Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Wanzhi Chen' _publ_contact_author_address ; Department of Chemistry Zhejiang University Tianmushan Road 148 Hangzhou 310023 CHINA ; _publ_contact_author_email CHENWZZ@ZJU.EDU.CN _publ_section_title ; Synthesis and characterization of amidate bridged dimeric and oligomeric chain platinum complexes having short platinum-platinum interactions ; loop_ _publ_author_name 'Wanzhi Chen' 'Fenghui Liu' data_318 _database_code_depnum_ccdc_archive 'CCDC 290072' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20.50 H53 N9 O15 Pt2' _chemical_formula_weight 1055.90 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.307(2) _cell_length_b 17.158(3) _cell_length_c 16.924(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.775(3) _cell_angle_gamma 90.00 _cell_volume 3837.2(11) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.828 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2060 _exptl_absorpt_coefficient_mu 7.353 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3074 _exptl_absorpt_correction_T_max 0.5268 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 17883 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0413 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 24.51 _reflns_number_total 6293 _reflns_number_gt 5133 _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^)+(0.0535P)^2^+22.7221P] 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 6293 _refine_ls_number_parameters 482 _refine_ls_number_restraints 1478 _refine_ls_R_factor_all 0.0525 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.1100 _refine_ls_wR_factor_gt 0.1027 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.013 _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 0.68774(2) 0.132770(18) 0.908097(18) 0.03367(12) Uani 1 1 d U . . Pt2 Pt 0.59322(2) 0.140604(16) 0.759321(19) 0.02941(11) Uani 1 1 d DU C . N1 N 0.7664(5) 0.2258(4) 0.8805(4) 0.0335(14) Uani 1 1 d U . . H1 H 0.8023 0.2519 0.9187 0.040 Uiso 1 1 calc RD . . N2 N 0.7861(5) 0.0625(4) 0.8614(4) 0.0360(15) Uani 1 1 d U . . H2 H 0.8445 0.0520 0.8893 0.043 Uiso 1 1 calc R . . N3 N 0.6178(7) 0.0373(5) 0.9464(5) 0.060(2) Uani 1 1 d U . . H3D H 0.6636 -0.0020 0.9562 0.090 Uiso 1 1 calc R . . H3E H 0.5677 0.0219 0.9084 0.090 Uiso 1 1 calc R . . H3F H 0.5908 0.0490 0.9919 0.090 Uiso 1 1 calc R . . N4 N 0.5975(7) 0.2071(5) 0.9610(5) 0.063(2) Uani 1 1 d U . . H4D H 0.6198 0.2107 1.0138 0.095 Uiso 1 1 calc R . . H4E H 0.5328 0.1890 0.9547 0.095 Uiso 1 1 calc R . . H4F H 0.5994 0.2551 0.9383 0.095 Uiso 1 1 calc R . . N5 N 0.4868(5) 0.2269(4) 0.7607(5) 0.0462(16) Uani 1 1 d U . . H5D H 0.4857 0.2457 0.8115 0.055 Uiso 1 1 calc R A 1 H5E H 0.5008 0.2675 0.7281 0.055 Uiso 1 1 calc R A 1 N6 N 0.4723(5) 0.0668(4) 0.7578(5) 0.0449(17) Uani 1 1 d U . . H6A H 0.4684 0.0359 0.7131 0.054 Uiso 1 1 calc R B 1 H6B H 0.4808 0.0349 0.8018 0.054 Uiso 1 1 calc R B 1 N7 N 0.5194(10) 0.4001(6) 0.8666(7) 0.085(3) Uani 1 1 d U . . N8 N 0.5263(7) 0.1096(5) 0.1387(5) 0.050(2) Uani 1 1 d U . . N9 N 0.6519(10) 0.8430(9) 0.0102(9) 0.108(4) Uani 1 1 d U . . O1 O 0.7037(5) 0.2191(4) 0.7505(4) 0.0546(15) Uani 1 1 d U . . O2 O 0.6899(5) 0.0531(4) 0.7448(4) 0.0523(15) Uani 1 1 d U . . C19 C 0.8548(10) -0.0017(5) 1.0361(7) 0.081(3) Uani 1 1 d DU . . H19A H 0.9159 -0.0333 1.0347 0.121 Uiso 1 1 calc R . . H19B H 0.7997 -0.0234 0.9992 0.121 Uiso 1 1 calc R . . H19C H 0.8353 -0.0018 1.0902 0.121 Uiso 1 1 calc R . . O4 O 0.5455(9) 0.1442(5) 0.6116(6) 0.102(3) Uani 1 1 d DU . . H23 H 0.6012 0.1527 0.5932 0.123 Uiso 1 1 d R C . H24 H 0.5092 0.1846 0.6014 0.123 Uiso 1 1 d R . . O5 O 0.4724(10) 0.3438(5) 0.8901(7) 0.106(3) Uani 1 1 d U . . O6 O 0.5905(9) 0.3873(7) 0.8275(7) 0.111(3) Uani 1 1 d U . . O7 O 0.4833(9) 0.4668(5) 0.8742(6) 0.103(3) Uani 1 1 d U . . O8 O 0.5683(5) 0.0509(4) 0.1138(4) 0.0526(16) Uani 1 1 d U . . O9 O 0.4515(7) 0.0971(5) 0.1743(5) 0.081(2) Uani 1 1 d U . . O10 O 0.5611(6) 0.1765(3) 0.1294(4) 0.0540(17) Uani 1 1 d U . . O11 O 0.6363(13) 0.7758(10) 0.0193(12) 0.193(6) Uani 1 1 d U . . O12 O 0.7204(11) 0.8627(8) -0.0176(10) 0.166(5) Uani 1 1 d U . . O13 O 0.5862(8) 0.8864(6) 0.0258(6) 0.097(3) Uani 1 1 d U . . O14 O 0.7425(13) 0.1928(10) 0.5764(10) 0.085(4) Uani 0.50 1 d PDU . . O15 O 0.105(2) 0.2151(18) 0.9975(18) 0.169(11) Uani 0.50 1 d PU . . H25 H 0.1510 0.2446 0.9834 0.203 Uiso 0.50 1 d PR . . H26 H 0.0995 0.1782 0.9638 0.203 Uiso 0.50 1 d PR . . O16 O 0.3500(13) 0.4107(10) 0.9980(10) 0.195(6) Uani 1 1 d U . . H27 H 0.4133 0.4187 0.9996 0.234 Uiso 1 1 d R . . H28 H 0.3415 0.3618 1.0022 0.234 Uiso 1 1 d R . . C1 C 0.7659(6) 0.2488(5) 0.8074(5) 0.0347(16) Uani 1 1 d U C . C2 C 0.8453(6) 0.3081(5) 0.7941(5) 0.042(2) Uani 1 1 d U . . C3 C 0.8197(9) 0.3503(7) 0.7137(7) 0.072(3) Uani 1 1 d U C . H3A H 0.8167 0.3123 0.6703 0.107 Uiso 1 1 calc R . . H3B H 0.8722 0.3891 0.7070 0.107 Uiso 1 1 calc R . . H3C H 0.7541 0.3764 0.7126 0.107 Uiso 1 1 calc R . . C4 C 0.9442(8) 0.2643(7) 0.7952(8) 0.079(3) Uani 1 1 d U C . H4A H 0.9640 0.2432 0.8486 0.119 Uiso 1 1 calc R . . H4B H 0.9969 0.2999 0.7811 0.119 Uiso 1 1 calc R . . H4C H 0.9358 0.2215 0.7567 0.119 Uiso 1 1 calc R . . C5 C 0.8512(9) 0.3696(6) 0.8609(7) 0.067(3) Uani 1 1 d U C . H5A H 0.7828 0.3878 0.8674 0.100 Uiso 1 1 calc R . . H5B H 0.8925 0.4137 0.8470 0.100 Uiso 1 1 calc R . . H5C H 0.8819 0.3462 0.9108 0.100 Uiso 1 1 calc RD . . C6 C 0.7657(6) 0.0326(5) 0.7916(5) 0.0354(17) Uani 1 1 d U C . C7 C 0.8450(7) -0.0256(5) 0.7678(6) 0.045(2) Uani 1 1 d U . . C8 C 0.8631(8) -0.0868(6) 0.8348(6) 0.059(3) Uani 1 1 d U C . H8A H 0.8008 -0.1167 0.8377 0.088 Uiso 1 1 calc R . . H8B H 0.8825 -0.0604 0.8857 0.088 Uiso 1 1 calc R . . H8C H 0.9174 -0.1222 0.8236 0.088 Uiso 1 1 calc R . . C9 C 0.9419(8) 0.0210(6) 0.7609(7) 0.063(3) Uani 1 1 d U C . H9A H 0.9912 -0.0123 0.7384 0.094 Uiso 1 1 calc R . . H9B H 0.9704 0.0390 0.8138 0.094 Uiso 1 1 calc R . . H9C H 0.9260 0.0661 0.7261 0.094 Uiso 1 1 calc R . . C10 C 0.8093(8) -0.0638(6) 0.6903(6) 0.060(3) Uani 1 1 d U C . H10A H 0.7404 -0.0834 0.6916 0.089 Uiso 1 1 calc R . . H10B H 0.8544 -0.1072 0.6813 0.089 Uiso 1 1 calc R . . H10C H 0.8098 -0.0258 0.6471 0.089 Uiso 1 1 calc R . . C11 C 0.3863(12) 0.1899(9) 0.7307(16) 0.056(3) Uani 0.561(17) 1 d PDU C 1 H11 H 0.3919 0.1828 0.6727 0.067 Uiso 0.561(17) 1 calc PR C 1 C12 C 0.3792(7) 0.1111(5) 0.7577(8) 0.0622(19) Uani 0.561(17) 1 d PDU C 1 H12 H 0.3820 0.1212 0.8162 0.075 Uiso 0.561(17) 1 calc PR C 1 C13 C 0.2807(6) 0.0693(6) 0.7450(8) 0.067(2) Uani 0.561(17) 1 d PDU C 1 H13A H 0.2820 0.0253 0.7829 0.081 Uiso 0.561(17) 1 calc PR C 1 H13B H 0.2717 0.0474 0.6905 0.081 Uiso 0.561(17) 1 calc PR C 1 C14 C 0.1901(14) 0.1227(11) 0.7560(17) 0.069(3) Uani 0.561(17) 1 d PDU C 1 H14A H 0.1263 0.0953 0.7368 0.083 Uiso 0.561(17) 1 calc PR C 1 H14B H 0.1895 0.1340 0.8133 0.083 Uiso 0.561(17) 1 calc PR C 1 C15 C 0.1955(13) 0.1993(11) 0.7104(17) 0.069(3) Uani 0.561(17) 1 d PDU C 1 H15A H 0.1849 0.1883 0.6526 0.083 Uiso 0.561(17) 1 calc PR C 1 H15B H 0.1400 0.2339 0.7231 0.083 Uiso 0.561(17) 1 calc PR C 1 C16 C 0.2947(12) 0.2412(12) 0.7297(16) 0.065(3) Uani 0.561(17) 1 d PDU C 1 H16A H 0.2991 0.2831 0.6900 0.078 Uiso 0.561(17) 1 calc PR C 1 H16B H 0.2956 0.2662 0.7825 0.078 Uiso 0.561(17) 1 calc PR C 1 C11' C 0.3913(15) 0.1939(10) 0.780(2) 0.057(3) Uani 0.439(17) 1 d PDU C 2 H11' H 0.4019 0.1916 0.8392 0.069 Uiso 0.439(17) 1 calc PR C 2 C12' C 0.3792(7) 0.1111(5) 0.7577(8) 0.0622(19) Uani 0.439(17) 1 d PU C 2 H12' H 0.3770 0.1233 0.6998 0.075 Uiso 0.439(17) 1 calc PR C 2 C13' C 0.2807(6) 0.0693(6) 0.7450(8) 0.067(2) Uani 0.439(17) 1 d PU C 2 H13C H 0.2667 0.0446 0.7954 0.081 Uiso 0.439(17) 1 calc PR C 2 H13D H 0.2843 0.0277 0.7049 0.081 Uiso 0.439(17) 1 calc PR C 2 C14' C 0.1939(18) 0.1267(13) 0.7160(19) 0.068(4) Uani 0.439(17) 1 d PDU C 2 H14C H 0.1954 0.1370 0.6586 0.082 Uiso 0.439(17) 1 calc PR C 2 H14D H 0.1283 0.1016 0.7223 0.082 Uiso 0.439(17) 1 calc PR C 2 C15' C 0.2000(17) 0.2053(13) 0.761(2) 0.069(3) Uani 0.439(17) 1 d PDU C 2 H15C H 0.1469 0.2405 0.7352 0.083 Uiso 0.439(17) 1 calc PR C 2 H15D H 0.1849 0.1960 0.8162 0.083 Uiso 0.439(17) 1 calc PR C 2 C16' C 0.3010(15) 0.2460(15) 0.764(2) 0.065(3) Uani 0.439(17) 1 d PDU C 2 H16C H 0.3042 0.2732 0.7130 0.078 Uiso 0.439(17) 1 calc PR C 2 H16D H 0.3048 0.2862 0.8064 0.078 Uiso 0.439(17) 1 calc PR C 2 C17 C 0.7877(7) 0.1289(5) 1.0160(5) 0.051(2) Uani 1 1 d DU . . H17A H 0.8144 0.1820 1.0281 0.061 Uiso 1 1 calc R . . H17B H 0.7489 0.1131 1.0598 0.061 Uiso 1 1 calc R . . C18 C 0.8743(10) 0.0747(7) 1.0138(8) 0.091(3) Uani 1 1 d DU . . O3 O 0.9629(8) 0.0919(7) 0.9943(8) 0.148(5) Uani 1 1 d DU . . C20 C 0.836(2) 0.0777(11) 0.5458(14) 0.109(8) Uani 0.50 1 d PDU . . H20A H 0.7721 0.0495 0.5441 0.163 Uiso 0.50 1 calc PR . . H20B H 0.8882 0.0507 0.5817 0.163 Uiso 0.50 1 calc PR . . H20C H 0.8574 0.0797 0.4923 0.163 Uiso 0.50 1 calc PR . . C21 C 0.8233(17) 0.1584(13) 0.5752(17) 0.101(7) Uani 0.50 1 d PDU . . C22 C 0.9253(17) 0.1984(18) 0.582(2) 0.138(9) Uani 0.50 1 d PDU . . H22A H 0.9789 0.1591 0.5837 0.207 Uiso 0.50 1 calc PR . . H22B H 0.9345 0.2291 0.6315 0.207 Uiso 0.50 1 calc PR . . H22C H 0.9286 0.2329 0.5366 0.207 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 0.0430(2) 0.02902(19) 0.03040(19) 0.00046(13) 0.01049(14) -0.00863(13) Pt2 0.02418(17) 0.02353(17) 0.0400(2) 0.00164(12) 0.00144(13) -0.00266(12) N1 0.041(3) 0.037(3) 0.022(3) 0.001(3) 0.002(3) -0.027(3) N2 0.030(3) 0.042(3) 0.033(3) -0.001(3) -0.010(3) 0.006(3) N3 0.083(6) 0.053(5) 0.045(4) 0.010(4) 0.016(4) -0.026(4) N4 0.091(6) 0.051(5) 0.054(5) -0.010(4) 0.032(4) 0.011(4) N5 0.033(3) 0.031(3) 0.075(4) 0.007(3) 0.008(3) 0.001(3) N6 0.028(3) 0.034(3) 0.070(4) 0.008(3) -0.005(3) -0.004(3) N7 0.098(7) 0.057(6) 0.101(7) -0.001(5) 0.015(6) 0.007(6) N8 0.070(5) 0.044(5) 0.040(4) -0.005(4) 0.028(4) -0.002(4) N9 0.096(8) 0.111(10) 0.133(10) 0.060(8) 0.076(8) 0.016(8) O1 0.048(3) 0.057(3) 0.058(3) 0.002(3) 0.005(3) -0.011(3) O2 0.046(3) 0.055(3) 0.055(3) -0.003(3) 0.001(3) 0.004(3) C19 0.132(9) 0.048(6) 0.055(6) 0.003(5) -0.019(6) 0.004(6) O4 0.120(7) 0.069(5) 0.112(7) 0.018(5) -0.010(6) -0.012(5) O5 0.163(8) 0.054(5) 0.111(7) 0.006(5) 0.051(6) -0.001(5) O6 0.087(6) 0.110(7) 0.135(8) -0.024(6) 0.014(6) 0.001(6) O7 0.156(9) 0.051(5) 0.103(7) -0.009(5) 0.022(6) 0.024(5) O8 0.070(4) 0.038(4) 0.052(4) -0.006(3) 0.020(3) -0.003(3) O9 0.096(6) 0.068(5) 0.090(6) 0.008(4) 0.050(5) 0.010(5) O10 0.085(5) 0.029(3) 0.051(4) -0.001(3) 0.022(3) -0.010(3) O11 0.195(13) 0.123(11) 0.265(16) 0.066(11) 0.036(12) 0.025(10) O12 0.145(11) 0.181(12) 0.189(13) 0.036(10) 0.092(10) 0.019(9) O13 0.087(6) 0.103(7) 0.107(7) 0.024(6) 0.033(6) 0.026(6) O14 0.107(8) 0.080(7) 0.067(7) 0.010(6) 0.001(7) 0.003(7) O15 0.168(13) 0.167(13) 0.171(13) 0.014(9) 0.019(9) 0.012(9) O16 0.203(9) 0.198(9) 0.185(8) -0.004(7) 0.020(7) 0.028(7) C1 0.032(3) 0.035(4) 0.037(4) 0.002(3) 0.003(3) -0.005(3) C2 0.036(4) 0.043(4) 0.048(5) 0.005(4) 0.002(4) -0.017(4) C3 0.075(7) 0.069(7) 0.070(7) 0.020(5) 0.005(6) -0.043(6) C4 0.045(6) 0.079(7) 0.114(9) 0.005(7) 0.014(6) -0.024(5) C5 0.076(7) 0.056(6) 0.069(7) -0.008(5) 0.011(6) -0.034(5) C6 0.034(4) 0.031(4) 0.041(4) 0.008(3) 0.004(3) 0.002(3) C7 0.037(4) 0.043(5) 0.055(5) 0.000(4) 0.007(4) 0.009(4) C8 0.071(6) 0.041(5) 0.062(6) 0.005(5) 0.000(5) 0.020(5) C9 0.049(5) 0.058(6) 0.086(7) 0.008(5) 0.029(5) 0.015(5) C10 0.070(6) 0.055(6) 0.054(6) -0.002(5) 0.009(5) 0.027(5) C11 0.032(5) 0.042(5) 0.092(6) 0.003(5) 0.002(5) 0.002(4) C12 0.036(3) 0.049(3) 0.100(4) 0.000(4) 0.004(4) 0.000(3) C13 0.036(3) 0.061(4) 0.105(5) 0.012(4) 0.004(4) -0.007(3) C14 0.039(5) 0.066(6) 0.103(7) 0.007(6) 0.007(6) -0.004(5) C15 0.040(5) 0.065(6) 0.100(7) 0.003(6) 0.000(6) 0.005(5) C16 0.038(5) 0.057(6) 0.100(7) 0.003(6) 0.004(6) 0.005(5) C11' 0.033(5) 0.046(5) 0.092(6) 0.010(6) 0.007(6) 0.002(5) C12' 0.036(3) 0.049(3) 0.100(4) 0.000(4) 0.004(4) 0.000(3) C13' 0.036(3) 0.061(4) 0.105(5) 0.012(4) 0.004(4) -0.007(3) C14' 0.039(6) 0.063(6) 0.102(7) 0.007(6) 0.001(6) -0.001(6) C15' 0.041(6) 0.062(6) 0.104(7) 0.008(6) 0.004(6) 0.004(6) C16' 0.037(5) 0.057(6) 0.100(7) 0.003(6) 0.004(6) 0.008(5) C17 0.069(5) 0.053(5) 0.027(4) 0.000(4) -0.002(4) -0.003(4) C18 0.098(7) 0.095(7) 0.075(6) 0.002(6) -0.017(6) -0.013(6) O3 0.122(9) 0.162(10) 0.142(9) -0.019(8) -0.054(8) 0.038(8) C20 0.177(18) 0.102(15) 0.048(12) 0.049(11) 0.017(13) -0.020(15) C21 0.133(14) 0.096(13) 0.075(12) 0.017(11) 0.017(12) -0.008(13) C22 0.170(18) 0.146(18) 0.092(16) -0.011(15) -0.010(16) 0.003(17) _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 N1 1.995(6) . ? Pt1 N2 2.008(7) . ? Pt1 N3 2.028(7) . ? Pt1 N4 2.031(8) . ? Pt1 C17 2.130(9) . ? Pt1 Pt2 2.6819(6) . ? Pt2 O2 2.012(6) . ? Pt2 O1 2.013(6) . ? Pt2 N6 2.046(7) . ? Pt2 N5 2.051(7) . ? Pt2 O4 2.507(9) . ? N1 C1 1.297(10) . ? N2 C6 1.287(10) . ? N5 C11' 1.46(2) . ? N5 C11 1.513(19) . ? N6 C12 1.454(11) . ? N7 O6 1.236(14) . ? N7 O5 1.240(14) . ? N7 O7 1.254(13) . ? N8 O9 1.241(10) . ? N8 O8 1.250(10) . ? N8 O10 1.254(10) . ? N9 O12 1.127(15) . ? N9 O11 1.185(18) . ? N9 O13 1.200(15) . ? O1 C1 1.297(10) . ? O2 C6 1.257(10) . ? C19 C18 1.397(13) . ? O14 C21 1.230(16) . ? C1 C2 1.504(11) . ? C2 C4 1.514(15) . ? C2 C5 1.542(14) . ? C2 C3 1.544(14) . ? C6 C7 1.540(11) . ? C7 C10 1.492(14) . ? C7 C9 1.533(13) . ? C7 C8 1.544(13) . ? C11 C12 1.434(15) . ? C11 C16 1.502(16) . ? C12 C13 1.486(11) . ? C13 C14 1.543(15) . ? C14 C15 1.531(17) . ? C15 C16 1.504(16) . ? C11' C16' 1.497(17) . ? C14' C15' 1.548(18) . ? C15' C16' 1.510(18) . ? C17 C18 1.484(13) . ? C18 O3 1.296(13) . ? C20 C21 1.489(16) . ? C21 C22 1.513(17) . ? 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 N1 Pt1 N2 90.2(3) . . ? N1 Pt1 N3 174.2(3) . . ? N2 Pt1 N3 89.2(3) . . ? N1 Pt1 N4 87.4(3) . . ? N2 Pt1 N4 175.6(3) . . ? N3 Pt1 N4 92.8(4) . . ? N1 Pt1 C17 86.2(3) . . ? N2 Pt1 C17 87.1(3) . . ? N3 Pt1 C17 88.0(4) . . ? N4 Pt1 C17 89.1(4) . . ? N1 Pt1 Pt2 86.61(18) . . ? N2 Pt1 Pt2 85.16(18) . . ? N3 Pt1 Pt2 99.1(2) . . ? N4 Pt1 Pt2 98.4(3) . . ? C17 Pt1 Pt2 169.4(3) . . ? O2 Pt2 O1 90.4(3) . . ? O2 Pt2 N6 92.9(3) . . ? O1 Pt2 N6 173.7(3) . . ? O2 Pt2 N5 173.2(3) . . ? O1 Pt2 N5 91.7(3) . . ? N6 Pt2 N5 84.5(3) . . ? O2 Pt2 O4 89.2(3) . . ? O1 Pt2 O4 90.6(3) . . ? N6 Pt2 O4 84.1(3) . . ? N5 Pt2 O4 84.2(3) . . ? O2 Pt2 Pt1 80.89(19) . . ? O1 Pt2 Pt1 80.67(19) . . ? N6 Pt2 Pt1 105.2(2) . . ? N5 Pt2 Pt1 105.9(2) . . ? O4 Pt2 Pt1 166.7(3) . . ? C1 N1 Pt1 121.5(5) . . ? C6 N2 Pt1 121.6(5) . . ? C11' N5 Pt2 110.0(8) . . ? C11 N5 Pt2 106.1(7) . . ? C12 N6 Pt2 110.2(5) . . ? O6 N7 O5 118.7(12) . . ? O6 N7 O7 122.8(13) . . ? O5 N7 O7 117.7(13) . . ? O9 N8 O8 116.1(8) . . ? O9 N8 O10 123.3(8) . . ? O8 N8 O10 120.6(7) . . ? O12 N9 O11 120.6(18) . . ? O12 N9 O13 123.5(16) . . ? O11 N9 O13 115.6(14) . . ? C1 O1 Pt2 127.9(6) . . ? C6 O2 Pt2 127.5(6) . . ? O1 C1 N1 121.4(7) . . ? O1 C1 C2 123.5(7) . . ? N1 C1 C2 115.1(7) . . ? C1 C2 C4 106.7(8) . . ? C1 C2 C5 109.2(7) . . ? C4 C2 C5 111.2(9) . . ? C1 C2 C3 111.3(7) . . ? C4 C2 C3 110.2(9) . . ? C5 C2 C3 108.2(8) . . ? O2 C6 N2 122.2(8) . . ? O2 C6 C7 122.6(8) . . ? N2 C6 C7 115.0(7) . . ? C10 C7 C9 110.2(9) . . ? C10 C7 C6 111.0(8) . . ? C9 C7 C6 106.9(7) . . ? C10 C7 C8 110.7(8) . . ? C9 C7 C8 110.5(8) . . ? C6 C7 C8 107.5(7) . . ? C12 C11 C16 118.1(15) . . ? C12 C11 N5 112.2(13) . . ? C16 C11 N5 116.2(13) . . ? C11 C12 N6 113.9(9) . . ? C11 C12 C13 119.9(10) . . ? N6 C12 C13 119.0(8) . . ? C12 C13 C14 112.6(11) . . ? C15 C14 C13 111.4(15) . . ? C16 C15 C14 113.2(18) . . ? C11 C16 C15 114.4(17) . . ? N5 C11' C16' 115.5(17) . . ? C16' C15' C14' 115(2) . . ? C11' C16' C15' 115(2) . . ? C18 C17 Pt1 114.0(7) . . ? O3 C18 C19 119.1(12) . . ? O3 C18 C17 126.6(11) . . ? C19 C18 C17 114.3(10) . . ? O14 C21 C20 126.1(18) . . ? O14 C21 C22 124.0(17) . . ? C20 C21 C22 108.1(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Pt1 Pt2 O2 101.6(3) . . . . ? N2 Pt1 Pt2 O2 11.1(3) . . . . ? N3 Pt1 Pt2 O2 -77.3(3) . . . . ? N4 Pt1 Pt2 O2 -171.5(3) . . . . ? C17 Pt1 Pt2 O2 54.2(13) . . . . ? N1 Pt1 Pt2 O1 9.7(3) . . . . ? N2 Pt1 Pt2 O1 -80.8(3) . . . . ? N3 Pt1 Pt2 O1 -169.2(3) . . . . ? N4 Pt1 Pt2 O1 96.5(3) . . . . ? C17 Pt1 Pt2 O1 -37.8(13) . . . . ? N1 Pt1 Pt2 N6 -167.9(3) . . . . ? N2 Pt1 Pt2 N6 101.6(3) . . . . ? N3 Pt1 Pt2 N6 13.2(3) . . . . ? N4 Pt1 Pt2 N6 -81.0(3) . . . . ? C17 Pt1 Pt2 N6 144.7(13) . . . . ? N1 Pt1 Pt2 N5 -79.4(3) . . . . ? N2 Pt1 Pt2 N5 -169.9(3) . . . . ? N3 Pt1 Pt2 N5 101.7(3) . . . . ? N4 Pt1 Pt2 N5 7.5(3) . . . . ? C17 Pt1 Pt2 N5 -126.9(13) . . . . ? N1 Pt1 Pt2 O4 59.1(9) . . . . ? N2 Pt1 Pt2 O4 -31.4(9) . . . . ? N3 Pt1 Pt2 O4 -119.8(9) . . . . ? N4 Pt1 Pt2 O4 146.0(9) . . . . ? C17 Pt1 Pt2 O4 11.7(16) . . . . ? N2 Pt1 N1 C1 71.9(7) . . . . ? N4 Pt1 N1 C1 -111.8(7) . . . . ? C17 Pt1 N1 C1 159.0(7) . . . . ? Pt2 Pt1 N1 C1 -13.2(6) . . . . ? N1 Pt1 N2 C6 -101.0(7) . . . . ? N3 Pt1 N2 C6 84.8(7) . . . . ? C17 Pt1 N2 C6 172.8(7) . . . . ? Pt2 Pt1 N2 C6 -14.4(6) . . . . ? O1 Pt2 N5 C11' -171.0(15) . . . . ? N6 Pt2 N5 C11' 14.1(15) . . . . ? O4 Pt2 N5 C11' 98.6(15) . . . . ? Pt1 Pt2 N5 C11' -90.2(15) . . . . ? O1 Pt2 N5 C11 155.3(11) . . . . ? N6 Pt2 N5 C11 -19.7(11) . . . . ? O4 Pt2 N5 C11 64.9(11) . . . . ? Pt1 Pt2 N5 C11 -123.9(11) . . . . ? O2 Pt2 N6 C12 -173.2(7) . . . . ? N5 Pt2 N6 C12 0.5(7) . . . . ? O4 Pt2 N6 C12 -84.3(7) . . . . ? Pt1 Pt2 N6 C12 105.5(7) . . . . ? O2 Pt2 O1 C1 -91.3(7) . . . . ? N5 Pt2 O1 C1 95.2(8) . . . . ? O4 Pt2 O1 C1 179.4(8) . . . . ? Pt1 Pt2 O1 C1 -10.6(7) . . . . ? O1 Pt2 O2 C6 67.1(7) . . . . ? N6 Pt2 O2 C6 -118.3(7) . . . . ? O4 Pt2 O2 C6 157.7(7) . . . . ? Pt1 Pt2 O2 C6 -13.4(7) . . . . ? Pt2 O1 C1 N1 4.1(12) . . . . ? Pt2 O1 C1 C2 -179.3(6) . . . . ? Pt1 N1 C1 O1 9.6(11) . . . . ? Pt1 N1 C1 C2 -167.3(6) . . . . ? O1 C1 C2 C4 -99.6(10) . . . . ? N1 C1 C2 C4 77.2(10) . . . . ? O1 C1 C2 C5 140.1(9) . . . . ? N1 C1 C2 C5 -43.1(11) . . . . ? O1 C1 C2 C3 20.7(13) . . . . ? N1 C1 C2 C3 -162.5(9) . . . . ? Pt2 O2 C6 N2 6.7(12) . . . . ? Pt2 O2 C6 C7 -168.8(6) . . . . ? Pt1 N2 C6 O2 9.4(11) . . . . ? Pt1 N2 C6 C7 -174.8(5) . . . . ? O2 C6 C7 C10 -10.7(12) . . . . ? N2 C6 C7 C10 173.5(8) . . . . ? O2 C6 C7 C9 109.5(10) . . . . ? N2 C6 C7 C9 -66.2(10) . . . . ? O2 C6 C7 C8 -131.8(9) . . . . ? N2 C6 C7 C8 52.4(10) . . . . ? C11' N5 C11 C12 -65.1(18) . . . . ? Pt2 N5 C11 C12 37.0(19) . . . . ? C11' N5 C11 C16 75(3) . . . . ? Pt2 N5 C11 C16 177.3(16) . . . . ? C16 C11 C12 N6 -178.9(17) . . . . ? N5 C11 C12 N6 -39(2) . . . . ? C16 C11 C12 C13 31(3) . . . . ? N5 C11 C12 C13 170.5(13) . . . . ? Pt2 N6 C12 C11 21.0(16) . . . . ? Pt2 N6 C12 C13 171.3(9) . . . . ? C11 C12 C13 C14 -38(2) . . . . ? N6 C12 C13 C14 173.5(13) . . . . ? C12 C13 C14 C15 48(3) . . . . ? C13 C14 C15 C16 -53(3) . . . . ? C12 C11 C16 C15 -34(3) . . . . ? N5 C11 C16 C15 -171.9(18) . . . . ? C14 C15 C16 C11 46(3) . . . . ? C11 N5 C11' C16' -78(3) . . . . ? Pt2 N5 C11' C16' -166.2(19) . . . . ? N5 C11' C16' C15' 163(2) . . . . ? C14' C15' C16' C11' -42(4) . . . . ? N1 Pt1 C17 C18 -95.8(8) . . . . ? N2 Pt1 C17 C18 -5.4(8) . . . . ? N3 Pt1 C17 C18 83.9(8) . . . . ? N4 Pt1 C17 C18 176.7(8) . . . . ? Pt2 Pt1 C17 C18 -48.3(18) . . . . ? Pt1 C17 C18 O3 92.2(15) . . . . ? Pt1 C17 C18 C19 -88.4(11) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 24.51 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.636 _refine_diff_density_min -0.860 _refine_diff_density_rms 0.164 #===END data_cy _database_code_depnum_ccdc_archive 'CCDC 290073' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23.50 H53 N9 O13.50 Pt2' _chemical_formula_weight 1067.93 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' 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.220(2) _cell_length_b 14.711(3) _cell_length_c 14.962(3) _cell_angle_alpha 106.182(3) _cell_angle_beta 109.348(3) _cell_angle_gamma 98.395(3) _cell_volume 1966.6(7) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.803 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1042 _exptl_absorpt_coefficient_mu 7.172 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3933 _exptl_absorpt_correction_T_max 0.5341 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 6476 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_sigmaI/netI 0.0506 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 4.64 _diffrn_reflns_theta_max 23.98 _reflns_number_total 5008 _reflns_number_gt 3927 _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^)+(0.0845P)^2^+5.9386P] 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 5008 _refine_ls_number_parameters 477 _refine_ls_number_restraints 675 _refine_ls_R_factor_all 0.0611 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1326 _refine_ls_wR_factor_gt 0.1236 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.006 _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 0.66618(4) 0.81390(3) 0.29301(3) 0.02486(18) Uani 1 1 d . . . Pt2 Pt 0.53099(4) 0.93713(3) 0.21570(3) 0.02609(18) Uani 1 1 d . C . O1 O 0.3607(10) 0.8304(7) 0.1860(7) 0.050(3) Uani 1 1 d . . . N2 N 0.5674(10) 0.8581(8) 0.0996(8) 0.036(3) Uani 1 1 d U . . H2 H 0.5164 0.8612 0.0408 0.043 Uiso 1 1 calc R . . N3 N 0.8648(10) 0.9057(7) 0.3753(7) 0.031(2) Uani 1 1 d . . . H3D H 0.9146 0.9055 0.3348 0.047 Uiso 1 1 calc R . . H3F H 0.9118 0.8855 0.4263 