Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Che, Chi-Ming' 'Lu, Wei' 'Zhu, Nianyong' _publ_contact_author_name 'Prof Chi-Ming Che' _publ_contact_author_address ; Department of Chemistry The University of Hong Kong, Pokful Hong Kong SAR CHINA ; _publ_contact_author_email 'CMCHE@HKU.HK' _publ_section_title ; Tethered trinuclear cyclometalated platinum(II) complexes: from crystal engineering to tunable photoluminescence ; data_mar373 _database_code_CSD 178372 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Complex 1(ClO4)3' ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C100 H100 P3 Pt3' _chemical_formula_sum 'C89 H72 Cl3 N6 O12 P3 Pt3' _chemical_formula_weight 2202.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 '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' 'O' 'O' 0.0106 0.0060 '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' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P 63/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x-y, z' '-x+y, -x, z' 'x-y, x, z+1/2' 'y, -x+y, z+1/2' '-x, -y, -z' 'x, y, -z-1/2' 'y, -x+y, -z' 'x-y, x, -z' '-x+y, -x, -z-1/2' '-y, x-y, -z-1/2' _cell_length_a 14.536(2) _cell_length_b 14.536(2) _cell_length_c 23.211(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4247.3(12) _cell_formula_units_Z 2 _cell_measurement_temperature 301(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.722 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2148 _exptl_absorpt_coefficient_mu 5.144 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 301(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28507 _diffrn_reflns_av_R_equivalents 0.0608 _diffrn_reflns_av_sigmaI/netI 0.0379 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 25.63 _reflns_number_total 2733 _reflns_number_gt 2140 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0583P)^2^+38.6135P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2733 _refine_ls_number_parameters 177 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0683 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1517 _refine_ls_wR_factor_gt 0.1454 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.095 _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 0.37997(4) 0.30711(4) 0.2500 0.0477(2) Uani 1 2 d S . . P1 P 0.4324(4) 0.1859(4) 0.2382(3) 0.047(3) Uani 0.50 1 d P . . N1 N 0.3135(9) 0.3997(10) 0.2500 0.056(3) Uani 1 2 d S . . C1 C 0.3601(18) 0.3158(19) 0.3427(10) 0.039(5) Uiso 0.50 1 d P A 1 C2 C 0.3127(19) 0.371(2) 0.3564(10) 0.053(6) Uiso 0.50 1 d P A 1 C3 C 0.2934(19) 0.3863(19) 0.4079(11) 0.064(6) Uiso 0.50 1 d P A 1 H3 H 0.2552 0.4211 0.4140 0.076 Uiso 0.50 1 calc PR A 1 C4 C 0.325(3) 0.355(3) 0.4521(16) 0.098(9) Uiso 0.50 1 d P A 1 H4 H 0.3157 0.3729 0.4894 0.118 Uiso 0.50 1 calc PR A 1 C5 C 0.376(2) 0.290(2) 0.4407(13) 0.076(7) Uiso 0.50 1 d P A 1 H5 H 0.3957 0.2606 0.4703 0.091 Uiso 0.50 1 calc PR A 1 C6 C 0.3912(18) 0.2765(19) 0.3855(10) 0.055(5) Uiso 0.50 1 d P A 1 H6 H 0.4248 0.2381 0.3765 0.066 Uiso 0.50 1 calc PR A 1 C7 C 0.2903(10) 0.4265(10) 0.2996(6) 0.070(3) Uani 1 1 d . . . C8 C 0.2334(11) 0.4817(11) 0.2999(8) 0.097(5) Uani 1 1 d . A . H8 H 0.2155 0.5003 0.3348 0.117 Uiso 1 1 calc R . . C9 C 0.2052(16) 0.5074(18) 0.2500 0.090(6) Uani 1 2 d S . . H9 H 0.1665 0.5426 0.2500 0.108 Uiso 1 2 calc SR A . C16 C 0.6667 0.3333 0.2500 0.046(5) Uani 1 6 d S . . C15 C 0.5707(15) 0.2295(16) 0.2191(9) 0.055(5) Uani 0.50 1 d P . . C17 C 0.6667 0.3333 0.3100(18) 0.064(10) Uani 0.50 3 d SP . . C18 C 0.362(2) 0.0951(19) 0.1831(11) 0.054(5) Uiso 0.50 1 d P . 1 C19 C 0.252(2) 0.0646(19) 0.1731(11) 0.065(6) Uiso 0.50 1 d P . 1 H19 H 0.2265 0.1024 0.1931 0.078 Uiso 0.50 1 calc PR . 1 C20 C 0.182(3) -0.015(2) 0.1369(14) 0.093(9) Uiso 0.50 1 d P . 1 H20 H 0.1093 -0.0391 0.1367 0.111 Uiso 0.50 1 calc PR . 1 C21 C 0.228(2) -0.055(2) 0.1017(14) 0.087(8) Uiso 0.50 1 d P . 1 H21 H 0.1891 -0.0947 0.0700 0.105 Uiso 0.50 1 calc PR . 1 C22 C 0.335(3) -0.041(3) 0.1102(17) 0.084(12) Uiso 0.50 1 d P . 1 H22 H 0.3591 -0.0809 0.0910 0.101 Uiso 0.50 1 calc PR . 1 C23 C 0.395(2) 0.037(2) 0.1489(12) 0.070(6) Uiso 0.50 1 d P . 1 H23 H 0.4653 0.0532 0.1531 0.084 Uiso 0.50 1 calc PR . 1 Cl1 Cl 0.6667 0.3333 0.4846(7) 0.094(4) Uiso 0.50 3 d SPD . 1 O1 O 0.6667 0.3333 0.5399(16) 0.094(4) Uiso 0.50 3 d SPD B 1 O2 O 0.580(3) 0.250(3) 0.4675(16) 0.189(13) Uiso 0.50 1 d PD C 1 Cl1' Cl 0.6667 0.3333 0.5274(13) 0.150(8) Uiso 0.50 3 d SPD . 2 O1' O 0.6667 0.3333 0.4664(18) 0.150(8) Uiso 0.50 3 d SPD D 2 O2' O 0.6561(18) 0.2348(18) 0.5450(11) 0.116(7) Uiso 0.50 1 d PD E 2 Cl2 Cl 0.0000 0.0000 0.2070(7) 0.104(4) Uiso 0.50 3 d SP . . O3 O 0.0000 0.0000 0.2500 0.27(3) Uiso 1 6 d S . . O4 O 0.080(3) 0.101(3) 0.1920(15) 0.183(13) Uiso 0.50 1 d P . . C24 C 0.398(2) 0.099(2) 0.2982(12) 0.063(7) Uiso 0.50 1 d P . 2 C25 C 0.300(3) 0.059(2) 0.3194(12) 0.073(7) Uiso 0.50 1 d P . 2 H25 H 0.2528 0.0696 0.2975 0.087 Uiso 0.50 1 calc PR . 2 C26 C 0.260(3) 0.002(2) 0.3704(14) 0.086(8) Uiso 0.50 1 d P . 2 H26 H 0.1919 -0.0188 0.3835 0.104 Uiso 0.50 1 calc PR . 2 C27 C 0.325(2) -0.022(2) 0.3996(14) 0.061(8) Uiso 0.50 1 d P . 2 H27 H 0.3004 -0.0647 0.4322 0.073 Uiso 0.50 1 calc PR . 