Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804017209/na6337sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804017209/na6337Isup2.hkl |
CCDC reference: 248749
Data collection: X-AREA (Stoe & Cie, 2000); cell refinement: X-AREA; data reduction: X-RED (Stoe & Cie, 2000); 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.
[Pt(C44H40Cl2N2O2P2)]·3CHCl3 | F(000) = 2600 |
Mr = 1314.81 | Dx = 1.670 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 58409 reflections |
a = 19.3200 (9) Å | θ = 24.9–0.0° |
b = 11.1284 (4) Å | µ = 3.35 mm−1 |
c = 25.6676 (12) Å | T = 153 K |
β = 108.638 (4)° | Needle plate, colourless |
V = 5229.2 (4) Å3 | 0.50 × 0.27 × 0.11 mm |
Z = 4 |
Stoe IPDS-2 diffractometer | 9068 independent reflections |
Radiation source: sealed X-ray tube, 12 x 0.4 mm long-fine focus' | 7600 reflections with I > 2σ(I) |
Plane graphite monochromator | Rint = 0.134 |
Detector resolution: 6.67 pixels mm-1 | θmax = 24.9°, θmin = 1.6° |
rotation method scans | h = −22→22 |
Absorption correction: multi-scan (Blessing et al., 1995) | k = −13→13 |
Tmin = 0.324, Tmax = 0.692 | l = −30→30 |
45476 measured reflections |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.036 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.092 | H-atom parameters constrained |
S = 1.06 | w = 1/[σ2(Fo2) + (0.0454P)2 + 9.7597P] where P = (Fo2 + 2Fc2)/3 |
9068 reflections | (Δ/σ)max < 0.001 |
586 parameters | Δρmax = 1.90 e Å−3 |
0 restraints | Δρmin = −1.19 e Å−3 |
Experimental. A crystal was mounted at 153 K on a Stoe Image Plate Diffraction System (Stoe & Cie, 2000) using Mo Kα graphite monochromated radiation. 259 frames, detector distance 140 mm. |
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 | 0.2010 (3) | 0.2612 (4) | 0.4937 (2) | 0.0289 (11) | |
H1 | 0.2483 | 0.2205 | 0.5072 | 0.035* | |
C2 | 0.2104 (3) | 0.3935 (5) | 0.5120 (2) | 0.0394 (13) | |
H2A | 0.2454 | 0.4313 | 0.4973 | 0.047* | |
H2B | 0.1641 | 0.4347 | 0.4967 | 0.047* | |
C3 | 0.2364 (4) | 0.4082 (5) | 0.5742 (2) | 0.0462 (15) | |
H3A | 0.2849 | 0.3744 | 0.5894 | 0.055* | |
H3B | 0.2390 | 0.4929 | 0.5834 | 0.055* | |
C4 | 0.1852 (3) | 0.3462 (5) | 0.5988 (2) | 0.0413 (14) | |
H4A | 0.1382 | 0.3863 | 0.5870 | 0.050* | |
H4B | 0.2046 | 0.3511 | 0.6386 | 0.050* | |
C5 | 0.1755 (3) | 0.2139 (5) | 0.5812 (2) | 0.0370 (13) | |
H5A | 0.2219 | 0.1725 | 0.5957 | 0.044* | |
H5B | 0.1409 | 0.1761 | 0.5963 | 0.044* | |
C6 | 0.1481 (3) | 0.2023 (4) | 0.5188 (2) | 0.0277 (11) | |
H6 | 0.1023 | 0.2475 | 0.5057 | 0.033* | |
C7 | 0.2163 (3) | 0.2891 (4) | 0.4035 (2) | 0.0260 (11) | |
C8 | 0.1766 (2) | 0.3041 (4) | 0.34245 (19) | 0.0226 (10) | |
C9 | 0.1751 (3) | 0.4214 (4) | 0.3237 (2) | 0.0277 (11) | |
H9 | 0.1987 | 0.4816 | 0.3480 | 0.033* | |
C10 | 0.1388 (3) | 0.4498 (4) | 0.2692 (2) | 0.0308 (11) | |
H10 | 0.1372 | 0.5289 | 0.2572 | 0.037* | |
C11 | 0.1049 (3) | 0.3600 (4) | 0.2328 (2) | 0.0306 (12) | |
H11 | 0.0809 | 0.3784 | 0.1961 | 0.037* | |
C12 | 0.1070 (3) | 0.2424 (4) | 0.2510 (2) | 0.0272 (11) | |
