Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807031005/gg2017sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807031005/gg2017Isup2.hkl |
CCDC reference: 654839
Key indicators
- Single-crystal X-ray study
- T = 125 K
- Mean (C-C)= 0.006 Å
- R factor = 0.041
- wR factor = 0.062
- Data-to-parameter ratio = 19.5
checkCIF/PLATON results
No syntax errors found No errors found in this datablock
For related literature on PtCl2L2 complexes, see: Bao et al. (1987); Fun et al. (2006); Slawin et al. (2007).
Cg1 and Cg2 are the centroids of the C7–c12 and C20–C25 rings.
0.8 g (2.14 mmol) of PtCl2(COD) was dissolved in the minimum volume of dichloromethane in a round-bottomed flask. To this, 0.921 ml (4.28 mmol) of methyldiphenylphosphinite was added. The solution was then 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, [PtCl2(P(OMe)Ph2)2] (1.93 mmol,ca 90%. 31P-{1H} NMR: δ 85.2 p.p.m. J{Pt—P} 4183 Hz.
All H atoms were included in calculated positions (C—H distances are 0.96 Å for methyl H atoms, 0.97 Å for methylene H atoms and 0.98 Å for methine H atoms) and were refined as riding atoms with Uiso(H) = 1.2 Ueq(parent atom, methylene and methine H atoms) or Uiso(H) = 1.5 Ueq(parent atom, methyl H atoms).
The title complex (I) can be compared to similar platinum dichloride complexes containing trimethoxy phosphite; [PtCl2(P(OMe)3)2] (Bao et al., 1987) and triphenyl phosphine [PtCl2(PPh3)2] (Fun et al., 2006). The geometry at the platinum atom in the title compound (I) bears a closer resemblance to the triphenyl phosphine complex and can be compared with [PtCl2(P(OMe)2Ph)2] (Slawin et al., 2007).
For related literature on PtCl2L2 complexes, see: Bao et al. (1987); Fun et al. (2006); Slawin et al. (2007).
Cg1 and Cg2 are the centroids of the C7–c12 and C20–C25 rings.
Data collection: SCXmini Software (Rigaku/MSC, 2006); cell refinement: PROCESS-AUTO (Rigaku, 1998); data reduction: PROCESS-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: CrystalStructure (Rigaku/MSC, 2006); software used to prepare material for publication: CrystalStructure.
Fig. 1. The structure of (1) with displacement ellipsoids drawn at the 50% probability level, H atoms omitted for clarity. |
[PtCl2(C13H13OP)2] | F(000) = 1360.00 |
Mr = 698.43 | Dx = 1.824 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71075 Å |
Hall symbol: -P 2yn | Cell parameters from 23439 reflections |
a = 12.4262 (6) Å | θ = 3.1–27.6° |
b = 13.6280 (7) Å | µ = 5.85 mm−1 |
c = 15.0494 (8) Å | T = 125 K |
β = 93.5316 (11)° | Prism, colorless |
V = 2543.7 (2) Å3 | 0.25 × 0.15 × 0.12 mm |
Z = 4 |
Rigaku SCXmini diffractometer | 4910 reflections with F2 > 2σ(F2) |
Detector resolution: 6.85 pixels mm-1 | Rint = 0.057 |
ω scans | θmax = 27.5° |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | h = −16→16 |
Tmin = 0.377, Tmax = 0.495 | k = −17→17 |
26133 measured reflections | l = −19→19 |
5827 independent reflections |
Refinement on F2 | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.041 | w = 1/[σ2(Fo2) + (0.0124P)2 + 7.7753P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.062 | (Δ/σ)max = 0.002 |
S = 1.13 | Δρmax = 0.99 e Å−3 |
5827 reflections | Δρmin = −1.02 e Å−3 |
299 parameters |
[PtCl2(C13H13OP)2] | V = 2543.7 (2) Å3 |
Mr = 698.43 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 12.4262 (6) Å | µ = 5.85 mm−1 |
b = 13.6280 (7) Å | T = 125 K |
c = 15.0494 (8) Å | 0.25 × 0.15 × 0.12 mm |
β = 93.5316 (11)° |