2 C28 C 0.433(2) 0.017(2) 0.3815(12) 0.073(6) Uiso 0.50 1 d P . 2 H28 H 0.4789 0.0039 0.4031 0.088 Uiso 0.50 1 calc PR . 2 C29 C 0.4662(19) 0.0749(18) 0.3309(10) 0.062(5) Uiso 0.50 1 d P . 2 H29 H 0.5350 0.0985 0.3178 0.075 Uiso 0.50 1 calc PR . 2 N2 N 0.382(2) 0.343(2) 0.1670(12) 0.075(9) Uiso 0.50 1 d P . 2 C10 C 0.4305(19) 0.3213(19) 0.1176(10) 0.055(6) Uiso 0.50 1 d P . 2 H10 H 0.4596 0.2774 0.1218 0.066 Uiso 0.50 1 calc PR . 2 C11 C 0.433(2) 0.366(2) 0.0644(12) 0.073(6) Uiso 0.50 1 d P . 2 H11 H 0.4659 0.3533 0.0333 0.088 Uiso 0.50 1 calc PR . 2 C12 C 0.388(2) 0.428(2) 0.0578(12) 0.074(7) Uiso 0.50 1 d P . 2 H12 H 0.3870 0.4536 0.0212 0.088 Uiso 0.50 1 calc PR . 2 C13 C 0.348(2) 0.451(2) 0.0978(11) 0.070(6) Uiso 0.50 1 d P . 2 H13 H 0.3216 0.4961 0.0908 0.083 Uiso 0.50 1 calc PR . 2 C14 C 0.340(2) 0.410(2) 0.1555(11) 0.058(6) Uiso 0.50 1 d P . 2 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 0.0444(3) 0.0501(3) 0.0506(3) 0.000 0.000 0.0252(3) P1 0.042(2) 0.046(2) 0.056(8) 0.000(2) -0.003(2) 0.0237(18) N1 0.037(6) 0.058(7) 0.076(9) 0.000 0.000 0.026(6) C7 0.073(7) 0.070(7) 0.084(9) -0.009(6) -0.002(6) 0.048(6) C8 0.083(9) 0.088(10) 0.147(15) -0.028(10) 0.000(9) 0.062(9) C9 0.081(13) 0.119(17) 0.115(17) 0.000 0.000 0.084(14) C16 0.045(8) 0.045(8) 0.048(14) 0.000 0.000 0.022(4) C15 0.038(10) 0.050(11) 0.069(13) 0.000(10) -0.005(9) 0.016(9) C17 0.062(14) 0.062(14) 0.07(3) 0.000 0.000 0.031(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 N2 1.99(3) . ? Pt1 N2 1.99(3) 8_556 ? Pt1 N1 2.011(12) . ? Pt1 C1 2.18(2) 8_556 ? Pt1 C1 2.18(2) . ? Pt1 P1 2.260(5) . ? Pt1 P1 2.260(5) 8_556 ? P1 P1 0.550(16) 8_556 ? P1 C24 1.38(3) 8_556 ? P1 C18 1.75(3) . ? P1 C24 1.77(3) . ? P1 C15 1.83(2) . ? P1 C15 2.04(2) 8_556 ? P1 C18 2.19(3) 8_556 ? P1 C25 2.31(3) 8_556 ? N1 C7 1.313(13) 8_556 ? N1 C7 1.313(13) . ? C1 C6 1.33(3) . ? C1 C2 1.33(3) . ? C2 C3 1.27(3) . ? C2 C7 1.66(3) . ? C3 C4 1.29(4) . ? C4 C5 1.49(4) . ? C5 C6 1.33(4) . ? C7 C14 1.36(3) 8_556 ? C7 C8 1.411(16) . ? C8 C9 1.344(18) . ? C9 C8 1.344(18) 8_556 ? C16 C17 1.39(4) 8_556 ? C16 C17 1.39(4) . ? C16 C15 1.623(19) 3_655 ? C16 C15 1.623(19) 12_656 ? C16 C15 1.623(19) . ? C16 C15 1.623(19) 8_556 ? C16 C15 1.623(19) 4_665 ? C16 C15 1.623(19) 11_666 ? C15 C15 1.43(4) 8_556 ? C15 C17 1.61(3) 8_556 ? C15 P1 2.04(2) 8_556 ? C17 C15 1.61(3) 12_656 ? C17 C15 1.61(3) 8_556 ? C17 C15 1.61(3) 11_666 ? C18 C23 1.40(3) . ? C18 C19 1.45(4) . ? C18 P1 2.19(3) 8_556 ? C19 C20 1.38(4) . ? C20 C21 1.36(4) . ? C21 C22 1.48(5) . ? C22 C23 1.36(5) . ? Cl1 O1 1.28(3) . ? Cl1 O2 1.30(3) 3_655 ? Cl1 O2 1.30(3) . ? Cl1 O2 1.30(3) 4_665 ? Cl1' O1' 1.42(3) . ? Cl1' O2' 1.42(2) . ? Cl1' O2' 1.42(2) 3_655 ? Cl1' O2' 1.42(2) 4_665 ? Cl2 O3 0.998(17) . ? Cl2 O4 1.39(3) 3 ? Cl2 O4 1.39(3) . ? Cl2 O4 1.39(3) 4 ? Cl2 Cl2 2.00(3) 8_556 ? O3 Cl2 0.998(17) 8_556 ? C24 C25 1.33(4) . ? C24 P1 1.38(3) 8_556 ? C24 C29 1.43(3) . ? C25 C26 1.40(4) . ? C25 P1 2.31(3) 8_556 ? C26 C27 1.35(4) . ? C27 C28 1.43(4) . ? C28 C29 1.38(3) . ? N2 C14 1.41(4) . ? N2 C10 1.45(3) . ? C10 C11 1.38(3) . ? C11 C12 1.37(3) . ? C12 C13 1.23(3) . ? C13 C14 1.45(4) . ? C14 C7 1.36(3) 8_556 ? 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 N2 Pt1 N2 150.8(16) . 8_556 ? N2 Pt1 N1 77.2(8) . . ? N2 Pt1 N1 77.2(8) 8_556 . ? N2 Pt1 C1 10.5(10) . 8_556 ? N2 Pt1 C1 157.6(8) 8_556 8_556 ? N1 Pt1 C1 80.8(6) . 8_556 ? N2 Pt1 C1 157.6(8) . . ? N2 Pt1 C1 10.5(10) 8_556 . ? N1 Pt1 C1 80.8(6) . . ? C1 Pt1 C1 160.6(11) 8_556 . ? N2 Pt1 P1 96.7(8) . . ? N2 Pt1 P1 110.6(8) 8_556 . ? N1 Pt1 P1 169.8(3) . . ? C1 Pt1 P1 91.8(6) 8_556 . ? C1 Pt1 P1 105.7(6) . . ? N2 Pt1 P1 110.6(8) . 8_556 ? N2 Pt1 P1 96.7(8) 8_556 8_556 ? N1 Pt1 P1 169.8(3) . 8_556 ? C1 Pt1 P1 105.7(6) 8_556 8_556 ? C1 Pt1 P1 91.8(6) . 8_556 ? P1 Pt1 P1 14.0(4) . 8_556 ? P1 P1 C24 127.5(12) 8_556 8_556 ? P1 P1 C18 136.9(8) 8_556 . ? C24 P1 C18 20.0(12) 8_556 . ? P1 P1 C24 38.3(9) 8_556 . ? C24 P1 C24 89(2) 8_556 . ? C18 P1 C24 100.7(10) . . ? P1 P1 C15 104.0(7) 8_556 . ? C24 P1 C15 90.3(13) 8_556 . ? C18 P1 C15 102.0(11) . . ? C24 P1 C15 107.9(11) . . ? P1 P1 C15 60.9(6) 8_556 8_556 ? C24 P1 C15 115.7(13) 8_556 8_556 ? C18 P1 C15 134.5(11) . 8_556 ? C24 P1 C15 74.0(10) . 8_556 ? C15 P1 C15 43.1(12) . 8_556 ? P1 P1 C18 33.2(7) 8_556 8_556 ? C24 P1 C18 96.4(11) 8_556 8_556 ? C18 P1 C18 103.6(15) . 8_556 ? C24 P1 C18 14.8(10) . 8_556 ? C15 P1 C18 120.7(10) . 8_556 ? C15 P1 C18 82.5(10) 8_556 8_556 ? P1 P1 Pt1 83.0(2) 8_556 . ? C24 P1 Pt1 132.3(12) 8_556 . ? C18 P1 Pt1 112.4(9) . . ? C24 P1 Pt1 111.8(10) . . ? C15 P1 Pt1 119.9(7) . . ? C15 P1 Pt1 111.3(6) 8_556 . ? C18 P1 Pt1 97.6(7) 8_556 . ? P1 P1 C25 125.3(8) 8_556 8_556 ? C24 P1 C25 30.9(13) 8_556 8_556 ? C18 P1 C25 15.9(10) . 8_556 ? C24 P1 C25 93.3(11) . 8_556 ? C15 P1 C25 117.9(11) . 8_556 ? C15 P1 C25 145.8(10) 8_556 8_556 ? C18 P1 C25 92.8(10) 8_556 8_556 ? Pt1 P1 C25 102.9(8) . 8_556 ? C7 N1 C7 122.6(14) 8_556 . ? C7 N1 Pt1 118.6(7) 8_556 . ? C7 N1 Pt1 118.6(7) . . ? C6 C1 C2 118(2) . . ? C6 C1 Pt1 128.9(17) . . ? C2 C1 Pt1 113.2(17) . . ? C3 C2 C1 124(2) . . ? C3 C2 C7 123(2) . . ? C1 C2 C7 112.9(19) . . ? C2 C3 C4 123(3) . . ? C3 C4 C5 117(3) . . ? C6 C5 C4 116(3) . . ? C1 C6 C5 122(2) . . ? N1 C7 C14 112.2(14) . 