0.047 Uiso 1 1 calc R . . H3E H 0.8575 0.9675 0.4017 0.047 Uiso 1 1 calc R . . N4 N 0.6059(11) 0.8438(8) 0.4120(7) 0.037(3) Uani 1 1 d . . . H4F H 0.5152 0.8515 0.3916 0.055 Uiso 1 1 calc R . . H4D H 0.6675 0.9000 0.4617 0.055 Uiso 1 1 calc R . . H4E H 0.6080 0.7933 0.4359 0.055 Uiso 1 1 calc R . . N5 N 0.6878(11) 1.0545(7) 0.2425(8) 0.035(3) Uani 1 1 d . . . H5A H 0.7745 1.0388 0.2555 0.042 Uiso 1 1 calc R A 1 H5B H 0.6672 1.0738 0.1871 0.042 Uiso 1 1 calc R A 1 N6 N 0.4893(10) 1.0332(7) 0.3254(8) 0.031(2) Uani 1 1 d D . . H6A H 0.3926 1.0182 0.3120 0.037 Uiso 1 1 calc R B 1 H6B H 0.5385 1.0300 0.3879 0.037 Uiso 1 1 calc R B 1 N7 N 0.7734(11) 0.0981(8) 0.5941(8) 0.0401(15) Uani 1 1 d DU . . N8 N 0.2544(11) 0.9140(8) 0.9789(8) 0.0401(15) Uani 1 1 d DU . . N9 N 0.9391(12) 0.8976(9) 0.6319(9) 0.0401(15) Uani 1 1 d U . . N1 N 0.4782(8) 0.7131(6) 0.2098(6) 0.0158(19) Uani 1 1 d U . . H1 H 0.4749 0.6503 0.1952 0.019 Uiso 1 1 calc RD . . O2 O 0.7232(8) 0.7810(6) 0.1742(6) 0.035(2) Uani 1 1 d . . . O3 O 0.5661(11) 0.6446(7) 0.3944(7) 0.053(3) Uani 1 1 d . . . O4 O 0.6410(11) 0.0806(9) 0.5722(9) 0.067(3) Uani 1 1 d DU . . O5 O 0.8120(9) 0.0354(7) 0.5397(7) 0.052(3) Uani 1 1 d DU . . O6 O 0.8613(15) 0.1688(11) 0.6575(11) 0.117(5) Uani 1 1 d DU . . O7 O 0.3329(16) 0.8919(12) 0.9390(11) 0.121(3) Uani 1 1 d DU . . O8 O 0.1585(14) 0.8960(12) 0.9958(11) 0.121(3) Uani 1 1 d DU . . O9 O 0.3536(15) 0.9932(10) 1.0701(10) 0.121(3) Uani 1 1 d DU . . O10 O 0.8144(10) 0.8529(8) 0.6048(7) 0.057(3) Uani 1 1 d U . . O11 O 1.0047(10) 0.8842(7) 0.5707(7) 0.045(2) Uani 1 1 d U . . O12 O 1.0106(10) 0.9591(9) 0.7195(7) 0.065(3) Uani 1 1 d U . . O13 O 0.1961(15) -0.0140(14) 0.2051(11) 0.130(6) Uani 1 1 d DU . . H13D H 0.1167 -0.0152 0.2291 0.156 Uiso 1 1 d R . . H13C H 0.2239 0.0505 0.1986 0.156 Uiso 1 1 d RD . . O14 O 1.092(2) 0.5749(17) 0.744(2) 0.096(7) Uani 0.50 1 d PDU . . C1 C 0.3601(13) 0.7402(9) 0.1769(9) 0.037(3) Uani 1 1 d D . . C2 C 0.2251(13) 0.6571(10) 0.1301(11) 0.047(4) Uani 1 1 d . . . C3 C 0.2171(19) 0.6046(13) 0.2031(16) 0.083(6) Uani 1 1 d . . . H3A H 0.1291 0.5507 0.1708 0.125 Uiso 1 1 calc R . . H3B H 0.2161 0.6509 0.2642 0.125 Uiso 1 1 calc R . . H3C H 0.3009 0.5782 0.2215 0.125 Uiso 1 1 calc R . . C4 C 0.0915(13) 0.6931(10) 0.0972(12) 0.050(4) Uani 1 1 d . . . H4A H 0.0060 0.6376 0.0677 0.075 Uiso 1 1 calc R . . H4B H 0.0937 0.7229 0.0465 0.075 Uiso 1 1 calc R . . H4C H 0.0886 0.7419 0.1558 0.075 Uiso 1 1 calc R . . C5 C 0.2311(14) 0.5865(10) 0.0331(12) 0.066(5) Uani 1 1 d D . . H5C H 0.3208 0.5665 0.0511 0.099 Uiso 1 1 calc RD . . H5D H 0.2270 0.6203 -0.0153 0.099 Uiso 1 1 calc R . . H5E H 0.1492 0.5284 0.0026 0.099 Uiso 1 1 calc R . . C6 C 0.6530(12) 0.8035(9) 0.0968(9) 0.033(3) Uani 1 1 d . . . C7 C 0.6892(14) 0.7619(10) 0.0038(9) 0.040(3) Uani 1 1 d . . . C8 C 0.6954(15) 0.6578(11) -0.0115(11) 0.049(4) Uani 1 1 d . . . H8A H 0.7187 0.6321 -0.0706 0.074 Uiso 1 1 calc R . . H8B H 0.6020 0.6180 -0.0225 0.074 Uiso 1 1 calc R . . H8C H 0.7696 0.6553 0.0486 0.074 Uiso 1 1 calc R . . C9 C 0.5726(18) 0.7670(15) -0.0928(11) 0.074(6) Uani 1 1 d . . . H9A H 0.5691 0.8353 -0.0824 0.111 Uiso 1 1 calc R . . H9B H 0.4784 0.7272 -0.1051 0.111 Uiso 1 1 calc R . . H9C H 0.5973 0.7417 -0.1513 0.111 Uiso 1 1 calc R . . C10 C 0.8357(15) 0.8283(11) 0.0248(12) 0.051(4) Uani 1 1 d . . . H10A H 0.8283 0.8957 0.0346 0.076 Uiso 1 1 calc R . . H10B H 0.8628 0.8045 -0.0328 0.076 Uiso 1 1 calc R . . H10C H 0.9088 0.8266 0.0859 0.076 Uiso 1 1 calc R . . C11 C 0.7533(13) 0.7065(9) 0.3456(9) 0.032(3) Uani 1 1 d . . . H11 H 0.8250 0.7389 0.4170 0.038 Uiso 1 1 calc R . . C12 C 0.6347(15) 0.6319(10) 0.3419(11) 0.043(3) Uani 1 1 d . . . C13 C 0.6165(16) 0.5347(9) 0.2627(11) 0.049(4) Uani 1 1 d . . . H13A H 0.6581 0.4896 0.2951 0.058 Uiso 1 1 calc R . . H13B H 0.5136 0.5027 0.2195 0.058 Uiso 1 1 calc R . . C14 C 0.6959(16) 0.5617(10) 0.2023(11) 0.058(4) Uani 1 1 d D . . H14A H 0.6342 0.5809 0.1479 0.070 Uiso 1 1 calc R . . H14B H 0.7307 0.5065 0.1717 0.070 Uiso 1 1 calc R . . C15 C 0.8232(13) 0.6498(10) 0.2812(10) 0.048(4) Uani 1 1 d D . . H15A H 0.9011 0.6275 0.3221 0.057 Uiso 1 1 calc R . . H15B H 0.8626 0.6899 0.2482 0.057 Uiso 1 1 calc R . . C16 C 0.695(3) 1.1382(19) 0.336(2) 0.036(4) Uani 0.504(15) 1 d PDU C 1 H16 H 0.7529 1.1309 0.4006 0.043 Uiso 0.504(15) 1 calc PR C 1 C17 C 0.538(3) 1.1336(12) 0.3236(18) 0.039(4) Uani 0.504(15) 1 d PDU C 1 H17 H 0.4799 1.1414 0.2592 0.047 Uiso 0.504(15) 1 calc PR C 1 C18 C 0.5472(14) 1.2147(8) 0.4174(10) 0.040(2) Uani 0.504(15) 1 d PDU C 1 H18A H 0.4497 1.2099 0.4177 0.048 Uiso 0.504(15) 1 calc PR C 1 H18B H 0.6080 1.2043 0.4788 0.048 Uiso 0.504(15) 1 calc PR C 1 C19 C 0.610(3) 1.3179(13) 0.422(2) 0.039(4) Uani 0.504(15) 1 d PDU C 1 H19A H 0.6125 1.3687 0.4822 0.047 Uiso 0.504(15) 1 calc PR C 1 H19B H 0.5523 1.3301 0.3604 0.047 Uiso 0.504(15) 1 calc PR C 1 C20 C 0.763(3) 1.3167(18) 0.4267(18) 0.042(4) Uani 0.504(15) 1 d PDU C 1 H20A H 0.8159 1.3010 0.4866 0.050 Uiso 0.504(15) 1 calc PR C 1 H20B H 0.8148 1.3827 0.4348 0.050 Uiso 0.504(15) 1 calc PR C 1 C21 C 0.7604(15) 1.2393(9) 0.3289(10) 0.043(3) Uani 0.504(15) 1 d PDU C 1 H21A H 0.8584 1.2437 0.3297 0.052 Uiso 0.504(15) 1 calc PR C 1 H21B H 0.6987 1.2483 0.2669 0.052 Uiso 0.504(15) 1 calc PR C 1 C16' C 0.652(3) 1.1488(19) 0.285(2) 0.038(4) Uani 0.496(15) 1 d PDU C 2 H16' H 0.5672 1.1544 0.2308 0.045 Uiso 0.496(15) 1 calc PR C 2 C17' C 0.606(3) 1.1310(15) 0.368(2) 0.034(4) Uani 0.496(15) 1 d PDU C 2 H17' H 0.6917 1.1268 0.4216 0.041 Uiso 0.496(15) 1 calc PR C 2 C18' C 0.5472(14) 1.2147(8) 0.4174(10) 0.040(2) Uani 0.496(15) 1 d PDU C 2 H18C H 0.5267 1.2042 0.4745 0.048 Uiso 0.496(15) 1 calc PR C 2 H18D H 0.4587 1.2194 0.3676 0.048 Uiso 0.496(15) 1 calc PR C 2 C19' C 0.674(3) 1.3087(16) 0.4553(19) 0.039(4) Uani 0.496(15) 1 d PDU C 2 H19C H 0.6473 1.3660 0.4911 0.047 Uiso 0.496(15) 1 calc PR C 2 H19D H 0.7600 1.3011 0.5047 0.047 Uiso 0.496(15) 1 calc PR C 2 C20' C 0.712(3) 1.3301(15) 0.371(2) 0.042(4) Uani 0.496(15) 1 d PDU C 2 H20C H 0.6279 1.3360 0.3180 0.050 Uiso 0.496(15) 1 calc PR C 2 H20D H 0.7910 1.3908 0.3978 0.050 Uiso 0.496(15) 1 calc PR C 2 C21' C 0.7604(15) 1.2393(9) 0.3289(10) 0.043(3) Uani 0.496(15) 1 d PDU C 2 H21C H 0.7964 1.2485 0.2773 0.052 Uiso 0.496(15) 1 calc PR C 2 H21D H 0.8417 1.2347 0.3846 0.052 Uiso 0.496(15) 1 calc PR C 2 C22 C 0.976(3) 0.5945(18) 0.7155(18) 0.056(6) Uani 0.50 1 d PDU . . C23 C 0.876(2) 0.579(2) 0.6080(19) 0.072(6) Uani 0.50 1 d PDU . . H23A H 0.8464 0.5091 0.5656 0.086 Uiso 0.50 1 calc PR . . H23B H 0.9267 0.6169 0.5780 0.086 Uiso 0.50 1 calc PR . . C24 C 0.744(3) 0.615(2) 0.612(2) 0.066(6) Uani 0.50 1 d PDU . . H24A H 0.7271 0.6623 0.5761 0.079 Uiso 0.50 1 calc PR . . H24B H 0.6571 0.5595 0.5820 0.079 Uiso 0.50 1 calc PR . . C25 C 0.786(3) 0.663(2) 0.722(2) 0.068(6) Uani 0.50 1 d PDU . . H25A H 0.7718 0.7301 0.7351 0.081 Uiso 0.50 1 calc PR . . H25B H 0.7192 0.6262 0.7432 0.081 Uiso 0.50 1 calc PR . . C26 C 0.935(3) 0.671(2) 0.788(2) 0.069(6) Uani 0.50 1 d PDU . . H26A H 0.9395 0.6537 0.8478 0.082 Uiso 0.50 1 calc PR . . H26B H 0.9988 0.7372 0.8096 0.082 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 0.0181(3) 0.0228(3) 0.0246(3) -0.0002(2) 0.0049(2) 0.00428(19) Pt2 0.0189(3) 0.0233(3) 0.0293(3) 0.0012(2) 0.0080(2) 0.0056(2) O1 0.048(6) 0.042(6) 0.053(6) 0.005(5) 0.023(5) 0.011(5) N2 0.026(5) 0.038(6) 0.035(5) 0.000(4) 0.009(4) 0.016(4) N3 0.021(5) 0.029(6) 0.035(6) 0.002(5) 0.008(4) 0.007(4) N4 0.036(6) 0.041(7) 0.032(6) 0.002(5) 0.017(5) 0.020(5) N5 0.034(6) 0.037(6) 0.039(6) 0.011(5) 0.023(5) 0.011(5) N6 0.027(5) 0.020(6) 0.041(6) 0.005(5) 0.014(5) 0.004(4) N7 0.036(3) 0.065(4) 0.051(3) 0.035(3) 0.035(3) 0.030(3) N8 0.036(3) 0.065(4) 0.051(3) 0.035(3) 0.035(3) 0.030(3) N9 0.036(3) 0.065(4) 0.051(3) 0.035(3) 0.035(3) 0.030(3) N1 0.006(4) 0.008(4) 0.028(4) 0.005(3) 0.001(3) 0.002(3) O2 0.026(5) 0.047(6) 0.029(5) 0.005(4) 0.013(4) 0.014(4) O3 0.063(7) 0.048(6) 0.048(6) 0.017(5) 0.027(5) 0.004(5) O4 0.066(7) 0.088(8) 0.086(7) 0.053(6) 0.049(6) 0.042(6) O5 0.037(5) 0.072(7) 0.048(6) 0.010(5) 0.028(4) 0.014(5) O6 0.096(9) 0.088(10) 0.109(10) -0.033(8) 0.038(8) -0.004(8) O7 0.131(7) 0.130(7) 0.107(6) 0.049(6) 0.035(6) 0.065(6) O8 0.131(7) 0.130(7) 0.107(6) 0.049(6) 0.035(6) 0.065(6) O9 0.131(7) 0.130(7) 0.107(6) 0.049(6) 0.035(6) 0.065(6) O10 0.031(5) 0.071(7) 0.059(6) 0.021(5) 0.017(4) -0.012(5) O11 0.044(5) 0.042(6) 0.046(5) 0.016(4) 0.011(4) 0.016(4) O12 0.037(5) 0.092(8) 0.036(6) -0.009(5) 0.012(4) 0.001(5) O13 0.080(9) 0.190(14) 0.108(10) 0.018(9) 0.034(8) 0.070(9) O14 0.090(14) 0.059(12) 0.144(16) 0.042(12) 0.045(13) 0.023(11) C1 0.036(8) 0.025(8) 0.036(7) -0.002(6) 0.014(6) -0.006(6) C2 0.017(7) 0.039(9) 0.052(9) -0.001(7) -0.006(6) -0.004(6) C3 0.051(11) 0.056(12) 0.134(18) 0.046(12) 0.022(11) -0.001(9) C4 0.021(7) 0.025(8) 0.081(11) 0.001(7) 0.010(7) -0.006(6) C5 0.028(8) 0.033(9) 0.090(12) -0.014(8) -0.005(8) 0.012(7) C6 0.019(6) 0.036(8) 0.034(7) 0.003(6) 0.007(6) 0.007(6) C7 0.040(8) 0.051(9) 0.033(7) 0.011(6) 0.015(6) 0.025(7) C8 0.045(8) 0.053(10) 0.041(8) -0.005(7) 0.021(7) 0.018(7) C9 0.069(11) 0.124(17) 0.030(8) 0.015(9) 0.020(8) 0.055(11) C10 0.058(10) 0.058(10) 0.071(10) 0.035(8) 0.046(9) 0.039(8) C11 0.030(7) 0.028(7) 0.031(7) 0.011(6) 0.004(5) 0.011(6) C12 0.045(8) 0.030(8) 0.042(8) 0.008(6) 0.005(7) 0.007(6) C13 0.056(9) 0.019(7) 0.059(9) 0.005(7) 0.018(8) 0.005(6) C14 0.082(12) 0.032(9) 0.049(9) 0.001(7) 0.024(9) 0.014(8) C15 0.040(8) 0.044(9) 0.049(9) 0.003(7) 0.011(7) 0.023(7) C16 0.045(7) 0.027(6) 0.048(7) 0.009(6) 0.033(6) 0.015(6) C17 0.050(7) 0.027(6) 0.047(7) 0.011(6) 0.031(6) 0.010(6) C18 0.051(5) 0.028(4) 0.048(5) 0.007(4) 0.031(4) 0.012(4) C19 0.049(7) 0.024(6) 0.049(7) 0.010(6) 0.025(6) 0.015(6) C20 0.050(7) 0.028(6) 0.051(7) 0.011(6) 0.025(6) 0.011(6) C21 0.050(5) 0.028(4) 0.052(5) 0.010(4) 0.026(4) 0.009(4) C16' 0.050(7) 0.027(6) 0.045(7) 0.012(6) 0.030(6) 0.012(6) C17' 0.050(7) 0.022(6) 0.044(7) 0.012(6) 0.032(6) 0.015(6) C18' 0.051(5) 0.028(4) 0.048(5) 0.007(4) 0.031(4) 0.012(4) C19' 0.054(7) 0.023(6) 0.047(7) 0.008(6) 0.029(6) 0.016(6) C20' 0.052(7) 0.025(6) 0.052(7) 0.013(6) 0.024(6) 0.011(6) C21' 0.050(5) 0.028(4) 0.052(5) 0.010(4) 0.026(4) 0.009(4) C22 0.054(11) 0.036(10) 0.111(13) 0.045(10) 0.053(10) 0.024(9) C23 0.070(11) 0.048(11) 0.103(12) 0.006(10) 0.066(10) -0.006(10) C24 0.066(11) 0.048(11) 0.098(12) 0.032(10) 0.046(10) 0.015(9) C25 0.066(11) 0.060(11) 0.101(12) 0.032(10) 0.057(10) 0.023(10) C26 0.073(11) 0.055(11) 0.095(12) 0.036(10) 0.050(10) 0.009(10) _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 N1 1.999(8) . ? Pt1 O2 2.006(8) . ? Pt1 N3 2.019(9) . ? Pt1 N4 2.027(9) . ? Pt1 C11 2.132(12) . ? Pt1 Pt2 2.7157(8) . ? Pt2 N2 1.984(9) . ? Pt2 O1 1.999(9) . ? Pt2 N5 2.022(10) . ? Pt2 N6 2.054(9) . ? O1 C1 1.295(16) . ? N2 C6 1.274(15) . ? N2 H2 0.8800 . ? N3 H3D 0.9100 . ? N3 H3F 0.9100 . ? N3 H3E 0.9100 . ? N4 H4F 0.9100 . ? N4 H4D 0.9100 . ? N4 H4E 0.9100 . ? N5 C16' 1.51(3) . ? N5 C16 1.55(3) . ? N5 H5A 0.9200 . ? N5 H5B 0.9200 . ? N6 C17 1.500(17) . ? N6 C17' 1.54(3) . ? N6 H6A 0.9200 . ? N6 H6B 0.9200 . ? N7 O6 1.183(12) . ? N7 O4 1.249(11) . ? N7 O5 1.253(11) . ? N8 O8 1.106(12) . ? N8 O7 1.179(12) . ? N8 O9 1.448(13) . ? N9 O10 1.219(13) . ? N9 O12 1.257(14) . ? N9 O11 1.294(12) . ? N1 C1 1.310(16) . ? N1 H1 0.8800 . ? O2 C6 1.303(15) . ? O3 C12 1.210(16) . ? O13 H13D 0.9900 . ? O13 H13C 0.9917 . ? O14 C22 1.231(16) . ? C1 C2 1.509(16) . ? C2 C4 1.515(19) . ? C2 C3 1.52(2) . ? C2 C5 1.56(2) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5C 0.9800 . ? C5 H5D 0.9800 . ? C5 H5E 0.9800 . ? C6 C7 1.543(17) . ? C7 C8 1.50(2) . ? C7 C10 1.544(19) . ? C7 C9 1.57(2) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.486(18) . ? C11 C15 1.523(17) . ? C11 H11 1.0000 . ? C12 C13 1.522(18) . ? C13 C14 1.49(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.551(14) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.541(18) . ? C16 C21 1.58(3) . ? C16 H16 1.0000 . ? C17 C18 1.535(17) . ? C17 H17 1.0000 . ? C18 C19 1.534(13) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.548(18) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.573(17) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C16' C17' 1.540(18) . ? C16' H16' 1.0000 . ? C17' H17' 1.0000 . ? C19' C20' 1.543(18) . ? C19' H19C 0.9900 . ? C19' H19D 0.9900 . ? C20' H20C 0.9900 . ? C20' H20D 0.9900 . ? C22 C23 1.524(17) . ? C22 C26 1.532(18) . ? C23 C24 1.529(18) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.488(19) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.487(19) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? 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 N1 Pt1 O2 89.9(3) . . ? N1 Pt1 N3 174.8(4) . . ? O2 Pt1 N3 87.7(4) . . ? N1 Pt1 N4 89.0(4) . . ? O2 Pt1 N4 178.7(4) . . ? N3 Pt1 N4 93.4(4) . . ? N1 Pt1 C11 89.4(4) . . ? O2 Pt1 C11 93.0(4) . . ? N3 Pt1 C11 86.2(4) . . ? N4 Pt1 C11 86.3(4) . . ? N1 Pt1 Pt2 85.1(2) . . ? O2 Pt1 Pt2 87.1(3) . . ? N3 Pt1 Pt2 99.3(3) . . ? N4 Pt1 Pt2 93.5(3) . . ? C11 Pt1 Pt2 174.5(3) . . ? N2 Pt2 O1 91.6(4) . . ? N2 Pt2 N5 91.3(4) . . ? O1 Pt2 N5 173.6(4) . . ? N2 Pt2 N6 171.8(4) . . ? O1 Pt2 N6 92.3(4) . . ? N5 Pt2 N6 84.1(4) . . ? N2 Pt2 Pt1 78.3(3) . . ? O1 Pt2 Pt1 80.1(3) . . ? N5 Pt2 Pt1 106.1(3) . . ? N6 Pt2 Pt1 109.5(3) . . ? C1 O1 Pt2 125.8(8) . . ? C6 N2 Pt2 130.2(9) . . ? C6 N2 H2 114.9 . . ? Pt2 N2 H2 114.9 . . ? Pt1 N3 H3D 109.5 . . ? Pt1 N3 H3F 109.5 . . ? H3D N3 H3F 109.5 . . ? Pt1 N3 H3E 109.5 . . ? H3D N3 H3E 109.5 . . ? H3F N3 H3E 109.5 . . ? Pt1 N4 H4F 109.5 . . ? Pt1 N4 H4D 109.5 . . ? H4F N4 H4D 109.5 . . ? Pt1 N4 H4E 109.5 . . ? H4F N4 H4E 109.5 . . ? H4D N4 H4E 109.5 . . ? C16' N5 Pt2 110.8(11) . . ? C16 N5 Pt2 107.4(11) . . ? C16' N5 H5A 131.0 . . ? C16 N5 H5A 110.2 . . ? Pt2 N5 H5A 110.2 . . ? C16' N5 H5B 80.8 . . ? C16 N5 H5B 110.2 . . ? Pt2 N5 H5B 110.2 . . ? H5A N5 H5B 108.5 . . ? C17 N6 Pt2 106.4(8) . . ? C17' N6 Pt2 107.3(8) . . ? C17' N6 H6A 133.0 . . ? Pt2 N6 H6A 110.4 . . ? C17' N6 H6B 82.5 . . ? Pt2 N6 H6B 110.4 . . ? O6 N7 O4 126.0(13) . . ? O6 N7 O5 119.0(11) . . ? O4 N7 O5 115.0(11) . . ? O8 N8 O7 151.8(16) . . ? O8 N8 O9 103.6(11) . . ? O7 N8 O9 100.6(11) . . ? O10 N9 O12 122.6(10) . . ? O10 N9 O11 121.0(11) . . ? O12 N9 O11 116.4(10) . . ? C1 N1 Pt1 120.2(7) . . ? C1 N1 H1 119.9 . . ? Pt1 N1 H1 119.9 . . ? C6 O2 Pt1 117.6(7) . . ? H13D O13 H13C 109.3 . . ? O1 C1 N1 122.5(11) . . ? O1 C1 C2 123.8(13) . . ? N1 C1 C2 113.7(11) . . ? C1 C2 C4 111.5(12) . . ? C1 C2 C3 111.1(12) . . ? C4 C2 C3 109.6(13) . . ? C1 C2 C5 106.2(11) . . ? C4 C2 C5 107.3(11) . . ? C3 C2 C5 111.1(14) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5C 109.5 . . ? C2 C5 H5D 109.5 . . ? H5C C5 H5D 109.5 . . ? C2 C5 H5E 109.5 . . ? H5C C5 H5E 109.5 . . ? H5D C5 H5E 109.5 . . ? N2 C6 O2 122.9(11) . . ? N2 C6 C7 123.5(12) . . ? O2 C6 C7 113.6(10) . . ? C8 C7 C6 110.0(11) . . ? C8 C7 C10 111.3(11) . . ? C6 C7 C10 106.7(10) . . ? C8 C7 C9 109.9(12) . . ? C6 C7 C9 110.0(10) . . ? C10 C7 C9 108.9(13) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C15 105.7(11) . . ? C12 C11 Pt1 108.8(8) . . ? C15 C11 Pt1 114.1(9) . . ? C12 C11 H11 109.4 . . ? C15 C11 H11 109.4 . . ? Pt1 C11 H11 109.4 . . ? O3 C12 C11 126.4(12) . . ? O3 C12 C13 125.1(13) . . ? C11 C12 C13 108.4(12) . . ? C14 C13 C12 104.4(11) . . ? C14 C13 H13A 110.9 . . ? C12 C13 H13A 110.9 . . ? C14 C13 H13B 110.9 . . ? C12 C13 H13B 110.9 . . ? H13A C13 H13B 108.9 . . ? C13 C14 C15 103.5(11) . . ? C13 C14 H14A 111.1 . . ? C15 C14 H14A 111.1 . . ? C13 C14 H14B 111.1 . . ? C15 C14 H14B 111.1 . . ? H14A C14 H14B 109.0 . . ? C11 C15 C14 102.4(10) . . ? C11 C15 H15A 111.3 . . ? C14 C15 H15A 111.3 . . ? C11 C15 H15B 111.3 . . ? C14 C15 H15B 111.3 . . ? H15A C15 H15B 109.2 . . ? C17 C16 N5 106.1(17) . . ? C17 C16 C21 107.6(18) . . ? N5 C16 C21 107.9(18) . . ? C17 C16 H16 111.6 . . ? N5 C16 H16 111.6 . . ? C21 C16 H16 111.6 . . ? N6 C17 C18 111.9(14) . . ? N6 C17 C16 101.5(17) . . ? C18 C17 C16 105.6(17) . . ? N6 C17 H17 112.4 . . ? C18 C17 H17 112.4 . . ? C16 C17 H17 112.4 . . ? C19 C18 C17 112.8(14) . . ? C19 C18 H18A 109.0 . . ? C17 C18 H18A 109.0 . . ? C19 C18 H18B 109.0 . . ? C17 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? C18 C19 C20 103.4(17) . . ? C18 C19 H19A 111.1 . . ? C20 C19 H19A 111.1 . . ? C18 C19 H19B 111.1 . . ? C20 C19 H19B 111.1 . . ? H19A C19 H19B 109.0 . . ? C19 C20 C21 111.8(18) . . ? C19 C20 H20A 109.2 . . ? C21 C20 H20A 109.2 . . ? C19 C20 H20B 109.2 . . ? C21 C20 H20B 109.2 . . ? H20A C20 H20B 107.9 . . ? C20 C21 C16 102.7(17) . . ? C20 C21 H21A 111.2 . . ? C16 C21 H21A 111.2 . . ? C20 C21 H21B 111.2 . . ? C16 C21 H21B 111.2 . . ? H21A C21 H21B 109.1 . . ? N5 C16' C17' 102.1(17) . . ? N5 C16' H16' 108.8 . . ? C17' C16' H16' 108.8 . . ? C16' C17' N6 111.0(19) . . ? C16' C17' H17' 108.1 . . ? N6 C17' H17' 108.1 . . ? C20' C19' H19C 108.7 . . ? C20' C19' H19D 108.7 . . ? H19C C19' H19D 107.6 . . ? C19' C20' H20C 111.4 . . ? C19' C20' H20D 111.4 . . ? H20C C20' H20D 109.2 . . ? O14 C22 C23 128.5(18) . . ? O14 C22 C26 121.2(18) . . ? C23 C22 C26 107(2) . . ? C22 C23 C24 109(2) . . ? C22 C23 H23A 110.0 . . ? C24 C23 H23A 110.0 . . ? C22 C23 H23B 110.0 . . ? C24 C23 H23B 110.0 . . ? H23A C23 H23B 108.4 . . ? C25 C24 C23 102(2) . . ? C25 C24 H24A 111.3 . . ? C23 C24 H24A 111.3 . . ? C25 C24 H24B 111.3 . . ? C23 C24 H24B 111.3 . . ? H24A C24 H24B 109.2 . . ? C26 C25 C24 116(2) . . ? C26 C25 H25A 108.4 . . ? C24 C25 H25A 108.4 . . ? C26 C25 H25B 108.4 . . ? C24 C25 H25B 108.4 . . ? H25A C25 H25B 107.4 . . ? C25 C26 C22 101(2) . . ? C25 C26 H26A 111.5 . . ? C22 C26 H26A 111.5 . . ? C25 C26 H26B 111.5 . . ? C22 C26 H26B 111.5 . . ? H26A C26 H26B 109.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Pt1 Pt2 N2 -76.2(4) . . . . ? O2 Pt1 Pt2 N2 13.9(4) . . . . ? N3 Pt1 Pt2 N2 101.1(4) . . . . ? N4 Pt1 Pt2 N2 -164.9(4) . . . . ? N1 Pt1 Pt2 O1 17.6(4) . . . . ? O2 Pt1 Pt2 O1 107.7(4) . . . . ? N3 Pt1 Pt2 O1 -165.1(4) . . . . ? N4 Pt1 Pt2 O1 -71.1(4) . . . . ? N1 Pt1 Pt2 N5 -164.1(4) . . . . ? O2 Pt1 Pt2 N5 -74.0(4) . . . . ? N3 Pt1 Pt2 N5 13.2(4) . . . . ? N4 Pt1 Pt2 N5 107.2(4) . . . . ? N1 Pt1 Pt2 N6 106.5(4) . . . . ? O2 Pt1 Pt2 N6 -163.4(4) . . . . ? N3 Pt1 Pt2 N6 -76.2(4) . . . . ? N4 Pt1 Pt2 N6 17.8(4) . . . . ? N2 Pt2 O1 C1 54.2(11) . . . . ? N6 Pt2 O1 C1 -133.0(10) . . . . ? Pt1 Pt2 O1 C1 -23.6(10) . . . . ? O1 Pt2 N2 C6 -96.3(12) . . . . ? Pt1 Pt2 N2 C6 -16.8(11) . . . . ? N2 Pt2 N5 C16' 148.0(14) . . . . ? N6 Pt2 N5 C16' -25.2(14) . . . . ? Pt1 Pt2 N5 C16' -133.8(14) . . . . ? N2 Pt2 N5 C16 -179.4(14) . . . . ? N6 Pt2 N5 C16 7.4(13) . . . . ? Pt1 Pt2 N5 C16 -101.3(13) . . . . ? O1 Pt2 N6 C17 -147.7(12) . . . . ? Pt1 Pt2 N6 C17 132.0(12) . . . . ? O1 Pt2 N6 C17' -179.3(13) . . . . ? Pt1 Pt2 N6 C17' 100.5(12) . . . . ? O2 Pt1 N1 C1 -106.1(9) . . . . ? N4 Pt1 N1 C1 74.6(9) . . . . ? C11 Pt1 N1 C1 160.9(9) . . . . ? Pt2 Pt1 N1 C1 -19.0(8) . . . . ? N1 Pt1 O2 C6 67.9(9) . . . . ? N3 Pt1 O2 C6 -116.7(9) . . . . ? C11 Pt1 O2 C6 157.2(9) . . . . ? Pt2 Pt1 O2 C6 -17.3(8) . . . . ? Pt2 O1 C1 N1 16.9(17) . . . . ? Pt2 O1 C1 C2 -164.5(10) . . . . ? Pt1 N1 C1 O1 8.2(16) . . . . ? Pt1 N1 C1 C2 -170.6(8) . . . . ? O1 C1 C2 C4 -0.9(19) . . . . ? N1 C1 C2 C4 177.8(12) . . . . ? O1 C1 C2 C3 -123.4(15) . . . . ? N1 C1 C2 C3 55.3(16) . . . . ? O1 C1 C2 C5 115.7(14) . . . . ? N1 C1 C2 C5 -65.6(15) . . . . ? Pt2 N2 C6 O2 8.6(19) . . . . ? Pt2 N2 C6 C7 -168.3(9) . . . . ? Pt1 O2 C6 N2 11.3(16) . . . . ? Pt1 O2 C6 C7 -171.5(8) . . . . ? N2 C6 C7 C8 -139.4(13) . . . . ? O2 C6 C7 C8 43.4(14) . . . . ? N2 C6 C7 C10 99.7(14) . . . . ? O2 C6 C7 C10 -77.5(14) . . . . ? N2 C6 C7 C9 -18.3(19) . . . . ? O2 C6 C7 C9 164.5(12) . . . . ? N1 Pt1 C11 C12 -27.0(9) . . . . ? O2 Pt1 C11 C12 -116.9(9) . . . . ? N3 Pt1 C11 C12 155.7(9) . . . . ? N4 Pt1 C11 C12 62.0(9) . . . . ? N1 Pt1 C11 C15 90.7(8) . . . . ? O2 Pt1 C11 C15 0.8(8) . . . . ? N3 Pt1 C11 C15 -86.6(9) . . . . ? N4 Pt1 C11 C15 179.7(9) . . . . ? C15 C11 C12 O3 168.7(14) . . . . ? Pt1 C11 C12 O3 -68.4(16) . . . . ? C15 C11 C12 C13 -9.4(14) . . . . ? Pt1 C11 C12 C13 113.5(10) . . . . ? O3 C12 C13 C14 166.2(14) . . . . ? C11 C12 C13 C14 -15.7(15) . . . . ? C12 C13 C14 C15 33.9(15) . . . . ? C12 C11 C15 C14 29.7(14) . . . . ? Pt1 C11 C15 C14 -89.8(12) . . . . ? C13 C14 C15 C11 -39.6(15) . . . . ? C16' N5 C16 C17 62(2) . . . . ? Pt2 N5 C16 C17 -40(2) . . . . ? C16' N5 C16 C21 -53(3) . . . . ? Pt2 N5 C16 C21 -154.9(12) . . . . ? C17' N6 C17 C18 -70(2) . . . . ? Pt2 N6 C17 C18 -166.4(13) . . . . ? C17' N6 C17 C16 42.1(19) . . . . ? Pt2 N6 C17 C16 -54.1(18) . . . . ? N5 C16 C17 N6 62(2) . . . . ? C21 C16 C17 N6 176.8(16) . . . . ? N5 C16 C17 C18 178.5(16) . . . . ? C21 C16 C17 C18 -66(2) . . . . ? N6 C17 C18 C19 175.1(17) . . . . ? C16 C17 C18 C19 65(2) . . . . ? C17 C18 C19 C20 -62(2) . . . . ? C18 C19 C20 C21 63(3) . . . . ? C19 C20 C21 C16 -67(2) . . . . ? C17 C16 C21 C20 66(2) . . . . ? N5 C16 C21 C20 -179.6(16) . . . . ? C16 N5 C16' C17' -42(2) . . . . ? Pt2 N5 C16' C17' 47(2) . . . . ? N5 C16' C17' N6 -52(3) . . . . ? C17 N6 C17' C16' -60(2) . . . . ? Pt2 N6 C17' C16' 33(2) . . . . ? O14 C22 C23 C24 180(3) . . . . ? C26 C22 C23 C24 -20(3) . . . . ? C22 C23 C24 C25 9(3) . . . . ? C23 