Rigaku SCXmini diffractometer | 5827 independent reflections |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | 4910 reflections with F2 > 2σ(F2) |
Tmin = 0.377, Tmax = 0.495 | Rint = 0.057 |
26133 measured reflections |
R[F2 > 2σ(F2)] = 0.041 | 299 parameters |
wR(F2) = 0.062 | H-atom parameters constrained |
S = 1.13 | Δρmax = 0.99 e Å−3 |
5827 reflections | Δρmin = −1.02 e Å−3 |
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 | ||
Pt(1) | 0.075336 (15) | 0.162861 (13) | 0.837844 (12) | 0.01364 (4) | |
Cl(1) | 0.10233 (10) | 0.03053 (9) | 0.73956 (8) | 0.0204 (2) | |
Cl(2) | −0.11089 (10) | 0.12977 (9) | 0.82742 (9) | 0.0229 (2) | |
P(1) | 0.25475 (9) | 0.16303 (10) | 0.85328 (8) | 0.0146 (2) | |
P(2) | 0.04528 (10) | 0.29335 (9) | 0.92198 (8) | 0.0135 (2) | |
O(1) | 0.3161 (2) | 0.1781 (2) | 0.7644 (2) | 0.0205 (7) | |
O(2) | 0.1320 (2) | 0.3806 (2) | 0.9213 (2) | 0.0162 (7) | |
C(1) | 0.3066 (3) | 0.0446 (3) | 0.8932 (3) | 0.0165 (10) | |
C(2) | 0.4104 (4) | 0.0170 (3) | 0.8755 (3) | 0.0229 (11) | |
C(3) | 0.4538 (4) | −0.0690 (3) | 0.9111 (3) | 0.0261 (12) | |
C(4) | 0.3943 (4) | −0.1272 (3) | 0.9644 (3) | 0.0277 (12) | |
C(5) | 0.2914 (4) | −0.0996 (3) | 0.9842 (3) | 0.0285 (12) | |
C(6) | 0.2473 (4) | −0.0138 (3) | 0.9477 (3) | 0.0238 (11) | |
C(7) | 0.3255 (3) | 0.2451 (3) | 0.9318 (3) | 0.0161 (10) | |
C(8) | 0.3143 (3) | 0.2328 (3) | 1.0229 (3) | 0.0182 (10) | |
C(9) | 0.3715 (4) | 0.2924 (3) | 1.0838 (3) | 0.0267 (12) | |
C(10) | 0.4417 (4) | 0.3621 (3) | 1.0537 (4) | 0.0279 (13) | |
C(11) | 0.4526 (4) | 0.3749 (3) | 0.9635 (3) | 0.0273 (12) | |
C(12) | 0.3945 (3) | 0.3163 (3) | 0.9024 (3) | 0.0219 (11) | |
C(13) | 0.2720 (4) | 0.2348 (4) | 0.6905 (3) | 0.0297 (13) | |
C(14) | 0.0499 (3) | 0.2684 (3) | 1.0394 (3) | 0.0156 (10) | |
C(15) | 0.0338 (3) | 0.1735 (3) | 1.0697 (3) | 0.0221 (11) | |
C(16) | 0.0487 (4) | 0.1518 (4) | 1.1591 (3) | 0.0287 (12) | |
C(17) | 0.0785 (4) | 0.2256 (4) | 1.2200 (3) | 0.0271 (12) | |
C(18) | 0.0940 (4) | 0.3196 (4) | 1.1909 (3) | 0.0267 (12) | |
C(19) | 0.0800 (3) | 0.3427 (3) | 1.1010 (3) | 0.0193 (10) | |
C(20) | −0.0821 (3) | 0.3548 (3) | 0.8926 (3) | 0.0167 (10) | |
C(21) | −0.1502 (4) | 0.3860 (3) | 0.9576 (3) | 0.0201 (11) | |
C(22) | −0.2438 (4) | 0.4369 (3) | 0.9331 (3) | 0.0264 (12) | |
C(23) | −0.2699 (4) | 0.4580 (3) | 0.8444 (3) | 0.0251 (12) | |
C(24) | −0.2024 (4) | 0.4278 (3) | 0.7794 (3) | 0.0246 (12) | |
C(25) | −0.1105 (4) | 0.3757 (3) | 0.8035 (3) | 0.0206 (11) | |
C(26) | 0.1466 (4) | 0.4373 (3) | 0.8418 (3) | 0.0242 (11) | |
H(30) | 0.2260 | 0.2868 | 0.7123 | 0.036* | |
H(2) | 0.4519 | 0.0571 | 0.8389 | 0.028* | |
H(3) | 0.5249 | −0.0879 | 0.8987 | 0.031* | |
H(4) | 0.4242 | −0.1867 | 0.9877 | 0.033* | |
H(5) | 0.2513 | −0.1389 | 1.0225 | 0.034* | |
H(6) | 0.1762 | 0.0049 | 0.9602 | 0.029* | |
H(31) | 0.2291 | 0.1921 | 0.6497 | 0.036* | |
H(8) | 0.2675 | 0.1836 | 1.0432 | 0.022* | |
H(9) | 0.3625 | 0.2855 | 1.1458 | 0.032* | |
H(10) | 0.4828 | 0.4014 | 1.0954 | 0.033* | |
H(11) | 0.4998 | 0.4239 | 0.9435 | 0.033* | |
H(12) | 0.4021 | 0.3249 | 0.8405 | 0.026* | |
H(33) | 0.3308 | 0.2642 | 0.6591 | 0.036* | |
H(28) | 0.2017 | 0.4061 | 0.8075 | 0.029* | |
H(15) | 0.0125 | 0.1232 | 1.0285 | 0.026* | |
H(16) | 0.0387 | 0.0866 | 1.1792 | 0.034* | |
H(17) | 0.0881 | 0.2107 | 1.2816 | 0.033* | |
H(18) | 0.1144 | 0.3695 | 1.2326 | 0.032* | |
H(19) | 0.0906 | 0.4079 | 1.0813 | 0.023* | |
H(21) | −0.1321 | 0.3723 | 1.0186 | 0.024* | |
H(22) | −0.2902 | 0.4575 | 0.9774 | 0.032* | |
H(23) | −0.3341 | 0.4932 | 0.8279 | 0.030* | |