8_556 ? N1 C7 C8 119.0(13) . . ? C14 C7 C8 128.1(16) 8_556 . ? N1 C7 C2 114.2(11) . . ? C14 C7 C2 18.7(13) 8_556 . ? C8 C7 C2 125.8(14) . . ? C9 C8 C7 120.1(15) . . ? C8 C9 C8 119.3(17) 8_556 . ? C17 C16 C17 180.000(5) 8_556 . ? C17 C16 C15 63.8(8) 8_556 3_655 ? C17 C16 C15 116.2(8) . 3_655 ? C17 C16 C15 116.2(8) 8_556 12_656 ? C17 C16 C15 63.8(8) . 12_656 ? C15 C16 C15 52.5(15) 3_655 12_656 ? C17 C16 C15 63.8(8) 8_556 . ? C17 C16 C15 116.2(8) . . ? C15 C16 C15 102.0(9) 3_655 . ? C15 C16 C15 126.7(4) 12_656 . ? C17 C16 C15 116.2(8) 8_556 8_556 ? C17 C16 C15 63.8(8) . 8_556 ? C15 C16 C15 126.7(4) 3_655 8_556 ? C15 C16 C15 102.0(9) 12_656 8_556 ? C15 C16 C15 52.5(15) . 8_556 ? C17 C16 C15 63.8(8) 8_556 4_665 ? C17 C16 C15 116.2(8) . 4_665 ? C15 C16 C15 102.0(9) 3_655 4_665 ? C15 C16 C15 126.7(4) 12_656 4_665 ? C15 C16 C15 102.0(9) . 4_665 ? C15 C16 C15 126.7(4) 8_556 4_665 ? C17 C16 C15 116.2(8) 8_556 11_666 ? C17 C16 C15 63.8(8) . 11_666 ? C15 C16 C15 126.7(4) 3_655 11_666 ? C15 C16 C15 102.0(9) 12_656 11_666 ? C15 C16 C15 126.7(4) . 11_666 ? C15 C16 C15 102.0(9) 8_556 11_666 ? C15 C16 C15 52.5(15) 4_665 11_666 ? C15 C15 C17 114.9(16) 8_556 8_556 ? C15 C15 C16 63.8(8) 8_556 . ? C17 C15 C16 51.1(15) 8_556 . ? C15 C15 P1 76.0(7) 8_556 . ? C17 C15 P1 135.6(13) 8_556 . ? C16 C15 P1 120.0(12) . . ? C15 C15 P1 60.9(6) 8_556 8_556 ? C17 C15 P1 139.2(13) 8_556 8_556 ? C16 C15 P1 109.3(11) . 8_556 ? P1 C15 P1 15.2(5) . 8_556 ? C16 C17 C15 65.1(16) . 12_656 ? C16 C17 C15 65.1(16) . 8_556 ? C15 C17 C15 103.5(18) 12_656 8_556 ? C16 C17 C15 65.1(16) . 11_666 ? C15 C17 C15 103.5(18) 12_656 11_666 ? C15 C17 C15 103.5(18) 8_556 11_666 ? C23 C18 C19 112(2) . . ? C23 C18 P1 128(2) . . ? C19 C18 P1 118.9(17) . . ? C23 C18 P1 130(2) . 8_556 ? C19 C18 P1 115.3(16) . 8_556 ? P1 C18 P1 9.9(4) . 8_556 ? C20 C19 C18 127(3) . . ? C21 C20 C19 114(3) . . ? C20 C21 C22 125(3) . . ? C23 C22 C21 113(3) . . ? C22 C23 C18 127(3) . . ? O1 Cl1 O2 107.8(19) . 3_655 ? O1 Cl1 O2 107.8(19) . . ? O2 Cl1 O2 111.1(17) 3_655 . ? O1 Cl1 O2 107.8(19) . 4_665 ? O2 Cl1 O2 111.1(17) 3_655 4_665 ? O2 Cl1 O2 111.1(17) . 4_665 ? O1' Cl1' O2' 106.7(16) . . ? O1' Cl1' O2' 106.7(16) . 3_655 ? O2' Cl1' O2' 112.1(14) . 3_655 ? O1' Cl1' O2' 106.7(16) . 4_665 ? O2' Cl1' O2' 112.1(14) . 4_665 ? O2' Cl1' O2' 112.1(14) 3_655 4_665 ? O3 Cl2 O4 104.6(17) . 3 ? O3 Cl2 O4 104.6(17) . . ? O4 Cl2 O4 113.9(14) 3 . ? O3 Cl2 O4 104.6(17) . 4 ? O4 Cl2 O4 113.9(14) 3 4 ? O4 Cl2 O4 113.9(14) . 4 ? O3 Cl2 Cl2 0.000(1) . 8_556 ? O4 Cl2 Cl2 104.6(17) 3 8_556 ? O4 Cl2 Cl2 104.6(17) . 8_556 ? O4 Cl2 Cl2 104.6(17) 4 8_556 ? Cl2 O3 Cl2 180.000(5) . 8_556 ? C25 C24 P1 117(2) . 8_556 ? C25 C24 C29 115(2) . . ? P1 C24 C29 125(2) 8_556 . ? C25 C24 P1 118(2) . . ? P1 C24 P1 14.2(6) 8_556 . ? C29 C24 P1 127(2) . . ? C24 C25 C26 128(3) . . ? C24 C25 P1 32.3(13) . 8_556 ? C26 C25 P1 154(3) . 8_556 ? C27 C26 C25 116(3) . . ? C26 C27 C28 121(3) . . ? C29 C28 C27 118(3) . . ? C28 C29 C24 122(2) . . ? C14 N2 C10 115(2) . . ? C14 N2 Pt1 113.9(19) . . ? C10 N2 Pt1 130.8(19) . . ? C11 C10 N2 120(2) . . ? C12 C11 C10 120(2) . . ? C13 C12 C11 123(3) . . ? C12 C13 C14 123(3) . . ? C7 C14 N2 116(2) 8_556 . ? C7 C14 C13 125(2) 8_556 . ? N2 C14 C13 119(2) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.63 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.967 _refine_diff_density_min -0.950 _refine_diff_density_rms 0.157 #===END data_mar216 _database_code_CSD 178373 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Complex 2(ClO4)3.H2O' ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C90 H90 P3 Pt3' _chemical_formula_sum 'C80 H64 Cl3 N6 O13 P3 Pt3' _chemical_formula_weight 2101.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 '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' 'O' 'O' 0.0106 0.0060 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 15.592(3) _cell_length_b 12.671(3) _cell_length_c 38.474(8) _cell_angle_alpha 90.00 _cell_angle_beta 92.92(3) _cell_angle_gamma 90.00 _cell_volume 7591(3) _cell_formula_units_Z 4 _cell_measurement_temperature 301(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour 'deep red' _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.839 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4080 _exptl_absorpt_coefficient_mu 5.752 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 301(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17209 _diffrn_reflns_av_R_equivalents 0.0711 _diffrn_reflns_av_sigmaI/netI 0.1189 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 25.56 _reflns_number_total 10070 _reflns_number_gt 6027 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0697P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10070 _refine_ls_number_parameters 965 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0794 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1438 _refine_ls_wR_factor_gt 0.1196 _refine_ls_goodness_of_fit_ref 0.880 _refine_ls_restrained_S_all 0.880 _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 