C24 C25 C26 6(4) . . . . ? C24 C25 C26 C22 -18(4) . . . . ? O14 C22 C26 C25 -176(3) . . . . ? C23 C22 C26 C25 22(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O13 H13D O12 0.99 1.89 2.821(16) 154.7 2_666 N6 H6B O4 0.92 2.44 3.313(15) 157.6 1_565 N6 H6A O13 0.92 2.00 2.797(17) 144.5 1_565 N5 H5B O7 0.92 2.08 2.984(19) 165.7 2_676 N5 H5A O11 0.92 2.62 3.232(14) 124.6 2_776 N5 H5A O12 0.92 2.10 2.990(14) 163.9 2_776 N4 H4D O5 0.91 2.05 2.938(14) 163.7 1_565 N4 H4F O4 0.91 2.14 2.955(14) 148.7 2_666 N3 H3E O11 0.91 2.26 2.945(14) 131.2 2_776 N3 H3E O5 0.91 2.26 2.924(12) 129.7 1_565 N3 H3D O12 0.91 2.47 3.101(16) 127.1 2_776 N2 H2 O7 0.88 2.19 2.995(19) 152.5 1_554 N4 H4E O3 0.91 2.04 2.823(15) 143.9 . N3 H3F O11 0.91 2.06 2.928(14) 159.4 . _diffrn_measured_fraction_theta_max 0.814 _diffrn_reflns_theta_full 23.98 _diffrn_measured_fraction_theta_full 0.814 _refine_diff_density_max 3.903 _refine_diff_density_min -1.404 _refine_diff_density_rms 0.206 #===END data_l266 _database_code_depnum_ccdc_archive 'CCDC 290074' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H104 Cl4 N12 O24 Pt4' _chemical_formula_weight 2107.55 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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.807(2) _cell_length_b 13.486(2) _cell_length_c 21.694(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.337(3) _cell_angle_gamma 90.00 _cell_volume 3746.0(11) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.868 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 7.661 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2229 _exptl_absorpt_correction_T_max 0.2961 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 20585 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_sigmaI/netI 0.0586 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 26.50 _reflns_number_total 7750 _reflns_number_gt 6516 _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^)+(0.0430P)^2^+26.1143P] 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 7750 _refine_ls_number_parameters 412 _refine_ls_number_restraints 273 _refine_ls_R_factor_all 0.0537 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.1115 _refine_ls_wR_factor_gt 0.1051 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.010 _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 -0.00219(2) 0.04446(2) 0.068984(12) 0.01752(9) Uani 1 1 d . . . Pt2 Pt -0.01181(2) 0.17859(2) 0.181142(12) 0.02062(9) Uani 1 1 d . D . Cl1 Cl 0.21227(18) 0.41687(16) 0.27175(10) 0.0363(5) Uani 1 1 d U . . Cl2 Cl 0.7298(2) 0.34148(18) 0.26837(10) 0.0444(6) Uani 1 1 d . . . N1 N -0.1291(6) 0.2279(5) 0.1261(3) 0.0335(17) Uani 1 1 d D . . H1 H -0.1737 0.2670 0.1446 0.040 Uiso 1 1 calc RD . . N2 N 0.0960(6) 0.2444(5) 0.1299(3) 0.0281(15) Uani 1 1 d . . . H2 H 0.1146 0.3038 0.1430 0.034 Uiso 1 1 calc R . . N3 N 0.1023(5) -0.0616(5) 0.0941(3) 0.0278(15) Uani 1 1 d . . . H3D H 0.0707 -0.1073 0.1182 0.042 Uiso 1 1 calc R . . H3E H 0.1565 -0.0334 0.1155 0.042 Uiso 1 1 calc R . . H3F H 0.1267 -0.0918 0.0598 0.042 Uiso 1 1 calc R . . N4 N -0.1220(5) -0.0509(5) 0.0786(3) 0.0276(15) Uani 1 1 d . . . H4D H -0.1832 -0.0166 0.0788 0.041 Uiso 1 1 calc R . . H4E H -0.1137 -0.0846 0.1147 0.041 Uiso 1 1 calc R . . H4F H -0.1233 -0.0946 0.0466 0.041 Uiso 1 1 calc R . . N5 N -0.1130(5) 0.1172(6) 0.2415(3) 0.0289(15) Uani 1 1 d . . . H5D H -0.1759 0.1502 0.2403 0.035 Uiso 1 1 calc R A 1 H5E H -0.1247 0.0515 0.2322 0.035 Uiso 1 1 calc R A 1 N6 N 0.0989(5) 0.1381(5) 0.2467(3) 0.0255(14) Uani 1 1 d . . . H6A H 0.1496 0.1001 0.2288 0.031 Uiso 1 1 calc R B 1 H6B H 0.1301 0.1938 0.2632 0.031 Uiso 1 1 calc R B 1 O1 O -0.1058(4) 0.1465(4) 0.0349(2) 0.0245(11) Uani 1 1 d . . . O2 O 0.1213(4) 0.1347(4) 0.0515(2) 0.0255(12) Uani 1 1 d . . . O3 O 0.6545(6) 1.0069(6) 0.0683(4) 0.063(2) Uani 1 1 d . . . O4 O 0.9905(7) 0.7501(6) 0.1194(4) 0.067(2) Uani 1 1 d . . . O5 O 0.2136(7) 0.4999(5) 0.3115(4) 0.061(2) Uani 1 1 d U . . O6 O 0.3155(8) 0.4126(8) 0.2475(5) 0.094(3) Uani 1 1 d U . . O7 O 0.1370(8) 0.4304(6) 0.2237(4) 0.083(3) Uani 1 1 d U . . O8 O 0.1937(6) 0.3280(5) 0.3052(4) 0.0553(19) Uani 1 1 d U . . O9 O 0.6941(6) 0.2502(6) 0.2429(4) 0.064(2) Uani 1 1 d . . . O10 O 0.7887(6) 0.3923(6) 0.2235(3) 0.0563(19) Uani 1 1 d . . . O11 O 0.6422(7) 0.4000(5) 0.2862(4) 0.063(2) Uani 1 1 d . . . O12 O 0.7932(9) 0.3204(6) 0.3215(4) 0.081(3) Uani 1 1 d . . . C1 C -0.1507(6) 0.2123(6) 0.0683(4) 0.0280(17) Uani 1 1 d U C . C2 C -0.2321(7) 0.2749(6) 0.0347(4) 0.038(2) Uani 1 1 d DU . . C3 C -0.3285(9) 0.2930(11) 0.0737(6) 0.092(3) Uani 1 1 d DU C . H3A H -0.3078 0.3282 0.1115 0.138 Uiso 1 1 calc RD . . H3B H -0.3602 0.2293 0.0843 0.138 Uiso 1 1 calc R . . H3C H -0.3793 0.3331 0.0501 0.138 Uiso 1 1 calc R . . C4 C -0.2751(10) 0.2247(10) -0.0226(6) 0.092(3) Uani 1 1 d DU C . H4A H -0.3474 0.2460 -0.0302 0.138 Uiso 1 1 calc R . . H4B H -0.2732 0.1527 -0.0169 0.138 Uiso 1 1 calc R . . H4C H -0.2327 0.2429 -0.0579 0.138 Uiso 1 1 calc R . . C5 C -0.203(5) 0.3799(19) 0.026(2) 0.092(3) Uani 0.36(9) 1 d PDU C 1 H5A H -0.1767 0.4076 0.0648 0.138 Uiso 0.36(9) 1 calc PR C 1 H5B H -0.2648 0.4174 0.0115 0.138 Uiso 0.36(9) 1 calc PR C 1 H5C H -0.1489 0.3843 -0.0053 0.138 Uiso 0.36(9) 1 calc PR C 1 C5' C -0.177(2) 0.3661(18) 0.0174(11) 0.092(3) Uani 0.64(9) 1 d PDU C 2 H5'1 H -0.1045 0.3633 0.0333 0.138 Uiso 0.64(9) 1 calc PR C 2 H5'2 H -0.2120 0.4237 0.0350 0.138 Uiso 0.64(9) 1 calc PR C 2 H5'3 H -0.1768 0.3721 -0.0277 0.138 Uiso 0.64(9) 1 calc PR C 2 C6 C 0.1434(6) 0.2158(6) 0.0811(4) 0.0256(16) Uani 1 1 d U C . C7 C 0.2354(7) 0.2747(6) 0.0563(4) 0.037(2) Uani 1 1 d DU . . C8 C 0.3309(10) 0.2499(10) 0.0962(6) 0.090(3) Uani 1 1 d DU C . H8A H 0.3331 0.1783 0.1039 0.136 Uiso 1 1 calc R . . H8B H 0.3272 0.2852 0.1355 0.136 Uiso 1 1 calc R . . H8C H 0.3942 0.2700 0.0749 0.136 Uiso 1 1 calc R . . C9 C 0.2164(11) 0.3847(8) 0.0611(7) 0.090(3) Uani 1 1 d DU C . H9A H 0.2751 0.4207 0.0436 0.136 Uiso 1 1 calc R . . H9B H 0.2098 0.4030 0.1046 0.136 Uiso 1 1 calc R . . H9C H 0.1519 0.4019 0.0384 0.136 Uiso 1 1 calc R . . C10 C 0.261(4) 0.250(3) -0.0102(9) 0.090(3) Uani 0.36(9) 1 d PDU C 1 H10A H 0.2726 0.1782 -0.0139 0.136 Uiso 0.36(9) 1 calc PR C 1 H10B H 0.3234 0.2856 -0.0221 0.136 Uiso 0.36(9) 1 calc PR C 1 H10C H 0.2018 0.2691 -0.0373 0.136 Uiso 0.36(9) 1 calc PR C 1 C11 C -0.0593(11) 0.1279(13) 0.3046(6) 0.024(3) Uani 0.517(14) 1 d PD D 1 H11 H -0.0526 0.1992 0.3169 0.028 Uiso 0.517(14) 1 calc PR D 1 C12 C -0.1204(7) 0.0676(8) 0.3532(4) 0.043(2) Uani 0.483(14) 1 d P D 1 H12A H -0.1238 -0.0035 0.3418 0.052 Uiso 0.483(14) 1 calc PR D 1 H12B H -0.1923 0.0933 0.3571 0.052 Uiso 0.483(14) 1 calc PR D 1 C13 C -0.0540(14) 0.0830(18) 0.4162(9) 0.040(5) Uani 0.517(14) 1 d PD D 1 H13A H -0.0452 0.1546 0.4251 0.049 Uiso 0.517(14) 1 calc PR D 1 H13B H -0.0901 0.0519 0.4511 0.049 Uiso 0.517(14) 1 calc PR D 1 C14 C 0.0497(16) 0.0354(18) 0.4075(11) 0.034(5) Uani 0.483(14) 1 d PD D 1 H14A H 0.0396 -0.0349 0.3956 0.040 Uiso 0.483(14) 1 calc PR D 1 H14B H 0.0905 0.0371 0.4468 0.040 Uiso 0.483(14) 1 calc PR D 1 C15 C 0.1091(7) 0.0882(7) 0.3584(4) 0.0337(19) Uani 0.517(14) 1 d P D 1 H15A H 0.1791 0.0579 0.3545 0.040 Uiso 0.517(14) 1 calc PR D 1 H15B H 0.1184 0.1588 0.3698 0.040 Uiso 0.517(14) 1 calc PR D 1 C16 C 0.0476(12) 0.0802(15) 0.2964(7) 0.024(3) Uani 0.483(14) 1 d PD D 1 H16 H 0.0396 0.0091 0.2839 0.028 Uiso 0.483(14) 1 calc PR D 1 C10' C 0.255(3) 0.247(2) -0.0096(7) 0.090(3) Uani 0.64(9) 1 d PDU C 2 H10D H 0.2644 0.1753 -0.0128 0.136 Uiso 0.64(9) 1 calc PR C 2 H10E H 0.3188 0.2806 -0.0232 0.136 Uiso 0.64(9) 1 calc PR C 2 H10F H 0.1959 0.2680 -0.0358 0.136 Uiso 0.64(9) 1 calc PR C 2 C11' C -0.0533(11) 0.0677(13) 0.2932(7) 0.018(4) Uani 0.483(14) 1 d P D 2 H11' H -0.0309 -0.0008 0.2818 0.022 Uiso 0.483(14) 1 calc PR D 2 C12' C -0.1204(7) 0.0676(8) 0.3532(4) 0.043(2) Uani 0.517(14) 1 d P D 2 H12C H -0.1854 0.0290 0.3463 0.052 Uiso 0.517(14) 1 calc PR D 2 H12D H -0.1393 0.1362 0.3647 0.052 Uiso 0.517(14) 1 calc PR D 2 C13' C -0.0506(17) 0.0183(17) 0.4060(9) 0.037(5) Uani 0.483(14) 1 d P D 2 H13C H -0.0912 0.0110 0.4440 0.044 Uiso 0.483(14) 1 calc PR D 2 H13D H -0.0269 -0.0482 0.3930 0.044 Uiso 0.483(14) 1 calc PR D 2 C14' C 0.0425(18) 0.086(2) 0.4178(9) 0.038(5) Uani 0.517(14) 1 d P D 2 H14C H 0.0851 0.0604 0.4530 0.045 Uiso 0.517(14) 1 calc PR D 2 H14D H 0.0184 0.1533 0.4279 0.045 Uiso 0.517(14) 1 calc PR D 2 C15' C 0.1091(7) 0.0882(7) 0.3584(4) 0.0337(19) Uani 0.483(14) 1 d P D 2 H15C H 0.1730 0.1283 0.3656 0.040 Uiso 0.483(14) 1 calc PR D 2 H15D H 0.1300 0.0202 0.3467 0.040 Uiso 0.483(14) 1 calc PR D 2 C16' C 0.0404(12) 0.1347(14) 0.3075(7) 0.024(4) Uani 0.517(14) 1 d P D 2 H16' H 0.0170 0.2026 0.3197 0.028 Uiso 0.517(14) 1 calc PR D 2 C17 C 0.4991(10) 0.9194(11) 0.0827(6) 0.073(4) Uani 1 1 d . . . H17A H 0.5242 0.8759 0.0501 0.109 Uiso 1 1 calc R . . H17B H 0.4381 0.9566 0.0673 0.109 Uiso 1 1 calc R . . H17C H 0.4795 0.8793 0.1183 0.109 Uiso 1 1 calc R . . C18 C 0.5826(8) 0.9894(8) 0.1014(6) 0.050(3) Uani 1 1 d . . . C19 C 0.5720(11) 1.0400(9) 0.1618(6) 0.072(4) Uani 1 1 d . . . H19A H 0.5540 0.9912 0.1933 0.108 Uiso 1 1 calc R . . H19B H 0.5168 1.0902 0.1585 0.108 Uiso 1 1 calc R . . H19C H 0.6383 1.0721 0.1735 0.108 Uiso 1 1 calc R . . C20 C 1.0621(11) 0.6938(10) 0.2135(7) 0.085(5) Uani 1 1 d . . . H20A H 1.1314 0.7194 0.2038 0.128 Uiso 1 1 calc R . . H20B H 1.0693 0.6286 0.2330 0.128 Uiso 1 1 calc R . . H20C H 1.0279 0.7395 0.2418 0.128 Uiso 1 1 calc R . . C21 C 0.9992(9) 0.6849(8) 0.1570(7) 0.061(3) Uani 1 1 d . . . C22 C 0.9386(12) 0.5871(10) 0.1493(8) 0.087(5) Uani 1 1 d . . . H22A H 0.8992 0.5740 0.1866 0.130 Uiso 1 1 calc R . . H22B H 0.9878 0.5327 0.1425 0.130 Uiso 1 1 calc R . . H22C H 0.8902 0.5922 0.1138 0.130 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 0.02170(15) 0.01590(15) 0.01491(14) -0.00026(10) -0.00095(10) 0.00002(10) Pt2 0.02833(17) 0.01877(16) 0.01469(14) -0.00069(10) -0.00085(11) 0.00191(11) Cl1 0.0443(12) 0.0300(11) 0.0346(11) 0.0007(9) -0.0031(9) -0.0006(9) Cl2 0.0650(16) 0.0381(12) 0.0303(11) -0.0057(10) 0.0044(11) 0.0038(11) N1 0.039(4) 0.038(4) 0.023(3) -0.003(3) -0.002(3) 0.018(3) N2 0.045(4) 0.023(3) 0.016(3) 0.000(3) 0.004(3) -0.005(3) N3 0.035(4) 0.026(3) 0.023(3) -0.002(3) -0.003(3) 0.009(3) N4 0.032(4) 0.027(4) 0.024(3) -0.001(3) -0.003(3) -0.007(3) N5 0.023(3) 0.044(4) 0.019(3) 0.000(3) -0.004(3) 0.004(3) N6 0.025(3) 0.030(4) 0.021(3) -0.004(3) -0.002(3) -0.001(3) O1 0.030(3) 0.025(3) 0.018(3) -0.002(2) -0.004(2) 0.008(2) O2 0.029(3) 0.023(3) 0.025(3) -0.003(2) 0.003(2) -0.008(2) O3 0.043(4) 0.066(5) 0.081(6) 0.011(4) 0.001(4) 0.006(4) O4 0.077(6) 0.043(4) 0.081(6) 0.024(4) -0.002(5) -0.003(4) O5 0.086(6) 0.038(4) 0.058(5) -0.014(3) -0.026(4) -0.003(4) O6 0.084(6) 0.085(7) 0.113(8) 0.033(6) 0.049(6) 0.013(5) O7 0.114(7) 0.059(5) 0.072(6) -0.013(4) -0.053(5) 0.003(5) O8 0.080(5) 0.029(4) 0.058(5) 0.007(3) 0.004(4) -0.017(3) O9 0.066(5) 0.050(5) 0.077(6) -0.028(4) -0.002(4) -0.001(4) O10 0.060(5) 0.062(5) 0.046(4) 0.004(4) 0.006(4) -0.004(4) O11 0.098(6) 0.043(4) 0.050(4) -0.003(4) 0.034(4) 0.021(4) O12 0.126(8) 0.065(6) 0.049(5) 0.012(4) -0.029(5) -0.019(5) C1 0.035(4) 0.028(4) 0.021(4) 0.004(3) -0.003(3) 0.008(3) C2 0.044(5) 0.036(5) 0.033(4) 0.001(4) -0.005(4) 0.018(4) C3 0.078(5) 0.099(6) 0.099(6) 0.011(5) -0.032(5) 0.047(5) C4 0.078(5) 0.099(6) 0.099(6) 0.011(5) -0.032(5) 0.047(5) C5 0.078(5) 0.099(6) 0.099(6) 0.011(5) -0.032(5) 0.047(5) C5' 0.078(5) 0.099(6) 0.099(6) 0.011(5) -0.032(5) 0.047(5) C6 0.033(4) 0.021(4) 0.022(4) 0.002(3) -0.005(3) -0.004(3) C7 0.042(5) 0.039(5) 0.029(4) -0.002(4) 0.006(4) -0.017(4) C8 0.094(5) 0.082(5) 0.096(6) 0.003(4) 0.025(5) -0.045(4) C9 0.094(5) 0.082(5) 0.096(6) 0.003(4) 0.025(5) -0.045(4) C10 0.094(5) 0.082(5) 0.096(6) 0.003(4) 0.025(5) -0.045(4) C11 0.043(8) 0.019(6) 0.009(5) -0.004(5) 0.003(4) -0.002(6) C12 0.033(5) 0.071(7) 0.027(4) 0.021(5) 0.006(4) -0.010(5) C13 0.046(12) 0.047(13) 0.029(10) 0.016(10) 0.016(8) 0.014(10) C14 0.043(12) 0.037(13) 0.021(11) -0.004(10) 0.006(8) 0.016(11) C15 0.034(5) 0.043(5) 0.024(4) 0.006(4) -0.006(3) -0.002(4) C16 0.043(8) 0.019(6) 0.009(5) -0.004(5) 0.003(4) -0.002(6) C10' 0.094(5) 0.082(5) 0.096(6) 0.003(4) 0.025(5) -0.045(4) C11' 0.018(8) 0.021(9) 0.015(7) 0.003(7) 0.003(6) 0.001(6) C12' 0.033(5) 0.071(7) 0.027(4) 0.021(5) 0.006(4) -0.010(5) C13' 0.056(13) 0.034(12) 0.020(9) 0.013(9) -0.009(8) -0.012(10) C14' 0.049(13) 0.054(14) 0.011(8) -0.015(10) 0.002(7) -0.005(12) C15' 0.034(5) 0.043(5) 0.024(4) 0.006(4) -0.006(3) -0.002(4) C16' 0.026(8) 0.023(9) 0.022(8) -0.004(7) -0.001(6) -0.011(7) C17 0.057(8) 0.098(11) 0.064(8) -0.015(7) 0.009(6) -0.023(7) C18 0.031(5) 0.055(7) 0.065(7) 0.015(6) 0.006(5) 0.011(5) C19 0.077(9) 0.066(8) 0.071(9) -0.024(7) -0.022(7) 0.018(7) C20 0.083(10) 0.054(8) 0.118(13) 0.035(8) -0.037(9) -0.033(7) C21 0.056(7) 0.030(5) 0.098(10) 0.027(6) 0.023(7) -0.004(5) C22 0.092(10) 0.051(8) 0.117(13) 0.029(8) -0.015(9) -0.017(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 N4 2.017(6) . ? Pt1 N3 2.024(6) . ? Pt1 O2 2.038(5) . ? Pt1 O1 2.039(5) . ? Pt1 Pt2 3.0368(5) . ? Pt1 Pt1 3.2261(7) 3 ? Pt2 N2 2.001(7) . ? Pt2 N1 2.010(7) . ? Pt2 N5 2.039(7) . ? Pt2 N6 2.057(6) . ? Cl1 O5 1.414(7) . ? Cl1 O7 1.416(8) . ? Cl1 O8 1.424(7) . ? Cl1 O6 1.435(9) . ? Cl2 O9 1.421(7) . ? Cl2 O10 1.421(8) . ? Cl2 O12 1.423(9) . ? Cl2 O11 1.432(8) . ? N1 C1 1.294(10) . ? N1 H1 0.8800 . ? N2 C6 1.292(10) . ? N2 H2 0.8800 . ? N3 H3D 0.9100 . ? N3 H3E 0.9100 . ? N3 H3F 0.9100 . ? N4 H4D 0.9100 . ? N4 H4E 0.9100 . ? N4 H4F 0.9100 . ? N5 C11' 1.500(16) . ? N5 C11 1.526(15) . ? N5 H5D 0.9200 . ? N5 H5E 0.9200 . ? N6 C16 1.496(18) . ? N6 C16' 1.534(17) . ? N6 H6A 0.9200 . ? N6 H6B 0.9200 . ? O1 C1 1.289(10) . ? O2 C6 1.295(9) . ? O3 C18 1.205(12) . ? O4 C21 1.202(13) . ? C1 C2 1.516(11) . ? C2 C5' 1.474(15) . ? C2 C5 1.478(18) . ? C2 C4 1.507(12) . ? C2 C3 1.533(12) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C5' H5'1 0.9800 . ? C5' H5'2 0.9800 . ? C5' H5'3 0.9800 . ? C6 C7 1.530(11) . ? C7 C10' 1.505(15) . ? C7 C9 1.508(12) . ? C7 C8 1.519(12) . ? C7 C10 1.522(18) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C16 1.528(16) . ? C11 C12 1.557(17) . ? C11 H11 1.0000 . ? C12 C13 1.61(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.491(17) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.50(2) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.547(17) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16 1.0000 . ? C10' H10D 0.9800 . ? C10' H10E 0.9800 . ? C10' H10F 0.9800 . ? C11' C16' 1.53(2) . ? C11' H11' 1.0000 . ? C13' C14' 1.52(3) . ? C13' H13C 0.9900 . ? C13' H13D 0.9900 . ? C14' H14C 0.9900 . ? C14' H14D 0.9900 . ? C16' H16' 1.0000 . ? C17 C18 1.476(16) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.487(17) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.456(19) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.538(16) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 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 N4 Pt1 N3 91.2(3) . . ? N4 Pt1 O2 174.7(2) . . ? N3 Pt1 O2 87.8(3) . . ? N4 Pt1 O1 88.7(3) . . ? N3 Pt1 O1 174.3(2) . . ? O2 Pt1 O1 91.8(2) . . ? N4 Pt1 Pt2 104.6(2) . . ? N3 Pt1 Pt2 104.14(19) . . ? O2 Pt1 Pt2 80.73(15) . . ? O1 Pt1 Pt2 81.37(14) . . ? N4 Pt1 Pt1 83.61(19) . 3 ? N3 Pt1 Pt1 87.78(19) . 3 ? O2 Pt1 Pt1 91.12(15) . 3 ? O1 Pt1 Pt1 86.56(14) . 3 ? Pt2 Pt1 Pt1 165.175(15) . 3 ? N2 Pt2 N1 92.2(3) . . ? N2 Pt2 N5 173.8(3) . . ? N1 Pt2 N5 92.2(3) . . ? N2 Pt2 N6 91.6(3) . . ? N1 Pt2 N6 172.4(3) . . ? N5 Pt2 N6 83.5(3) . . ? N2 Pt2 Pt1 77.15(19) . . ? N1 Pt2 Pt1 76.4(2) . . ? N5 Pt2 Pt1 108.1(2) . . ? N6 Pt2 Pt1 110.81(19) . . ? O5 Cl1 O7 110.3(5) . . ? O5 Cl1 O8 110.8(5) . . ? O7 Cl1 O8 111.4(5) . . ? O5 Cl1 O6 104.9(6) . . ? O7 Cl1 O6 110.7(7) . . ? O8 Cl1 O6 108.6(5) . . ? O9 Cl2 O10 108.8(5) . . ? O9 Cl2 O12 108.3(5) . . ? O10 Cl2 O12 110.5(6) . . ? O9 Cl2 O11 109.6(5) . . ? O10 Cl2 O11 110.5(5) . . ? O12 Cl2 O11 109.0(6) . . ? C1 N1 Pt2 131.3(6) . . ? C1 N1 H1 114.3 . . ? Pt2 N1 H1 114.3 . . ? C6 N2 Pt2 131.8(6) . . ? C6 N2 H2 114.1 . . ? Pt2 N2 H2 114.1 . . ? Pt1 N3 H3D 109.5 . . ? Pt1 N3 H3E 109.5 . . ? H3D N3 H3E 109.5 . . ? Pt1 N3 H3F 109.5 . . ? H3D N3 H3F 109.5 . . ? H3E N3 H3F 109.5 . . ? Pt1 N4 H4D 109.5 . . ? Pt1 N4 H4E 109.5 . . ? H4D N4 H4E 109.5 . . ? Pt1 N4 H4F 109.5 . . ? H4D N4 H4F 109.5 . . ? H4E N4 H4F 109.5 . . ? C11' N5 Pt2 109.9(7) . . ? C11 N5 Pt2 104.9(7) . . ? C11' N5 H5D 131.8 . . ? C11 N5 H5D 110.8 . . ? Pt2 N5 H5D 110.8 . . ? C11' N5 H5E 79.1 . . ? C11 N5 H5E 110.8 . . ? Pt2 N5 H5E 110.8 . . ? H5D N5 H5E 108.8 . . ? C16 N6 Pt2 109.3(7) . . ? C16' N6 Pt2 105.1(7) . . ? C16 N6 H6A 109.8 . . ? C16' N6 H6A 135.2 . . ? Pt2 N6 H6A 109.8 . . ? C16 N6 H6B 109.8 . . ? C16' N6 H6B 84.5 . . ? Pt2 N6 H6B 109.8 . . ? H6A N6 H6B 108.3 . . ? C1 O1 Pt1 123.7(5) . . ? C6 O2 Pt1 125.0(5) . . ? O1 C1 N1 124.7(7) . . ? O1 C1 C2 115.0(7) . . ? N1 C1 C2 120.3(7) . . ? C5' C2 C4 109.5(11) . . ? C5 C2 C4 114.1(16) . . ? C5' C2 C1 104.9(13) . . ? C5 C2 C1 115(2) . . ? C4 C2 C1 112.4(7) . . ? C5' C2 C3 114.0(13) . . ? C5 C2 C3 97(3) . . ? C4 C2 C3 104.0(8) . . ? C1 C2 C3 112.1(8) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C2 C5' H5'1 109.5 . . ? C2 C5' H5'2 109.5 . . ? H5'1 C5' H5'2 109.5 . . ? C2 C5' H5'3 109.5 . . ? H5'1 C5' H5'3 109.5 . . ? H5'2 C5' H5'3 109.5 . . ? N2 C6 O2 123.8(7) . . ? N2 C6 C7 120.9(7) . . ? O2 C6 C7 115.2(7) . . ? C10' C7 C9 109.8(12) . . ? C10' C7 C8 109.6(13) . . ? C9 C7 C8 107.9(8) . . ? C9 C7 C10 108.8(16) . . ? C8 C7 C10 107.8(15) . . ? C10' C7 C6 110.9(15) . . ? C9 C7 C6 111.0(8) . . ? C8 C7 C6 107.6(8) . . ? C10 C7 C6 114(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N5 C11 C16 104.0(11) . . ? N5 C11 C12 109.6(11) . . ? C16 C11 C12 108.9(12) . . ? N5 C11 H11 111.4 . . ? C16 C11 H11 111.4 . . ? C12 C11 H11 111.4 . . ? C11 C12 C13 104.1(11) . . ? C11 C12 H12A 110.9 . . ? C13 C12 H12A 110.9 . . ? C11 C12 H12B 110.9 . . ? C13 C12 H12B 110.9 . . ? H12A C12 H12B 109.0 . . ? C14 C13 C12 106.9(16) . . ? C14 C13 H13A 110.3 . . ? C12 C13 H13A 110.3 . . ? C14 C13 H13B 110.3 . . ? C12 C13 H13B 110.3 . . ? H13A C13 H13B 108.6 . . ? C13 C14 C15 110.7(16) . . ? C13 C14 H14A 109.5 . . ? C15 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C14 C15 C16 109.1(13) . . ? C14 C15 H15A 109.9 . . ? C16 C15 H15A 109.9 . . ? C14 C15 H15B 109.9 . . ? C16 C15 H15B 109.9 . . ? H15A C15 H15B 108.3 . . ? N6 C16 C11 105.9(12) . . ? N6 C16 C15 111.6(12) . . ? C11 C16 C15 107.9(12) . . ? N6 C16 H16 110.4 . . ? C11 C16 H16 110.4 . . ? C15 C16 H16 110.4 . . ? C7 C10' H10D 109.5 . . ? C7 C10' H10E 109.5 . . ? H10D C10' H10E 109.5 . . ? C7 C10' H10F 109.5 . . ? H10D C10' H10F 109.5 . . ? H10E C10' H10F 109.5 . . ? N5 C11' C16' 105.8(12) . . ? N5 C11' H11' 111.6 . . ? C16' C11' H11' 111.6 . . ? C14' C13' H13C 110.2 . . ? C14' C13' H13D 110.2 . . ? H13C C13' H13D 108.5 . . ? C13' C14' H14C 110.0 . . ? C13' C14' H14D 110.0 . . ? H14C C14' H14D 108.4 . . ? C11' C16' N6 103.8(12) . . ? C11' C16' H16' 110.8 . . ? N6 C16' H16' 110.8 . . ? C18 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C18 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O3 C18 C17 121.4(12) . . ? O3 C18 C19 121.5(12) . . ? C17 C18 C19 117.1(11) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 H20A 109.5 . . ? C21 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C21 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O4 C21 C20 123.4(11) . . ? O4 C21 C22 121.0(13) . . ? C20 C21 C22 115.5(10) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Pt1 Pt2 N2 -171.5(3) . . . . ? N3 Pt1 Pt2 N2 93.5(3) . . . . ? O2 Pt1 Pt2 N2 8.1(3) . . . . ? O1 Pt1 Pt2 N2 -85.1(3) . . . . ? Pt1 Pt1 Pt2 N2 -49.2(2) 3 . . . ? N4 Pt1 Pt2 N1 -76.0(3) . . . . ? N3 Pt1 Pt2 N1 -171.0(3) . . . . ? O2 Pt1 Pt2 N1 103.7(3) . . . . ? O1 Pt1 Pt2 N1 10.4(3) . . . . ? Pt1 Pt1 Pt2 N1 46.3(2) 3 . . . ? N4 Pt1 Pt2 N5 11.9(3) . . . . ? N3 Pt1 Pt2 N5 -83.2(3) . . . . ? O2 Pt1 Pt2 N5 -168.5(2) . . . . ? O1 Pt1 Pt2 N5 98.3(2) . . . . ? Pt1 Pt1 Pt2 N5 134.1(2) 3 . . . ? N4 Pt1 Pt2 N6 101.7(3) . . . . ? N3 Pt1 Pt2 N6 6.6(3) . . . . ? O2 Pt1 Pt2 N6 -78.7(3) . . . . ? O1 Pt1 Pt2 N6 -171.9(3) . . . . ? Pt1 Pt1 Pt2 N6 -136.1(2) 3 . . . ? N2 Pt2 N1 C1 61.5(9) . . . . ? N5 Pt2 N1 C1 -122.8(9) . . . . ? Pt1 Pt2 N1 C1 -14.7(8) . . . . ? N1 Pt2 N2 C6 -85.8(8) . . . . ? N6 Pt2 N2 C6 100.7(8) . . . . ? Pt1 Pt2 N2 C6 -10.2(7) . . . . ? N1 Pt2 N5 C11' 179.3(9) . . . . ? N6 Pt2 N5 C11' -6.9(8) . . . . ? Pt1 Pt2 N5 C11' 102.9(8) . . . . ? N1 Pt2 N5 C11 -146.7(8) . . . . ? N6 Pt2 N5 C11 27.1(8) . . . . ? Pt1 Pt2 N5 C11 136.9(7) . . . . ? N5 Pt2 N6 C16 5.4(9) . . . . ? Pt1 Pt2 N6 C16 -101.5(9) . . . . ? N2 Pt2 N6 C16' 150.6(8) . . . . ? N5 Pt2 N6 C16' -25.6(8) . . . . ? Pt1 Pt2 N6 C16' -132.5(7) . . . . ? N4 Pt1 O1 C1 93.0(7) . . . . ? O2 Pt1 O1 C1 -92.3(6) . . . . ? Pt2 Pt1 O1 C1 -12.0(6) . . . . ? Pt1 Pt1 O1 C1 176.7(6) 3 . . . ? N3 Pt1 O2 C6 -115.3(6) . . . . ? O1 Pt1 O2 C6 70.3(6) . . . . ? Pt2 Pt1 O2 C6 -10.6(6) . . . . ? Pt1 Pt1 O2 C6 156.9(6) 3 . . . ? Pt1 O1 C1 N1 6.5(12) . . . . ? Pt1 O1 C1 C2 -174.8(5) . . . . ? Pt2 N1 C1 O1 11.0(14) . . . . ? Pt2 N1 C1 C2 -167.7(6) . . . . ? O1 C1 C2 C5' -96.5(14) . . . . ? N1 C1 C2 C5' 82.3(14) . . . . ? O1 C1 C2 C5 -111(3) . . . . ? N1 C1 C2 C5 68(3) . . . . ? O1 C1 C2 C4 22.4(12) . . . . ? N1 C1 C2 C4 -158.8(10) . . . . ? O1 C1 C2 C3 139.2(9) . . . . ? N1 C1 C2 C3 -42.0(12) . . . . ? Pt2 N2 C6 O2 5.9(12) . . . . ? Pt2 N2 C6 C7 -170.6(6) . . . . ? Pt1 O2 C6 N2 7.7(11) . . . . ? Pt1 O2 C6 C7 -175.7(5) . . . . ? N2 C6 C7 C10' -162.1(11) . . . . ? O2 C6 C7 C10' 21.1(13) . . . . ? N2 C6 C7 C9 -39.8(11) . . . . ? O2 C6 C7 C9 143.5(9) . . . . ? N2 C6 C7 C8 78.1(10) . . . . ? O2 C6 C7 C8 -98.7(9) . . . . ? N2 C6 C7 C10 -162.7(13) . . . . ? O2 C6 C7 C10 20.5(15) . . . . ? C11' N5 C11 C16 49.7(14) . . . . ? Pt2 N5 C11 C16 -54.0(13) . . . . ? C11' N5 C11 C12 -66.7(16) . . . . ? Pt2 N5 C11 C12 -170.3(8) . . . . ? N5 C11 C12 C13 178.5(11) . . . . ? C16 C11 C12 C13 65.3(15) . . . . ? C11 C12 C13 C14 -64.8(19) . . . . ? C12 C13 C14 C15 65(2) . . . . ? C13 C14 C15 C16 -62(2) . . . . ? C16' N6 C16 C11 50.0(15) . . . . ? Pt2 N6 C16 C11 -36.9(14) . . . . ? C16' N6 C16 C15 -67.2(18) . . . . ? Pt2 N6 C16 C15 -154.1(9) . . . . ? N5 C11 C16 N6 59.9(15) . . . . ? C12 C11 C16 N6 176.7(11) . . . . ? N5 C11 C16 C15 179.5(11) . . . . ? C12 C11 C16 C15 -63.7(16) . . . . ? C14 C15 C16 N6 175.6(12) . . . . ? C14 C15 C16 C11 59.7(17) . . . . ? C11 N5 C11' C16' -48.5(15) . . . . ? Pt2 N5 C11' C16' 38.2(14) . . . . ? N5 C11' C16' N6 -59.6(15) . . . . ? C16 N6 C16' C11' -50.0(15) . . . . ? Pt2 N6 C16' C11' 52.5(13) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 4.223 _refine_diff_density_min -1.629 _refine_diff_density_rms 0.219 #===END data_l394 _database_code_depnum_ccdc_archive 'CCDC 290075' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H34 Cl2 N6 O10 Pt2' _chemical_formula_weight 883.53 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' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.3961(8) _cell_length_b 10.0151(11) _cell_length_c 17.5650(19) _cell_angle_alpha 85.266(2) _cell_angle_beta 82.683(2) _cell_angle_gamma 76.947(2) _cell_volume 1255.