# 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_global data_e2673a #TrackingRef 's2673.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C61 H65 N5 O8 P2 Pt), C4 H10 O' _chemical_formula_sum 'C126 H140 N10 O17 P4 Pt2' _chemical_formula_weight 2580.54 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' _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 15.7504(7) _cell_length_b 19.2503(8) _cell_length_c 23.5828(10) _cell_angle_alpha 98.761(2) _cell_angle_beta 92.067(2) _cell_angle_gamma 107.459(2) _cell_volume 6715.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9977 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 26.01 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.276 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2636 _exptl_absorpt_coefficient_mu 2.190 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8798 _exptl_absorpt_correction_T_max 0.9175 _exptl_absorpt_process_details sadabs _exptl_special_details ; Owing to large disorder of the solvent present in the cavities of this structure, the SQUEEZE command has been applied. ; _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 125016 _diffrn_reflns_av_R_equivalents 0.1063 _diffrn_reflns_av_sigmaI/netI 0.1357 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 29.15 _reflns_number_total 35268 _reflns_number_gt 20826 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0856P)^2^+56.7234P] 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 35268 _refine_ls_number_parameters 1313 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1587 _refine_ls_R_factor_gt 0.0922 _refine_ls_wR_factor_ref 0.2329 _refine_ls_wR_factor_gt 0.2144 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.046 _refine_ls_shift/su_mean 0.001 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 0.77778(2) 0.29885(2) 0.764584(13) 0.02928(10) Uani 1 1 d . . . P1 P 0.81132(17) 0.19024(14) 0.76208(11) 0.0339(6) Uani 1 1 d . . . C1 C 0.7143(7) 0.1193(7) 0.7796(6) 0.054(3) Uani 1 1 d . . . C2 C 0.7049(10) 0.1046(8) 0.8345(7) 0.080(5) Uani 1 1 d . . . H2 H 0.7523 0.1297 0.8633 0.096 Uiso 1 1 calc R . . C3 C 0.6302(12) 0.0554(12) 0.8495(11) 0.131(9) Uani 1 1 d . . . H3 H 0.6230 0.0485 0.8883 0.157 Uiso 1 1 calc R . . C4 C 0.5653(11) 0.0161(11) 0.8048(12) 0.127(9) Uani 1 1 d . . . H4 H 0.5143 -0.0210 0.8131 0.152 Uiso 1 1 calc R . . C5 C 0.5722(9) 0.0289(13) 0.7496(11) 0.140(10) Uani 1 1 d . . . H5 H 0.5241 0.0040 0.7212 0.168 Uiso 1 1 calc R . . C6 C 0.6474(7) 0.0771(7) 0.7348(7) 0.065(4) Uani 1 1 d . . . H6 H 0.6550 0.0823 0.6957 0.078 Uiso 1 1 calc R . . C7 C 0.9057(6) 0.1933(5) 0.8105(4) 0.033(2) Uani 1 1 d . . . C8 C 0.9180(8) 0.1258(7) 0.8199(5) 0.054(3) Uani 1 1 d . . . H8 H 0.8768 0.0794 0.8029 0.065 Uiso 1 1 calc R . . C9 C 0.9927(11) 0.1306(10) 0.8550(6) 0.078(4) Uani 1 1 d . . . H9 H 1.0010 0.0859 0.8626 0.094 Uiso 1 1 calc R . . C10 C 1.0554(9) 0.1956(9) 0.8794(6) 0.067(4) Uani 1 1 d . . . H10 H 1.1065 0.1965 0.9026 0.081 Uiso 1 1 calc R . . C11 C 1.0409(9) 0.2582(9) 0.8690(5) 0.065(4) Uani 1 1 d . . . H11 H 1.0834 0.3043 0.8852 0.078 Uiso 1 1 calc R . . C12 C 0.9662(7) 0.2584(7) 0.8354(4) 0.047(3) Uani 1 1 d . . . H12 H 0.9578 0.3038 0.8300 0.056 Uiso 1 1 calc R . . C13 C 0.8356(7) 0.1481(5) 0.6929(4) 0.035(2) Uani 1 1 d . . . H13A H 0.8345 0.0969 0.6951 0.042 Uiso 1 1 calc R . . H13B H 0.7877 0.1453 0.6634 0.042 Uiso 1 1 calc R . . C14 C 0.9236(6) 0.1884(5) 0.6737(4) 0.033(2) Uani 1 1 d . . . H14A H 0.9274 0.2405 0.6728 0.040 Uiso 1 1 calc R . . H14B H 0.9731 0.1877 0.7005 0.040 Uiso 1 1 calc R . . O1 O 0.9293(5) 0.1518(4) 0.6180(3) 0.0470(18) Uani 1 1 d . . . C15 C 1.0122(7) 0.1655(7) 0.5984(5) 0.061(4) Uani 1 1 d . . . H15A H 1.0479 0.1438 0.6217 0.073 Uiso 1 1 calc R . . H15B H 1.0414 0.2196 0.6054 0.073 Uiso 1 1 calc R . . C16 C 1.0155(7) 0.1382(8) 0.5394(6) 0.074(5) Uani 1 1 d . . . H16A H 1.0277 0.1809 0.5188 0.089 Uiso 1 1 calc R . . H16B H 1.0678 0.1199 0.5366 0.089 Uiso 1 1 calc R . . O2 O 0.9459(5) 0.0853(5) 0.5105(4) 0.065(2) Uani 1 1 d . . . C17 C 0.9518(8) 0.0618(7) 0.4514(5) 0.056(3) Uani 1 1 d . . . H17A H 1.0008 0.0396 0.4469 0.067 Uiso 1 1 calc R . . H17B H 0.9655 0.1048 0.4312 0.067 Uiso 1 1 calc R . . C18 C 0.8670(8) 0.0072(6) 0.4258(5) 0.050(3) Uani 1 1 d . . . H18A H 0.8745 -0.0160 0.3866 0.059 Uiso 1 1 calc R . . H18B H 0.8480 -0.0320 0.4495 0.059 Uiso 1 1 calc R . . O3 O 0.8020(5) 0.0439(4) 0.4231(3) 0.0407(16) Uani 1 1 d . . . C19 C 0.7200(7) -0.0041(6) 0.3966(5) 0.044(2) Uani 1 1 d . . . H19A H 0.6959 -0.0437 0.4194 0.052 Uiso 1 1 calc R . . H19B H 0.7279 -0.0273 0.3575 0.052 Uiso 1 1 calc R . . C20 C 0.6567(6) 0.0402(5) 0.3929(4) 0.036(2) Uani 1 1 d . . . H20A H 0.5962 0.0057 0.3799 0.043 Uiso 1 1 calc R . . H20B H 0.6543 0.0667 0.4319 0.043 Uiso 1 1 calc R . . N1 N 0.6802(5) 0.0933(4) 0.3543(3) 0.0320(17) Uani 1 1 d . . . H1 H 0.7034 0.1406 0.3689 0.038 Uiso 1 1 calc R . . C21 C 0.6677(6) 0.0725(6) 0.2969(4) 0.036(2) Uani 1 1 d . . . O4 O 0.6357(5) 0.0080(4) 0.2727(3) 0.0492(19) Uani 1 1 d . . . C22 C 0.7001(7) 0.1348(6) 0.2626(4) 0.041(2) Uani 1 1 d . . . N2 N 0.7273(5) 0.2038(4) 0.2915(3) 0.0316(17) Uani 1 1 d . . . C23 C 0.7538(7) 0.2575(7) 0.2614(4) 0.043(3) Uani 1 1 d . . . C24 C 0.7526(8) 0.2449(7) 0.2022(5) 0.055(3) Uani 1 1 d . . . H24 H 0.7716 0.2853 0.1821 0.066 Uiso 1 1 calc R . . C25 C 0.7242(10) 0.1747(8) 0.1729(5) 0.070(4) Uani 1 1 d . . . H25 H 0.7243 0.1655 0.1321 0.084 Uiso 1 1 calc R . . C26 C 0.6947(8) 0.1161(7) 0.2029(5) 0.056(3) Uani 1 1 d . . . H26 H 0.6722 0.0662 0.1838 0.067 Uiso 1 1 calc R . . C27 C 0.7866(6) 0.3349(6) 0.2947(4) 0.039(2) Uani 1 1 d . . . O5 O 0.8141(5) 0.3883(4) 0.2702(3) 0.055(2) Uani 1 1 d . . . N3 N 0.7844(5) 0.3426(5) 0.3516(3) 0.0385(19) Uani 1 1 d . . . H3A H 0.7630 0.3028 0.3671 0.046 Uiso 1 1 calc R . . C28 C 0.8158(6) 0.4137(5) 0.3889(5) 0.041(2) Uani 1 1 d . . . H28A H 0.8721 0.4433 0.3756 0.049 Uiso 1 1 calc R . . H28B H 0.8292 0.4062 0.4284 0.049 Uiso 1 1 calc R . . C29 C 0.7492(7) 0.4569(6) 0.3905(5) 0.049(3) Uani 1 1 d . . . H29A H 0.7776 0.5079 0.4114 0.059 Uiso 1 1 calc R . . H29B H 0.7291 0.4596 0.3509 0.059 Uiso 1 1 calc R . . O6 O 0.6744(5) 0.4203(4) 0.4192(3) 0.0434(17) Uani 1 1 d . . . C30 C 0.6089(8) 0.4569(7) 0.4243(5) 0.055(3) Uani 1 1 d . . . H30A H 0.5859 0.4604 0.3855 0.066 Uiso 1 1 calc R . . H30B H 0.6355 0.5076 0.4461 0.066 Uiso 1 1 calc R . . C31 C 0.5338(8) 0.4144(8) 0.4549(5) 0.054(3) Uani 1 1 d . . . H31A H 0.4827 0.4340 0.4521 0.065 Uiso 1 1 calc R . . H31B H 0.5138 0.3617 0.4365 0.065 Uiso 1 1 calc R . . O7 O 0.5622(5) 0.4206(4) 0.5126(3) 0.0504(19) Uani 1 1 d . . . C32 C 0.5003(7) 0.3798(8) 0.5440(5) 0.063(4) Uani 1 1 d . . . H32A H 0.4886 0.3271 0.5275 0.076 Uiso 1 1 calc R . . H32B H 0.4440 0.3915 0.5375 0.076 Uiso 1 1 calc R . . C33 C 0.5184(7) 0.3874(8) 0.6040(6) 0.064(4) Uani 1 1 d . . . H33A H 0.4967 0.4276 0.6229 0.077 Uiso 1 1 calc R . . H33B H 0.4828 0.3412 0.6162 0.077 Uiso 1 1 calc R . . O8 O 0.6053(4) 0.4020(4) 0.6244(3) 0.0392(16) Uani 1 1 d . . . C34 C 0.6205(6) 0.3887(5) 0.6810(4) 0.033(2) Uani 1 1 d . . . H34A H 0.6134 0.3356 0.6799 0.040 Uiso 1 1 calc R . . H34B H 0.5764 0.4018 0.7058 0.040 Uiso 1 1 calc R . . C35 C 0.7136(6) 0.4345(5) 0.7054(4) 0.031(2) Uani 1 1 d . . . H35A H 0.7169 0.4873 0.7128 0.037 Uiso 1 1 calc R . . H35B H 0.7563 0.4284 0.6767 0.037 Uiso 1 1 calc R . . P2 P 0.74616(16) 0.40858(13) 0.77200(10) 0.0295(5) Uani 1 1 d . . . C36 C 0.6625(6) 0.4211(6) 0.8204(4) 0.037(2) Uani 1 1 d . . . C37 C 0.6056(7) 0.3599(7) 0.8401(4) 0.049(3) Uani 1 1 d . . . H37 H 0.6119 0.3123 0.8286 0.059 Uiso 1 1 calc R . . C38 C 0.5401(7) 0.3680(8) 0.8763(5) 0.060(3) Uani 1 1 d . . . H38 H 0.5028 0.3265 0.8902 0.072 Uiso 1 1 calc R . . C39 C 0.5299(9) 0.4362(9) 0.8918(6) 0.073(4) Uani 1 1 d . . . H39 H 0.4840 0.4418 0.9154 0.088 Uiso 1 1 calc R . . C40 C 0.5865(9) 0.4977(8) 0.8729(6) 0.068(4) Uani 1 1 d . . . H40 H 0.5805 0.5453 0.8848 0.082 Uiso 1 1 calc R . . C41 C 0.6514(8) 0.4891(6) 0.8367(5) 0.050(3) Uani 1 1 d . . . H41 H 0.6886 0.5308 0.8231 0.060 Uiso 1 1 calc R . . C42 C 0.8475(7) 0.4818(6) 0.8004(5) 0.045(3) Uani 1 1 d . . . C43 C 0.9123(8) 0.5067(7) 0.7650(6) 0.064(4) Uani 1 1 d . . . H43 H 0.9009 0.4878 0.7249 0.077 Uiso 1 1 calc R . . C44 C 0.9941(10) 0.5585(8) 0.7850(8) 0.085(5) Uani 1 1 d . . . H44 H 1.0371 0.5758 0.7590 0.102 Uiso 1 1 calc R . . C45 C 1.0115(10) 0.5835(10) 0.8413(9) 0.094(5) Uani 1 1 d . . . H45 H 1.0685 0.6178 0.8547 0.113 Uiso 1 1 calc R . . C46 C 0.9538(10) 0.5631(8) 0.8795(7) 0.083(3) Uani 1 1 d . . . H46 H 0.9679 0.5866 0.9186 0.100 Uiso 1 1 calc R . . C47 C 0.8745(10) 0.5090(8) 0.8636(7) 0.083(3) Uani 1 1 d . . . H47 H 0.8372 0.4889 0.8917 0.100 Uiso 1 1 calc R . . C48 C 0.7806(8) 0.3043(7) 0.8504(5) 0.051(3) Uani 1 1 d . . . C49 C 0.7823(10) 0.2999(7) 0.9000(5) 0.066(4) Uani 1 1 d . . . C50 C 0.7895(6) 0.2925(5) 0.9586(2) 0.066(4) Uani 1 1 d G . . C51 C 0.8645(5) 0.2783(5) 0.9806(3) 0.066(4) Uani 1 1 d G . . H51 H 0.9107 0.2747 0.9566 0.081 Uiso 1 1 calc R . . C52 C 0.8719(5) 0.2693(5) 1.0378(3) 0.066(4) Uani 1 1 d G . . H52 H 0.9231 0.2596 1.0528 0.081 Uiso 1 1 calc R . . N4 N 0.8043(6) 0.2745(4) 1.0729(2) 0.066(4) Uani 1 1 d G . . C53 C 0.7293(5) 0.2887(5) 1.0509(3) 0.066(4) Uani 1 1 d G . . H53 H 0.6831 0.2923 1.0749 0.081 Uiso 1 1 calc R . . C54 C 0.7219(5) 0.2977(5) 0.9937(3) 0.066(4) Uani 1 1 d G . . H54 H 0.6707 0.3074 0.9786 0.081 Uiso 1 1 calc R . . C55 C 0.7723(5) 0.2869(4) 0.6787(3) 0.0196(16) Uani 1 1 d . . . C56 C 0.7664(5) 0.2781(5) 0.6269(3) 0.0242(18) Uani 1 1 d . . . C57 C 0.7592(5) 0.2662(5) 0.5653(3) 0.0223(17) Uani 1 1 d . . . C58 C 0.7984(6) 0.2178(5) 0.5341(4) 0.0269(18) Uani 1 1 d . . . H58 H 0.8306 0.1923 0.5533 0.032 Uiso 1 1 calc R . . C59 C 0.7890(6) 0.2079(6) 0.4744(4) 0.037(2) Uani 1 1 d . . . H59 H 0.8169 0.1758 0.4537 0.045 Uiso 1 1 calc R . . N5 N 0.7438(6) 0.2404(5) 0.4442(3) 0.040(2) Uani 1 1 d . . . C60 C 0.7055(7) 0.2853(5) 0.4744(4) 0.037(2) Uani 1 1 d . . . H60 H 0.6702 0.3070 0.4537 0.045 Uiso 1 1 calc R . . C61 C 0.7138(6) 0.3025(5) 0.5340(4) 0.0275(19) Uani 1 1 d . . . H61 H 0.6892 0.3381 0.5532 0.033 Uiso 1 1 calc R . . C62 C 0.3604(6) 0.1716(5) 