0.46322(3) 0.13966(4) 0.179355(12) 0.04083(15) Uani 1 1 d . . . Pt2 Pt 0.28596(3) 0.11705(3) 0.134602(11) 0.03948(14) Uani 1 1 d . . . Pt3 Pt 0.12041(3) 0.11105(4) 0.073654(13) 0.04628(16) Uani 1 1 d . . . P1 P 0.5410(2) 0.1309(2) 0.13137(8) 0.0386(7) Uani 1 1 d . . . P2 P 0.3613(2) 0.1708(2) 0.08910(8) 0.0386(7) Uani 1 1 d . . . P3 P 0.2134(2) 0.1244(2) 0.03079(8) 0.0432(8) Uani 1 1 d . . . N1 N 0.4597(6) -0.0203(8) 0.1981(3) 0.049(3) Uani 1 1 d . . . N2 N 0.3948(6) 0.1523(9) 0.2227(3) 0.050(3) Uani 1 1 d . . . N3 N 0.2280(7) 0.2579(8) 0.1575(3) 0.051(3) Uani 1 1 d . . . N4 N 0.2161(6) 0.0578(8) 0.1720(3) 0.046(3) Uani 1 1 d . . . N5 N 0.1290(7) -0.0570(8) 0.0839(3) 0.051(3) Uani 1 1 d . . . N6 N 0.0392(7) 0.0926(10) 0.1119(3) 0.058(3) Uani 1 1 d . . . C1 C 0.4457(8) 0.2998(10) 0.1794(4) 0.050(3) Uani 1 1 d . . . C2 C 0.4728(8) 0.3728(11) 0.1568(4) 0.060(4) Uani 1 1 d . . . H2 H 0.5030 0.3524 0.1377 0.072 Uiso 1 1 calc R . . C3 C 0.4545(10) 0.4805(11) 0.1626(5) 0.082(5) Uani 1 1 d . . . H3 H 0.4737 0.5311 0.1473 0.099 Uiso 1 1 calc R . . C4 C 0.4078(11) 0.5123(13) 0.1911(5) 0.088(6) Uani 1 1 d . . . H4 H 0.3947 0.5830 0.1947 0.105 Uiso 1 1 calc R . . C5 C 0.3825(10) 0.4361(12) 0.2133(4) 0.072(4) Uani 1 1 d . . . H5 H 0.3532 0.4561 0.2327 0.086 Uiso 1 1 calc R . . C6 C 0.3985(8) 0.3315(10) 0.2082(4) 0.051(3) Uani 1 1 d . . . C7 C 0.3679(9) 0.2511(11) 0.2309(4) 0.061(4) Uani 1 1 d . . . C8 C 0.3152(10) 0.2668(15) 0.2592(4) 0.086(6) Uani 1 1 d . . . H8 H 0.2938 0.3328 0.2648 0.103 Uiso 1 1 calc R . . C9 C 0.2974(11) 0.1750(15) 0.2784(5) 0.094(6) Uani 1 1 d . . . H9 H 0.2635 0.1808 0.2975 0.112 Uiso 1 1 calc R . . C10 C 0.3279(10) 0.0792(14) 0.2700(4) 0.083(5) Uani 1 1 d . . . H10 H 0.3151 0.0207 0.2833 0.100 Uiso 1 1 calc R . . C11 C 0.3773(9) 0.0674(12) 0.2419(3) 0.059(4) Uani 1 1 d . . . C12 C 0.4131(8) -0.0288(11) 0.2277(4) 0.053(4) Uani 1 1 d . . . C13 C 0.4041(10) -0.1221(12) 0.2438(4) 0.076(5) Uani 1 1 d . . . H13 H 0.3736 -0.1254 0.2639 0.091 Uiso 1 1 calc R . . C14 C 0.4393(10) -0.2135(13) 0.2308(4) 0.078(5) Uani 1 1 d . . . H14 H 0.4330 -0.2783 0.2417 0.094 Uiso 1 1 calc R . . C15 C 0.4846(10) -0.2042(11) 0.2006(4) 0.073(5) Uani 1 1 d . . . H15 H 0.5091 -0.2638 0.1911 0.088 Uiso 1 1 calc R . . C16 C 0.4933(9) -0.1091(10) 0.1850(4) 0.058(4) Uani 1 1 d . . . H16 H 0.5233 -0.1050 0.1647 0.070 Uiso 1 1 calc R . . C17 C 0.3140(8) -0.0406(9) 0.1298(3) 0.044(3) Uani 1 1 d . . . C18 C 0.3655(7) -0.0947(8) 0.1073(3) 0.041(3) Uani 1 1 d . . . H18 H 0.3931 -0.0574 0.0903 0.049 Uiso 1 1 calc R . . C19 C 0.3769(8) -0.2037(10) 0.1097(4) 0.059(4) Uani 1 1 d . . . H19 H 0.4120 -0.2378 0.0944 0.071 Uiso 1 1 calc R . . C20 C 0.3364(9) -0.2619(10) 0.1347(4) 0.068(4) Uani 1 1 d . . . H20 H 0.3450 -0.3344 0.1364 0.081 Uiso 1 1 calc R . . C21 C 0.2842(9) -0.2121(10) 0.1565(3) 0.059(4) Uani 1 1 d . . . H21 H 0.2556 -0.2507 0.1729 0.070 Uiso 1 1 calc R . . C22 C 0.2734(8) -0.1042(9) 0.1545(3) 0.049(3) Uani 1 1 d . . . C23 C 0.2197(8) -0.0466(10) 0.1785(3) 0.048(3) Uani 1 1 d . . . C24 C 0.1704(9) -0.0897(11) 0.2048(4) 0.068(4) Uani 1 1 d . . . H24 H 0.1699 -0.1622 0.2085 0.082 Uiso 1 1 calc R . . C25 C 0.1231(10) -0.0244(13) 0.2248(4) 0.084(5) Uani 1 1 d . . . H25 H 0.0944 -0.0508 0.2436 0.101 Uiso 1 1 calc R . . C26 C 0.1191(9) 0.0801(12) 0.2166(4) 0.074(5) Uani 1 1 d . . . H26 H 0.0827 0.1235 0.2286 0.089 Uiso 1 1 calc R . . C27 C 0.1665(8) 0.1240(10) 0.1914(3) 0.054(4) Uani 1 1 d . . . C28 C 0.1711(9) 0.2327(11) 0.1813(4) 0.056(4) Uani 1 1 d . . . C29 C 0.1231(9) 0.3141(12) 0.1956(4) 0.073(5) Uani 1 1 d . . . H29 H 0.0834 0.2966 0.2119 0.088 Uiso 1 1 calc R . . C30 C 0.1319(10) 0.4162(13) 0.1869(5) 0.079(5) Uani 1 1 d . . . H30 H 0.0967 0.4681 0.1955 0.095 Uiso 1 1 calc R . . C31 C 0.1960(10) 0.4407(11) 0.1644(5) 0.076(5) Uani 1 1 d . . . H31 H 0.2084 0.5106 0.1593 0.092 Uiso 1 1 calc R . . C32 C 0.2419(9) 0.3584(9) 0.1494(3) 0.054(3) Uani 1 1 d . . . H32 H 0.2829 0.3745 0.1335 0.065 Uiso 1 1 calc R . . C33 C 0.0738(9) 0.2605(10) 0.0748(4) 0.058(4) Uani 1 1 d . . . C34 C 0.0797(9) 0.3419(12) 0.0547(5) 0.081(5) Uani 1 1 d . . . H34 H 0.1110 0.3331 0.0350 0.098 Uiso 1 1 calc R . . C35 C 0.0428(12) 0.4449(14) 0.0598(6) 0.099(7) Uani 1 1 d . . . H35 H 0.0512 0.5005 0.0445 0.119 Uiso 1 1 calc R . . C36 C -0.0044(12) 0.4552(15) 0.0878(7) 0.119(9) Uani 1 1 d . . . H36 H -0.0281 0.5209 0.0923 0.143 Uiso 1 1 calc R . . C37 C -0.0203(9) 0.3697(15) 0.1113(5) 0.097(7) Uani 1 1 d . . . H37 H -0.0549 0.3782 0.1301 0.116 Uiso 1 1 calc R . . C38 C 0.0201(8) 0.2707(13) 0.1042(4) 0.065(4) Uani 1 1 d . . . C39 C -0.0024(9) 0.1767(13) 0.1245(4) 0.068(4) Uani 1 1 d . . . C40 C -0.0598(10) 0.1631(17) 0.1514(5) 0.097(6) Uani 1 1 d . . . H40 H -0.0888 0.2201 0.1605 0.117 Uiso 1 1 calc R . . C41 C -0.0709(12) 0.0651(17) 0.1631(5) 0.097(6) Uani 1 1 d . . . H41 H -0.1075 0.0558 0.1812 0.117 Uiso 1 1 calc R . . C42 C -0.0324(10) -0.0214(16) 0.1505(5) 0.090(5) Uani 1 1 d . . . H42 H -0.0427 -0.0887 0.1590 0.108 Uiso 1 1 calc R . . C43 C 0.0245(9) -0.0033(14) 0.1236(5) 0.070(4) Uani 1 1 d . . . C44 C 0.0712(8) -0.0894(12) 0.1074(4) 0.059(4) Uani 1 1 d . . . C45 C 0.0617(11) -0.1925(14) 0.1147(5) 0.087(5) Uani 1 1 d . . . H45 H 0.0219 -0.2130 0.1306 0.104 Uiso 1 1 calc R . . C46 C 0.1097(13) -0.2675(14) 0.0992(6) 0.111(8) Uani 1 1 d . . . H46 H 0.1034 -0.3385 0.1046 0.133 Uiso 1 1 calc R . . C47 C 0.1686(12) -0.2354(11) 0.0749(5) 0.095(6) Uani 1 1 d . . . H47 H 0.2015 -0.2839 0.0632 0.115 Uiso 1 1 calc R . . C48 C 0.1751(8) -0.1291(10) 0.0693(3) 0.055(3) Uani 1 1 d . . . H48 H 0.2154 -0.1064 0.0539 0.066 Uiso 1 1 calc R . . C49 C 0.4738(7) 0.1314(8) 0.0903(3) 0.039(3) Uani 1 1 d . . . H49A H 0.5022 0.1769 0.0742 0.047 Uiso 1 1 calc R . . H49B H 0.4757 0.0605 0.0808 0.047 Uiso 1 1 calc R . . C50 C 0.3251(7) 0.1086(8) 0.0474(3) 0.037(3) Uani 1 1 d . . . H50A H 0.3616 0.1349 0.0297 0.044 Uiso 1 1 calc R . . H50B H 0.3360 0.0334 0.0496 0.044 Uiso 1 1 calc R . . C51 C 0.6093(8) 0.0133(9) 0.1279(3) 0.047(3) Uani 1 1 d . . . C52 C 0.6041(9) -0.0574(11) 0.1009(4) 0.070(4) Uani 1 1 d . . . H52 H 0.5642 -0.0466 0.0824 0.084 Uiso 1 1 calc R . . C53 C 0.6585(11) -0.1463(13) 0.1008(5) 0.090(6) Uani 1 1 d . . . H53 H 0.6525 -0.1954 0.0829 0.108 Uiso 1 1 calc R . . C54 C 0.7184(10) -0.1602(12) 0.1262(5) 0.085(5) Uani 1 1 d . . . H54 H 0.7551 -0.2179 0.1258 0.102 Uiso 1 1 calc R . . C55 C 0.7262(8) -0.0874(11) 0.1539(4) 0.063(4) Uani 1 1 d . . . H55 H 0.7682 -0.0967 0.1716 0.075 Uiso 1 1 calc R . . C56 C 0.6711(8) -0.0019(9) 0.1546(4) 0.056(4) Uani 1 1 d . . . H56 H 0.6755 0.0455 0.1731 0.067 Uiso 1 1 calc R . . C57 C 0.6228(7) 0.2339(9) 0.1286(3) 0.041(3) Uani 1 1 d . . . C58 C 0.6474(8) 0.2714(10) 0.0966(4) 0.058(4) Uani 1 1 d . . . H58 H 0.6221 0.2450 0.0759 0.070 Uiso 1 1 calc R . . C59 C 0.7113(10) 0.3499(12) 0.0960(4) 0.076(5) Uani 1 1 d . . . H59 H 0.7284 0.3759 0.0748 0.091 Uiso 1 1 calc R . . C60 C 0.7481(10) 0.3876(11) 0.1262(5) 0.078(5) Uani 1 1 d . . . H60 H 0.7883 0.4418 0.1258 0.093 Uiso 1 1 calc R . . C61 C 0.7258(9) 0.3459(11) 0.1567(5) 0.077(5) Uani 1 1 d . . . H61 H 0.7539 0.3689 0.1772 0.092 Uiso 1 1 calc R . . C62 C 0.6629(8) 0.2705(10) 0.1583(4) 0.058(4) Uani 1 1 d . . . H62 H 0.6478 0.2446 0.1798 0.070 Uiso 1 1 calc R . . C63 C 0.3615(8) 0.3114(8) 0.0765(3) 0.038(3) Uani 1 1 d . . . C64 C 0.2828(9) 0.3610(9) 0.0731(4) 0.060(4) Uani 1 1 d . . . H64 H 0.2338 0.3229 0.0779 0.072 Uiso 1 1 calc R . . C65 C 0.2740(11) 0.4628(11) 0.0631(5) 0.084(5) Uani 1 1 d . . . H65 H 0.2206 0.4958 0.0615 0.101 Uiso 1 1 calc R . . C66 C 0.3489(13) 0.5157(12) 0.0554(5) 0.099(7) Uani 1 1 d . . . H66 H 0.3444 0.5862 0.0487 0.119 Uiso 1 1 calc R . . C67 C 0.4309(11) 0.4695(12) 0.0570(4) 0.086(5) Uani 1 1 d . . . H67 H 0.4792 0.5055 0.0501 0.103 Uiso 1 1 calc R . . C68 C 0.4352(9) 0.3667(10) 0.0694(4) 0.059(4) Uani 1 1 d . . . H68 H 0.4884 0.3343 0.0729 0.071 Uiso 1 1 calc R . . C69 C 0.2122(8) 0.2322(9) -0.0008(3) 0.050(3) Uani 1 1 d . . . C70 C 0.2804(9) 0.2923(10) -0.0081(4) 0.060(4) Uani 1 1 d . . . H70 H 0.3303 0.2867 0.0061 0.072 Uiso 1 1 calc R . . C71 C 0.2790(13) 0.3642(11) -0.0366(4) 0.095(6) Uani 1 1 d . . . H71 H 0.3269 0.4046 -0.0413 0.114 Uiso 1 1 calc R . . C72 C 0.2053(15) 0.3716(13) -0.0568(4) 0.109(7) Uani 1 1 d . . . H72 H 0.2021 0.4182 -0.0755 0.130 Uiso 1 1 calc R . . C73 C 0.1356(13) 0.3107(16) -0.0499(5) 0.117(8) Uani 1 1 d . . . H73 H 0.0855 0.3170 -0.0639 0.141 Uiso 1 1 calc R . . C74 C 0.1378(10) 0.2408(12) -0.0227(4) 0.079(5) Uani 1 1 d . . . H74 H 0.0902 0.1991 -0.0188 0.095 Uiso 1 1 calc R . . C75 C 0.1973(8) 0.0165(9) -0.0006(3) 0.046(3) Uani 1 1 d . . . C76 C 0.2587(9) -0.0087(12) -0.0235(4) 0.072(5) Uani 1 1 d . . . H76 H 0.3129 0.0220 -0.0211 0.087 Uiso 1 1 calc R . . C77 C 0.2405(12) -0.0794(14) -0.0503(4) 0.095(6) Uani 1 1 d . . . H77 H 0.2812 -0.0917 -0.0667 0.114 Uiso 1 1 calc R . . C78 C 0.1623(12) -0.1326(13) -0.0533(5) 0.092(6) Uani 1 1 d . . . H78 H 0.1524 -0.1854 -0.0698 0.111 Uiso 1 1 calc R . . C79 C 0.1013(11) -0.1049(12) -0.0313(5) 0.081(5) Uani 1 1 d . . . H79 H 0.0470 -0.1350 -0.0341 0.097 Uiso 1 1 calc R . . C80 C 0.1179(9) -0.0321(11) -0.0045(4) 0.071(4) Uani 1 1 d . . . H80 H 0.0754 -0.0163 0.0108 0.085 Uiso 1 1 calc R . . Cl1 Cl 0.7770(4) 0.1273(3) 0.24384(11) 0.0837(13) Uani 1 1 d . . . O1 O 0.7898(10) 0.1393(9) 0.2791(3) 0.130(6) Uani 1 1 d . . . O2 O 0.8000(8) 0.0245(9) 0.2335(3) 0.119(5) Uani 1 1 d . . . O3 O 0.8138(10) 0.2039(12) 0.2241(4) 0.165(7) Uani 1 1 d . . . O4 O 0.6867(12) 0.1350(13) 0.2364(5) 0.182(8) Uani 1 1 d . . . Cl2 Cl 0.9140(3) 0.6278(3) 0.17204(13) 0.0832(13) Uani 1 1 d . . . O5 O 1.0006(11) 0.6222(13) 0.1699(6) 0.188(9) Uani 1 1 d . . . O6 O 0.8862(13) 0.5433(13) 0.1877(4) 0.216(10) Uani 1 1 d . . . O7 O 0.8816(14) 0.6286(13) 0.1380(5) 0.199(9) Uani 1 1 d . . . O8 O 0.8966(10) 0.7265(11) 0.1846(5) 0.172(7) Uani 1 1 d . . . Cl3 Cl 0.5479(4) 0.1955(4) 0.98456(13) 0.1021(16) Uani 1 1 d . . . O9 O 0.5009(10) 0.2719(14) 0.9634(5) 0.174(7) Uiso 1 1 d . . . O10 O 0.489(4) 0.184(4) 1.0098(16) 0.29(3) Uiso 0.50 1 d P . . O11 O 0.5308(19) 0.088(2) 0.9694(8) 0.131(10) Uiso 0.50 1 d P . . O12 O 0.6427(15) 0.210(2) 0.9771(7) 0.098(7) Uiso 0.50 1 d P . . O10' O 0.603(3) 0.129(3) 0.9654(12) 0.186(16) Uiso 0.50 1 d P . . O11' O 0.597(2) 