# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_e2756a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C65 H65 N5 O8 P2 Pt), 3(C H Cl3)' _chemical_formula_sum 'C133 H133 Cl9 N10 O16 P4 Pt2' _chemical_formula_weight 2960.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 17.3360(4) _cell_length_b 21.4653(5) _cell_length_c 21.4776(4) _cell_angle_alpha 113.8400(10) _cell_angle_beta 104.1150(10) _cell_angle_gamma 102.1680(10) _cell_volume 6644.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9953 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 27.39 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2996 _exptl_absorpt_coefficient_mu 2.398 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8501 _exptl_absorpt_correction_T_max 0.8895 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 132009 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0664 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 29.14 _reflns_number_total 35751 _reflns_number_gt 24738 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0726P)^2^+25.9771P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 35751 _refine_ls_number_parameters 1567 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0930 _refine_ls_R_factor_gt 0.0556 _refine_ls_wR_factor_ref 0.1605 _refine_ls_wR_factor_gt 0.1403 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.463523(12) 0.302722(10) 0.771730(10) 0.01919(6) Uani 1 1 d . . . P1 P 0.58042(8) 0.37706(7) 0.87820(7) 0.0196(3) Uani 1 1 d . . . C1 C 0.6643(3) 0.3388(3) 0.8799(3) 0.0243(11) Uani 1 1 d . . . C2 C 0.6766(4) 0.3039(4) 0.8146(4) 0.0392(15) Uani 1 1 d . . . H2 H 0.6369 0.2950 0.7700 0.047 Uiso 1 1 calc R . . C3 C 0.7465(5) 0.2820(4) 0.8143(4) 0.0532(19) Uani 1 1 d . . . H3 H 0.7546 0.2580 0.7697 0.064 Uiso 1 1 calc R . . C4 C 0.8037(5) 0.2955(4) 0.8791(5) 0.058(2) Uani 1 1 d . . . H4 H 0.8529 0.2826 0.8794 0.070 Uiso 1 1 calc R . . C5 C 0.7905(4) 0.3274(4) 0.9438(4) 0.053(2) Uani 1 1 d . . . H5 H 0.8292 0.3345 0.9879 0.064 Uiso 1 1 calc R . . C6 C 0.7207(4) 0.3493(3) 0.9445(3) 0.0341(13) Uani 1 1 d . . . H6 H 0.7117 0.3715 0.9891 0.041 Uiso 1 1 calc R . . C7 C 0.5658(3) 0.3961(3) 0.9639(3) 0.0233(11) Uani 1 1 d . . . C8 C 0.5391(4) 0.3383(3) 0.9771(3) 0.0318(13) Uani 1 1 d . . . H8 H 0.5305 0.2902 0.9423 0.038 Uiso 1 1 calc R . . C9 C 0.5249(4) 0.3519(4) 1.0424(4) 0.0445(17) Uani 1 1 d . . . H9 H 0.5053 0.3124 1.0510 0.053 Uiso 1 1 calc R . . C10 C 0.5385(4) 0.4196(4) 1.0928(4) 0.0454(17) Uani 1 1 d . . . H10 H 0.5289 0.4276 1.1367 0.054 Uiso 1 1 calc R . . C11 C 0.5662(4) 0.4775(4) 1.0814(3) 0.0443(17) Uani 1 1 d . . . H11 H 0.5762 0.5254 1.1175 0.053 Uiso 1 1 calc R . . C12 C 0.5795(4) 0.4658(3) 1.0167(3) 0.0347(13) Uani 1 1 d . . . H12 H 0.5980 0.5059 1.0087 0.042 Uiso 1 1 calc R . . P2 P 0.36664(8) 0.22448(7) 0.65447(7) 0.0208(3) Uani 1 1 d . . . C13 C 0.2845(3) 0.1431(3) 0.6349(3) 0.0271(12) Uani 1 1 d . . . C14 C 0.2605(4) 0.1356(3) 0.6891(4) 0.0359(14) Uani 1 1 d . . . H14 H 0.2874 0.1735 0.7384 0.043 Uiso 1 1 calc R . . C15 C 0.1974(4) 0.0727(4) 0.6718(4) 0.0458(17) Uani 1 1 d . . . H15 H 0.1813 0.0678 0.7093 0.055 Uiso 1 1 calc R . . C16 C 0.1582(4) 0.0179(3) 0.6010(5) 0.053(2) Uani 1 1 d . . . H16 H 0.1160 -0.0254 0.5896 0.063 Uiso 1 1 calc R . . C17 C 0.1792(4) 0.0252(3) 0.5475(4) 0.053(2) Uani 1 1 d . . . H17 H 0.1505 -0.0127 0.4984 0.063 Uiso 1 1 calc R . . C18 C 0.2427(4) 0.0876(3) 0.5625(4) 0.0415(16) Uani 1 1 d . . . H18 H 0.2569 0.0921 0.5241 0.050 Uiso 1 1 calc R . . C19 C 0.4290(3) 0.1893(3) 0.6005(3) 0.0250(11) Uani 1 1 d . . . C20 C 0.4817(4) 0.1556(3) 0.6233(3) 0.0340(13) Uani 1 1 d . . . H20 H 0.4833 0.1506 0.6656 0.041 Uiso 1 1 calc R . . C21 C 0.5312(4) 0.1296(4) 0.5856(4) 0.0423(16) Uani 1 1 d . . . H21 H 0.5669 0.1068 0.6018 0.051 Uiso 1 1 calc R . . C22 C 0.5290(4) 0.1368(4) 0.5235(4) 0.0461(17) Uani 1 1 d . . . H22 H 0.5635 0.1190 0.4974 0.055 Uiso 1 1 calc R . . C23 C 0.4771(4) 0.1693(4) 0.5002(3) 0.0392(15) Uani 1 1 d . . . H23 H 0.4756 0.1738 0.4577 0.047 Uiso 1 1 calc R . . C24 C 0.4267(4) 0.1959(3) 0.5381(3) 0.0302(12) Uani 1 1 d . . . H24 H 0.3908 0.2184 0.5216 0.036 Uiso 1 1 calc R . . C25 C 0.6335(3) 0.4675(3) 0.8926(3) 0.0241(11) Uani 1 1 d . . . H25A H 0.5919 0.4929 0.8925 0.029 Uiso 1 1 calc R . . H25B H 0.6790 0.4952 0.9418 0.029 Uiso 1 1 calc R . . C26 C 0.6722(3) 0.4696(3) 0.8370(3) 0.0272(12) Uani 1 1 d . . . H26A H 0.7173 0.4480 0.8384 0.033 Uiso 1 1 calc R . . H26B H 0.6283 0.4421 0.7870 0.033 Uiso 1 1 calc R . . O1 O 0.7066(2) 0.5437(2) 0.8564(2) 0.0317(9) Uani 1 1 d . . . C27 C 0.7453(4) 0.5541(3) 0.8083(4) 0.0388(15) Uani 1 1 d . . . H27A H 0.7019 0.5330 0.7588 0.047 Uiso 1 1 calc R . . H27B H 0.7876 0.5296 0.8046 0.047 Uiso 1 1 calc R . . C28 C 0.7878(4) 0.6341(4) 0.8382(5) 0.052(2) Uani 1 1 d . . . H28A H 0.8266 0.6557 0.8897 0.063 Uiso 1 1 calc R . . H28B H 0.8222 0.6420 0.8096 0.063 Uiso 1 1 calc R . . O2 O 0.7271(3) 0.6691(2) 0.8349(3) 0.0498(12) Uani 1 1 d . . . C29 C 0.7639(5) 0.7455(4) 0.8760(5) 0.067(2) Uani 1 1 d . . . H29A H 0.8066 0.7633 0.8581 0.080 Uiso 1 1 calc R . . H29B H 0.7931 0.7601 0.9281 0.080 Uiso 1 1 calc R . . C30 C 0.6968(5) 0.7789(4) 0.8693(5) 0.062(2) Uani 1 1 d . . . H30A H 0.6491 0.7536 0.8779 0.074 Uiso 1 1 calc R . . H30B H 0.7206 0.8303 0.9081 0.074 Uiso 1 1 calc R . . O3 O 0.6644(3) 0.7764(3) 0.8001(3) 0.0552(13) Uani 1 1 d . . . C31 C 0.7156(6) 0.8333(5) 0.7958(5) 0.069(2) Uani 1 1 d . . . H31A H 0.7744 0.8330 0.8071 0.083 Uiso 1 1 calc R . . H31B H 0.7168 0.8804 0.8322 0.083 Uiso 1 1 calc R . . C32 C 0.6816(5) 0.8247(5) 0.7201(5) 0.062(2) Uani 1 1 d . . . H32A H 0.7263 0.8567 0.7143 0.074 Uiso 1 1 calc R . . H32B H 0.6706 0.7740 0.6841 0.074 Uiso 1 1 calc R . . N1 N 0.6038(4) 0.8412(3) 0.7022(3) 0.0504(15) Uani 1 1 d . . . H1 H 0.5546 0.8065 0.6846 0.060 Uiso 1 1 calc R . . C33 C 0.6042(6) 0.9067(4) 0.7113(4) 0.055(2) Uani 1 1 d . . . O4 O 0.6693(4) 0.9603(3) 0.7400(3) 0.0779(19) Uani 1 1 d . . . C34 C 0.5194(6) 0.9122(4) 0.6844(4) 0.054(2) Uani 1 1 d . . . N2 N 0.4520(4) 0.8507(3) 0.6477(3) 0.0470(14) Uani 1 1 d . . . C35 C 0.3760(6) 0.8537(4) 0.6240(4) 0.0507(19) Uani 1 1 d . . . C36 C 0.3612(7) 0.9196(5) 0.6358(5) 0.072(3) Uani 1 1 d . . . H36 H 0.3058 0.9210 0.6192 0.087 Uiso 1 1 calc R . . C37 C 0.4341(8) 0.9823(5) 0.6737(5) 0.076(3) Uani 1 1 d . . . H37 H 0.4284 1.0278 0.6823 0.092 Uiso 1 1 calc R . . C38 C 0.5127(7) 0.9798(4) 0.6985(5) 0.067(2) Uani 1 1 d . . . H38 H 0.5615 1.0227 0.7246 0.080 Uiso 1 1 calc R . . C39 C 0.3005(5) 0.7833(5) 0.5835(4) 0.053(2) Uani 1 1 d . . . O5 O 0.2281(4) 0.7820(4) 0.5636(3) 0.0704(17) Uani 1 1 d . . . N3 N 0.3222(4) 0.7244(3) 0.5718(3) 0.0505(15) Uani 1 1 d . . . H3A H 0.3765 0.7305 0.5857 0.061 Uiso 1 1 calc R . . C40 C 0.2617(5) 0.6515(4) 0.5375(4) 0.0526(18) Uani 1 1 d . . . H40A H 0.2878 0.6159 0.5148 0.063 Uiso 1 1 calc R . . H40B H 0.2115 0.6452 0.4985 0.063 Uiso 1 1 calc R . . C41 C 0.2345(5) 0.6380(4) 0.5937(4) 0.0548(19) Uani 1 1 d . . . H41A H 0.2853 0.6517 0.6363 0.066 Uiso 1 1 calc R . . H41B H 0.2007 0.6685 0.6108 0.066 Uiso 1 1 calc R . . O6 O 0.1857(3) 0.5643(3) 0.5634(3) 0.0514(12) Uani 1 1 d . . . C42 C 0.1332(5) 0.5544(4) 0.6032(5) 0.056(2) Uani 1 1 d . . . H42A H 0.0908 0.5783 0.5981 0.068 Uiso 1 1 calc R . . H42B H 0.1686 0.5775 0.6558 0.068 Uiso 1 1 calc R . . C43 C 0.0886(5) 0.4754(4) 0.5754(4) 0.0485(17) Uani 1 1 d . . . H43A H 0.0374 0.4688 0.5880 0.058 Uiso 1 1 calc R . . H43B H 0.0705 0.4490 0.5214 0.058 Uiso 1 1 calc R . . O57 O 0.1436(3) 0.4463(2) 0.6069(3) 0.0437(11) Uani 1 1 d . . . C44 C 0.0973(4) 0.3765(4) 0.5944(4) 0.0438(16) Uani 1 1 d . . . H44A H 0.0782 0.3409 0.5419 0.053 Uiso 1 1 calc R . . H44B H 0.0463 0.3783 0.6071 0.053 Uiso 1 1 calc R . . C45 C 0.1512(4) 0.3525(3) 0.6395(3) 0.0328(13) Uani 1 1 d . . . H45A H 0.1850 0.3943 0.6889 0.039 Uiso 1 1 calc R . . H45B H 0.1142 0.3147 0.6451 0.039 Uiso 1 1 calc R . . O8 O 0.2066(2) 0.3243(2) 0.6069(2) 0.0293(8) Uani 1 1 d . . . C46 C 0.2505(3) 0.2953(3) 0.6463(3) 0.0273(12) Uani 1 1 d . . . H46A H 0.2097 0.2567 0.6481 0.033 Uiso 1 1 calc R . . H46B H 0.2856 0.3339 0.6971 0.033 Uiso 1 1 calc R . . C47 C 0.3068(3) 0.2640(3) 0.6078(3) 0.0231(11) Uani 1 1 d . . . H47A H 0.3469 0.3029 0.6059 0.028 Uiso 1 1 calc R . . H47B H 0.2711 0.2261 0.5568 0.028 Uiso 1 1 calc R . . C48 C 0.4596(3) 0.3853(3) 0.7517(3) 0.0218(10) Uani 1 1 d . . . C49 C 0.4552(3) 0.4333(3) 0.7371(3) 0.0240(11) Uani 1 1 d . . . C50 C 0.4534(3) 0.4893(3) 0.7172(3) 0.0242(11) Uani 1 1 d . . . C51 C 0.5276(3) 0.5500(3) 0.7470(3) 0.0267(11) Uani 1 1 d . . . H51 H 0.5765 0.5558 0.7834 0.032 Uiso 1 1 calc R . . C52 C 0.5295(4) 0.6010(3) 0.7235(3) 0.0311(12) Uani 1 1 d . . . H52 H 0.5802 0.6412 0.7428 0.037 Uiso 1 1 calc R . . C53 C 0.4567(4) 0.5933(3) 0.6712(3) 0.0331(13) Uani 1 1 d . . . C54 C 0.3821(4) 0.5358(3) 0.6436(4) 0.0395(15) Uani 1 1 d . . . H54 H 0.3326 0.5317 0.6089 0.047 Uiso 1 1 calc R . . C55 C 0.3799(4) 0.4842(3) 0.6669(3) 0.0342(13) Uani 1 1 d . . . H55 H 0.3285 0.4451 0.6488 0.041 Uiso 1 1 calc R . . C56 C 0.4643(4) 0.6452(3) 0.6444(3) 0.0374(14) Uani 1 1 d . . . N4 N 0.4727(4) 0.6866(3) 0.6238(4) 0.0538(16) Uani 1 1 d . . . C57 C 0.4614(3) 0.2216(3) 0.7948(3) 0.0264(11) Uani 1 1 d . . . C58 C 0.4560(4) 0.1744(3) 0.8129(3) 0.0326(13) Uani 1 1 d . . . C59 C 0.4433(4) 0.1228(3) 0.8388(3) 0.0369(14) Uani 1 1 d . . . C60 C 0.5081(5) 0.1228(4) 0.8910(4) 0.059(2) Uani 1 1 d . . . H60 H 0.5638 0.1560 0.9079 0.071 Uiso 1 1 calc R . . C61 C 0.4943(5) 0.0761(4) 0.9189(4) 0.063(2) Uani 1 1 d . . . H61 H 0.5398 0.0772 0.9550 0.075 Uiso 1 1 calc R . . C62 C 0.4124(5) 0.0268(4) 0.8938(4) 0.0488(18) Uani 1 1 d . . . C63 C 0.3496(4) 0.0234(4) 0.8413(4) 0.0534(19) Uani 1 1 d . . . H63 H 0.2947 -0.0116 0.8231 0.064 Uiso 1 1 calc R . . C64 C 0.3634(4) 0.0706(4) 0.8124(4) 0.0473(17) Uani 1 1 d . . . H64 H 0.3180 0.0672 0.7745 0.057 Uiso 1 1 calc R . . C65 C 0.3975(5) -0.0241(4) 0.9214(4) 0.055(2) Uani 1 1 d . . . N5 N 0.3847(4) -0.0649(4) 0.9424(4) 0.068(2) Uani 1 1 d . . . Pt2 Pt 0.978444(12) 0.311590(10) 0.772206(10) 0.02155(6) Uani 1 1 d . . . P3 P 0.88070(8) 0.23110(7) 0.65578(7) 0.0214(3) Uani 1 1 d . . . C66 C 0.8044(3) 0.1484(3) 0.6405(3) 0.0278(12) Uani 1 1 d . . . C67 C 0.7478(4) 0.0981(3) 0.5695(4) 0.0384(15) Uani 1 1 d . . . H67 H 0.7496 0.1061 0.5294 0.046 Uiso 1 1 calc R . . C68 C 0.6884(4) 0.0357(3) 0.5583(4) 0.0459(18) Uani 1 1 d . . . H68 H 0.6497 0.0011 0.5101 0.055 Uiso 1 1 calc R . . C69 C 0.6848(4) 0.0235(3) 0.6141(5) 0.053(2) Uani 1 1 d . . . H69 H 0.6444 -0.0197 0.6050 0.063 Uiso 1 1 calc R . . C70 C 0.7395(4) 0.0732(4) 0.6847(5) 0.0485(18) Uani 1 1 d . . . H70 H 0.7362 0.0646 0.7242 0.058 Uiso 1 1 calc R . . C71 C 0.7993(4) 0.1359(3) 0.6978(4) 0.0355(14) Uani 1 1 d . . . H71 H 0.8368 0.1703 0.7464 0.043 Uiso 1 1 calc R . . C72 C 0.9399(3) 0.1978(3) 0.5979(3) 0.0245(11) Uani 1 1 d . . . C73 C 0.9935(4) 0.1626(3) 0.6170(3) 0.0312(13) Uani 1 1 d . . . H73 H 0.9961 0.1546 0.6578 0.037 Uiso 1 1 calc R . . C74 C 1.0425(4) 0.1396(4) 0.5768(4) 0.0414(15) Uani 1 1 d . . . H74 H 1.0788 0.1157 0.5898 0.050 Uiso 1 1 calc R . . C75 C 1.0390(4) 0.1512(4) 0.5171(3) 0.0411(16) Uani 1 1 d . . . H75 H 1.0730 0.1354 0.4896 0.049 Uiso 1 1 calc R . . C76 C 0.9864(4) 0.1855(4) 0.4981(3) 0.0378(14) Uani 1 1 d . . . H76 H 0.9843 0.1934 0.4574 0.045 Uiso 1 1 calc R . . C77 C 0.9368(4) 0.2084(3) 0.5375(3) 0.0321(13) Uani 1 1 d . . . H77 H 0.9002 0.2317 0.5235 0.039 Uiso 1 1 calc R . . P4 P 1.09038(8) 0.38987(7) 0.88127(7) 0.0206(3) Uani 1 1 d . . . C78 C 1.1801(3) 0.3586(3) 0.8911(3) 0.0238(11) Uani 1 1 d . . . C79 C 1.2264(3) 0.3630(3) 0.9561(3) 0.0268(11) Uani 1 1 d . . . H79 H 1.2094 0.3799 0.9970 0.032 Uiso 1 1 calc R . . C80 C 1.2977(4) 0.3426(3) 0.9617(4) 0.0384(15) Uani 1 1 d . . . H80 H 1.3285 0.3445 1.0059 0.046 Uiso 1 1 calc R . . C81 C 1.3239(4) 0.3195(4) 0.9029(4) 0.0421(16) Uani 1 1 d . . . H81 H 1.3732 0.3065 0.9072 0.051 Uiso 1 1 calc R . . C82 C 1.2789(4) 0.3155(4) 0.8385(4) 0.0417(16) Uani 1 1 d . . . H82 H 1.2978 0.3004 0.7987 0.050 Uiso 1 1 calc R . . C83 C 1.2054(4) 0.3333(3) 0.8310(3) 0.0342(13) Uani 1 1 d . . . H83 H 1.1729 0.3284 0.7856 0.041 Uiso 1 1 calc R . . C84 C 1.0675(3) 0.4051(3) 0.9637(3) 0.0262(11) Uani 1 1 d . . . C85 C 1.0292(4) 0.3447(3) 0.9693(3) 0.0346(13) Uani 1 1 d . . . H85 H 1.0144 0.2969 0.9309 0.041 Uiso 1 1 calc R . . C86 C 1.0127(4) 0.3566(4) 1.0337(4) 0.0467(17) Uani 1 1 d . . . H86 H 0.9865 0.3160 1.0385 0.056 Uiso 1 1 calc R . . C87 C 1.0335(4) 0.4245(4) 1.0888(4) 0.0462(17) Uani 1 1 d . . . H87 H 1.0221 0.4310 1.1317 0.055 Uiso 1 1 calc R . . C88 C 1.0710(4) 0.4839(4) 1.0831(3) 0.0433(16) Uani 1 1 d . . . H88 H 1.0856 0.5314 1.1220 0.052 Uiso 1 1 calc R . . C89 C 1.0876(4) 0.4747(4) 1.0202(3) 0.0371(14) Uani 1 1 d . . . H89 H 1.1126 0.5160 1.0160 0.045 Uiso 1 1 calc R . . C90 C 0.8148(3) 0.2678(3) 0.6101(3) 0.0259(11) Uani 1 1 d . . . H90A H 0.8520 0.3100 0.6106 0.031 Uiso 1 1 calc R . . H90B H 0.7824 0.2303 0.5583 0.031 Uiso 1 1 calc R . . C91 C 0.7532(3) 0.2914(3) 0.6459(3) 0.0269(11) Uani 1 1 d . . . H91A H 0.7144 0.2497 0.6449 0.032 Uiso 1 1 calc R . . H91B H 0.7844 0.3297 0.6975 0.032 Uiso 1 1 calc R . . O9 O 0.7065(2) 0.3186(2) 0.6055(2) 0.0298(9) Uani 1 1 d . . . C92 C 0.6459(4) 0.3402(3) 0.6352(3) 0.0331(13) Uani 1 1 d . . . H92A H 0.6755 0.3817 0.6854 0.040 Uiso 1 1 calc R . . H92B H 0.6103 0.2996 0.6380 0.040 Uiso 1 1 calc R . . C93 C 0.5905(4) 0.3620(3) 0.5881(4) 0.0401(15) Uani 1 1 d . . . H93A H 0.5743 0.3269 0.5358 0.048 Uiso 1 1 calc R . . H93B H 0.5379 0.3611 0.5987 0.048 Uiso 1 1 calc R . . O10 O 0.6340(3) 0.4328(2) 0.6017(3) 0.0410(10) Uani 1 1 d . . . C94 C 0.5773(4) 0.4597(4) 0.5682(4) 0.0439(16) Uani 1 1 d . . . H94A H 0.5251 0.4515 0.5794 0.053 Uiso 1 1 calc R . . H94B H 0.5610 0.4334 0.5144 0.053 Uiso 1 1 calc R . . C95 C 0.6200(5) 0.5390(4) 0.5965(4) 0.0499(18) Uani 1 1 d . . . H95A H 0.5766 0.5621 0.5919 0.060 Uiso 1 1 calc R . . H95B H 0.6558 0.5621 0.6490 0.060 Uiso 1 1 calc R . . O11 O 0.6711(3) 0.5502(3) 0.5568(3) 0.0483(12) Uani 1 1 d . . . C96 C 0.7183(5) 0.6248(4) 0.5879(4) 0.0523(18) Uani 1 1 d . . . H96A H 0.7694 0.6388 0.6303 0.063 Uiso 1 1 calc R . . H96B H 0.6835 0.6540 0.6055 0.063 Uiso 1 1 calc R . . C97 C 0.7444(5) 0.6405(4) 0.5321(4) 0.0472(17) Uani 1 1 d . . . H97A H 0.7727 0.6068 0.5096 0.057 Uiso 1 1 calc R . . H97B H 0.6936 0.6329 0.4929 0.057 Uiso 1 1 calc R . . N6 N 0.8019(4) 0.7148(3) 0.5676(3) 0.0440(13) Uani 1 1 d . . . H6A H 0.8567 0.7225 0.5810 0.053 Uiso 1 1 calc R . . C98 C 0.7778(4) 0.7721(4) 0.5813(3) 0.0394(15) Uani 1 1 d . . . O12 O 0.7032(3) 0.7685(3) 0.5634(3) 0.0545(13) Uani 1 1 d . . . C99 C 0.8491(4) 0.8440(4) 0.6200(3) 0.0380(14) Uani 1 1 d . . . N7 N 0.9274(3) 0.8438(3) 0.6428(3) 0.0339(11) Uani 1 1 d . . . C100 C 0.9926(4) 0.9065(3) 0.6778(3) 0.0368(14) Uani 1 1 d . . . C101 C 0.9825(5) 0.9726(4) 0.6905(4) 0.0491(18) Uani 1 1 d . . . H101 H 1.0302 1.0162 0.7141 0.059 Uiso 1 1 calc R . . C102 C 0.9011(5) 0.9727(4) 0.6677(5) 0.061(2) Uani 1 1 d . . . H102 H 0.8918 1.0171 0.6767 0.073 Uiso 1 1 calc R . . C103 C 0.8321(5) 0.9074(4) 0.6313(4) 0.0476(17) Uani 1 1 d . . . H103 H 0.7756 0.9064 0.6148 0.057 Uiso 1 1 calc R . . C104 C 1.0808(4) 0.9036(4) 0.7029(4) 0.0385(14) Uani 1 1 d . . . O13 O 1.1431(3) 0.9586(3) 0.7313(3) 0.0546(13) Uani 1 1 d . . . N8 N 1.0825(3) 0.8377(3) 0.6895(3) 0.0387(12) Uani 1 1 d . . . H8A H 1.0343 0.8018 0.6718 0.046 Uiso 1 1 calc R . . C105 C 1.1618(5) 0.8230(4) 0.7031(4) 0.0513(18) Uani 1 1 d . . . H10A H 1.2033 0.8553 0.6949 0.062 Uiso 1 1 calc R . . H10B H 1.1510 0.7723 0.6674 0.062 Uiso 1 1 calc R . . C106 C 1.2003(4) 0.8339(4) 0.7795(5) 0.057(2) Uani 1 1 d . . . H10C H 1.2585 0.8324 0.7885 0.068 Uiso 1 1 calc R . . H10D H 1.2037 0.8820 0.8159 0.068 Uiso 1 1 calc R . . O14 O 1.1491(3) 0.7781(3) 0.7869(3) 0.0517(13) Uani 1 1 d . . . C107 C 1.1819(5) 0.7873(4) 0.8590(5) 0.0559(19) Uani 1 1 d . . . H10E H 1.1350 0.7626 0.8689 0.067 Uiso 1 1 calc R . . H10F H 1.2028 0.8398 0.8945 0.067 Uiso 1 1 calc R . . C108 C 1.2520(5) 0.7586(4) 0.8715(5) 0.057(2) Uani 1 1 d . . . H10G H 1.2958 0.7773 0.8550 0.068 Uiso 1 1 calc R . . H10H H 1.2789 0.7752 0.9244 0.068 Uiso 1 1 calc R . . O15 O 1.2195(3) 0.6815(2) 0.8322(3) 0.0469(12) Uani 1 1 d . . . C109 C 1.2849(4) 0.6517(4) 0.8411(5) 0.0514(19) Uani 1 1 d . . . H10I H 1.3211 0.6753 0.8935 0.062 Uiso 1 1 calc R . . H10J H 1.3210 0.6609 0.8142 0.062 Uiso 1 1 calc R . . C110 C 1.2458(4) 0.5713(4) 0.8121(4) 0.0413(15) Uani 1 1 d . . . H11A H 1.2027 0.5487 0.7622 0.050 Uiso 1 1 calc R . . H11B H 1.2900 0.5488 0.8098 0.050 Uiso 1 1 calc R . . O16 O 1.2073(3) 0.5603(2) 0.8602(2) 0.0336(9) Uani 1 1 d . . . C111 C 1.1764(4) 0.4855(3) 0.8409(3) 0.0300(12) Uani 1 1 d . . . H11C H 1.2232 0.4659 0.8424 0.036 Uiso 1 1 calc R . . H11D H 1.1325 0.4569 0.7909 0.036 Uiso 1 1 calc R . . C112 C 1.1391(4) 0.4812(3) 0.8960(3) 0.0286(12) Uani 1 1 d . . . H11E H 1.0957 0.5047 0.8960 0.034 Uiso 1 1 calc R . . H11F H 1.1846 0.5096 0.9452 0.034 Uiso 1 1 calc R . . C113 C 0.9629(3) 0.3928(3) 0.7543(3) 0.0222(11) Uani 1 1 d . . . C114 C 0.9554(3) 0.4401(3) 0.7393(3) 0.0266(12) Uani 1 1 d . . . C115 C 0.9501(3) 0.4940(3) 0.7163(3) 0.0253(11) Uani 1 1 d . . . C116 C 1.0220(3) 0.5558(3) 0.7443(3) 0.0283(12) Uani 1 1 d . . . H116 H 1.0716 0.5640 0.7818 0.034 Uiso 1 1 calc R . . C117 C 1.0217(4) 0.6043(3) 0.7183(3) 0.0318(13) Uani 1 1 d . . . H117 H 1.0705 0.6462 0.7380 0.038 Uiso 1 1 calc R . . C118 C 0.9487(4) 0.5918(3) 0.6625(3) 0.0340(13) Uani 1 1 d . . . C119 C 0.8758(4) 0.5325(3) 0.6358(4) 0.0431(16) Uani 1 1 d . . . H119 H 0.8259 0.5256 0.5995 0.052 Uiso 1 1 calc R . . C120 C 0.8761(4) 0.4834(3) 0.6623(3) 0.0370(14) Uani 1 1 d . . . H120 H 0.8263 0.4426 0.6441 0.044 Uiso 1 1 calc R . . C121 C 0.9531(4) 0.6409(3) 0.6325(3) 0.0379(14) Uani 1 1 d . . . N9 N 0.9584(4) 0.6796(3) 0.6083(3) 0.0528(16) Uani 1 1 d . . . C122 C 1.0010(4) 0.2341(3) 0.7933(3) 0.0296(12) Uani 1 1 d . . . C123 C 1.0256(4) 0.1941(3) 0.8129(3) 0.0370(14) Uani 1 1 d . . . C124 C 1.0625(4) 0.1540(3) 0.8432(4) 0.0394(15) Uani 1 1 d . . . C125 C 1.0173(6) 0.1119(5) 0.8658(6) 0.079(3) Uani 1 1 d . . . H125 H 0.9610 0.1097 0.8623 0.095 Uiso 1 1 calc R . . C126 C 1.0540(7) 0.0730(6) 0.8937(7) 0.101(4) Uani 1 1 d . . . H126 H 1.0228 0.0450 0.9101 0.121 Uiso 1 1 calc R . . C127 C 1.1354(6) 0.0737(5) 0.8983(5) 0.069(3) Uani 1 1 d . . . C128 C 1.1805(5) 0.1150(4) 0.8754(5) 0.066(2) Uani 1 1 d . . . H128 H 1.2358 0.1153 0.8769 0.079 Uiso 1 1 calc R . . C129 C 1.1445(4) 0.1563(4) 0.8500(4) 0.0499(18) Uani 1 1 d . . . H129 H 1.1772 0.1870 0.8370 0.060 Uiso 1 1 calc R . . C130 C 1.1702(8) 0.0305(7) 0.9226(7) 0.099(4) Uani 1 1 d . . . N10 N 1.1922(8) -0.0087(7) 0.9387(7) 0.139(5) Uani 1 1 d . . . C131 C 0.5070(7) 0.8229(6) 0.8342(6) 0.095(3) Uani 1 1 d . . . H131 H 0.5391 0.7958 0.8076 0.114 Uiso 1 1 calc R . . Cl1 Cl 0.4995(2) 0.7968(3) 0.8978(3) 0.159(2) Uani 1 1 d . . . Cl2 Cl 0.4101(2) 0.7995(3) 0.77071(18) 0.1469(17) Uani 1 1 d . . . Cl3 Cl 0.5651(3) 0.91316(19) 0.8751(3) 0.182(2) Uani 1 1 d . . . C132 C 0.7729(7) 0.0723(7) 0.8949(7) 0.103(4) Uani 1 1 d . . . H132 H 0.7342 0.0401 0.8426 0.124 Uiso 1 1 calc R . . Cl4 Cl 0.7129(3) 0.0752(3) 0.9468(3) 0.1620(17) Uani 1 1 d . . . Cl5 Cl 0.8493(3) 0.0339(3) 0.9133(4) 0.187(2) Uani 