H12 | 0.0843 | 0.1824 | 0.2262 | 0.033* | |
C13 | 0.1425 (2) | 0.2126 (4) | 0.30599 (19) | 0.0213 (10) | |
C14 | 0.1755 (3) | −0.0187 (4) | 0.51574 (19) | 0.0275 (11) | |
C15 | 0.1388 (2) | −0.1411 (4) | 0.5152 (2) | 0.0246 (10) | |
C16 | 0.1451 (3) | −0.1798 (5) | 0.5681 (2) | 0.0308 (11) | |
H16 | 0.1716 | −0.1339 | 0.5981 | 0.037* | |
C17 | 0.1126 (3) | −0.2851 (5) | 0.5768 (2) | 0.0344 (12) | |
H17 | 0.1175 | −0.3099 | 0.6124 | 0.041* | |
C18 | 0.0731 (3) | −0.3531 (5) | 0.5325 (2) | 0.0378 (13) | |
H18 | 0.0499 | −0.4229 | 0.5380 | 0.045* | |
C19 | 0.0680 (3) | −0.3172 (4) | 0.4802 (2) | 0.0333 (12) | |
H19 | 0.0414 | −0.3641 | 0.4506 | 0.040* | |
C20 | 0.1018 (2) | −0.2118 (4) | 0.46993 (19) | 0.0229 (10) | |
C21 | 0.2450 (2) | 0.0417 (4) | 0.36320 (19) | 0.0229 (10) | |
C22 | 0.2709 (3) | 0.0020 (4) | 0.4171 (2) | 0.0278 (11) | |
H22 | 0.2381 | −0.0212 | 0.4351 | 0.033* | |
C23 | 0.3452 (3) | −0.0033 (5) | 0.4444 (2) | 0.0366 (13) | |
H23 | 0.3622 | −0.0304 | 0.4805 | 0.044* | |
C24 | 0.3942 (3) | 0.0313 (5) | 0.4182 (2) | 0.0381 (13) | |
H24 | 0.4441 | 0.0255 | 0.4363 | 0.046* | |
C25 | 0.3686 (3) | 0.0747 (4) | 0.3648 (2) | 0.0304 (11) | |
H25 | 0.4015 | 0.0996 | 0.3473 | 0.036* | |
C26 | 0.2945 (2) | 0.0811 (4) | 0.3375 (2) | 0.0259 (11) | |
H26 | 0.2776 | 0.1118 | 0.3020 | 0.031* | |
C27 | 0.1220 (3) | −0.0258 (4) | 0.26326 (19) | 0.0230 (10) | |
C28 | 0.1706 (3) | −0.0565 (4) | 0.2358 (2) | 0.0273 (11) | |
H28 | 0.2203 | −0.0419 | 0.2522 | 0.033* | |
C29 | 0.1459 (3) | −0.1087 (5) | 0.1841 (2) | 0.0319 (12) | |
H29 | 0.1787 | −0.1288 | 0.1658 | 0.038* | |
C30 | 0.0721 (3) | −0.1308 (5) | 0.1599 (2) | 0.0368 (13) | |
H30 | 0.0551 | −0.1650 | 0.1251 | 0.044* | |
C31 | 0.0242 (3) | −0.1024 (5) | 0.1873 (2) | 0.0367 (13) | |
H31 | −0.0253 | −0.1182 | 0.1710 | 0.044* | |
C32 | 0.0484 (3) | −0.0504 (5) | 0.2391 (2) | 0.0299 (11) | |
H32 | 0.0154 | −0.0320 | 0.2575 | 0.036* | |
C33 | 0.0306 (3) | −0.2831 (4) | 0.35612 (19) | 0.0244 (10) | |
C34 | −0.0385 (3) | −0.2431 (4) | 0.3259 (2) | 0.0277 (11) | |
H34 | −0.0494 | −0.1615 | 0.3248 | 0.033* | |
C35 | −0.0911 (3) | −0.3244 (5) | 0.2974 (2) | 0.0365 (13) | |
H35 | −0.1378 | −0.2975 | 0.2779 | 0.044* | |
C36 | −0.0746 (3) | −0.4453 (5) | 0.2977 (2) | 0.0379 (13) | |
H36 | −0.1103 | −0.4998 | 0.2788 | 0.046* | |
C37 | −0.0057 (3) | −0.4847 (5) | 0.3261 (2) | 0.0398 (14) | |
H37 | 0.0055 | −0.5659 | 0.3260 | 0.048* | |
C38 | 0.0472 (3) | −0.4047 (4) | 0.3549 (2) | 0.0317 (12) | |
H38 | 0.0941 | −0.4319 | 0.3736 | 0.038* | |
C39 | 0.1847 (3) | −0.2460 (4) | 0.3962 (2) | 0.0268 (11) | |
C40 | 0.2392 (3) | −0.2867 (4) | 0.4424 (2) | 0.0317 (12) | |
H40 | 0.2326 | −0.2840 | 0.4767 | 0.038* | |
C41 | 0.3036 (3) | −0.3313 (5) | 0.4372 (3) | 0.0399 (14) | |
H41 | 0.3397 | −0.3606 | 0.4680 | 0.048* | |
C42 | 0.3146 (3) | −0.3325 (5) | 0.3869 (3) | 0.0381 (14) | |
H42 | 0.3589 | −0.3594 | 0.3841 | 0.046* | |
C43 | 0.2606 (3) | −0.2943 (4) | 0.3409 (2) | 0.0340 (12) | |
H43 | 0.2681 | −0.2958 | 0.3069 | 0.041* | |