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.338 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 836 _exptl_absorpt_coefficient_mu 11.402 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1882 _exptl_absorpt_correction_T_max 0.5994 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 7277 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0820 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 27.51 _reflns_number_total 5317 _reflns_number_gt 4647 _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^)+(0.0896P)^2^+0.0000P] 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 5317 _refine_ls_number_parameters 283 _refine_ls_number_restraints 600 _refine_ls_R_factor_all 0.0573 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1420 _refine_ls_wR_factor_gt 0.1362 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 0.967 _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 0.40550(4) 0.44615(3) 0.275801(15) 0.01161(12) Uani 1 1 d . . . Pt2 Pt 0.76634(4) 0.26120(3) 0.311930(15) 0.01230(12) Uani 1 1 d . . . Cl1 Cl 0.7722(2) 0.66157(17) 0.44864(10) 0.0147(3) Uani 1 1 d U . . Cl2 Cl 0.2473(3) 0.95614(19) 0.28246(13) 0.0266(5) Uani 1 1 d U . . O1 O 0.8527(8) 0.4359(6) 0.2666(3) 0.0190(11) Uani 1 1 d U . . N1 N 0.5888(9) 0.5480(6) 0.2178(4) 0.0165(9) Uani 1 1 d U . . H1 H 0.5412 0.6166 0.1866 0.020 Uiso 1 1 calc R . . N2 N 0.7544(9) 0.2123(7) 0.2044(4) 0.0165(9) Uani 1 1 d U . . H2 H 0.8585 0.1646 0.1811 0.020 Uiso 1 1 calc R . . N3 N 0.2119(9) 0.3405(6) 0.3282(4) 0.0150(13) Uani 1 1 d U . . H3D H 0.0985 0.3784 0.3119 0.023 Uiso 1 1 calc R . . H3E H 0.2041 0.3450 0.3801 0.023 Uiso 1 1 calc R . . H3F H 0.2471 0.2511 0.3158 0.023 Uiso 1 1 calc R . . N4 N 0.3419(9) 0.5883(6) 0.3575(4) 0.0174(13) Uani 1 1 d U . . H4D H 0.3958 0.6603 0.3411 0.026 Uiso 1 1 calc R . . H4E H 0.3858 0.5493 0.4021 0.026 Uiso 1 1 calc R . . H4F H 0.2158 0.6186 0.3657 0.026 Uiso 1 1 calc R . . N5 N 0.7754(9) 0.2963(6) 0.4256(3) 0.0152(12) Uani 1 1 d U . . H5D H 0.8731 0.3371 0.4299 0.018 Uiso 1 1 calc R . . H5E H 0.6661 0.3534 0.4446 0.018 Uiso 1 1 calc R . . N6 N 0.7149(9) 0.0775(6) 0.3564(4) 0.0186(13) Uani 1 1 d U . . H6A H 0.6152 0.0597 0.3357 0.022 Uiso 1 1 calc R . . H6B H 0.8175 0.0084 0.3442 0.022 Uiso 1 1 calc R . . O2 O 0.4551(8) 0.3161(6) 0.1902(3) 0.0196(12) Uani 1 1 d U . . O3 O 0.9333(8) 0.5666(6) 0.4146(3) 0.0252(13) Uani 1 1 d U . . O4 O 0.6407(8) 0.5850(6) 0.4890(3) 0.0243(13) Uani 1 1 d U . . O5 O 0.6826(9) 0.7514(6) 0.3905(4) 0.0278(13) Uani 1 1 d U . . O6 O 0.8302(9) 0.7402(6) 0.5028(3) 0.0241(13) Uani 1 1 d U . . O7 O 0.3385(11) 1.0357(8) 0.3225(6) 0.061(2) Uani 1 1 d U . . O8 O 0.3843(10) 0.8449(7) 0.2489(4) 0.0404(17) Uani 1 1 d U . . O9 O 0.1163(9) 0.8999(6) 0.3362(4) 0.0330(15) Uani 1 1 d U . . O10 O 0.1475(12) 1.0402(9) 0.2251(5) 0.060(3) Uani 1 1 d U . . C1 C 0.7671(11) 0.5271(8) 0.2199(4) 0.0158(14) Uani 1 1 d U . . C2 C 0.8870(11) 0.6081(9) 0.1660(5) 0.0201(16) Uani 1 1 d U . . C3 C 0.7754(13) 0.7010(10) 0.1057(5) 0.031(2) Uani 1 1 d U . . H3A H 0.7264 0.6443 0.0741 0.047 Uiso 1 1 calc R . . H3B H 0.8575 0.7517 0.0729 0.047 Uiso 1 1 calc R . . H3C H 0.6714 0.7660 0.1319 0.047 Uiso 1 1 calc R . . C4 C 0.9641(14) 0.6991(10) 0.2134(5) 0.032(2) Uani 1 1 d U . . H4A H 0.8633 0.7752 0.2314 0.048 Uiso 1 1 calc R . . H4B H 1.0625 0.7356 0.1815 0.048 Uiso 1 1 calc R . . H4C H 1.0159 0.6448 0.2577 0.048 Uiso 1 1 calc R . . C5 C 1.0470(13) 0.5048(10) 0.1246(5) 0.030(2) Uani 1 1 d U . . H5A H 1.1051 0.4359 0.1622 0.046 Uiso 1 1 calc R . . H5B H 1.1403 0.5530 0.0980 0.046 Uiso 1 1 calc R . . H5C H 0.9976 0.4593 0.0871 0.046 Uiso 1 1 calc R . . C6 C 0.6124(11) 0.2424(8) 0.1651(4) 0.0153(14) Uani 1 1 d U . . C7 C 0.6279(12) 0.1934(9) 0.0845(5) 0.0218(16) Uani 1 1 d U . . C8 C 0.4548(14) 0.1315(10) 0.0782(6) 0.034(2) Uani 1 1 d U . . H8A H 0.4477 0.1176 0.0242 0.050 Uiso 1 1 calc R . . H8B H 0.3408 0.1948 0.0986 0.050 Uiso 1 1 calc R . . H8C H 0.4672 0.0432 0.1078 0.050 Uiso 1 1 calc R . . C9 C 0.8047(15) 0.0948(11) 0.0596(6) 0.039(2) Uani 1 1 d U . . H9A H 0.9108 0.1379 0.0606 0.058 Uiso 1 1 calc R . . H9B H 0.8015 0.0692 0.0072 0.058 Uiso 1 1 calc R . . H9C H 0.8182 0.0125 0.0945 0.058 Uiso 1 1 calc R . . C10 C 0.6061(15) 0.3246(10) 0.0310(5) 0.033(2) Uani 1 1 d U . . H10A H 0.7111 0.3683 0.0332 0.050 Uiso 1 1 calc R . . H10B H 0.4888 0.3882 0.0475 0.050 Uiso 1 1 calc R . . H10C H 0.6047 0.3006 -0.0219 0.050 Uiso 1 1 calc R . . C11 C 0.8013(13) 0.1597(8) 0.4698(5) 0.0234(17) Uani 1 1 d U . . H11A H 0.7697 0.1725 0.5256 0.028 Uiso 1 1 calc R . . H11B H 0.9326 0.1086 0.4607 0.028 Uiso 1 1 calc R . . C12 C 0.6724(12) 0.0820(8) 0.4418(5) 0.0232(17) Uani 1 1 d U . . H12A H 0.6923 -0.0124 0.4659 0.028 Uiso 1 1 calc R . . H12B H 0.5406 0.1286 0.4556 0.028 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 0.01135(18) 0.01229(18) 0.01056(18) 0.00040(12) 0.00096(12) -0.00286(12) Pt2 0.01253(18) 0.01406(18) 0.01024(18) 0.00247(12) -0.00042(12) -0.00434(13) Cl1 0.0174(8) 0.0140(8) 0.0130(8) 0.0015(6) 0.0012(7) -0.0067(7) Cl2 0.0202(10) 0.0136(9) 0.0431(13) 0.0028(8) 0.0003(9) -0.0018(8) O1 0.016(3) 0.023(3) 0.019(3) 0.005(2) -0.001(2) -0.008(2) N1 0.016(2) 0.019(2) 0.010(2) 0.0041(17) -0.0013(16) 0.0027(18) N2 0.016(2) 0.019(2) 0.010(2) 0.0041(17) -0.0013(16) 0.0027(18) N3 0.013(3) 0.017(3) 0.015(3) 0.000(2) -0.001(2) -0.005(3) N4 0.019(3) 0.017(3) 0.014(3) 0.002(2) 0.000(3) -0.003(3) N5 0.022(3) 0.013(3) 0.011(3) 0.004(2) -0.002(2) -0.006(3) N6 0.014(3) 0.015(3) 0.025(3) 0.001(3) 0.003(3) -0.004(2) O2 0.022(3) 0.021(3) 0.014(3) -0.004(2) -0.003(2) 0.002(2) O3 0.023(3) 0.025(3) 0.026(3) -0.008(2) 0.006(2) -0.006(3) O4 0.022(3) 0.025(3) 0.025(3) 0.001(2) 0.006(2) -0.011(3) O5 0.033(3) 0.024(3) 0.026(3) 0.009(3) -0.012(3) -0.006(3) O6 0.035(3) 0.023(3) 0.018(3) -0.005(2) -0.007(3) -0.012(3) O7 0.034(4) 0.033(4) 0.124(7) -0.026(4) -0.020(5) -0.010(3) O8 0.028(4) 0.029(3) 0.053(4) 0.004(3) 0.010(3) 0.007(3) O9 0.031(4) 0.026(3) 0.039(4) 0.004(3) 0.002(3) -0.005(3) O10 0.032(4) 0.060(5) 0.065(6) 0.037(4) 0.005(4) 0.015(4) C1 0.019(3) 0.016(3) 0.012(3) 0.004(3) 0.001(3) -0.004(3) C2 0.020(4) 0.025(4) 0.017(4) 0.006(3) -0.003(3) -0.011(3) C3 0.030(5) 0.041(5) 0.022(4) 0.018(4) -0.001(4) -0.014(4) C4 0.036(5) 0.038(5) 0.024(4) 0.013(4) -0.005(4) -0.016(4) C5 0.020(4) 0.037(5) 0.028(5) 0.008(4) 0.006(4) -0.003(4) C6 0.020(3) 0.013(3) 0.011(3) 0.002(3) 0.002(3) -0.004(3) C7 0.027(4) 0.026(4) 0.009(3) -0.001(3) -0.001(3) -0.001(3) C8 0.042(5) 0.037(5) 0.025(5) -0.010(4) -0.003(4) -0.015(4) C9 0.039(5) 0.046(5) 0.028(5) -0.016(4) 0.008(4) -0.004(5) C10 0.050(6) 0.037(5) 0.015(4) 0.003(4) -0.003(4) -0.016(4) C11 0.033(4) 0.012(3) 0.023(4) 0.010(3) -0.004(3) -0.005(3) C12 0.028(4) 0.016(4) 0.025(4) 0.004(3) 0.003(3) -0.006(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 N1 2.004(7) . ? Pt1 O2 2.014(5) . ? Pt1 N4 2.042(6) . ? Pt1 N3 2.051(6) . ? Pt1 Pt2 2.9934(4) . ? Pt2 N2 2.008(7) . ? Pt2 N6 2.036(6) . ? Pt2 O1 2.061(5) . ? Pt2 N5 2.068(6) . ? Cl1 O5 1.430(6) . ? Cl1 O3 1.443(6) . ? Cl1 O6 1.446(6) . ? Cl1 O4 1.452(6) . ? Cl2 O7 1.429(8) . ? Cl2 O10 1.428(8) . ? Cl2 O8 1.436(7) . ? Cl2 O9 1.439(7) . ? O1 C1 1.286(9) . ? N1 C1 1.293(10) . ? N1 H1 0.8800 . ? N2 C6 1.296(10) . ? N2 H2 0.8800 . ? N3 H3D 0.9100 . ? N3 H3E 0.9100 . ? N3 H3F 0.9100 . ? N4 H4D 0.9100 . ? N4 H4E 0.9100 . ? N4 H4F 0.9100 . ? N5 C11 1.502(9) . ? N5 H5D 0.9200 . ? N5 H5E 0.9200 . ? N6 C12 1.495(10) . ? N6 H6A 0.9200 . ? N6 H6B 0.9200 . ? O2 C6 1.276(9) . ? C1 C2 1.524(11) . ? C2 C4 1.525(13) . ? C2 C5 1.534(12) . ? C2 C3 1.543(12) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.518(11) . ? C7 C9 1.490(12) . ? C7 C10 1.541(12) . ? C7 C8 1.563(13) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.509(12) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? 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 N1 Pt1 O2 89.1(2) . . ? N1 Pt1 N4 90.1(3) . . ? O2 Pt1 N4 175.6(2) . . ? N1 Pt1 N3 176.1(2) . . ? O2 Pt1 N3 87.9(2) . . ? N4 Pt1 N3 92.7(3) . . ? N1 Pt1 Pt2 79.42(17) . . ? O2 Pt1 Pt2 78.71(16) . . ? N4 Pt1 Pt2 105.40(18) . . ? N3 Pt1 Pt2 102.38(18) . . ? N2 Pt2 N6 91.8(3) . . ? N2 Pt2 O1 88.6(2) . . ? N6 Pt2 O1 173.0(2) . . ? N2 Pt2 N5 175.5(3) . . ? N6 Pt2 N5 83.7(3) . . ? O1 Pt2 N5 95.9(2) . . ? N2 Pt2 Pt1 78.75(19) . . ? N6 Pt2 Pt1 108.74(19) . . ? O1 Pt2 Pt1 78.21(15) . . ? N5 Pt2 Pt1 102.85(18) . . ? O5 Cl1 O3 110.4(4) . . ? O5 Cl1 O6 110.1(4) . . ? O3 Cl1 O6 109.3(4) . . ? O5 Cl1 O4 108.8(4) . . ? O3 Cl1 O4 109.1(3) . . ? O6 Cl1 O4 109.1(4) . . ? O7 Cl2 O10 110.4(6) . . ? O7 Cl2 O8 109.1(5) . . ? O10 Cl2 O8 111.1(5) . . ? O7 Cl2 O9 109.1(5) . . ? O10 Cl2 O9 108.5(5) . . ? O8 Cl2 O9 108.6(4) . . ? C1 O1 Pt2 125.7(5) . . ? C1 N1 Pt1 129.1(5) . . ? C1 N1 H1 115.5 . . ? Pt1 N1 H1 115.5 . . ? C6 N2 Pt2 128.0(6) . . ? C6 N2 H2 116.0 . . ? Pt2 N2 H2 116.0 . . ? Pt1 N3 H3D 109.5 . . ? Pt1 N3 H3E 109.5 . . ? H3D N3 H3E 109.5 . . ? Pt1 N3 H3F 109.5 . . ? H3D N3 H3F 109.5 . . ? H3E N3 H3F 109.5 . . ? Pt1 N4 H4D 109.5 . . ? Pt1 N4 H4E 109.5 . . ? H4D N4 H4E 109.5 . . ? Pt1 N4 H4F 109.5 . . ? H4D N4 H4F 109.5 . . ? H4E N4 H4F 109.5 . . ? C11 N5 Pt2 107.4(5) . . ? C11 N5 H5D 110.2 . . ? Pt2 N5 H5D 110.2 . . ? C11 N5 H5E 110.2 . . ? Pt2 N5 H5E 110.2 . . ? H5D N5 H5E 108.5 . . ? C12 N6 Pt2 109.3(5) . . ? C12 N6 H6A 109.8 . . ? Pt2 N6 H6A 109.8 . . ? C12 N6 H6B 109.8 . . ? Pt2 N6 H6B 109.8 . . ? H6A N6 H6B 108.3 . . ? C6 O2 Pt1 127.0(5) . . ? O1 C1 N1 121.8(7) . . ? O1 C1 C2 116.7(7) . . ? N1 C1 C2 121.5(7) . . ? C1 C2 C4 108.9(6) . . ? C1 C2 C5 107.8(7) . . ? C4 C2 C5 110.5(8) . . ? C1 C2 C3 112.4(7) . . ? C4 C2 C3 108.2(7) . . ? C5 C2 C3 109.1(7) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O2 C6 N2 122.8(7) . . ? O2 C6 C7 116.4(7) . . ? N2 C6 C7 120.7(7) . . ? C9 C7 C6 115.5(7) . . ? C9 C7 C10 110.2(8) . . ? C6 C7 C10 105.4(7) . . ? C9 C7 C8 110.8(8) . . ? C6 C7 C8 108.3(7) . . ? C10 C7 C8 106.1(7) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N5 C11 C12 106.9(6) . . ? N5 C11 H11A 110.3 . . ? C12 C11 H11A 110.3 . . ? N5 C11 H11B 110.3 . . ? C12 C11 H11B 110.3 . . ? H11A C11 H11B 108.6 . . ? N6 C12 C11 107.8(7) . . ? N6 C12 H12A 110.2 . . ? C11 C12 H12A 110.2 . . ? N6 C12 H12B 110.2 . . ? C11 C12 H12B 110.2 . . ? H12A C12 H12B 108.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Pt1 Pt2 N2 -77.4(3) . . . . ? O2 Pt1 Pt2 N2 13.8(3) . . . . ? N4 Pt1 Pt2 N2 -164.6(3) . . . . ? N3 Pt1 Pt2 N2 99.1(3) . . . . ? N1 Pt1 Pt2 N6 -165.4(3) . . . . ? O2 Pt1 Pt2 N6 -74.2(3) . . . . ? N4 Pt1 Pt2 N6 107.4(3) . . . . ? N3 Pt1 Pt2 N6 11.1(3) . . . . ? N1 Pt1 Pt2 O1 13.5(2) . . . . ? O2 Pt1 Pt2 O1 104.8(2) . . . . ? N4 Pt1 Pt2 O1 -73.7(2) . . . . ? N3 Pt1 Pt2 O1 -170.0(2) . . . . ? N1 Pt1 Pt2 N5 106.9(3) . . . . ? O2 Pt1 Pt2 N5 -161.8(3) . . . . ? N4 Pt1 Pt2 N5 19.7(3) . . . . ? N3 Pt1 Pt2 N5 -76.6(3) . . . . ? N2 Pt2 O1 C1 54.2(6) . . . . ? N5 Pt2 O1 C1 -126.5(6) . . . . ? Pt1 Pt2 O1 C1 -24.6(6) . . . . ? O2 Pt1 N1 C1 -88.7(7) . . . . ? N4 Pt1 N1 C1 95.6(7) . . . . ? Pt2 Pt1 N1 C1 -10.1(6) . . . . ? N6 Pt2 N2 C6 95.0(7) . . . . ? O1 Pt2 N2 C6 -92.0(7) . . . . ? Pt1 Pt2 N2 C6 -13.8(7) . . . . ? N6 Pt2 N5 C11 17.6(5) . . . . ? O1 Pt2 N5 C11 -155.4(5) . . . . ? Pt1 Pt2 N5 C11 125.4(5) . . . . ? N2 Pt2 N6 C12 -168.3(5) . . . . ? N5 Pt2 N6 C12 11.9(5) . . . . ? Pt1 Pt2 N6 C12 -89.6(5) . . . . ? N1 Pt1 O2 C6 57.7(7) . . . . ? N3 Pt1 O2 C6 -124.7(7) . . . . ? Pt2 Pt1 O2 C6 -21.6(6) . . . . ? Pt2 O1 C1 N1 26.4(10) . . . . ? Pt2 O1 C1 C2 -152.8(5) . . . . ? Pt1 N1 C1 O1 -4.5(11) . . . . ? Pt1 N1 C1 C2 174.6(5) . . . . ? O1 C1 C2 C4 -67.5(9) . . . . ? N1 C1 C2 C4 113.4(9) . . . . ? O1 C1 C2 C5 52.4(9) . . . . ? N1 C1 C2 C5 -126.7(8) . . . . ? O1 C1 C2 C3 172.7(7) . . . . ? N1 C1 C2 C3 -6.5(11) . . . . ? Pt1 O2 C6 N2 19.6(11) . . . . ? Pt1 O2 C6 C7 -158.9(5) . . . . ? Pt2 N2 C6 O2 3.1(12) . . . . ? Pt2 N2 C6 C7 -178.5(6) . . . . ? O2 C6 C7 C9 -173.3(8) . . . . ? N2 C6 C7 C9 8.2(12) . . . . ? O2 C6 C7 C10 64.9(9) . . . . ? N2 C6 C7 C10 -113.6(9) . . . . ? O2 C6 C7 C8 -48.4(10) . . . . ? N2 C6 C7 C8 133.1(8) . . . . ? Pt2 N5 C11 C12 -43.4(7) . . . . ? Pt2 N6 C12 C11 -39.2(7) . . . . ? N5 C11 C12 N6 54.7(8) . . . . ? _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.921 _refine_diff_density_max 4.147 _refine_diff_density_min -4.477 _refine_diff_density_rms 0.387 #===END data_l406 _database_code_depnum_ccdc_archive 'CCDC 290076' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H34.50 N10 O10.25 Pt3' _chemical_formula_weight 1068.27 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(2)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z+1/2' 'y, -x, z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z-1/2' '-y, x, -z-1/2' _cell_length_a 15.4352(9) _cell_length_b 15.4352(9) _cell_length_c 12.5412(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2987.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.375 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1970 _exptl_absorpt_coefficient_mu 14.069 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1014 _exptl_absorpt_correction_T_max 0.4857 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 14873 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2710 _reflns_number_gt 2219 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0493P)^2^+49.9911P] 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 2710 _refine_ls_number_parameters 191 _refine_ls_number_restraints 504 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.1055 _refine_ls_wR_factor_gt 0.0969 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.044 _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 0.89796(4) 0.22459(3) 0.0000 0.02726(18) Uani 1 2 d SU . . Pt2 Pt 0.97338(4) 0.40176(4) 0.0000 0.02744(18) Uani 1 2 d SU . . Pt3 Pt 0.75333(4) 0.06242(5) 0.0000 0.0356(2) Uani 1 2 d SU . . N1 N 0.8310(7) 0.2873(6) 0.1152(9) 0.049(2) Uani 1 1 d U . . H1A H 0.7921 0.2548 0.1472 0.059 Uiso 1 1 calc R . . N2 N 0.9602(7) 0.1563(7) 0.1169(9) 0.047(2) Uani 1 1 d U . . H2A H 0.9225 0.1186 0.1477 0.21(13) Uiso 1 1 calc R . . H2B H 0.9808 0.1936 0.1671 0.10(6) Uiso 1 1 calc R . . H2C H 1.0052 0.1263 0.0878 0.16(11) Uiso 1 1 calc R . . N3 N 1.0709(7) 0.3892(7) 0.1051(11) 0.056(3) Uani 1 1 d DU . . H3D H 1.0794 0.4413 0.1392 0.10(6) Uiso 1 1 calc R . . H3E H 1.0558 0.3489 0.1557 0.22(14) Uiso 1 1 calc R . . N4 N 0.7461(7) 0.0609(7) 0.1598(10) 0.052(2) Uani 1 1 d U . . N5 N 0.6606(10) 0.1596(11) 0.0000 0.051(3) Uani 1 2 d SU . . N6 N 0.8443(11) -0.0279(12) 0.0000 0.056(3) Uani 1 2 d SU . . O1 O 0.8852(7) 0.4230(6) 0.1150(9) 0.066(2) Uani 1 1 d U . . O2 O 0.7879(7) 0.1081(7) 0.2202(8) 0.067(3) Uani 1 1 d U A . O3 O 0.725(2) -0.010(2) 0.201(2) 0.062(6) Uani 0.52(5) 1 d PU A 1 O4 O 0.6416(9) 0.1951(10) 0.0761(13) 0.112(4) Uani 1 1 d U A . O5 O 0.9019(16) -0.0312(15) -0.062(2) 0.060(6) Uani 0.47(3) 1 d PU . 1 O6 O 0.5000 0.0000 0.0000 0.105(14) Uani 0.50 4 d SPU . . H11 H 0.5000 0.0000 0.0678 0.2(7) Uiso 0.25 2 d SPR . . H12 H 0.4688 0.0454 0.0000 0.1(3) Uiso 0.25 2 d SPR . . O3' O 0.684(3) 0.020(2) 0.202(2) 0.063(6) Uani 0.48(5) 1 d PU A 2 O5' O 0.8503(18) -0.0733(18) -0.079(2) 0.094(8) Uani 0.53(3) 1 d PU A 2 C1 C 0.8341(9) 0.3647(8) 0.1506(12) 0.060(3) Uani 1 1 d DU . . C2 C 0.7733(10) 0.3930(10) 0.2391(13) 0.084(4) Uani 1 1 d DU . . C3 C 0.7310(15) 0.3209(13) 0.3002(18) 0.133(4) Uani 1 1 d DU . . H3A H 0.7019 0.2816 0.2503 0.199 Uiso 1 1 calc R . . H3B H 0.6883 0.3452 0.3498 0.199 Uiso 1 1 calc R . . H3C H 0.7750 0.2889 0.3403 0.199 Uiso 1 1 calc R . . C4 C 0.6993(13) 0.4427(14) 0.1811(17) 0.133(4) Uani 1 1 d DU . . H4A H 0.6809 0.4098 0.1182 0.199 Uiso 1 1 calc R . . H4B H 0.7203 0.4998 0.1589 0.199 Uiso 1 1 calc R . . H4C H 0.6501 0.4498 0.2297 0.199 Uiso 1 1 calc R . . C7 C 0.8153(14) 0.4596(14) 0.3120(17) 0.133(4) Uani 1 1 d DU . . H7A H 0.7702 0.4957 0.3446 0.199 Uiso 1 1 calc R . . H7B H 0.8545 0.4962 0.2703 0.199 Uiso 1 1 calc R . . H7C H 0.8480 0.4298 0.3680 0.199 Uiso 1 1 calc R . . C6 C 1.1525(10) 0.3624(15) 0.0537(16) 0.100(5) Uani 1 1 d DU . . H6A H 1.1992 0.4014 0.0785 0.24(16) Uiso 1 1 calc R . . H6B H 1.1668 0.3032 0.0785 0.09(6) 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 0.0267(3) 0.0198(3) 0.0353(3) 0.000 0.000 0.0011(2) Pt2 0.0292(3) 0.0197(3) 0.0334(3) 0.000 0.000 0.0011(2) Pt3 0.0257(3) 0.0559(4) 0.0252(3) 0.000 0.000 -0.0037(3) N1 0.049(5) 0.036(4) 0.062(5) -0.001(4) 0.030(4) 0.000(4) N2 0.054(6) 0.038(5) 0.048(6) 0.003(5) -0.005(5) -0.005(5) N3 0.058(6) 0.033(5) 0.078(7) 0.001(5) -0.019(5) 0.002(5) N4 0.055(5) 0.051(5) 0.050(6) 0.004(5) 0.003(5) -0.008(5) N5 0.043(6) 0.056(7) 0.054(7) 0.000 0.000 -0.001(6) N6 0.044(7) 0.056(7) 0.067(8) 0.000 0.000 0.013(6) O1 0.071(5) 0.039(4) 0.088(6) -0.010(4) 0.043(5) 0.003(4) O2 0.086(6) 0.074(6) 0.041(5) -0.007(5) 0.008(5) -0.023(5) O3 0.064(13) 0.070(12) 0.052(9) 0.009(9) 0.010(10) -0.019(10) O4 0.094(8) 0.120(9) 0.122(9) -0.024(8) 0.013(8) 0.030(7) O5 0.052(10) 0.053(10) 0.077(10) -0.005(9) 0.015(9) 0.007(8) O6 0.10(3) 0.11(3) 0.10(3) 0.000 0.000 -0.01(3) O3' 0.067(13) 0.074(12) 0.049(10) 0.005(10) 0.030(10) -0.017(11) O5' 0.072(14) 0.095(15) 0.116(15) -0.055(13) -0.022(12) 0.037(12) C1 0.066(6) 0.040(5) 0.072(6) -0.006(5) 0.031(6) 0.001(5) C2 0.088(8) 0.061(7) 0.102(9) -0.007(7) 0.046(8) 0.004(7) C3 0.142(8) 0.131(8) 0.126(8) -0.009(7) 0.067(7) 0.008(7) C4 0.142(8) 0.131(8) 0.126(8) -0.009(7) 0.067(7) 0.008(7) C7 0.142(8) 0.131(8) 0.126(8) -0.009(7) 0.067(7) 0.008(7) C6 0.072(9) 0.104(10) 0.126(11) -0.016(10) -0.019(9) 0.029(9) _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 N1 2.023(10) 6 ? Pt1 N1 2.023(10) . ? Pt1 N2 2.045(10) 6 ? Pt1 N2 2.045(10) . ? Pt1 Pt2 2.9721(8) . ? Pt1 Pt3 3.3540(9) . ? Pt2 O1 2.010(9) 6 ? Pt2 O1 2.010(9) . ? Pt2 N3 2.010(11) . ? Pt2 N3 2.010(11) 6 ? Pt2 Pt2 3.1420(11) 5_765 ? Pt3 N6 1.978(16) . ? Pt3 N4 2.007(12) . ? Pt3 N4 2.007(12) 6 ? Pt3 N5 2.073(17) . ? N1 C1 1.275(16) . ? N1 H1A 0.8800 . ? N2 H2A 0.9100 . ? N2 H2B 0.9100 . ? N2 H2C 0.9100 . ? N3 C6 1.473(12) . ? N3 H3D 0.9200 . ? N3 H3E 0.9200 . ? N4 O2 1.233(14) . ? N4 O3 1.26(3) . ? N4 O3' 1.26(3) . ? N5 O4 1.139(16) . ? N5 O4 1.139(16) 6 ? N6 O5 1.19(2) 6 ? N6 O5 1.19(2) . ? N6 O5' 1.22(2) . ? N6 O5' 1.22(2) 6 ? O1 C1 1.278(15) . ? O5 O5 1.56(5) 6 ? O6 H11 0.8502 . ? O6 H11 0.8502 . ? O6 H12 0.8502 . ? C1 C2 1.518(14) . ? C2 C3 1.501(15) . ? C2 C7 1.520(16) . ? C2 C4 1.556(16) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C6 C6 1.35(4) 6 ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? 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 N1 Pt1 N1 91.2(7) 6 . ? N1 Pt1 N2 88.6(5) 6 6 ? N1 Pt1 N2 176.9(4) . 6 ? N1 Pt1 N2 176.9(4) 6 . ? N1 Pt1 N2 88.6(5) . . ? N2 Pt1 N2 91.6(7) 6 . ? N1 Pt1 Pt2 76.1(3) 6 . ? N1 Pt1 Pt2 76.1(3) . . ? N2 Pt1 Pt2 106.9(3) 6 . ? N2 Pt1 Pt2 106.9(3) . . ? N1 Pt1 Pt3 91.0(3) 6 . ? N1 Pt1 Pt3 91.0(3) . . ? N2 Pt1 Pt3 85.9(3) 6 . ? N2 Pt1 Pt3 85.9(3) . . ? Pt2 Pt1 Pt3 161.33(3) . . ? O1 Pt2 O1 91.7(7) 6 . ? O1 Pt2 N3 173.3(5) 6 . ? O1 Pt2 N3 93.0(5) . . ? O1 Pt2 N3 93.0(5) 6 6 ? O1 Pt2 N3 173.3(5) . 6 ? N3 Pt2 N3 81.9(7) . 6 ? O1 Pt2 Pt1 83.4(3) 6 . ? O1 Pt2 Pt1 83.4(3) . . ? N3 Pt2 Pt1 101.8(3) . . ? N3 Pt2 Pt1 101.8(3) 6 . ? O1 Pt2 Pt2 91.1(3) 6 5_765 ? O1 Pt2 Pt2 91.1(3) . 5_765 ? N3 Pt2 Pt2 84.1(3) . 5_765 ? N3 Pt2 Pt2 84.1(3) 6 5_765 ? Pt1 Pt2 Pt2 172.10(3) . 