0.285(3) 1.0045(10) 0.198(15) Uiso 0.50 1 d P . . O12' O 0.5464(16) 0.1857(17) 1.0203(6) 0.083(7) Uiso 0.50 1 d P . . O13 O 0.9820(12) 0.2659(16) 0.2541(6) 0.237(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0413(3) 0.0443(3) 0.0367(2) -0.0008(2) -0.0008(2) 0.0016(2) Pt2 0.0402(3) 0.0400(3) 0.0381(2) -0.00167(19) 0.0005(2) 0.0019(2) Pt3 0.0390(3) 0.0481(3) 0.0516(3) -0.0067(2) 0.0009(2) 0.0009(2) P1 0.038(2) 0.0398(16) 0.0371(15) -0.0032(13) -0.0031(14) 0.0061(14) P2 0.040(2) 0.0348(16) 0.0406(16) -0.0003(12) -0.0039(14) 0.0036(14) P3 0.042(2) 0.0434(18) 0.0434(16) 0.0011(14) -0.0044(15) 0.0037(15) N1 0.048(7) 0.061(7) 0.037(6) 0.017(5) -0.009(5) -0.012(6) N2 0.028(6) 0.077(8) 0.045(6) -0.005(6) 0.012(5) -0.004(5) N3 0.060(8) 0.045(6) 0.045(6) -0.010(5) -0.014(6) 0.001(5) N4 0.050(7) 0.042(6) 0.047(6) -0.004(5) -0.003(5) 0.008(5) N5 0.046(7) 0.054(7) 0.054(7) -0.009(5) 0.002(6) 0.002(5) N6 0.044(8) 0.077(8) 0.054(7) -0.002(6) 0.010(6) -0.001(6) C1 0.035(8) 0.045(7) 0.069(9) -0.010(6) -0.004(7) 0.009(6) C2 0.051(10) 0.073(10) 0.057(8) -0.013(7) -0.002(7) 0.026(7) C3 0.097(14) 0.054(9) 0.095(14) 0.010(8) -0.006(11) 0.005(9) C4 0.099(14) 0.066(11) 0.098(14) -0.026(10) 0.005(12) 0.025(10) C5 0.091(13) 0.077(11) 0.048(8) -0.022(8) 0.006(8) 0.019(9) C6 0.044(9) 0.057(8) 0.054(8) -0.017(7) 0.012(7) 0.021(7) C7 0.064(11) 0.067(9) 0.050(8) -0.018(7) -0.008(7) 0.004(8) C8 0.073(12) 0.113(15) 0.074(12) -0.044(10) 0.024(10) -0.006(10) C9 0.090(14) 0.118(16) 0.078(12) 0.002(11) 0.047(11) -0.009(11) C10 0.109(14) 0.084(12) 0.059(10) -0.003(8) 0.036(10) 0.000(10) C11 0.054(10) 0.087(11) 0.037(7) -0.003(7) 0.007(7) -0.013(8) C12 0.046(9) 0.065(9) 0.050(8) 0.019(7) 0.007(7) -0.016(7) C13 0.087(13) 0.082(12) 0.059(9) 0.007(8) 0.003(9) -0.022(10) C14 0.082(13) 0.078(11) 0.074(11) 0.039(10) -0.004(9) -0.031(10) C15 0.073(12) 0.054(9) 0.090(13) 0.011(8) -0.026(10) -0.003(8) C16 0.056(10) 0.051(8) 0.068(9) 0.001(7) 0.006(7) 0.010(7) C17 0.047(8) 0.037(6) 0.048(7) 0.004(5) 0.001(6) 0.014(6) C18 0.045(8) 0.033(6) 0.046(6) 0.005(5) 0.010(6) 0.012(5) C19 0.070(10) 0.047(8) 0.061(9) -0.004(6) 0.010(8) 0.031(7) C20 0.090(12) 0.036(7) 0.078(11) 0.005(7) 0.002(9) -0.001(7) C21 0.075(11) 0.050(8) 0.052(8) 0.019(6) 0.020(8) 0.007(7) C22 0.054(9) 0.049(8) 0.045(7) 0.007(6) 0.007(6) 0.017(6) C23 0.048(9) 0.055(8) 0.042(7) 0.009(6) 0.008(6) -0.002(6) C24 0.073(11) 0.063(9) 0.071(10) -0.002(8) 0.031(9) -0.007(8) C25 0.101(14) 0.081(12) 0.073(11) 0.001(9) 0.039(10) -0.012(10) C26 0.058(11) 0.075(11) 0.093(12) -0.017(9) 0.039(9) 0.002(8) C27 0.050(9) 0.065(9) 0.049(7) -0.017(6) 0.020(6) -0.007(7) C28 0.045(9) 0.067(9) 0.057(8) 0.010(7) 0.001(7) -0.011(7) C29 0.064(11) 0.074(11) 0.082(11) -0.028(9) 0.011(9) 0.028(9) C30 0.056(12) 0.088(12) 0.093(13) -0.032(10) -0.006(10) 0.026(9) C31 0.069(12) 0.043(8) 0.115(15) -0.031(9) -0.009(11) 0.005(8) C32 0.072(10) 0.033(6) 0.058(8) -0.001(6) 0.004(7) 0.004(6) C33 0.047(10) 0.052(8) 0.073(10) -0.009(7) -0.007(8) 0.006(7) C34 0.063(11) 0.062(10) 0.117(15) -0.022(9) -0.020(10) 0.015(9) C35 0.096(16) 0.090(14) 0.112(18) -0.009(12) 0.002(13) 0.034(12) C36 0.083(16) 0.067(12) 0.20(3) -0.015(15) -0.015(17) 0.022(11) C37 0.042(11) 0.119(15) 0.131(17) -0.062(13) 0.023(11) 0.035(10) C38 0.013(8) 0.110(13) 0.073(10) -0.019(9) -0.005(7) -0.007(8) C39 0.038(10) 0.096(12) 0.070(10) -0.005(9) 0.012(8) -0.016(8) C40 0.055(12) 0.136(18) 0.101(16) -0.038(13) 0.017(11) -0.013(11) C41 0.092(15) 0.112(16) 0.092(14) -0.001(12) 0.028(12) -0.014(13) C42 0.074(13) 0.112(15) 0.085(13) 0.006(11) 0.020(10) 0.012(11) C43 0.035(10) 0.096(13) 0.078(11) -0.014(9) -0.004(8) -0.005(9) C44 0.036(9) 0.075(10) 0.066(9) 0.013(8) 0.007(7) -0.020(7) C45 0.086(14) 0.086(13) 0.089(13) 0.019(10) -0.002(11) -0.035(11) C46 0.121(19) 0.056(12) 0.15(2) 0.002(12) -0.023(16) -0.023(12) C47 0.134(17) 0.035(8) 0.114(17) -0.009(9) -0.028(14) 0.002(10) C48 0.053(10) 0.059(9) 0.055(8) -0.009(6) 0.006(7) 0.010(7) C49 0.047(8) 0.031(6) 0.039(6) 0.003(5) 0.008(6) -0.002(5) C50 0.032(7) 0.035(6) 0.044(6) 0.011(5) 0.006(5) -0.001(5) C51 0.037(9) 0.045(7) 0.060(8) 0.006(6) -0.001(6) 0.002(6) C52 0.065(11) 0.077(10) 0.067(10) -0.016(8) 0.001(8) 0.034(9) C53 0.096(15) 0.084(12) 0.088(13) -0.006(9) -0.012(11) 0.041(10) C54 0.068(13) 0.069(11) 0.115(16) -0.001(9) -0.014(11) 0.027(9) C55 0.040(9) 0.061(9) 0.086(11) 0.013(8) -0.014(8) 0.011(7) C56 0.047(10) 0.043(7) 0.077(10) -0.005(6) -0.006(8) 0.009(6) C57 0.025(8) 0.047(7) 0.051(7) -0.002(5) 0.001(6) -0.001(6) C58 0.050(10) 0.066(9) 0.058(9) -0.006(7) -0.002(7) 0.009(7) C59 0.067(12) 0.086(11) 0.076(11) 0.025(9) 0.007(9) -0.024(9) C60 0.056(11) 0.058(10) 0.118(16) -0.002(9) -0.002(11) -0.015(8) C61 0.064(12) 0.055(9) 0.110(15) -0.004(9) -0.008(10) -0.014(8) C62 0.049(10) 0.060(9) 0.064(9) 0.009(7) -0.013(7) -0.006(7) C63 0.041(8) 0.033(6) 0.041(6) -0.008(5) 0.006(6) 0.002(5) C64 0.069(11) 0.042(7) 0.069(9) 0.005(6) 0.000(8) 0.011(7) C65 0.083(13) 0.046(9) 0.122(16) 0.014(9) -0.005(11) 0.001(9) C66 0.124(17) 0.041(9) 0.130(18) 0.027(9) -0.019(14) 0.024(10) C67 0.092(14) 0.053(9) 0.113(15) 0.019(9) 0.012(11) -0.023(9) C68 