C44 | 0.1952 (3) | −0.2537 (4) | 0.3449 (2) | 0.0269 (11) | |
H44 | 0.1578 | −0.2312 | 0.3134 | 0.032* | |
C45 | −0.1603 (4) | 0.0863 (6) | 0.2780 (3) | 0.0599 (19) | |
H45 | −0.1145 | 0.0878 | 0.3088 | 0.072* | |
C46 | 0.3664 (4) | −0.1420 (6) | 0.6132 (3) | 0.0603 (19) | |
H46 | 0.3264 | −0.0921 | 0.5904 | 0.072* | |
C47 | 0.4197 (4) | 0.3047 (6) | 0.5294 (3) | 0.0523 (16) | |
H47 | 0.3759 | 0.2980 | 0.4971 | 0.063* | |
N1 | 0.1746 (2) | 0.2562 (3) | 0.43357 (16) | 0.0260 (9) | |
H1N | 0.1310 | 0.2312 | 0.4172 | 0.031* | |
N2 | 0.1300 (2) | 0.0746 (3) | 0.50271 (16) | 0.0256 (9) | |
H2N | 0.0856 | 0.0595 | 0.4830 | 0.031* | |
O1 | 0.28204 (18) | 0.3126 (3) | 0.42277 (14) | 0.0319 (8) | |
O2 | 0.24200 (19) | −0.0091 (3) | 0.53219 (16) | 0.0371 (9) | |
P1 | 0.14720 (6) | 0.05542 (10) | 0.32844 (5) | 0.0208 (3) | |
P2 | 0.09921 (7) | −0.18090 (10) | 0.39940 (5) | 0.0217 (3) | |
Cl1 | −0.02269 (6) | −0.02111 (10) | 0.41598 (5) | 0.0265 (3) | |
Cl2 | 0.01068 (6) | 0.19747 (10) | 0.34761 (6) | 0.0313 (3) | |
Cl3 | −0.22484 (13) | −0.00530 (19) | 0.29660 (10) | 0.0873 (7) | |
Cl4 | −0.19533 (10) | 0.23145 (15) | 0.26676 (8) | 0.0638 (5) | |
Cl5 | −0.14425 (14) | 0.0236 (3) | 0.22188 (10) | 0.1095 (10) | |
Cl6 | 0.41783 (13) | −0.1970 (2) | 0.57361 (8) | 0.0876 (7) | |
Cl7 | 0.33118 (11) | −0.2568 (2) | 0.64363 (12) | 0.0959 (8) | |
Cl8 | 0.42580 (19) | −0.0540 (3) | 0.66502 (10) | 0.1154 (10) | |
Cl9 | 0.49579 (12) | 0.2810 (3) | 0.50893 (10) | 0.1034 (9) | |
Cl10 | 0.42135 (13) | 0.44896 (19) | 0.55826 (10) | 0.0854 (6) | |
Cl11 | 0.41560 (13) | 0.1954 (2) | 0.57718 (9) | 0.0806 (6) | |
Pt1 | 0.067827 (9) | 0.010584 (14) | 0.374085 (7) | 0.01984 (7) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.031 (3) | 0.029 (3) | 0.026 (3) | −0.004 (2) | 0.008 (2) | −0.003 (2) |
C2 | 0.062 (4) | 0.023 (3) | 0.036 (3) | −0.011 (3) | 0.019 (3) | −0.007 (2) |
C3 | 0.067 (4) | 0.035 (3) | 0.039 (3) | −0.018 (3) | 0.019 (3) | −0.015 (3) |
C4 | 0.050 (3) | 0.042 (3) | 0.036 (3) | −0.013 (3) | 0.020 (3) | −0.011 (3) |
C5 | 0.045 (3) | 0.038 (3) | 0.033 (3) | −0.016 (2) | 0.020 (3) | −0.005 (2) |
C6 | 0.033 (3) | 0.022 (2) | 0.030 (3) | −0.006 (2) | 0.013 (2) | −0.006 (2) |
C7 | 0.036 (3) | 0.016 (2) | 0.028 (3) | −0.001 (2) | 0.013 (2) | −0.0042 (19) |
C8 | 0.019 (2) | 0.022 (2) | 0.028 (3) | 0.0004 (18) | 0.009 (2) | 0.0029 (19) |
C9 | 0.030 (3) | 0.023 (2) | 0.031 (3) | 0.000 (2) | 0.012 (2) | −0.004 (2) |
C10 | 0.036 (3) | 0.022 (2) | 0.038 (3) | 0.000 (2) | 0.017 (2) | 0.005 (2) |
C11 | 0.032 (3) | 0.028 (3) | 0.030 (3) | 0.002 (2) | 0.008 (2) | 0.009 (2) |
C12 | 0.029 (3) | 0.024 (2) | 0.028 (3) | −0.002 (2) | 0.008 (2) | −0.001 (2) |
C13 | 0.020 (2) | 0.019 (2) | 0.028 (3) | −0.0016 (18) | 0.013 (2) | 0.0007 (19) |
C14 | 0.030 (3) | 0.036 (3) | 0.018 (2) | −0.005 (2) | 0.008 (2) | −0.002 (2) |
C15 | 0.020 (2) | 0.025 (2) | 0.029 (3) | 0.0068 (19) | 0.008 (2) | 0.003 (2) |
C16 | 0.032 (3) | 0.033 (3) | 0.028 (3) | 0.003 (2) | 0.011 (2) | −0.002 (2) |
C17 | 0.043 (3) | 0.035 (3) | 0.032 (3) | 0.011 (2) | 0.021 (3) | 0.009 (2) |