H(24) | −0.2197 | 0.4431 | 0.7187 | 0.029* | |
H(25) | −0.0656 | 0.3535 | 0.7587 | 0.025* | |
H(26) | 0.1697 | 0.5039 | 0.8585 | 0.029* | |
H(27) | 0.0784 | 0.4402 | 0.8057 | 0.029* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pt(1) | 0.01313 (9) | 0.01225 (9) | 0.01551 (9) | 0.00037 (9) | 0.00053 (6) | −0.00182 (9) |
Cl(1) | 0.0223 (6) | 0.0175 (6) | 0.0212 (6) | 0.0008 (5) | 0.0010 (5) | −0.0066 (4) |
Cl(2) | 0.0150 (6) | 0.0211 (6) | 0.0326 (7) | −0.0030 (4) | 0.0014 (5) | −0.0064 (5) |
P(1) | 0.0142 (5) | 0.0143 (5) | 0.0155 (5) | 0.0010 (5) | 0.0013 (4) | −0.0010 (5) |
P(2) | 0.0130 (6) | 0.0122 (6) | 0.0155 (6) | 0.0007 (4) | 0.0014 (5) | 0.0005 (4) |
O(1) | 0.0209 (18) | 0.024 (2) | 0.0172 (17) | 0.0041 (15) | 0.0050 (14) | 0.0029 (14) |
O(2) | 0.0180 (17) | 0.0141 (16) | 0.0167 (17) | −0.0023 (14) | 0.0024 (14) | 0.0011 (13) |
C(1) | 0.018 (2) | 0.015 (2) | 0.016 (2) | 0.005 (2) | −0.001 (2) | −0.0011 (19) |
C(2) | 0.023 (2) | 0.026 (2) | 0.020 (2) | 0.005 (2) | −0.001 (2) | −0.006 (2) |
C(3) | 0.024 (2) | 0.028 (3) | 0.026 (3) | 0.014 (2) | −0.003 (2) | −0.008 (2) |
C(4) | 0.036 (3) | 0.019 (2) | 0.027 (3) | 0.010 (2) | −0.005 (2) | −0.004 (2) |
C(5) | 0.041 (3) | 0.019 (2) | 0.026 (3) | −0.001 (2) | 0.002 (2) | 0.003 (2) |
C(6) | 0.021 (2) | 0.018 (2) | 0.032 (3) | 0.006 (2) | 0.006 (2) | −0.001 (2) |
C(7) | 0.012 (2) | 0.017 (2) | 0.020 (2) | 0.0057 (19) | −0.001 (2) | −0.002 (2) |
C(8) | 0.014 (2) | 0.015 (2) | 0.025 (2) | 0.003 (2) | −0.002 (2) | 0.001 (2) |
C(9) | 0.032 (3) | 0.029 (3) | 0.018 (2) | 0.012 (2) | −0.007 (2) | −0.003 (2) |
C(10) | 0.021 (2) | 0.019 (2) | 0.042 (3) | 0.004 (2) | −0.012 (2) | −0.015 (2) |
C(11) | 0.022 (2) | 0.017 (2) | 0.043 (3) | −0.002 (2) | 0.001 (2) | −0.004 (2) |
C(12) | 0.020 (2) | 0.017 (2) | 0.029 (2) | 0.003 (2) | 0.003 (2) | 0.001 (2) |
C(13) | 0.031 (3) | 0.040 (3) | 0.019 (2) | 0.005 (2) | 0.005 (2) | 0.009 (2) |
C(14) | 0.013 (2) | 0.016 (2) | 0.019 (2) | 0.0050 (19) | 0.0029 (19) | 0.0043 (19) |
C(15) | 0.020 (2) | 0.020 (2) | 0.027 (2) | −0.002 (2) | 0.007 (2) | −0.000 (2) |
C(16) | 0.032 (3) | 0.020 (2) | 0.035 (3) | −0.004 (2) | 0.009 (2) | 0.014 (2) |
C(17) | 0.028 (3) | 0.037 (3) | 0.017 (2) | 0.004 (2) | 0.003 (2) | 0.010 (2) |
C(18) | 0.029 (2) | 0.033 (3) | 0.019 (2) | −0.002 (2) | 0.002 (2) | −0.003 (2) |
C(19) | 0.025 (2) | 0.016 (2) | 0.017 (2) | 0.002 (2) | 0.003 (2) | 0.001 (2) |
C(20) | 0.016 (2) | 0.010 (2) | 0.023 (2) | −0.0010 (19) | −0.001 (2) | −0.0001 (19) |
C(21) | 0.021 (2) | 0.018 (2) | 0.021 (2) | −0.000 (2) | 0.002 (2) | −0.001 (2) |
C(22) | 0.020 (2) | 0.028 (3) | 0.032 (3) | 0.004 (2) | 0.003 (2) | −0.007 (2) |
C(23) | 0.016 (2) | 0.016 (2) | 0.042 (3) | 0.009 (2) | −0.008 (2) | −0.004 (2) |
C(24) | 0.025 (2) | 0.023 (2) | 0.024 (2) | −0.002 (2) | −0.011 (2) | 0.000 (2) |
C(25) | 0.019 (2) | 0.021 (2) | 0.021 (2) | 0.001 (2) | −0.001 (2) | 0.000 (2) |
C(26) | 0.026 (2) | 0.022 (2) | 0.025 (2) | −0.006 (2) | 0.004 (2) | 0.004 (2) |
Pt1—Cl1 | 2.3693 (12) | C(20)—C(25) | 1.395 (6) |
Pt1—Cl2 | 2.3533 (12) | C(21)—C(22) | 1.385 (7) |
Pt1—P1 | 2.2272 (11) | C(22)—C(23) | 1.385 (7) |
Pt1—P2 | 2.2279 (12) | C(23)—C(24) | 1.389 (7) |
P(1)—O(1) | 1.593 (3) | C(24)—C(25) | 1.375 (7) |
P(1)—C(1) | 1.826 (4) | C(2)—H(2) | 0.950 |
P(1)—C(7) | 1.815 (4) | C(3)—H(3) | 0.950 |
P(2)—O(2) | 1.605 (3) | C(4)—H(4) | 0.950 |
P(2)—C(14) | 1.797 (4) | C(5)—H(5) | 0.950 |
P(2)—C(20) | 1.821 (4) | C(6)—H(6) | 0.950 |
O(1)—C(13) | 1.434 (6) | C(8)—H(8) | 0.950 |