1 1 d . . . Cl6 Cl 0.8213(4) 0.1547(2) 0.9034(3) 0.178(2) Uani 1 1 d . . . C133 C 0.9975(7) 0.8450(6) 0.8709(9) 0.198(2) Uani 1 1 d D . . H133 H 1.0574 0.8694 0.8783 0.254 Uiso 1 1 calc R . . Cl7 Cl 0.9372(6) 0.7997(7) 0.7829(4) 0.198(2) Uani 1 1 d D . . Cl8 Cl 0.9935(3) 0.7902(4) 0.9079(4) 0.198(2) Uani 1 1 d D . . Cl9 Cl 0.9581(3) 0.9097(3) 0.9281(3) 0.198(2) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02137(10) 0.01583(9) 0.01879(10) 0.00802(8) 0.00660(8) 0.00508(7) P1 0.0209(6) 0.0181(6) 0.0189(6) 0.0089(5) 0.0065(5) 0.0060(5) C1 0.023(2) 0.022(2) 0.030(3) 0.012(2) 0.013(2) 0.009(2) C2 0.048(4) 0.051(4) 0.039(4) 0.029(3) 0.023(3) 0.033(3) C3 0.067(5) 0.069(5) 0.056(5) 0.036(4) 0.041(4) 0.049(4) C4 0.049(4) 0.060(5) 0.080(6) 0.034(5) 0.031(4) 0.036(4) C5 0.038(4) 0.056(5) 0.052(5) 0.016(4) 0.001(3) 0.028(3) C6 0.028(3) 0.031(3) 0.031(3) 0.009(3) 0.003(3) 0.011(2) C7 0.019(2) 0.033(3) 0.017(2) 0.011(2) 0.006(2) 0.011(2) C8 0.029(3) 0.037(3) 0.026(3) 0.016(3) 0.006(2) 0.008(2) C9 0.033(3) 0.068(5) 0.034(4) 0.033(4) 0.010(3) 0.007(3) C10 0.036(3) 0.080(5) 0.026(3) 0.028(4) 0.016(3) 0.023(4) C11 0.046(4) 0.068(5) 0.027(3) 0.018(3) 0.022(3) 0.035(4) C12 0.040(3) 0.041(3) 0.029(3) 0.017(3) 0.015(3) 0.021(3) P2 0.0215(6) 0.0164(6) 0.0199(6) 0.0059(5) 0.0062(5) 0.0057(5) C13 0.023(3) 0.014(2) 0.033(3) 0.004(2) 0.008(2) 0.003(2) C14 0.031(3) 0.033(3) 0.041(4) 0.020(3) 0.009(3) 0.006(3) C15 0.032(3) 0.043(4) 0.068(5) 0.034(4) 0.019(3) 0.008(3) C16 0.034(3) 0.025(3) 0.088(6) 0.022(4) 0.019(4) 0.004(3) C17 0.031(3) 0.024(3) 0.067(5) -0.006(3) 0.016(3) 0.003(3) C18 0.027(3) 0.030(3) 0.041(4) -0.002(3) 0.010(3) 0.004(3) C19 0.020(2) 0.025(3) 0.021(3) 0.004(2) 0.006(2) 0.005(2) C20 0.034(3) 0.034(3) 0.034(3) 0.015(3) 0.013(3) 0.016(3) C21 0.040(3) 0.042(4) 0.044(4) 0.014(3) 0.017(3) 0.023(3) C22 0.039(4) 0.049(4) 0.040(4) 0.005(3) 0.024(3) 0.017(3) C23 0.035(3) 0.048(4) 0.027(3) 0.011(3) 0.016(3) 0.011(3) C24 0.028(3) 0.030(3) 0.022(3) 0.006(2) 0.006(2) 0.009(2) C25 0.025(3) 0.018(2) 0.024(3) 0.010(2) 0.006(2) 0.004(2) C26 0.024(3) 0.024(3) 0.029(3) 0.013(2) 0.007(2) 0.004(2) O1 0.034(2) 0.0244(19) 0.031(2) 0.0163(17) 0.0062(18) 0.0006(17) C27 0.030(3) 0.044(4) 0.047(4) 0.029(3) 0.014(3) 0.007(3) C28 0.029(3) 0.055(4) 0.083(6) 0.051(4) 0.014(3) 0.006(3) O2 0.036(2) 0.038(3) 0.067(3) 0.031(2) 0.007(2) 0.003(2) C29 0.057(5) 0.043(4) 0.076(6) 0.031(4) -0.004(4) 0.003(4) C30 0.068(5) 0.048(4) 0.058(5) 0.022(4) 0.011(4) 0.017(4) O3 0.060(3) 0.044(3) 0.065(3) 0.032(3) 0.021(3) 0.016(2) C31 0.064(5) 0.053(5) 0.078(6) 0.033(5) 0.016(5) 0.004(4) C32 0.070(5) 0.052(5) 0.070(6) 0.034(4) 0.033(5) 0.016(4) N1 0.062(4) 0.037(3) 0.056(4) 0.025(3) 0.028(3) 0.013(3) C33 0.081(6) 0.046(4) 0.045(4) 0.025(4) 0.031(4) 0.016(4) O4 0.099(5) 0.047(3) 0.076(4) 0.034(3) 0.028(4) 0.000(3) C34 0.099(6) 0.031(3) 0.044(4) 0.021(3) 0.042(4) 0.024(4) N2 0.076(4) 0.042(3) 0.036(3) 0.025(3) 0.026(3) 0.027(3) C35 0.090(6) 0.051(4) 0.038(4) 0.031(4) 0.036(4) 0.041(4) C36 0.128(9) 0.077(6) 0.062(5) 0.049(5) 0.061(6) 0.068(7) C37 0.138(10) 0.048(5) 0.075(6) 0.038(5) 0.062(7) 0.048(6) C38 0.108(8) 0.044(4) 0.064(5) 0.028(4) 0.048(6) 0.032(5) C39 0.076(5) 0.079(6) 0.030(4) 0.038(4) 0.025(4) 0.048(5) O5 0.079(4) 0.104(5) 0.053(3) 0.048(3) 0.024(3) 0.057(4) N3 0.058(4) 0.057(4) 0.045(3) 0.031(3) 0.016(3) 0.024(3) C40 0.055(4) 0.060(5) 0.043(4) 0.027(4) 0.015(4) 0.020(4) C41 0.070(5) 0.053(5) 0.053(5) 0.026(4) 0.031(4) 0.029(4) O6 0.060(3) 0.062(3) 0.049(3) 0.029(3) 0.031(3) 0.033(3) C42 0.071(5) 0.066(5) 0.062(5) 0.041(4) 0.037(4) 0.041(4) C43 0.049(4) 0.065(5) 0.048(4) 0.034(4) 0.019(3) 0.036(4) O57 0.042(2) 0.043(3) 0.052(3) 0.026(2) 0.015(2) 0.023(2) C44 0.034(3) 0.050(4) 0.053(4) 0.027(3) 0.016(3) 0.019(3) C45 0.032(3) 0.038(3) 0.035(3) 0.019(3) 0.016(3) 0.019(3) O8 0.0257(19) 0.034(2) 0.030(2) 0.0146(18) 0.0103(17) 0.0150(17) C46 0.023(3) 0.030(3) 0.026(3) 0.013(2) 0.004(2) 0.011(2) C47 0.024(2) 0.023(2) 0.020(3) 0.008(2) 0.006(2) 0.011(2) C48 0.021(2) 0.020(2) 0.020(2) 0.007(2) 0.007(2) 0.005(2) C49 0.023(2) 0.022(3) 0.020(3) 0.009(2) 0.004(2) 0.004(2) C50 0.025(3) 0.023(3) 0.023(3) 0.011(2) 0.005(2) 0.008(2) C51 0.025(3) 0.026(3) 0.026(3) 0.011(2) 0.006(2) 0.010(2) C52 0.031(3) 0.024(3) 0.033(3) 0.012(2) 0.010(3) 0.005(2) C53 0.038(3) 0.026(3) 0.036(3) 0.017(3) 0.010(3) 0.014(3) C54 0.038(3) 0.033(3) 0.042(4) 0.022(3) -0.001(3) 0.012(3) C55 0.030(3) 0.024(3) 0.038(3) 0.015(3) 0.000(3) 0.002(2) C56 0.041(3) 0.029(3) 0.039(3) 0.017(3) 0.008(3) 0.011(3) N4 0.061(4) 0.040(3) 0.064(4) 0.033(3) 0.013(3) 0.018(3) C57 0.029(3) 0.022(3) 0.022(3) 0.009(2) 0.005(2) 0.006(2) C58 0.035(3) 0.028(3) 0.031(3) 0.016(3) 0.008(3) 0.007(2) C59 0.042(3) 0.031(3) 0.034(3) 0.019(3) 0.005(3) 0.007(3) C60 0.045(4) 0.061(5) 0.065(5) 0.048(4) -0.005(4) -0.001(4) C61 0.052(4) 0.060(5) 0.069(5) 0.048(4) -0.006(4) 0.003(4) C62 0.057(4) 0.040(4) 0.049(4) 0.033(3) 0.007(3) 0.006(3) C63 0.038(4) 0.046(4) 0.073(5) 0.039(4) 0.004(4) 0.005(3) C64 0.044(4) 0.047(4) 0.056(4) 0.040(4) 0.006(3) 0.009(3) C65 0.051(4) 0.056(4) 0.048(4) 0.036(4) -0.001(3) -0.002(3) N5 0.068(4) 0.067(4) 0.070(5) 0.053(4) 0.007(4) 0.006(4) Pt2 0.02309(10) 0.01854(10) 0.01851(11) 0.00664(8) 0.00408(8) 0.00771(8) P3 0.0208(6) 0.0189(6) 0.0189(6) 0.0056(5) 0.0045(5) 0.0071(5) C66 0.022(3) 0.017(2) 0.035(3) 0.004(2) 0.011(2) 0.005(2) C67 0.028(3) 0.030(3) 0.036(3) 0.000(3) 0.011(3) 0.005(2) C68 0.029(3) 0.025(3) 0.053(4) -0.004(3) 0.011(3) 0.001(3) C69 0.035(4) 0.024(3) 0.091(6) 0.019(4) 0.027(4) 0.008(3) C70 0.045(4) 0.038(4) 0.077(5) 0.035(4) 0.033(4) 0.016(3) C71 0.029(3) 0.027(3) 0.044(4) 0.012(3) 0.013(3) 0.008(2) C72 0.017(2) 0.021(2) 0.026(3) 0.004(2) 0.007(2) 0.007(2) C73 0.029(3) 0.033(3) 0.028(3) 0.009(2) 0.010(2) 0.016(2) C74 0.029(3) 0.044(4) 0.045(4) 0.018(3) 0.008(3) 0.018(3) C75 0.026(3) 0.047(4) 0.033(3) 0.005(3) 0.013(3) 0.007(3) C76 0.033(3) 0.049(4) 0.029(3) 0.014(3) 0.015(3) 0.014(3) C77 0.031(3) 0.032(3) 0.029(3) 0.012(3) 0.008(3) 0.012(2) P4 0.0219(6) 0.0195(6) 0.0181(6) 0.0073(5) 0.0049(5) 0.0090(5) C78 0.020(2) 0.022(2) 0.027(3) 0.010(2) 0.007(2) 0.008(2) C79 0.022(3) 0.025(3) 0.023(3) 0.005(2) 0.005(2) 0.005(2) C80 0.022(3) 0.042(4) 0.044(4) 0.020(3) 0.002(3) 0.011(3) C81 0.026(3) 0.050(4) 0.062(5) 0.031(4) 0.021(3) 0.019(3) C82 0.050(4) 0.047(4) 0.053(4) 0.030(3) 0.035(4) 0.029(3) C83 0.040(3) 0.037(3) 0.037(3) 0.021(3) 0.019(3) 0.022(3) C84 0.023(2) 0.036(3) 0.019(3) 0.011(2) 0.007(2) 0.015(2) C85 0.030(3) 0.037(3) 0.033(3) 0.014(3) 0.013(3) 0.010(3) C86 0.036(3) 0.071(5) 0.049(4) 0.040(4) 0.023(3) 0.019(3) C87 0.039(4) 0.075(5) 0.030(3) 0.023(4) 0.016(3) 0.031(4) C88 0.047(4) 0.056(4) 0.025(3) 0.012(3) 0.014(3) 0.030(3) C89 0.041(3) 0.046(4) 0.025(3) 0.014(3) 0.011(3) 0.023(3) C90 0.023(3) 0.029(3) 0.020(3) 0.009(2) 0.003(2) 0.010(2) C91 0.026(3) 0.027(3) 0.024(3) 0.010(2) 0.007(2) 0.011(2) O9 0.0260(19) 0.036(2) 0.033(2) 0.0186(18) 0.0109(17) 0.0164(17) C92 0.032(3) 0.036(3) 0.041(3) 0.021(3) 0.020(3) 0.018(3) C93 0.032(3) 0.040(3) 0.054(4) 0.026(3) 0.016(3) 0.015(3) O10 0.038(2) 0.036(2) 0.055(3) 0.026(2) 0.016(2) 0.018(2) C94 0.042(4) 0.054(4) 0.048(4) 0.033(4) 0.016(3) 0.022(3) C95 0.058(4) 0.058(5) 0.062(5) 0.040(4) 0.035(4) 0.035(4) O11 0.061(3) 0.045(3) 0.048(3) 0.024(2) 0.029(3) 0.022(2) C96 0.069(5) 0.045(4) 0.046(4) 0.022(3) 0.025(4) 0.019(4) C97 0.049(4) 0.040(4) 0.044(4) 0.021(3) 0.010(3) 0.007(3) N6 0.043(3) 0.042(3) 0.040(3) 0.021(3) 0.007(3) 0.008(3) C98 0.043(4) 0.050(4) 0.035(3) 0.029(3) 0.013(3) 0.019(3) O12 0.042(3) 0.074(4) 0.052(3) 0.040(3) 0.010(2) 0.018(3) C99 0.049(4) 0.040(3) 0.035(3) 0.024(3) 0.017(3) 0.020(3) N7 0.038(3) 0.036(3) 0.030(3) 0.018(2) 0.011(2) 0.013(2) C100 0.048(4) 0.033(3) 0.036(3) 0.019(3) 0.019(3) 0.018(3) C101 0.061(5) 0.032(3) 0.056(4) 0.020(3) 0.023(4) 0.019(3) C102 0.072(5) 0.042(4) 0.086(6) 0.035(4) 0.035(5) 0.036(4) C103 0.048(4) 0.051(4) 0.057(4) 0.031(4) 0.021(4) 0.028(4) C104 0.042(3) 0.041(4) 0.038(4) 0.023(3) 0.017(3) 0.014(3) O13 0.045(3) 0.037(3) 0.077(4) 0.029(3) 0.018(3) 0.008(2) N8 0.039(3) 0.033(3) 0.047(3) 0.022(3) 0.015(3) 0.014(2) C105 0.048(4) 0.050(4) 0.073(5) 0.038(4) 0.026(4) 0.025(4) C106 0.038(4) 0.048(4) 0.090(6) 0.047(4) 0.013(4) 0.008(3) O14 0.043(3) 0.044(3) 0.073(4) 0.040(3) 0.010(3) 0.013(2) C107 0.056(5) 0.047(4) 0.069(5) 0.032(4) 0.020(4) 0.020(4) C108 0.051(4) 0.039(4) 0.073(5) 0.035(4) 0.003(4) 0.009(3) O15 0.035(2) 0.036(2) 0.064(3) 0.031(2) 0.003(2) 0.007(2) C109 0.029(3) 0.055(4) 0.077(5) 0.047(4) 0.008(3) 0.008(3) C110 0.030(3) 0.049(4) 0.054(4) 0.034(3) 0.014(3) 0.013(3) O16 0.035(2) 0.025(2) 0.036(2) 0.0161(18) 0.0061(18) 0.0059(17) C111 0.026(3) 0.024(3) 0.033(3) 0.012(2) 0.007(2) 0.007(2) C112 0.031(3) 0.021(3) 0.026(3) 0.008(2) 0.003(2) 0.008(2) C113 0.020(2) 0.019(2) 0.016(2) 0.002(2) 0.002(2) 0.005(2) C114 0.025(3) 0.025(3) 0.021(3) 0.006(2) 0.004(2) 0.006(2) C115 0.029(3) 0.020(2) 0.020(3) 0.006(2) 0.004(2) 0.008(2) C116 0.027(3) 0.030(3) 0.025(3) 0.011(2) 0.008(2) 0.012(2) C117 0.033(3) 0.027(3) 0.032(3) 0.013(2) 0.007(3) 0.010(2) C118 0.042(3) 0.028(3) 0.033(3) 0.015(3) 0.011(3) 0.017(3) C119 0.037(3) 0.036(3) 0.044(4) 0.021(3) -0.006(3) 0.009(3) C120 0.035(3) 0.025(3) 0.040(3) 0.015(3) -0.001(3) 0.007(2) C121 0.040(3) 0.032(3) 0.036(3) 0.014(3) 0.009(3) 0.014(3) N9 0.063(4) 0.039(3) 0.055(4) 0.029(3) 0.010(3) 0.015(3) C122 0.030(3) 0.024(3) 0.022(3) 0.008(2) -0.001(2) 0.004(2) C123 0.043(3) 0.025(3) 0.034(3) 0.009(3) 0.009(3) 0.013(3) C124 0.050(4) 0.034(3) 0.039(4) 0.020(3) 0.016(3) 0.020(3) C125 0.085(6) 0.110(8) 0.129(9) 0.102(7) 0.069(7) 0.067(6) C126 0.121(9) 0.131(10) 0.166(11) 0.130(10) 0.099(9) 