C18 | 0.049 (3) | 0.027 (3) | 0.042 (3) | −0.001 (2) | 0.021 (3) | 0.009 (2) |
C19 | 0.041 (3) | 0.027 (3) | 0.034 (3) | −0.005 (2) | 0.015 (2) | 0.001 (2) |
C20 | 0.023 (2) | 0.023 (2) | 0.024 (2) | 0.0051 (19) | 0.008 (2) | 0.0030 (19) |
C21 | 0.026 (2) | 0.017 (2) | 0.028 (3) | −0.0020 (19) | 0.012 (2) | −0.0022 (19) |
C22 | 0.029 (3) | 0.025 (3) | 0.029 (3) | −0.005 (2) | 0.009 (2) | 0.000 (2) |
C23 | 0.035 (3) | 0.035 (3) | 0.034 (3) | −0.002 (2) | 0.002 (2) | 0.007 (2) |
C24 | 0.022 (3) | 0.033 (3) | 0.049 (3) | −0.003 (2) | −0.003 (2) | −0.001 (3) |
C25 | 0.025 (3) | 0.029 (3) | 0.040 (3) | −0.003 (2) | 0.015 (2) | −0.006 (2) |
C26 | 0.024 (2) | 0.028 (3) | 0.023 (2) | −0.001 (2) | 0.004 (2) | −0.002 (2) |
C27 | 0.027 (2) | 0.018 (2) | 0.025 (2) | 0.0015 (19) | 0.010 (2) | 0.0027 (19) |
C28 | 0.023 (2) | 0.027 (3) | 0.031 (3) | −0.003 (2) | 0.007 (2) | −0.003 (2) |
C29 | 0.032 (3) | 0.033 (3) | 0.033 (3) | −0.001 (2) | 0.013 (2) | −0.009 (2) |
C30 | 0.044 (3) | 0.037 (3) | 0.030 (3) | −0.008 (2) | 0.012 (3) | −0.010 (2) |
C31 | 0.024 (3) | 0.047 (3) | 0.036 (3) | −0.004 (2) | 0.004 (2) | −0.013 (3) |
C32 | 0.025 (3) | 0.038 (3) | 0.027 (3) | −0.003 (2) | 0.009 (2) | −0.007 (2) |
C33 | 0.027 (3) | 0.020 (2) | 0.027 (3) | −0.0032 (19) | 0.011 (2) | −0.0002 (19) |
C34 | 0.030 (3) | 0.024 (2) | 0.028 (3) | −0.003 (2) | 0.007 (2) | −0.004 (2) |
C35 | 0.024 (3) | 0.043 (3) | 0.039 (3) | −0.005 (2) | 0.005 (2) | −0.007 (2) |
C36 | 0.033 (3) | 0.033 (3) | 0.044 (3) | −0.012 (2) | 0.008 (3) | −0.012 (2) |
C37 | 0.052 (4) | 0.022 (3) | 0.047 (3) | −0.007 (2) | 0.018 (3) | −0.006 (2) |
C38 | 0.032 (3) | 0.022 (3) | 0.039 (3) | 0.000 (2) | 0.010 (2) | 0.000 (2) |
C39 | 0.023 (2) | 0.018 (2) | 0.038 (3) | −0.0022 (19) | 0.009 (2) | −0.003 (2) |
C40 | 0.029 (3) | 0.030 (3) | 0.035 (3) | 0.002 (2) | 0.009 (2) | 0.000 (2) |
C41 | 0.025 (3) | 0.039 (3) | 0.050 (4) | 0.008 (2) | 0.004 (3) | 0.001 (3) |
C42 | 0.022 (3) | 0.031 (3) | 0.062 (4) | 0.000 (2) | 0.015 (3) | −0.010 (3) |
C43 | 0.036 (3) | 0.024 (3) | 0.050 (3) | −0.004 (2) | 0.025 (3) | −0.007 (2) |
C44 | 0.035 (3) | 0.020 (2) | 0.028 (3) | −0.002 (2) | 0.014 (2) | 0.000 (2) |
C45 | 0.046 (4) | 0.054 (4) | 0.065 (5) | 0.009 (3) | −0.004 (3) | −0.014 (3) |
C46 | 0.059 (4) | 0.064 (4) | 0.059 (4) | 0.018 (3) | 0.021 (4) | 0.022 (3) |
C47 | 0.046 (4) | 0.060 (4) | 0.046 (4) | −0.010 (3) | 0.008 (3) | −0.001 (3) |
N1 | 0.030 (2) | 0.023 (2) | 0.024 (2) | −0.0068 (17) | 0.0073 (18) | −0.0063 (17) |
N2 | 0.027 (2) | 0.025 (2) | 0.023 (2) | −0.0037 (17) | 0.0056 (18) | −0.0011 (17) |
O1 | 0.0262 (19) | 0.0344 (19) | 0.032 (2) | −0.0067 (15) | 0.0057 (16) | −0.0051 (15) |
O2 | 0.027 (2) | 0.042 (2) | 0.040 (2) | −0.0029 (16) | 0.0076 (17) | 0.0014 (17) |
P1 | 0.0223 (6) | 0.0185 (6) | 0.0226 (6) | −0.0011 (5) | 0.0086 (5) | −0.0006 (5) |
P2 | 0.0223 (6) | 0.0179 (6) | 0.0252 (6) | −0.0005 (5) | 0.0082 (5) | 0.0011 (5) |
Cl1 | 0.0235 (6) | 0.0264 (6) | 0.0332 (6) | −0.0015 (5) | 0.0144 (5) | −0.0005 (5) |