0.8460(3) 0.053(3) Uani 1 1 d G . . C63 C 0.4494(6) 0.1737(5) 0.8477(4) 0.072(4) Uani 1 1 d G . . H63 H 0.4822 0.1831 0.8151 0.087 Uiso 1 1 calc R . . C64 C 0.4905(5) 0.1621(6) 0.8970(5) 0.112(7) Uani 1 1 d G . . H64 H 0.5514 0.1635 0.8981 0.134 Uiso 1 1 calc R . . C65 C 0.4426(8) 0.1484(7) 0.9446(4) 0.112(7) Uani 1 1 d G . . H65 H 0.4706 0.1405 0.9783 0.120 Uiso 1 1 calc R . . C66 C 0.3535(8) 0.1463(6) 0.9429(4) 0.112(7) Uani 1 1 d G . . H66 H 0.3207 0.1370 0.9754 0.120 Uiso 1 1 calc R . . C67 C 0.3124(5) 0.1579(6) 0.8936(4) 0.112(7) Uani 1 1 d G . . H67 H 0.2516 0.1565 0.8924 0.120 Uiso 1 1 calc R . . Pt2 Pt 0.28278(2) 0.30710(2) 0.793011(13) 0.02971(10) Uani 1 1 d . . . P3 P 0.30350(17) 0.19184(14) 0.78442(10) 0.0328(5) Uani 1 1 d . . . C68 C 0.2012(6) 0.1153(5) 0.7670(5) 0.041(3) Uani 1 1 d . . . C69 C 0.1995(8) 0.0437(6) 0.7736(6) 0.056(3) Uani 1 1 d . . . H69 H 0.2512 0.0366 0.7905 0.067 Uiso 1 1 calc R . . C70 C 0.1263(9) -0.0155(7) 0.7565(7) 0.071(4) Uani 1 1 d . . . H70 H 0.1275 -0.0633 0.7613 0.085 Uiso 1 1 calc R . . C71 C 0.0517(8) -0.0070(7) 0.7325(7) 0.070(4) Uani 1 1 d . . . H71 H -0.0002 -0.0485 0.7214 0.084 Uiso 1 1 calc R . . C72 C 0.0512(9) 0.0638(8) 0.7242(6) 0.065(4) Uani 1 1 d . . . H72 H -0.0007 0.0701 0.7067 0.078 Uiso 1 1 calc R . . C73 C 0.1257(7) 0.1235(6) 0.7414(5) 0.049(3) Uani 1 1 d . . . H73 H 0.1252 0.1711 0.7356 0.059 Uiso 1 1 calc R . . C74 C 0.3642(6) 0.1711(5) 0.7226(4) 0.036(2) Uani 1 1 d . . . H74A H 0.3826 0.1272 0.7271 0.044 Uiso 1 1 calc R . . H74B H 0.3226 0.1576 0.6874 0.044 Uiso 1 1 calc R . . C75 C 0.4480(7) 0.2337(5) 0.7135(4) 0.040(2) Uani 1 1 d . . . H75A H 0.4348 0.2813 0.7184 0.048 Uiso 1 1 calc R . . H75B H 0.4974 0.2381 0.7423 0.048 Uiso 1 1 calc R . . O9 O 0.4738(4) 0.2174(4) 0.6567(3) 0.0375(16) Uani 1 1 d . . . C76 C 0.5252(6) 0.1668(6) 0.6509(5) 0.039(2) Uani 1 1 d . . . H76A H 0.4901 0.1188 0.6605 0.047 Uiso 1 1 calc R . . H76B H 0.5804 0.1868 0.6774 0.047 Uiso 1 1 calc R . . C77 C 0.5484(6) 0.1567(6) 0.5898(5) 0.049(3) Uani 1 1 d . . . H77A H 0.5688 0.2054 0.5773 0.059 Uiso 1 1 calc R . . H77B H 0.5978 0.1348 0.5871 0.059 Uiso 1 1 calc R . . O10 O 0.4739(4) 0.1104(4) 0.5537(3) 0.0459(18) Uani 1 1 d . . . C78 C 0.4905(8) 0.1067(8) 0.4951(5) 0.057(3) Uani 1 1 d . . . H78A H 0.5473 0.0956 0.4895 0.068 Uiso 1 1 calc R . . H78B H 0.4964 0.1551 0.4835 0.068 Uiso 1 1 calc R . . C79 C 0.4147(8) 0.0472(8) 0.4579(5) 0.060(3) Uani 1 1 d . . . H79A H 0.4329 0.0377 0.4184 0.072 Uiso 1 1 calc R . . H79B H 0.4020 0.0008 0.4738 0.072 Uiso 1 1 calc R . . O11 O 0.3377(5) 0.0687(4) 0.4557(3) 0.0439(17) Uani 1 1 d . . . C80 C 0.2655(7) 0.0147(5) 0.4224(5) 0.042(2) Uani 1 1 d . . . H80A H 0.2467 -0.0294 0.4413 0.050 Uiso 1 1 calc R . . H80B H 0.2842 -0.0005 0.3840 0.050 Uiso 1 1 calc R . . C81 C 0.1887(7) 0.0444(5) 0.4156(4) 0.038(2) Uani 1 1 d . . . H81A H 0.1351 0.0029 0.3990 0.045 Uiso 1 1 calc R . . H81B H 0.1761 0.0653 0.4542 0.045 Uiso 1 1 calc R . . N6 N 0.2036(5) 0.1010(4) 0.3794(3) 0.0357(18) Uani 1 1 d . . . H6A H 0.2197 0.1479 0.3954 0.043 Uiso 1 1 calc R . . C82 C 0.1931(6) 0.0826(5) 0.3224(4) 0.032(2) Uani 1 1 d . . . O12 O 0.1717(6) 0.0180(4) 0.2967(3) 0.052(2) Uani 1 1 d . . . C83 C 0.2082(7) 0.1448(5) 0.2888(4) 0.036(2) Uani 1 1 d . . . N7 N 0.2292(5) 0.2139(4) 0.3196(3) 0.0304(17) Uani 1 1 d . . . C84 C 0.2456(7) 0.2703(5) 0.2892(4) 0.036(2) Uani 1 1 d . . . C85 C 0.2394(9) 0.2594(6) 0.2303(4) 0.054(3) Uani 1 1 d . . . H85 H 0.2510 0.3006 0.2108 0.065 Uiso 1 1 calc R . . C86 C 0.2164(9) 0.1892(6) 0.1993(5) 0.060(4) Uani 1 1 d . . . H86 H 0.2113 0.1811 0.1584 0.073 Uiso 1 1 calc R . . C87 C 0.2007(9) 0.1296(7) 0.2293(5) 0.057(3) Uani 1 1 d . . . H87 H 0.1853 0.0801 0.2093 0.069 Uiso 1 1 calc R . . C88 C 0.2671(7) 0.3453(5) 0.3231(4) 0.038(2) Uani 1 1 d . . . O13 O 0.2886(6) 0.3998(4) 0.2974(3) 0.062(2) Uani 1 1 d . . . N8 N 0.2676(5) 0.3526(4) 0.3796(3) 0.0336(18) Uani 1 1 d . . . H8A H 0.2528 0.3124 0.3953 0.040 Uiso 1 1 calc R . . C89 C 0.2914(7) 0.4240(5) 0.4172(4) 0.039(2) Uani 1 1 d . . . H89A H 0.3415 0.4588 0.4018 0.047 Uiso 1 1 calc R . . H89B H 0.3127 0.4186 0.4558 0.047 Uiso 1 1 calc R . . C90 C 0.2145(8) 0.4573(6) 0.4235(5) 0.048(3) Uani 1 1 d . . . H90A H 0.2374 0.5093 0.4435 0.058 Uiso 1 1 calc R . . H90B H 0.1864 0.4565 0.3851 0.058 Uiso 1 1 calc R . . O14 O 0.1503(5) 0.4146(4) 0.4562(3) 0.0432(17) Uani 1 1 d . . . C91 C 0.0743(8) 0.4372(6) 0.4611(5) 0.049(3) Uani 1 1 d . . . H91A H 0.0441 0.4311 0.4223 0.059 Uiso 1 1 calc R . . H91B H 0.0922 0.4902 0.4783 0.059 Uiso 1 1 calc R . . C92 C 0.0107(7) 0.3935(7) 0.4977(5) 0.047(3) Uani 1 1 d . . . H92A H -0.0482 0.4012 0.4923 0.057 Uiso 1 1 calc R . . H92B H 0.0028 0.3402 0.4857 0.057 Uiso 1 1 calc R . . O15 O 0.0435(4) 0.4155(4) 0.5570(3) 0.0426(17) Uani 1 1 d . . . C93 C -0.0226(6) 0.3842(6) 0.5935(5) 0.044(3) Uani 1 1 d . . . H93A H -0.0456 0.3300 0.5811 0.053 Uiso 1 1 calc R . . H93B H -0.0732 0.4043 0.5903 0.053 Uiso 1 1 calc R . . C94 C 0.0155(7) 0.4013(7) 0.6546(5) 0.047(3) Uani 1 1 d . . . H94A H 0.0531 0.4537 0.6641 0.056 Uiso 1 1 calc R . . H94B H -0.0332 0.3934 0.6805 0.056 Uiso 1 1 calc R . . O16 O 0.0681(4) 0.3543(4) 0.6624(3) 0.0403(16) Uani 1 1 d . . . C95 C 0.0996(8) 0.3601(6) 0.7217(5) 0.048(3) Uani 1 1 d . . . H95A H 0.1120 0.3141 0.7274 0.058 Uiso 1 1 calc R . . H95B H 0.0533 0.3673 0.7472 0.058 Uiso 1 1 calc R . . C96 C 0.1857(7) 0.4264(6) 0.7368(4) 0.044(3) Uani 1 1 d . . . H96A H 0.1685 0.4718 0.7472 0.052 Uiso 1 1 calc R . . H96B H 0.2187 0.4312 0.7019 0.052 Uiso 1 1 calc R . . P4 P 0.26094(19) 0.42106(14) 0.79534(10) 0.0363(6) Uani 1 1 d . . . C97 C 0.2263(10) 0.4590(7) 0.8630(5) 0.058(3) Uani 1 1 d . . . C98 C 0.2891(10) 0.4883(6) 0.9115(5) 0.058(3) Uani 1 1 d . . . H98 H 0.3504 0.4934 0.9076 0.069 Uiso 1 1 calc R . . C99 C 0.2617(9) 0.5097(6) 0.9649(5) 0.058(3) Uani 1 1 d . . . H99 H 0.3034 0.5283 0.9979 0.069 Uiso 1 1 calc R . . C100 C 0.1743(9) 0.5033(6) 0.9690(5) 0.058(3) Uani 1 1 d . . . H100 H 0.1553 0.5157 1.0059 0.069 Uiso 1 1 calc R . . C101 C 0.1123(13) 0.4801(10) 0.9228(7) 0.096(5) Uani 1 1 d . . . H101 H 0.0522 0.4792 0.9263 0.115 Uiso 1 1 calc R . . C102 C 0.1409(11) 0.4579(8) 0.8708(6) 0.077(4) Uani 1 1 d . . . H102 H 0.0983 0.4407 0.8382 0.093 Uiso 1 1 calc R . . C103 C 0.3595(8) 0.4943(6) 0.7822(5) 0.050(3) Uani 1 1 d . . . C104 C 0.4327(8) 0.4796(6) 0.7595(6) 0.056(3) Uani 1 1 d . . . H104 H 0.4355 0.4304 0.7549 0.067 Uiso 1 1 calc R . . C105 C 0.5012(9) 0.5333(8) 0.7435(7) 0.076(4) Uani 1 1 d . . . H105 H 0.5494 0.5209 0.7261 0.091 Uiso 1 1 calc R . . C106 C 0.5009(11) 0.6054(8) 0.7524(8) 0.093(6) Uani 1 1 d . . . H106 H 0.5511 0.6437 0.7448 0.112 Uiso 1 1 calc R . . C107 C 0.4257(13) 0.6215(8) 0.7727(9) 0.102(6) Uani 1 1 d . . . H107 H 0.4217 0.6701 0.7750 0.122 Uiso 1 1 calc R . . C108 C 0.3562(10) 0.5662(7) 0.7896(7) 0.077(4) Uani 1 1 d . . . H108 H 0.3069 0.5778 0.8060 0.092 Uiso 1 1 calc R . . C109 C 0.2904(7) 0.3180(6) 0.8786(4) 0.040(2) Uani 1 1 d . . . C110 C 0.2910(8) 0.3203(6) 0.9296(4) 0.047(3) Uani 1 1 d . . . C111 C 0.2904(7) 0.3224(5) 0.9910(3) 0.047(3) Uani 1 1 d G . . C112 C 0.3605(6) 0.3102(5) 1.0212(4) 0.047(3) Uani 1 1 d G . . H112 H 0.4106 0.3047 1.0021 0.065 Uiso 1 1 calc R . . C113 C 0.3571(5) 0.3063(5) 1.0795(4) 0.047(3) Uani 1 1 d G . . H113 H 0.4051 0.2979 1.1001 0.065 Uiso 1 1 calc R . . N9 N 0.2837(6) 0.3144(5) 1.1075(3) 0.047(3) Uani 1 1 d G . . C114 C 0.2136(5) 0.3266(5) 1.0773(3) 0.047(3) Uani 1 1 d G . . H114 H 0.1634 0.3322 1.0965 0.065 Uiso 1 1 calc R . . C115 C 0.2169(6) 0.3306(5) 1.0190(3) 0.075(4) Uani 1 1 d G . . H115 H 0.1690 0.3389 0.9984 0.090 Uiso 1 1 calc R . . C116 C 0.2716(7) 0.2931(5) 0.7071(4) 0.036(2) Uani 1 1 d . . . C117 C 0.2681(7) 0.2862(6) 0.6554(4) 0.037(2) Uani 1 1 d . . . C118 C 0.2609(6) 0.2729(5) 0.5934(4) 0.031(2) Uani 1 1 d . . . C119 C 0.3072(6) 0.2309(5) 0.5625(4) 0.034(2) Uani 1 1 d . . . H119 H 0.3443 0.2098 0.5823 0.041 Uiso 1 1 calc R . . C120 C 0.2993(7) 0.2198(5) 0.5029(4) 0.038(2) Uani 1 1 d . . . H120 H 0.3333 0.1924 0.4827 0.046 Uiso 1 1 calc R . . N10 N 0.2468(6) 0.2456(5) 0.4726(3) 0.0390(19) Uani 1 1 d . . . C121 C 0.2003(7) 0.2849(6) 0.5021(4) 0.039(2) Uani 1 1 d . . . H121 H 0.1612 0.3025 0.4808 0.047 Uiso 1 1 calc R . . C122 C 0.2055(7) 0.3014(5) 0.5611(4) 0.034(2) Uani 1 1 d . . . H122 H 0.1728 0.3312 0.5797 0.041 Uiso 1 1 calc R . . O17 O 0.5078(8) 0.8132(8) 0.7637(5) 0.046(4) Uani 0.50 1 d PD . . C123 C 0.5119(19) 0.8264(15) 0.8717(8) 0.075(8) Uani 0.50 1 d PD . . H12A H 0.5024 0.8747 0.8811 0.112 Uiso 0.50 1 calc PR . . H12B H 0.5460 0.8181 0.9042 0.112 Uiso 0.50 1 calc PR . . H12C H 0.4540 0.7876 0.8641 0.112 Uiso 0.50 1 calc PR . . C124 C 0.5633(13) 0.8244(13) 0.8189(7) 0.064(7) Uani 0.50 1 d PD . . H12D H 0.6125 0.8715 0.8225 0.077 Uiso 0.50 1 calc PR . . H12E H 0.5904 0.7840 0.8175 0.077 Uiso 0.50 1 calc PR . . C125 C 0.5525(12) 0.8151(12) 0.7105(7) 0.079(11) Uani 0.50 1 d PD . . H12F H 0.5918 0.7834 0.7096 0.095 Uiso 0.50 1 calc PR . . H12G H 0.5907 0.8663 0.7101 0.095 Uiso 0.50 1 calc PR . . C126 C 0.4870(14) 0.7890(14) 0.6571(7) 0.054(6) Uani 0.50 1 d PD . . H12H H 0.4466 0.7396 0.6585 0.081 Uiso 0.50 1 calc PR . . H12I H 0.5200 0.7873 0.6227 0.081 Uiso 0.50 1 calc PR . . H12J H 0.4523 0.8234 0.6557 0.081 Uiso 0.50 1 calc PR . . O18 O 0.0174(13) 0.7901(10) 0.7421(9) 0.106(6) Uani 0.50 1 d PD . . C127 C 0.019(2) 0.8123(15) 0.8492(10) 0.106(6) Uani 0.50 1 d PD . . H12K H 0.0766 0.8204 0.8700 0.158 Uiso 0.50 1 calc PR . . H12L H -0.0292 0.7945 0.8740 0.158 Uiso 0.50 1 calc PR . . H12M H 0.0157 0.8588 0.8386 0.158 Uiso 0.50 1 calc PR . . C128 C 0.007(2) 0.7552(13) 0.7953(10) 0.106(6) Uani 0.50 1 d PD . . H12N H 0.0516 0.7289 0.7980 0.127 Uiso 0.50 1 calc PR . . H12O H -0.0533 0.7185 0.7924 0.127 Uiso 0.50 1 calc PR . . C129 C 0.002(2) 0.7398(13) 0.6864(10) 0.106(6) Uani 0.50 1 d PD . . H12P H -0.0583 0.7040 0.6832 0.127 Uiso 0.50 1 calc PR . . H12Q H 0.0457 0.7116 0.6856 0.127 Uiso 0.50 1 calc PR . . C130 C 0.012(2) 0.7793(15) 0.6348(10) 0.106(6) Uani 0.50 1 d PD . . H13C H -0.0404 0.7954 0.6287 0.158 Uiso 0.50 1 calc PR . . H13D H 0.0171 0.7455 0.6004 0.158 Uiso 0.50 1 calc PR . . H13E H 0.0659 0.8224 0.6418 0.158 Uiso 0.50 1 calc PR . . 