O(2)—C(26) | 1.444 (6) | C(9)—H(9) | 0.950 |
C(1)—C(2) | 1.385 (7) | C(10)—H(10) | 0.950 |
C(1)—C(6) | 1.388 (7) | C(11)—H(11) | 0.950 |
C(2)—C(3) | 1.384 (7) | C(12)—H(12) | 0.950 |
C(3)—C(4) | 1.375 (7) | C(13)—H(30) | 0.980 |
C(4)—C(5) | 1.383 (8) | C(13)—H(31) | 0.980 |
C(5)—C(6) | 1.390 (7) | C(13)—H(33) | 0.980 |
C(7)—C(8) | 1.396 (6) | C(15)—H(15) | 0.950 |
C(7)—C(12) | 1.386 (6) | C(16)—H(16) | 0.950 |
C(8)—C(9) | 1.387 (7) | C(17)—H(17) | 0.950 |
C(9)—C(10) | 1.385 (7) | C(18)—H(18) | 0.950 |
C(10)—C(11) | 1.383 (8) | C(19)—H(19) | 0.950 |
C(11)—C(12) | 1.387 (7) | C(21)—H(21) | 0.950 |
C(14)—C(15) | 1.390 (6) | C(22)—H(22) | 0.950 |
C(14)—C(19) | 1.407 (6) | C(23)—H(23) | 0.950 |
C(15)—C(16) | 1.379 (7) | C(24)—H(24) | 0.950 |
C(16)—C(17) | 1.395 (7) | C(25)—H(25) | 0.950 |
C(17)—C(18) | 1.372 (7) | C(26)—H(28) | 0.980 |
C(18)—C(19) | 1.389 (6) | C(26)—H(26) | 0.980 |
C(20)—C(21) | 1.398 (7) | C(26)—H(27) | 0.980 |
Cl(1)···C(16)i | 3.518 (5) | H(31)···H(22)x | 3.295 |
O(2)···C(22)ii | 3.542 (6) | H(31)···H(26)iii | 2.863 |
C(2)···C(26)iii | 3.478 (7) | H(8)···H(3)iv | 2.974 |
C(3)···C(3)iv | 3.412 (7) | H(8)···H(24)vi | 3.152 |
C(4)···C(13)iii | 3.557 (7) | H(9)···Cl(2)vi | 2.968 |
C(5)···C(13)iii | 3.518 (7) | H(9)···C(25)vi | 3.236 |
C(13)···C(4)v | 3.557 (7) | H(9)···H(3)iv | 3.125 |
C(13)···C(5)v | 3.518 (7) | H(9)···H(23)ii | 3.066 |
C(16)···Cl(1)i | 3.518 (5) | H(9)···H(24)vi | 3.477 |
C(17)···C(23)vi | 3.589 (7) | H(9)···H(25)vi | 2.663 |
C(17)···C(24)vi | 3.504 (7) | H(10)···Cl(1)vi | 2.716 |
C(22)···O(2)ii | 3.542 (6) | H(10)···C(11)ix | 3.287 |
C(23)···C(17)vii | 3.589 (7) | H(10)···C(23)ii | 3.433 |
C(24)···C(17)vii | 3.504 (7) | H(10)···H(4)iv | 3.412 |
C(26)···C(2)v | 3.478 (7) | H(10)···H(31)vi | 3.369 |
Cl(1)···H(10)vii | 2.716 | H(10)···H(11)ix | 2.463 |
Cl(1)···H(11)iii | 3.298 | H(10)···H(22)xi | 3.508 |
Cl(1)···H(12)iii | 3.049 | H(10)···H(22)ii | 3.210 |
Cl(1)···H(28)iii | 3.085 | H(10)···H(23)ii | 2.660 |
Cl(1)···H(16)i | 2.716 | H(11)···Cl(1)v | 3.298 |
Cl(1)···H(23)viii | 3.462 | H(11)···C(10)ix | 3.005 |
Cl(1)···H(26)iii | 3.294 | H(11)···C(11)ix | 3.118 |
Cl(2)···H(5)i | 2.941 | H(11)···C(22)xi | 3.205 |
Cl(2)···H(9)vii | 2.968 | H(11)···C(23)xi | 3.340 |
Cl(2)···H(16)i | 3.085 | H(11)···H(4)iv | 3.506 |
Cl(2)···H(23)viii | 3.034 | H(11)···H(10)ix | 2.463 |
Cl(2)···H(24)viii | 3.347 | H(11)···H(11)ix | 2.682 |
O(1)···H(26)iii | 3.021 | H(11)···H(17)x | 3.291 |
O(2)···H(21)ii | 3.488 | H(11)···H(22)xi | 2.667 |
O(2)···H(22)ii | 3.270 | H(11)···H(22)ii | 3.346 |
C(1)···H(28)iii | 3.556 | H(11)···H(23)xi | 2.935 |
C(2)···H(3)iv | 3.577 | H(12)···Cl(1)v | 3.049 |
C(2)···H(28)iii | 3.366 | H(12)···C(16)x | 3.389 |
C(2)···H(27)iii | 2.931 | H(12)···C(17)x | 3.010 |
C(3)···H(30)iii | 3.434 | H(12)···H(16)x | 3.276 |
C(3)···H(3)iv | 3.570 | H(12)···H(17)x | 2.572 |
C(3)···H(25)iii | 3.165 | H(33)···C(4)v | 3.583 |
C(3)···H(27)iii | 3.265 | H(33)···C(5)v | 3.163 |
C(4)···H(30)iii | 3.192 | H(33)···C(6)v | 3.534 |
C(4)···H(2)iv | 3.554 | H(33)···C(14)x | 3.385 |
C(4)···H(31)iii | 3.323 | H(33)···C(15)x | 3.052 |
C(4)···H(33)iii | 3.583 | H(33)···C(16)x | 2.940 |
C(5)···H(30)iii | 3.334 | H(33)···C(17)x | 3.160 |
C(5)···H(31)iii | 3.482 | H(33)···C(18)x | 3.468 |
C(5)···H(33)iii | 3.163 | H(33)···C(19)x | 3.578 |
C(6)···H(33)iii | 3.534 | H(33)···H(5)v | 3.148 |
C(6)···H(15)i | 3.594 | H(33)···H(15)x | 3.444 |
C(7)···H(4)iv | 3.363 | H(33)···H(16)x | 3.287 |
C(8)···H(3)iv | 2.999 | H(33)···H(21)x | 2.874 |
C(8)···H(4)iv | 3.324 | H(33)···H(26)iii | 3.557 |