Cl2 | 0.0268 (6) | 0.0216 (6) | 0.0478 (8) | 0.0059 (5) | 0.0153 (6) | 0.0079 (5) |
Cl3 | 0.0827 (15) | 0.0744 (14) | 0.0844 (15) | −0.0277 (11) | −0.0020 (12) | 0.0043 (11) |
Cl4 | 0.0539 (10) | 0.0514 (10) | 0.0743 (12) | 0.0068 (8) | 0.0039 (9) | −0.0007 (8) |
Cl5 | 0.0788 (15) | 0.165 (3) | 0.0718 (14) | 0.0568 (16) | 0.0054 (12) | −0.0338 (15) |
Cl6 | 0.0993 (16) | 0.1125 (17) | 0.0544 (11) | 0.0597 (14) | 0.0294 (11) | 0.0272 (11) |
Cl7 | 0.0502 (11) | 0.1010 (17) | 0.135 (2) | 0.0094 (11) | 0.0280 (12) | 0.0484 (15) |
Cl8 | 0.175 (3) | 0.1030 (19) | 0.0636 (14) | −0.0216 (19) | 0.0311 (16) | −0.0032 (13) |
Cl9 | 0.0576 (12) | 0.166 (3) | 0.0958 (18) | −0.0275 (14) | 0.0372 (12) | −0.0362 (17) |
Cl10 | 0.0928 (16) | 0.0622 (12) | 0.0967 (16) | −0.0186 (11) | 0.0240 (13) | −0.0119 (11) |
Cl11 | 0.0899 (15) | 0.0757 (13) | 0.0701 (13) | −0.0041 (11) | 0.0168 (11) | 0.0174 (10) |
Pt1 | 0.01984 (11) | 0.01687 (11) | 0.02382 (11) | −0.00016 (7) | 0.00840 (8) | −0.00007 (7) |
C1—N1 | 1.462 (6) | C25—H25 | 0.9300 |
C1—C6 | 1.520 (7) | C26—H26 | 0.9300 |
C1—C2 | 1.539 (7) | C27—C32 | 1.384 (7) |
C1—H1 | 0.9800 | C27—C28 | 1.384 (7) |
C2—C3 | 1.520 (8) | C27—P1 | 1.826 (5) |
C2—H2A | 0.9700 | C28—C29 | 1.387 (7) |
C2—H2B | 0.9700 | C28—H28 | 0.9300 |
C3—C4 | 1.501 (8) | C29—C30 | 1.383 (7) |
C3—H3A | 0.9700 | C29—H29 | 0.9300 |
C3—H3B | 0.9700 | C30—C31 | 1.365 (8) |
C4—C5 | 1.534 (8) | C30—H30 | 0.9300 |
C4—H4A | 0.9700 | C31—C32 | 1.388 (7) |
C4—H4B | 0.9700 | C31—H31 | 0.9300 |
C5—C6 | 1.523 (7) | C32—H32 | 0.9300 |
C5—H5A | 0.9700 | C33—C34 | 1.385 (7) |
C5—H5B | 0.9700 | C33—C38 | 1.393 (7) |
C6—N2 | 1.490 (6) | C33—P2 | 1.828 (5) |
C6—H6 | 0.9800 | C34—C35 | 1.383 (7) |
C7—O1 | 1.235 (6) | C34—H34 | 0.9300 |
C7—N1 | 1.332 (6) | C35—C36 | 1.382 (8) |
C7—C8 | 1.518 (7) | C35—H35 | 0.9300 |
C8—C9 | 1.388 (7) | C36—C37 | 1.370 (8) |
C8—C13 | 1.398 (6) | C36—H36 | 0.9300 |
C9—C10 | 1.387 (7) | C37—C38 | 1.378 (7) |
C9—H9 | 0.9300 | C37—H37 | 0.9300 |
C10—C11 | 1.382 (7) | C38—H38 | 0.9300 |
C10—H10 | 0.9300 | C39—C40 | 1.386 (7) |
C11—C12 | 1.385 (7) | C39—C44 | 1.397 (7) |
C11—H11 | 0.9300 | C39—P2 | 1.828 (5) |
C12—C13 | 1.398 (7) | C40—C41 | 1.384 (7) |
C12—H12 | 0.9300 | C40—H40 | 0.9300 |
C13—P1 | 1.834 (4) | C41—C42 | 1.375 (8) |
C14—O2 | 1.222 (6) | C41—H41 | 0.9300 |
C14—N2 | 1.332 (6) | C42—C43 | 1.370 (8) |
C14—C15 | 1.534 (7) | C42—H42 | 0.9300 |
C15—C16 | 1.393 (7) | C43—C44 | 1.377 (7) |
C15—C20 | 1.396 (7) | C43—H43 | 0.9300 |
C16—C17 | 1.381 (7) | C44—H44 | 0.9300 |
C16—H16 | 0.9300 | C45—Cl5 | 1.717 (8) |
C17—C18 | 1.376 (8) | C45—Cl4 | 1.739 (7) |
C17—H17 | 0.9300 | C45—Cl3 | 1.789 (8) |
C18—C19 | 1.374 (7) | C45—H45 | 0.9800 |
C18—H18 | 0.9300 | C46—Cl6 | 1.744 (7) |
C19—C20 | 1.407 (7) | C46—Cl7 | 1.745 (7) |
C19—H19 | 0.9300 | C46—Cl8 | 1.752 (8) |
C20—P2 | 1.828 (5) | C46—H46 | 0.9800 |
C21—C22 | 1.385 (7) | C47—Cl9 | 1.731 (7) |
C21—C26 | 1.394 (7) | C47—Cl11 | 1.748 (7) |
C21—P1 | 1.820 (5) | C47—Cl10 | 1.764 (7) |
C22—C23 | 1.383 (7) | C47—H47 | 0.9800 |
C22—H22 | 0.9300 | N1—H1N | 0.8600 |