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 0.0404(2) 0.0297(2) 0.02192(16) 0.00873(14) 0.00523(15) 0.01469(17) P1 0.0372(13) 0.0339(14) 0.0389(12) 0.0212(11) 0.0096(11) 0.0154(12) C1 0.038(6) 0.057(8) 0.085(9) 0.039(7) 0.023(6) 0.029(6) C2 0.081(10) 0.060(9) 0.096(11) 0.028(8) 0.036(9) 0.005(8) C3 0.063(11) 0.136(18) 0.21(2) 0.126(18) 0.031(13) -0.001(11) C4 0.049(10) 0.115(16) 0.24(3) 0.112(18) 0.057(13) 0.015(10) C5 0.027(7) 0.18(2) 0.22(3) 0.13(2) -0.002(10) -0.006(10) C6 0.017(5) 0.050(8) 0.121(12) 0.043(8) -0.015(6) -0.014(5) C7 0.037(5) 0.025(5) 0.034(4) 0.010(4) 0.000(4) 0.003(4) C8 0.063(8) 0.042(7) 0.064(7) 0.017(6) -0.004(6) 0.024(6) C9 0.096(12) 0.100(13) 0.067(9) 0.035(9) 0.001(8) 0.064(11) C10 0.053(8) 0.098(12) 0.064(8) 0.028(8) 0.002(6) 0.036(8) C11 0.051(7) 0.090(11) 0.051(7) 0.016(7) -0.003(6) 0.016(7) C12 0.041(6) 0.064(8) 0.040(5) 0.023(5) 0.003(5) 0.015(6) C13 0.040(5) 0.019(5) 0.043(5) 0.003(4) 0.003(4) 0.007(4) C14 0.032(5) 0.032(6) 0.037(5) 0.005(4) 0.003(4) 0.012(4) O1 0.038(4) 0.047(5) 0.047(4) -0.007(3) 0.011(3) 0.008(4) C15 0.028(6) 0.063(9) 0.069(8) -0.016(7) 0.008(5) -0.007(6) C16 0.031(6) 0.085(11) 0.072(8) -0.034(8) 0.017(6) -0.010(7) O2 0.050(5) 0.066(6) 0.055(5) -0.014(4) 0.014(4) -0.006(4) C17 0.046(7) 0.063(8) 0.054(7) -0.008(6) 0.013(6) 0.017(6) C18 0.065(8) 0.049(7) 0.041(5) 0.004(5) 0.008(5) 0.029(6) O3 0.039(4) 0.035(4) 0.050(4) 0.005(3) 0.002(3) 0.015(3) C19 0.048(6) 0.034(6) 0.050(6) 0.014(5) 0.009(5) 0.012(5) C20 0.032(5) 0.023(5) 0.048(5) 0.005(4) 0.007(4) 0.001(4) N1 0.032(4) 0.025(4) 0.032(4) -0.007(3) -0.005(3) 0.005(4) C21 0.026(5) 0.044(7) 0.037(5) -0.004(5) 0.004(4) 0.013(5) O4 0.042(4) 0.036(5) 0.052(4) -0.017(4) -0.011(3) 0.000(4) C22 0.033(5) 0.064(8) 0.030(5) 0.004(5) 0.004(4) 0.023(5) N2 0.030(4) 0.038(5) 0.026(3) 0.009(3) 0.005(3) 0.006(4) C23 0.037(5) 0.070(8) 0.031(5) 0.019(5) 0.010(4) 0.023(5) C24 0.065(8) 0.066(9) 0.033(5) 0.015(6) 0.009(5) 0.017(7) C25 0.096(11) 0.086(11) 0.026(5) 0.011(6) 0.016(6) 0.025(9) C26 0.063(8) 0.067(9) 0.036(5) -0.006(6) 0.007(5) 0.025(7) C27 0.024(5) 0.060(7) 0.039(5) 0.021(5) 0.014(4) 0.012(5) O5 0.052(5) 0.057(5) 0.067(5) 0.042(4) 0.026(4) 0.015(4) N3 0.036(4) 0.044(5) 0.040(4) 0.016(4) 0.012(4) 0.014(4) C28 0.025(5) 0.024(6) 0.067(7) 0.012(5) 0.008(5) -0.005(4) C29 0.053(7) 0.040(7) 0.059(7) 0.022(5) 0.009(6) 0.013(6) O6 0.039(4) 0.035(4) 0.062(5) 0.016(3) 0.007(3) 0.016(3) C30 0.072(8) 0.073(9) 0.044(6) 0.026(6) 0.013(6) 0.048(7) C31 0.049(7) 0.080(9) 0.044(6) 0.015(6) -0.001(5) 0.035(7) O7 0.050(4) 0.057(5) 0.036(4) 0.011(4) -0.010(3) 0.004(4) C32 0.026(5) 0.102(11) 0.056(7) 0.028(7) -0.007(5) 0.005(6) C33 0.037(6) 0.087(10) 0.069(8) 0.040(8) -0.005(6) 0.009(6) O8 0.029(3) 0.051(5) 0.040(4) 0.019(3) 0.000(3) 0.012(3) C34 0.034(5) 0.032(6) 0.035(5) 0.009(4) 0.008(4) 0.013(4) C35 0.038(5) 0.021(5) 0.037(5) 0.006(4) 0.004(4) 0.013(4) P2 0.0298(12) 0.0241(13) 0.0321(11) 0.0021(10) 0.0040(10) 0.0060(10) C36 0.028(5) 0.052(7) 0.031(4) -0.008(4) -0.004(4) 0.019(5) C37 0.043(6) 0.056(8) 0.039(5) -0.001(5) 0.007(5) 0.005(6) C38 0.035(6) 0.073(9) 0.053(7) -0.006(6) 0.016(5) -0.004(6) C39 0.054(8) 0.101(12) 0.057(7) -0.012(8) 0.020(6) 0.023(8) C40 0.078(9) 0.072(10) 0.065(8) -0.007(7) 0.016(7) 0.047(8) C41 0.052(7) 0.036(7) 0.066(7) 0.007(5) 0.014(6) 0.018(6) C42 0.048(6) 0.036(7) 0.046(6) -0.004(5) -0.003(5) 0.011(5) C43 0.044(7) 0.050(8) 0.086(9) 0.001(7) 0.017(7) 0.000(6) C44 0.057(9) 0.052(10) 0.125(14) 0.004(9) 0.031(9) -0.012(7) C45 0.050(9) 0.084(13) 0.121(15) -0.005(11) -0.015(9) -0.006(8) C46 0.084(7) 0.049(6) 0.094(8) 0.012(6) 0.038(6) -0.017(5) C47 0.084(7) 0.049(6) 0.094(8) 0.012(6) 0.038(6) -0.017(5) C48 0.072(8) 0.058(8) 0.038(5) 0.023(5) 0.014(6) 0.033(7) C49 0.108(11) 0.059(9) 0.029(5) 0.003(5) -0.003(6) 0.028(8) C50 0.108(11) 0.059(9) 0.029(5) 0.003(5) -0.003(6) 0.028(8) C51 0.108(11) 0.059(9) 0.029(5) 0.003(5) -0.003(6) 0.028(8) C52 0.108(11) 0.059(9) 0.029(5) 0.003(5) -0.003(6) 0.028(8) N4 0.108(11) 0.059(9) 0.029(5) 0.003(5) -0.003(6) 0.028(8) C53 0.108(11) 0.059(9) 0.029(5) 0.003(5) -0.003(6) 0.028(8) C54 0.108(11) 0.059(9) 0.029(5) 0.003(5) -0.003(6) 0.028(8) C55 0.020(4) 0.021(5) 0.021(3) 0.002(3) 0.004(3) 0.012(4) C56 0.024(4) 0.032(5) 0.023(4) 0.007(4) 0.006(3) 0.017(4) C57 0.020(4) 0.028(5) 0.025(4) 0.010(3) 0.007(3) 0.013(4) C58 0.026(4) 0.027(5) 0.027(4) 0.000(4) -0.006(3) 0.010(4) C59 0.038(5) 0.045(6) 0.028(4) -0.004(4) 0.005(4) 0.016(5) N5 0.056(5) 0.042(5) 0.024(3) 0.001(3) 0.002(4) 0.021(4) C60 0.054(6) 0.037(6) 0.027(4) 0.007(4) -0.001(4) 0.024(5) C61 0.028(4) 0.031(5) 0.029(4) 0.010(4) 0.003(4) 0.015(4) C62 0.084(9) 0.043(7) 0.041(6) 0.004(5) 0.001(6) 0.033(7) C63 0.077(10) 0.069(10) 0.078(9) 0.014(8) -0.014(8) 0.036(8) C64 0.113(15) 0.118(16) 0.126(16) 0.016(12) -0.033(12) 0.075(13) C65 0.113(15) 0.118(16) 0.126(16) 0.016(12) -0.033(12) 0.075(13) C66 0.113(15) 0.118(16) 0.126(16) 0.016(12) -0.033(12) 0.075(13) C67 0.113(15) 0.118(16) 0.126(16) 0.016(12) -0.033(12) 0.075(13) Pt2 0.0406(2) 0.0278(2) 0.02148(16) 0.00238(14) 0.00253(15) 0.01258(17) P3 0.0416(14) 0.0274(14) 0.0323(11) 0.0056(10) 0.0108(11) 0.0140(12) C68 0.029(5) 0.030(6) 0.067(7) 0.012(5) 0.026(5) 0.008(4) C69 0.050(7) 0.026(6) 0.085(9) 0.010(6) 0.014(6) 0.000(5) C70 0.058(8) 0.024(7) 0.121(13) 0.003(7) 0.017(8) 0.000(6) C71 0.041(7) 0.043(8) 0.111(12) -0.001(7) 0.032(7) -0.004(6) C72 0.056(8) 0.065(9) 0.077(9) 0.016(7) 0.020(7) 0.020(7) C73 0.047(6) 0.037(7) 0.055(6) 0.007(5) 0.002(5) 0.002(5) C74 0.036(5) 0.034(6) 0.037(5) -0.002(4) 0.004(4) 0.010(5) C75 0.044(6) 0.029(6) 0.041(5) 0.004(4) 0.009(5) 0.003(5) O9 0.028(3) 0.035(4) 0.044(4) 0.006(3) 0.010(3) 0.001(3) C76 0.020(4) 0.035(6) 0.057(6) -0.005(5) -0.004(4) 0.007(4) C77 0.023(5) 0.048(7) 0.061(7) -0.010(5) 0.017(5) -0.003(5) O10 0.031(4) 0.052(5) 0.042(4) -0.002(3) 0.014(3) -0.003(3) C78 0.053(7) 0.092(10) 0.044(6) 0.017(6) 0.019(5) 0.045(7) C79 0.070(8) 0.074(9) 0.047(6) -0.006(6) 0.008(6) 0.044(8) O11 0.049(4) 0.039(4) 0.047(4) -0.002(3) 0.001(3) 0.024(4) C80 0.056(7) 0.022(6) 0.048(6) 0.006(5) -0.004(5) 0.014(5) C81 0.040(5) 0.023(5) 0.044(5) 0.011(4) 0.000(4) -0.003(4) N6 0.041(5) 0.030(5) 0.034(4) 0.010(3) 0.004(4) 0.005(4) C82 0.029(5) 0.022(6) 0.037(5) -0.002(4) -0.003(4) -0.001(4) O12 0.084(6) 0.016(4) 0.046(4) 0.003(3) -0.009(4) 0.003(4) C83 0.042(6) 0.026(6) 0.031(4) -0.003(4) -0.005(4) 0.003(5) N7 0.045(5) 0.016(4) 0.027(3) 0.006(3) 0.006(3) 0.003(3) C84 0.059(6) 0.026(5) 0.028(4) 0.009(4) 0.007(4) 0.016(5) C85 0.092(9) 0.043(7) 0.028(5) 0.012(5) 0.011(6) 0.019(7) C86 0.100(10) 0.041(7) 0.034(5) 0.007(5) 0.015(6) 0.010(7) C87 0.094(10) 0.038(7) 0.035(5) -0.003(5) -0.001(6) 0.018(7) C88 0.050(6) 0.030(6) 0.036(5) 0.013(4) 0.014(5) 0.012(5) O13 0.112(7) 0.027(4) 0.050(4) 0.020(4) 0.030(5) 0.019(4) N8 0.045(5) 0.021(4) 0.033(4) 0.005(3) 0.008(4) 0.008(4) C89 0.040(6) 0.023(6) 0.044(5) -0.007(4) 0.006(5) -0.002(5) C90 0.070(8) 0.034(6) 0.045(6) 0.013(5) 0.013(5) 0.020(6) O14 0.050(4) 0.035(4) 0.051(4) 0.011(3) 0.008(3) 0.019(4) C91 0.059(7) 0.050(7) 0.048(6) 0.010(5) 0.007(5) 0.032(6) C92 0.043(6) 0.050(7) 0.045(6) 0.004(5) -0.003(5) 0.010(5) O15 0.036(4) 0.043(5) 0.040(4) 0.004(3) -0.004(3) 0.001(3) C93 0.023(5) 0.050(7) 0.053(6) 0.008(5) -0.006(4) 0.002(5) C94 0.031(5) 0.054(7) 0.056(6) 0.010(5) 0.012(5) 0.015(5) O16 0.038(4) 0.033(4) 0.047(4) 0.000(3) -0.003(3) 0.009(3) C95 0.058(7) 0.038(7) 0.055(6) 0.023(5) 0.011(6) 0.015(6) C96 0.050(6) 0.037(6) 0.046(6) 0.018(5) 0.010(5) 0.011(5) P4 0.0481(15) 0.0290(15) 0.0319(12) -0.0009(10) -0.0037(11) 0.0157(12) C97 0.091(10) 0.043(7) 0.052(7) 0.004(5) 0.004(7) 0.041(7) C98 0.091(10) 0.043(7) 0.052(7) 0.004(5) 0.004(7) 0.041(7) C99 0.091(10) 0.043(7) 0.052(7) 0.004(5) 0.004(7) 0.041(7) C100 0.091(10) 0.043(7) 0.052(7) 0.004(5) 0.004(7) 0.041(7) C101 0.123(15) 0.100(14) 0.085(11) 0.019(10) 0.026(11) 0.063(12) C102 0.097(11) 0.072(10) 0.072(9) -0.005(7) 0.029(8) 0.046(9) C103 0.067(8) 0.034(7) 0.048(6) 0.005(5) -0.016(6) 0.018(6) C104 0.064(8) 0.028(6) 0.075(8) 0.019(6) 0.006(7) 0.007(6) C105 0.058(8) 0.064(10) 0.105(12) 0.036(9) 0.008(8) 0.006(7) C106 0.060(10) 0.044(10) 0.156(17) 0.028(10) -0.032(10) -0.015(8) C107 0.100(14) 0.033(9) 0.162(19) 0.028(10) -0.010(13) 0.003(9) C108 0.064(9) 0.045(9) 0.123(13) 0.016(8) -0.003(9) 0.021(7) C109 0.049(6) 0.044(6) 0.033(5) 0.005(4) 0.009(5) 0.026(5) C110 0.062(7) 0.049(7) 0.037(5) 0.008(5) 0.006(5) 0.029(6) C111 0.062(7) 0.049(7) 0.037(5) 0.008(5) 0.006(5) 0.029(6) C112 0.062(7) 0.049(7) 0.037(5) 0.008(5) 0.006(5) 0.029(6) C113 0.062(7) 0.049(7) 0.037(5) 0.008(5) 0.006(5) 0.029(6) N9 0.062(7) 0.049(7) 0.037(5) 0.008(5) 0.006(5) 0.029(6) C114 0.062(7) 0.049(7) 0.037(5) 0.008(5) 0.006(5) 0.029(6) C115 0.098(11) 0.059(9) 0.054(7) 0.001(6) 0.031(8) 0.005(8) C116 0.038(5) 0.026(6) 0.039(5) -0.003(4) -0.006(4) 0.007(4) C117 0.042(6) 0.034(6) 0.030(5) 0.004(4) -0.001(4) 0.004(5) C118 0.039(5) 0.018(5) 0.029(4) 0.003(4) 0.000(4) -0.001(4) C119 0.040(5) 0.030(6) 0.028(4) 0.003(4) -0.006(4) 0.008(4) C120 0.053(6) 0.031(6) 0.033(5) 0.002(4) 0.007(5) 0.016(5) N10 0.054(5) 0.038(5) 0.024(4) 0.003(3) 0.002(4) 0.014(4) C121 0.046(6) 0.044(6) 0.032(5) 0.015(4) 0.005(4) 0.015(5) C122 0.044(6) 0.025(5) 0.031(4) -0.002(4) 0.005(4) 0.012(5) O17 0.021(6) 0.065(10) 0.058(9) 0.014(8) 0.014(6) 0.020(7) C123 0.10(2) 0.058(18) 0.078(19) 0.027(15) 0.029(17) 0.039(17) C124 0.047(14) 0.023(13) 0.11(2) 0.005(13) -0.019(15) 0.003(11) C125 0.033(12) 0.017(12) 0.18(3) 0.000(15) 0.034(17) 0.010(10) C126 0.040(12) 0.072(17) 0.069(15) 0.028(13) 0.013(11) 0.035(12) O18 0.055(7) 0.055(9) 0.215(19) 0.058(9) 0.008(10) 0.012(7) C127 0.055(7) 0.055(9) 0.215(19) 0.058(9) 0.008(10) 0.012(7) C128 0.055(7) 0.055(9) 0.215(19) 0.058(9) 0.008(10) 0.012(7) C129 0.055(7) 0.055(9) 0.215(19) 0.058(9) 0.008(10) 0.012(7) C130 0.055(7) 0.055(9) 0.215(19) 0.058(9) 0.008(10) 0.012(7) _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 C55 1.999(7) . ? Pt1 C48 2.010(10) . ? Pt1 P2 2.295(2) . ? Pt1 P1 2.298(2) . ? P1 C13 1.815(9) . ? P1 C7 1.823(10) . ? P1 C1 1.826(11) . ? C1 C2 1.370(18) . ? C1 