5_765 ? N6 Pt3 N4 91.8(3) . . ? N6 Pt3 N4 91.8(3) . 6 ? N4 Pt3 N4 173.5(7) . 6 ? N6 Pt3 N5 178.4(7) . . ? N4 Pt3 N5 88.3(3) . . ? N4 Pt3 N5 88.3(3) 6 . ? N6 Pt3 Pt1 93.0(5) . . ? N4 Pt3 Pt1 92.6(3) . . ? N4 Pt3 Pt1 92.6(3) 6 . ? N5 Pt3 Pt1 85.4(4) . . ? C1 N1 Pt1 132.7(9) . . ? C1 N1 H1A 113.6 . . ? Pt1 N1 H1A 113.6 . . ? Pt1 N2 H2A 109.5 . . ? Pt1 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? Pt1 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? C6 N3 Pt2 112.4(11) . . ? C6 N3 H3D 109.1 . . ? Pt2 N3 H3D 109.1 . . ? C6 N3 H3E 109.1 . . ? Pt2 N3 H3E 109.1 . . ? H3D N3 H3E 107.9 . . ? O2 N4 O3 113.5(16) . . ? O2 N4 O3' 115.8(16) . . ? O2 N4 Pt3 125.2(9) . . ? O3 N4 Pt3 115.8(15) . . ? O3' N4 Pt3 117.8(15) . . ? O4 N5 O4 114(2) . 6 ? O4 N5 Pt3 121.7(11) . . ? O4 N5 Pt3 121.7(11) 6 . ? O5 N6 O5 83(3) 6 . ? O5 N6 O5' 117(2) 6 . ? O5 N6 O5' 51.8(15) . . ? O5 N6 O5' 51.8(15) 6 6 ? O5 N6 O5' 117(2) . 6 ? O5' N6 O5' 109(3) . 6 ? O5 N6 Pt3 124.3(14) 6 . ? O5 N6 Pt3 124.3(14) . . ? O5' N6 Pt3 117.4(13) . . ? O5' N6 Pt3 117.4(13) 6 . ? C1 O1 Pt2 123.6(8) . . ? N6 O5 O5 48.7(14) . 6 ? H11 O6 H12 90.0 . . ? H11 O6 H12 90.0 . . ? N1 C1 O1 124.2(11) . . ? N1 C1 C2 120.1(12) . . ? O1 C1 C2 115.7(11) . . ? C3 C2 C1 115.4(13) . . ? C3 C2 C7 112.4(16) . . ? C1 C2 C7 111.8(13) . . ? C3 C2 C4 106.5(15) . . ? C1 C2 C4 104.7(13) . . ? C7 C2 C4 105.1(14) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C6 N3 115.9(9) 6 . ? C6 C6 H6A 108.3 6 . ? N3 C6 H6A 108.3 . . ? C6 C6 H6B 108.3 6 . ? N3 C6 H6B 108.3 . . ? H6A C6 H6B 107.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Pt1 Pt2 O1 1.1(5) 6 . . 6 ? N1 Pt1 Pt2 O1 -93.6(5) . . . 6 ? N2 Pt1 Pt2 O1 85.3(5) 6 . . 6 ? N2 Pt1 Pt2 O1 -177.8(5) . . . 6 ? Pt3 Pt1 Pt2 O1 -46.3(3) . . . 6 ? N1 Pt1 Pt2 O1 93.6(5) 6 . . . ? N1 Pt1 Pt2 O1 -1.1(5) . . . . ? N2 Pt1 Pt2 O1 177.8(5) 6 . . . ? N2 Pt1 Pt2 O1 -85.3(5) . . . . ? Pt3 Pt1 Pt2 O1 46.3(3) . . . . ? N1 Pt1 Pt2 N3 -174.7(5) 6 . . . ? N1 Pt1 Pt2 N3 90.6(5) . . . . ? N2 Pt1 Pt2 N3 -90.5(5) 6 . . . ? N2 Pt1 Pt2 N3 6.4(5) . . . . ? Pt3 Pt1 Pt2 N3 138.0(4) . . . . ? N1 Pt1 Pt2 N3 -90.6(5) 6 . . 6 ? N1 Pt1 Pt2 N3 174.7(5) . . . 6 ? N2 Pt1 Pt2 N3 -6.4(5) 6 . . 6 ? N2 Pt1 Pt2 N3 90.5(5) . . . 6 ? Pt3 Pt1 Pt2 N3 -138.0(4) . . . 6 ? N1 Pt1 Pt3 N6 134.4(3) 6 . . . ? N1 Pt1 Pt3 N6 -134.4(3) . . . . ? N2 Pt1 Pt3 N6 45.9(3) 6 . . . ? N2 Pt1 Pt3 N6 -45.9(3) . . . . ? Pt2 Pt1 Pt3 N6 180.0 . . . . ? N1 Pt1 Pt3 N4 -133.7(5) 6 . . . ? N1 Pt1 Pt3 N4 -42.5(5) . . . . ? N2 Pt1 Pt3 N4 137.9(5) 6 . . . ? N2 Pt1 Pt3 N4 46.0(5) . . . . ? Pt2 Pt1 Pt3 N4 -88.1(3) . . . . ? N1 Pt1 Pt3 N4 42.5(5) 6 . . 6 ? N1 Pt1 Pt3 N4 133.7(5) . . . 6 ? N2 Pt1 Pt3 N4 -46.0(5) 6 . . 6 ? N2 Pt1 Pt3 N4 -137.9(5) . . . 6 ? Pt2 Pt1 Pt3 N4 88.1(3) . . . 6 ? N1 Pt1 Pt3 N5 -45.6(3) 6 . . . ? N1 Pt1 Pt3 N5 45.6(3) . . . . ? N2 Pt1 Pt3 N5 -134.1(3) 6 . . . ? N2 Pt1 Pt3 N5 134.1(3) . . . . ? Pt2 Pt1 Pt3 N5 0.0 . . . . ? N1 Pt1 N1 C1 -74.7(16) 6 . . . ? Pt2 Pt1 N1 C1 0.7(14) . . . . ? Pt3 Pt1 N1 C1 -165.7(15) . . . . ? O1 Pt2 N3 C6 173.7(12) . . . . ? N3 Pt2 N3 C6 -10.6(14) 6 . . . ? Pt1 Pt2 N3 C6 89.8(12) . . . . ? Pt2 Pt2 N3 C6 -95.5(12) 5_765 . . . ? N6 Pt3 N4 O2 91.8(12) . . . . ? N5 Pt3 N4 O2 -86.6(12) . . . . ? Pt1 Pt3 N4 O2 -1.3(11) . . . . ? N6 Pt3 N4 O3 -60(2) . . . . ? N5 Pt3 N4 O3 121(2) . . . . ? Pt1 Pt3 N4 O3 -153(2) . . . . ? N6 Pt3 N4 O3' -101(3) . . . . ? N5 Pt3 N4 O3' 81(3) . . . . ? Pt1 Pt3 N4 O3' 166(3) . . . . ? N4 Pt3 N5 O4 12.6(17) . . . . ? N4 Pt3 N5 O4 -173.0(17) 6 . . . ? Pt1 Pt3 N5 O4 -80.2(17) . . . . ? N4 Pt3 N5 O4 173.0(17) . . . 6 ? N4 Pt3 N5 O4 -12.6(17) 6 . . 6 ? Pt1 Pt3 N5 O4 80.2(17) . . . 6 ? N4 Pt3 N6 O5 -40(2) . . . 6 ? N4 Pt3 N6 O5 146(2) 6 . . 6 ? Pt1 Pt3 N6 O5 53(2) . . . 6 ? N4 Pt3 N6 O5 -146(2) . . . . ? N4 Pt3 N6 O5 40(2) 6 . . . ? Pt1 Pt3 N6 O5 -53(2) . . . . ? N4 Pt3 N6 O5' 154(2) . . . . ? N4 Pt3 N6 O5' -21(2) 6 . . . ? Pt1 Pt3 N6 O5' -114(2) . . . . ? N4 Pt3 N6 O5' 21(2) . . . 6 ? Pt1 Pt3 N6 O5' 114(2) . . . 6 ? O1 Pt2 O1 C1 85.3(13) 6 . . . ? N3 Pt2 O1 C1 -99.5(13) . . . . ? Pt1 Pt2 O1 C1 2.1(13) . . . . ? Pt2 Pt2 O1 C1 176.4(13) 5_765 . . . ? O5' N6 O5 O5 -133(2) . . . 6 ? O5' N6 O5 O5 -40(2) 6 . . 6 ? Pt3 N6 O5 O5 127(2) . . . 6 ? Pt1 N1 C1 O1 1(3) . . . . ? Pt1 N1 C1 C2 179.4(11) . . . . ? Pt2 O1 C1 N1 -2(2) . . . . ? Pt2 O1 C1 C2 178.8(11) . . . . ? N1 C1 C2 C3 17(2) . . . . ? O1 C1 C2 C3 -164.4(17) . . . . ? N1 C1 C2 C7 146.8(18) . . . . ? O1 C1 C2 C7 -34(2) . . . . ? N1 C1 C2 C4 -99.9(18) . . . . ? O1 C1 C2 C4 78.9(18) . . . . ? Pt2 N3 C6 C6 8.9(11) . . . 6 ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 4.426 _refine_diff_density_min -2.572 _refine_diff_density_rms 0.233 #===END #===END data_pr _database_code_depnum_ccdc_archive 'CCDC 290077' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H60 N12 O16 Pd Pt2' _chemical_formula_weight 1293.44 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' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.644(5) _cell_length_b 11.104(5) _cell_length_c 11.577(5) _cell_angle_alpha 113.877(5) _cell_angle_beta 104.490(6) _cell_angle_gamma 103.086(6) _cell_volume 1125.4(9) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.908 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 630 _exptl_absorpt_coefficient_mu 6.669 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2760 _exptl_absorpt_correction_T_max 0.6904 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 3323 _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_sigmaI/netI 0.0521 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 4.82 _diffrn_reflns_theta_max 22.98 _reflns_number_total 2679 _reflns_number_gt 2398 _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^)+(0.1034P)^2^+10.1755P] 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 2679 _refine_ls_number_parameters 253 _refine_ls_number_restraints 1393 _refine_ls_R_factor_all 0.0617 _refine_ls_R_factor_gt 0.0564 _refine_ls_wR_factor_ref 0.1615 _refine_ls_wR_factor_gt 0.1558 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 0.931 _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 Pd1 Pd 0.5000 1.0000 0.5000 0.0325(3) Uani 1 2 d S . . Pt1 Pt 0.61443(5) 0.95307(5) 0.70219(4) 0.0393(2) Uani 1 1 d . . . N1 N 0.6042(14) 0.7775(15) 0.5438(14) 0.0672(18) Uani 1 1 d U . . H1 H 0.6391 0.7232 0.5654 0.081 Uiso 1 1 calc R . . N2 N 0.4136(14) 0.8654(14) 0.6699(13) 0.0632(17) Uani 1 1 d U . . H2 H 0.3979 0.8301 0.7210 0.076 Uiso 1 1 calc R . . N3 N 0.6419(14) 1.1409(15) 0.8638(14) 0.0691(19) Uani 1 1 d U . . H3D H 0.5980 1.1878 0.8314 0.083 Uiso 1 1 calc R . . H3E H 0.6022 1.1220 0.9176 0.083 Uiso 1 1 calc R . . N4 N 0.8216(15) 1.0556(15) 0.7462(15) 0.0743(19) Uani 1 1 d U . . H4D H 0.8749 1.0164 0.7805 0.089 Uiso 1 1 calc R . . H4E H 0.8335 1.0492 0.6699 0.089 Uiso 1 1 calc R . . N5 N 0.5923(13) 0.8587(15) 0.9721(13) 0.073(2) Uani 1 1 d DU . . N6 N 0.8584(15) 0.7419(14) 0.7753(14) 0.082(2) Uani 1 1 d DU . . O1 O 0.4958(11) 0.8110(11) 0.3701(10) 0.0618(12) Uani 1 1 d U . . O2 O 0.3144(11) 0.9029(11) 0.4947(10) 0.0618(12) Uani 1 1 d U . . O3 O 0.4646(10) 0.8292(13) 0.9164(11) 0.076(2) Uani 1 1 d DU . . O4 O 0.6731(12) 0.8839(14) 0.9169(12) 0.087(2) Uani 1 1 d DU . . O5 O 0.6393(13) 0.8637(15) 1.0833(11) 0.096(3) Uani 1 1 d DU . . O6 O 0.9355(14) 0.8702(12) 0.8371(13) 0.108(3) Uani 1 1 d DU . . O7 O 0.9017(16) 0.6732(14) 0.8354(14) 0.120(4) Uani 1 1 d DU . . O8 O 0.8004(15) 0.6761(14) 0.6545(12) 0.114(3) Uani 1 1 d DU . . C1 C 0.5523(18) 0.7358(18) 0.4145(17) 0.0671(19) Uani 1 1 d U . . C2 C 0.5529(18) 0.6043(18) 0.3055(17) 0.069(2) Uani 1 1 d U . . C3 C 0.596(2) 0.507(2) 0.353(2) 0.092(3) Uani 1 1 d U . . H3A H 0.6698 0.5617 0.4416 0.138 Uiso 1 1 calc R . . H3B H 0.6270 0.4469 0.2893 0.138 Uiso 1 1 calc R . . H3C H 0.5170 0.4490 0.3576 0.138 Uiso 1 1 calc R . . C4 C 0.670(2) 0.659(2) 0.255(2) 0.095(4) Uani 1 1 d U . . H4A H 0.6348 0.6978 0.1992 0.143 Uiso 1 1 calc R . . H4B H 0.6923 0.5805 0.2020 0.143 Uiso 1 1 calc R . . H4C H 0.7521 0.7301 0.3326 0.143 Uiso 1 1 calc R . . C5 C 0.418(2) 0.526(2) 0.185(2) 0.101(4) Uani 1 1 d U . . H5A H 0.3542 0.4619 0.1993 0.152 Uiso 1 1 calc R . . H5B H 0.4331 0.4733 0.1043 0.152 Uiso 1 1 calc R . . H5C H 0.3782 0.5922 0.1740 0.152 Uiso 1 1 calc R . . C6 C 0.3043(17) 0.8561(17) 0.5803(16) 0.0635(19) Uani 1 1 d U . . C7 C 0.1555(16) 0.7851(17) 0.5634(16) 0.062(2) Uani 1 1 d U . . C8 C 0.0791(19) 0.6545(19) 0.4179(18) 0.080(3) Uani 1 1 d U . . H8A H 0.0871 0.6834 0.3514 0.120 Uiso 1 1 calc R . . H8B H -0.0177 0.6144 0.4013 0.120 Uiso 1 1 calc R . . H8C H 0.1208 0.5850 0.4108 0.120 Uiso 1 1 calc R . . C9 C 0.0829(17) 0.8936(18) 0.5805(18) 0.070(3) Uani 1 1 d U . . H9A H 0.1316 0.9743 0.6706 0.105 Uiso 1 1 calc R . . H9B H -0.0120 0.8503 0.5680 0.105 Uiso 1 1 calc R . . H9C H 0.0839 0.9236 0.5136 0.105 Uiso 1 1 calc R . . C10 C 0.1521(18) 0.7387(18) 0.6722(17) 0.070(3) Uani 1 1 d U . . H10A H 0.1927 0.6678 0.6602 0.104 Uiso 1 1 calc R . . H10B H 0.0572 0.7003 0.6619 0.104 Uiso 1 1 calc R . . H10C H 0.2045 0.8192 0.7619 0.104 Uiso 1 1 calc R . . C11 C 0.7864(18) 1.230(2) 0.9445(18) 0.080(2) Uani 1 1 d DU . . H11 H 0.8187 1.1845 0.9964 0.096 Uiso 1 1 calc R . . C12 C 0.8613(19) 1.207(2) 0.8487(18) 0.083(2) Uani 1 1 d DU . . H12A H 0.8434 1.2587 0.8003 0.100 Uiso 1 1 calc R . . H12B H 0.9609 1.2460 0.9021 0.100 Uiso 1 1 calc R . . C13 C 0.815(2) 1.371(2) 1.050(2) 0.105(4) Uani 1 1 d U . . H13A H 0.9040 1.4044 1.1219 0.157 Uiso 1 1 calc R . . H13B H 0.7435 1.3697 1.0858 0.157 Uiso 1 1 calc R . . H13C H 0.8183 1.4339 1.0117 0.157 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 Pd1 0.0407(7) 0.0333(7) 0.0305(7) 0.0187(6) 0.0168(5) 0.0161(5) Pt1 0.0447(4) 0.0494(4) 0.0340(3) 0.0257(3) 0.0181(2) 0.0214(2) N1 0.083(3) 0.079(3) 0.068(3) 0.049(2) 0.039(2) 0.041(3) N2 0.080(3) 0.076(3) 0.066(3) 0.051(2) 0.040(2) 0.041(3) N3 0.082(3) 0.081(3) 0.068(3) 0.048(3) 0.037(3) 0.038(3) N4 0.083(3) 0.086(3) 0.070(3) 0.045(3) 0.036(3) 0.039(3) N5 0.086(3) 0.083(3) 0.069(3) 0.049(3) 0.036(3) 0.036(3) N6 0.092(3) 0.087(3) 0.074(3) 0.042(3) 0.034(3) 0.035(3) O1 0.078(2) 0.075(2) 0.065(2) 0.050(2) 0.0388(19) 0.042(2) O2 0.078(2) 0.075(2) 0.065(2) 0.050(2) 0.0388(19) 0.042(2) O3 0.085(4) 0.092(4) 0.069(4) 0.048(3) 0.037(3) 0.038(3) O4 0.092(4) 0.095(4) 0.083(4) 0.051(3) 0.030(3) 0.039(3) O5 0.103(5) 0.104(5) 0.078(4) 0.046(4) 0.026(4) 0.038(4) O6 0.106(4) 0.105(4) 0.092(4) 0.035(4) 0.033(4) 0.035(4) O7 0.113(5) 0.110(5) 0.101(5) 0.035(5) 0.024(5) 0.034(5) O8 0.107(4) 0.108(4) 0.094(4) 0.030(4) 0.025(4) 0.035(4) C1 0.082(3) 0.078(3) 0.068(3) 0.048(3) 0.039(3) 0.041(3) C2 0.084(3) 0.078(3) 0.070(3) 0.046(3) 0.037(3) 0.044(3) C3 0.102(5) 0.090(5) 0.084(5) 0.039(4) 0.033(4) 0.042(4) C4 0.100(5) 0.095(5) 0.081(5) 0.028(5) 0.043(5) 0.039(5) C5 0.100(5) 0.091(5) 0.090(5) 0.028(5) 0.027(5) 0.039(5) C6 0.079(3) 0.076(3) 0.066(3) 0.050(3) 0.038(3) 0.041(3) C7 0.077(3) 0.075(3) 0.066(3) 0.050(3) 0.041(3) 0.040(3) C8 0.084(5) 0.083(5) 0.075(5) 0.037(4) 0.037(4) 0.031(5) C9 0.077(5) 0.081(5) 0.076(5) 0.046(4) 0.040(4) 0.041(5) C10 0.080(5) 0.080(4) 0.072(4) 0.049(4) 0.041(4) 0.035(4) C11 0.087(3) 0.086(3) 0.074(3) 0.041(3) 0.035(3) 0.036(3) C12 0.088(3) 0.089(3) 0.075(3) 0.040(3) 0.036(3) 0.033(3) C13 0.103(6) 0.100(5) 0.087(5) 0.034(5) 0.028(5) 0.029(5) _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 Pd1 O2 1.998(10) 2_676 ? Pd1 O2 1.998(10) . ? Pd1 O1 2.009(11) . ? Pd1 O1 2.009(11) 2_676 ? Pd1 Pt1 2.6613(10) . ? Pd1 Pt1 2.6613(10) 2_676 ? Pt1 N2 2.005(13) . ? Pt1 N1 2.021(14) . ? Pt1 N3 2.056(14) . ? Pt1 N4 2.062(14) . ? N1 C1 1.29(2) . ? N1 H1 0.8600 . ? N2 C6 1.302(19) . ? N2 H2 0.8600 . ? N3 C11 1.44(2) . ? N3 H3D 0.9000 . ? N3 H3E 0.9000 . ? N4 C12 1.49(2) . ? N4 H4D 0.9000 . ? N4 H4E 0.9000 . ? N5 O5 1.232(11) . ? N5 O4 1.240(12) . ? N5 O3 1.249(11) . ? N6 O8 1.186(12) . ? N6 O6 1.252(12) . ? N6 O7 1.307(12) . ? O1 C1 1.321(17) . ? O2 C6 1.306(16) . ? C1 C2 1.50(2) . ? C2 C5 1.49(2) . ? C2 C3 1.50(2) . ? C2 C4 1.60(2) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.52(2) . ? C7 C10 1.546(19) . ? C7 C9 1.55(2) . ? C7 C8 1.55(2) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C13 1.44(3) . ? C11 C12 1.495(15) . ? C11 H11 0.9800 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? 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 O2 Pd1 O2 180.0 2_676 . ? O2 Pd1 O1 90.6(4) 2_676 . ? O2 Pd1 O1 89.4(4) . . ? O2 Pd1 O1 89.4(4) 2_676 2_676 ? O2 Pd1 O1 90.6(4) . 2_676 ? O1 Pd1 O1 180.0 . 2_676 ? O2 Pd1 Pt1 92.8(3) 2_676 . ? O2 Pd1 Pt1 87.2(3) . . ? O1 Pd1 Pt1 87.4(3) . . ? O1 Pd1 Pt1 92.6(3) 2_676 . ? O2 Pd1 Pt1 87.2(3) 2_676 2_676 ? O2 Pd1 Pt1 92.8(3) . 2_676 ? O1 Pd1 Pt1 92.6(3) . 2_676 ? O1 Pd1 Pt1 87.4(3) 2_676 2_676 ? Pt1 Pd1 Pt1 180.0 . 2_676 ? N2 Pt1 N1 92.3(6) . . ? N2 Pt1 N3 92.8(5) . . ? N1 Pt1 N3 174.8(5) . . ? N2 Pt1 N4 176.1(5) . . ? N1 Pt1 N4 91.6(6) . . ? N3 Pt1 N4 83.3(6) . . ? N2 Pt1 Pd1 82.0(3) . . ? N1 Pt1 Pd1 81.4(4) . . ? N3 Pt1 Pd1 98.2(4) . . ? N4 Pt1 Pd1 98.5(4) . . ? C1 N1 Pt1 128.7(11) . . ? C1 N1 H1 115.7 . . ? Pt1 N1 H1 115.7 . . ? C6 N2 Pt1 127.3(10) . . ? C6 N2 H2 116.4 . . ? Pt1 N2 H2 116.4 . . ? C11 N3 Pt1 112.9(10) . . ? C11 N3 H3D 109.0 . . ? Pt1 N3 H3D 109.0 . . ? C11 N3 H3E 109.0 . . ? Pt1 N3 H3E 109.0 . . ? H3D N3 H3E 107.8 . . ? C12 N4 Pt1 107.0(10) . . ? C12 N4 H4D 110.3 . . ? Pt1 N4 H4D 110.3 . . ? C12 N4 H4E 110.3 . . ? Pt1 N4 H4E 110.3 . . ? H4D N4 H4E 108.6 . . ? O5 N5 O4 119.3(12) . . ? O5 N5 O3 120.1(11) . . ? O4 N5 O3 120.6(11) . . ? O8 N6 O6 122.4(13) . . ? O8 N6 O7 116.4(13) . . ? O6 N6 O7 112.5(12) . . ? C1 O1 Pd1 121.6(10) . . ? C6 O2 Pd1 121.4(10) . . ? N1 C1 O1 120.7(15) . . ? N1 C1 C2 124.1(14) . . ? O1 C1 C2 115.2(13) . . ? C5 C2 C1 111.7(15) . . ? C5 C2 C3 111.0(16) . . ? C1 C2 C3 115.2(14) . . ? C5 C2 C4 107.1(16) . . ? C1 C2 C4 105.3(14) . . ? C3 C2 C4 106.0(15) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 O2 122.2(15) . . ? N2 C6 C7 122.8(12) . . ? O2 C6 C7 115.0(13) . . ? C6 C7 C10 112.0(12) . . ? C6 C7 C9 108.0(12) . . ? C10 C7 C9 108.3(13) . . ? C6 C7 C8 108.1(13) . . ? C10 C7 C8 110.1(13) . . ? C9 C7 C8 110.3(13) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N3 C11 C13 116.7(15) . . ? N3 C11 C12 107.0(15) . . ? C13 C11 C12 120.8(17) . . ? N3 C11 H11 103.3 . . ? C13 C11 H11 103.3 . . ? C12 C11 H11 103.3 . . ? N4 C12 C11 114.9(15) . . ? N4 C12 H12A 108.5 . . ? C11 C12 H12A 108.5 . . ? N4 C12 H12B 108.5 . . ? C11 C12 H12B 108.5 . . ? H12A C12 H12B 107.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Pd1 Pt1 N2 179.3(5) 2_676 . . . ? O2 Pd1 Pt1 N2 -0.7(5) . . . . ? O1 Pd1 Pt1 N2 -90.3(5) . . . . ? O1 Pd1 Pt1 N2 89.7(5) 2_676 . . . ? O2 Pd1 Pt1 N1 -87.2(5) 2_676 . . . ? O2 Pd1 Pt1 N1 92.8(5) . . . . ? O1 Pd1 Pt1 N1 3.3(5) . . . . ? O1 Pd1 Pt1 N1 -176.7(5) 2_676 . . . ? O2 Pd1 Pt1 N3 87.6(5) 2_676 . . . ? O2 Pd1 Pt1 N3 -92.4(5) . . . . ? O1 Pd1 Pt1 N3 178.1(4) . . . . ? O1 Pd1 Pt1 N3 -1.9(4) 2_676 . . . ? O2 Pd1 Pt1 N4 3.2(5) 2_676 . . . ? O2 Pd1 Pt1 N4 -176.8(5) . . . . ? O1 Pd1 Pt1 N4 93.7(5) . . . . ? O1 Pd1 Pt1 N4 -86.3(5) 2_676 . . . ? N2 Pt1 N1 C1 78.7(15) . . . . ? N4 Pt1 N1 C1 -101.2(15) . . . . ? Pd1 Pt1 N1 C1 -2.9(14) . . . . ? N1 Pt1 N2 C6 -81.2(14) . . . . ? N3 Pt1 N2 C6 97.8(14) . . . . ? Pd1 Pt1 N2 C6 -0.2(13) . . . . ? N2 Pt1 N3 C11 165.7(11) . . . . ? N4 Pt1 N3 C11 -14.4(11) . . . . ? Pd1 Pt1 N3 C11 -112.1(10) . . . . ? N1 Pt1 N4 C12 169.8(11) . . . . ? N3 Pt1 N4 C12 -9.1(10) . . . . ? Pd1 Pt1 N4 C12 88.2(10) . . . . ? O2 Pd1 O1 C1 87.6(11) 2_676 . . . ? O2 Pd1 O1 C1 -92.4(11) . . . . ? Pt1 Pd1 O1 C1 -5.1(11) . . . . ? Pt1 Pd1 O1 C1 174.9(11) 2_676 . . . ? O1 Pd1 O2 C6 89.2(11) . . . . ? O1 Pd1 O2 C6 -90.8(11) 2_676 . . . ? Pt1 Pd1 O2 C6 1.9(11) . . . . ? Pt1 Pd1 O2 C6 -178.1(11) 2_676 . . . ? Pt1 N1 C1 O1 0(2) . . . . ? Pt1 N1 C1 C2 178.7(12) . . . . ? Pd1 O1 C1 N1 5(2) . . . . ? Pd1 O1 C1 C2 -174.4(10) . . . . ? N1 C1 C2 C5 138.3(18) . . . . ? O1 C1 C2 C5 -43(2) . . . . ? N1 C1 C2 C3 11(2) . . . . ? O1 C1 C2 C3 -170.5(15) . . . . ? N1 C1 C2 C4 -105.9(18) . . . . ? O1 C1 C2 C4 73.0(18) . . . . ? Pt1 N2 C6 O2 2(2) . . . . ? Pt1 N2 C6 C7 179.2(11) . . . . ? Pd1 O2 C6 N2 -3(2) . . . . ? Pd1 O2 C6 C7 179.7(9) . . . . ? N2 C6 C7 C10 5(2) . . . . ? O2 C6 C7 C10 -177.4(14) . . . . ? N2 C6 C7 C9 124.1(16) . . . . ? O2 C6 C7 C9 -58.2(17) . . . . ? N2 C6 C7 C8 -116.6(17) . . . . ? O2 C6 C7 C8 61.1(17) . . . . ? Pt1 N3 C11 C13 172.6(14) . . . . ? Pt1 N3 C11 C12 33.7(16) . . . . ? Pt1 N4 C12 C11 31.7(18) . . . . ? N3 C11 C12 N4 -44(2) . . . . ? C13 C11 C12 N4 179.4(16) . . . . ? _diffrn_measured_fraction_theta_max 0.856 _diffrn_reflns_theta_full 22.98 _diffrn_measured_fraction_theta_full 0.856 _refine_diff_density_max 2.513 _refine_diff_density_min -1.935 _refine_diff_density_rms 0.220 #===END data_pt2 _database_code_depnum_ccdc_archive 'CCDC 290078' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H50 Cl2 N6 O11 Pt2' _chemical_formula_weight 1035.76 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' 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 10.513(3) _cell_length_b 16.117(4) _cell_length_c 10.945(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1854.5(9) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.855 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1004 _exptl_absorpt_coefficient_mu 7.734 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1436 _exptl_absorpt_correction_T_max 0.2693 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 9003 _diffrn_reflns_av_R_equivalents 0.0695 _diffrn_reflns_av_sigmaI/netI 0.0658 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3248 _reflns_number_gt 2808 _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^)+(0.0747P)^2^+4.9200P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.16(3) _refine_ls_number_reflns 3248 _refine_ls_number_parameters 199 _refine_ls_number_restraints 168 _refine_ls_R_factor_all 0.0601 _refine_ls_R_factor_gt 0.0523 _refine_ls_wR_factor_ref 0.1375 _refine_ls_wR_factor_gt 0.1324 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.002 _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 0.35455(4) 1.00342(2) 0.15443(4) 0.03993(18) Uani 1 1 d . . . Cl1 Cl 0.9959(5) 0.78301(15) 0.0885(3) 0.0502(7) Uani 1 1 d U . . O1 O 0.3911(10) 0.9181(6) 0.2849(12) 0.054(3) Uani 1 1 d U . . N2 N 0.2948(11) 0.9150(6) 0.0351(14) 0.038(3) Uani 1 1 d . . . H2A H 0.3628 0.8831 0.0109 0.045 Uiso 1 1 calc R . . H2B H 0.2366 0.8809 0.0727 0.045 Uiso 1 1 calc R . . N3 N 0.3043(10) 1.0823(6) 0.0200(14) 0.039(3) Uani 1 1 d . . . H3A H 0.2253 1.1044 0.0360 0.047 Uiso 1 1 calc R . . H3B H 0.3619 1.1252 0.0154 0.047 Uiso 1 1 calc R . . N1 N 0.6010(11) 0.9024(6) 0.2700(12) 0.040(3) Uani 1 1 d . . . H1 H 0.6649 0.8702 0.2912 0.048 Uiso 1 1 calc R . . O2 O 0.8890(12) 0.7814(8) 0.169(2) 0.087(4) Uani 1 1 d U . . O3 O 1.1120(12) 0.7883(8) 0.154(2) 0.083(4) Uani 1 1 d U . . O4 O 0.9870(13) 0.8538(6) 0.0117(11) 0.083(3) Uani 1 1 d U . . O5 O 0.9961(14) 0.7120(6) 0.0094(11) 0.083(3) Uani 1 1 d U . . O6 O 0.098(2) 0.9365(16) 0.386(2) 0.077(6) Uani 0.50 1 d PU . . H6A H 0.1747 0.9518 0.3391 0.092 Uiso 0.50 1 d PR . . H6B H 0.0914 0.9797 0.4502 0.092 Uiso 0.50 1 d PR . . C1 C 0.4963(17) 0.8838(6) 0.3150(10) 0.041(2) Uani 1 1 d U . . C2 C 0.4909(18) 0.8136(7) 0.4119(11) 0.047(3) Uani 1 1 d U . . C3 C 0.4390(18) 0.8464(10) 0.5241(16) 0.074(4) Uani 1 1 d U . . H3C H 0.4920 0.8925 0.5525 0.110 Uiso 1 1 calc R . . H3D H 0.4375 0.8027 0.5863 0.110 Uiso 1 1 calc R . . H3E H 0.3522 0.8663 0.5095 0.110 Uiso 1 1 calc R . . C4 C 0.6334(17) 0.7819(9) 0.4417(17) 0.069(4) Uani 1 1 d U . . H4A H 0.6718 0.7590 0.3675 0.104 Uiso 1 1 calc R . . H4B H 0.6301 0.7389 0.5050 0.104 Uiso 1 1 calc R . . H4C H 0.6847 0.8287 0.4709 0.104 Uiso 1 1 calc R . . C5 C 0.424(2) 0.7428(10) 0.3529(17) 0.075(4) Uani 1 1 d U . . H5A H 0.4694 0.7267 0.2784 0.112 Uiso 1 1 calc R . . H5B H 0.3370 0.7593 0.3321 0.112 Uiso 1 1 calc R . . H5C H 0.4215 0.6956 0.4094 0.112 Uiso 1 1 calc R . . C6 C 0.2358(12) 0.9548(7) -0.0731(13) 0.039(3) Uani 1 1 d . . . H6 H 0.1455 0.9678 -0.0519 0.046 Uiso 1 1 calc R . . C7 C 0.3016(12) 1.0350(7) -0.1000(15) 0.044(3) Uani 1 1 d . . . H7 H 0.3911 1.0226 -0.1247 0.052 Uiso 1 1 calc R . . C8 C 0.2378(14) 1.0825(8) -0.2025(17) 0.052(5) Uani 1 1 d . . . H8A H 0.2859 1.1339 -0.2204 0.062 Uiso 1 1 calc R . . H8B H 0.1502 1.0981 -0.1786 0.062 Uiso 1 1 calc R . . C9 C 0.2349(18) 1.0262(9) -0.316(2) 0.077(6) Uani 1 1 d . . . H9A H 0.1908 1.0554 -0.3836 0.093 Uiso 1 1 calc R . . H9B H 0.3231 1.0145 -0.3428 0.093 Uiso 1 1 calc R . . C10 C 0.1680(17) 0.9462(8) -0.2902(15) 0.060(4) Uani 1 1 d . . . H10A H 0.1698 0.9105 -0.3638 0.071 Uiso 1 1 calc R . . H10B H 0.0781 0.9573 -0.2691 0.071 Uiso 1 1 calc R . . C11 C 0.2347(16) 0.9011(7) -0.1825(16) 0.048(4) Uani 1 1 d . . . H11A H 0.1891 0.8489 -0.1639 0.057 Uiso 1 1 calc R . . H11B H 0.3230 0.8870 -0.2058 0.057 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 0.0418(3) 0.0185(2) 0.0596(3) 0.0010(3) 0.00202(19) 0.0030(2) Cl1 0.0498(15) 0.0218(13) 0.079(2) 0.0015(13) -0.012(3) -0.0075(14) O1 0.061(6) 0.039(5) 0.061(6) 0.011(5) 0.014(5) -0.001(4) N2 0.043(7) 0.021(5) 0.049(8) 0.014(5) 0.008(6) -0.001(4) N3 0.035(6) 0.025(5) 0.058(9) 0.003(6) -0.011(6) -0.003(4) N1 0.050(7) 0.029(5) 0.042(7) 0.004(5) 0.001(6) 0.012(4) O2 0.074(8) 0.073(7) 0.114(11) 0.000(8) 0.024(9) -0.028(6) O3 0.076(8) 0.072(7) 0.100(9) 0.025(8) -0.037(8) -0.018(6) O4 0.085(7) 0.059(6) 0.104(8) 0.036(6) 0.017(8) 0.002(6) O5 0.071(5) 0.057(5) 0.121(7) -0.035(5) -0.014(7) 0.004(5) O6 0.078(9) 0.080(9) 0.073(9) -0.007(8) 0.025(7) -0.009(7) C1 0.065(6) 0.017(4) 0.040(5) -0.002(4) -0.005(8) -0.001(5) C2 0.068(7) 0.027(5) 0.046(6) 0.010(5) -0.004(8) 0.000(6) C3 0.120(11) 0.050(8) 0.051(8) 0.001(7) 0.013(8) -0.003(8) C4 0.098(10) 0.039(7) 0.070(10) 0.001(7) -0.014(9) 0.003(7) C5 0.110(11) 0.054(8) 0.060(9) -0.002(8) 0.013(9) -0.015(8) C6 0.043(7) 0.024(6) 0.049(9) 0.004(5) 0.010(6) -0.005(5) C7 0.046(7) 0.017(5) 0.068(10) 0.013(6) 0.013(7) 0.007(5) C8 0.044(8) 0.029(7) 0.082(15) 0.011(7) -0.010(8) 0.003(5) C9 0.082(11) 0.032(7) 0.118(17) 0.000(9) -0.013(11) 0.010(7) C10 0.091(11) 0.025(6) 0.062(10) -0.004(6) -0.032(10) 0.013(7) C11 0.076(10) 0.016(5) 0.051(11) -0.003(6) -0.006(8) 0.001(5) _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 N3 2.015(13) . ? Pt1 O1 2.019(11) . ? Pt1 N1 2.030(12) 2_675 ? Pt1 N2 2.033(13) . ? Pt1 Pt1 3.0602(12) 2_675 ? Cl1 O3 1.418(15) . ? Cl1 O4 1.420(10) . ? Cl1 O2 1.431(17) . ? Cl1 O5 1.435(10) . ? O1 C1 1.280(18) . ? N2 C6 1.483(19) . ? N2 H2A 0.9200 . ? N2 H2B 0.9200 . ? N3 C7 1.52(2) . ? N3 H3A 0.9200 . ? N3 H3B 0.9200 . ? N1 C1 1.243(18) . ? N1 Pt1 2.030(12) 2_675 ? N1 H1 0.8800 . ? O6 H6A 0.9900 . ? O6 H6B 0.9900 . ? C1 C2 1.552(15) . ? C2 C3 1.44(2) . ? C2 C5 1.49(2) . ? C2 C4 1.62(3) . ? C3 H3C 0.9800 . ? C3 H3D 0.9800 . ? C3 H3E 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C11 1.477(19) . ? C6 C7 1.494(15) . ? C6 H6 1.0000 . ? C7 C8 1.52(2) . ? C7 H7 1.0000 . ? C8 C9 1.54(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.50(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.55(2) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? 