C(9)···H(3)iv | 3.074 | H(28)···Cl(1)v | 3.085 |
C(9)···H(4)iv | 3.166 | H(28)···C(1)v | 3.556 |
C(9)···H(23)ii | 3.255 | H(28)···C(2)v | 3.366 |
C(9)···H(25)vi | 3.353 | H(28)···H(2)v | 3.494 |
C(10)···H(4)iv | 3.001 | H(15)···C(6)i | 3.594 |
C(10)···H(11)ix | 3.005 | H(15)···H(5)i | 3.327 |
C(10)···H(22)ii | 3.115 | H(15)···H(6)i | 2.937 |
C(10)···H(23)ii | 3.024 | H(15)···H(33)xii | 3.444 |
C(11)···H(4)iv | 3.054 | H(15)···H(15)i | 3.476 |
C(11)···H(10)ix | 3.287 | H(16)···Cl(1)i | 2.716 |
C(11)···H(11)ix | 3.118 | H(16)···Cl(2)i | 3.085 |
C(11)···H(17)x | 3.502 | H(16)···C(23)vi | 3.387 |
C(11)···H(22)xi | 3.382 | H(16)···C(24)vi | 3.473 |
C(11)···H(22)ii | 3.209 | H(16)···H(6)i | 3.521 |
C(12)···H(4)iv | 3.235 | H(16)···H(12)xii | 3.276 |
C(12)···H(17)x | 3.125 | H(16)···H(33)xii | 3.287 |
C(13)···H(21)x | 3.259 | H(16)···H(23)vi | 2.873 |
C(13)···H(26)iii | 3.322 | H(16)···H(24)vi | 3.051 |
C(14)···H(33)xii | 3.385 | H(17)···C(11)xii | 3.502 |
C(15)···H(6)i | 3.575 | H(17)···C(12)xii | 3.125 |
C(15)···H(33)xii | 3.052 | H(17)···C(23)vi | 3.014 |
C(16)···H(12)xii | 3.389 | H(17)···C(24)vi | 3.217 |
C(16)···H(33)xii | 2.940 | H(17)···H(11)xii | 3.291 |
C(16)···H(23)vi | 3.468 | H(17)···H(12)xii | 2.572 |
C(16)···H(24)vi | 3.231 | H(17)···H(23)vi | 3.009 |
C(17)···H(12)xii | 3.010 | H(17)···H(24)vi | 3.358 |
C(17)···H(33)xii | 3.160 | H(18)···C(23)ii | 3.298 |
C(17)···H(23)vi | 3.534 | H(18)···C(24)ii | 2.980 |
C(17)···H(24)vi | 3.403 | H(18)···C(25)ii | 3.514 |
C(18)···H(2)xii | 3.374 | H(18)···H(2)xii | 2.835 |
C(18)···H(33)xii | 3.468 | H(18)···H(23)ii | 3.477 |
C(19)···H(33)xii | 3.578 | H(18)···H(24)ii | 2.941 |
C(20)···H(19)ii | 3.259 | H(18)···H(27)ii | 3.553 |
C(21)···H(31)xii | 3.503 | H(19)···C(20)ii | 3.259 |
C(21)···H(19)ii | 2.971 | H(19)···C(21)ii | 2.971 |
C(21)···H(26)ii | 3.170 | H(19)···C(22)ii | 2.861 |
C(22)···H(11)xiii | 3.205 | H(19)···C(23)ii | 3.040 |
C(22)···H(19)ii | 2.861 | H(19)···C(24)ii | 3.313 |
C(22)···H(26)ii | 3.313 | H(19)···C(25)ii | 3.422 |
C(23)···H(10)ii | 3.433 | H(19)···H(21)ii | 3.405 |
C(23)···H(11)xiii | 3.340 | H(19)···H(22)ii | 3.250 |
C(23)···H(16)vii | 3.387 | H(19)···H(23)ii | 3.511 |
C(23)···H(17)vii | 3.014 | H(19)···H(27)ii | 3.468 |
C(23)···H(18)ii | 3.298 | H(21)···O(2)ii | 3.488 |
C(23)···H(19)ii | 3.040 | H(21)···C(13)xii | 3.259 |
C(24)···H(3)v | 3.582 | H(21)···C(26)ii | 3.351 |
C(24)···H(16)vii | 3.473 | H(21)···H(5)i | 3.546 |
C(24)···H(17)vii | 3.217 | H(21)···H(31)xii | 2.837 |
C(24)···H(18)ii | 2.980 | H(21)···H(33)xii | 2.874 |
C(24)···H(19)ii | 3.313 | H(21)···H(19)ii | 3.405 |
C(25)···H(3)v | 3.322 | H(21)···H(26)ii | 2.568 |
C(25)···H(9)vii | 3.236 | H(22)···O(2)ii | 3.270 |
C(25)···H(18)ii | 3.514 | H(22)···C(10)ii | 3.115 |
C(25)···H(19)ii | 3.422 | H(22)···C(11)xiii | 3.382 |
C(26)···H(2)v | 3.340 | H(22)···C(11)ii | 3.209 |
C(26)···H(21)ii | 3.351 | H(22)···C(26)ii | 3.471 |
C(26)···H(22)ii | 3.471 | H(22)···H(31)xii | 3.295 |
H(30)···C(3)v | 3.434 | H(22)···H(10)xiii | 3.508 |
H(30)···C(4)v | 3.192 | H(22)···H(10)ii | 3.210 |
H(30)···C(5)v | 3.334 | H(22)···H(11)xiii | 2.667 |
H(30)···H(4)v | 3.461 | H(22)···H(11)ii | 3.346 |
H(2)···C(4)iv | 3.554 | H(22)···H(19)ii | 3.250 |
H(2)···C(18)x | 3.374 | H(22)···H(26)ii | 2.858 |
H(2)···C(26)iii | 3.340 | H(23)···Cl(1)xiv | 3.462 |
H(2)···H(4)iv | 3.436 | H(23)···Cl(2)xiv | 3.034 |
H(2)···H(28)iii | 3.494 | H(23)···C(9)ii | 3.255 |
H(2)···H(18)x | 2.835 | H(23)···C(10)ii | 3.024 |