C23—C24 | 1.378 (8) | N2—H2N | 0.8600 |
C23—H23 | 0.9300 | P1—Pt1 | 2.2631 (12) |
C24—C25 | 1.387 (8) | P2—Pt1 | 2.2535 (11) |
C24—H24 | 0.9300 | Cl1—Pt1 | 2.3540 (12) |
C25—C26 | 1.380 (7) | Cl2—Pt1 | 2.3509 (11) |
N1—C1—C6 | 112.1 (4) | C32—C27—C28 | 119.4 (4) |
N1—C1—C2 | 109.0 (4) | C32—C27—P1 | 116.3 (4) |
C6—C1—C2 | 108.2 (4) | C28—C27—P1 | 124.2 (4) |
N1—C1—H1 | 109.1 | C27—C28—C29 | 120.5 (5) |
C6—C1—H1 | 109.1 | C27—C28—H28 | 119.8 |
C2—C1—H1 | 109.1 | C29—C28—H28 | 119.8 |
C3—C2—C1 | 113.0 (4) | C30—C29—C28 | 119.7 (5) |
C3—C2—H2A | 109.0 | C30—C29—H29 | 120.2 |
C1—C2—H2A | 109.0 | C28—C29—H29 | 120.2 |
C3—C2—H2B | 109.0 | C31—C30—C29 | 119.9 (5) |
C1—C2—H2B | 109.0 | C31—C30—H30 | 120.0 |
H2A—C2—H2B | 107.8 | C29—C30—H30 | 120.0 |
C4—C3—C2 | 110.7 (5) | C30—C31—C32 | 120.9 (5) |
C4—C3—H3A | 109.5 | C30—C31—H31 | 119.6 |
C2—C3—H3A | 109.5 | C32—C31—H31 | 119.6 |
C4—C3—H3B | 109.5 | C27—C32—C31 | 119.7 (5) |
C2—C3—H3B | 109.5 | C27—C32—H32 | 120.2 |
H3A—C3—H3B | 108.1 | C31—C32—H32 | 120.2 |
C3—C4—C5 | 110.5 (5) | C34—C33—C38 | 119.1 (4) |
C3—C4—H4A | 109.5 | C34—C33—P2 | 121.5 (4) |
C5—C4—H4A | 109.5 | C38—C33—P2 | 119.4 (4) |
C3—C4—H4B | 109.5 | C35—C34—C33 | 120.0 (5) |
C5—C4—H4B | 109.5 | C35—C34—H34 | 120.0 |
H4A—C4—H4B | 108.1 | C33—C34—H34 | 120.0 |
C6—C5—C4 | 111.2 (5) | C36—C35—C34 | 120.3 (5) |
C6—C5—H5A | 109.4 | C36—C35—H35 | 119.9 |
C4—C5—H5A | 109.4 | C34—C35—H35 | 119.9 |
C6—C5—H5B | 109.4 | C37—C36—C35 | 119.8 (5) |
C4—C5—H5B | 109.4 | C37—C36—H36 | 120.1 |
H5A—C5—H5B | 108.0 | C35—C36—H36 | 120.1 |
N2—C6—C1 | 115.1 (4) | C36—C37—C38 | 120.4 (5) |
N2—C6—C5 | 110.2 (4) | C36—C37—H37 | 119.8 |
C1—C6—C5 | 110.7 (4) | C38—C37—H37 | 119.8 |
N2—C6—H6 | 106.8 | C37—C38—C33 | 120.2 (5) |
C1—C6—H6 | 106.8 | C37—C38—H38 | 119.9 |
C5—C6—H6 | 106.8 | C33—C38—H38 | 119.9 |
O1—C7—N1 | 124.1 (5) | C40—C39—C44 | 119.0 (5) |
O1—C7—C8 | 120.4 (4) | C40—C39—P2 | 122.9 (4) |
N1—C7—C8 | 115.4 (4) | C44—C39—P2 | 118.1 (4) |
C9—C8—C13 | 120.0 (4) | C41—C40—C39 | 119.8 (5) |
C9—C8—C7 | 114.1 (4) | C41—C40—H40 | 120.1 |
C13—C8—C7 | 125.8 (4) | C39—C40—H40 | 120.1 |
C10—C9—C8 | 120.7 (5) | C42—C41—C40 | 120.4 (5) |
C10—C9—H9 | 119.6 | C42—C41—H41 | 119.8 |
C8—C9—H9 | 119.6 | C40—C41—H41 | 119.8 |
C11—C10—C9 | 119.7 (5) | C43—C42—C41 | 120.2 (5) |
C11—C10—H10 | 120.2 | C43—C42—H42 | 119.9 |
C9—C10—H10 | 120.2 | C41—C42—H42 | 119.9 |
C10—C11—C12 | 119.9 (5) | C42—C43—C44 | 120.1 (5) |
C10—C11—H11 | 120.1 | C42—C43—H43 | 119.9 |
C12—C11—H11 | 120.1 | C44—C43—H43 | 119.9 |
C11—C12—C13 | 121.1 (4) | C43—C44—C39 | 120.3 (5) |
C11—C12—H12 | 119.4 | C43—C44—H44 | 119.9 |
C13—C12—H12 | 119.4 | C39—C44—H44 | 119.9 |
C8—C13—C12 | 118.5 (4) | Cl5—C45—Cl4 | 113.7 (4) |
C8—C13—P1 | 121.3 (3) | Cl5—C45—Cl3 | 108.7 (4) |
C12—C13—P1 | 120.2 (3) | Cl4—C45—Cl3 | 107.9 (4) |
O2—C14—N2 | 123.8 (5) | Cl5—C45—H45 | 108.8 |
O2—C14—C15 | 120.9 (4) | Cl4—C45—H45 | 108.8 |
N2—C14—C15 | 115.0 (4) | Cl3—C45—H45 | 108.8 |
C16—C15—C20 | 119.9 (4) | Cl6—C46—Cl7 | 112.4 (4) |
C16—C15—C14 | 111.7 (4) | Cl6—C46—Cl8 | 106.4 (4) |