C6 1.426(18) . ? C2 C3 1.367(19) . ? C2 H2 0.9500 . ? C3 C4 1.40(3) . ? C3 H3 0.9500 . ? C4 C5 1.36(3) . ? C4 H4 0.9500 . ? C5 C6 1.361(18) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.357(15) . ? C7 C8 1.418(14) . ? C8 C9 1.386(18) . ? C8 H8 0.9500 . ? C9 C10 1.37(2) . ? C9 H9 0.9500 . ? C10 C11 1.349(19) . ? C10 H10 0.9500 . ? C11 C12 1.395(16) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.495(13) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 O1 1.413(11) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? O1 C15 1.364(12) . ? C15 C16 1.418(16) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 O2 1.330(13) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? O2 C17 1.413(13) . ? C17 C18 1.470(16) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 O3 1.412(12) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? O3 C19 1.401(12) . ? C19 C20 1.501(14) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 N1 1.447(12) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? N1 C21 1.342(11) . ? N1 H1 0.8800 . ? C21 O4 1.228(12) . ? C21 C22 1.522(15) . ? C22 N2 1.332(13) . ? C22 C26 1.390(13) . ? N2 C23 1.315(12) . ? C23 C24 1.378(13) . ? C23 C27 1.502(16) . ? C24 C25 1.355(18) . ? C24 H24 0.9500 . ? C25 C26 1.396(18) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 O5 1.228(11) . ? C27 N3 1.330(11) . ? N3 C28 1.444(13) . ? N3 H3A 0.8800 . ? C28 C29 1.520(14) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 O6 1.429(12) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? O6 C30 1.412(12) . ? C30 C31 1.500(16) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 O7 1.393(12) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? O7 C32 1.373(13) . ? C32 C33 1.408(16) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 O8 1.365(12) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? O8 C34 1.421(10) . ? C34 C35 1.506(13) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 P2 1.819(9) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? P2 C42 1.808(11) . ? P2 C36 1.821(9) . ? C36 C41 1.371(14) . ? C36 C37 1.404(15) . ? C37 C38 1.392(14) . ? C37 H37 0.9500 . ? C38 C39 1.366(19) . ? C38 H38 0.9500 . ? C39 C40 1.40(2) . ? C39 H39 0.9500 . ? C40 C41 1.387(15) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 C43 1.363(16) . ? C42 C47 1.504(18) . ? C43 C44 1.385(19) . ? C43 H43 0.9500 . ? C44 C45 1.33(2) . ? C44 H44 0.9500 . ? C45 C46 1.32(2) . ? C45 H45 0.9500 . ? C46 C47 1.362(19) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C48 C49 1.184(14) . ? C49 C50 1.415(12) . ? C50 C51 1.3900 . ? C50 C54 1.3900 . ? C51 C52 1.3900 . ? C51 H51 0.9500 . ? C52 N4 1.3900 . ? C52 H52 0.9500 . ? N4 C53 1.3900 . ? C53 C54 1.3900 . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C56 1.203(10) . ? C56 C57 1.432(10) . ? C57 C58 1.400(11) . ? C57 C61 1.402(11) . ? C58 C59 1.388(11) . ? C58 H58 0.9500 . ? C59 N5 1.330(12) . ? C59 H59 0.9500 . ? N5 C60 1.332(12) . ? C60 C61 1.387(11) . ? C60 H60 0.9500 . ? C61 H61 0.9500 . ? C62 C63 1.3900 . ? C62 C67 1.3900 . ? C62 P3 1.830(7) . ? C63 C64 1.3900 . ? C63 H63 0.9500 . ? C64 C65 1.3900 . ? C64 H64 0.9500 . ? C65 C66 1.3900 . ? C65 H65 0.9500 . ? C66 C67 1.3900 . ? C66 H66 0.9500 . ? C67 H67 0.9500 . ? Pt2 C109 1.992(9) . ? Pt2 C116 1.997(10) . ? Pt2 P4 2.313(3) . ? Pt2 P3 2.318(2) . ? P3 C68 1.811(10) . ? P3 C74 1.830(9) . ? C68 C73 1.378(15) . ? C68 C69 1.401(15) . ? C69 C70 1.352(17) . ? C69 H69 0.9500 . ? C70 C71 1.350(19) . ? C70 H70 0.9500 . ? C71 C72 1.409(18) . ? C71 H71 0.9500 . ? C72 C73 1.370(17) . ? C72 H72 0.9500 . ? C73 H73 0.9500 . ? C74 C75 1.545(13) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 O9 1.429(11) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? O9 C76 1.436(11) . ? C76 C77 1.496(14) . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 O10 1.403(12) . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? O10 C78 1.409(12) . ? C78 C79 1.518(18) . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C79 O11 1.396(13) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? O11 C80 1.403(13) . ? C80 C81 1.499(14) . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? C81 N6 1.455(11) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? N6 C82 1.328(11) . ? N6 H6A 0.8800 . ? C82 O12 1.236(11) . ? C82 C83 1.501(13) . ? C83 N7 1.352(12) . ? C83 C87 1.382(13) . ? N7 C84 1.358(11) . ? C84 C85 1.369(12) . ? C84 C88 1.474(14) . ? C85 C86 1.371(16) . ? C85 H85 0.9500 . ? C86 C87 1.402(15) . ? C86 H86 0.9500 . ? C87 H87 0.9500 . ? C88 O13 1.258(11) . ? C88 N8 1.318(11) . ? N8 C89 1.452(12) . ? N8 H8A 0.8800 . ? C89 C90 1.533(14) . ? C89 H89A 0.9900 . ? C89 H89B 0.9900 . ? C90 O14 1.428(12) . ? C90 H90A 0.9900 . ? C90 H90B 0.9900 . ? O14 C91 1.393(12) . ? C91 C92 1.494(15) . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? C92 O15 1.427(12) . ? C92 H92A 0.9900 . ? C92 H92B 0.9900 . ? O15 C93 1.428(12) . ? C93 C94 1.489(15) . ? C93 H93A 0.9900 . ? C93 H93B 0.9900 . ? C94 O16 1.424(12) . ? C94 H94A 0.9900 . ? C94 H94B 0.9900 . ? O16 C95 1.442(13) . ? C95 C96 1.543(15) . ? C95 H95A 0.9900 . ? C95 H95B 0.9900 . ? C96 P4 1.822(11) . ? C96 H96A 0.9900 . ? C96 H96B 0.9900 . ? P4 C97 1.824(12) . ? P4 C103 1.830(13) . ? C97 C102 1.358(19) . ? C97 C98 1.410(18) . ? C98 C99 1.390(15) . ? C98 H98 0.9500 . ? C99 C100 1.352(17) . ? C99 H99 0.9500 . ? C100 C101 1.36(2) . ? C100 H100 0.9500 . ? C101 C102 1.372(19) . ? C101 H101 0.9500 . ? C102 H102 0.9500 . ? C103 C104 1.375(17) . ? C103 C108 1.385(16) . ? C104 C105 1.363(17) . ? C104 H104 0.9500 . ? C105 C106 1.37(2) . ? C105 H105 0.9500 . ? C106 C107 1.39(2) . ? C106 H106 0.9500 . ? C107 C108 1.40(2) . ? C107 H107 0.9500 . ? C108 H108 0.9500 . ? C109 C110 1.198(13) . ? C110 C111 1.441(11) . ? C111 C112 1.3900 . ? C111 C115 1.3900 . ? C112 C113 1.3900 . ? C112 H112 0.9500 . ? C113 N9 1.3900 . ? C113 H113 0.9500 . ? N9 C114 1.3900 . ? C114 C115 1.3900 . ? C114 H114 0.9500 . ? C115 H115 0.9500 . ? C116 C117 1.203(13) . ? C117 C118 1.439(12) . ? C118 C119 1.389(13) . ? C118 C122 1.420(13) . ? C119 C120 1.386(12) . ? C119 H119 0.9500 . ? C120 N10 1.324(12) . ? C120 H120 0.9500 . ? N10 C121 1.343(12) . ? C121 C122 1.371(12) . ? C121 H121 0.9500 . ? C122 H122 0.9500 . ? O17 C125 1.461(15) . ? O17 C124 1.490(15) . ? C123 C124 1.512(17) . ? C123 H12A 0.9800 . ? C123 H12B 0.9800 . ? C123 H12C 0.9800 . ? C124 H12D 0.9900 . ? C124 H12E 0.9900 . ? C125 C126 1.518(16) . ? C125 H12F 0.9900 . ? C125 H12G 0.9900 . ? C126 H12H 0.9800 . ? C126 H12I 0.9800 . ? C126 H12J 0.9800 . ? O18 C129 1.474(16) . ? O18 C128 1.502(16) . ? C127 C128 1.514(17) . ? C127 H12K 0.9800 . ? C127 H12L 0.9800 . ? C127 H12M 0.9800 . ? C128 H12N 0.9900 . ? C128 H12O 0.9900 . ? C129 C130 1.520(17) . ? C129 H12P 0.9900 . ? C129 H12Q 0.9900 . ? C130 H13C 0.9800 . ? C130 H13D 0.9800 . ? C130 H13E 0.9800 . ? 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 C55 Pt1 C48 176.6(4) . . ? C55 Pt1 P2 92.0(2) . . ? C48 Pt1 P2 90.9(3) . . ? C55 Pt1 P1 90.9(2) . . ? C48 Pt1 P1 86.2(3) . . ? P2 Pt1 P1 177.11(9) . . ? C13 P1 C7 103.3(5) . . ? C13 P1 C1 103.1(5) . . ? C7 P1 C1 106.9(5) . . ? C13 P1 Pt1 116.6(3) . . ? C7 P1 Pt1 116.4(3) . . ? C1 P1 Pt1 109.3(3) . . ? C2 C1 C6 119.0(12) . . ? C2 C1 P1 121.8(11) . . ? C6 C1 P1 119.2(9) . . ? C3 C2 C1 123.0(18) . . ? C3 C2 H2 118.5 . . ? C1 C2 H2 118.5 . . ? C2 C3 C4 116.3(19) . . ? C2 C3 H3 121.9 . . ? C4 C3 H3 121.9 . . ? C5 C4 C3 122.4(15) . . ? C5 C4 H4 118.8 . . ? C3 C4 H4 118.8 . . ? C6 C5 C4 120.8(19) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C1 118.0(16) . . ? C5 C6 H6 121.0 . . ? C1 C6 H6 121.0 . . ? C12 C7 C8 119.7(10) . . ? C12 C7 P1 121.5(8) . . ? C8 C7 P1 118.7(8) . . ? C9 C8 C7 116.9(12) . . ? C9 C8 H8 121.5 . . ? C7 C8 H8 121.5 . . ? C10 C9 C8 124.2(13) . . ? C10 C9 H9 117.9 . . ? C8 C9 H9 117.9 . . ? C11 C10 C9 116.5(13) . . ? C11 C10 H10 121.7 . . ? C9 C10 H10 121.7 . . ? C10 C11 C12 122.9(14) . . ? C10 C11 H11 118.6 . . ? C12 C11 H11 118.6 . . ? C7 C12 C11 119.7(12) . . ? C7 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C14 C13 P1 114.1(7) . . ? C14 C13 H13A 108.7 . . ? P1 C13 H13A 108.7 . . ? C14 C13 H13B 108.7 . . ? P1 C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? O1 C14 C13 107.0(8) . . ? O1 C14 H14A 110.3 . . ? C13 C14 H14A 110.3 . . ? O1 C14 H14B 110.3 . . ? C13 C14 H14B 110.3 . . ? H14A C14 H14B 108.6 . . ? C15 O1 C14 117.0(8) . . ? O1 C15 C16 116.4(10) . . ? O1 C15 H15A 108.2 . . ? C16 C15 H15A 108.2 . . ? O1 C15 H15B 108.2 . . ? C16 C15 H15B 108.2 . . ? H15A C15 H15B 107.3 . . ? O2 C16 C15 120.1(10) . . ? O2 C16 H16A 107.3 . . ? C15 C16 H16A 107.3 . . ? O2 C16 H16B 107.3 . . ? C15 C16 H16B 107.3 . . ? H16A C16 H16B 106.9 . . ? C16 O2 C17 117.7(9) . . ? O2 C17 C18 110.1(9) . . ? O2 C17 H17A 109.7 . . ? C18 C17 H17A 109.7 . . ? O2 C17 H17B 109.6 . . ? C18 C17 H17B 109.6 . . ? H17A C17 H17B 108.2 . . ? O3 C18 C17 108.3(9) . . ? 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 111.7(8) . . ? O3 C19 C20 108.1(8) . . ? 