0.084(8) C127 0.101(7) 0.075(6) 0.090(7) 0.065(6) 0.059(6) 0.061(6) C128 0.061(5) 0.057(5) 0.091(7) 0.043(5) 0.024(5) 0.033(4) C129 0.044(4) 0.043(4) 0.069(5) 0.032(4) 0.018(4) 0.020(3) C130 0.134(10) 0.135(10) 0.128(10) 0.109(9) 0.078(8) 0.106(9) N10 0.166(11) 0.200(12) 0.193(12) 0.158(11) 0.110(10) 0.143(10) C131 0.099(8) 0.087(8) 0.093(8) 0.053(7) 0.017(7) 0.025(6) Cl1 0.104(2) 0.280(6) 0.223(5) 0.217(5) 0.082(3) 0.085(3) Cl2 0.116(3) 0.275(5) 0.083(2) 0.091(3) 0.053(2) 0.100(3) Cl3 0.200(4) 0.081(2) 0.241(5) 0.024(3) 0.162(4) 0.019(3) C132 0.078(7) 0.112(9) 0.123(10) 0.055(8) 0.051(7) 0.025(7) Cl4 0.144(4) 0.185(4) 0.155(4) 0.078(3) 0.079(3) 0.035(3) Cl5 0.120(3) 0.171(4) 0.330(7) 0.167(5) 0.088(4) 0.059(3) Cl6 0.255(6) 0.106(3) 0.230(5) 0.107(3) 0.131(5) 0.066(3) C133 0.153(4) 0.166(4) 0.208(5) 0.071(4) 0.044(4) -0.002(3) Cl7 0.153(4) 0.166(4) 0.208(5) 0.071(4) 0.044(4) -0.002(3) Cl8 0.153(4) 0.166(4) 0.208(5) 0.071(4) 0.044(4) -0.002(3) Cl9 0.153(4) 0.166(4) 0.208(5) 0.071(4) 0.044(4) -0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C57 1.990(5) . ? Pt1 C48 1.996(5) . ? Pt1 P1 2.3042(13) . ? Pt1 P2 2.3050(13) . ? P1 C7 1.812(5) . ? P1 C1 1.814(5) . ? P1 C25 1.826(5) . ? C1 C6 1.388(8) . ? C1 C2 1.390(8) . ? C2 C3 1.390(9) . ? C2 H2 0.9500 . ? C3 C4 1.373(11) . ? C3 H3 0.9500 . ? C4 C5 1.379(11) . ? C4 H4 0.9500 . ? C5 C6 1.388(9) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.390(8) . ? C7 C8 1.392(8) . ? C8 C9 1.409(8) . ? C8 H8 0.9500 . ? C9 C10 1.342(10) . ? C9 H9 0.9500 . ? C10 C11 1.373(10) . ? C10 H10 0.9500 . ? C11 C12 1.395(8) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? P2 C13 1.823(5) . ? P2 C19 1.825(5) . ? P2 C47 1.831(5) . ? C13 C14 1.384(8) . ? C13 C18 1.396(8) . ? C14 C15 1.389(8) . ? C14 H14 0.9500 . ? C15 C16 1.369(11) . ? C15 H15 0.9500 . ? C16 C17 1.343(11) . ? C16 H16 0.9500 . ? C17 C18 1.402(9) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.395(8) . ? C19 C20 1.395(8) . ? C20 C21 1.371(9) . ? C20 H20 0.9500 . ? C21 C22 1.396(10) . ? C21 H21 0.9500 . ? C22 C23 1.370(10) . ? C22 H22 0.9500 . ? C23 C24 1.391(9) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.517(7) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O1 1.415(6) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? O1 C27 1.423(7) . ? C27 C28 1.499(9) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 O2 1.421(8) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? O2 C29 1.411(9) . ? C29 C30 1.497(11) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 O3 1.428(9) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? O3 C31 1.401(9) . ? C31 C32 1.505(11) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 N1 1.469(10) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? N1 C33 1.336(9) . ? N1 H1 0.8800 . ? C33 O4 1.232(9) . ? C33 C34 1.490(12) . ? C34 N2 1.337(10) . ? C34 C38 1.395(10) . ? N2 C35 1.315(10) . ? C35 C36 1.424(10) . ? C35 C39 1.517(12) . ? C36 C37 1.404(14) . ? C36 H36 0.9500 . ? C37 C38 1.357(14) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 O5 1.213(9) . ? C39 N3 1.337(9) . ? N3 C40 1.447(9) . ? N3 H3A 0.8800 . ? C40 C41 1.504(10) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 O6 1.407(9) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? O6 C42 1.431(9) . ? C42 C43 1.495(11) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 O57 1.426(7) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? O57 C44 1.424(8) . ? C44 C45 1.498(8) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 O8 1.418(7) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? O8 C46 1.413(6) . ? C46 C47 1.519(8) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.204(7) . ? C49 C50 1.433(7) . ? C50 C55 1.405(7) . ? C50 C51 1.406(7) . ? C51 C52 1.374(8) . ? C51 H51 0.9500 . ? C52 C53 1.399(8) . ? C52 H52 0.9500 . ? C53 C54 1.381(9) . ? C53 C56 1.444(8) . ? C54 C55 1.385(8) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? C56 N4 1.139(8) . ? C57 C58 1.217(7) . ? C58 C59 1.428(8) . ? C59 C60 1.380(9) . ? C59 C64 1.395(9) . ? C60 C61 1.371(9) . ? C60 H60 0.9500 . ? C61 C62 1.399(10) . ? C61 H61 0.9500 . ? C62 C63 1.328(9) . ? C62 C65 1.444(9) . ? C63 C64 1.396(9) . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? C65 N5 1.143(8) . ? Pt2 C122 1.979(6) . ? Pt2 C113 1.988(5) . ? Pt2 P4 2.3028(13) . ? Pt2 P3 2.3056(13) . ? P3 C72 1.823(5) . ? P3 C66 1.826(5) . ? P3 C90 1.829(5) . ? C66 C71 1.380(8) . ? C66 C67 1.396(8) . ? C67 C68 1.396(9) . ? C67 H67 0.9500 . ? C68 C69 1.338(11) . ? C68 H68 0.9500 . ? C69 C70 1.378(11) . ? C69 H69 0.9500 . ? C70 C71 1.389(8) . ? C70 H70 0.9500 . ? C71 H71 0.9500 . ? C72 C77 1.396(8) . ? C72 C73 1.401(8) . ? C73 C74 1.380(9) . ? C73 H73 0.9500 . ? C74 C75 1.390(9) . ? C74 H74 0.9500 . ? C75 C76 1.373(9) . ? C75 H75 0.9500 . ? C76 C77 1.377(9) . ? C76 H76 0.9500 . ? C77 H77 0.9500 . ? P4 C78 1.819(5) . ? P4 C84 1.824(5) . ? P4 C112 1.824(5) . ? C78 C79 1.385(7) . ? C78 C83 1.401(8) . ? C79 C80 1.390(8) . ? C79 H79 0.9500 . ? C80 C81 1.383(10) . ? C80 H80 0.9500 . ? C81 C82 1.370(9) . ? C81 H81 0.9500 . ? C82 C83 1.397(9) . ? C82 H82 0.9500 . ? C83 H83 0.9500 . ? C84 C89 1.392(8) . ? C84 C85 1.392(8) . ? C85 C86 1.414(9) . ? C85 H85 0.9500 . ? C86 C87 1.353(10) . ? C86 H86 0.9500 . ? C87 C88 1.372(10) . ? C87 H87 0.9500 . ? C88 C89 1.394(9) . ? C88 H88 0.9500 . ? C89 H89 0.9500 . ? C90 C91 1.517(8) . ? C90 H90A 0.9900 . ? C90 H90B 0.9900 . ? C91 O9 1.419(6) . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? O9 C92 1.422(7) . ? C92 C93 1.504(8) . ? C92 H92A 0.9900 . ? C92 H92B 0.9900 . ? C93 O10 1.419(7) . ? C93 H93A 0.9900 . ? C93 H93B 0.9900 . ? O10 C94 1.430(7) . ? C94 C95 1.493(10) . ? C94 H94A 0.9900 . ? C94 H94B 0.9900 . ? C95 O11 1.420(8) . ? C95 H95A 0.9900 . ? C95 H95B 0.9900 . ? O11 C96 1.412(8) . ? C96 C97 1.509(10) . ? C96 H96A 0.9900 . ? C96 H96B 0.9900 . ? C97 N6 1.448(8) . ? C97 H97A 0.9900 . ? C97 H97B 0.9900 . ? N6 C98 1.326(9) . ? N6 H6A 0.8800 . ? C98 O12 1.232(8) . ? C98 C99 1.502(9) . ? C99 N7 1.328(8) . ? C99 C103 1.390(9) . ? N7 C100 1.335(8) . ? C100 C101 1.390(9) . ? C100 C104 1.515(9) . ? C101 C102 1.377(11) . ? C101 H101 0.9500 . ? C102 C103 1.399(11) . ? C102 H102 0.9500 . ? C103 H103 0.9500 . ? C104 O13 1.222(8) . ? C104 N8 1.332(8) . ? N8 C105 1.461(8) . ? N8 H8A 0.8800 . ? C105 C106 1.509(11) . ? C105 H10A 0.9900 . ? C105 H10B 0.9900 . ? C106 O14 1.423(8) . ? C106 H10C 0.9900 . ? C106 H10D 0.9900 . ? O14 C107 1.426(9) . ? C107 C108 1.491(10) . ? C107 H10E 0.9900 . ? C107 H10F 0.9900 . ? C108 O15 1.418(8) . ? C108 H10G 0.9900 . ? C108 H10H 0.9900 . ? O15 C109 1.423(8) . ? C109 C110 1.503(9) . ? C109 H10I 0.9900 . ? C109 H10J 0.9900 . ? C110 O16 1.426(7) . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? O16 C111 1.426(6) . ? C111 C112 1.503(8) . ? C111 H11C 0.9900 . ? C111 H11D 0.9900 . ? C112 H11E 0.9900 . ? C112 H11F 0.9900 . ? C113 C114 1.204(7) . ? C114 C115 1.440(8) . ? C115 C116 1.404(8) . ? C115 C120 1.407(8) . ? C116 C117 1.365(8) . ? C116 H116 0.9500 . ? C117 C118 1.403(8) . ? C117 H117 0.9500 . ? C118 C119 1.387(9) . ? C118 C121 1.438(8) . ? C119 C120 1.388(8) . ? C119 H119 0.9500 . ? C120 H120 0.9500 . ? C121 N9 1.144(8) . ? C122 C123 1.208(8) . ? C123 C124 1.433(8) . ? C124 C129 1.380(9) . ? C124 C125 1.383(10) . ? C125 C126 1.379(11) . ? C125 H125 0.9500 . ? C126 C127 1.387(13) . ? C126 H126 0.9500 . ? C127 C128 1.374(11) . ? C127 C130 1.401(11) . ? C128 C129 1.390(10) . ? C128 H128 0.9500 . ? C129 H129 0.9500 . ? C130 N10 1.134(11) . ? C131 Cl1 1.693(11) . ? C131 Cl2 1.705(11) . ? C131 Cl3 1.706(11) . ? C131 H131 1.0000 . ? C132 Cl4 1.691(11) . ? C132 Cl6 1.704(12) . ? C132 Cl5 1.750(12) . ? C132 H132 1.0000 . ? C133 Cl7 1.654(15) . ? C133 Cl8 1.663(12) . ? C133 Cl9 1.827(12) . ? C133 H133 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C57 Pt1 C48 176.0(2) . . ? C57 Pt1 P1 88.74(15) . . ? C48 Pt1 P1 91.72(14) . . ? C57 Pt1 P2 91.82(15) . . ? C48 Pt1 P2 88.52(14) . . ? P1 Pt1 P2 168.40(5) . . ? C7 P1 C1 105.0(2) . . ? C7 P1 C25 102.8(2) . . ? C1 P1 C25 102.7(2) . . ? C7 P1 Pt1 117.46(17) . . ? C1 P1 Pt1 110.83(18) . . ? C25 P1 Pt1 116.43(17) . . ? C6 C1 C2 119.6(5) . . ? C6 C1 P1 122.2(4) . . ? C2 C1 P1 117.9(4) . . ? C3 C2 C1 120.4(6) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C4 C3 C2 119.4(7) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 120.7(7) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C4 C5 C6 120.2(7) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C1 119.6(6) . . ? C5 C6 H6 120.2 . . ? C1 C6 H6 120.2 . . ? C12 C7 C8 118.6(5) . . ? C12 C7 P1 122.8(4) . . ? C8 C7 P1 118.6(4) . . ? C7 C8 C9 119.3(6) . . ? C7 C8 H8 120.3 . . ? C9 C8 H8 120.3 . . ? C10 C9 C8 121.2(6) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C9 C10 C11 120.5(6) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C10 C11 C12 119.8(7) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C7 C12 C11 120.6(6) . . ? C7 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C13 P2 C19 103.9(2) . . ? C13 P2 C47 102.6(2) . . ? C19 P2 C47 105.5(2) . . ? C13 P2 Pt1 120.81(19) . . ? C19 P2 Pt1 105.44(17) . . ? C47 P2 Pt1 116.93(17) . . ? C14 C13 C18 119.1(5) . . ? C14 C13 P2 122.1(4) . . ? C18 C13 P2 118.8(5) . . ? C13 C14 C15 120.2(6) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C16 C15 C14 120.2(7) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C17 C16 C15 120.2(6) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 121.5(7) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? C13 C18 C17 118.7(7) . . ? C13 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? C24 C19 C20 