0.052(10) 0.055(8) 0.072(9) 0.002(7) 0.009(8) 0.002(7) C69 0.041(9) 0.047(7) 0.062(9) 0.003(6) -0.007(7) -0.004(6) C70 0.067(11) 0.055(8) 0.056(9) 0.001(6) -0.018(8) 0.004(7) C71 0.158(19) 0.062(10) 0.065(11) 0.024(8) 0.011(12) -0.025(11) C72 0.18(2) 0.086(13) 0.059(10) 0.049(9) -0.010(12) -0.008(14) C73 0.113(17) 0.107(16) 0.13(2) 0.055(14) -0.032(14) 0.002(13) C74 0.077(12) 0.077(11) 0.081(12) 0.029(8) -0.028(10) 0.000(9) C75 0.040(8) 0.052(7) 0.043(7) -0.009(6) -0.007(6) 0.002(6) C76 0.057(10) 0.096(12) 0.064(10) -0.030(8) 0.005(8) 0.001(9) C77 0.089(14) 0.125(15) 0.071(12) -0.054(11) 0.016(10) 0.006(12) C78 0.079(14) 0.103(14) 0.093(14) -0.056(11) -0.006(11) 0.004(11) C79 0.070(12) 0.082(11) 0.090(13) -0.039(9) -0.017(10) -0.011(9) C80 0.054(11) 0.077(10) 0.082(11) -0.025(8) 0.002(9) -0.023(8) Cl1 0.124(4) 0.071(3) 0.058(2) 0.0017(19) 0.019(3) 0.012(3) O1 0.260(17) 0.082(8) 0.045(7) -0.005(6) -0.008(9) -0.005(9) O2 0.172(12) 0.089(9) 0.101(10) -0.034(7) 0.047(9) 0.014(8) O3 0.243(17) 0.121(12) 0.136(15) 0.048(10) 0.047(13) -0.059(12) O4 0.172(16) 0.22(2) 0.163(19) 0.051(13) 0.061(14) 0.083(13) Cl2 0.093(4) 0.078(3) 0.081(3) 0.006(2) 0.022(3) 0.009(3) O5 0.113(13) 0.186(18) 0.27(3) 0.071(14) 0.059(15) 0.049(11) O6 0.40(3) 0.125(13) 0.134(16) 0.016(11) 0.119(17) -0.084(15) O7 0.30(3) 0.178(18) 0.110(16) -0.004(11) -0.056(16) 0.045(15) O8 0.187(14) 0.086(10) 0.24(2) -0.054(11) 0.030(14) 0.007(10) Cl3 0.137(5) 0.101(4) 0.069(3) 0.012(3) 0.016(3) 0.003(3) O13 0.227(19) 0.23(2) 0.25(3) 0.009(18) 0.068(18) 0.065(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 N2 2.033(10) . ? Pt1 C1 2.048(12) . ? Pt1 N1 2.153(10) . ? Pt1 P1 2.262(3) . ? Pt1 Pt2 3.1938(11) . ? Pt2 N4 1.995(10) . ? Pt2 C17 2.055(11) . ? Pt2 N3 2.204(10) . ? Pt2 P2 2.262(3) . ? Pt3 N6 2.004(11) . ? Pt3 C33 2.029(13) . ? Pt3 N5 2.169(10) . ? Pt3 P3 2.257(3) . ? P1 C57 1.832(12) . ? P1 C51 1.840(12) . ? P1 C49 1.851(11) . ? P2 C49 1.823(11) . ? P2 C63 1.846(11) . ? P2 C50 1.849(11) . ? P3 C69 1.828(13) . ? P3 C75 1.834(12) . ? P3 C50 1.836(11) . ? N1 C16 1.349(15) . ? N1 C12 1.386(15) . ? N2 C11 1.339(17) . ? N2 C7 1.362(15) . ? N3 C32 1.332(14) . ? N3 C28 1.346(15) . ? N4 C23 1.348(15) . ? N4 C27 1.384(14) . ? N5 C48 1.307(14) . ? N5 C44 1.373(15) . ? N6 C43 1.319(18) . ? N6 C39 1.349(18) . ? C1 C2 1.350(18) . ? C1 C6 1.419(16) . ? C2 C3 1.414(17) . ? C3 C4 1.41(2) . ? C4 C5 1.36(2) . ? C5 C6 1.365(18) . ? C6 C7 1.440(19) . ? C7 C8 1.410(18) . ? C8 C9 1.41(2) . ? C9 C10 1.35(2) . ? C10 C11 1.367(17) . ? C11 C12 1.458(19) . ? C12 C13 1.345(18) . ? C13 C14 1.39(2) . ? C14 C15 1.39(2) . ? C15 C16 1.357(17) . ? C17 C18 1.391(15) . ? C17 C22 1.419(16) . ? C18 C19 1.395(14) . ? C19 C20 1.387(18) . ? C20 C21 1.356(18) . ? C21 C22 1.379(16) . ? C22 C23 1.473(16) . ? C23 C24 1.409(16) . ? C24 C25 1.371(18) . ? C25 C26 1.363(19) . ? C26 C27 1.366(18) . ? C27 C28 1.435(18) . ? C28 C29 1.403(18) . ? C29 C30 1.35(2) . ? C30 C31 1.39(2) . ? C31 C32 1.404(17) . ? C33 C34 1.29(2) . ? C33 C38 1.447(18) . ? C34 C35 1.44(2) . ? C35 C36 1.34(3) . ? C36 C37 1.44(3) . ? C37 C38 1.436(19) . ? C38 C39 1.48(2) . ? C39 C40 1.41(2) . ? C40 C41 1.34(2) . ? C41 C42 1.35(2) . ? C42 C43 1.42(2) . ? C43 C44 1.468(19) . ? C44 C45 1.35(2) . ? C45 C46 1.37(2) . ? C46 C47 1.40(2) . ? C47 C48 1.369(17) . ? C51 C52 1.372(18) . ? C51 C56 1.386(16) . ? C52 C53 1.410(18) . ? C53 C54 1.33(2) . ? C54 C55 1.41(2) . ? C55 C56 1.383(15) . ? C57 C62 1.356(16) . ? C57 C58 1.394(16) . ? C58 C59 1.409(17) . ? C59 C60 1.36(2) . ? C60 C61 1.35(2) . ? C61 C62 1.372(17) . ? C63 C64 1.379(15) . ? C63 C68 1.385(16) . ? C64 C65 1.351(17) . ? C65 C66 1.39(2) . ? C66 C67 1.40(2) . ? C67 C68 1.388(17) . ? C69 C70 1.349(16) . ? C69 C74 1.402(17) . ? C70 C71 1.427(18) . ? C71 C72 1.36(2) . ? C72 C73 1.37(2) . ? C73 C74 1.37(2) . ? C75 C76 1.372(17) . ? C75 C80 1.384(16) . ? C76 C77 1.384(18) . ? C77 C78 1.39(2) . ? C78 C79 1.35(2) . ? C79 C80 1.400(18) . ? Cl1 O1 1.370(11) . ? Cl1 O3 1.375(12) . ? Cl1 O2 1.414(11) . ? Cl1 O4 1.427(17) . ? Cl2 O6 1.313(14) . ? Cl2 O5 1.359(15) . ? Cl2 O8 1.371(13) . ? Cl2 O7 1.379(18) . ? Cl3 O12' 1.38(2) . ? Cl3 O10 1.38(6) . ? Cl3 O10' 1.44(4) . ? Cl3 O9 1.442(18) . ? Cl3 O11 1.50(3) . ? Cl3 O12 1.53(2) . ? Cl3 O11' 1.56(4) . ? O10 O12' 0.97(6) . ? O11 O10' 1.26(4) . ? O12 O10' 1.26(4) . ? O12 O11' 1.61(4) . ? O11' O12' 1.63(4) . ? 