H(2)···H(25)iii | 3.480 | H(23)···C(16)vii | 3.468 |
H(2)···H(26)iii | 3.329 | H(23)···C(17)vii | 3.534 |
H(2)···H(27)iii | 2.704 | H(23)···H(9)ii | 3.066 |
H(3)···C(2)iv | 3.577 | H(23)···H(10)ii | 2.660 |
H(3)···C(3)iv | 3.570 | H(23)···H(11)xiii | 2.935 |
H(3)···C(8)iv | 2.999 | H(23)···H(16)vii | 2.873 |
H(3)···C(9)iv | 3.074 | H(23)···H(17)vii | 3.009 |
H(3)···C(24)iii | 3.582 | H(23)···H(18)ii | 3.477 |
H(3)···C(25)iii | 3.322 | H(23)···H(19)ii | 3.511 |
H(3)···H(8)iv | 2.974 | H(24)···Cl(2)xiv | 3.347 |
H(3)···H(9)iv | 3.125 | H(24)···C(16)vii | 3.231 |
H(3)···H(24)iii | 3.112 | H(24)···C(17)vii | 3.403 |
H(3)···H(25)iii | 2.579 | H(24)···H(3)v | 3.112 |
H(3)···H(27)iii | 3.281 | H(24)···H(8)vii | 3.152 |
H(4)···C(7)iv | 3.363 | H(24)···H(9)vii | 3.477 |
H(4)···C(8)iv | 3.324 | H(24)···H(16)vii | 3.051 |
H(4)···C(9)iv | 3.166 | H(24)···H(17)vii | 3.358 |
H(4)···C(10)iv | 3.001 | H(24)···H(18)ii | 2.941 |
H(4)···C(11)iv | 3.054 | H(25)···C(3)v | 3.165 |
H(4)···C(12)iv | 3.235 | H(25)···C(9)vii | 3.353 |
H(4)···H(30)iii | 3.461 | H(25)···H(2)v | 3.480 |
H(4)···H(2)iv | 3.436 | H(25)···H(3)v | 2.579 |
H(4)···H(31)iii | 3.185 | H(25)···H(9)vii | 2.663 |
H(4)···H(10)iv | 3.412 | H(26)···Cl(1)v | 3.294 |
H(4)···H(11)iv | 3.506 | H(26)···O(1)v | 3.021 |
H(5)···Cl(2)i | 2.941 | H(26)···C(13)v | 3.322 |
H(5)···H(31)iii | 3.486 | H(26)···C(21)ii | 3.170 |
H(5)···H(33)iii | 3.148 | H(26)···C(22)ii | 3.313 |
H(5)···H(15)i | 3.327 | H(26)···H(2)v | 3.329 |
H(5)···H(21)i | 3.546 | H(26)···H(31)v | 2.863 |
H(6)···C(15)i | 3.575 | H(26)···H(33)v | 3.557 |
H(6)···H(15)i | 2.937 | H(26)···H(21)ii | 2.568 |
H(6)···H(16)i | 3.521 | H(26)···H(22)ii | 2.858 |
H(31)···C(4)v | 3.323 | H(27)···C(2)v | 2.931 |
H(31)···C(5)v | 3.482 | H(27)···C(3)v | 3.265 |
H(31)···C(21)x | 3.503 | H(27)···H(2)v | 2.704 |
H(31)···H(4)v | 3.185 | H(27)···H(3)v | 3.281 |
H(31)···H(5)v | 3.486 | H(27)···H(18)ii | 3.553 |
H(31)···H(10)vii | 3.369 | H(27)···H(19)ii | 3.468 |
H(31)···H(21)x | 2.837 | ||
Cl1—Pt1—Cl2 | 89.37 (4) | C(1)—C(2)—H(2) | 120.0 |
P1—Pt1—P2 | 98.14 (4) | C(3)—C(2)—H(2) | 120.0 |
Cl1—Pt1—P1 | 83.49 (4) | C(2)—C(3)—H(3) | 119.9 |
Cl1—Pt1—P2 | 175.95 (4) | C(4)—C(3)—H(3) | 119.9 |
Cl2—Pt1—P1 | 168.82 (4) | C(3)—C(4)—H(4) | 119.8 |
Cl2—Pt1—P2 | 89.56 (4) | C(5)—C(4)—H(4) | 119.8 |
Pt(1)—P(1)—O(1) | 116.11 (12) | C(4)—C(5)—H(5) | 120.3 |
Pt(1)—P(1)—C(1) | 111.37 (16) | C(6)—C(5)—H(5) | 120.3 |
Pt(1)—P(1)—C(7) | 120.68 (16) | C(1)—C(6)—H(6) | 119.8 |
O(1)—P(1)—C(1) | 102.3 (2) | C(5)—C(6)—H(6) | 119.8 |
O(1)—P(1)—C(7) | 103.3 (2) | C(7)—C(8)—H(8) | 120.0 |
C(1)—P(1)—C(7) | 100.6 (2) | C(9)—C(8)—H(8) | 120.0 |
Pt(1)—P(2)—O(2) | 116.82 (13) | C(8)—C(9)—H(9) | 120.3 |
Pt(1)—P(2)—C(14) | 114.29 (15) | C(10)—C(9)—H(9) | 120.3 |
Pt(1)—P(2)—C(20) | 113.76 (15) | C(9)—C(10)—H(10) | 119.7 |
O(2)—P(2)—C(14) | 99.56 (19) | C(11)—C(10)—H(10) | 119.7 |
O(2)—P(2)—C(20) | 103.39 (19) | C(10)—C(11)—H(11) | 120.0 |
C(14)—P(2)—C(20) | 107.5 (2) | C(12)—C(11)—H(11) | 120.0 |
P(1)—O(1)—C(13) | 122.7 (3) | C(7)—C(12)—H(12) | 120.0 |
P(2)—O(2)—C(26) | 121.4 (2) | C(11)—C(12)—H(12) | 120.0 |
P(1)—C(1)—C(2) | 119.4 (3) | O(1)—C(13)—H(30) | 109.5 |
P(1)—C(1)—C(6) | 120.8 (3) | O(1)—C(13)—H(31) | 109.5 |
C(2)—C(1)—C(6) | 119.5 (4) | O(1)—C(13)—H(33) | 109.5 |
C(1)—C(2)—C(3) | 120.0 (4) | H(30)—C(13)—H(31) | 109.5 |
C(2)—C(3)—C(4) | 120.3 (5) | H(30)—C(13)—H(33) | 109.5 |
C(3)—C(4)—C(5) | 120.4 (4) | H(31)—C(13)—H(33) | 109.5 |
C(4)—C(5)—C(6) | 119.4 (5) | C(14)—C(15)—H(15) | 119.8 |