C20—C15—C14 | 128.4 (4) | Cl7—C46—Cl8 | 108.9 (4) |
C17—C16—C15 | 121.3 (5) | Cl6—C46—H46 | 109.7 |
C17—C16—H16 | 119.4 | Cl7—C46—H46 | 109.7 |
C15—C16—H16 | 119.4 | Cl8—C46—H46 | 109.7 |
C18—C17—C16 | 119.6 (5) | Cl9—C47—Cl11 | 109.9 (4) |
C18—C17—H17 | 120.2 | Cl9—C47—Cl10 | 111.3 (4) |
C16—C17—H17 | 120.2 | Cl11—C47—Cl10 | 109.7 (4) |
C19—C18—C17 | 119.6 (5) | Cl9—C47—H47 | 108.6 |
C19—C18—H18 | 120.2 | Cl11—C47—H47 | 108.6 |
C17—C18—H18 | 120.2 | Cl10—C47—H47 | 108.6 |
C18—C19—C20 | 122.2 (5) | C7—N1—C1 | 122.0 (4) |
C18—C19—H19 | 118.9 | C7—N1—H1N | 119.0 |
C20—C19—H19 | 118.9 | C1—N1—H1N | 119.0 |
C15—C20—C19 | 117.3 (4) | C14—N2—C6 | 126.5 (4) |
C15—C20—P2 | 124.2 (4) | C14—N2—H2N | 116.7 |
C19—C20—P2 | 118.4 (4) | C6—N2—H2N | 116.7 |
C22—C21—C26 | 119.3 (4) | C21—P1—C27 | 109.8 (2) |
C22—C21—P1 | 120.2 (4) | C21—P1—C13 | 100.0 (2) |
C26—C21—P1 | 120.2 (4) | C27—P1—C13 | 102.2 (2) |
C23—C22—C21 | 120.3 (5) | C21—P1—Pt1 | 119.79 (16) |
C23—C22—H22 | 119.9 | C27—P1—Pt1 | 109.82 (16) |
C21—C22—H22 | 119.9 | C13—P1—Pt1 | 113.52 (15) |
C24—C23—C22 | 120.3 (5) | C20—P2—C33 | 105.7 (2) |
C24—C23—H23 | 119.8 | C20—P2—C39 | 103.3 (2) |
C22—C23—H23 | 119.8 | C33—P2—C39 | 102.5 (2) |
C23—C24—C25 | 119.7 (5) | C20—P2—Pt1 | 112.54 (15) |
C23—C24—H24 | 120.2 | C33—P2—Pt1 | 109.69 (16) |
C25—C24—H24 | 120.2 | C39—P2—Pt1 | 121.68 (16) |
C26—C25—C24 | 120.2 (5) | P2—Pt1—P1 | 101.15 (4) |
C26—C25—H25 | 119.9 | P2—Pt1—Cl2 | 167.98 (4) |
C24—C25—H25 | 119.9 | P1—Pt1—Cl2 | 89.35 (4) |
C25—C26—C21 | 120.1 (5) | P2—Pt1—Cl1 | 84.11 (4) |
C25—C26—H26 | 120.0 | P1—Pt1—Cl1 | 174.15 (4) |
C21—C26—H26 | 120.0 | Cl2—Pt1—Cl1 | 85.17 (4) |
N1—C1—C2—C3 | 178.9 (5) | P2—C39—C40—C41 | −177.8 (4) |
C6—C1—C2—C3 | 56.7 (6) | C39—C40—C41—C42 | 1.7 (8) |
C1—C2—C3—C4 | −56.3 (7) | C40—C41—C42—C43 | −2.8 (8) |
C2—C3—C4—C5 | 54.8 (7) | C41—C42—C43—C44 | 0.5 (8) |
C3—C4—C5—C6 | −56.9 (7) | C42—C43—C44—C39 | 2.9 (7) |
N1—C1—C6—N2 | 56.8 (6) | C40—C39—C44—C43 | −3.9 (7) |
C2—C1—C6—N2 | 177.1 (4) | P2—C39—C44—C43 | 175.6 (4) |
N1—C1—C6—C5 | −177.5 (4) | O1—C7—N1—C1 | 8.9 (7) |
C2—C1—C6—C5 | −57.2 (6) | C8—C7—N1—C1 | −167.5 (4) |
C4—C5—C6—N2 | −172.7 (4) | C6—C1—N1—C7 | −171.6 (4) |
C4—C5—C6—C1 | 58.8 (6) | C2—C1—N1—C7 | 68.5 (6) |
O1—C7—C8—C9 | −62.6 (6) | O2—C14—N2—C6 | −17.2 (8) |
N1—C7—C8—C9 | 113.9 (5) | C15—C14—N2—C6 | 156.0 (4) |
O1—C7—C8—C13 | 118.2 (5) | C1—C6—N2—C14 | 66.5 (6) |
N1—C7—C8—C13 | −65.3 (6) | C5—C6—N2—C14 | −59.5 (6) |
C13—C8—C9—C10 | 1.4 (7) | C22—C21—P1—C27 | −127.3 (4) |
C7—C8—C9—C10 | −177.9 (5) | C26—C21—P1—C27 | 58.5 (4) |
C8—C9—C10—C11 | −1.4 (8) | C22—C21—P1—C13 | 125.7 (4) |
C9—C10—C11—C12 | 0.6 (8) | C26—C21—P1—C13 | −48.5 (4) |
C10—C11—C12—C13 | 0.3 (8) | C22—C21—P1—Pt1 | 1.1 (4) |
C9—C8—C13—C12 | −0.5 (7) | C26—C21—P1—Pt1 | −173.1 (3) |
C7—C8—C13—C12 | 178.7 (4) | C32—C27—P1—C21 | 163.7 (4) |
C9—C8—C13—P1 | 176.9 (4) | C28—C27—P1—C21 | −20.5 (5) |
C7—C8—C13—P1 | −3.9 (7) | C32—C27—P1—C13 | −90.8 (4) |
C11—C12—C13—C8 | −0.4 (7) | C28—C27—P1—C13 | 85.0 (4) |