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 114.3(8) . . ? N1 C20 H20A 108.7 . . ? C19 C20 H20A 108.7 . . ? N1 C20 H20B 108.7 . . ? C19 C20 H20B 108.7 . . ? H20A C20 H20B 107.6 . . ? C21 N1 C20 121.7(8) . . ? C21 N1 H1 119.2 . . ? C20 N1 H1 119.2 . . ? O4 C21 N1 123.8(10) . . ? O4 C21 C22 121.2(9) . . ? N1 C21 C22 115.0(9) . . ? N2 C22 C26 124.5(10) . . ? N2 C22 C21 117.7(8) . . ? C26 C22 C21 117.7(10) . . ? C23 N2 C22 117.4(8) . . ? N2 C23 C24 122.8(11) . . ? N2 C23 C27 116.8(8) . . ? C24 C23 C27 120.4(10) . . ? C25 C24 C23 119.7(11) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C24 C25 C26 119.5(10) . . ? C24 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? C22 C26 C25 116.1(12) . . ? C22 C26 H26 122.0 . . ? C25 C26 H26 122.0 . . ? O5 C27 N3 122.0(11) . . ? O5 C27 C23 121.2(9) . . ? N3 C27 C23 116.8(9) . . ? C27 N3 C28 122.6(9) . . ? C27 N3 H3A 118.7 . . ? C28 N3 H3A 118.7 . . ? N3 C28 C29 113.5(9) . . ? N3 C28 H28A 108.9 . . ? C29 C28 H28A 108.9 . . ? N3 C28 H28B 108.9 . . ? C29 C28 H28B 108.9 . . ? H28A C28 H28B 107.7 . . ? O6 C29 C28 108.6(8) . . ? O6 C29 H29A 110.0 . . ? C28 C29 H29A 110.0 . . ? O6 C29 H29B 110.0 . . ? C28 C29 H29B 110.0 . . ? H29A C29 H29B 108.4 . . ? C30 O6 C29 113.4(8) . . ? O6 C30 C31 109.2(9) . . ? O6 C30 H30A 109.8 . . ? C31 C30 H30A 109.8 . . ? O6 C30 H30B 109.8 . . ? C31 C30 H30B 109.8 . . ? H30A C30 H30B 108.3 . . ? O7 C31 C30 109.9(10) . . ? O7 C31 H31A 109.7 . . ? C30 C31 H31A 109.7 . . ? O7 C31 H31B 109.7 . . ? C30 C31 H31B 109.7 . . ? H31A C31 H31B 108.2 . . ? C32 O7 C31 114.9(9) . . ? O7 C32 C33 119.7(10) . . ? O7 C32 H32A 107.4 . . ? C33 C32 H32A 107.4 . . ? O7 C32 H32B 107.4 . . ? C33 C32 H32B 107.4 . . ? H32A C32 H32B 106.9 . . ? O8 C33 C32 117.4(10) . . ? O8 C33 H33A 108.0 . . ? C32 C33 H33A 108.0 . . ? O8 C33 H33B 108.0 . . ? C32 C33 H33B 108.0 . . ? H33A C33 H33B 107.2 . . ? C33 O8 C34 116.9(8) . . ? O8 C34 C35 109.5(7) . . ? O8 C34 H34A 109.8 . . ? C35 C34 H34A 109.8 . . ? O8 C34 H34B 109.8 . . ? C35 C34 H34B 109.8 . . ? H34A C34 H34B 108.2 . . ? C34 C35 P2 112.3(6) . . ? C34 C35 H35A 109.1 . . ? P2 C35 H35A 109.1 . . ? C34 C35 H35B 109.1 . . ? P2 C35 H35B 109.1 . . ? H35A C35 H35B 107.9 . . ? C42 P2 C35 104.0(5) . . ? C42 P2 C36 105.2(5) . . ? C35 P2 C36 104.8(4) . . ? C42 P2 Pt1 107.5(4) . . ? C35 P2 Pt1 117.1(3) . . ? C36 P2 Pt1 116.9(4) . . ? C41 C36 C37 118.8(9) . . ? C41 C36 P2 121.4(9) . . ? C37 C36 P2 119.8(8) . . ? C38 C37 C36 120.8(11) . . ? C38 C37 H37 119.6 . . ? C36 C37 H37 119.6 . . ? C39 C38 C37 119.4(12) . . ? C39 C38 H38 120.3 . . ? C37 C38 H38 120.3 . . ? C38 C39 C40 120.4(11) . . ? C38 C39 H39 119.8 . . ? C40 C39 H39 119.8 . . ? C41 C40 C39 119.8(12) . . ? C41 C40 H40 120.1 . . ? C39 C40 H40 120.1 . . ? C36 C41 C40 120.8(11) . . ? C36 C41 H41 119.6 . . ? C40 C41 H41 119.6 . . ? C43 C42 C47 115.0(11) . . ? C43 C42 P2 120.2(9) . . ? C47 C42 P2 123.8(9) . . ? C42 C43 C44 122.7(14) . . ? C42 C43 H43 118.6 . . ? C44 C43 H43 118.6 . . ? C45 C44 C43 118.9(14) . . ? C45 C44 H44 120.5 . . ? C43 C44 H44 120.5 . . ? C46 C45 C44 123.5(15) . . ? C46 C45 H45 118.3 . . ? C44 C45 H45 118.3 . . ? C45 C46 C47 121.0(16) . . ? C45 C46 H46 119.5 . . ? C47 C46 H46 119.5 . . ? C46 C47 C42 118.1(12) . . ? C46 C47 H47 121.0 . . ? C42 C47 H47 121.0 . . ? C49 C48 Pt1 172.9(11) . . ? C48 C49 C50 176.0(15) . . ? C51 C50 C54 120.0 . . ? C51 C50 C49 119.2(8) . . ? C54 C50 C49 120.8(8) . . ? C52 C51 C50 120.0 . . ? C52 C51 H51 120.0 . . ? C50 C51 H51 120.0 . . ? C51 C52 N4 120.0 . . ? C51 C52 H52 120.0 . . ? N4 C52 H52 120.0 . . ? C53 N4 C52 120.0 . . ? C54 C53 N4 120.0 . . ? C54 C53 H53 120.0 . . ? N4 C53 H53 120.0 . . ? C53 C54 C50 120.0 . . ? C53 C54 H54 120.0 . . ? C50 C54 H54 120.0 . . ? C56 C55 Pt1 178.0(8) . . ? C55 C56 C57 178.8(9) . . ? C58 C57 C61 117.7(7) . . ? C58 C57 C56 120.6(7) . . ? C61 C57 C56 121.7(7) . . ? C59 C58 C57 118.2(8) . . ? C59 C58 H58 120.9 . . ? C57 C58 H58 120.9 . . ? N5 C59 C58 124.7(8) . . ? N5 C59 H59 117.6 . . ? C58 C59 H59 117.6 . . ? C59 N5 C60 116.5(8) . . ? N5 C60 C61 124.3(8) . . ? N5 C60 H60 117.9 . . ? C61 C60 H60 117.9 . . ? C60 C61 C57 118.5(8) . . ? C60 C61 H61 120.8 . . ? C57 C61 H61 120.8 . . ? C63 C62 C67 120.0 . . ? C63 C62 P3 122.6(6) . . ? C67 C62 P3 117.3(6) . . ? C64 C63 C62 120.0 . . ? C64 C63 H63 120.0 . . ? C62 C63 H63 120.0 . . ? C63 C64 C65 120.0 . . ? C63 C64 H64 120.0 . . ? C65 C64 H64 120.0 . . ? C66 C65 C64 120.0 . . ? C66 C65 H65 120.0 . . ? C64 C65 H65 120.0 . . ? C67 C66 C65 120.0 . . ? C67 C66 H66 120.0 . . ? C65 C66 H66 120.0 . . ? C66 C67 C62 120.0 . . ? C66 C67 H67 120.0 . . ? C62 C67 H67 120.0 . . ? C109 Pt2 C116 178.1(4) . . ? C109 Pt2 P4 92.2(3) . . ? C116 Pt2 P4 88.8(3) . . ? C109 Pt2 P3 91.4(3) . . ? C116 Pt2 P3 87.6(3) . . ? P4 Pt2 P3 176.40(8) . . ? C68 P3 C62 105.0(5) . . ? C68 P3 C74 99.5(5) . . ? C62 P3 C74 105.3(4) . . ? C68 P3 Pt2 114.0(3) . . ? C62 P3 Pt2 117.6(3) . . ? C74 P3 Pt2 113.5(3) . . ? C73 C68 C69 117.6(10) . . ? C73 C68 P3 121.5(8) . . ? C69 C68 P3 120.6(9) . . ? C70 C69 C68 121.9(13) . . ? C70 C69 H69 119.0 . . ? C68 C69 H69 119.0 . . ? C71 C70 C69 120.4(13) . . ? C71 C70 H70 119.8 . . ? C69 C70 H70 119.8 . . ? C70 C71 C72 119.5(12) . . ? C70 C71 H71 120.3 . . ? C72 C71 H71 120.3 . . ? C73 C72 C71 119.8(13) . . ? C73 C72 H72 120.1 . . ? C71 C72 H72 120.1 . . ? C72 C73 C68 120.8(11) . . ? C72 C73 H73 119.6 . . ? C68 C73 H73 119.6 . . ? C75 C74 P3 116.0(7) . . ? C75 C74 H74A 108.3 . . ? P3 C74 H74A 108.3 . . ? C75 C74 H74B 108.3 . . ? P3 C74 H74B 108.3 . . ? H74A C74 H74B 107.4 . . ? O9 C75 C74 109.2(8) . . ? O9 C75 H75A 109.8 . . ? C74 C75 H75A 109.8 . . ? O9 C75 H75B 109.8 . . ? C74 C75 H75B 109.8 . . ? H75A C75 H75B 108.3 . . ? C75 O9 C76 114.5(8) . . ? O9 C76 C77 108.0(9) . . ? O9 C76 H76A 110.1 . . ? C77 C76 H76A 110.1 . . ? O9 C76 H76B 110.1 . . ? C77 C76 H76B 110.1 . . ? H76A C76 H76B 108.4 . . ? O10 C77 C76 110.4(7) . . ? O10 C77 H77A 109.6 . . ? C76 C77 H77A 109.6 . . ? O10 C77 H77B 109.6 . . ? C76 C77 H77B 109.6 . . ? H77A C77 H77B 108.1 . . ? C77 O10 C78 111.8(8) . . ? O10 C78 C79 110.4(10) . . ? O10 C78 H78A 109.6 . . ? C79 C78 H78A 109.6 . . ? O10 C78 H78B 109.6 . . ? C79 C78 H78B 109.6 . . ? H78A C78 H78B 108.1 . . ? O11 C79 C78 110.9(9) . . ? O11 C79 H79A 109.5 . . ? C78 C79 H79A 109.5 . . ? O11 C79 H79B 109.5 . . ? C78 C79 H79B 109.5 . . ? H79A C79 H79B 108.0 . . ? C79 O11 C80 112.8(8) . . ? O11 C80 C81 110.2(8) . . ? O11 C80 H80A 109.6 . . ? C81 C80 H80A 109.6 . . ? O11 C80 H80B 109.6 . . ? C81 C80 H80B 109.6 . . ? H80A C80 H80B 108.1 . . ? N6 C81 C80 114.3(8) . . ? N6 C81 H81A 108.7 . . ? C80 C81 H81A 108.7 . . ? N6 C81 H81B 108.7 . . ? C80 C81 H81B 108.7 . . ? H81A C81 H81B 107.6 . . ? C82 N6 C81 120.7(8) . . ? C82 N6 H6A 119.7 . . ? C81 N6 H6A 119.7 . . ? O12 C82 N6 123.4(9) . . ? O12 C82 C83 119.9(8) . . ? N6 C82 C83 116.7(8) . . ? N7 C83 C87 123.8(9) . . ? N7 C83 C82 116.7(8) . . ? C87 C83 C82 119.6(9) . . ? C83 N7 C84 116.6(8) . . ? N7 C84 C85 122.9(9) . . ? N7 C84 C88 116.3(8) . . ? C85 C84 C88 120.8(9) . . ? C84 C85 C86 120.1(10) . . ? C84 C85 H85 120.0 . . ? C86 C85 H85 120.0 . . ? C85 C86 C87 118.7(10) . . ? C85 C86 H86 120.7 . . ? C87 C86 H86 120.7 . . ? C83 C87 C86 118.0(10) . . ? C83 C87 H87 121.0 . . ? C86 C87 H87 121.0 . . ? O13 C88 N8 122.5(9) . . ? O13 C88 C84 118.8(8) . . ? N8 C88 C84 118.5(8) . . ? C88 N8 C89 123.0(8) . . ? C88 N8 H8A 118.5 . . ? C89 N8 H8A 118.5 . . ? N8 C89 C90 114.0(9) . . ? N8 C89 H89A 108.7 . . ? C90 C89 H89A 108.7 . . ? N8 C89 H89B 108.7 . . ? C90 C89 H89B 108.7 . . ? H89A C89 H89B 107.6 . . ? O14 C90 C89 108.4(8) . . ? O14 C90 H90A 110.0 . . ? C89 C90 H90A 110.0 . . ? O14 C90 H90B 110.0 . . ? C89 C90 H90B 110.0 . . ? H90A C90 H90B 108.4 . . ? C91 O14 C90 113.1(8) . . ? O14 C91 C92 111.5(9) . . ? O14 C91 H91A 109.3 . . ? C92 C91 H91A 109.3 . . ? O14 C91 H91B 109.3 . . ? C92 C91 H91B 109.3 . . ? H91A C91 H91B 108.0 . . ? O15 C92 C91 110.5(9) . . ? O15 C92 H92A 109.6 . . ? C91 C92 H92A 109.6 . . ? O15 C92 H92B 109.6 . . ? C91 C92 H92B 109.6 . . ? H92A C92 H92B 108.1 . . ? C92 O15 C93 111.5(8) . . ? O15 C93 C94 110.8(8) . . ? O15 C93 H93A 109.5 . . ? C94 C93 H93A 109.5 . . ? O15 C93 H93B 109.5 . . ? C94 C93 H93B 109.5 . . ? H93A C93 H93B 108.1 . . ? O16 C94 C93 108.9(9) . . ? O16 C94 H94A 109.9 . . ? C93 C94 H94A 109.9 . . ? O16 C94 H94B 109.9 . . ? C93 C94 H94B 109.9 . . ? H94A C94 H94B 108.3 . . ? C94 O16 C95 113.5(8) . . ? O16 C95 C96 109.1(8) . . ? O16 C95 H95A 109.9 . . ? C96 C95 H95A 109.9 . . ? O16 C95 H95B 109.9 . . ? C96 C95 H95B 109.9 . . ? H95A C95 H95B 108.3 . . ? C95 C96 P4 115.6(7) . . ? C95 C96 H96A 108.4 . . ? P4 C96 H96A 108.4 . . ? C95 C96 H96B 108.4 . . ? P4 C96 H96B 108.4 . . ? H96A C96 H96B 107.5 . . ? C96 P4 C97 108.1(5) . . ? C96 P4 C103 97.8(5) . . ? C97 P4 C103 104.3(6) . . ? C96 P4 Pt2 115.2(4) . . ? C97 P4 Pt2 115.2(4) . . ? C103 P4 Pt2 114.4(4) . . ? C102 C97 C98 116.8(12) . . ? C102 C97 P4 123.5(11) . . ? C98 C97 P4 119.6(10) . . ? C99 C98 C97 120.3(13) . . ? C99 C98 H98 119.9 . . ? C97 C98 H98 119.9 . . ? C100 C99 C98 118.6(13) . . ? C100 C99 H99 120.7 . . ? C98 C99 H99 120.7 . . ? C99 C100 C101 123.2(13) . . ? C99 C100 H100 118.4 . . ? C101 C100 H100 118.4 . . ? C100 C101 C102 116.8(17) . . ? C100 C101 H101 121.6 . . ? C102 C101 H101 121.6 . . ? C97 C102 C101 124.1(17) . . ? C97 C102 H102 118.0 . . ? C101 C102 H102 118.0 . . ? C104 C103 C108 118.8(12) . . ? C104 C103 P4 122.3(8) . . ? C108 C103 P4 118.6(10) . . ? C105 C104 C103 121.9(12) . . ? C105 C104 H104 119.0 . . ? C103 C104 H104 119.0 . . ? C104 C105 C106 120.2(15) . . ? C104 C105 H105 119.9 . . ? C106 C105 H105 119.9 . . ? C105 C106 C107 119.0(14) . . ? C105 C106 H106 120.5 . . ? C107 C106 H106 120.5 . . ? C106 C107 C108 120.1(14) . . ? C106 C107 H107 120.0 . . ? C108 C107 H107 120.0 . . ? C103 C108 C107 119.7(15) . . ? C103 C108 H108 120.2 . . ? C107 C108 H108 120.2 . . ? C110 C109 Pt2 175.8(11) . . ? C109 C110 C111 179.2(14) . . ? C112 C111 C115 120.0 . . ? C112 C111 C110 119.5(8) . . ? C115 C111 C110 120.3(8) . . ? C111 C112 C113 120.0 . . ? C111 C112 H112 120.0 . . ? C113 C112 H112 120.0 . . ? N9 C113 C112 120.0 . . ? N9 C113 H113 120.0 . . ? C112 C113 H113 120.0 . . ? C114 N9 C113 120.0 . . ? N9 C114 C115 120.0 . . ? N9 C114 H114 120.0 . . ? C115 C114 H114 120.0 . . ? C114 C115 C111 120.0 . . ? C114 C115 H115 120.0 . . ? C111 C115 H115 120.0 . . ? C117 C116 Pt2 177.6(10) . . ? C116 C117 C118 176.2(11) . . ? C119 C118 C122 116.9(8) . . ? C119 C118 C117 121.5(9) . . ? C122 C118 C117 121.5(8) . . ? C120 C119 C118 119.9(9) . . ? C120 C119 H119 120.0 . . ? C118 C119 H119 120.0 . . ? N10 C120 C119 123.2(9) . . ? N10 C120 H120 118.4 . . ? C119 C120 H120 118.4 . . ? C120 N10 C121 117.2(8) . . ? N10 C121 C122 124.4(9) . . ? N10 C121 H121 117.8 . . ? C122 C121 H121 117.8 . . ? C121 C122 C118 118.2(8) . . ? C121 C122 H122 120.9 . . ? C118 C122 H122 120.9 . . ? C125 O17 C124 118.0(12) . . ? C124 C123 H12A 109.5 . . ? C124 C123 H12B 109.5 . . ? H12A C123 H12B 109.5 . . ? C124 C123 H12C 109.5 . . ? H12A C123 H12C 109.5 . . ? H12B C123 H12C 109.5 . . ? O17 C124 C123 113.9(15) . . ? O17 C124 H12D 108.8 . . ? C123 C124 H12D 108.8 . . ? O17 C124 H12E 108.8 . . ? C123 C124 H12E 108.8 . . ? H12D C124 H12E 107.7 . . ? O17 C125 C126 112.5(13) . . ? O17 C125 H12F 109.1 . . ? C126 C125 H12F 109.1 . . ? O17 C125 H12G 109.1 . . ? C126 C125 H12G 109.1 . . ? H12F C125 H12G 107.8 . . ? C125 C126 H12H 109.5 . . ? C125 C126 H12I 109.5 . . ? H12H C126 H12I 109.5 . . ? C125 C126 H12J 109.5 . . ? H12H C126 H12J 109.5 . . ? H12I C126 H12J 109.5 . . ? C129 O18 C128 116.9(13) . . ? C128 C127 H12K 109.5 . . ? C128 C127 H12L 109.5 . . ? H12K C127 H12L 109.5 . . ? C128 C127 H12M 109.5 . . ? H12K C127 H12M 109.5 . . ? H12L C127 H12M 109.5 . . ? O18 C128 C127 111.6(16) . . ? O18 C128 H12N 109.3 . . ? C127 C128 H12N 109.3 . . ? O18 C128 H12O 109.3 . . ? C127 C128 H12O 109.3 . . ? H12N C128 H12O 108.0 . . ? O18 C129 C130 113.6(16) . . ? O18 C129 H12P 108.8 . . ? C130 C129 H12P 108.8 . . ? O18 C129 H12Q 108.8 . . ? C130 C129 H12Q 108.8 . . ? H12P C129 H12Q 107.7 . . ? C129 C130 H13C 109.5 . . ? C129 C130 H13D 109.5 . . ? H13C C130 H13D 109.5 . . ? C129 C130 H13E 109.5 . . ? H13C C130 H13E 109.5 . . ? H13D C130 H13E 109.