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 N3 Pt1 O1 174.8(4) . . ? N3 Pt1 N1 92.5(5) . 2_675 ? O1 Pt1 N1 91.4(4) . 2_675 ? N3 Pt1 N2 83.8(4) . . ? O1 Pt1 N2 92.1(5) . . ? N1 Pt1 N2 174.6(4) 2_675 . ? N3 Pt1 Pt1 106.6(3) . 2_675 ? O1 Pt1 Pt1 77.6(3) . 2_675 ? N1 Pt1 Pt1 78.3(3) 2_675 2_675 ? N2 Pt1 Pt1 106.5(3) . 2_675 ? O3 Cl1 O4 107.9(8) . . ? O3 Cl1 O2 111.4(7) . . ? O4 Cl1 O2 109.1(9) . . ? O3 Cl1 O5 110.6(9) . . ? O4 Cl1 O5 106.5(7) . . ? O2 Cl1 O5 111.1(9) . . ? C1 O1 Pt1 129.8(9) . . ? C6 N2 Pt1 109.8(7) . . ? C6 N2 H2A 109.7 . . ? Pt1 N2 H2A 109.7 . . ? C6 N2 H2B 109.7 . . ? Pt1 N2 H2B 109.7 . . ? H2A N2 H2B 108.2 . . ? C7 N3 Pt1 108.6(7) . . ? C7 N3 H3A 110.0 . . ? Pt1 N3 H3A 110.0 . . ? C7 N3 H3B 110.0 . . ? Pt1 N3 H3B 110.0 . . ? H3A N3 H3B 108.4 . . ? C1 N1 Pt1 129.1(9) . 2_675 ? C1 N1 H1 115.4 . . ? Pt1 N1 H1 115.4 2_675 . ? H6A O6 H6B 104.4 . . ? N1 C1 O1 124.0(10) . . ? N1 C1 C2 118.6(14) . . ? O1 C1 C2 117.4(14) . . ? C3 C2 C5 118.1(15) . . ? C3 C2 C1 109.1(11) . . ? C5 C2 C1 106.2(12) . . ? C3 C2 C4 107.1(13) . . ? C5 C2 C4 106.5(12) . . ? C1 C2 C4 109.5(14) . . ? C2 C3 H3C 109.5 . . ? C2 C3 H3D 109.5 . . ? H3C C3 H3D 109.5 . . ? C2 C3 H3E 109.5 . . ? H3C C3 H3E 109.5 . . ? H3D C3 H3E 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C11 C6 N2 113.4(11) . . ? C11 C6 C7 110.5(12) . . ? N2 C6 C7 109.8(11) . . ? C11 C6 H6 107.6 . . ? N2 C6 H6 107.6 . . ? C7 C6 H6 107.6 . . ? C6 C7 C8 112.3(12) . . ? C6 C7 N3 105.8(11) . . ? C8 C7 N3 113.2(10) . . ? C6 C7 H7 108.5 . . ? C8 C7 H7 108.5 . . ? N3 C7 H7 108.5 . . ? C7 C8 C9 108.0(11) . . ? C7 C8 H8A 110.1 . . ? C9 C8 H8A 110.1 . . ? C7 C8 H8B 110.1 . . ? C9 C8 H8B 110.1 . . ? H8A C8 H8B 108.4 . . ? C10 C9 C8 111.4(16) . . ? C10 C9 H9A 109.4 . . ? C8 C9 H9A 109.4 . . ? C10 C9 H9B 109.4 . . ? C8 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? C9 C10 C11 109.6(14) . . ? C9 C10 H10A 109.7 . . ? C11 C10 H10A 109.7 . . ? C9 C10 H10B 109.7 . . ? C11 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? C6 C11 C10 110.2(10) . . ? C6 C11 H11A 109.6 . . ? C10 C11 H11A 109.6 . . ? C6 C11 H11B 109.6 . . ? C10 C11 H11B 109.6 . . ? H11A C11 H11B 108.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Pt1 O1 C1 -86.2(12) 2_675 . . . ? N2 Pt1 O1 C1 97.9(12) . . . . ? Pt1 Pt1 O1 C1 -8.5(11) 2_675 . . . ? N3 Pt1 N2 C6 -6.5(8) . . . . ? O1 Pt1 N2 C6 170.3(8) . . . . ? Pt1 Pt1 N2 C6 -112.0(8) 2_675 . . . ? N1 Pt1 N3 C7 162.8(8) 2_675 . . . ? N2 Pt1 N3 C7 -21.1(7) . . . . ? Pt1 Pt1 N3 C7 84.3(8) 2_675 . . . ? Pt1 N1 C1 O1 7.4(18) 2_675 . . . ? Pt1 N1 C1 C2 -173.8(9) 2_675 . . . ? Pt1 O1 C1 N1 4.6(18) . . . . ? Pt1 O1 C1 C2 -174.2(8) . . . . ? N1 C1 C2 C3 120.9(16) . . . . ? O1 C1 C2 C3 -60.2(17) . . . . ? N1 C1 C2 C5 -110.7(16) . . . . ? O1 C1 C2 C5 68.2(16) . . . . ? N1 C1 C2 C4 3.9(15) . . . . ? O1 C1 C2 C4 -177.2(11) . . . . ? Pt1 N2 C6 C11 157.8(10) . . . . ? Pt1 N2 C6 C7 33.7(12) . . . . ? C11 C6 C7 C8 59.4(15) . . . . ? N2 C6 C7 C8 -174.7(12) . . . . ? C11 C6 C7 N3 -176.6(11) . . . . ? N2 C6 C7 N3 -50.7(12) . . . . ? Pt1 N3 C7 C6 44.1(10) . . . . ? Pt1 N3 C7 C8 167.5(9) . . . . ? C6 C7 C8 C9 -57.2(16) . . . . ? N3 C7 C8 C9 -177.0(12) . . . . ? C7 C8 C9 C10 57.0(16) . . . . ? C8 C9 C10 C11 -57.7(16) . . . . ? N2 C6 C11 C10 178.3(12) . . . . ? C7 C6 C11 C10 -57.9(17) . . . . ? C9 C10 C11 C6 57.8(17) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.568 _refine_diff_density_min -2.145 _refine_diff_density_rms 0.216 #===END data_pt2ac _database_code_depnum_ccdc_archive 'CCDC 290079' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H50 N12 O21 Pt2' _chemical_formula_weight 1208.92 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' 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.795(7) _cell_length_b 13.271(7) _cell_length_c 14.866(8) _cell_angle_alpha 94.157(6) _cell_angle_beta 94.387(6) _cell_angle_gamma 118.081(7) _cell_volume 2203(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.822 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1180 _exptl_absorpt_coefficient_mu 6.426 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4080 _exptl_absorpt_correction_T_max 0.6619 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 6266 _diffrn_reflns_av_R_equivalents 0.0912 _diffrn_reflns_av_sigmaI/netI 0.0969 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 4.57 _diffrn_reflns_theta_max 22.00 _reflns_number_total 4829 _reflns_number_gt 3245 _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^)+(0.1037P)^2^+6.5525P] 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 4829 _refine_ls_number_parameters 572 _refine_ls_number_restraints 2043 _refine_ls_R_factor_all 0.1011 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.1858 _refine_ls_wR_factor_gt 0.1622 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 0.927 _refine_ls_shift/su_max 0.000 _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 C1 C 0.214(2) -0.1770(19) 0.1266(14) 0.069(3) Uani 1 1 d U B . C2 C 0.209(2) -0.263(2) 0.0504(14) 0.077(4) Uani 1 1 d U . . C3 C 0.327(2) -0.236(2) 0.0232(17) 0.110(7) Uani 1 1 d U . . H3A H 0.3726 -0.2486 0.0710 0.165 Uiso 1 1 calc R . . H3B H 0.3676 -0.1573 0.0121 0.165 Uiso 1 1 calc R . . H3C H 0.3164 -0.2852 -0.0312 0.165 Uiso 1 1 calc R . . C4 C 0.163(3) -0.378(2) 0.0860(17) 0.108(7) Uani 1 1 d U . . H4A H 0.1571 -0.4346 0.0392 0.162 Uiso 1 1 calc R . . H4B H 0.0854 -0.4003 0.1044 0.162 Uiso 1 1 calc R . . H4C H 0.2167 -0.3719 0.1373 0.162 Uiso 1 1 calc R . . C5 C 0.124(2) -0.270(2) -0.0313(15) 0.101(6) Uani 1 1 d U . . H5A H 0.1605 -0.1999 -0.0588 0.151 Uiso 1 1 calc R . . H5B H 0.0505 -0.2797 -0.0112 0.151 Uiso 1 1 calc R . . H5C H 0.1079 -0.3338 -0.0750 0.151 Uiso 1 1 calc R . . C6 C 0.122(2) -0.2061(19) 0.3546(14) 0.068(4) Uani 1 1 d U B . C7 C 0.0702(18) -0.3048(17) 0.4079(12) 0.074(4) Uani 1 1 d DU . . C11 C 0.486(5) 0.214(4) 0.374(3) 0.085(4) Uani 0.50(3) 1 d PDU A 1 H11 H 0.5517 0.1968 0.3833 0.101 Uiso 0.50(3) 1 calc PR A 1 C12 C 0.479(4) 0.229(2) 0.275(2) 0.086(4) Uani 0.50(3) 1 d PDU A 1 H12 H 0.4073 0.2377 0.2651 0.103 Uiso 0.50(3) 1 calc PR A 1 C13 C 0.572(4) 0.342(2) 0.265(2) 0.091(4) Uani 0.50(3) 1 d PRDU A 1 H13A H 0.5517 0.3559 0.2043 0.109 Uiso 0.50(3) 1 calc PR A 1 H13B H 0.6432 0.3341 0.2622 0.109 Uiso 0.50(3) 1 calc PR A 1 C14 C 0.611(5) 0.451(3) 0.323(2) 0.097(5) Uani 0.50(3) 1 d PDU A 1 H14A H 0.5573 0.4816 0.3079 0.116 Uiso 0.50(3) 1 calc PR A 1 H14B H 0.6904 0.5067 0.3108 0.116 Uiso 0.50(3) 1 calc PR A 1 C15 C 0.614(4) 0.435(4) 0.421(2) 0.089(5) Uani 0.50(3) 1 d PDU A 1 H15A H 0.6924 0.4441 0.4414 0.107 Uiso 0.50(3) 1 calc PR A 1 H15B H 0.6067 0.4961 0.4538 0.107 Uiso 0.50(3) 1 calc PR A 1 C16 C 0.530(4) 0.332(4) 0.445(2) 0.088(4) Uani 0.50(3) 1 d PRDU A 1 H16A H 0.4606 0.3403 0.4550 0.106 Uiso 0.50(3) 1 calc PR A 1 H16B H 0.5620 0.3213 0.5023 0.106 Uiso 0.50(3) 1 calc PR A 1 C17 C 0.128(3) 0.159(2) 0.297(2) 0.079(4) Uani 0.56(2) 1 d PDU B 1 H17 H 0.2105 0.1897 0.3251 0.094 Uiso 0.56(2) 1 calc PR B 1 C18 C 0.151(3) 0.179(2) 0.205(2) 0.083(3) Uani 0.56(2) 1 d PRDU B 1 H18 H 0.0650 0.1409 0.1841 0.100 Uiso 0.56(2) 1 calc PR B 1 C19 C 0.170(2) 0.2774(17) 0.1579(13) 0.087(4) Uani 1 1 d DU . . H19A H 0.1232 0.2514 0.0983 0.104 Uiso 1 1 calc R B 1 H19B H 0.2536 0.3214 0.1499 0.104 Uiso 1 1 calc R B 1 C20 C 0.133(3) 0.351(2) 0.213(2) 0.090(4) Uani 0.56(2) 1 d PDU B 1 H20A H 0.0524 0.3308 0.1876 0.108 Uiso 0.56(2) 1 calc PR B 1 H20B H 0.1837 0.4298 0.2029 0.108 Uiso 0.56(2) 1 calc PR B 1 C21 C 0.132(3) 0.352(2) 0.322(2) 0.087(5) Uani 0.56(2) 1 d PRDU B 1 H21A H 0.2105 0.4069 0.3523 0.104 Uiso 0.56(2) 1 calc PR B 1 H21B H 0.0757 0.3768 0.3405 0.104 Uiso 0.56(2) 1 calc PR B 1 C22 C 0.098(4) 0.236(3) 0.351(3) 0.081(5) Uani 0.56(2) 1 d PDU B 1 H22A H 0.1353 0.2479 0.4129 0.098 Uiso 0.56(2) 1 calc PR B 1 H22B H 0.0123 0.1969 0.3523 0.098 Uiso 0.56(2) 1 calc PR B 1 C11' C 0.442(4) 0.227(2) 0.386(3) 0.086(4) Uani 0.50(3) 1 d PDU A 2 H11' H 0.3787 0.2424 0.3606 0.103 Uiso 0.50(3) 1 calc PR A 2 C12' C 0.499(4) 0.215(3) 0.303(2) 0.088(4) Uani 0.50(3) 1 d PDU A 2 H12' H 0.5573 0.1961 0.3326 0.106 Uiso 0.50(3) 1 calc PR A 2 C13' C 0.584(5) 0.334(3) 0.282(3) 0.091(4) Uani 0.50(3) 1 d PDU A 2 H13C H 0.5430 0.3555 0.2355 0.109 Uiso 0.50(3) 1 calc PR A 2 H13D H 0.6504 0.3310 0.2564 0.109 Uiso 0.50(3) 1 calc PR A 2 C14' C 0.631(4) 0.424(4) 0.364(3) 0.087(5) Uani 0.50(3) 1 d PDU A 2 H14C H 0.7000 0.4222 0.3944 0.104 Uiso 0.50(3) 1 calc PR A 2 H14D H 0.6609 0.4983 0.3412 0.104 Uiso 0.50(3) 1 calc PR A 2 C15' C 0.553(5) 0.422(4) 0.435(3) 0.091(5) Uani 0.50(3) 1 d PDU A 2 H15C H 0.6014 0.4793 0.4859 0.109 Uiso 0.50(3) 1 calc PR A 2 H15D H 0.4936 0.4410 0.4097 0.109 Uiso 0.50(3) 1 calc PR A 2 C16' C 0.492(4) 0.306(4) 0.468(3) 0.088(4) Uani 0.50(3) 1 d PDU A 2 H16C H 0.5488 0.2915 0.5037 0.106 Uiso 0.50(3) 1 calc PR A 2 H16D H 0.4301 0.3007 0.5037 0.106 Uiso 0.50(3) 1 calc PR A 2 C17' C 0.051(5) 0.120(4) 0.267(3) 0.081(4) Uani 0.44(2) 1 d PDU B 2 H17' H -0.0307 0.0754 0.2356 0.097 Uiso 0.44(2) 1 calc PR B 2 C18' C 0.135(5) 0.165(5) 0.196(4) 0.083(3) Uani 0.44(2) 1 d PDU B 2 H18' H 0.2066 0.1982 0.2407 0.100 Uiso 0.44(2) 1 calc PR B 2 C20' C 0.175(4) 0.373(3) 0.219(3) 0.090(4) Uani 0.44(2) 1 d PDU B 2 H20C H 0.1703 0.4307 0.1853 0.108 Uiso 0.44(2) 1 calc PR B 2 H20D H 0.2472 0.4090 0.2621 0.108 Uiso 0.44(2) 1 calc PR B 2 C21' C 0.064(4) 0.314(4) 0.269(3) 0.082(5) Uani 0.44(2) 1 d PDU B 2 H21C H 0.0592 0.3723 0.3084 0.098 Uiso 0.44(2) 1 calc PR B 2 H21D H -0.0058 0.2791 0.2240 0.098 Uiso 0.44(2) 1 calc PR B 2 C22' C 0.060(6) 0.222(4) 0.325(3) 0.081(5) Uani 0.44(2) 1 d PDU B 2 H22C H -0.0082 0.1971 0.3589 0.097 Uiso 0.44(2) 1 calc PR B 2 H22D H 0.1316 0.2543 0.3690 0.097 Uiso 0.44(2) 1 calc PR B 2 N1 N 0.3043(16) -0.1323(15) 0.1857(11) 0.069(3) Uani 1 1 d U . . H1 H 0.3589 -0.1518 0.1801 0.082 Uiso 1 1 calc R . . O2 O 0.2395(15) -0.1436(13) 0.3635(9) 0.079(3) Uani 1 1 d U . . N3 N 0.3764(16) 0.1045(14) 0.4002(11) 0.075(3) Uani 1 1 d DU . . H3D H 0.3157 0.1188 0.4095 0.090 Uiso 1 1 calc R A 1 H3E H 0.3976 0.0820 0.4510 0.090 Uiso 1 1 calc R A 1 N4 N 0.4410(17) 0.1158(15) 0.2271(12) 0.088(3) Uani 1 1 d DU . . H4D H 0.5060 0.1081 0.2189 0.105 Uiso 1 1 calc R A 1 H4E H 0.4035 0.1103 0.1718 0.105 Uiso 1 1 calc R A 1 N5 N 0.0814(15) 0.0409(13) 0.3179(11) 0.070(3) Uani 1 1 d DU . . H5D H 0.0018 0.0086 0.3175 0.084 Uiso 1 1 calc R B 1 H5E H 0.1136 0.0411 0.3739 0.084 Uiso 1 1 calc R B 1 N6 N 0.1641(16) 0.0832(15) 0.1506(11) 0.071(3) Uani 1 1 d U . . H6A H 0.2398 0.1103 0.1384 0.085 Uiso 1 1 calc R B 1 H6B H 0.1157 0.0593 0.0976 0.085 Uiso 1 1 calc R B 1 N7 N 0.531(2) -0.0485(18) 0.3923(14) 0.087(4) Uani 1 1 d U A . N8 N -0.100(2) -0.140(2) 0.0947(16) 0.095(5) Uani 1 1 d U B . N9 N 0.432(3) 0.671(3) 0.282(2) 0.151(7) Uani 1 1 d U . . N10 N 0.376(2) 0.157(3) 0.0178(19) 0.113(6) Uani 1 1 d U . . N11 N 0.1599(19) 0.080(2) 0.5483(14) 0.073(4) Uani 1 1 d U . . N12 N 0.702(3) 0.089(3) 0.2018(19) 0.114(6) Uani 1 1 d U . . O1 O 0.1289(14) -0.1550(12) 0.1263(9) 0.073(3) Uani 1 1 d U . . N2 N 0.0617(15) -0.1807(14) 0.3017(10) 0.062(3) Uani 1 1 d U . . H2 H -0.0144 -0.2238 0.2967 0.074 Uiso 1 1 calc R B . O3 O 0.5009(13) -0.0058(13) 0.3262(10) 0.081(3) Uani 1 1 d U . . O4 O 0.4613(16) -0.1053(18) 0.4388(12) 0.116(5) Uani 1 1 d U . . O5 O 0.6264(18) -0.0417(18) 0.3999(12) 0.117(5) Uani 1 1 d U . . O6 O -0.0666(13) -0.1247(13) 0.1840(10) 0.081(3) Uani 1 1 d U . . O7 O -0.0602(18) -0.0942(18) 0.0448(12) 0.116(6) Uani 1 1 d U . . O8 O -0.205(2) -0.214(3) 0.0771(17) 0.201(10) Uani 1 1 d U . . O9 O 0.483(2) 0.6155(19) 0.3075(16) 0.144(6) Uani 1 1 d U . . O10 O 0.488(3) 0.749(2) 0.2392(19) 0.188(9) Uani 1 1 d U . . O11 O 0.330(3) 0.647(2) 0.3013(17) 0.177(8) Uani 1 1 d U . . O12 O 0.4002(18) 0.2385(19) 0.0698(13) 0.122(5) Uani 1 1 d U . . O13 O 0.377(2) 0.164(2) -0.0730(16) 0.170(8) Uani 1 1 d U . . O14 O 0.3280(19) 0.0553(19) 0.0294(12) 0.121(5) Uani 1 1 d U . . O15 O 0.2242(16) 0.1629(15) 0.5109(10) 0.092(4) Uani 1 1 d U . . O16 O 0.1449(15) 0.0951(15) 0.6286(11) 0.098(5) Uani 1 1 d U . . O17 O 0.1158(16) -0.0145(16) 0.5078(11) 0.094(4) Uani 1 1 d U . . O18 O 0.609(2) 0.036(2) 0.1536(14) 0.144(7) Uani 1 1 d U . . O19 O 0.742(2) 0.169(2) 0.2516(17) 0.152(7) Uani 1 1 d U . . O20 O 0.769(2) 0.036(2) 0.1871(17) 0.154(7) Uani 1 1 d U . . O21 O 0.692(2) 0.724(2) 0.2602(15) 0.170(7) Uani 1 1 d U . . H3 H 0.6640 0.7585 0.2290 0.204 Uiso 1 1 d R . . H4 H 0.6317 0.6725 0.2808 0.204 Uiso 1 1 d R . . Pt1 Pt 0.32922(6) -0.01666(6) 0.29353(5) 0.0487(3) Uani 1 1 d . A . Pt2 Pt 0.11904(6) -0.05329(6) 0.22740(4) 0.0471(3) Uani 1 1 d . A . C10 C -0.0520(19) -0.324(2) 0.4320(17) 0.117(4) Uani 1 1 d DU . . H10A H -0.1070 -0.3468 0.3774 0.175 Uiso 1 1 calc R . . H10B H -0.0435 -0.2533 0.4623 0.175 Uiso 1 1 calc R . . H10C H -0.0817 -0.3827 0.4715 0.175 Uiso 1 1 calc R . . C8 C 0.148(2) -0.278(2) 0.4980(14) 0.117(4) Uani 1 1 d DU . . H8A H 0.1002 -0.2928 0.5468 0.175 Uiso 1 1 calc R . . H8B H 0.2088 -0.1989 0.5061 0.175 Uiso 1 1 calc R . . H8C H 0.1858 -0.3263 0.4979 0.175 Uiso 1 1 calc R . . C9 C 0.055(2) -0.4081(19) 0.3454(15) 0.117(4) Uani 1 1 d DU . . H9A H -0.0142 -0.4344 0.3017 0.175 Uiso 1 1 calc R . . H9B H 0.0461 -0.4688 0.3808 0.175 Uiso 1 1 calc R . . H9C H 0.1245 -0.3861 0.3144 0.175 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 C1 0.096(6) 0.080(6) 0.057(6) 0.024(5) 0.016(6) 0.059(5) C2 0.106(9) 0.088(8) 0.055(8) 0.017(7) 0.016(8) 0.058(7) C3 0.122(13) 0.118(12) 0.084(12) -0.015(11) 0.016(11) 0.055(11) C4 0.144(13) 0.093(12) 0.084(12) 0.018(10) 0.007(11) 0.055(11) C5 0.139(13) 0.101(12) 0.062(11) -0.006(10) 0.012(11) 0.059(10) C6 0.091(7) 0.079(6) 0.061(6) 0.023(6) 0.020(6) 0.059(5) C7 0.093(8) 0.082(8) 0.060(8) 0.027(7) 0.030(7) 0.048(7) C11 0.099(6) 0.103(6) 0.074(6) 0.035(6) 0.014(6) 0.062(6) C12 0.099(6) 0.104(6) 0.075(6) 0.035(6) 0.014(6) 0.061(6) C13 0.102(5) 0.107(5) 0.076(5) 0.035(5) 0.015(5) 0.056(5) C14 0.107(7) 0.110(7) 0.083(7) 0.033(6) 0.018(6) 0.056(6) C15 0.100(7) 0.106(7) 0.077(7) 0.032(7) 0.016(7) 0.058(7) C16 0.100(6) 0.105(5) 0.076(5) 0.032(5) 0.018(5) 0.059(5) C17 0.097(6) 0.094(6) 0.071(6) 0.027(6) 0.011(6) 0.065(5) C18 0.102(5) 0.094(5) 0.070(5) 0.026(4) 0.006(5) 0.058(4) C19 0.102(6) 0.096(6) 0.076(6) 0.028(6) 0.007(6) 0.057(6) C20 0.106(6) 0.100(5) 0.077(5) 0.025(5) 0.008(5) 0.059(5) C21 0.104(7) 0.098(7) 0.075(7) 0.022(7) 0.007(7) 0.060(6) C22 0.101(7) 0.094(7) 0.071(7) 0.025(6) 0.007(6) 0.063(6) C11' 0.100(6) 0.104(6) 0.073(6) 0.033(6) 0.014(6) 0.061(6) C12' 0.101(6) 0.105(6) 0.076(6) 0.034(6) 0.016(6) 0.059(6) C13' 0.102(5) 0.107(5) 0.076(5) 0.035(5) 0.015(5) 0.056(5) C14' 0.099(7) 0.103(7) 0.078(7) 0.034(7) 0.015(7) 0.061(6) C15' 0.103(7) 0.107(7) 0.078(7) 0.033(6) 0.017(6) 0.058(6) C16' 0.100(6) 0.105(5) 0.076(5) 0.032(5) 0.018(5) 0.059(5) C17' 0.099(6) 0.095(6) 0.070(6) 0.025(6) 0.006(6) 0.061(6) C18' 0.102(5) 0.094(5) 0.070(5) 0.026(4) 0.006(5) 0.058(4) C20' 0.106(6) 0.100(5) 0.077(5) 0.025(5) 0.008(5) 0.059(5) C21' 0.100(7) 0.095(7) 0.073(7) 0.023(7) 0.006(7) 0.065(7) C22' 0.100(7) 0.095(6) 0.070(6) 0.027(6) 0.009(6) 0.063(6) N1 0.093(6) 0.090(6) 0.056(5) 0.025(5) 0.016(5) 0.068(5) O2 0.097(6) 0.088(5) 0.067(5) 0.034(5) 0.015(5) 0.053(5) N3 0.093(5) 0.095(5) 0.065(5) 0.039(5) 0.015(5) 0.064(4) N4 0.100(5) 0.108(5) 0.068(5) 0.030(5) 0.019(5) 0.056(5) N5 0.091(5) 0.087(5) 0.064(5) 0.030(5) 0.013(5) 0.066(4) N6 0.088(5) 0.094(5) 0.061(5) 0.029(5) 0.005(5) 0.065(4) N7 0.097(7) 0.111(7) 0.074(7) 0.047(6) 0.012(7) 0.062(6) N8 0.098(8) 0.106(8) 0.067(7) 0.011(7) 0.005(7) 0.038(7) N9 0.143(12) 0.157(12) 0.120(11) 0.018(10) 0.027(11) 0.043(11) N10 0.118(10) 0.128(10) 0.089(10) 0.023(10) 0.023(9) 0.053(9) N11 0.080(9) 0.099(9) 0.071(9) 0.030(8) 0.022(8) 0.064(7) N12 0.115(9) 0.131(9) 0.082(9) 0.032(8) 0.021(8) 0.042(8) O1 0.095(6) 0.087(5) 0.058(5) 0.012(5) 0.014(5) 0.059(5) N2 0.079(6) 0.077(5) 0.058(5) 0.021(5) 0.017(5) 0.058(5) O3 0.094(5) 0.106(5) 0.072(5) 0.034(5) 0.012(5) 0.066(5) O4 0.097(10) 0.169(11) 0.083(9) 0.061(9) 0.008(8) 0.059(9) O5 0.111(10) 0.174(11) 0.105(10) 0.052(9) 0.013(9) 0.094(9) O6 0.092(6) 0.097(6) 0.069(5) 0.030(5) 0.002(5) 0.056(5) O7 0.119(11) 0.134(11) 0.061(9) 0.025(9) -0.017(9) 0.036(9) O8 0.141(15) 0.216(17) 0.120(14) 0.009(14) 0.004(13) -0.013(14) O9 0.165(12) 0.145(11) 0.143(12) 0.034(10) 0.012(10) 0.090(10) O10 0.188(16) 0.175(15) 0.147(15) 0.048(13) 0.045(14) 0.034(14) O11 0.164(13) 0.168(13) 0.134(12) 0.007(11) 0.033(12) 0.026(12) O12 0.127(9) 0.130(9) 0.091(9) 0.029(8) 0.020(8) 0.046(8) O13 0.212(17) 0.170(15) 0.115(14) 0.062(12) 0.052(13) 0.072(13) O14 0.136(10) 0.134(10) 0.085(9) 0.015(9) 0.031(8) 0.057(9) O15 0.111(9) 0.114(8) 0.068(8) 0.031(7) 0.025(7) 0.063(7) O16 0.092(11) 0.135(12) 0.060(9) 0.000(9) 0.020(9) 0.048(9) O17 0.105(8) 0.107(8) 0.071(8) 0.019(7) 0.011(7) 0.050(7) O18 0.137(12) 0.174(12) 0.079(10) 0.032(10) 0.024(10) 0.036(11) O19 0.147(11) 0.154(11) 0.120(11) 0.027(10) 0.027(10) 0.041(10) O20 0.148(14) 0.167(14) 0.146(14) 0.022(12) 0.021(12) 0.075(12) O21 0.154(11) 0.166(11) 0.132(11) 0.005(10) 0.039(10) 0.029(10) Pt1 0.0510(6) 0.0674(6) 0.0369(5) 0.0214(4) 0.0104(4) 0.0331(5) Pt2 0.0538(6) 0.0616(6) 0.0358(4) 0.0131(4) 0.0047(4) 0.0348(4) C10 0.124(8) 0.114(7) 0.095(7) 0.036(6) 0.031(7) 0.038(7) C8 0.124(8) 0.114(7) 0.095(7) 0.036(6) 0.031(7) 0.038(7) C9 0.124(8) 0.114(7) 0.095(7) 0.036(6) 0.031(7) 0.038(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 C1 O1 1.25(2) . ? C1 N1 1.26(2) . ? C1 C2 1.53(3) . ? C2 C3 1.47(3) . ? C2 C4 1.50(3) . ? C2 C5 1.53(3) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 N2 1.23(2) . ? C6 O2 1.32(2) . ? C6 C7 1.48(3) . ? C7 C8 1.521(15) . ? C7 C9 1.524(15) . ? C7 C10 1.538(15) . ? C11 C12 1.502(18) . ? C11 N3 1.57(5) . ? C11 C16 1.65(6) . ? C11 H11 0.9800 . ? C12 C13 1.4330 . ? C12 N4 1.456(17) . ? C12 H12 0.9800 . ? C13 C14 1.469(18) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.489(18) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.3695 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.4388 . ? C17 C22 1.45(5) . ? C17 N5 1.463(16) . ? C17 H17 0.9800 . ? C18 C19 1.456(16) . ? C18 N6 1.54(4) . ? C18 H18 0.9800 . ? C19 C20' 1.483(18) . ? C19 C20 1.498(17) . ? C19 C18' 1.51(5) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.6126 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.493(17) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C11' C16' 1.43(6) . ? C11' N3 1.481(18) . ? C11' C12' 1.504(18) . ? C11' H11' 0.9800 . ? C12' C13' 1.509(18) . ? C12' N4 1.520(18) . ? C12' H12' 0.9800 . ? C13' C14' 1.514(18) . ? C13' H13C 0.9700 . ? C13' H13D 0.9700 . ? C14' C15' 1.501(18) . ? C14' H14C 0.9700 . ? C14' H14D 0.9700 . ? C15' C16' 1.495(13) . ? C15' H15C 0.9700 . ? C15' H15D 0.9700 . ? C16' H16C 0.9700 . ? C16' H16D 0.9700 . ? C17' C18' 1.509(18) . ? C17' C22' 1.510(18) . ? C17' N5 1.513(17) . ? C17' H17' 0.9800 . ? C18' N6 1.45(6) . ? C18' H18' 0.9800 . ? C20' C21' 1.531(18) . ? C20' H20C 0.9700 . ? C20' H20D 0.9700 . ? C21' C22' 1.507(18) . ? C21' H21C 0.9700 . ? C21' H21D 0.9700 . ? C22' H22C 0.9700 . ? C22' H22D 0.9700 . ? N1 Pt1 2.032(16) . ? N1 H1 0.8600 . ? O2 Pt1 1.964(14) . ? N3 Pt1 2.009(17) . ? N3 H3D 0.9000 . ? N3 H3E 0.9000 . ? N4 Pt1 2.052(18) . ? N4 H4D 0.9000 . ? N4 H4E 0.9000 . ? N5 Pt2 2.006(15) . ? N5 H5D 0.9000 . ? N5 H5E 0.9000 . ? N6 Pt2 2.082(15) . ? N6 H6A 0.9000 . ? N6 H6B 0.9000 . ? N7 O5 1.17(2) . ? N7 O4 1.18(2) . ? N7 O3 1.29(2) . ? N8 O7 1.00(2) . ? N8 O8 1.23(3) . ? N8 O6 1.33(2) . ? N9 O10 1.20(3) . ? N9 O9 1.25(4) . ? N9 O11 1.26(4) . ? N10 O12 1.18(3) . ? N10 O14 1.22(3) . ? N10 O13 1.36(3) . ? N11 O17 1.20(2) . ? N11 O15 1.23(2) . ? N11 O16 1.24(2) . ? N12 O19 1.12(3) . ? N12 O18 1.19(3) . ? N12 O20 1.36(3) . ? O1 Pt2 1.997(13) . ? N2 Pt2 1.960(15) . ? N2 H2 0.8600 . ? O3 Pt1 2.147(14) . ? O6 Pt2 2.124(15) . ? O21 H4 0.8500 . ? O21 H3 0.8500 . ? O21 H3 0.8500 . ? O21 H4 0.8500 . ? Pt1 Pt2 2.5942(17) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? 