C(1)—C(6)—C(5) | 120.4 (4) | C(16)—C(15)—H(15) | 119.8 |
P(1)—C(7)—C(8) | 119.5 (3) | C(15)—C(16)—H(16) | 120.0 |
P(1)—C(7)—C(12) | 120.5 (3) | C(17)—C(16)—H(16) | 120.0 |
C(8)—C(7)—C(12) | 119.9 (4) | C(16)—C(17)—H(17) | 120.0 |
C(7)—C(8)—C(9) | 120.1 (4) | C(18)—C(17)—H(17) | 120.0 |
C(8)—C(9)—C(10) | 119.5 (4) | C(17)—C(18)—H(18) | 119.7 |
C(9)—C(10)—C(11) | 120.7 (4) | C(19)—C(18)—H(18) | 119.6 |
C(10)—C(11)—C(12) | 120.0 (4) | C(14)—C(19)—H(19) | 120.3 |
C(7)—C(12)—C(11) | 119.9 (4) | C(18)—C(19)—H(19) | 120.3 |
P(2)—C(14)—C(15) | 120.1 (3) | C(20)—C(21)—H(21) | 120.0 |
P(2)—C(14)—C(19) | 120.2 (3) | C(22)—C(21)—H(21) | 120.0 |
C(15)—C(14)—C(19) | 119.4 (4) | C(21)—C(22)—H(22) | 119.9 |
C(14)—C(15)—C(16) | 120.4 (4) | C(23)—C(22)—H(22) | 119.9 |
C(15)—C(16)—C(17) | 120.1 (4) | C(22)—C(23)—H(23) | 120.0 |
C(16)—C(17)—C(18) | 120.0 (4) | C(24)—C(23)—H(23) | 120.0 |
C(17)—C(18)—C(19) | 120.7 (4) | C(23)—C(24)—H(24) | 120.1 |
C(14)—C(19)—C(18) | 119.4 (4) | C(25)—C(24)—H(24) | 120.1 |
P(2)—C(20)—C(21) | 121.6 (3) | C(20)—C(25)—H(25) | 119.5 |
P(2)—C(20)—C(25) | 119.5 (3) | C(24)—C(25)—H(25) | 119.5 |
C(21)—C(20)—C(25) | 118.8 (4) | O(2)—C(26)—H(28) | 109.5 |
C(20)—C(21)—C(22) | 120.1 (4) | O(2)—C(26)—H(26) | 109.5 |
C(21)—C(22)—C(23) | 120.2 (5) | O(2)—C(26)—H(27) | 109.5 |
C(22)—C(23)—C(24) | 120.1 (4) | H(28)—C(26)—H(26) | 109.5 |
C(23)—C(24)—C(25) | 119.7 (4) | H(28)—C(26)—H(27) | 109.5 |
C(20)—C(25)—C(24) | 121.0 (4) | H(26)—C(26)—H(27) | 109.5 |
Cl(1)—Pt(1)—P(1)—O(1) | 58.22 (15) | O(2)—P(2)—C(20)—C(25) | 80.4 (3) |
Cl(1)—Pt(1)—P(1)—C(1) | −58.24 (16) | C(20)—P(2)—O(2)—C(26) | −60.0 (3) |
Cl(1)—Pt(1)—P(1)—C(7) | −175.70 (19) | C(14)—P(2)—C(20)—C(21) | 8.2 (4) |
Cl(2)—Pt(1)—P(1)—O(1) | 108.8 (2) | C(14)—P(2)—C(20)—C(25) | −174.9 (3) |
Cl(2)—Pt(1)—P(1)—C(1) | −7.6 (3) | C(20)—P(2)—C(14)—C(15) | 105.2 (4) |
Cl(2)—Pt(1)—P(1)—C(7) | −125.1 (2) | C(20)—P(2)—C(14)—C(19) | −80.9 (4) |
Cl(2)—Pt(1)—P(2)—O(2) | −154.11 (14) | P(1)—C(1)—C(2)—C(3) | 175.0 (3) |
Cl(2)—Pt(1)—P(2)—C(14) | 90.27 (17) | P(1)—C(1)—C(6)—C(5) | −174.2 (3) |
Cl(2)—Pt(1)—P(2)—C(20) | −33.70 (17) | C(2)—C(1)—C(6)—C(5) | −0.2 (6) |
P(1)—Pt(1)—P(2)—O(2) | 34.03 (14) | C(6)—C(1)—C(2)—C(3) | 0.9 (7) |
P(1)—Pt(1)—P(2)—C(14) | −81.59 (17) | C(1)—C(2)—C(3)—C(4) | −0.3 (6) |
P(1)—Pt(1)—P(2)—C(20) | 154.44 (17) | C(2)—C(3)—C(4)—C(5) | −1.2 (8) |
P(2)—Pt(1)—P(1)—O(1) | −118.04 (15) | C(3)—C(4)—C(5)—C(6) | 1.9 (7) |
P(2)—Pt(1)—P(1)—C(1) | 125.50 (16) | C(4)—C(5)—C(6)—C(1) | −1.2 (7) |
P(2)—Pt(1)—P(1)—C(7) | 8.04 (19) | P(1)—C(7)—C(8)—C(9) | 177.3 (3) |
Pt(1)—P(1)—O(1)—C(13) | 30.6 (3) | P(1)—C(7)—C(12)—C(11) | −176.5 (3) |
Pt(1)—P(1)—C(1)—C(2) | 155.6 (3) | C(8)—C(7)—C(12)—C(11) | 0.2 (5) |
Pt(1)—P(1)—C(1)—C(6) | −30.4 (4) | C(12)—C(7)—C(8)—C(9) | 0.6 (7) |
Pt(1)—P(1)—C(7)—C(8) | 65.7 (4) | C(7)—C(8)—C(9)—C(10) | −1.8 (7) |
Pt(1)—P(1)—C(7)—C(12) | −117.6 (3) | C(8)—C(9)—C(10)—C(11) | 2.2 (7) |
O(1)—P(1)—C(1)—C(2) | 31.0 (4) | C(9)—C(10)—C(11)—C(12) | −1.4 (7) |
O(1)—P(1)—C(1)—C(6) | −155.0 (3) | C(10)—C(11)—C(12)—C(7) | 0.2 (5) |
C(1)—P(1)—O(1)—C(13) | 152.1 (3) | P(2)—C(14)—C(15)—C(16) | 173.0 (3) |
O(1)—P(1)—C(7)—C(8) | −162.6 (3) | P(2)—C(14)—C(19)—C(18) | −173.4 (3) |
O(1)—P(1)—C(7)—C(12) | 14.1 (4) | C(15)—C(14)—C(19)—C(18) | 0.6 (7) |
C(7)—P(1)—O(1)—C(13) | −103.8 (3) | C(19)—C(14)—C(15)—C(16) | −1.0 (7) |
C(1)—P(1)—C(7)—C(8) | −57.1 (4) | C(14)—C(15)—C(16)—C(17) | 1.0 (7) |
C(1)—P(1)—C(7)—C(12) | 119.6 (4) | C(15)—C(16)—C(17)—C(18) | −0.6 (7) |
C(7)—P(1)—C(1)—C(2) | −75.3 (4) | C(16)—C(17)—C(18)—C(19) | 0.2 (6) |