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 29.15 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.494 _refine_diff_density_min -0.412 _refine_diff_density_rms 0.178 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.004 0.000 0.000 545.8 24.8 2 0.447 0.616 0.952 27.9 0.4 3 0.553 0.384 0.048 27.8 0.5 _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 929708' ####################################################################### # # 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_global # Attachment 's2695.cif.cif' data_e2695a #TrackingRef 's2695.cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C61 H63 N5 O8 P2 Pd Pt,C6 H14 O,C H Cl3' _chemical_formula_sum 'C68 H78 Cl3 N5 O9 P2 Pd Pt' _chemical_formula_weight 1579.13 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' Cl Cl 0.1484 0.1585 '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' Pd Pd -0.9988 1.0072 '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 7.9136(2) _cell_length_b 18.6050(4) _cell_length_c 23.8040(5) _cell_angle_alpha 96.7200(10) _cell_angle_beta 90.6200(10) _cell_angle_gamma 96.4710(10) _cell_volume 3457.45(14) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9962 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 25.83 _exptl_crystal_description colorless _exptl_crystal_colour plate _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.517 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1596 _exptl_absorpt_coefficient_mu 2.501 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8851 _exptl_absorpt_correction_T_max 0.9287 _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 85720 _diffrn_reflns_av_R_equivalents 0.0682 _diffrn_reflns_av_sigmaI/netI 0.0663 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 29.15 _reflns_number_total 18604 _reflns_number_gt 14305 _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^)+(0.0345P)^2^+3.7732P] 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 18604 _refine_ls_number_parameters 806 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0654 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.0901 _refine_ls_wR_factor_gt 0.0812 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.001 _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 0.809595(19) 0.291673(7) 0.280883(6) 0.01649(4) Uani 1 1 d . . . Pd1 Pd 0.71678(4) 0.234616(14) -0.118858(11) 0.01708(7) Uani 1 1 d . . . P1 P 0.96458(13) 0.40495(5) 0.28457(4) 0.0175(2) Uani 1 1 d . . . C1 C 1.1186(5) 0.4230(2) 0.34332(17) 0.0248(9) Uani 1 1 d . . . C2 C 1.0927(7) 0.4704(2) 0.3912(2) 0.0411(12) Uani 1 1 d . . . H2 H 0.9959 0.4965 0.3927 0.049 Uiso 1 1 calc R . . C3 C 1.2074(8) 0.4802(3) 0.4369(2) 0.0553(15) Uani 1 1 d . . . H3 H 1.1893 0.5134 0.4692 0.066 Uiso 1 1 calc R . . C4 C 1.3476(7) 0.4418(3) 0.4357(2) 0.0487(14) Uani 1 1 d . . . H4 H 1.4274 0.4494 0.4665 0.058 Uiso 1 1 calc R . . C5 C 1.3696(6) 0.3933(3) 0.3900(2) 0.0421(12) Uani 1 1 d . . . H5 H 1.4649 0.3664 0.3889 0.050 Uiso 1 1 calc R . . C6 C 1.2541(6) 0.3828(2) 0.3447(2) 0.0382(11) Uani 1 1 d . . . H6 H 1.2689 0.3470 0.3139 0.046 Uiso 1 1 calc R . . C7 C 0.8335(5) 0.4789(2) 0.29292(17) 0.0242(9) Uani 1 1 d . . . C8 C 0.9108(6) 0.5518(2) 0.29420(19) 0.0338(10) Uani 1 1 d . . . H8 H 1.0308 0.5617 0.2920 0.041 Uiso 1 1 calc R . . C9 C 0.8099(7) 0.6081(2) 0.2986(2) 0.0411(12) Uani 1 1 d . . . H9 H 0.8604 0.6571 0.2997 0.049 Uiso 1 1 calc R . . C10 C 0.6341(7) 0.5930(3) 0.3014(3) 0.0571(16) Uani 1 1 d . . . H10 H 0.5654 0.6319 0.3051 0.069 Uiso 1 1 calc R . . C11 C 0.5610(7) 0.5244(3) 0.2990(4) 0.081(2) Uani 1 1 d . . . H11 H 0.4407 0.5147 0.3001 0.097 Uiso 1 1 calc R . . C12 C 0.6623(7) 0.4667(3) 0.2950(3) 0.0572(17) Uani 1 1 d . . . H12 H 0.6093 0.4181 0.2937 0.069 Uiso 1 1 calc R . . C13 C 1.0763(6) 0.4232(2) 0.21992(17) 0.0271(9) Uani 1 1 d . . . H13A H 0.9898 0.4238 0.1897 0.032 Uiso 1 1 calc R . . H13B H 1.1386 0.4728 0.2267 0.032 Uiso 1 1 calc R . . C14 C 1.2007(6) 0.3714(3) 0.19793(18) 0.0356(11) Uani 1 1 d . . . H14A H 1.3102 0.3834 0.2193 0.043 Uiso 1 1 calc R . . H14B H 1.1552 0.3207 0.2025 0.043 Uiso 1 1 calc R . . O1 O 1.2252(4) 0.3787(3) 0.13982(14) 0.0602(12) Uani 1 1 d D . . C15 C 1.3885(6) 0.3897(4) 0.1231(2) 0.0545(15) Uani 1 1 d D . . H15A H 1.4549 0.3547 0.1392 0.065 Uiso 1 1 calc R . . H15B H 1.4378 0.4394 0.1387 0.065 Uiso 1 1 calc R . . C16 C 1.4068(6) 0.3815(3) 0.0615(2) 0.0429(12) Uani 1 1 d D . . H16A H 1.5275 0.3957 0.0533 0.051 Uiso 1 1 calc R . . H16B H 1.3794 0.3294 0.0471 0.051 Uiso 1 1 calc R . . O2 O 1.3082(4) 0.42103(18) 0.03188(13) 0.0392(8) Uani 1 1 d . . . C17 C 1.3470(6) 0.4176(3) -0.02665(19) 0.0353(10) Uani 1 1 d . . . H17A H 1.3354 0.3661 -0.0438 0.042 Uiso 1 1 calc R . . H17B H 1.4659 0.4388 -0.0309 0.042 Uiso 1 1 calc R . . C18 C 1.2277(6) 0.4590(2) -0.05664(19) 0.0312(10) Uani 1 1 d . . . H18A H 1.2125 0.5053 -0.0332 0.037 Uiso 1 1 calc R . . H18B H 1.2761 0.4708 -0.0931 0.037 Uiso 1 1 calc R . . O3 O 1.0694(4) 0.41601(15) -0.06638(13) 0.0307(7) Uani 1 1 d . . . C19 C 0.9532(5) 0.4525(2) -0.09613(18) 0.0283(9) Uani 1 1 d . . . H19A H 0.9941 0.4578 -0.1347 0.034 Uiso 1 1 calc R . . H19B H 0.9457 0.5017 -0.0761 0.034 Uiso 1 1 calc R . . C20 C 0.7796(5) 0.4083(2) -0.09941(17) 0.0254(9) Uani 1 1 d . . . H20A H 0.7491 0.3972 -0.0609 0.030 Uiso 1 1 calc R . . H20B H 0.6950 0.4388 -0.1120 0.030 Uiso 1 1 calc R . . N1 N 0.7660(4) 0.33995(15) -0.13724(13) 0.0191(7) Uani 1 1 d . . . C21 C 0.7477(5) 0.3471(2) -0.19223(17) 0.0227(8) Uani 1 1 d . . . O4 O 0.7507(4) 0.40505(15) -0.21389(12) 0.0309(7) Uani 1 1 d . . . C22 C 0.7149(5) 0.2759(2) -0.22956(16) 0.0209(8) Uani 1 1 d . . . N2 N 0.6913(4) 0.21816(16) -0.20025(13) 0.0196(7) Uani 1 1 d . . . C23 C 0.7045(5) 0.2656(2) -0.28801(17) 0.0276(9) Uani 1 1 d . . . H23 H 0.7214 0.3058 -0.3093 0.033 Uiso 1 1 calc R . . C24 C 0.6688(6) 0.1950(2) -0.31481(18) 0.0325(10) Uani 1 1 d . . . H24 H 0.6631 0.1865 -0.3550 0.039 Uiso 1 1 calc R . . C25 C 0.6412(5) 0.1363(2) -0.28311(17) 0.0292(9) Uani 1 1 d . . . H25 H 0.6141 0.0881 -0.3014 0.035 Uiso 1 1 calc R . . C26 C 0.6540(5) 0.1495(2) -0.22468(16) 0.0213(8) Uani 1 1 d . . . C27 C 0.6401(5) 0.0942(2) -0.18352(16) 0.0208(8) Uani 1 1 d . . . O5 O 0.6119(4) 0.02826(14) -0.20141(12) 0.0304(7) Uani 1 1 d . . . N3 N 0.6632(4) 0.12325(16) -0.12934(13) 0.0190(7) Uani 1 1 d . . . C28 C 0.6642(6) 0.0701(2) -0.08828(17) 0.0275(9) Uani 1 1 d . . . H28A H 0.7111 0.0957 -0.0517 0.033 Uiso 1 1 calc R . . H28B H 0.7413 0.0337 -0.1017 0.033 Uiso 1 1 calc R . . C29 C 0.4918(6) 0.0307(2) -0.07860(18) 0.0297(10) Uani 1 1 d . . . H29A H 0.4340 0.0125 -0.1154 0.036 Uiso 1 1 calc R . . H29B H 0.5053 -0.0117 -0.0581 0.036 Uiso 1 1 calc R . . O6 O 0.3913(4) 0.07873(15) -0.04644(12) 0.0324(7) Uani 1 1 d . . . C30 C 0.2231(6) 0.0471(3) -0.04120(19) 0.0391(12) Uani 1 1 d . . . H30A H 0.2237 -0.0005 -0.0266 0.047 Uiso 1 1 calc R . . H30B H 0.1650 0.0386 -0.0788 0.047 Uiso 1 1 calc R . . C31 C 0.1276(6) 0.0965(3) -0.00145(18) 0.0359(11) Uani 1 1 d . . . H31A H 0.1456 0.1467 -0.0118 0.043 Uiso 1 1 calc R . . H31B H 0.0043 0.0797 -0.0048 0.043 Uiso 1 1 calc R . . O7 O 0.1851(4) 0.09600(17) 0.05486(12) 0.0337(7) Uani 1 1 d . . . C32 C 0.0883(6) 0.1363(3) 0.0941(2) 0.0353(11) Uani 1 1 d . . . H32A H -0.0296 0.1119 0.0940 0.042 Uiso 1 1 calc R . . H32B H 0.0839 0.1856 0.0830 0.042 Uiso 1 1 calc R . . C33 C 0.1654(5) 0.1420(2) 0.15203(19) 0.0311(10) Uani 1 1 d . . . H33A H 0.0815 0.1565 0.1805 0.037 Uiso 1 1 calc R . . H33B H 0.1991 0.0943 0.1594 0.037 Uiso 1 1 calc R . . O8 O 0.3103(3) 0.19498(15) 0.15625(12) 0.0276(6) Uani 1 1 d . . . C34 C 0.3936(5) 0.2061(2) 0.21019(17) 0.0258(9) Uani 1 1 d . . . H34A H 0.3075 0.2023 0.2399 0.031 Uiso 1 1 calc R . . H34B H 0.4554 0.2558 0.2161 0.031 Uiso 1 1 calc R . . C35 C 0.5180(5) 0.15086(19) 0.21583(17) 0.0219(8) Uani 1 1 d . . . H35A H 0.5834 0.1452 0.1807 0.026 Uiso 1 1 calc R . . H35B H 0.4532 0.1031 0.2199 0.026 Uiso 1 1 calc R . . P2 P 0.66636(12) 0.17591(5) 0.27583(4) 0.01690(19) Uani 1 1 d . . . C36 C 0.8156(5) 0.10805(19) 0.26929(16) 0.0201(8) Uani 1 1 d . . . C37 C 0.7807(6) 0.0429(2) 0.23377(19) 0.0339(10) Uani 1 1 d . . . H37 H 0.6782 0.0332 0.2117 0.041 Uiso 1 1 calc R . . C38 C 0.8974(7) -0.0076(3) 0.2310(2) 0.0464(13) Uani 1 1 d . . . H38 H 0.8755 -0.0516 0.2062 0.056 Uiso 1 1 calc R . . C39 C 1.0436(7) 0.0052(3) 0.2636(2) 0.0454(13) Uani 1 1 d . . . H39 H 1.1217 -0.0301 0.2617 0.054 Uiso 1 1 calc R . . C40 C 1.0774(6) 0.0692(3) 0.2991(2) 0.0415(12) Uani 1 1 d . . . H40 H 1.1789 0.0779 0.3217 0.050 Uiso 1 1 calc R . . C41 C 0.9638(5) 0.1213(2) 0.30194(19) 0.0303(10) Uani 1 1 d . . . H41 H 0.9880 0.1657 0.3262 0.036 Uiso 1 1 calc R . . C42 C 0.5415(5) 0.1561(2) 0.33712(16) 0.0229(8) Uani 1 1 d . . . C43 C 0.4349(6) 0.2061(2) 0.35888(19) 0.0335(10) Uani 1 1 d . . . H43 H 0.4284 0.2494 0.3418 0.040 Uiso 1 1 calc R . . C44 C 0.3370(6) 0.1930(3) 0.4058(2) 0.0443(13) Uani 1 1 d . . . H44 H 0.2611 0.2265 0.4200 0.053 Uiso 1 1 calc R . . C45 C 0.3509(7) 0.1311(3) 0.4316(2) 0.0454(13) Uani 1 1 d . . . H45 H 0.2869 0.1226 0.4642 0.055 Uiso 1 1 calc R . . C46 C 0.4570(6) 0.0820(3) 0.4101(2) 0.0482(14) Uani 1 1 d . . . H46 H 0.4654 0.0395 0.4280 0.058 Uiso 1 1 calc R . . C47 C 0.5521(6) 