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 O1 C1 N1 124(2) . . ? O1 C1 C2 118(2) . . ? N1 C1 C2 117(2) . . ? C3 C2 C4 106(2) . . ? C3 C2 C1 113(2) . . ? C4 C2 C1 107.4(18) . . ? C3 C2 C5 111(2) . . ? C4 C2 C5 111(2) . . ? C1 C2 C5 108.7(18) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 O2 119(2) . . ? N2 C6 C7 124(2) . . ? O2 C6 C7 117.8(17) . . ? C6 C7 C8 110.2(19) . . ? C6 C7 C9 105.3(16) . . ? C8 C7 C9 115.4(17) . . ? C6 C7 C10 109.7(17) . . ? C8 C7 C10 106.1(16) . . ? C9 C7 C10 110.2(16) . . ? C12 C11 N3 115(4) . . ? C12 C11 C16 115(3) . . ? N3 C11 C16 115(3) . . ? C12 C11 H11 103.2 . . ? N3 C11 H11 103.2 . . ? C16 C11 H11 103.2 . . ? C13 C12 N4 132.9(19) . . ? C13 C12 C11 108(2) . . ? N4 C12 C11 105(3) . . ? C13 C12 H12 102.3 . . ? N4 C12 H12 102.3 . . ? C11 C12 H12 102.3 . . ? C12 C13 C14 129(2) . . ? C12 C13 H13A 105.1 . . ? C14 C13 H13A 105.1 . . ? C12 C13 H13B 105.1 . . ? C14 C13 H13B 105.1 . . ? H13A C13 H13B 105.9 . . ? C13 C14 C15 111(3) . . ? C13 C14 H14A 109.5 . . ? C15 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 108.0 . . ? C16 C15 C14 118(2) . . ? C16 C15 H15A 107.8 . . ? C14 C15 H15A 107.8 . . ? C16 C15 H15B 107.8 . . ? C14 C15 H15B 107.8 . . ? H15A C15 H15B 107.1 . . ? C15 C16 C11 119(2) . . ? C15 C16 H16A 107.7 . . ? C11 C16 H16A 107.7 . . ? C15 C16 H16B 107.7 . . ? C11 C16 H16B 107.7 . . ? H16A C16 H16B 107.1 . . ? C18 C17 C22 118.7(16) . . ? C18 C17 N5 116.6(16) . . ? C22 C17 N5 119(3) . . ? C18 C17 H17 98.2 . . ? C22 C17 H17 98.2 . . ? N5 C17 H17 98.2 . . ? C17 C18 C19 130.1(16) . . ? C17 C18 N6 114.2(11) . . ? C19 C18 N6 116(2) . . ? C17 C18 H18 91.0 . . ? C19 C18 H18 91.0 . . ? N6 C18 H18 91.0 . . ? C18 C19 C20' 112(3) . . ? C18 C19 C20 108(2) . . ? C20' C19 C18' 117(3) . . ? C20 C19 C18' 111(3) . . ? C18 C19 H19A 110.0 . . ? C20' C19 H19A 122.2 . . ? C20 C19 H19A 110.0 . . ? C18' C19 H19A 101.8 . . ? C18 C19 H19B 110.0 . . ? C20' C19 H19B 92.5 . . ? C20 C19 H19B 110.0 . . ? C18' C19 H19B 115.5 . . ? H19A C19 H19B 108.4 . . ? C19 C20 C21 122.7(14) . . ? C19 C20 H20A 106.7 . . ? C21 C20 H20A 106.7 . . ? C19 C20 H20B 106.7 . . ? C21 C20 H20B 106.7 . . ? H20A C20 H20B 106.6 . . ? C22 C21 C20 112(2) . . ? C22 C21 H21A 109.2 . . ? C20 C21 H21A 109.2 . . ? C22 C21 H21B 109.2 . . ? C20 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? C17 C22 C21 118(3) . . ? C17 C22 H22A 107.7 . . ? C21 C22 H22A 107.7 . . ? C17 C22 H22B 107.7 . . ? C21 C22 H22B 107.7 . . ? H22A C22 H22B 107.1 . . ? C16' C11' N3 115(3) . . ? C16' C11' C12' 131(4) . . ? N3 C11' C12' 99(3) . . ? C16' C11' H11' 103.0 . . ? N3 C11' H11' 103.0 . . ? C12' C11' H11' 103.0 . . ? C11' C12' C13' 109(3) . . ? C11' C12' N4 125(3) . . ? C13' C12' N4 119(3) . . ? C11' C12' H12' 98.6 . . ? C13' C12' H12' 98.6 . . ? N4 C12' H12' 98.6 . . ? C12' C13' C14' 113(4) . . ? C12' C13' H13C 109.0 . . ? C14' C13' H13C 109.0 . . ? C12' C13' H13D 109.0 . . ? C14' C13' H13D 109.0 . . ? H13C C13' H13D 107.8 . . ? C15' C14' C13' 121(5) . . ? C15' C14' H14C 107.1 . . ? C13' C14' H14C 107.1 . . ? C15' C14' H14D 107.1 . . ? C13' C14' H14D 107.1 . . ? H14C C14' H14D 106.8 . . ? C16' C15' C14' 112(4) . . ? C16' C15' H15C 109.3 . . ? C14' C15' H15C 109.3 . . ? C16' C15' H15D 109.3 . . ? C14' C15' H15D 109.3 . . ? H15C C15' H15D 107.9 . . ? C11' C16' C15' 104(4) . . ? C11' C16' H16C 110.9 . . ? C15' C16' H16C 110.9 . . ? C11' C16' H16D 110.9 . . ? C15' C16' H16D 110.9 . . ? H16C C16' H16D 108.9 . . ? C18' C17' C22' 108(5) . . ? C18' C17' N5 109(3) . . ? C22' C17' N5 114(3) . . ? C18' C17' H17' 108.6 . . ? C22' C17' H17' 108.6 . . ? N5 C17' H17' 108.6 . . ? N6 C18' C19 118(3) . . ? N6 C18' C17' 115(4) . . ? C19 C18' C17' 125(4) . . ? N6 C18' H18' 93.5 . . ? C19 C18' H18' 93.5 . . ? C17' C18' H18' 93.5 . . ? C19 C20' C21' 104(3) . . ? C19 C20' H20C 111.0 . . ? C21' C20' H20C 111.0 . . ? C19 C20' H20D 111.0 . . ? C21' C20' H20D 111.0 . . ? H20C C20' H20D 109.0 . . ? C22' C21' C20' 116(4) . . ? C22' C21' H21C 108.2 . . ? C20' C21' H21C 108.2 . . ? C22' C21' H21D 108.2 . . ? C20' C21' H21D 108.2 . . ? H21C C21' H21D 107.3 . . ? C21' C22' C17' 111(4) . . ? C21' C22' H22C 109.4 . . ? C17' C22' H22C 109.4 . . ? C21' C22' H22D 109.4 . . ? C17' C22' H22D 109.4 . . ? H22C C22' H22D 108.0 . . ? C1 N1 Pt1 124.1(15) . . ? C1 N1 H1 117.9 . . ? Pt1 N1 H1 117.9 . . ? C6 O2 Pt1 125.3(12) . . ? C11' N3 Pt1 118.7(18) . . ? C11 N3 Pt1 105.2(19) . . ? C11 N3 H3D 110.7 . . ? Pt1 N3 H3D 110.7 . . ? C11' N3 H3E 119.1 . . ? C11 N3 H3E 110.7 . . ? Pt1 N3 H3E 110.7 . . ? H3D N3 H3E 108.8 . . ? C12 N4 Pt1 113.8(18) . . ? C12' N4 Pt1 101.8(19) . . ? C12 N4 H4D 108.8 . . ? C12' N4 H4D 97.8 . . ? Pt1 N4 H4D 108.8 . . ? C12 N4 H4E 108.8 . . ? C12' N4 H4E 130.4 . . ? Pt1 N4 H4E 108.8 . . ? H4D N4 H4E 107.7 . . ? C17 N5 Pt2 111.5(17) . . ? C17' N5 Pt2 107.6(19) . . ? C17 N5 H5D 109.3 . . ? C17' N5 H5D 77.6 . . ? Pt2 N5 H5D 109.3 . . ? C17 N5 H5E 109.3 . . ? C17' N5 H5E 137.8 . . ? Pt2 N5 H5E 109.3 . . ? H5D N5 H5E 108.0 . . ? C18' N6 Pt2 108(2) . . ? C18 N6 Pt2 108.7(13) . . ? C18' N6 H6A 116.6 . . ? C18 N6 H6A 110.0 . . ? Pt2 N6 H6A 110.0 . . ? C18' N6 H6B 103.2 . . ? C18 N6 H6B 110.0 . . ? Pt2 N6 H6B 110.0 . . ? H6A N6 H6B 108.3 . . ? O5 N7 O4 119(2) . . ? O5 N7 O3 120(2) . . ? O4 N7 O3 121(2) . . ? O7 N8 O8 118(3) . . ? O7 N8 O6 132(3) . . ? O8 N8 O6 109(2) . . ? O10 N9 O9 116(4) . . ? O10 N9 O11 123(4) . . ? O9 N9 O11 121(4) . . ? O12 N10 O14 129(3) . . ? O12 N10 O13 121(3) . . ? O14 N10 O13 109(3) . . ? O17 N11 O15 119(2) . . ? O17 N11 O16 121(2) . . ? O15 N11 O16 120(2) . . ? O19 N12 O18 134(4) . . ? O19 N12 O20 118(3) . . ? O18 N12 O20 108(3) . . ? C1 O1 Pt2 122.0(14) . . ? C6 N2 Pt2 127.6(17) . . ? C6 N2 H2 116.2 . . ? Pt2 N2 H2 116.2 . . ? N7 O3 Pt1 126.3(15) . . ? N8 O6 Pt2 116.7(15) . . ? H4 O21 H3 104.0 . . ? H4 O21 H3 104.0 . . ? H3 O21 H4 104.0 . . ? H3 O21 H4 104.0 . . ? O2 Pt1 N3 93.5(6) . . ? O2 Pt1 N1 89.9(6) . . ? N3 Pt1 N1 172.6(7) . . ? O2 Pt1 N4 173.1(7) . . ? N3 Pt1 N4 85.5(7) . . ? N1 Pt1 N4 90.4(7) . . ? O2 Pt1 O3 97.1(6) . . ? N3 Pt1 O3 86.5(6) . . ? N1 Pt1 O3 86.6(6) . . ? N4 Pt1 O3 76.0(6) . . ? O2 Pt1 Pt2 84.0(4) . . ? N3 Pt1 Pt2 103.9(5) . . ? N1 Pt1 Pt2 83.0(5) . . ? N4 Pt1 Pt2 102.9(5) . . ? O3 Pt1 Pt2 169.5(4) . . ? N2 Pt2 O1 90.1(6) . . ? N2 Pt2 N5 90.7(6) . . ? O1 Pt2 N5 170.2(6) . . ? N2 Pt2 N6 174.1(6) . . ? O1 Pt2 N6 93.3(6) . . ? N5 Pt2 N6 85.2(6) . . ? N2 Pt2 O6 82.0(6) . . ? O1 Pt2 O6 89.2(6) . . ? N5 Pt2 O6 81.3(7) . . ? N6 Pt2 O6 93.1(6) . . ? N2 Pt2 Pt1 84.3(5) . . ? O1 Pt2 Pt1 86.3(4) . . ? N5 Pt2 Pt1 103.5(5) . . ? N6 Pt2 Pt1 100.8(5) . . ? O6 Pt2 Pt1 165.6(4) . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 146(2) . . . . ? N1 C1 C2 C3 -34(3) . . . . ? O1 C1 C2 C4 -97(2) . . . . ? N1 C1 C2 C4 83(3) . . . . ? O1 C1 C2 C5 22(3) . . . . ? N1 C1 C2 C5 -157(2) . . . . ? N2 C6 C7 C8 -149(2) . . . . ? O2 C6 C7 C8 32(2) . . . . ? N2 C6 C7 C9 86(2) . . . . ? O2 C6 C7 C9 -93(2) . . . . ? N2 C6 C7 C10 -32(3) . . . . ? O2 C6 C7 C10 148.8(18) . . . . ? N3 C11 C12 C13 170(3) . . . . ? C16 C11 C12 C13 33(4) . . . . ? N3 C11 C12 N4 -44(5) . . . . ? C16 C11 C12 N4 179(3) . . . . ? N4 C12 C13 C14 -173(5) . . . . ? C11 C12 C13 C14 -41(4) . . . . ? C12 C13 C14 C15 41(6) . . . . ? C13 C14 C15 C16 -34(5) . . . . ? C14 C15 C16 C11 34(4) . . . . ? C12 C11 C16 C15 -35(5) . . . . ? N3 C11 C16 C15 -171.5(18) . . . . ? C22 C17 C18 C19 12(3) . . . . ? N5 C17 C18 C19 164(4) . . . . ? C22 C17 C18 N6 -172(4) . . . . ? N5 C17 C18 N6 -19.7(11) . . . . ? C17 C18 C19 C20' 5(4) . . . . ? N6 C18 C19 C20' -171(3) . . . . ? C17 C18 C19 C20 -14(3) . . . . ? N6 C18 C19 C20 170(2) . . . . ? C18 C19 C20 C21 25(3) . . . . ? C20' C19 C20 C21 -79(9) . . . . ? C18' C19 C20 C21 34(3) . . . . ? C19 C20 C21 C22 -35(2) . . . . ? C18 C17 C22 C21 -20(4) . . . . ? N5 C17 C22 C21 -172(3) . . . . ? C20 C21 C22 C17 30(4) . . . . ? C16' C11' C12' C13' -40(7) . . . . ? N3 C11' C12' C13' -173(3) . . . . ? C16' C11' C12' N4 170(4) . . . . ? N3 C11' C12' N4 36(6) . . . . ? C11' C12' C13' C14' 26(6) . . . . ? N4 C12' C13' C14' 178(4) . . . . ? C12' C13' C14' C15' -38(7) . . . . ? C13' C14' C15' C16' 51(6) . . . . ? N3 C11' C16' C15' 180(3) . . . . ? C12' C11' C16' C15' 51(7) . . . . ? C14' C15' C16' C11' -49(6) . . . . ? C20' C19 C18' N6 -161(4) . . . . ? C20 C19 C18' N6 -180(4) . . . . ? C20' C19 C18' C17' 31(7) . . . . ? C20 C19 C18' C17' 13(7) . . . . ? C22' C17' C18' N6 163(4) . . . . ? N5 C17' C18' N6 38(6) . . . . ? C22' C17' C18' C19 -29(7) . . . . ? N5 C17' C18' C19 -154(4) . . . . ? C18 C19 C20' C21' -49(5) . . . . ? C20 C19 C20' C21' 33(6) . . . . ? C18' C19 C20' C21' -41(5) . . . . ? C19 C20' C21' C22' 61(6) . . . . ? C20' C21' C22' C17' -66(6) . . . . ? C18' C17' C22' C21' 42(6) . . . . ? N5 C17' C22' C21' 163(4) . . . . ? O1 C1 N1 Pt1 1(3) . . . . ? C2 C1 N1 Pt1 -179.4(14) . . . . ? N2 C6 O2 Pt1 -4(3) . . . . ? C7 C6 O2 Pt1 175.1(12) . . . . ? C16' C11' N3 C11 -105(8) . . . . ? C12' C11' N3 C11 38(4) . . . . ? C16' C11' N3 Pt1 -168(3) . . . . ? C12' C11' N3 Pt1 -25(4) . . . . ? C12 C11 N3 C11' -91(7) . . . . ? C16 C11 N3 C11' 46(6) . . . . ? C12 C11 N3 Pt1 35(4) . . . . ? C16 C11 N3 Pt1 172(2) . . . . ? C13 C12 N4 C12' 106(9) . . . . ? C11 C12 N4 C12' -27(6) . . . . ? C13 C12 N4 Pt1 165.8(8) . . . . ? C11 C12 N4 Pt1 32(4) . . . . ? C11' C12' N4 C12 98(10) . . . . ? C13' C12' N4 C12 -50(8) . . . . ? C11' C12' N4 Pt1 -28(5) . . . . ? C13' C12' N4 Pt1 -176(4) . . . . ? C18 C17 N5 C17' -69(4) . . . . ? C22 C17 N5 C17' 83(5) . . . . ? C18 C17 N5 Pt2 21.7(16) . . . . ? C22 C17 N5 Pt2 174(3) . . . . ? C18' C17' N5 C17 62(6) . . . . ? C22' C17' N5 C17 -58(5) . . . . ? C18' C17' N5 Pt2 -40(5) . . . . ? C22' C17' N5 Pt2 -161(4) . . . . ? C19 C18' N6 C18 81(16) . . . . ? C19 C18' N6 Pt2 174(3) . . . . ? C17' C18' N6 Pt2 -17(5) . . . . ? C19 C18 N6 C18' -86(18) . . . . ? C17 C18 N6 Pt2 8.0(15) . . . . ? C19 C18 N6 Pt2 -175(2) . . . . ? N1 C1 O1 Pt2 -5(3) . . . . ? C2 C1 O1 Pt2 175.1(14) . . . . ? O2 C6 N2 Pt2 -1(3) . . . . ? C7 C6 N2 Pt2 -179.9(13) . . . . ? O5 N7 O3 Pt1 176.0(17) . . . . ? O4 N7 O3 Pt1 5(3) . . . . ? O7 N8 O6 Pt2 -35(4) . . . . ? O8 N8 O6 Pt2 157(2) . . . . ? C6 O2 Pt1 N3 108.5(17) . . . . ? C6 O2 Pt1 N1 -78.0(17) . . . . ? C6 O2 Pt1 O3 -164.6(16) . . . . ? C6 O2 Pt1 Pt2 4.9(16) . . . . ? C11' N3 Pt1 O2 -175(3) . . . . ? C11 N3 Pt1 O2 161(2) . . . . ? C11' N3 Pt1 N4 12(3) . . . . ? C11 N3 Pt1 N4 -12(2) . . . . ? C11' N3 Pt1 O3 88(3) . . . . ? C11 N3 Pt1 O3 65(2) . . . . ? C11' N3 Pt1 Pt2 -90(3) . . . . ? C11 N3 Pt1 Pt2 -113.9(19) . . . . ? C1 N1 Pt1 O2 86.5(17) . . . . ? C1 N1 Pt1 N4 -100.4(18) . . . . ? C1 N1 Pt1 O3 -176.4(17) . . . . ? C1 N1 Pt1 Pt2 2.5(16) . . . . ? C12 N4 Pt1 N3 -12(2) . . . . ? C12' N4 Pt1 N3 7(2) . . . . ? C12 N4 Pt1 N1 174(2) . . . . ? C12' N4 Pt1 N1 -167(2) . . . . ? C12 N4 Pt1 O3 -99(2) . . . . ? C12' N4 Pt1 O3 -81(2) . . . . ? C12 N4 Pt1 Pt2 91(2) . . . . ? C12' N4 Pt1 Pt2 110(2) . . . . ? N7 O3 Pt1 O2 -17.3(18) . . . . ? N7 O3 Pt1 N3 75.8(17) . . . . ? N7 O3 Pt1 N1 -106.8(17) . . . . ? N7 O3 Pt1 N4 162.0(18) . . . . ? N7 O3 Pt1 Pt2 -113(2) . . . . ? C6 N2 Pt2 O1 89.9(18) . . . . ? C6 N2 Pt2 N5 -99.9(18) . . . . ? C6 N2 Pt2 O6 179.0(18) . . . . ? C6 N2 Pt2 Pt1 3.6(17) . . . . ? C1 O1 Pt2 N2 -78.9(16) . . . . ? C1 O1 Pt2 N6 106.0(16) . . . . ? C1 O1 Pt2 O6 -161.0(16) . . . . ? C1 O1 Pt2 Pt1 5.3(16) . . . . ? C17 N5 Pt2 N2 171.4(18) . . . . ? C17' N5 Pt2 N2 -150(2) . . . . ? C17 N5 Pt2 N6 -12.9(18) . . . . ? C17' N5 Pt2 N6 25(2) . . . . ? C17 N5 Pt2 O6 -106.8(18) . . . . ? C17' N5 Pt2 O6 -68(2) . . . . ? C17 N5 Pt2 Pt1 87.1(17) . . . . ? C17' N5 Pt2 Pt1 125(2) . . . . ? C18' N6 Pt2 O1 165(3) . . . . ? C18 N6 Pt2 O1 173.2(17) . . . . ? C18' N6 Pt2 N5 -5(3) . . . . ? C18 N6 Pt2 N5 2.9(17) . . . . ? C18' N6 Pt2 O6 76(3) . . . . ? C18 N6 Pt2 O6 83.8(18) . . . . ? C18' N6 Pt2 Pt1 -108(3) . . . . ? C18 N6 Pt2 Pt1 -100.0(17) . . . . ? N8 O6 Pt2 N2 -132.7(15) . . . . ? N8 O6 Pt2 O1 -42.5(15) . . . . ? N8 O6 Pt2 N5 135.4(15) . . . . ? N8 O6 Pt2 N6 50.8(16) . . . . ? N8 O6 Pt2 Pt1 -114.0(18) . . . . ? O2 Pt1 Pt2 N2 -3.4(6) . . . . ? N3 Pt1 Pt2 N2 -95.5(6) . . . . ? N1 Pt1 Pt2 N2 87.3(6) . . . . ? N4 Pt1 Pt2 N2 176.0(7) . . . . ? O3 Pt1 Pt2 N2 93(2) . . . . ? O2 Pt1 Pt2 O1 -93.8(6) . . . . ? N3 Pt1 Pt2 O1 174.0(6) . . . . ? N1 Pt1 Pt2 O1 -3.2(6) . . . . ? N4 Pt1 Pt2 O1 85.6(7) . . . . ? O3 Pt1 Pt2 O1 3(2) . . . . ? O2 Pt1 Pt2 N5 85.9(6) . . . . ? N3 Pt1 Pt2 N5 -6.2(6) . . . . ? N1 Pt1 Pt2 N5 176.6(6) . . . . ? N4 Pt1 Pt2 N5 -94.7(7) . . . . ? O3 Pt1 Pt2 N5 -177(2) . . . . ? O2 Pt1 Pt2 N6 173.5(6) . . . . ? N3 Pt1 Pt2 N6 81.4(7) . . . . ? N1 Pt1 Pt2 N6 -95.8(7) . . . . ? N4 Pt1 Pt2 N6 -7.0(7) . . . . ? O3 Pt1 Pt2 N6 -90(2) . . . . ? O2 Pt1 Pt2 O6 -21.9(17) . . . . ? N3 Pt1 Pt2 O6 -114.1(17) . . . . ? N1 Pt1 Pt2 O6 68.7(17) . . . . ? N4 Pt1 Pt2 O6 157.5(18) . . . . ? O3 Pt1 Pt2 O6 75(3) . . . . ? _diffrn_measured_fraction_theta_max 0.893 _diffrn_reflns_theta_full 22.00 _diffrn_measured_fraction_theta_full 0.893 _refine_diff_density_max 1.884 _refine_diff_density_min -1.669 _refine_diff_density_rms 0.203 #===END data_pt5a _database_code_depnum_ccdc_archive 'CCDC 290080' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H70 Cl8 N8 O7 Pt5' _chemical_formula_weight 1950.02 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' 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.764(6) _cell_length_b 11.444(7) _cell_length_c 15.520(10) _cell_angle_alpha 73.253(7) _cell_angle_beta 76.759(7) _cell_angle_gamma 68.931(8) _cell_volume 1534.3(17) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.110 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 906 _exptl_absorpt_coefficient_mu 11.747 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0916 _exptl_absorpt_correction_T_max 0.3863 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 2946 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0656 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 4.86 _diffrn_reflns_theta_max 19.00 _reflns_number_total 2253 _reflns_number_gt 2099 _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^)+(0.1024P)^2^+0.0000P] 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 2253 _refine_ls_number_parameters 313 _refine_ls_number_restraints 104 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.1333 _refine_ls_wR_factor_gt 0.1307 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.000 _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 C1 C 0.4890(18) 0.1639(18) 0.2642(13) 0.049(4) Uani 1 1 d . . . C2 C 0.398(2) 0.2060(17) 0.3496(11) 0.067(5) Uani 1 1 d . . . C3 C 0.502(2) 0.233(2) 0.3974(12) 0.084(6) Uani 1 1 d . . . H3A H 0.5951 0.1659 0.3975 0.126 Uiso 1 1 calc R . . H3B H 0.4573 0.2374 0.4589 0.126 Uiso 1 1 calc R . . H3C H 0.5173 0.3140 0.3656 0.126 Uiso 1 1 calc R . . C4 C 0.266(2) 0.3289(17) 0.3296(13) 0.077(6) Uani 1 1 d . . . H4A H 0.3020 0.4010 0.3018 0.116 Uiso 1 1 calc R . . H4B H 0.2025 0.3428 0.3853 0.116 Uiso 1 1 calc R . . H4C H 0.2115 0.3198 0.2890 0.116 Uiso 1 1 calc R . . C5 C 0.335(2) 0.0978(19) 0.4058(13) 0.093(7) Uani 1 1 d . . . H5A H 0.2906 0.0730 0.3674 0.140 Uiso 1 1 calc R . . H5B H 0.2605 0.1277 0.4540 0.140 Uiso 1 1 calc R . . H5C H 0.4127 0.0252 0.4311 0.140 Uiso 1 1 calc R . . C6 C 0.8645(18) 0.1544(18) 0.1587(12) 0.047(4) Uani 1 1 d . . . C7 C 0.9733(16) 0.1907(15) 0.1936(11) 0.053(5) Uani 1 1 d . . . C8 C 0.998(2) 0.3194(18) 0.1341(14) 0.085(6) Uani 1 1 d . . . H8A H 1.0230 0.3148 0.0713 0.128 Uiso 1 1 calc R . . H8B H 1.0779 0.3324 0.1527 0.128 Uiso 1 1 calc R . . H8C H 0.9093 0.3897 0.1416 0.128 Uiso 1 1 calc R . . C9 C 1.1283(17) 0.0811(18) 0.1928(13) 0.078(6) Uani 1 1 d . . . H9A H 1.1160 0.0016 0.2302 0.117 Uiso 1 1 calc R . . H9B H 1.1960 0.1037 0.2161 0.117 Uiso 1 1 calc R . . H9C H 1.1671 0.0714 0.1317 0.117 Uiso 1 1 calc R . . C10 C 0.908(2) 0.210(2) 0.2863(14) 0.099(7) Uani 1 1 d . . . H10A H 0.8197 0.2824 0.2834 0.149 Uiso 1 1 calc R . . H10B H 0.9783 0.2246 0.3129 0.149 Uiso 1 1 calc R . . H10C H 0.8845 0.1343 0.3228 0.149 Uiso 1 1 calc R . . C11 C 0.7997(18) -0.1835(16) 0.2789(13) 0.068(5) Uani 1 1 d . . . H11 H 0.8164 -0.1512 0.3263 0.082 Uiso 1 1 calc R . . C12 C 0.943(3) -0.275(2) 0.2446(16) 0.093(7) Uani 1 1 d . . . C13 C 0.920(3) -0.385(2) 0.2368(19) 0.116(10) Uani 1 1 d . . . H13A H 0.9835 -0.4615 0.2727 0.140 Uiso 1 1 calc R . . H13B H 0.9444 -0.3922 0.1739 0.140 Uiso 1 1 calc R . . C14 C 0.764(3) -0.375(2) 0.2696(19) 0.113(9) Uani 1 1 d . . . H14A H 0.7549 -0.4557 0.3096 0.135 Uiso 1 1 calc R . . H14B H 0.7098 -0.3546 0.2191 0.135 Uiso 1 1 calc R . . C15 C 0.705(2) -0.2682(19) 0.3206(14) 0.082(6) Uani 1 1 d . . . H15A H 0.6016 -0.2208 0.3135 0.098 Uiso 1 1 calc R . . H15B H 0.7121 -0.3027 0.3848 0.098 Uiso 1 1 calc R . . C16 C 0.080(3) 0.680(3) 0.4598(19) 0.049(9) Uani 0.25 1 d PDU . . C17 C 0.224(4) 0.573(3) 0.464(4) 0.056(9) Uani 0.25 1 d PDU . . H17A H 0.2285 0.5134 0.4287 0.067 Uiso 0.25 1 calc PR . . H17B H 0.2343 0.5259 0.5261 0.067 Uiso 0.25 1 calc PR . . C18 C 0.348(3) 0.634(4) 0.424(4) 0.057(9) Uani 0.25 1 d PDU . . H18A H 0.4199 0.6038 0.4659 0.068 Uiso 0.25 1 calc PR . . H18B H 0.3983 0.6097 0.3671 0.068 Uiso 0.25 1 calc PR . . C19 C 0.278(4) 0.778(4) 0.408(4) 0.049(9) Uani 0.25 1 d PDU . . H19A H 0.2963 0.8183 0.3445 0.059 Uiso 0.25 1 calc PR . . H19B H 0.3198 0.8126 0.4429 0.059 Uiso 0.25 1 calc PR . . C20 C 0.109(4) 0.807(3) 0.440(4) 0.055(9) Uani 0.25 1 d PDU . . H20A H 0.0795 0.8407 0.4945 0.066 Uiso 0.25 1 calc PR . . H20B H 0.0529 0.8688 0.3931 0.066 Uiso 0.25 1 calc PR . . Cl1 Cl 0.5131(5) -0.0821(4) 0.1591(3) 0.0593(13) Uani 1 1 d . . . Cl2 Cl 0.8531(5) -0.1101(4) 0.0531(3) 0.0647(14) Uani 1 1 d . . . Cl3 Cl 0.2601(4) 0.5033(4) 0.0627(3) 0.0587(13) Uani 1 1 d . . . Cl4 Cl 0.5341(5) 0.5358(4) 0.1317(3) 0.0613(12) Uani 1 1 d . . . N1 N 0.4762(13) 0.2409(13) 0.1836(9) 0.045(4) Uani 1 1 d . . . H1 H 0.4034 0.3115 0.1810 0.054 Uiso 1 1 calc R . . N2 N 0.7707(14) 0.2355(13) 0.1086(10) 0.050(4) Uani 1 1 d . . . H2 H 0.7802 0.3110 0.0900 0.061 Uiso 1 1 calc R . . N3 N 0.7352(14) 0.1942(12) -0.0569(8) 0.054(4) Uani 1 1 d . . . H3D H 0.6821 0.2406 -0.1019 0.080 Uiso 1 1 calc R . . H3E H 0.7675 0.1118 -0.0593 0.080 Uiso 1 1 calc R . . H3F H 0.8122 0.2213 -0.0625 0.080 Uiso 1 1 calc R . . N4 N 0.4236(13) 0.2037(12) 0.0245(9) 0.055(4) Uani 1 1 d . . . H4D H 0.3715 0.1655 0.0718 0.083 Uiso 1 1 calc R . . H4E H 0.4549 0.1582 -0.0181 0.083 Uiso 1 1 calc R . . H4F H 0.3666 0.2825 0.0019 0.083 Uiso 1 1 calc R . . O1 O 0.5861(12) 0.0518(12) 0.2753(7) 0.055(3) Uani 1 1 d . . . O2 O 0.8734(12) 0.0347(11) 0.1863(8) 0.060(3) Uani 1 1 d . . . O3 O 1.062(2) -0.2463(17) 0.2331(12) 0.131(7) Uani 1 1 d . . . O4 O -0.040(3) 0.667(4) 0.470(3) 0.089(12) Uani 0.25 1 d PDU . . Pt1 Pt 0.70931(7) -0.02281(6) 0.17127(4) 0.0442(4) Uani 1 1 d . . . Pt2 Pt 0.60453(6) 0.21503(5) 0.06607(4) 0.0396(4) Uani 1 1 d . . . Pt3 Pt 0.5000 0.5000 0.0000 0.0434(4) Uani 1 2 d S . . 