119.1(5) . . ? C24 C19 P2 122.4(4) . . ? C20 C19 P2 118.5(4) . . ? C21 C20 C19 120.8(6) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C20 C21 C22 119.8(6) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C23 C22 C21 119.9(6) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 120.7(6) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C23 C24 C19 119.6(6) . . ? C23 C24 H24 120.2 . . ? C19 C24 H24 120.2 . . ? C26 C25 P1 115.7(4) . . ? C26 C25 H25A 108.4 . . ? P1 C25 H25A 108.4 . . ? C26 C25 H25B 108.4 . . ? P1 C25 H25B 108.4 . . ? H25A C25 H25B 107.4 . . ? O1 C26 C25 106.5(4) . . ? O1 C26 H26A 110.4 . . ? C25 C26 H26A 110.4 . . ? O1 C26 H26B 110.4 . . ? C25 C26 H26B 110.4 . . ? H26A C26 H26B 108.6 . . ? C26 O1 C27 112.8(4) . . ? O1 C27 C28 108.5(6) . . ? O1 C27 H27A 110.0 . . ? C28 C27 H27A 110.0 . . ? O1 C27 H27B 110.0 . . ? C28 C27 H27B 110.0 . . ? H27A C27 H27B 108.4 . . ? O2 C28 C27 111.0(5) . . ? O2 C28 H28A 109.4 . . ? C27 C28 H28A 109.4 . . ? O2 C28 H28B 109.4 . . ? C27 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? C29 O2 C28 112.8(5) . . ? O2 C29 C30 110.0(6) . . ? O2 C29 H29A 109.7 . . ? C30 C29 H29A 109.7 . . ? O2 C29 H29B 109.7 . . ? C30 C29 H29B 109.7 . . ? H29A C29 H29B 108.2 . . ? O3 C30 C29 114.6(7) . . ? O3 C30 H30A 108.6 . . ? C29 C30 H30A 108.6 . . ? O3 C30 H30B 108.6 . . ? C29 C30 H30B 108.6 . . ? H30A C30 H30B 107.6 . . ? C31 O3 C30 112.6(6) . . ? O3 C31 C32 110.1(7) . . ? O3 C31 H31A 109.6 . . ? C32 C31 H31A 109.6 . . ? O3 C31 H31B 109.6 . . ? C32 C31 H31B 109.6 . . ? H31A C31 H31B 108.2 . . ? N1 C32 C31 115.8(7) . . ? N1 C32 H32A 108.3 . . ? C31 C32 H32A 108.3 . . ? N1 C32 H32B 108.3 . . ? C31 C32 H32B 108.3 . . ? H32A C32 H32B 107.4 . . ? C33 N1 C32 123.0(7) . . ? C33 N1 H1 118.5 . . ? C32 N1 H1 118.5 . . ? O4 C33 N1 123.7(9) . . ? O4 C33 C34 120.5(7) . . ? N1 C33 C34 115.8(7) . . ? N2 C34 C38 122.5(9) . . ? N2 C34 C33 117.6(6) . . ? C38 C34 C33 119.9(8) . . ? C35 N2 C34 119.2(7) . . ? N2 C35 C36 123.3(8) . . ? N2 C35 C39 118.1(6) . . ? C36 C35 C39 118.6(8) . . ? C37 C36 C35 115.2(9) . . ? C37 C36 H36 122.4 . . ? C35 C36 H36 122.4 . . ? C38 C37 C36 121.8(8) . . ? C38 C37 H37 119.1 . . ? C36 C37 H37 119.1 . . ? C37 C38 C34 117.9(9) . . ? C37 C38 H38 121.0 . . ? C34 C38 H38 121.0 . . ? O5 C39 N3 124.5(8) . . ? O5 C39 C35 122.0(7) . . ? N3 C39 C35 113.5(7) . . ? C39 N3 C40 124.0(7) . . ? C39 N3 H3A 118.0 . . ? C40 N3 H3A 118.0 . . ? N3 C40 C41 109.9(6) . . ? N3 C40 H40A 109.7 . . ? C41 C40 H40A 109.7 . . ? N3 C40 H40B 109.7 . . ? C41 C40 H40B 109.7 . . ? H40A C40 H40B 108.2 . . ? O6 C41 C40 110.3(6) . . ? O6 C41 H41A 109.6 . . ? C40 C41 H41A 109.6 . . ? O6 C41 H41B 109.6 . . ? C40 C41 H41B 109.6 . . ? H41A C41 H41B 108.1 . . ? C41 O6 C42 111.3(6) . . ? O6 C42 C43 110.7(6) . . ? O6 C42 H42A 109.5 . . ? C43 C42 H42A 109.5 . . ? O6 C42 H42B 109.5 . . ? C43 C42 H42B 109.5 . . ? H42A C42 H42B 108.1 . . ? O57 C43 C42 110.2(6) . . ? O57 C43 H43A 109.6 . . ? C42 C43 H43A 109.6 . . ? O57 C43 H43B 109.6 . . ? C42 C43 H43B 109.6 . . ? H43A C43 H43B 108.1 . . ? C44 O57 C43 110.8(5) . . ? O57 C44 C45 110.6(5) . . ? O57 C44 H44A 109.5 . . ? C45 C44 H44A 109.5 . . ? O57 C44 H44B 109.5 . . ? C45 C44 H44B 109.5 . . ? H44A C44 H44B 108.1 . . ? O8 C45 C44 111.4(5) . . ? O8 C45 H45A 109.3 . . ? C44 C45 H45A 109.3 . . ? O8 C45 H45B 109.3 . . ? C44 C45 H45B 109.3 . . ? H45A C45 H45B 108.0 . . ? C46 O8 C45 110.5(4) . . ? O8 C46 C47 108.2(4) . . ? O8 C46 H46A 110.1 . . ? C47 C46 H46A 110.1 . . ? O8 C46 H46B 110.1 . . ? C47 C46 H46B 110.1 . . ? H46A C46 H46B 108.4 . . ? C46 C47 P2 111.8(4) . . ? C46 C47 H47A 109.3 . . ? P2 C47 H47A 109.3 . . ? C46 C47 H47B 109.3 . . ? P2 C47 H47B 109.3 . . ? H47A C47 H47B 107.9 . . ? C49 C48 Pt1 177.7(5) . . ? C48 C49 C50 176.3(6) . . ? C55 C50 C51 119.0(5) . . ? C55 C50 C49 121.6(5) . . ? C51 C50 C49 119.4(5) . . ? C52 C51 C50 120.3(5) . . ? C52 C51 H51 119.8 . . ? C50 C51 H51 119.8 . . ? C51 C52 C53 119.7(5) . . ? C51 C52 H52 120.1 . . ? C53 C52 H52 120.1 . . ? C54 C53 C52 120.8(5) . . ? C54 C53 C56 121.8(5) . . ? C52 C53 C56 117.3(5) . . ? C53 C54 C55 119.6(5) . . ? C53 C54 H54 120.2 . . ? C55 C54 H54 120.2 . . ? C54 C55 C50 120.4(5) . . ? C54 C55 H55 119.8 . . ? C50 C55 H55 119.8 . . ? N4 C56 C53 178.1(7) . . ? C58 C57 Pt1 174.0(5) . . ? C57 C58 C59 172.8(7) . . ? C60 C59 C64 117.4(6) . . ? C60 C59 C58 122.1(6) . . ? C64 C59 C58 120.5(5) . . ? C61 C60 C59 121.8(7) . . ? C61 C60 H60 119.1 . . ? C59 C60 H60 119.1 . . ? C60 C61 C62 119.3(7) . . ? C60 C61 H61 120.4 . . ? C62 C61 H61 120.4 . . ? C63 C62 C61 120.2(6) . . ? C63 C62 C65 119.9(6) . . ? C61 C62 C65 119.7(6) . . ? C62 C63 C64 120.7(6) . . ? C62 C63 H63 119.7 . . ? C64 C63 H63 119.7 . . ? C59 C64 C63 120.5(6) . . ? C59 C64 H64 119.7 . . ? C63 C64 H64 119.7 . . ? N5 C65 C62 179.1(9) . . ? C122 Pt2 C113 176.7(2) . . ? C122 Pt2 P4 85.01(15) . . ? C113 Pt2 P4 92.08(14) . . ? C122 Pt2 P3 93.93(15) . . ? C113 Pt2 P3 88.73(14) . . ? P4 Pt2 P3 171.91(5) . . ? C72 P3 C66 103.9(2) . . ? C72 P3 C90 104.7(3) . . ? C66 P3 C90 103.5(3) . . ? C72 P3 Pt2 107.23(17) . . ? C66 P3 Pt2 119.1(2) . . ? C90 P3 Pt2 116.82(18) . . ? C71 C66 C67 119.3(5) . . ? C71 C66 P3 121.6(4) . . ? C67 C66 P3 119.1(5) . . ? C66 C67 C68 118.9(7) . . ? C66 C67 H67 120.6 . . ? C68 C67 H67 120.6 . . ? C69 C68 C67 121.4(6) . . ? C69 C68 H68 119.3 . . ? C67 C68 H68 119.3 . . ? C68 C69 C70 120.5(6) . . ? C68 C69 H69 119.8 . . ? C70 C69 H69 119.8 . . ? C69 C70 C71 119.7(7) . . ? C69 C70 H70 120.1 . . ? C71 C70 H70 120.1 . . ? C66 C71 C70 120.3(6) . . ? C66 C71 H71 119.9 . . ? C70 C71 H71 119.9 . . ? C77 C72 C73 118.8(5) . . ? C77 C72 P3 123.0(4) . . ? C73 C72 P3 118.1(4) . . ? C74 C73 C72 120.0(6) . . ? C74 C73 H73 120.0 . . ? C72 C73 H73 120.0 . . ? C73 C74 C75 120.3(6) . . ? C73 C74 H74 119.9 . . ? C75 C74 H74 119.9 . . ? C76 C75 C74 119.9(6) . . ? C76 C75 H75 120.1 . . ? C74 C75 H75 120.1 . . ? C75 C76 C77 120.6(6) . . ? C75 C76 H76 119.7 . . ? C77 C76 H76 119.7 . . ? C76 C77 C72 120.4(6) . . ? C76 C77 H77 119.8 . . ? C72 C77 H77 119.8 . . ? C78 P4 C84 104.4(2) . . ? C78 P4 C112 102.3(3) . . ? C84 P4 C112 104.0(3) . . ? C78 P4 Pt2 112.64(18) . . ? C84 P4 Pt2 115.53(18) . . ? C112 P4 Pt2 116.44(18) . . ? C79 C78 C83 119.7(5) . . ? C79 C78 P4 122.8(4) . . ? C83 C78 P4 117.5(4) . . ? C78 C79 C80 120.1(5) . . ? C78 C79 H79 120.0 . . ? C80 C79 H79 120.0 . . ? C81 C80 C79 120.1(6) . . ? C81 C80 H80 119.9 . . ? C79 C80 H80 119.9 . . ? C82 C81 C80 120.2(6) . . ? C82 C81 H81 119.9 . . ? C80 C81 H81 119.9 . . ? C81 C82 C83 120.5(6) . . ? C81 C82 H82 119.8 . . ? C83 C82 H82 119.8 . . ? C82 C83 C78 119.3(6) . . ? C82 C83 H83 120.3 . . ? C78 C83 H83 120.3 . . ? C89 C84 C85 119.9(5) . . ? C89 C84 P4 121.9(5) . . ? C85 C84 P4 118.2(4) . . ? C84 C85 C86 118.2(6) . . ? C84 C85 H85 120.9 . . ? C86 C85 H85 120.9 . . ? C87 C86 C85 121.4(7) . . ? C87 C86 H86 119.3 . . ? C85 C86 H86 119.3 . . ? C86 C87 C88 120.3(6) . . ? C86 C87 H87 119.8 . . ? C88 C87 H87 119.8 . . ? C87 C88 C89 120.2(6) . . ? C87 C88 H88 119.9 . . ? C89 C88 H88 119.9 . . ? C84 C89 C88 120.0(6) . . ? C84 C89 H89 120.0 . . ? C88 C89 H89 120.0 . . ? C91 C90 P3 112.9(4) . . ? C91 C90 H90A 109.0 . . ? P3 C90 H90A 109.0 . . ? C91 C90 H90B 109.0 . . ? P3 C90 H90B 109.0 . . ? H90A C90 H90B 107.8 . . ? O9 C91 C90 107.1(4) . . ? O9 C91 H91A 110.3 . . ? C90 C91 H91A 110.3 . . ? O9 C91 H91B 110.3 . . ? C90 C91 H91B 110.3 . . ? H91A C91 H91B 108.5 . . ? C91 O9 C92 110.1(4) . . ? O9 C92 C93 110.2(5) . . ? O9 C92 H92A 109.6 . . ? C93 C92 H92A 109.6 . . ? O9 C92 H92B 109.6 . . ? C93 C92 H92B 109.6 . . ? H92A C92 H92B 108.1 . . ? O10 C93 C92 110.4(5) . . ? O10 C93 H93A 109.6 . . ? C92 C93 H93A 109.6 . . ? O10 C93 H93B 109.6 . . ? C92 C93 H93B 109.6 . . ? H93A C93 H93B 108.1 . . ? C93 O10 C94 110.9(5) . . ? O10 C94 C95 109.4(6) . . ? O10 C94 H94A 109.8 . . ? C95 C94 H94A 109.8 . . ? O10 C94 H94B 109.8 . . ? C95 C94 H94B 109.8 . . ? H94A C94 H94B 108.2 . . ? O11 C95 C94 110.4(6) . . ? O11 C95 H95A 109.6 . . ? C94 C95 H95A 109.6 . . ? O11 C95 H95B 109.6 . . ? C94 C95 H95B 109.6 . . ? H95A C95 H95B 108.1 . . ? C96 O11 C95 110.8(5) . . ? O11 C96 C97 110.6(6) . . ? O11 C96 H96A 109.5 . . ? C97 C96 H96A 109.5 . . ? O11 C96 H96B 109.5 . . ? C97 C96 H96B 109.5 . . ? H96A C96 H96B 108.1 . . ? N6 C97 C96 109.5(6) . . ? N6 C97 H97A 109.8 . . ? C96 C97 H97A 109.8 . . ? N6 C97 H97B 109.8 . . ? C96 C97 H97B 109.8 . . ? H97A C97 H97B 108.2 . . ? C98 N6 C97 124.6(6) . . ? C98 N6 H6A 117.7 . . ? C97 N6 H6A 117.7 . . ? O12 C98 N6 124.0(7) . . ? O12 C98 C99 121.0(6) . . ? N6 C98 C99 115.0(6) . . ? N7 C99 C103 122.5(6) . . ? N7 C99 C98 117.1(6) . . ? C103 C99 C98 120.4(6) . . ? C99 N7 C100 119.1(5) . . ? N7 C100 C101 122.8(6) . . ? N7 C100 C104 117.3(5) . . ? C101 C100 C104 119.9(6) . . ? C102 C101 C100 117.8(7) . . ? C102 C101 H101 121.1 . . ? C100 C101 H101 121.1 . . ? C101 C102 C103 120.0(7) . . ? C101 C102 H102 120.0 . . ? C103 C102 H102 120.0 . . ? C99 C103 C102 117.8(7) . . ? C99 C103 H103 121.1 . . ? C102 C103 H103 121.1 . . ? O13 C104 N8 125.2(6) . . ? O13 C104 C100 120.1(6) . . ? N8 C104 C100 114.6(6) . . ? C104 N8 C105 122.3(6) . . ? C104 N8 H8A 118.8 . . ? C105 N8 H8A 118.8 . . ? N8 C105 C106 113.6(6) . . ? N8 C105 H10A 108.8 . . ? C106 C105 H10A 108.8 . . ? N8 C105 H10B 108.8 . . ? C106 C105 H10B 108.8 . . ? H10A C105 H10B 107.7 . . ? O14 C106 C105 109.3(6) . . ? O14 C106 H10C 109.8 . . ? C105 C106 H10C 109.8 . . ? O14 C106 H10D 109.8 . . ? C105 C106 H10D 109.8 . . ? H10C C106 H10D 108.3 . . ? C106 O14 C107 111.2(6) . . ? O14 C107 C108 114.4(7) . . ? O14 C107 H10E 108.7 . . ? C108 C107 H10E 108.7 . . ? O14 C107 H10F 108.7 . . ? C108 C107 