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
Key indicators
- Single-crystal X-ray study
- T = 153 K
- Mean (C-C) = 0.007 Å
- R factor = 0.036
- wR factor = 0.092
- Data-to-parameter ratio = 15.5
checkCIF/PLATON results
No syntax errors found
Alert level A PLAT027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 24.91 Deg.
Alert level B PLAT482_ALERT_4_B Small D-H..A Angle Rep for C1 .. O1 .. 89.00 Deg.
Alert level C RINTA01_ALERT_3_C The value of Rint is greater than 0.10 Rint given 0.133 PLAT020_ALERT_3_C The value of Rint is greater than 0.10 ......... 0.13 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors for C45 PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors for C46 PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors for C47 PLAT369_ALERT_2_C Long C(sp2)-C(sp2) Bond C14 - C15 ... 1.53 Ang. PLAT431_ALERT_2_C Short Inter HL..A Contact Cl6 .. Cl9 .. 3.23 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H1 .. O1 .. 2.66 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H1 .. O2 .. 2.65 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H9 .. C1X .. 2.82 Ang. PLAT716_ALERT_1_C H...A Unknown or Inconsistent Label .......... C1X H9 C1X PLAT717_ALERT_1_C D...A Unknown or Inconsistent Label .......... C1X C9 C1X PLAT718_ALERT_1_C D-H..A Unknown or Inconsistent Label .......... C1X C9 H9 C1X PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 C H Cl3 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 3 C H Cl3
1 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 16 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 9 ALERT type 4 Improvement, methodology, query or suggestion
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. |
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