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 C1 0.050(12) 0.052(13) 0.043(13) -0.025(11) 0.008(10) -0.010(10) C2 0.076(13) 0.060(13) 0.038(12) 0.009(10) -0.001(10) -0.011(11) C3 0.092(15) 0.108(17) 0.057(13) -0.037(12) -0.015(11) -0.021(13) C4 0.069(13) 0.063(13) 0.067(14) -0.017(10) 0.005(10) 0.009(11) C5 0.084(15) 0.089(16) 0.074(15) -0.011(12) 0.039(12) -0.025(12) C6 0.041(11) 0.052(14) 0.060(12) -0.022(10) 0.011(10) -0.033(10) C7 0.048(11) 0.052(11) 0.054(12) -0.014(9) -0.002(9) -0.010(9) C8 0.073(14) 0.080(15) 0.123(19) -0.023(13) -0.032(12) -0.037(11) C9 0.049(12) 0.085(15) 0.094(16) -0.020(12) -0.030(11) -0.001(10) C10 0.067(14) 0.17(2) 0.096(17) -0.078(16) 0.003(12) -0.050(14) C11 0.050(12) 0.048(12) 0.085(14) 0.002(10) -0.010(10) -0.002(10) C12 0.054(16) 0.10(2) 0.100(18) -0.029(14) 0.009(13) -0.010(15) C13 0.086(19) 0.061(16) 0.18(3) -0.051(16) 0.053(16) -0.023(14) C14 0.12(2) 0.051(15) 0.17(2) -0.042(15) -0.077(19) 0.018(13) C15 0.101(17) 0.074(15) 0.072(15) 0.000(12) -0.026(12) -0.035(13) C16 0.06(2) 0.069(19) 0.031(18) -0.006(16) -0.007(17) -0.038(16) C17 0.07(2) 0.066(19) 0.035(18) -0.005(16) -0.011(16) -0.029(16) C18 0.06(2) 0.069(19) 0.037(18) -0.003(16) -0.007(16) -0.028(17) C19 0.06(2) 0.064(19) 0.034(18) 0.000(16) -0.012(16) -0.036(17) C20 0.07(2) 0.068(19) 0.032(18) -0.005(16) -0.010(16) -0.026(17) Cl1 0.053(3) 0.046(3) 0.082(3) -0.015(2) -0.011(2) -0.016(2) Cl2 0.062(3) 0.050(3) 0.068(3) -0.024(2) 0.006(2) -0.001(2) Cl3 0.037(3) 0.047(3) 0.077(3) -0.004(2) 0.005(2) -0.011(2) Cl4 0.076(3) 0.048(3) 0.059(3) -0.013(2) -0.018(2) -0.012(2) N1 0.028(8) 0.061(10) 0.028(9) -0.015(8) 0.008(6) 0.001(7) N2 0.042(9) 0.035(8) 0.075(11) -0.013(7) -0.040(8) 0.006(7) N3 0.047(8) 0.052(9) 0.051(9) -0.022(7) 0.017(7) -0.009(7) N4 0.045(8) 0.047(9) 0.075(10) -0.020(7) -0.010(7) -0.009(7) O1 0.044(7) 0.053(9) 0.055(8) -0.028(6) 0.007(6) 0.004(7) O2 0.063(8) 0.042(8) 0.078(9) -0.008(6) -0.010(6) -0.023(6) O3 0.096(13) 0.111(14) 0.137(16) -0.004(11) -0.011(11) 0.002(11) O4 0.09(2) 0.10(2) 0.06(2) -0.001(19) 0.00(2) -0.03(2) Pt1 0.0422(6) 0.0294(6) 0.0540(6) -0.0091(4) -0.0053(4) -0.0041(4) Pt2 0.0383(6) 0.0304(5) 0.0445(6) -0.0077(4) -0.0038(4) -0.0060(4) Pt3 0.0402(7) 0.0304(7) 0.0523(7) -0.0060(5) -0.0040(5) -0.0067(5) _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 C1 O1 1.284(19) . ? C1 N1 1.309(19) . ? C1 C2 1.52(2) . ? C2 C3 1.54(2) . ? C2 C4 1.54(2) . ? C2 C5 1.54(2) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 N2 1.27(2) . ? C6 O2 1.289(18) . ? C6 C7 1.52(2) . ? C7 C10 1.48(2) . ? C7 C9 1.58(2) . ? C7 C8 1.57(2) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C15 1.49(2) . ? C11 C12 1.51(3) . ? C11 Pt1 2.165(16) . ? C11 H11 0.9800 . ? C12 O3 1.28(3) . ? C12 C13 1.40(3) . ? C13 C14 1.47(3) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.52(3) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 O4 1.205(16) . ? C16 C17 1.494(17) . ? C16 C20 1.508(17) . ? C17 C18 1.530(18) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.518(18) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.555(18) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? Cl1 Pt1 2.311(4) . ? Cl2 Pt1 2.281(4) . ? Cl3 Pt3 2.312(4) . ? Cl4 Pt3 2.312(4) . ? N1 Pt2 1.996(12) . ? N1 H1 0.8600 . ? N2 Pt2 1.994(13) . ? N2 H2 0.8600 . ? N3 Pt2 2.063(11) . ? N3 H3D 0.8900 . ? N3 H3E 0.8900 . ? N3 H3F 0.8900 . ? N4 Pt2 2.071(12) . ? N4 H4D 0.8900 . ? N4 H4E 0.8900 . ? N4 H4F 0.8900 . ? O1 Pt1 1.987(11) . ? O2 Pt1 2.018(12) . ? Pt1 Pt2 2.7060(15) . ? Pt2 Pt3 2.9812(19) . ? Pt3 Cl3 2.312(4) 2_665 ? Pt3 Cl4 2.312(4) 2_665 ? Pt3 Pt2 2.9812(19) 2_665 ? 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 O1 C1 N1 121.5(14) . . ? O1 C1 C2 116.6(17) . . ? N1 C1 C2 121.8(16) . . ? C3 C2 C4 108.3(16) . . ? C3 C2 C1 107.1(14) . . ? C4 C2 C1 112.8(16) . . ? C3 C2 C5 114.4(16) . . ? C4 C2 C5 107.3(16) . . ? C1 C2 C5 107.0(15) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 O2 123.0(15) . . ? N2 C6 C7 122.8(15) . . ? O2 C6 C7 114.2(16) . . ? C10 C7 C6 107.1(13) . . ? C10 C7 C9 111.8(15) . . ? C6 C7 C9 109.8(14) . . ? C10 C7 C8 108.0(16) . . ? C6 C7 C8 112.0(14) . . ? C9 C7 C8 108.0(14) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C15 C11 C12 102.6(17) . . ? C15 C11 Pt1 114.0(13) . . ? C12 C11 Pt1 112.1(13) . . ? C15 C11 H11 109.3 . . ? C12 C11 H11 109.3 . . ? Pt1 C11 H11 109.3 . . ? O3 C12 C13 131(2) . . ? O3 C12 C11 118(2) . . ? C13 C12 C11 111(2) . . ? C12 C13 C14 108.4(19) . . ? C12 C13 H13A 110.0 . . ? C14 C13 H13A 110.0 . . ? C12 C13 H13B 110.0 . . ? C14 C13 H13B 110.0 . . ? H13A C13 H13B 108.4 . . ? C13 C14 C15 105.3(19) . . ? C13 C14 H14A 110.7 . . ? C15 C14 H14A 110.7 . . ? C13 C14 H14B 110.7 . . ? C15 C14 H14B 110.7 . . ? H14A C14 H14B 108.8 . . ? C11 C15 C14 105.2(18) . . ? C11 C15 H15A 110.7 . . ? C14 C15 H15A 110.7 . . ? C11 C15 H15B 110.7 . . ? C14 C15 H15B 110.7 . . ? H15A C15 H15B 108.8 . . ? O4 C16 C17 125.5(18) . . ? O4 C16 C20 124.8(18) . . ? C17 C16 C20 109.7(11) . . ? C16 C17 C18 107.1(11) . . ? C16 C17 H17A 110.3 . . ? C18 C17 H17A 110.3 . . ? C16 C17 H17B 110.3 . . ? C18 C17 H17B 110.3 . . ? H17A C17 H17B 108.5 . . ? C19 C18 C17 107.9(11) . . ? C19 C18 H18A 110.1 . . ? C17 C18 H18A 110.1 . . ? C19 C18 H18B 110.1 . . ? C17 C18 H18B 110.1 . . ? H18A C18 H18B 108.4 . . ? C18 C19 C20 107.5(11) . . ? C18 C19 H19A 110.2 . . ? C20 C19 H19A 110.2 . . ? C18 C19 H19B 110.2 . . ? C20 C19 H19B 110.2 . . ? H19A C19 H19B 108.5 . . ? C16 C20 C19 105.9(11) . . ? C16 C20 H20A 110.6 . . ? C19 C20 H20A 110.6 . . ? C16 C20 H20B 110.6 . . ? C19 C20 H20B 110.6 . . ? H20A C20 H20B 108.7 . . ? C1 N1 Pt2 128.1(11) . . ? C1 N1 H1 116.0 . . ? Pt2 N1 H1 116.0 . . ? C6 N2 Pt2 129.9(12) . . ? C6 N2 H2 115.0 . . ? Pt2 N2 H2 115.0 . . ? Pt2 N3 H3D 109.5 . . ? Pt2 N3 H3E 109.5 . . ? H3D N3 H3E 109.5 . . ? Pt2 N3 H3F 109.5 . . ? H3D N3 H3F 109.5 . . ? H3E N3 H3F 109.5 . . ? Pt2 N4 H4D 109.5 . . ? Pt2 N4 H4E 109.5 . . ? H4D N4 H4E 109.5 . . ? Pt2 N4 H4F 109.5 . . ? H4D N4 H4F 109.5 . . ? H4E N4 H4F 109.5 . . ? C1 O1 Pt1 122.3(11) . . ? C6 O2 Pt1 119.5(11) . . ? O1 Pt1 O2 88.4(5) . . ? O1 Pt1 C11 82.6(6) . . ? O2 Pt1 C11 82.2(6) . . ? O1 Pt1 Cl2 179.2(4) . . ? O2 Pt1 Cl2 91.1(4) . . ? C11 Pt1 Cl2 96.7(5) . . ? O1 Pt1 Cl1 88.7(3) . . ? O2 Pt1 Cl1 177.0(3) . . ? C11 Pt1 Cl1 98.1(5) . . ? Cl2 Pt1 Cl1 91.79(17) . . ? O1 Pt1 Pt2 86.1(3) . . ? O2 Pt1 Pt2 86.7(3) . . ? C11 Pt1 Pt2 164.3(6) . . ? Cl2 Pt1 Pt2 94.49(12) . . ? Cl1 Pt1 Pt2 92.50(12) . . ? N1 Pt2 N2 90.4(5) . . ? N1 Pt2 N3 178.3(5) . . ? N2 Pt2 N3 89.5(6) . . ? N1 Pt2 N4 87.3(5) . . ? N2 Pt2 N4 176.6(5) . . ? N3 Pt2 N4 92.7(5) . . ? N1 Pt2 Pt1 80.5(4) . . ? N2 Pt2 Pt1 79.8(4) . . ? N3 Pt2 Pt1 101.2(4) . . ? N4 Pt2 Pt1 102.3(4) . . ? N1 Pt2 Pt3 87.2(4) . . ? N2 Pt2 Pt3 87.5(4) . . ? N3 Pt2 Pt3 91.1(4) . . ? N4 Pt2 Pt3 89.9(4) . . ? Pt1 Pt2 Pt3 162.18(3) . . ? Cl3 Pt3 Cl3 180.0 . 2_665 ? Cl3 Pt3 Cl4 90.02(17) . . ? Cl3 Pt3 Cl4 89.98(17) 2_665 . ? Cl3 Pt3 Cl4 89.98(17) . 2_665 ? Cl3 Pt3 Cl4 90.02(17) 2_665 2_665 ? Cl4 Pt3 Cl4 180.0 . 2_665 ? Cl3 Pt3 Pt2 89.85(10) . . ? Cl3 Pt3 Pt2 90.15(10) 2_665 . ? Cl4 Pt3 Pt2 93.18(10) . . ? Cl4 Pt3 Pt2 86.82(10) 2_665 . ? Cl3 Pt3 Pt2 90.15(10) . 2_665 ? Cl3 Pt3 Pt2 89.85(10) 2_665 2_665 ? Cl4 Pt3 Pt2 86.82(10) . 2_665 ? Cl4 Pt3 Pt2 93.18(10) 2_665 2_665 ? Pt2 Pt3 Pt2 180.0 . 2_665 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 71.8(18) . . . . ? N1 C1 C2 C3 -103.9(18) . . . . ? O1 C1 C2 C4 -169.1(15) . . . . ? N1 C1 C2 C4 15(2) . . . . ? O1 C1 C2 C5 -51(2) . . . . ? N1 C1 C2 C5 133.0(17) . . . . ? N2 C6 C7 C10 96.6(19) . . . . ? O2 C6 C7 C10 -81.7(18) . . . . ? N2 C6 C7 C9 -141.8(16) . . . . ? O2 C6 C7 C9 39.9(18) . . . . ? N2 C6 C7 C8 -22(2) . . . . ? O2 C6 C7 C8 160.0(13) . . . . ? C15 C11 C12 O3 -157(2) . . . . ? Pt1 C11 C12 O3 80(2) . . . . ? C15 C11 C12 C13 19(3) . . . . ? Pt1 C11 C12 C13 -103(2) . . . . ? O3 C12 C13 C14 172(2) . . . . ? C11 C12 C13 C14 -3(3) . . . . ? C12 C13 C14 C15 -15(3) . . . . ? C12 C11 C15 C14 -27(2) . . . . ? Pt1 C11 C15 C14 94.2(16) . . . . ? C13 C14 C15 C11 26(2) . . . . ? O4 C16 C17 C18 167(4) . . . . ? C20 C16 C17 C18 -13(4) . . . . ? C16 C17 C18 C19 8(6) . . . . ? C17 C18 C19 C20 1(7) . . . . ? O4 C16 C20 C19 -166(4) . . . . ? C17 C16 C20 C19 14(4) . . . . ? C18 C19 C20 C16 -9(5) . . . . ? O1 C1 N1 Pt2 -5(2) . . . . ? C2 C1 N1 Pt2 170.0(12) . . . . ? O2 C6 N2 Pt2 6(2) . . . . ? C7 C6 N2 Pt2 -172.5(10) . . . . ? N1 C1 O1 Pt1 -7(2) . . . . ? C2 C1 O1 Pt1 177.2(11) . . . . ? N2 C6 O2 Pt1 -12(2) . . . . ? C7 C6 O2 Pt1 166.0(9) . . . . ? C1 O1 Pt1 O2 97.9(12) . . . . ? C1 O1 Pt1 C11 -179.8(13) . . . . ? C1 O1 Pt1 Cl1 -81.5(12) . . . . ? C1 O1 Pt1 Pt2 11.1(12) . . . . ? C6 O2 Pt1 O1 -75.8(11) . . . . ? C6 O2 Pt1 Cl2 104.8(11) . . . . ? C6 O2 Pt1 Pt2 10.4(11) . . . . ? C15 C11 Pt1 O1 79.3(14) . . . . ? C12 C11 Pt1 O1 -164.7(16) . . . . ? C15 C11 Pt1 O2 168.7(15) . . . . ? C12 C11 Pt1 O2 -75.2(16) . . . . ? C15 C11 Pt1 Cl2 -101.1(14) . . . . ? C12 C11 Pt1 Cl2 15.0(16) . . . . ? C15 C11 Pt1 Cl1 -8.3(14) . . . . ? C12 C11 Pt1 Cl1 107.7(15) . . . . ? C15 C11 Pt1 Pt2 123.7(17) . . . . ? C12 C11 Pt1 Pt2 -120(2) . . . . ? C1 N1 Pt2 N2 -69.2(14) . . . . ? C1 N1 Pt2 N4 113.3(14) . . . . ? C1 N1 Pt2 Pt1 10.4(13) . . . . ? C1 N1 Pt2 Pt3 -156.7(13) . . . . ? C6 N2 Pt2 N1 82.3(15) . . . . ? C6 N2 Pt2 N3 -99.4(15) . . . . ? C6 N2 Pt2 Pt1 2.0(14) . . . . ? C6 N2 Pt2 Pt3 169.5(15) . . . . ? O1 Pt1 Pt2 N1 -8.7(5) . . . . ? O2 Pt1 Pt2 N1 -97.3(5) . . . . ? C11 Pt1 Pt2 N1 -52.8(17) . . . . ? Cl2 Pt1 Pt2 N1 171.8(4) . . . . ? Cl1 Pt1 Pt2 N1 79.8(4) . . . . ? O1 Pt1 Pt2 N2 83.4(5) . . . . ? O2 Pt1 Pt2 N2 -5.2(5) . . . . ? C11 Pt1 Pt2 N2 39.3(17) . . . . ? Cl2 Pt1 Pt2 N2 -96.1(4) . . . . ? Cl1 Pt1 Pt2 N2 171.9(4) . . . . ? O1 Pt1 Pt2 N3 170.9(5) . . . . ? O2 Pt1 Pt2 N3 82.2(5) . . . . ? C11 Pt1 Pt2 N3 126.8(17) . . . . ? Cl2 Pt1 Pt2 N3 -8.6(4) . . . . ? Cl1 Pt1 Pt2 N3 -100.6(4) . . . . ? O1 Pt1 Pt2 N4 -93.8(5) . . . . ? O2 Pt1 Pt2 N4 177.5(5) . . . . ? C11 Pt1 Pt2 N4 -137.9(17) . . . . ? Cl2 Pt1 Pt2 N4 86.6(4) . . . . ? Cl1 Pt1 Pt2 N4 -5.3(4) . . . . ? O1 Pt1 Pt2 Pt3 38.2(3) . . . . ? O2 Pt1 Pt2 Pt3 -50.4(3) . . . . ? C11 Pt1 Pt2 Pt3 -5.9(16) . . . . ? Cl2 Pt1 Pt2 Pt3 -141.33(15) . . . . ? Cl1 Pt1 Pt2 Pt3 126.68(14) . . . . ? N1 Pt2 Pt3 Cl3 -44.3(4) . . . . ? N2 Pt2 Pt3 Cl3 -134.8(4) . . . . ? N3 Pt2 Pt3 Cl3 135.7(4) . . . . ? N4 Pt2 Pt3 Cl3 43.0(4) . . . . ? Pt1 Pt2 Pt3 Cl3 -90.42(15) . . . . ? N1 Pt2 Pt3 Cl3 135.7(4) . . . 2_665 ? N2 Pt2 Pt3 Cl3 45.2(4) . . . 2_665 ? N3 Pt2 Pt3 Cl3 -44.3(4) . . . 2_665 ? N4 Pt2 Pt3 Cl3 -137.0(4) . . . 2_665 ? Pt1 Pt2 Pt3 Cl3 89.58(15) . . . 2_665 ? N1 Pt2 Pt3 Cl4 45.7(4) . . . . ? N2 Pt2 Pt3 Cl4 -44.8(4) . . . . ? N3 Pt2 Pt3 Cl4 -134.3(4) . . . . ? N4 Pt2 Pt3 Cl4 133.1(4) . . . . ? Pt1 Pt2 Pt3 Cl4 -0.40(14) . . . . ? N1 Pt2 Pt3 Cl4 -134.3(4) . . . 2_665 ? N2 Pt2 Pt3 Cl4 135.2(4) . . . 2_665 ? N3 Pt2 Pt3 Cl4 45.7(4) . . . 2_665 ? N4 Pt2 Pt3 Cl4 -46.9(4) . . . 2_665 ? Pt1 Pt2 Pt3 Cl4 179.60(14) . . . 2_665 ? _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 19.00 _diffrn_measured_fraction_theta_full 0.916 _refine_diff_density_max 2.048 _refine_diff_density_min -1.480 _refine_diff_density_rms 0.226 # data_bi # REPLACEMENT CIF for Compound 1 _database_code_depnum_ccdc_archive 'CCDC 290178' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H32 N6 O2 Pt2, 2(Cl O4), 0.19(H2 O)' _chemical_formula_sum 'C10 H32.38 Cl2 N6 O10.19 Pt2' _chemical_formula_weight 860.90 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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 17.858(12) _cell_length_b 9.697(7) _cell_length_c 16.759(12) _cell_angle_alpha 90.00 _cell_angle_beta 105.043(8) _cell_angle_gamma 90.00 _cell_volume 2803(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.039 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1623.6 _exptl_absorpt_coefficient_mu 10.209 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2918 _exptl_absorpt_correction_T_max 0.5793 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 3980 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_sigmaI/netI 0.0532 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 4.83 _diffrn_reflns_theta_max 24.05 _reflns_number_total 1997 _reflns_number_gt 1727 _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. The t-butyl methyl groups at C2 and C6 are disordered. The disorder at the C2 (C3 C4 C3' C4') sited was modelled with two sets of equal occupancy sites - but there may be further disorder to produce a lumpy torus of density where we would expect to find methyl carbon atoms The disorder at the C6 site is not so severe and disorder was taken up by the anisotropic displacement parameters Because the cation lies about a mirror plane, there is equal disorder of N3/O8 and N4/O9 sites as well. A peak of low density in difference maps was allowed for as a partial occupancy [0.19(5)] water oxygen O7. No allowance was made for any H atoms bonded to O7 ; _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^)+(0.1310P)^2^] 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 1997 _refine_ls_number_parameters 165 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.0601 _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.1636 _refine_ls_wR_factor_gt 0.1586 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.029 _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 0.17276(2) 0.65592(4) 0.68622(2) 0.0398(3) Uani 1 1 d . . . N1 N 0.0666(5) 0.7080(11) 0.6139(6) 0.054(2) Uani 1 1 d . A . H1A H 0.0329 0.7125 0.6447 0.082 Uiso 1 1 calc R . . H1B H 0.0510 0.6445 0.5747 0.082 Uiso 1 1 calc R . . H1C H 0.0694 0.7896 0.5906 0.082 Uiso 1 1 calc R . . N2 N 0.2253(5) 0.7109(10) 0.5976(6) 0.052(2) Uani 1 1 d . A . H2A H 0.2241 0.8023 0.5923 0.078 Uiso 1 1 calc R . . H2B H 0.2005 0.6725 0.5498 0.078 Uiso 1 1 calc R . . H2C H 0.2743 0.6822 0.6117 0.078 Uiso 1 1 calc R . . N3 N 0.2774(5) 0.6169(10) 0.7612(6) 0.055(2) Uani 0.50 1 d P A 1 H3 H 0.3048 0.6877 0.7814 0.066 Uiso 0.50 1 calc PR A 1 N4 N 0.1244(7) 0.6147(10) 0.7783(7) 0.073(3) Uani 0.50 1 d P A 1 H4 H 0.1064 0.6853 0.7983 0.087 Uiso 0.50 1 calc PR A 1 O8 O 0.2774(5) 0.6169(10) 0.7612(6) 0.055(2) Uani 0.50 1 d P A 2 O9 O 0.1244(7) 0.6147(10) 0.7783(7) 0.073(3) Uani 0.50 1 d P A 2 C1 C 0.3083(8) 0.5000 0.7825(9) 0.048(4) Uani 1 2 d SD . . C2 C 0.3865(11) 0.5000 0.8487(13) 0.085(8) Uani 1 2 d SD . . C3 C 0.4209(16) 0.6459(18) 0.857(3) 0.21(4) Uani 0.50 1 d PD . . H3A H 0.3797 0.7124 0.8473 0.318 Uiso 0.50 1 calc PR A . H3B H 0.4508 0.6585 0.8178 0.318 Uiso 0.50 1 calc PR . . H3C H 0.4537 0.6582 0.9121 0.318 Uiso 0.50 1 calc PR . . C3' C 0.4426(14) 0.603(4) 0.825(3) 0.21(4) Uani 0.50 1 d PD . . H3'1 H 0.4689 0.5591 0.7890 0.318 Uiso 0.50 1 calc PR A . H3'2 H 0.4800 0.6328 0.8746 0.318 Uiso 0.50 1 calc PR . . H3'3 H 0.4141 0.6810 0.7982 0.318 Uiso 0.50 1 calc PR . . C4 C 0.370(2) 0.544(5) 0.9311(13) 0.28(7) Uani 0.50 1 d PD . . H4A H 0.3440 0.4706 0.9515 0.425 Uiso 0.50 1 calc PR A . H4B H 0.3372 0.6246 0.9221 0.425 Uiso 0.50 1 calc PR . . H4C H 0.4177 0.5651 0.9709 0.425 Uiso 0.50 1 calc PR . . C5 C 0.1160(11) 0.5000 0.8121(11) 0.056(4) Uani 1 2 d S . . C6 C 0.0902(13) 0.5000 0.8890(11) 0.086(8) Uani 1 2 d SD . . C7 C 0.0030(12) 0.5000 0.8715(18) 0.124(10) Uani 1 2 d SD . . H7A H -0.0117 0.5000 0.9227 0.186 Uiso 1 2 calc SR A . H7B H -0.0174 0.4192 0.8403 0.186 Uiso 0.50 1 calc PR . . H7C H -0.0174 0.5808 0.8403 0.186 Uiso 0.50 1 calc PR . . C8 C 0.1206(17) 0.6260(17) 0.9446(11) 0.133(10) Uani 1 1 d D . . H8A H 0.1017 0.6219 0.9933 0.200 Uiso 1 1 calc R A . H8B H 0.1027 0.7093 0.9148 0.200 Uiso 1 1 calc R . . H8C H 0.1763 0.6250 0.9603 0.200 Uiso 1 1 calc R . . Cl1 Cl 0.0924(2) 1.0000 0.4378(3) 0.0573(11) Uani 1 2 d S . . O1 O 0.0985(8) 0.8759(15) 0.4783(11) 0.129(5) Uani 1 1 d . . . O2 O 0.1466(8) 1.0000 0.3918(10) 0.082(4) Uani 1 2 d S . . O3 O 0.0153(8) 1.0000 0.3865(11) 0.098(5) Uani 1 2 d S . . Cl2 Cl 0.1174(2) 0.5000 0.3971(3) 0.0625(12) Uani 1 2 d S . . O4 O 0.1038(10) 0.6174(15) 0.3487(11) 0.132(5) Uani 1 1 d . . . O5 O 0.0702(10) 0.5000 0.4545(12) 0.097(5) Uani 1 2 d S . . O6 O 0.1983(9) 0.5000 0.4435(12) 0.103(5) Uani 1 2 d S . . O7 O 0.243(4) 1.0000 0.787(4) 0.07(3) Uiso 0.19(5) 2 d SP . . 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 0.0473(4) 0.0272(4) 0.0424(5) 0.00346(13) 0.0070(3) 0.00284(14) N1 0.049(5) 0.047(5) 0.065(7) 0.016(6) 0.010(4) 0.005(5) N2 0.050(5) 0.036(5) 0.069(7) 0.011(5) 0.015(4) -0.002(5) N3 0.064(6) 0.035(4) 0.049(6) -0.004(4) -0.015(4) 0.002(5) N4 0.123(9) 0.036(4) 0.075(8) -0.005(5) 0.056(7) 0.004(6) O8 0.064(6) 0.035(4) 0.049(6) -0.004(4) -0.015(4) 0.002(5) O9 0.123(9) 0.036(4) 0.075(8) -0.005(5) 0.056(7) 0.004(6) C1 0.046(9) 0.054(11) 0.034(9) 0.000 -0.005(6) 0.000 C2 0.070(13) 0.050(11) 0.097(18) 0.000 -0.048(12) 0.000 C3 0.08(3) 0.05(2) 0.41(8) -0.02(3) -0.10(4) -0.01(2) C3' 0.08(3) 0.05(2) 0.41(8) -0.02(3) -0.10(4) -0.01(2) C4 0.17(5) 0.50(18) 0.11(3) -0.14(7) -0.10(3) 0.18(9) C5 0.076(12) 0.038(10) 0.063(12) 0.000 0.032(9) 0.000 C6 0.19(3) 0.041(10) 0.051(13) 0.000 0.066(14) 0.000 C7 0.066(15) 0.19(3) 0.13(3) 0.000 0.053(16) 0.000 C8 0.26(3) 0.092(12) 0.060(13) -0.006(9) 0.071(16) -0.024(15) Cl1 0.050(2) 0.039(2) 0.086(3) 0.000 0.025(2) 0.000 O1 0.101(9) 0.120(10) 0.159(15) 0.071(10) 0.024(9) 0.006(8) O2 0.069(8) 0.084(9) 0.106(12) 0.000 0.049(8) 0.000 O3 0.068(9) 0.094(10) 0.132(15) 0.000 0.027(9) 0.000 Cl2 0.056(2) 0.046(2) 0.080(3) 0.000 0.007(2) 0.000 O4 0.146(12) 0.101(8) 0.143(14) 0.051(10) 0.027(10) 0.035(9) O5 0.090(11) 0.104(12) 0.109(14) 0.000 0.048(10) 0.000 O6 0.068(9) 0.124(13) 0.109(14) 0.000 0.009(8) 0.000 _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 N4 1.995(10) . ? Pt1 N3 1.999(9) . ? Pt1 N2 2.023(9) . ? Pt1 N1 2.031(9) . ? Pt1 Pt1 3.024(2) 6_565 ? N1 H1A 0.89 . ? N1 H1B 0.89 . ? N1 H1C 0.89 . ? N2 H2A 0.89 . ? N2 H2B 0.89 . ? N2 H2C 0.89 . ? N3 C1 1.271(11) . ? N3 H3 0.86 . ? N4 C5 1.275(13) . ? N4 H4 0.86 . ? C1 O8 1.271(11) 6_565 ? C1 N3 1.271(11) 6_565 ? C1 C2 1.542(19) . ? C2 C3' 1.534(17) . ? C2 C3' 1.534(16) 6_565 ? C2 C3 1.534(15) . ? C2 C3 1.534(15) 6_565 ? C2 C4 1.547(17) . ? C2 C4 1.547(17) 6_565 ? C3 H3A 0.96 . ? C3 H3B 0.96 . ? C3 H3C 0.96 . ? C3' H3'1 0.96 . ? C3' H3'2 0.96 . ? C3' H3'3 0.96 . ? C4 H4A 0.96 . ? C4 H4B 0.96 . ? C4 H4C 0.96 . ? C5 O9 1.275(13) 6_565 ? C5 N4 1.275(13) 6_565 ? C5 C6 1.48(2) . ? C6 C7 1.508(18) . ? C6 C8 1.547(16) . ? C6 C8 1.547(16) 6_565 ? C7 H7A 0.96 . ? C7 H7B 0.96 . ? C7 H7C 0.96 . ? C8 H8A 0.96 . ? C8 H8B 0.96 . ? C8 H8C 0.96 . ? Cl1 O1 1.372(12) 6_575 ? Cl1 O1 1.372(12) . ? Cl1 O2 1.385(13) . ? Cl1 O3 1.422(16) . ? Cl2 O4 1.382(13) 6_565 ? Cl2 O4 1.382(13) . ? Cl2 O5 1.434(17) . ? Cl2 O6 1.452(16) . ? 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 N4 Pt1 N3 89.9(5) . . ? N4 Pt1 N2 175.6(4) . . ? N3 Pt1 N2 88.6(4) . . ? N4 Pt1 N1 89.3(5) . . ? N3 Pt1 N1 176.2(4) . . ? N2 Pt1 N1 92.0(4) . . ? N4 Pt1 Pt1 78.4(3) . 6_565 ? N3 Pt1 Pt1 79.1(3) . 6_565 ? N2 Pt1 Pt1 105.3(3) . 6_565 ? N1 Pt1 Pt1 104.4(3) . 6_565 ? Pt1 N1 H1A 109.5 . . ? Pt1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? Pt1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? Pt1 N2 H2A 109.5 . . ? Pt1 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? Pt1 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? C1 N3 Pt1 127.8(8) . . ? C1 N3 H3 116.1 . . ? Pt1 N3 H3 116.1 . . ? C5 N4 Pt1 130.1(9) . . ? C5 N4 H4 115.0 . . ? Pt1 N4 H4 115.0 . . ? O8 C1 N3 126.2(13) 6_565 . ? N3 C1 N3 126.2(13) 6_565 . ? O8 C1 C2 116.7(7) 6_565 . ? N3 C1 C2 116.7(7) 6_565 . ? N3 C1 C2 116.7(7) . . ? C3' C2 C3 110.6(11) 6_565 . ? C3' C2 C3 110.6(11) . 6_565 ? C3 C2 C3 135(2) . 6_565 ? C3' C2 C1 110.3(11) . . ? C3' C2 C1 110.3(11) 6_565 . ? C3 C2 C1 109.4(8) . . ? C3 C2 C1 109.4(8) 6_565 . ? C3' C2 C4 109.7(11) . . ? C3' C2 C4 134(2) 6_565 . ? C3 C2 C4 80(4) . . ? C3 C2 C4 109.8(11) 6_565 . ? C1 C2 C4 107.1(13) . . ? C3' C2 C4 134(2) . 6_565 ? C3' C2 C4 109.7(11) 6_565 6_565 ? C3 C2 C4 109.8(11) . 6_565 ? C3 C2 C4 80(4) 6_565 6_565 ? C1 C2 C4 107.1(13) . 6_565 ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C3' H3'1 109.5 . . ? C2 C3' H3'2 109.5 . . ? H3'1 C3' H3'2 109.5 . . ? C2 C3' H3'3 109.5 . . ? H3'1 C3' H3'3 109.5 . . ? H3'2 C3' H3'3 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O9 C5 N4 121.5(16) 6_565 . ? N4 C5 N4 121.5(16) 6_565 . ? O9 C5 C6 119.2(8) 6_565 . ? N4 C5 C6 119.2(8) 6_565 . ? N4 C5 C6 119.2(8) . . ? C5 C6 C7 111.7(18) . . ? C5 C6 C8 112.7(12) . . ? C7 C6 C8 107.5(15) . . ? C5 C6 C8 112.7(12) . 6_565 ? C7 C6 C8 107.5(15) . 6_565 ? C8 C6 C8 104(2) . 6_565 ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O1 Cl1 O1 122.7(17) 6_575 . ? O1 Cl1 O2 107.4(8) 6_575 . ? O1 Cl1 O2 107.4(8) . . ? O1 Cl1 O3 103.8(7) 6_575 . ? O1 Cl1 O3 103.8(7) . . ? O2 Cl1 O3 111.7(11) . . ? O4 Cl2 O4 110.9(16) 6_565 . ? O4 Cl2 O5 110.4(9) 6_565 . ? O4 Cl2 O5 110.4(9) . . ? O4 Cl2 O6 108.2(9) 6_565 . ? O4 Cl2 O6 108.2(9) . . ? O5 Cl2 O6 108.5(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Pt1 N3 C1 78.9(12) . . . . ? N2 Pt1 N3 C1 -105.2(12) . . . . ? N1 Pt1 N3 C1 156(5) . . . . ? Pt1 Pt1 N3 C1 0.7(12) 6_565 . . . ? N3 Pt1 N4 C5 -71.3(16) . . . . ? N2 Pt1 N4 C5 -141(5) . . . . ? N1 Pt1 N4 C5 112.4(16) . . . . ? Pt1 Pt1 N4 C5 7.5(15) 6_565 . . . ? Pt1 N3 C1 O8 -2(3) . . . 6_565 ? Pt1 N3 C1 N3 -2(3) . . . 6_565 ? Pt1 N3 C1 C2 -173.6(12) . . . . ? O8 C1 C2 C3' 137(2) 6_565 . . . ? N3 C1 C2 C3' 137(2) 6_565 . . . ? N3 C1 C2 C3' -50(2) . . . . ? O8 C1 C2 C3' 50(2) 6_565 . . 6_565 ? N3 C1 C2 C3' 50(2) 6_565 . . 6_565 ? N3 C1 C2 C3' -137(2) . . . 6_565 ? O8 C1 C2 C3 172(2) 6_565 . . . ? N3 C1 C2 C3 172(2) 6_565 . . . ? N3 C1 C2 C3 -16(3) . . . . ? O8 C1 C2 C3 16(3) 6_565 . . 6_565 ? N3 C1 C2 C3 16(3) 6_565 . . 6_565 ? N3 C1 C2 C3 -172(2) . . . 6_565 ? O8 C1 C2 C4 -103(2) 6_565 . . . ? N3 C1 C2 C4 -103(2) 6_565 . . . ? N3 C1 C2 C4 70(2) . . . . ? O8 C1 C2 C4 -70(2) 6_565 . . 6_565 ? N3 C1 C2 C4 -70(2) 6_565 . . 6_565 ? N3 C1 C2 C4 103(2) . . . 6_565 ? Pt1 N4 C5 O9 -15(3) . . . 6_565 ? Pt1 N4 C5 N4 -15(3) . . . 6_565 ? Pt1 N4 C5 C6 169.5(13) . . . . ? O9 C5 C6 C7 -87.7(16) 6_565 . . . ? N4 C5 C6 C7 -87.7(16) 6_565 . . . ? N4 C5 C6 C7 87.7(16) . . . . ? O9 C5 C6 C8 151.1(19) 6_565 . . . ? N4 C5 C6 C8 151.1(19) 6_565 . . . ? N4 C5 C6 C8 -33(3) . . . . ? O9 C5 C6 C8 33(3) 6_565 . . 6_565 ? N4 C5 C6 C8 33(3) 6_565 . . 6_565 ? N4 C5 C6 C8 -151.1(19) . . . 6_565 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O4 0.89 2.64 3.379(19) 141.2 2_556 N1 H1B O5 0.89 2.52 3.145(17) 128.1 5_566 N1 H1B O5 0.89 2.55 3.361(18) 152.0 . N1 H1C O1 0.89 2.24 2.968(17) 138.8 . N2 H2A O6 0.89 2.53 3.269(13) 141.2 7_566 N2 H2B O6 0.89 2.44 3.231(18) 148.8 . N2 H2C O2 0.89 2.27 3.040(13) 144.3 7_566 _diffrn_measured_fraction_theta_max 0.842 _diffrn_reflns_theta_full 24.05 _diffrn_measured_fraction_theta_full 0.842 _refine_diff_density_max 3.031 # Adjacent to Pt1 _refine_diff_density_min -1.593 # Adjacent to Pt1 _refine_diff_density_rms 0.276 # End of B516410A revised CIF ##########################################################