C11—C12—C13—P1 | −177.8 (4) | C32—C27—P1—Pt1 | 30.0 (4) |
O2—C14—C15—C16 | 71.4 (6) | C28—C27—P1—Pt1 | −154.2 (4) |
N2—C14—C15—C16 | −102.0 (5) | C8—C13—P1—C21 | −49.2 (4) |
O2—C14—C15—C20 | −109.1 (6) | C12—C13—P1—C21 | 128.1 (4) |
N2—C14—C15—C20 | 77.5 (6) | C8—C13—P1—C27 | −162.2 (4) |
C20—C15—C16—C17 | −2.8 (7) | C12—C13—P1—C27 | 15.2 (4) |
C14—C15—C16—C17 | 176.7 (5) | C8—C13—P1—Pt1 | 79.6 (4) |
C15—C16—C17—C18 | −0.2 (8) | C12—C13—P1—Pt1 | −103.1 (4) |
C16—C17—C18—C19 | 1.8 (8) | C15—C20—P2—C33 | −169.7 (4) |
C17—C18—C19—C20 | −0.4 (8) | C19—C20—P2—C33 | 14.0 (4) |
C16—C15—C20—C19 | 4.1 (7) | C15—C20—P2—C39 | 83.0 (4) |
C14—C15—C20—C19 | −175.3 (5) | C19—C20—P2—C39 | −93.3 (4) |
C16—C15—C20—P2 | −172.2 (4) | C15—C20—P2—Pt1 | −50.0 (4) |
C14—C15—C20—P2 | 8.4 (7) | C19—C20—P2—Pt1 | 133.7 (4) |
C18—C19—C20—C15 | −2.6 (8) | C34—C33—P2—C20 | 103.5 (4) |
C18—C19—C20—P2 | 173.9 (4) | C38—C33—P2—C20 | −74.3 (4) |
C26—C21—C22—C23 | −2.8 (7) | C34—C33—P2—C39 | −148.7 (4) |
P1—C21—C22—C23 | −177.1 (4) | C38—C33—P2—C39 | 33.6 (5) |
C21—C22—C23—C24 | 0.2 (8) | C34—C33—P2—Pt1 | −18.1 (5) |
C22—C23—C24—C25 | 1.8 (8) | C38—C33—P2—Pt1 | 164.2 (4) |
C23—C24—C25—C26 | −1.3 (8) | C40—C39—P2—C20 | −9.9 (5) |
C24—C25—C26—C21 | −1.3 (7) | C44—C39—P2—C20 | 170.7 (4) |
C22—C21—C26—C25 | 3.3 (7) | C40—C39—P2—C33 | −119.5 (4) |
P1—C21—C26—C25 | 177.6 (4) | C44—C39—P2—C33 | 61.0 (4) |
C32—C27—C28—C29 | 1.5 (7) | C40—C39—P2—Pt1 | 117.6 (4) |
P1—C27—C28—C29 | −174.2 (4) | C44—C39—P2—Pt1 | −61.8 (4) |
C27—C28—C29—C30 | −0.3 (8) | C20—P2—Pt1—P1 | 137.81 (16) |
C28—C29—C30—C31 | −0.8 (8) | C33—P2—Pt1—P1 | −104.87 (17) |
C29—C30—C31—C32 | 0.6 (9) | C39—P2—Pt1—P1 | 14.5 (2) |
C28—C27—C32—C31 | −1.6 (7) | C20—P2—Pt1—Cl2 | −71.7 (3) |
P1—C27—C32—C31 | 174.4 (4) | C33—P2—Pt1—Cl2 | 45.6 (3) |
C30—C31—C32—C27 | 0.6 (8) | C39—P2—Pt1—Cl2 | 165.0 (3) |
C38—C33—C34—C35 | 3.4 (8) | C20—P2—Pt1—Cl1 | −44.79 (17) |
P2—C33—C34—C35 | −174.3 (4) | C33—P2—Pt1—Cl1 | 72.53 (17) |
C33—C34—C35—C36 | −1.6 (8) | C39—P2—Pt1—Cl1 | −168.1 (2) |
C34—C35—C36—C37 | −0.5 (9) | C21—P1—Pt1—P2 | −57.43 (18) |
C35—C36—C37—C38 | 0.8 (9) | C27—P1—Pt1—P2 | 70.96 (16) |
C36—C37—C38—C33 | 1.0 (9) | C13—P1—Pt1—P2 | −175.29 (17) |
C34—C33—C38—C37 | −3.1 (8) | C21—P1—Pt1—Cl2 | 128.47 (17) |
P2—C33—C38—C37 | 174.7 (4) | C27—P1—Pt1—Cl2 | −103.14 (16) |
C44—C39—C40—C41 | 1.6 (7) | C13—P1—Pt1—Cl2 | 10.60 (17) |
D—H···A | D—H | H···A | D···A | D—H···A |
C1—H1···O1 | 0.98 | 2.66 | 2.814 (8) | 89 |
C1—H1···O2 | 0.98 | 2.65 | 3.187 (8) | 115 |
C2—H2A···O1 | 0.97 | 2.60 | 3.163 (9) | 117 |
C22—H22···O2 | 0.93 | 2.47 | 3.178 (8) | 133 |
C5—H5B···Cl1i | 0.97 | 2.80 | 3.669 (7) | 150 |
C9—H9···C1Xii | 0.93 | 2.82 | 3.71 (1) | 162 |
C34—H34···Cl1 | 0.93 | 2.72 | 3.330 (6) | 124 |
C45—H45···Cl2 | 0.98 | 2.61 | 3.445 (9) | 144 |
C46—H46···O2 | 0.98 | 2.05 | 3.015 (10) | 170 |
C47—H47···O1 | 0.98 | 2.18 | 3.151 (9) | 171 |
N2—H2N···Cl1 | 0.86 | 2.42 | 3.254 (5) | 164 |
N1—H1N···Cl2 | 0.86 | 2.46 | 3.296 (5) | 163 |
Symmetry codes: (i) −x, −y, −z+1; (ii) x, y+1, z. |