H10F 108.7 . . ? H10E C107 H10F 107.6 . . ? O15 C108 C107 109.8(6) . . ? O15 C108 H10G 109.7 . . ? C107 C108 H10G 109.7 . . ? O15 C108 H10H 109.7 . . ? C107 C108 H10H 109.7 . . ? H10G C108 H10H 108.2 . . ? C108 O15 C109 111.7(5) . . ? O15 C109 C110 109.5(5) . . ? O15 C109 H10I 109.8 . . ? C110 C109 H10I 109.8 . . ? O15 C109 H10J 109.8 . . ? C110 C109 H10J 109.8 . . ? H10I C109 H10J 108.2 . . ? O16 C110 C109 108.3(6) . . ? O16 C110 H11A 110.0 . . ? C109 C110 H11A 110.0 . . ? O16 C110 H11B 110.0 . . ? C109 C110 H11B 110.0 . . ? H11A C110 H11B 108.4 . . ? C111 O16 C110 111.8(5) . . ? O16 C111 C112 106.7(5) . . ? O16 C111 H11C 110.4 . . ? C112 C111 H11C 110.4 . . ? O16 C111 H11D 110.4 . . ? C112 C111 H11D 110.4 . . ? H11C C111 H11D 108.6 . . ? C111 C112 P4 115.7(4) . . ? C111 C112 H11E 108.4 . . ? P4 C112 H11E 108.4 . . ? C111 C112 H11F 108.4 . . ? P4 C112 H11F 108.4 . . ? H11E C112 H11F 107.4 . . ? C114 C113 Pt2 175.3(5) . . ? C113 C114 C115 174.5(6) . . ? C116 C115 C120 119.2(5) . . ? C116 C115 C114 119.4(5) . . ? C120 C115 C114 121.3(5) . . ? C117 C116 C115 120.9(5) . . ? C117 C116 H116 119.6 . . ? C115 C116 H116 119.6 . . ? C116 C117 C118 119.6(5) . . ? C116 C117 H117 120.2 . . ? C118 C117 H117 120.2 . . ? C119 C118 C117 120.6(5) . . ? C119 C118 C121 121.5(6) . . ? C117 C118 C121 117.9(6) . . ? C118 C119 C120 119.7(6) . . ? C118 C119 H119 120.1 . . ? C120 C119 H119 120.1 . . ? C119 C120 C115 119.9(5) . . ? C119 C120 H120 120.0 . . ? C115 C120 H120 120.0 . . ? N9 C121 C118 178.1(8) . . ? C123 C122 Pt2 171.0(5) . . ? C122 C123 C124 173.3(7) . . ? C129 C124 C125 118.3(6) . . ? C129 C124 C123 120.5(6) . . ? C125 C124 C123 121.3(7) . . ? C126 C125 C124 120.0(8) . . ? C126 C125 H125 120.0 . . ? C124 C125 H125 120.0 . . ? C125 C126 C127 121.5(8) . . ? C125 C126 H126 119.2 . . ? C127 C126 H126 119.2 . . ? C128 C127 C126 118.8(7) . . ? C128 C127 C130 120.1(9) . . ? C126 C127 C130 121.0(9) . . ? C127 C128 C129 119.4(8) . . ? C127 C128 H128 120.3 . . ? C129 C128 H128 120.3 . . ? C124 C129 C128 121.9(7) . . ? C124 C129 H129 119.1 . . ? C128 C129 H129 119.1 . . ? N10 C130 C127 174.5(16) . . ? Cl1 C131 Cl2 112.2(7) . . ? Cl1 C131 Cl3 110.7(7) . . ? Cl2 C131 Cl3 112.9(7) . . ? Cl1 C131 H131 106.9 . . ? Cl2 C131 H131 106.9 . . ? Cl3 C131 H131 106.9 . . ? Cl4 C132 Cl6 113.9(7) . . ? Cl4 C132 Cl5 111.5(7) . . ? Cl6 C132 Cl5 109.3(6) . . ? Cl4 C132 H132 107.3 . . ? Cl6 C132 H132 107.3 . . ? Cl5 C132 H132 107.3 . . ? Cl7 C133 Cl8 110.7(8) . . ? Cl7 C133 Cl9 114.4(7) . . ? Cl8 C133 Cl9 98.9(8) . . ? Cl7 C133 H133 110.8 . . ? Cl8 C133 H133 110.8 . . ? Cl9 C133 H133 110.8 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 29.14 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.553 _refine_diff_density_min -1.742 _refine_diff_density_rms 0.160 _database_code_depnum_ccdc_archive 'CCDC 950508' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_e2759a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C65 H63 N5 O8 P2 Pd Pt,2(H2 O)' _chemical_formula_sum 'C65 H67 N5 O10 P2 Pd Pt' _chemical_formula_weight 1441.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4259(2) _cell_length_b 16.0554(4) _cell_length_c 19.5520(3) _cell_angle_alpha 78.7480(10) _cell_angle_beta 73.7260(10) _cell_angle_gamma 75.1560(10) _cell_volume 3298.62(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9949 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 30.01 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1452 _exptl_absorpt_coefficient_mu 2.498 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8853 _exptl_absorpt_correction_T_max 0.9067 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 63105 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_av_sigmaI/netI 0.0311 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 29.15 _reflns_number_total 17682 _reflns_number_gt 15260 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0889P)^2^+5.4919P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17682 _refine_ls_number_parameters 766 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0528 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.1399 _refine_ls_wR_factor_gt 0.1329 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.867840(13) 0.313840(10) 1.108511(8) 0.02080(6) Uani 1 1 d . . . Pd1 Pd 0.90823(3) 0.13280(3) 0.538727(19) 0.03342(9) Uani 1 1 d . . . P1 P 0.65578(9) 0.32739(7) 1.13457(6) 0.0205(2) Uani 1 1 d . . . C1 C 0.5849(4) 0.2608(3) 1.2131(3) 0.0313(10) Uani 1 1 d . . . C2 C 0.6559(6) 0.1869(4) 1.2423(4) 0.0526(16) Uani 1 1 d . . . H2 H 0.7439 0.1731 1.2244 0.063 Uiso 1 1 calc R . . C3 C 0.5967(8) 0.1330(6) 1.2984(5) 0.079(3) Uani 1 1 d . . . H3 H 0.6447 0.0806 1.3175 0.095 Uiso 1 1 calc R . . C4 C 0.4696(8) 0.1538(7) 1.3271(4) 0.079(3) Uani 1 1 d . . . H4 H 0.4310 0.1178 1.3671 0.094 Uiso 1 1 calc R . . C5 C 0.3998(7) 0.2272(6) 1.2969(4) 0.064(2) Uani 1 1 d . . . H5 H 0.3120 0.2418 1.3156 0.077 Uiso 1 1 calc R . . C6 C 0.4562(5) 0.2794(4) 1.2399(3) 0.0456(13) Uani 1 1 d . . . H6 H 0.4068 0.3291 1.2184 0.055 Uiso 1 1 calc R . . C7 C 0.5829(4) 0.4390(3) 1.1473(2) 0.0261(9) Uani 1 1 d . . . C8 C 0.5365(5) 0.4639(4) 1.2162(3) 0.0407(12) Uani 1 1 d . . . H8 H 0.5391 0.4223 1.2579 0.049 Uiso 1 1 calc R . . C9 C 0.4858(5) 0.5529(5) 1.2217(4) 0.063(2) Uani 1 1 d . . . H9 H 0.4498 0.5715 1.2678 0.075 Uiso 1 1 calc R . . C10 C 0.4882(6) 0.6145(4) 1.1597(5) 0.069(2) Uani 1 1 d . . . H10 H 0.4563 0.6745 1.1640 0.083 Uiso 1 1 calc R . . C11 C 0.5349(6) 0.5889(4) 1.0949(4) 0.0556(18) Uani 1 1 d . . . H11 H 0.5365 0.6311 1.0534 0.067 Uiso 1 1 calc R . . C12 C 0.5814(5) 0.5016(3) 1.0866(3) 0.0381(11) Uani 1 1 d . . . H12 H 0.6121 0.4845 1.0398 0.046 Uiso 1 1 calc R . . C13 C 0.5863(4) 0.3097(3) 1.0662(2) 0.0246(8) Uani 1 1 d . . . H13A H 0.4958 0.3357 1.0785 0.029 Uiso 1 1 calc R . . H13B H 0.6236 0.3404 1.0192 0.029 Uiso 1 1 calc R . . C14 C 0.6042(4) 0.2146(3) 1.0590(3) 0.0268(9) Uani 1 1 d . . . H14A H 0.6940 0.1884 1.0428 0.032 Uiso 1 1 calc R . . H14B H 0.5698 0.1822 1.1058 0.032 Uiso 1 1 calc R . . O1 O 0.5394(3) 0.2117(2) 1.00726(17) 0.0268(6) Uani 1 1 d . . . C15 C 0.5501(5) 0.1248(3) 0.9965(3) 0.0302(9) Uani 1 1 d . . . H15A H 0.5314 0.0882 1.0435 0.036 Uiso 1 1 calc R . . H15B H 0.6365 0.1010 0.9705 0.036 Uiso 1 1 calc R . . C16 C 0.4611(5) 0.1227(3) 0.9539(3) 0.0300(9) Uani 1 1 d . . . H16A H 0.4534 0.0620 0.9567 0.036 Uiso 1 1 calc R . . H16B H 0.3777 0.1572 0.9745 0.036 Uiso 1 1 calc R . . O2 O 0.5030(3) 0.1568(2) 0.88153(17) 0.0295(7) Uani 1 1 d . . . C17 C 0.4135(5) 0.1585(4) 0.8427(3) 0.0388(12) Uani 1 1 d . . . H17A H 0.3378 0.2037 0.8577 0.047 Uiso 1 1 calc R . . H17B H 0.3890 0.1016 0.8532 0.047 Uiso 1 1 calc R . . C18 C 0.4701(5) 0.1781(4) 0.7625(3) 0.0404(12) Uani 1 1 d . . . H18A H 0.4042 0.1921 0.7357 0.048 Uiso 1 1 calc R . . H18B H 0.5095 0.2287 0.7531 0.048 Uiso 1 1 calc R . . O3 O 0.5609(3) 0.1038(3) 0.73957(18) 0.0397(8) Uani 1 1 d . . . C19 C 0.6116(5) 0.1155(4) 0.6642(3) 0.0368(11) Uani 1 1 d . . . H19A H 0.6471 0.1683 0.6500 0.044 Uiso 1 1 calc R . . H19B H 0.5455 0.1226 0.6386 0.044 Uiso 1 1 calc R . . C20 C 0.7127(5) 0.0359(4) 0.6452(3) 0.0360(11) Uani 1 1 d . . . H20A H 0.7674 0.0212 0.6790 0.043 Uiso 1 1 calc R . . H20B H 0.6742 -0.0141 0.6496 0.043 Uiso 1 1 calc R . . N1 N 0.7872(4) 0.0523(3) 0.5715(2) 0.0339(9) Uani 1 1 d . . . C21 C 0.7672(4) 0.0211(3) 0.5184(3) 0.0324(10) Uani 1 1 d . . . O4 O 0.6895(4) -0.0240(3) 0.5238(2) 0.0419(9) Uani 1 1 d . . . C22 C 0.8469(5) 0.0477(3) 0.4461(3) 0.0321(10) Uani 1 1 d . . . C23 C 0.8519(5) 0.0242(4) 0.3808(3) 0.0394(12) Uani 1 1 d . . . H23 H 0.8035 -0.0146 0.3780 0.047 Uiso 1 1 calc R . . C24 C 0.9297(6) 0.0587(4) 0.3192(3) 0.0429(13) Uani 1 1 d . . . H24 H 0.9359 0.0421 0.2740 0.051 Uiso 1 1 calc R . . C25 C 0.9977(5) 0.1165(4) 0.3227(3) 0.0401(12) Uani 1 1 d . . . H25 H 1.0490 0.1409 0.2804 0.048 Uiso 1 1 calc R . . C26 C 0.9898(4) 0.1385(4) 0.3897(3) 0.0333(10) Uani 1 1 d . . . N2 N 0.9155(4) 0.1022(3) 0.4483(2) 0.0305(8) Uani 1 1 d . . . C27 C 1.0499(5) 0.2024(4) 0.4060(3) 0.0419(12) Uani 1 1 d . . . O5 O 1.1119(4) 0.2454(4) 0.3560(2) 0.0576(12) Uani 1 1 d . . . N3 N 1.0254(4) 0.2073(3) 0.4762(3) 0.0440(11) Uani 1 1 d . . . C28 C 1.0645(6) 0.2745(4) 0.5006(4) 0.0525(15) Uani 1 1 d . . . H28A H 0.9928 0.3059 0.5347 0.063 Uiso 1 1 calc R . . H28B H 1.0920 0.3171 0.4589 0.063 Uiso 1 1 calc R . . C29 C 1.1709(5) 0.2339(4) 0.5373(3) 0.0480(14) Uani 1 1 d . . . H29A H 1.1532 0.1812 0.5707 0.058 Uiso 1 1 calc R . . H29B H 1.2501 0.2173 0.5012 0.058 Uiso 1 1 calc R . . O6 O 1.1796(4) 0.2979(3) 0.5756(2) 0.0453(9) Uani 1 1 d . . . C30 C 1.2868(5) 0.2708(5) 0.6048(4) 0.0510(15) Uani 1 1 d . . . H30A H 1.3621 0.2532 0.5664 0.061 Uiso 1 1 calc R . . H30B H 1.2773 0.2198 0.6421 0.061 Uiso 1 1 calc R . . C31 C 1.3025(5) 0.3441(5) 0.6375(3) 0.0482(14) Uani 1 1 d . . . H31A H 1.3897 0.3331 0.6415 0.058 Uiso 1 1 calc R . . H31B H 1.2861 0.3993 0.6053 0.058 Uiso 1 1 calc R . . O7 O 1.2202(4) 0.3526(3) 0.7068(2) 0.0457(9) Uani 1 1 d . . . C32 C 1.2526(6) 0.4138(4) 0.7392(3) 0.0450(13) Uani 1 1 d . . . H32A H 1.2549 0.4683 0.7054 0.054 Uiso 1 1 calc R . . H32B H 1.3374 0.3901 0.7471 0.054 Uiso 1 1 calc R . . C33 C 1.1615(6) 0.4348(4) 0.8112(3) 0.0453(13) Uani 1 1 d . . . H33A H 1.1724 0.4889 0.8234 0.054 Uiso 1 1 calc R . . H33B H 1.0745 0.4441 0.8071 0.054 Uiso 1 1 calc R . . O8 O 1.1845(3) 0.3650(2) 0.86635(18) 0.0311(7) Uani 1 1 d . . . C34 C 1.1222(4) 0.3900(3) 0.9357(2) 0.0296(9) Uani 1 1 d . . . H34A H 1.0306 0.4017 0.9425 0.035 Uiso 1 1 calc R . . H34B H 1.1453 0.4430 0.9416 0.035 Uiso 1 1 calc R . . C35 C 1.1646(4) 0.3136(3) 0.9895(2) 0.0268(9) Uani 1 1 d . . . H35A