystal size (mm) | 0.28 × 0.16 × 0.12 |
Data collection | |
Diffractometer | Stoe IPDS diffractometer |
Absorption correction | Numerical (X-SHAPE; Stoe, 1997) |
Tmin, Tmax | 0.818, 0.916 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 26396, 6755, 4139 |
Rint | 0.091 |
(sin θ/λ)max (Å−1) | 0.620 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.044, 0.107, 0.86 |
No. of reflections | 6755 |
No. of parameters | 424 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 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.
O1—P1 | 1.583 (3) | O6—P2 | 1.584 (3) |
O2—P1 | 1.585 (3) | P1—Pd1 | 2.2299 (11) |
O3—P1 | 1.588 (3) | P2—Pd1 | 2.2314 (12) |
O4—P2 | 1.580 (3) | Cl1—Pd1 | 2.3273 (11) |
O5—P2 | 1.584 (3) | Cl2—Pd1 | 2.3354 (11) |
O1—P1—O2 | 94.12 (16) | O4—P2—Pd1 | 118.29 (12) |
O1—P1—O3 | 108.35 (16) | O5—P2—Pd1 | 113.44 (12) |
O2—P1—O3 | 104.66 (16) | O6—P2—Pd1 | 115.38 (12) |
O1—P1—Pd1 | 114.54 (12) | P1—Pd1—P2 | 98.15 (4) |
O2—P1—Pd1 | 118.95 (12) | P1—Pd1—Cl1 | 85.63 (4) |
O3—P1—Pd1 | 114.05 (12) | P2—Pd1—Cl1 | 176.07 (4) |
O4—P2—O5 | 94.95 (16) | P1—Pd1—Cl2 | 176.26 (4) |
O4—P2—O6 | 105.28 (16) | P2—Pd1—Cl2 | 85.46 (4) |
O5—P2—O6 | 107.18 (17) | Cl1—Pd1—Cl2 | 90.74 (4) |
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).