0.0930(3) 0.3628(2) 0.0365(11) Uani 1 1 d . . . H47 H 0.6238 0.0580 0.3480 0.044 Uiso 1 1 calc R . . C48 C 0.8009(5) 0.28220(19) 0.19634(16) 0.0199(8) Uani 1 1 d . . . C49 C 0.7887(5) 0.2766(2) 0.14545(16) 0.0216(8) Uani 1 1 d . . . C50 C 0.7730(5) 0.26890(19) 0.08502(16) 0.0211(8) Uani 1 1 d . . . C51 C 0.8972(5) 0.3007(2) 0.05172(16) 0.0235(8) Uani 1 1 d . . . H51 H 0.9952 0.3292 0.0690 0.028 Uiso 1 1 calc R . . C52 C 0.8776(5) 0.2905(2) -0.00612(16) 0.0220(8) Uani 1 1 d . . . H52 H 0.9639 0.3125 -0.0281 0.026 Uiso 1 1 calc R . . N4 N 0.7413(4) 0.25085(16) -0.03318(13) 0.0196(7) Uani 1 1 d . . . C53 C 0.6195(5) 0.22139(19) -0.00101(16) 0.0205(8) Uani 1 1 d . . . H53 H 0.5215 0.1941 -0.0194 0.025 Uiso 1 1 calc R . . C54 C 0.6294(5) 0.22871(19) 0.05687(16) 0.0198(8) Uani 1 1 d . . . H54 H 0.5401 0.2069 0.0778 0.024 Uiso 1 1 calc R . . C55 C 0.8114(5) 0.3034(2) 0.36528(16) 0.0230(8) Uani 1 1 d . . . C56 C 0.8099(6) 0.3114(2) 0.41601(17) 0.0291(9) Uani 1 1 d . . . C57 C 0.8095(7) 0.3210(2) 0.47680(17) 0.0337(11) Uani 1 1 d . . . C58 C 0.9601(7) 0.3388(2) 0.50873(19) 0.0407(12) Uani 1 1 d . . . H58 H 1.0655 0.3455 0.4903 0.049 Uiso 1 1 calc R . . C59 C 0.9568(9) 0.3466(3) 0.5673(2) 0.0526(15) Uani 1 1 d . . . H59 H 1.0618 0.3586 0.5878 0.063 Uiso 1 1 calc R . . N5 N 0.8156(8) 0.3384(3) 0.59601(19) 0.0639(15) Uani 1 1 d . . . C60 C 0.6712(9) 0.3222(3) 0.5660(2) 0.0670(19) Uani 1 1 d . . . H60 H 0.5684 0.3164 0.5860 0.080 Uiso 1 1 calc R . . C61 C 0.6599(8) 0.3131(3) 0.5071(2) 0.0537(15) Uani 1 1 d . . . H61 H 0.5525 0.3017 0.4879 0.064 Uiso 1 1 calc R . . C62 C 0.1682(6) 0.2620(3) 0.8345(2) 0.0411(12) Uani 1 1 d . . . H62 H 0.0656 0.2841 0.8494 0.049 Uiso 1 1 calc R . . Cl1 Cl 0.2340(2) 0.20556(10) 0.88300(8) 0.0813(5) Uani 1 1 d . . . Cl2 Cl 0.33030(18) 0.33187(8) 0.82659(6) 0.0537(3) Uani 1 1 d . . . Cl3 Cl 0.11428(19) 0.20958(8) 0.76868(6) 0.0558(3) Uani 1 1 d . . . C63 C -0.0832(6) 0.1317(3) 0.5316(2) 0.0408(12) Uani 1 1 d . . . H63 H -0.1004 0.1797 0.5531 0.049 Uiso 1 1 calc R . . C64 C -0.0921(7) 0.1376(3) 0.4686(2) 0.0558(15) Uani 1 1 d . . . H64A H -0.0103 0.1780 0.4598 0.084 Uiso 1 1 calc R . . H64B H -0.2072 0.1465 0.4579 0.084 Uiso 1 1 calc R . . H64C H -0.0647 0.0921 0.4476 0.084 Uiso 1 1 calc R . . C65 C -0.2144(8) 0.0740(3) 0.5480(3) 0.0683(18) Uani 1 1 d . . . H65A H -0.2018 0.0275 0.5253 0.102 Uiso 1 1 calc R . . H65B H -0.3282 0.0877 0.5412 0.102 Uiso 1 1 calc R . . H65C H -0.1993 0.0689 0.5882 0.102 Uiso 1 1 calc R . . O9 O 0.0831(4) 0.11381(19) 0.54428(14) 0.0471(9) Uani 1 1 d . . . C66 C 0.1422(7) 0.1330(3) 0.6015(2) 0.0519(14) Uani 1 1 d . . . H66 H 0.0423 0.1361 0.6267 0.062 Uiso 1 1 calc R . . C67 C 0.2492(10) 0.2051(3) 0.6074(3) 0.090(2) Uani 1 1 d . . . H67A H 0.3457 0.2026 0.5820 0.135 Uiso 1 1 calc R . . H67B H 0.2916 0.2173 0.6466 0.135 Uiso 1 1 calc R . . H67C H 0.1807 0.2427 0.5974 0.135 Uiso 1 1 calc R . . C68 C 0.2432(10) 0.0761(3) 0.6178(3) 0.085(2) Uani 1 1 d . . . H68A H 0.1702 0.0296 0.6161 0.127 Uiso 1 1 calc R . . H68B H 0.2892 0.0901 0.6564 0.127 Uiso 1 1 calc R . . H68C H 0.3371 0.0708 0.5917 0.127 Uiso 1 1 calc R . . 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 0.02182(8) 0.01478(6) 0.01204(7) 0.00223(5) -0.00021(5) -0.00215(5) Pd1 0.02084(16) 0.01702(13) 0.01294(13) 0.00266(10) 0.00017(12) -0.00061(11) P1 0.0211(5) 0.0141(4) 0.0166(5) 0.0024(3) -0.0009(4) -0.0011(4) C1 0.027(2) 0.0217(18) 0.023(2) 0.0003(15) -0.0083(17) -0.0050(16) C2 0.051(3) 0.037(2) 0.035(3) -0.005(2) -0.015(2) 0.016(2) C3 0.083(4) 0.040(3) 0.039(3) -0.010(2) -0.023(3) 0.012(3) C4 0.054(3) 0.038(3) 0.051(3) -0.008(2) -0.030(3) 0.007(2) C5 0.038(3) 0.042(3) 0.047(3) 0.004(2) -0.014(2) 0.008(2) C6 0.041(3) 0.036(2) 0.037(3) -0.003(2) -0.014(2) 0.011(2) C7 0.031(2) 0.0197(18) 0.022(2) -0.0005(15) -0.0012(17) 0.0048(16) C8 0.039(3) 0.027(2) 0.035(3) 0.0059(18) 0.002(2) 0.0038(19) C9 0.061(4) 0.027(2) 0.038(3) 0.0045(19) 0.000(2) 0.014(2) C10 0.052(4) 0.049(3) 0.076(4) 0.009(3) -0.006(3) 0.029(3) C11 0.032(3) 0.040(3) 0.173(8) 0.015(4) 0.001(4) 0.012(2) C12 0.035(3) 0.027(2) 0.108(5) 0.000(3) -0.001(3) 0.005(2) C13 0.036(3) 0.0215(19) 0.022(2) 0.0039(16) 0.0016(18) -0.0027(17) C14 0.024(2) 0.057(3) 0.026(2) 0.001(2) 0.0031(19) 0.006(2) O1 0.0241(19) 0.133(4) 0.0242(18) 0.008(2) 0.0094(15) 0.012(2) C15 0.030(3) 0.094(4) 0.048(3) 0.034(3) 0.004(3) 0.017(3) C16 0.027(3) 0.063(3) 0.045(3) 0.021(3) 0.016(2) 0.020(2) O2 0.0323(18) 0.058(2) 0.0331(18) 0.0168(16) 0.0097(15) 0.0182(16) C17 0.026(2) 0.050(3) 0.028(2) 0.001(2) 0.007(2) -0.001(2) C18 0.031(2) 0.033(2) 0.027(2) 0.0051(18) 0.0009(19) -0.0095(19) O3 0.0253(16) 0.0265(14) 0.0390(18) 0.0103(13) -0.0013(14) -0.0098(12) C19 0.034(2) 0.0196(18) 0.031(2) 0.0055(16) -0.0007(19) 0.0004(17) C20 0.026(2) 0.0231(19) 0.027(2) 0.0039(16) 0.0018(18) 0.0027(16) N1 0.0196(17) 0.0155(14) 0.0216(16) 0.0041(12) 0.0007(14) -0.0017(12) C21 0.017(2) 0.0255(19) 0.026(2) 0.0078(16) 0.0008(17) -0.0010(15) O4 0.0359(18) 0.0253(14) 0.0329(17) 0.0150(12) -0.0016(14) -0.0016(12) C22 0.017(2) 0.0287(19) 0.0184(19) 0.0078(15) 0.0021(16) 0.0037(16) N2 0.0198(17) 0.0225(15) 0.0172(16) 0.0045(12) 0.0010(13) 0.0028(13) C23 0.029(2) 0.034(2) 0.021(2) 0.0100(17) 0.0016(18) 0.0044(18) C24 0.037(3) 0.045(3) 0.0150(19) 0.0024(18) -0.0021(18) 0.008(2) C25 0.033(2) 0.032(2) 0.021(2) -0.0007(17) -0.0055(18) 0.0060(18) C26 0.020(2) 0.0235(18) 0.0188(19) -0.0028(15) -0.0007(16) 0.0012(15) C27 0.021(2) 0.0207(18) 0.0203(19) 0.0046(15) 0.0063(16) -0.0010(15) O5 0.0381(18) 0.0196(13) 0.0311(16) -0.0019(12) 0.0033(14) -0.0024(12) N3 0.0208(17) 0.0171(14) 0.0188(16) 0.0033(12) -0.0005(13) -0.0008(12) C28 0.038(3) 0.0204(18) 0.025(2) 0.0064(16) -0.0002(19) 0.0028(17) C29 0.041(3) 0.0228(19) 0.023(2) 0.0055(16) 0.0044(19) -0.0062(18) O6 0.0364(18) 0.0278(15) 0.0292(16) 0.0030(12) 0.0028(14) -0.0121(13) C30 0.039(3) 0.045(3) 0.028(2) 0.008(2) 0.001(2) -0.021(2) C31 0.029(3) 0.050(3) 0.029(2) 0.019(2) -0.007(2) -0.009(2) O7 0.0332(18) 0.0457(18) 0.0239(16) 0.0078(13) -0.0029(13) 0.0080(14) C32 0.023(2) 0.041(2) 0.043(3) 0.002(2) -0.006(2) 0.0071(19) C33 0.024(2) 0.035(2) 0.034(2) 0.0050(19) 0.0002(19) -0.0001(18) O8 0.0223(15) 0.0335(15) 0.0275(15) 0.0125(12) -0.0079(12) -0.0032(12) C34 0.029(2) 0.0245(19) 0.023(2) 0.0060(16) -0.0045(18) 0.0009(17) C35 0.024(2) 0.0158(16) 0.026(2) 0.0043(15) -0.0038(17) -0.0014(15) P2 0.0186(5) 0.0155(4) 0.0164(5) 0.0035(3) -0.0013(4) -0.0008(4) C36 0.021(2) 0.0172(17) 0.0227(19) 0.0067(14) 0.0011(16) 0.0015(15) C37 0.040(3) 0.026(2) 0.036(2) -0.0025(18) -0.010(2) 0.0090(19) C38 0.058(3) 0.034(2) 0.049(3) -0.005(2) -0.006(3) 0.020(2) C39 0.047(3) 0.041(3) 0.054(3) 0.012(2) 0.008(3) 0.023(2) C40 0.024(2) 0.046(3) 0.057(3) 0.017(2) -0.008(2) 0.006(2) C41 0.023(2) 0.031(2) 0.037(2) 0.0086(18) -0.0042(19) -0.0006(17) C42 0.020(2) 0.0258(19) 0.021(2) 0.0058(16) -0.0001(17) -0.0049(16) C43 0.039(3) 0.028(2) 0.032(2) 0.0012(18) 0.010(2) -0.0026(19) C44 0.038(3) 0.049(3) 0.041(3) -0.006(2) 0.016(2) -0.006(2) C45 0.034(3) 0.069(4) 0.032(3) 0.016(2) 0.011(2) -0.011(3) C46 0.032(3) 0.064(3) 0.054(3) 0.038(3) 0.002(3) -0.006(2) C47 0.028(3) 0.042(3) 0.044(3) 0.024(2) 0.002(2) 0.001(2) C48 0.022(2) 0.0168(17) 0.0203(19) 0.0022(14) 0.0013(16) -0.0022(15) C49 0.024(2) 0.0224(18) 0.0171(19) 0.0017(15) 0.0017(16) -0.0029(16) C50 0.027(2) 0.0198(17) 0.0167(18) 0.0028(14) 0.0012(16) 0.0044(15) C51 0.022(2) 0.0252(19) 0.022(2) 0.0029(16) -0.0006(17) -0.0050(16) C52 0.022(2) 0.0217(18) 0.0211(19) 0.0067(15) 0.0036(17) -0.0055(15) N4 0.0245(18) 0.0189(15) 0.0147(15) 0.0019(12) -0.0015(14) -0.0003(13) C53 0.021(2) 0.0194(17) 0.0198(19) 0.0014(15) -0.0006(16) -0.0028(15) C54 0.019(2) 0.0218(18) 0.0179(18) 0.0059(14) 0.0030(16) -0.0029(15) C55 0.026(2) 0.0210(18) 0.021(2) 0.0049(15) -0.0011(17) -0.0045(16) C56 0.036(3) 0.028(2) 0.021(2) 0.0027(17) -0.0017(19) -0.0057(18) C57 0.056(3) 0.030(2) 0.0142(19) 0.0053(17) -0.002(2) -0.001(2) C58 0.062(3) 0.036(2) 0.022(2) -0.0011(19) -0.009(2) 0.001(2) C59 0.089(5) 0.039(3) 0.028(3) 0.004(2) -0.018(3) 0.002(3) N5 0.109(5) 0.055(3) 0.024(2) 0.011(2) -0.007(3) -0.012(3) C60 0.089(5) 0.074(4) 0.031(3) 0.005(3) 0.017(3) -0.022(4) C61 0.061(4) 0.067(4) 0.026(3) 0.004(2) 0.006(3) -0.019(3) C62 0.036(3) 0.053(3) 0.038(3) 0.013(2) 0.009(2) 0.011(2) Cl1 0.0937(13) 0.0913(12) 0.0654(11) 0.0458(10) -0.0184(9) 0.0028(10) Cl2 0.0485(8) 0.0603(8) 0.0506(8) 0.0054(6) 0.0048(7) 0.0001(6) Cl3 0.0613(9) 0.0520(8) 0.0542(8) 0.0083(6) -0.0079(7) 0.0054(7) C63 0.034(3) 0.038(3) 0.048(3) -0.002(2) 0.007(2) 0.003(2) C64 0.051(4) 0.063(4) 0.053(4) 0.008(3) -0.003(3) 0.002(3) C65 0.054(4) 0.072(4) 0.074(5) 0.008(3) 0.015(3) -0.010(3) O9 0.045(2) 0.060(2) 0.036(2) 0.0000(17) 0.0026(16) 0.0143(17) C66 0.049(3) 0.067(4) 0.040(3) 0.003(3) 0.000(3) 0.010(3) C67 0.122(7) 0.048(4) 0.097(6) -0.001(4) -0.045(5) 0.012(4) C68 0.100(6) 0.053(4) 0.100(6) 0.014(4) -0.042(5) 0.008(4) _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 C55 1.995(4) . ? Pt1 C48 1.999(4) . ? Pt1 P2 2.3074(9) . ? Pt1 P1 2.3077(9) . ? Pd1 N2 1.930(3) . ? Pd1 N4 2.030(3) . ? Pd1 N3 2.053(3) . ? Pd1 N1 2.053(3) . ? P1 C7 1.809(4) . ? P1 C1 1.821(4) . ? P1 C13 1.830(4) . ? C1 C6 1.377(6) . ? C1 C2 1.389(6) . ? C2 C3 1.392(7) . ? C2 H2 0.9500 . ? C3 C4 1.384(7) . ? C3 H3 0.9500 . ? C4 C5 1.356(7) . ? C4 H4 0.9500 . ? C5 C6 1.387(6) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.351(6) . ? C7 C8 1.420(6) . ? C8 C9 1.383(6) . ? C8 H8 0.9500 . ? C9 C10 1.392(7) . ? C9 H9 0.9500 . ? C10 C11 1.334(8) . ? C10 H10 0.9500 . ? C11 C12 1.406(7) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.509(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 O1 1.419(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? O1 C15 1.357(6) . ? C15 C16 1.466(7) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 O2 1.373(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? O2 C17 1.426(5) . ? C17 C18 1.508(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 O3 1.410(5) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? O3 C19 1.430(5) . ? C19 C20 1.516(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 N1 