H 1.2524 0.3125 0.9877 0.032 Uiso 1 1 calc R . . H35B H 1.1644 0.2598 0.9720 0.032 Uiso 1 1 calc R . . P2 P 1.07961(9) 0.30700(7) 1.08425(6) 0.0227(2) Uani 1 1 d . . . C36 C 1.1562(4) 0.1986(3) 1.1175(2) 0.0270(9) Uani 1 1 d . . . C37 C 1.2616(4) 0.1841(4) 1.1449(3) 0.0379(11) Uani 1 1 d . . . H37 H 1.2949 0.2315 1.1476 0.046 Uiso 1 1 calc R . . C38 C 1.3170(5) 0.0993(4) 1.1681(3) 0.0430(13) Uani 1 1 d . . . H38 H 1.3862 0.0891 1.1888 0.052 Uiso 1 1 calc R . . C39 C 1.2725(5) 0.0300(4) 1.1615(3) 0.0446(14) Uani 1 1 d . . . H39 H 1.3130 -0.0277 1.1758 0.054 Uiso 1 1 calc R . . C40 C 1.1693(7) 0.0443(4) 1.1342(4) 0.0504(15) Uani 1 1 d . . . H40 H 1.1383 -0.0035 1.1300 0.061 Uiso 1 1 calc R . . C41 C 1.1101(5) 0.1291(3) 1.1126(3) 0.0415(12) Uani 1 1 d . . . H41 H 1.0380 0.1389 1.0945 0.050 Uiso 1 1 calc R . . C42 C 1.1299(4) 0.3799(3) 1.1249(3) 0.0277(9) Uani 1 1 d . . . C43 C 1.1118(5) 0.3679(4) 1.1996(3) 0.0351(10) Uani 1 1 d . . . H43 H 1.0746 0.3218 1.2278 0.042 Uiso 1 1 calc R . . C44 C 1.1477(6) 0.4228(4) 1.2330(3) 0.0464(14) Uani 1 1 d . . . H44 H 1.1354 0.4145 1.2837 0.056 Uiso 1 1 calc R . . C45 C 1.2023(6) 0.4905(4) 1.1910(4) 0.0450(13) Uani 1 1 d . . . H45 H 1.2271 0.5284 1.2132 0.054 Uiso 1 1 calc R . . C46 C 1.2199(5) 0.5020(4) 1.1189(3) 0.0421(12) Uani 1 1 d . . . H46 H 1.2572 0.5481 1.0908 0.051 Uiso 1 1 calc R . . C47 C 1.1842(5) 0.4475(3) 1.0851(3) 0.0338(10) Uani 1 1 d . . . H47 H 1.1972 0.4567 1.0343 0.041 Uiso 1 1 calc R . . C48 C 0.8835(4) 0.2915(3) 1.0098(2) 0.0265(9) Uani 1 1 d . . . C49 C 0.8892(4) 0.2758(3) 0.9513(3) 0.0310(10) Uani 1 1 d . . . C50 C 0.8917(4) 0.2555(3) 0.8827(3) 0.0312(10) Uani 1 1 d . . . C51 C 0.9932(6) 0.2631(5) 0.8243(3) 0.0555(18) Uani 1 1 d . . . H51 H 1.0628 0.2806 0.8301 0.067 Uiso 1 1 calc R . . C52 C 0.9932(6) 0.2451(6) 0.7576(3) 0.062(2) Uani 1 1 d . . . H52 H 1.0594 0.2543 0.7169 0.075 Uiso 1 1 calc R . . C53 C 0.8947(5) 0.2132(4) 0.7517(3) 0.0392(12) Uani 1 1 d . . . C54 C 0.7929(5) 0.2073(3) 0.8078(3) 0.0333(10) Uani 1 1 d . . . H54 H 0.7247 0.1879 0.8020 0.040 Uiso 1 1 calc R . . C55 C 0.7903(4) 0.2297(4) 0.8730(3) 0.0336(10) Uani 1 1 d . . . H55 H 0.7186 0.2276 0.9117 0.040 Uiso 1 1 calc R . . C56 C 0.8984(5) 0.1883(4) 0.6848(3) 0.0425(13) Uani 1 1 d . . . N4 N 0.9025(5) 0.1669(4) 0.6331(2) 0.0465(12) Uani 1 1 d . . . C57 C 0.8414(3) 0.3306(3) 1.2171(2) 0.0243(9) Uani 1 1 d . . . C58 C 0.8124(5) 0.3293(4) 1.2750(4) 0.0436(13) Uani 1 1 d . . . C59 C 0.7769(5) 0.3319(4) 1.3518(3) 0.0439(13) Uani 1 1 d . . . C60 C 0.6919(7) 0.2844(5) 1.3962(3) 0.0575(17) Uani 1 1 d . . . H60 H 0.6568 0.2518 1.3746 0.069 Uiso 1 1 calc R . . C61 C 0.6553(7) 0.2817(5) 1.4706(4) 0.066(2) Uani 1 1 d . . . H61 H 0.6003 0.2463 1.5001 0.079 Uiso 1 1 calc R . . C62 C 0.7060(7) 0.3357(5) 1.4993(3) 0.0609(18) Uani 1 1 d . . . C63 C 0.7921(7) 0.3856(5) 1.4544(4) 0.0604(18) Uani 1 1 d . . . H63 H 0.8264 0.4206 1.4743 0.072 Uiso 1 1 calc R . . C64 C 0.8235(6) 0.3822(5) 1.3840(3) 0.0521(15) Uani 1 1 d . . . H64 H 0.8807 0.4158 1.3541 0.063 Uiso 1 1 calc R . . C65 C 0.6734(9) 0.3362(6) 1.5767(4) 0.076(2) Uani 1 1 d . . . N5 N 0.6492(10) 0.3355(6) 1.6363(4) 0.106(3) Uani 1 1 d . . . O9 O 0.4272(6) 0.0605(4) 0.5727(4) 0.0870(19) Uani 1 1 d . . . O10 O 0.3824(10) 0.4258(6) 0.4245(4) 0.081(4) Uani 0.50 1 d P . . O11 O 0.1379(8) 0.5095(4) 0.4001(3) 0.082(4) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01869(8) 0.02315(9) 0.02029(9) -0.00448(6) -0.00450(6) -0.00310(6) Pd1 0.03184(18) 0.0491(2) 0.02428(17) -0.01049(16) -0.00688(14) -0.01297(16) P1 0.0185(4) 0.0233(5) 0.0201(5) -0.0053(4) -0.0045(4) -0.0035(4) C1 0.030(2) 0.039(3) 0.028(2) 0.000(2) -0.0097(18) -0.015(2) C2 0.050(3) 0.052(3) 0.061(4) 0.021(3) -0.028(3) -0.024(3) C3 0.081(5) 0.088(6) 0.081(6) 0.051(5) -0.048(5) -0.053(5) C4 0.079(5) 0.120(7) 0.055(4) 0.028(5) -0.022(4) -0.076(6) C5 0.048(4) 0.093(6) 0.052(4) 0.000(4) 0.004(3) -0.042(4) C6 0.032(3) 0.056(4) 0.046(3) -0.005(3) -0.001(2) -0.016(2) C7 0.0201(18) 0.029(2) 0.033(2) -0.0120(19) -0.0092(16) -0.0022(16) C8 0.032(2) 0.052(3) 0.044(3) -0.027(3) -0.006(2) -0.008(2) C9 0.034(3) 0.076(5) 0.094(5) -0.071(5) -0.010(3) -0.001(3) C10 0.050(3) 0.038(3) 0.142(8) -0.045(4) -0.058(4) 0.012(3) C11 0.060(4) 0.026(2) 0.097(5) -0.006(3) -0.054(4) -0.002(2) C12 0.046(3) 0.028(2) 0.049(3) -0.005(2) -0.025(2) -0.008(2) C13 0.0267(19) 0.026(2) 0.024(2) -0.0052(17) -0.0083(16) -0.0068(16) C14 0.028(2) 0.025(2) 0.030(2) -0.0062(18) -0.0101(17) -0.0056(16) O1 0.0310(15) 0.0227(14) 0.0313(16) -0.0073(13) -0.0111(13) -0.0072(12) C15 0.039(2) 0.022(2) 0.033(2) -0.0072(19) -0.0109(19) -0.0073(18) C16 0.036(2) 0.027(2) 0.031(2) -0.0065(19) -0.0072(19) -0.0131(18) O2 0.0264(15) 0.0362(17) 0.0279(16) -0.0093(14) -0.0071(12) -0.0059(13) C17 0.027(2) 0.053(3) 0.037(3) -0.012(2) -0.0103(19) -0.001(2) C18 0.033(2) 0.052(3) 0.032(2) -0.013(2) -0.012(2) 0.010(2) O3 0.0390(18) 0.048(2) 0.0247(16) -0.0098(16) -0.0067(14) 0.0052(16) C19 0.033(2) 0.052(3) 0.024(2) -0.007(2) -0.0078(18) -0.004(2) C20 0.036(2) 0.046(3) 0.027(2) -0.010(2) -0.0040(19) -0.009(2) N1 0.034(2) 0.046(2) 0.0236(19) -0.0066(18) -0.0057(16) -0.0119(18) C21 0.031(2) 0.039(3) 0.029(2) -0.009(2) -0.0092(18) -0.0066(19) O4 0.046(2) 0.048(2) 0.039(2) -0.0069(18) -0.0126(17) -0.0200(18) C22 0.032(2) 0.037(3) 0.028(2) -0.006(2) -0.0108(18) -0.0036(19) C23 0.045(3) 0.047(3) 0.032(3) -0.012(2) -0.015(2) -0.007(2) C24 0.050(3) 0.051(3) 0.028(2) -0.011(2) -0.013(2) -0.004(3) C25 0.031(2) 0.059(3) 0.022(2) -0.002(2) -0.0036(18) -0.002(2) C26 0.023(2) 0.048(3) 0.027(2) -0.006(2) -0.0049(17) -0.0041(19) N2 0.0254(17) 0.043(2) 0.0230(18) -0.0056(17) -0.0072(14) -0.0056(16) C27 0.031(2) 0.061(4) 0.037(3) -0.002(3) -0.011(2) -0.014(2) O5 0.045(2) 0.087(3) 0.043(2) 0.007(2) -0.0081(19) -0.034(2) N3 0.041(2) 0.061(3) 0.038(2) -0.006(2) -0.0130(19) -0.022(2) C28 0.053(3) 0.048(3) 0.063(4) 0.004(3) -0.027(3) -0.019(3) C29 0.040(3) 0.059(4) 0.050(3) -0.009(3) -0.018(3) -0.010(3) O6 0.039(2) 0.055(2) 0.049(2) -0.011(2) -0.0176(17) -0.0128(18) C30 0.036(3) 0.071(4) 0.047(3) -0.009(3) -0.014(2) -0.009(3) C31 0.039(3) 0.075(4) 0.037(3) -0.005(3) -0.006(2) -0.030(3) O7 0.042(2) 0.066(3) 0.035(2) -0.0056(19) -0.0060(16) -0.0280(19) C32 0.057(3) 0.053(3) 0.030(3) 0.006(3) -0.010(2) -0.030(3) C33 0.057(3) 0.034(3) 0.037(3) 0.008(2) -0.010(3) -0.005(2) O8 0.0346(17) 0.0329(17) 0.0246(16) 0.0015(14) -0.0068(13) -0.0092(14) C34 0.029(2) 0.030(2) 0.029(2) -0.0033(19) -0.0088(18) -0.0049(18) C35 0.0199(18) 0.031(2) 0.026(2) -0.0022(18) -0.0032(16) -0.0035(16) P2 0.0189(4) 0.0244(5) 0.0236(5) -0.0033(4) -0.0054(4) -0.0025(4) C36 0.0251(19) 0.029(2) 0.022(2) -0.0016(18) -0.0033(16) -0.0009(17) C37 0.025(2) 0.039(3) 0.044(3) 0.007(2) -0.011(2) -0.0044(19) C38 0.032(2) 0.043(3) 0.046(3) 0.008(3) -0.013(2) 0.001(2) C39 0.047(3) 0.034(3) 0.037(3) -0.001(2) -0.006(2) 0.013(2) C40 0.070(4) 0.026(2) 0.060(4) -0.011(3) -0.027(3) 0.000(3) C41 0.047(3) 0.031(2) 0.051(3) -0.010(2) -0.024(3) 0.000(2) C42 0.0230(19) 0.031(2) 0.031(2) -0.0065(19) -0.0090(17) -0.0033(17) C43 0.035(2) 0.044(3) 0.031(2) -0.003(2) -0.0104(19) -0.016(2) C44 0.048(3) 0.063(4) 0.039(3) -0.009(3) -0.015(2) -0.023(3) C45 0.047(3) 0.043(3) 0.055(4) -0.013(3) -0.022(3) -0.013(2) C46 0.043(3) 0.034(3) 0.054(3) -0.008(3) -0.013(3) -0.015(2) C47 0.035(2) 0.033(2) 0.034(3) -0.005(2) -0.008(2) -0.0066(19) C48 0.0225(18) 0.033(2) 0.024(2) -0.0065(18) -0.0035(16) -0.0062(17) C49 0.028(2) 0.038(3) 0.028(2) -0.010(2) -0.0018(17) -0.0113(19) C50 0.032(2) 0.038(3) 0.026(2) -0.009(2) -0.0011(18) -0.0140(19) C51 0.046(3) 0.102(5) 0.034(3) -0.023(3) 0.005(2) -0.048(3) C52 0.053(3) 0.121(6) 0.031(3) -0.030(4) 0.011(2) -0.058(4) C53 0.041(3) 0.056(3) 0.028(2) -0.012(2) -0.003(2) -0.025(2) C54 0.032(2) 0.039(3) 0.033(2) -0.011(2) -0.0073(19) -0.011(2) C55 0.028(2) 0.046(3) 0.028(2) -0.013(2) -0.0012(18) -0.011(2) C56 0.040(3) 0.064(4) 0.030(3) -0.012(3) -0.002(2) -0.025(3) N4 0.051(3) 0.070(3) 0.028(2) -0.016(2) -0.0027(19) -0.029(2) C57 0.0094(15) 0.027(2) 0.027(2) 0.0118(18) -0.0008(14) -0.0029(14) C58 0.033(3) 0.047(3) 0.053(4) -0.009(3) -0.015(2) -0.006(2) C59 0.038(3) 0.058(4) 0.033(3) -0.009(3) -0.010(2) -0.002(2) C60 0.058(4) 0.078(5) 0.039(3) -0.015(3) -0.002(3) -0.024(3) C61 0.069(4) 0.079(5) 0.037(3) -0.013(3) -0.005(3) 0.005(4) C62 0.063(4) 0.077(5) 0.033(3) -0.017(3) 0.001(3) -0.005(4) C63 0.054(4) 0.073(5) 0.055(4) -0.015(4) -0.016(3) -0.007(3) C64 0.047(3) 0.068(4) 0.044(3) -0.016(3) -0.018(3) -0.005(3) C65 0.095(6) 0.081(6) 0.038(4) -0.012(4) 0.004(4) -0.015(5) N5 0.155(8) 0.108(6) 0.049(4) -0.035(4) -0.004(5) -0.021(6) O9 0.082(4) 0.103(5) 0.099(5) -0.050(4) -0.041(3) -0.010(3) O10 0.085(7) 0.067(6) 0.020(3) 0.023(4) 0.010(4) 0.059(5) O11 0.086(5) 0.063(3) 0.022(3) 0.024(3) 0.019(3) 0.061(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C48 1.983(4) . ? Pt1 C57 2.120(5) . ? Pt1 P1 2.2932(10) . ? Pt1 P2 2.3092(10) . ? Pd1 N2 1.901(4) . ? Pd1 N4 2.004(4) . ? Pd1 N3 2.012(5) . ? Pd1 N1 2.023(4) . ? P1 C7 1.806(4) . ? P1 C1 1.806(5) . ? P1 C13 1.832(4) . ? C1 C2 1.377(8) . ? C1 C6 1.389(7) . ? C2 C3 1.387(10) . ? C2 H2 0.9500 . ? C3 C4 1.379(12) . ? C3 H3 0.9500 . ? C4 C5 1.374(12) . ? C4 H4 0.9500 . ? C5 C6 1.367(9) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.398(7) . ? C7 C8 1.400(7) . ? C8 C9 1.411(9) . ? C8 H8 0.9500 . ? C9 C10 1.407(12) . ? C9 H9 0.9500 . ? C10 C11 1.332(11) . ? C10 H10 0.9500 . ? C11 C12 1.390(7) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.517(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 O1 1.425(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? O1 C15 1.421(5) . ? C15 