C(7)—P(1)—C(1)—C(6) | 98.7 (4) | C(17)—C(18)—C(19)—C(14) | −0.2 (5) |
Pt(1)—P(2)—O(2)—C(26) | 65.8 (3) | P(2)—C(20)—C(21)—C(22) | 176.7 (3) |
Pt(1)—P(2)—C(14)—C(15) | −22.1 (4) | P(2)—C(20)—C(25)—C(24) | −175.6 (3) |
Pt(1)—P(2)—C(14)—C(19) | 151.8 (3) | C(21)—C(20)—C(25)—C(24) | 1.4 (7) |
Pt(1)—P(2)—C(20)—C(21) | 135.8 (3) | C(25)—C(20)—C(21)—C(22) | −0.2 (5) |
Pt(1)—P(2)—C(20)—C(25) | −47.3 (4) | C(20)—C(21)—C(22)—C(23) | −0.6 (7) |
O(2)—P(2)—C(14)—C(15) | −147.4 (3) | C(21)—C(22)—C(23)—C(24) | 0.2 (6) |
O(2)—P(2)—C(14)—C(19) | 26.5 (4) | C(22)—C(23)—C(24)—C(25) | 1.0 (7) |
C(14)—P(2)—O(2)—C(26) | −170.7 (3) | C(23)—C(24)—C(25)—C(20) | −1.8 (7) |
O(2)—P(2)—C(20)—C(21) | −96.5 (4) |
Symmetry codes: (i) −x, −y, −z+2; (ii) −x, −y+1, −z+2; (iii) −x+1/2, y−1/2, −z+3/2; (iv) −x+1, −y, −z+2; (v) −x+1/2, y+1/2, −z+3/2; (vi) x+1/2, −y+1/2, z+1/2; (vii) x−1/2, −y+1/2, z−1/2; (viii) −x−1/2, y−1/2, −z+3/2; (ix) −x+1, −y+1, −z+2; (x) x+1/2, −y+1/2, z−1/2; (xi) x+1, y, z; (xii) x−1/2, −y+1/2, z+1/2; (xiii) x−1, y, z; (xiv) −x−1/2, y+1/2, −z+3/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
C10—H10···Cl1vi | 0.95 | 2.72 | 3.642 (6) | 165 |
C16—H16···Cl1i | 0.95 | 2.72 | 3.518 (5) | 143 |
C4—H4···Cg1iv | 0.95 | 2.88 | 3.692 (5) | 145 |
C19—H19···Cg2ii | 0.95 | 2.83 | 3.641 (4) | 144 |
Symmetry codes: (i) −x, −y, −z+2; (ii) −x, −y+1, −z+2; (iv) −x+1, −y, −z+2; (vi) x+1/2, −y+1/2, z+1/2. |
Experimental details
Crystal data | |
Chemical formula | [PtCl2(C13H13OP)2] |
Mr | 698.43 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 125 |
a, b, c (Å) | 12.4262 (6), 13.6280 (7), 15.0494 (8) |
β (°) | 93.5316 (11) |
V (Å3) | 2543.7 (2) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 5.85 |
Crystal size (mm) | 0.25 × 0.15 × 0.12 |
Data collection | |
Diffractometer | Rigaku SCXmini |
Absorption correction | Multi-scan (ABSCOR; Higashi, 1995) |
Tmin, Tmax | 0.377, 0.495 |
No. of measured, independent and observed [F2 > 2σ(F2)] reflections | 26133, 5827, 4910 |
Rint | 0.057 |
(sin θ/λ)max (Å−1) | 0.649 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.041, 0.062, 1.13 |
No. of reflections | 5827 |
No. of parameters | 299 |
No. of restraints | ? |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.99, −1.02 |
Computer programs: SCXmini Software (Rigaku/MSC, 2006), PROCESS-AUTO (Rigaku, 1998), PROCESS-AUTO, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), CrystalStructure (Rigaku/MSC, 2006), CrystalStructure.
Pt1—Cl1 | 2.3693 (12) | Pt1—P1 | 2.2272 (11) |
Pt1—Cl2 | 2.3533 (12) | Pt1—P2 | 2.2279 (12) |
Cl1—Pt1—Cl2 | 89.37 (4) | Cl1—Pt1—P2 | 175.95 (4) |
P1—Pt1—P2 | 98.14 (4) | Cl2—Pt1—P1 | 168.82 (4) |
Cl1—Pt1—P1 | 83.49 (4) | Cl2—Pt1—P2 | 89.56 (4) |
D—H···A | D—H | H···A | D···A | D—H···A |
C10—H10···Cl1i | 0.95 | 2.72 | 3.642 (6) | 165 |
C16—H16···Cl1ii | 0.95 | 2.72 | 3.518 (5) | 143 |
C4—H4···Cg1iii | 0.95 | 2.88 | 3.692 (5) | 145 |
C19—H19···Cg2iv | 0.95 | 2.83 | 3.641 (4) | 144 |
Symmetry codes: (i) x+1/2, −y+1/2, z+1/2; (ii) −x, −y, −z+2; (iii) −x+1, −y, −z+2; (iv) −x, −y+1, −z+2. |
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The title complex (I) can be compared to similar platinum dichloride complexes containing trimethoxy phosphite; [PtCl2(P(OMe)3)2] (Bao et al., 1987) and triphenyl phosphine [PtCl2(PPh3)2] (Fun et al., 2006). The geometry at the platinum atom in the title compound (I) bears a closer resemblance to the triphenyl phosphine complex and can be compared with [PtCl2(P(OMe)2Ph)2] (Slawin et al., 2007).