1.463(5) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? N1 C21 1.339(5) . ? C21 O4 1.246(4) . ? C21 C22 1.501(5) . ? C22 N2 1.345(5) . ? C22 C23 1.383(5) . ? N2 C26 1.340(4) . ? C23 C24 1.390(6) . ? C23 H23 0.9500 . ? C24 C25 1.397(6) . ? C24 H24 0.9500 . ? C25 C26 1.384(5) . ? C25 H25 0.9500 . ? C26 C27 1.497(5) . ? C27 O5 1.246(4) . ? C27 N3 1.341(5) . ? N3 C28 1.470(5) . ? C28 C29 1.507(6) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 O6 1.425(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? O6 C30 1.406(5) . ? C30 C31 1.509(7) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 O7 1.412(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? O7 C32 1.415(5) . ? C32 C33 1.488(6) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 O8 1.420(5) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? O8 C34 1.419(5) . ? C34 C35 1.517(5) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 P2 1.822(4) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? P2 C36 1.819(4) . ? P2 C42 1.821(4) . ? C36 C41 1.382(5) . ? C36 C37 1.392(5) . ? C37 C38 1.386(6) . ? C37 H37 0.9500 . ? C38 C39 1.368(7) . ? C38 H38 0.9500 . ? C39 C40 1.375(7) . ? C39 H39 0.9500 . ? C40 C41 1.391(6) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 C43 1.385(6) . ? C42 C47 1.397(6) . ? C43 C44 1.397(6) . ? C43 H43 0.9500 . ? C44 C45 1.380(7) . ? C44 H44 0.9500 . ? C45 C46 1.369(7) . ? C45 H45 0.9500 . ? C46 C47 1.383(7) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C48 C49 1.206(5) . ? C49 C50 1.431(5) . ? C50 C51 1.393(6) . ? C50 C54 1.405(5) . ? C51 C52 1.372(5) . ? C51 H51 0.9500 . ? C52 N4 1.348(5) . ? C52 H52 0.9500 . ? N4 C53 1.346(5) . ? C53 C54 1.369(5) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C56 1.200(5) . ? C56 C57 1.437(6) . ? C57 C58 1.393(7) . ? C57 C61 1.396(7) . ? C58 C59 1.384(6) . ? C58 H58 0.9500 . ? C59 N5 1.320(8) . ? C59 H59 0.9500 . ? N5 C60 1.328(8) . ? C60 C61 1.392(7) . ? C60 H60 0.9500 . ? C61 H61 0.9500 . ? C62 Cl2 1.749(5) . ? C62 Cl1 1.760(5) . ? C62 Cl3 1.768(5) . ? C62 H62 1.0000 . ? C63 O9 1.431(6) . ? C63 C65 1.497(7) . ? C63 C64 1.516(7) . ? C63 H63 1.0000 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? O9 C66 1.427(6) . ? C66 C68 1.481(8) . ? C66 C67 1.494(8) . ? C66 H66 1.0000 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? 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 C55 Pt1 C48 177.92(16) . . ? C55 Pt1 P2 91.99(11) . . ? C48 Pt1 P2 88.44(10) . . ? C55 Pt1 P1 88.84(11) . . ? C48 Pt1 P1 90.83(10) . . ? P2 Pt1 P1 177.22(4) . . ? N2 Pd1 N4 179.28(13) . . ? N2 Pd1 N3 80.51(12) . . ? N4 Pd1 N3 98.89(12) . . ? N2 Pd1 N1 80.37(12) . . ? N4 Pd1 N1 100.24(12) . . ? N3 Pd1 N1 160.85(12) . . ? C7 P1 C1 105.73(18) . . ? C7 P1 C13 101.01(19) . . ? C1 P1 C13 108.0(2) . . ? C7 P1 Pt1 113.10(14) . . ? C1 P1 Pt1 112.70(13) . . ? C13 P1 Pt1 115.28(13) . . ? C6 C1 C2 117.5(4) . . ? C6 C1 P1 120.4(3) . . ? C2 C1 P1 121.6(3) . . ? C1 C2 C3 120.6(5) . . ? C1 C2 H2 119.7 . . ? C3 C2 H2 119.7 . . ? C4 C3 C2 120.4(5) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C5 C4 C3 119.2(5) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 120.4(5) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C1 C6 C5 121.7(4) . . ? C1 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? C12 C7 C8 118.7(4) . . ? C12 C7 P1 121.8(3) . . ? C8 C7 P1 119.5(3) . . ? C9 C8 C7 119.4(4) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C8 C9 C10 119.9(5) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C11 C10 C9 120.8(5) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 C12 119.9(5) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C7 C12 C11 121.4(5) . . ? C7 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C14 C13 P1 117.5(3) . . ? C14 C13 H13A 107.9 . . ? P1 C13 H13A 107.9 . . ? C14 C13 H13B 107.9 . . ? P1 C13 H13B 107.9 . . ? H13A C13 H13B 107.2 . . ? O1 C14 C13 108.0(4) . . ? O1 C14 H14A 110.1 . . ? C13 C14 H14A 110.1 . . ? O1 C14 H14B 110.1 . . ? C13 C14 H14B 110.1 . . ? H14A C14 H14B 108.4 . . ? C15 O1 C14 116.7(4) . . ? O1 C15 C16 114.0(4) . . ? O1 C15 H15A 108.8 . . ? C16 C15 H15A 108.8 . . ? O1 C15 H15B 108.8 . . ? C16 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? O2 C16 C15 116.1(4) . . ? O2 C16 H16A 108.3 . . ? C15 C16 H16A 108.3 . . ? O2 C16 H16B 108.3 . . ? C15 C16 H16B 108.3 . . ? H16A C16 H16B 107.4 . . ? C16 O2 C17 113.2(3) . . ? O2 C17 C18 109.9(4) . . ? O2 C17 H17A 109.7 . . ? C18 C17 H17A 109.7 . . ? O2 C17 H17B 109.7 . . ? C18 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? O3 C18 C17 109.1(3) . . ? O3 C18 H18A 109.9 . . ? C17 C18 H18A 109.9 . . ? O3 C18 H18B 109.9 . . ? C17 C18 H18B 109.9 . . ? H18A C18 H18B 108.3 . . ? C18 O3 C19 111.1(3) . . ? O3 C19 C20 109.1(3) . . ? O3 C19 H19A 109.9 . . ? C20 C19 H19A 109.9 . . ? O3 C19 H19B 109.9 . . ? C20 C19 H19B 109.9 . . ? H19A C19 H19B 108.3 . . ? N1 C20 C19 115.2(3) . . ? N1 C20 H20A 108.5 . . ? C19 C20 H20A 108.5 . . ? N1 C20 H20B 108.5 . . ? C19 C20 H20B 108.5 . . ? H20A C20 H20B 107.5 . . ? C21 N1 C20 114.8(3) . . ? C21 N1 Pd1 113.9(2) . . ? C20 N1 Pd1 129.7(2) . . ? O4 C21 N1 127.0(4) . . ? O4 C21 C22 119.1(4) . . ? N1 C21 C22 113.8(3) . . ? N2 C22 C23 119.8(4) . . ? N2 C22 C21 113.0(3) . . ? C23 C22 C21 127.2(4) . . ? C26 N2 C22 123.4(3) . . ? C26 N2 Pd1 118.1(3) . . ? C22 N2 Pd1 118.4(3) . . ? C22 C23 C24 118.3(4) . . ? C22 C23 H23 120.8 . . ? C24 C23 H23 120.8 . . ? C23 C24 C25 120.5(4) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C26 C25 C24 119.0(4) . . ? C26 C25 H25 120.5 . . ? C24 C25 H25 120.5 . . ? N2 C26 C25 119.0(4) . . ? N2 C26 C27 113.7(3) . . ? C25 C26 C27 127.2(3) . . ? O5 C27 N3 126.7(4) . . ? O5 C27 C26 119.5(3) . . ? N3 C27 C26 113.8(3) . . ? C27 N3 C28 115.0(3) . . ? C27 N3 Pd1 113.9(2) . . ? C28 N3 Pd1 130.7(2) . . ? N3 C28 C29 114.3(3) . . ? N3 C28 H28A 108.7 . . ? C29 C28 H28A 108.7 . . ? N3 C28 H28B 108.7 . . ? C29 C28 H28B 108.7 . . ? H28A C28 H28B 107.6 . . ? O6 C29 C28 109.9(3) . . ? O6 C29 H29A 109.7 . . ? C28 C29 H29A 109.7 . . ? O6 C29 H29B 109.7 . . ? C28 C29 H29B 109.7 . . ? H29A C29 H29B 108.2 . . ? C30 O6 C29 112.3(3) . . ? O6 C30 C31 110.3(4) . . ? 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 110.1(4) . . ? O7 C31 H31A 109.6 . . ? C30 C31 H31A 109.6 . . ? O7 C31 H31B 109.6 . . ? C30 C31 H31B 109.6 . . ? H31A C31 H31B 108.2 . . ? C31 O7 C32 112.0(3) . . ? O7 C32 C33 110.3(3) . . ? O7 C32 H32A 109.6 . . ? C33 C32 H32A 109.6 . . ? O7 C32 H32B 109.6 . . ? C33 C32 H32B 109.6 . . ? H32A C32 H32B 108.1 . . ? O8 C33 C32 108.9(4) . . ? O8 C33 H33A 109.9 . . ? C32 C33 H33A 109.9 . . ? O8 C33 H33B 109.9 . . ? C32 C33 H33B 109.9 . . ? H33A C33 H33B 108.3 . . ? C34 O8 C33 114.1(3) . . ? O8 C34 C35 111.8(3) . . ? O8 C34 H34A 109.3 . . ? C35 C34 H34A 109.3 . . ? O8 C34 H34B 109.3 . . ? C35 C34 H34B 109.3 . . ? H34A C34 H34B 107.9 . . ? C34 C35 P2 113.5(3) . . ? C34 C35 H35A 108.9 . . ? P2 C35 H35A 108.9 . . ? C34 C35 H35B 108.9 . . ? P2 C35 H35B 108.9 . . ? H35A C35 H35B 107.7 . . ? C36 P2 C42 104.55(18) . . ? C36 P2 C35 105.48(17) . . ? C42 P2 C35 104.50(18) . . ? C36 P2 Pt1 110.46(13) . . ? C42 P2 Pt1 115.83(13) . . ? C35 P2 Pt1 114.99(12) . . ? C41 C36 C37 120.1(4) . . ? C41 C36 P2 118.5(3) . . ? C37 C36 P2 121.4(3) . . ? C38 C37 C36 119.2(4) . . ? C38 C37 H37 120.4 . . ? C36 C37 H37 120.4 . . ? C39 C38 C37 120.8(4) . . ? C39 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C38 C39 C40 120.0(4) . . ? C38 C39 H39 120.0 . . ? C40 C39 H39 120.0 . . ? C39 C40 C41 120.3(4) . . ? C39 C40 H40 119.8 . . ? C41 C40 H40 119.8 . . ? C36 C41 C40 119.6(4) . . ? C36 C41 H41 120.2 . . ? C40 C41 H41 120.2 . . ? C43 C42 C47 119.7(4) . . ? C43 C42 P2 118.3(3) . . ? C47 C42 P2 122.0(3) . . ? C42 C43 C44 120.1(4) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C45 C44 C43 119.7(5) . . ? C45 C44 H44 120.1 . . ? C43 C44 H44 120.1 . . ? C46 C45 C44 119.9(5) . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C45 C46 C47 121.4(5) . . ? C45 C46 H46 119.3 . . ? C47 C46 H46 119.3 . . ? C46 C47 C42 119.1(5) . . ? C46 C47 H47 120.4 . . ? C42 C47 H47 120.4 . . ? C49 C48 Pt1 177.4(4) . . ? C48 C49 C50 179.2(4) . . ? C51 C50 C54 117.2(3) . . ? C51 C50 C49 122.1(4) . . ? C54 C50 C49 120.7(4) . . ? C52 C51 C50 119.8(4) . . ? C52 C51 H51 120.1 . . ? C50 C51 H51 120.1 . . ? N4 C52 C51 123.0(4) . . ? N4 C52 H52 118.5 . . ? C51 C52 H52 118.5 . . ? C53 N4 C52 117.3(3) . . ? C53 N4 Pd1 120.3(2) . . ? C52 N4 Pd1 122.4(3) . . ? N4 C53 C54 123.4(4) . . ? N4 C53 H53 118.3 . . ? C54 C53 H53 118.3 . . ? C53 C54 C50 119.3(4) . . ? C53 C54 H54 120.4 . . ? C50 C54 H54 120.4 . . ? C56 C55 Pt1 178.6(4) . . ? C55 C56 C57 179.6(5) . . ? C58 C57 C61 116.3(4) . . ? C58 C57 C56 121.3(5) . . ? C61 C57 C56 122.3(5) . . ? C59 C58 C57 120.3(5) . . ? C59 C58 H58 119.8 . . ? C57 C58 H58 119.8 . . ? N5 C59 C58 123.5(6) . . ? N5 C59 H59 118.3 . . ? C58 C59 H59 118.3 . . ? C59 N5 C60 116.7(5) . . ? N5 C60 C61 124.6(6) . . ? N5 C60 H60 117.7 . . ? C61 C60 H60 117.7 . . ? C60 C61 C57 118.6(6) . . ? C60 C61 H61 120.7 . . ? C57 C61 H61 120.7 . . ? Cl2 C62 Cl1 110.0(3) . . ? Cl2 C62 Cl3 110.4(3) . . ? Cl1 C62 Cl3 109.7(3) . . ? Cl2 C62 H62 108.9 . . ? Cl1 C62 H62 108.9 . . ? Cl3 C62 H62 108.9 . . ? O9 C63 C65 109.6(5) . . ? O9 C63 C64 107.2(4) . . ? C65 C63 C64 111.6(5) . . ? O9 C63 H63 109.5 . . ? C65 C63 H63 109.5 . . ? C64 C63 H63 109.5 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C63 C65 H65A 109.5 . . ? C63 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C63 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C66 O9 C63 115.9(4) . . ? O9 C66 C68 108.9(5) . . ? O9 C66 C67 110.0(5) . . ? C68 C66 C67 110.0(5) . . ? O9 C66 H66 109.3 . . ? C68 C66 H66 109.3 . . ? C67 C66 H66 109.3 . . ? C66 C67 H67A 109.5 . . ? C66 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C66 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C66 C68 H68A 109.5 . . ? C66 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C66 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 29.15 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.001 _refine_diff_density_min -1.070 _refine_diff_density_rms 0.134 _database_code_depnum_ccdc_archive 'CCDC 929709'