C16 1.493(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 O2 1.409(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? O2 C17 1.427(6) . ? C17 C18 1.523(7) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 O3 1.419(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? O3 C19 1.418(6) . ? C19 C20 1.515(7) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 N1 1.465(6) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? N1 C21 1.333(6) . ? C21 O4 1.253(6) . ? C21 C22 1.501(7) . ? C22 N2 1.330(7) . ? C22 C23 1.382(7) . ? C23 C24 1.392(8) . ? C23 H23 0.9500 . ? C24 C25 1.377(9) . ? C24 H24 0.9500 . ? C25 C26 1.395(7) . ? C25 H25 0.9500 . ? C26 N2 1.349(7) . ? C26 C27 1.495(8) . ? C27 O5 1.238(7) . ? C27 N3 1.337(7) . ? N3 C28 1.470(8) . ? C28 C29 1.523(8) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 O6 1.422(7) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? O6 C30 1.427(7) . ? C30 C31 1.514(9) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 O7 1.425(7) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? O7 C32 1.436(7) . ? C32 C33 1.537(8) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 O8 1.423(6) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? O8 C34 1.424(6) . ? C34 C35 1.525(6) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 P2 1.831(5) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? P2 C42 1.816(5) . ? P2 C36 1.820(4) . ? C36 C41 1.380(7) . ? C36 C37 1.400(6) . ? C37 C38 1.393(7) . ? C37 H37 0.9500 . ? C38 C39 1.377(9) . ? C38 H38 0.9500 . ? C39 C40 1.376(9) . ? C39 H39 0.9500 . ? C40 C41 1.398(7) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 C47 1.383(7) . ? C42 C43 1.398(7) . ? C43 C44 1.390(7) . ? C43 H43 0.9500 . ? C44 C45 1.398(9) . ? C44 H44 0.9500 . ? C45 C46 1.349(9) . ? C45 H45 0.9500 . ? C46 C47 1.388(7) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C48 C49 1.199(6) . ? C49 C50 1.432(6) . ? C50 C51 1.392(7) . ? C50 C55 1.397(7) . ? C51 C52 1.390(8) . ? C51 H51 0.9500 . ? C52 C53 1.390(7) . ? C52 H52 0.9500 . ? C53 C54 1.366(7) . ? C53 C56 1.426(7) . ? C54 C55 1.382(7) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? C56 N4 1.116(7) . ? C57 C58 1.084(8) . ? C58 C59 1.448(8) . ? C59 C60 1.389(9) . ? C59 C64 1.392(9) . ? C60 C61 1.391(9) . ? C60 H60 0.9500 . ? C61 C62 1.427(12) . ? C61 H61 0.9500 . ? C62 C63 1.424(11) . ? C62 C65 1.453(9) . ? C63 C64 1.331(9) . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? C65 N5 1.119(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C48 Pt1 C57 175.40(17) . . ? C48 Pt1 P1 90.57(13) . . ? C57 Pt1 P1 86.21(10) . . ? C48 Pt1 P2 91.21(13) . . ? C57 Pt1 P2 92.16(11) . . ? P1 Pt1 P2 177.07(4) . . ? N2 Pd1 N4 178.8(2) . . ? N2 Pd1 N3 81.67(19) . . ? N4 Pd1 N3 97.2(2) . . ? N2 Pd1 N1 80.75(17) . . ? N4 Pd1 N1 100.40(18) . . ? N3 Pd1 N1 162.25(17) . . ? C7 P1 C1 106.6(2) . . ? C7 P1 C13 102.36(19) . . ? C1 P1 C13 101.7(2) . . ? C7 P1 Pt1 107.94(14) . . ? C1 P1 Pt1 117.81(16) . . ? C13 P1 Pt1 118.79(15) . . ? C2 C1 C6 119.5(5) . . ? C2 C1 P1 120.4(4) . . ? C6 C1 P1 119.8(4) . . ? C1 C2 C3 118.9(6) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C4 C3 C2 121.4(8) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C5 C4 C3 119.1(7) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C6 C5 C4 120.2(7) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C1 120.9(6) . . ? C5 C6 H6 119.6 . . ? C1 C6 H6 119.6 . . ? C12 C7 C8 120.3(5) . . ? C12 C7 P1 118.5(4) . . ? C8 C7 P1 121.0(4) . . ? C7 C8 C9 117.7(6) . . ? C7 C8 H8 121.1 . . ? C9 C8 H8 121.1 . . ? C10 C9 C8 120.6(6) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C11 C10 C9 120.1(5) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 121.5(7) . . ? C10 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C11 C12 C7 119.7(6) . . ? C11 C12 H12 120.1 . . ? C7 C12 H12 120.1 . . ? C14 C13 P1 113.7(3) . . ? C14 C13 H13A 108.8 . . ? P1 C13 H13A 108.8 . . ? C14 C13 H13B 108.8 . . ? P1 C13 H13B 108.8 . . ? H13A C13 H13B 107.7 . . ? O1 C14 C13 106.8(3) . . ? O1 C14 H14A 110.4 . . ? C13 C14 H14A 110.4 . . ? O1 C14 H14B 110.4 . . ? C13 C14 H14B 110.4 . . ? H14A C14 H14B 108.6 . . ? C15 O1 C14 111.4(3) . . ? O1 C15 C16 109.9(4) . . ? O1 C15 H15A 109.7 . . ? C16 C15 H15A 109.7 . . ? O1 C15 H15B 109.7 . . ? C16 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? O2 C16 C15 110.6(4) . . ? O2 C16 H16A 109.5 . . ? C15 C16 H16A 109.5 . . ? O2 C16 H16B 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? C16 O2 C17 109.7(4) . . ? O2 C17 C18 109.2(4) . . ? O2 C17 H17A 109.8 . . ? C18 C17 H17A 109.8 . . ? O2 C17 H17B 109.8 . . ? C18 C17 H17B 109.8 . . ? H17A C17 H17B 108.3 . . ? O3 C18 C17 108.5(4) . . ? O3 C18 H18A 110.0 . . ? C17 C18 H18A 110.0 . . ? O3 C18 H18B 110.0 . . ? C17 C18 H18B 110.0 . . ? H18A C18 H18B 108.4 . . ? C19 O3 C18 111.4(4) . . ? O3 C19 C20 107.9(4) . . ? O3 C19 H19A 110.1 . . ? C20 C19 H19A 110.1 . . ? O3 C19 H19B 110.1 . . ? C20 C19 H19B 110.1 . . ? H19A C19 H19B 108.4 . . ? N1 C20 C19 110.3(4) . . ? N1 C20 H20A 109.6 . . ? C19 C20 H20A 109.6 . . ? N1 C20 H20B 109.6 . . ? C19 C20 H20B 109.6 . . ? H20A C20 H20B 108.1 . . ? C21 N1 C20 120.0(4) . . ? C21 N1 Pd1 114.4(3) . . ? C20 N1 Pd1 125.2(3) . . ? O4 C21 N1 126.7(5) . . ? O4 C21 C22 120.2(4) . . ? N1 C21 C22 113.0(4) . . ? N2 C22 C23 119.5(5) . . ? N2 C22 C21 113.0(4) . . ? C23 C22 C21 127.5(5) . . ? C22 C23 C24 118.4(5) . . ? C22 C23 H23 120.8 . . ? C24 C23 H23 120.8 . . ? C25 C24 C23 121.0(5) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C24 C25 C26 118.8(5) . . ? C24 C25 H25 120.6 . . ? C26 C25 H25 120.6 . . ? N2 C26 C25 118.4(5) . . ? N2 C26 C27 113.5(4) . . ? C25 C26 C27 128.0(5) . . ? C22 N2 C26 124.0(4) . . ? C22 N2 Pd1 118.7(3) . . ? C26 N2 Pd1 117.3(3) . . ? O5 C27 N3 127.3(6) . . ? O5 C27 C26 119.6(5) . . ? N3 C27 C26 113.1(5) . . ? C27 N3 C28 119.8(5) . . ? C27 N3 Pd1 114.3(4) . . ? C28 N3 Pd1 124.9(4) . . ? N3 C28 C29 110.5(5) . . ? N3 C28 H28A 109.6 . . ? C29 C28 H28A 109.6 . . ? N3 C28 H28B 109.6 . . ? C29 C28 H28B 109.6 . . ? H28A C28 H28B 108.1 . . ? O6 C29 C28 106.5(5) . . ? O6 C29 H29A 110.4 . . ? C28 C29 H29A 110.4 . . ? O6 C29 H29B 110.4 . . ? C28 C29 H29B 110.4 . . ? H29A C29 H29B 108.6 . . ? C29 O6 C30 111.3(5) . . ? O6 C30 C31 110.2(5) . . ? O6 C30 H30A 109.6 . . ? C31 C30 H30A 109.6 . . ? O6 C30 H30B 109.6 . . ? C31 C30 H30B 109.6 . . ? H30A C30 H30B 108.1 . . ? O7 C31 C30 112.1(5) . . ? O7 C31 H31A 109.2 . . ? C30 C31 H31A 109.2 . . ? O7 C31 H31B 109.2 . . ? C30 C31 H31B 109.2 . . ? H31A C31 H31B 107.9 . . ? C31 O7 C32 109.2(4) . . ? O7 C32 C33 113.5(5) . . ? O7 C32 H32A 108.9 . . ? C33 C32 H32A 108.9 . . ? O7 C32 H32B 108.9 . . ? C33 C32 H32B 108.9 . . ? H32A C32 H32B 107.7 . . ? O8 C33 C32 109.8(5) . . ? O8 C33 H33A 109.7 . . ? C32 C33 H33A 109.7 . . ? O8 C33 H33B 109.7 . . ? C32 C33 H33B 109.7 . . ? H33A C33 H33B 108.2 . . ? C33 O8 C34 111.1(4) . . ? O8 C34 C35 106.0(4) . . ? O8 C34 H34A 110.5 . . ? C35 C34 H34A 110.5 . . ? O8 C34 H34B 110.5 . . ? C35 C34 H34B 110.5 . . ? H34A C34 H34B 108.7 . . ? C34 C35 P2 120.2(3) . . ? C34 C35 H35A 107.3 . . ? P2 C35 H35A 107.3 . . ? C34 C35 H35B 107.3 . . ? P2 C35 H35B 107.3 . . ? H35A C35 H35B 106.9 . . ? C42 P2 C36 104.6(2) . . ? C42 P2 C35 107.0(2) . . ? C36 P2 C35 100.1(2) . . ? C42 P2 Pt1 117.45(15) . . ? C36 P2 Pt1 109.01(15) . . ? C35 P2 Pt1 116.70(14) . . ? C41 C36 C37 119.9(4) . . ? C41 C36 P2 117.9(4) . . ? C37 C36 P2 122.2(4) . . ? C38 C37 C36 119.2(5) . . ? C38 C37 H37 120.4 . . ? C36 C37 H37 120.4 . . ? C39 C38 C37 120.7(5) . . ? C39 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C40 C39 C38 120.0(5) . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C39 C40 C41 120.1(6) . . ? C39 C40 H40 119.9 . . ? C41 C40 H40 119.9 . . ? C36 C41 C40 120.0(5) . . ? C36 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? C47 C42 C43 118.6(4) . . ? C47 C42 P2 122.7(4) . . ? C43 C42 P2 118.7(4) . . ? C44 C43 C42 120.5(5) . . ? C44 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? C43 C44 C45 119.3(5) . . ? C43 C44 H44 120.4 . . ? C45 C44 H44 120.4 . . ? C46 C45 C44 120.2(5) . . ? C46 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? C45 C46 C47 121.0(6) . . ? C45 C46 H46 119.5 . . ? C47 C46 H46 119.5 . . ? C42 C47 C46 120.4(5) . . ? C42 C47 H47 119.8 . . ? C46 C47 H47 119.8 . . ? C49 C48 Pt1 177.1(4) . . ? C48 C49 C50 177.7(5) . . ? C51 C50 C55 118.9(5) . . ? C51 C50 C49 120.9(5) . . ? C55 C50 C49 120.2(4) . . ? C52 C51 C50 120.3(5) . . ? C52 C51 H51 119.8 . . ? C50 C51 H51 119.8 . . ? C51 C52 C53 118.8(5) . . ? C51 C52 H52 120.6 . . ? C53 C52 H52 120.6 . . ? C54 C53 C52 121.6(5) . . ? C54 C53 C56 119.1(5) . . ? C52 C53 C56 119.3(5) . . ? C53 C54 C55 119.1(5) . . ? C53 C54 H54 120.4 . . ? C55 C54 H54 120.4 . . ? C54 C55 C50 120.9(5) . . ? C54 C55 H55 119.5 . . ? C50 C55 H55 119.5 . . ? N4 C56 C53 178.5(8) . . ? C56 N4 Pd1 178.1(6) . . ? C58 C57 Pt1 166.5(5) . . ? C57 C58 C59 176.6(7) . . ? C60 C59 C64 117.4(6) . . ? C60 C59 C58 120.2(6) . . ? C64 C59 C58 122.4(6) . . ? C59 C60 C61 123.8(7) . . ? C59 C60 H60 118.1 . . ? C61 C60 H60 118.1 . . ? C60 C61 C62 115.4(8) . . ? C60 C61 H61 122.3 . . ? C62 C61 H61 122.3 . . ? C63 C62 C61 121.5(6) . . ? C63 C62 C65 119.5(8) . . ? C61 C62 C65 118.9(7) . . ? C64 C63 C62 118.5(7) . . ? C64 C63 H63 120.8 . . ? C62 C63 H63 120.8 . . ? C63 C64 C59 123.4(7) . . ? C63 C64 H64 118.3 . . ? C59 C64 H64 118.3 . . ? N5 C65 C62 179.1(11) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 29.15 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.818 _refine_diff_density_min -1.415 _refine_diff_density_rms 0.193 _database_code_depnum_ccdc_archive 'CCDC 950509'