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 N2 Pt1 C1 81.1(5) . . ? N2 Pt1 N1 77.0(4) . . ? C1 Pt1 N1 158.0(5) . . ? N2 Pt1 P1 178.2(3) . . ? C1 Pt1 P1 97.2(4) . . ? N1 Pt1 P1 104.5(3) . . ? N2 Pt1 Pt2 88.5(3) . . ? C1 Pt1 Pt2 88.7(3) . . ? N1 Pt1 Pt2 93.4(3) . . ? P1 Pt1 Pt2 92.33(8) . . ? N4 Pt2 C17 79.9(4) . . ? N4 Pt2 N3 76.5(4) . . ? C17 Pt2 N3 156.4(4) . . ? N4 Pt2 P2 174.6(3) . . ? C17 Pt2 P2 95.9(3) . . ? N3 Pt2 P2 107.8(3) . . ? N4 Pt2 Pt1 97.7(3) . . ? C17 Pt2 Pt1 87.3(3) . . ? N3 Pt2 Pt1 94.2(2) . . ? P2 Pt2 Pt1 85.47(8) . . ? N6 Pt3 C33 81.5(6) . . ? N6 Pt3 N5 77.7(4) . . ? C33 Pt3 N5 158.6(5) . . ? N6 Pt3 P3 177.6(4) . . ? C33 Pt3 P3 100.9(4) . . ? N5 Pt3 P3 99.8(3) . . ? C57 P1 C51 99.5(5) . . ? C57 P1 C49 108.3(5) . . ? C51 P1 C49 104.1(5) . . ? C57 P1 Pt1 114.6(4) . . ? C51 P1 Pt1 115.8(4) . . ? C49 P1 Pt1 113.2(4) . . ? C49 P2 C63 104.9(5) . . ? C49 P2 C50 99.0(5) . . ? C63 P2 C50 100.9(5) . . ? C49 P2 Pt2 115.8(4) . . ? C63 P2 Pt2 120.1(4) . . ? C50 P2 Pt2 113.2(3) . . ? C69 P3 C75 97.0(6) . . ? C69 P3 C50 106.9(5) . . ? C75 P3 C50 104.1(5) . . ? C69 P3 Pt3 123.8(4) . . ? C75 P3 Pt3 110.8(4) . . ? C50 P3 Pt3 111.7(4) . . ? C16 N1 C12 118.2(10) . . ? C16 N1 Pt1 130.0(9) . . ? C12 N1 Pt1 111.8(8) . . ? C11 N2 C7 122.5(12) . . ? C11 N2 Pt1 121.2(9) . . ? C7 N2 Pt1 116.3(9) . . ? C32 N3 C28 120.4(12) . . ? C32 N3 Pt2 127.3(9) . . ? C28 N3 Pt2 112.2(9) . . ? C23 N4 C27 120.8(11) . . ? C23 N4 Pt2 119.0(8) . . ? C27 N4 Pt2 120.1(8) . . ? C48 N5 C44 118.0(12) . . ? C48 N5 Pt3 129.6(9) . . ? C44 N5 Pt3 112.1(9) . . ? C43 N6 C39 120.7(13) . . ? C43 N6 Pt3 118.9(11) . . ? C39 N6 Pt3 120.3(10) . . ? C2 C1 C6 120.0(12) . . ? C2 C1 Pt1 129.2(10) . . ? C6 C1 Pt1 110.8(10) . . ? C1 C2 C3 119.2(14) . . ? C4 C3 C2 121.0(15) . . ? C5 C4 C3 117.7(15) . . ? C4 C5 C6 122.4(14) . . ? C5 C6 C1 119.6(13) . . ? C5 C6 C7 122.0(13) . . ? C1 C6 C7 118.4(12) . . ? N2 C7 C8 120.4(14) . . ? N2 C7 C6 113.3(12) . . ? C8 C7 C6 126.3(14) . . ? C7 C8 C9 115.2(15) . . ? C10 C9 C8 122.2(16) . . ? C9 C10 C11 120.6(16) . . ? N2 C11 C10 119.0(14) . . ? N2 C11 C12 111.9(12) . . ? C10 C11 C12 129.0(14) . . ? C13 C12 N1 121.2(14) . . ? C13 C12 C11 120.8(14) . . ? N1 C12 C11 118.0(11) . . ? C12 C13 C14 121.1(16) . . ? C13 C14 C15 117.1(13) . . ? C16 C15 C14 120.7(15) . . ? N1 C16 C15 121.7(15) . . ? C18 C17 C22 115.3(11) . . ? C18 C17 Pt2 131.9(9) . . ? C22 C17 Pt2 112.8(9) . . ? C17 C18 C19 121.6(11) . . ? C20 C19 C18 120.7(12) . . ? C21 C20 C19 119.4(13) . . ? C20 C21 C22 120.1(13) . . ? C21 C22 C17 122.9(11) . . ? C21 C22 C23 121.8(12) . . ? C17 C22 C23 115.3(11) . . ? N4 C23 C24 119.7(12) . . ? N4 C23 C22 112.8(11) . . ? C24 C23 C22 127.4(13) . . ? C25 C24 C23 119.9(14) . . ? C26 C25 C24 118.3(14) . . ? C25 C26 C27 122.7(14) . . ? C26 C27 N4 118.3(13) . . ? C26 C27 C28 128.2(13) . . ? N4 C27 C28 113.5(12) . . ? N3 C28 C29 118.5(13) . . ? N3 C28 C27 117.1(13) . . ? C29 C28 C27 124.4(14) . . ? C30 C29 C28 123.1(15) . . ? C29 C30 C31 117.1(14) . . ? C30 C31 C32 119.1(14) . . ? N3 C32 C31 121.5(14) . . ? C34 C33 C38 117.1(14) . . ? C34 C33 Pt3 134.0(13) . . ? C38 C33 Pt3 108.9(11) . . ? C33 C34 C35 126.9(18) . . ? C36 C35 C34 115.7(19) . . ? C35 C36 C37 123.3(18) . . ? C38 C37 C36 116.5(17) . . ? C37 C38 C33 120.3(15) . . ? C37 C38 C39 119.1(16) . . ? C33 C38 C39 120.2(14) . . ? N6 C39 C40 120.0(15) . . ? N6 C39 C38 108.4(13) . . ? C40 C39 C38 131.5(17) . . ? C41 C40 C39 117.3(18) . . ? C40 C41 C42 124.4(19) . . ? C41 C42 C43 115.9(18) . . ? N6 C43 C42 121.6(15) . . ? N6 C43 C44 116.3(15) . . ? C42 C43 C44 122.1(16) . . ? C45 C44 N5 120.7(15) . . ? C45 C44 C43 124.9(15) . . ? N5 C44 C43 114.4(13) . . ? C44 C45 C46 121.0(17) . . ? C45 C46 C47 118.8(17) . . ? C48 C47 C46 116.5(17) . . ? N5 C48 C47 124.9(15) . . ? P2 C49 P1 121.6(6) . . ? P3 C50 P2 119.9(6) . . ? C52 C51 C56 118.9(12) . . ? C52 C51 P1 124.9(11) . . ? C56 C51 P1 116.2(10) . . ? C51 C52 C53 120.7(15) . . ? C54 C53 C52 120.3(16) . . ? C53 C54 C55 120.0(15) . . ? C56 C55 C54 119.9(14) . . ? C55 C56 C51 120.2(13) . . ? C62 C57 C58 119.6(12) . . ? C62 C57 P1 119.2(10) . . ? C58 C57 P1 121.2(10) . . ? C57 C58 C59 118.8(13) . . ? C60 C59 C58 120.2(15) . . ? C61 C60 C59 119.4(15) . . ? C60 C61 C62 122.0(16) . . ? C57 C62 C61 119.9(14) . . ? C64 C63 C68 119.5(11) . . ? C64 C63 P2 116.8(9) . . ? C68 C63 P2 123.6(9) . . ? C65 C64 C63 122.7(14) . . ? C64 C65 C66 116.5(15) . . ? C65 C66 C67 124.1(14) . . ? C68 C67 C66 115.8(14) . . ? C63 C68 C67 121.2(13) . . ? C70 C69 C74 118.0(13) . . ? C70 C69 P3 125.3(10) . . ? C74 C69 P3 115.9(10) . . ? C69 C70 C71 122.5(14) . . ? C72 C71 C70 117.7(16) . . ? C71 C72 C73 120.4(14) . . ? C74 C73 C72 121.6(18) . . ? C73 C74 C69 119.8(16) . . ? C76 C75 C80 118.5(12) . . ? C76 C75 P3 121.4(10) . . ? C80 C75 P3 119.6(10) . . ? C75 C76 C77 120.4(14) . . ? C76 C77 C78 121.3(15) . . ? C79 C78 C77 117.8(14) . . ? C78 C79 C80 121.6(15) . . ? C75 C80 C79 120.2(14) . . ? O1 Cl1 O3 115.2(10) . . ? O1 Cl1 O2 110.8(8) . . ? O3 Cl1 O2 112.1(10) . . ? O1 Cl1 O4 106.5(11) . . ? O3 Cl1 O4 106.0(10) . . ? O2 Cl1 O4 105.6(10) . . ? O6 Cl2 O5 109.7(12) . . ? O6 Cl2 O8 120.4(12) . . ? O5 Cl2 O8 106.5(11) . . ? O6 Cl2 O7 109.2(12) . . ? O5 Cl2 O7 105.1(15) . . ? O8 Cl2 O7 104.9(10) . . ? O12' Cl3 O10 41(2) . . ? O12' Cl3 O10' 120(2) . . ? O10 Cl3 O10' 138(3) . . ? O12' Cl3 O9 126.1(13) . . ? O10 Cl3 O9 97(2) . . ? O10' Cl3 O9 113.9(19) . . ? O12' Cl3 O11 107.0(16) . . ? O10 Cl3 O11 94(3) . . ? O10' Cl3 O11 50.9(16) . . ? O9 Cl3 O11 108.4(15) . . ? O12' Cl3 O12 105.2(15) . . ? O10 Cl3 O12 146(3) . . ? O10' Cl3 O12 50.2(16) . . ? O9 Cl3 O12 106.4(12) . . ? O11 Cl3 O12 100.9(14) . . ? O12' Cl3 O11' 67.0(16) . . ? O10 Cl3 O11' 94(3) . . ? O10' Cl3 O11' 113(2) . . ? O9 Cl3 O11' 90.7(17) . . ? O11 Cl3 O11' 158.4(19) . . ? O12 Cl3 O11' 63.0(15) . . ? O12' O10 Cl3 69(4) . . ? O10' O11 Cl3 62(2) . . ? O10' O12 Cl3 61(2) . . ? O10' O12 O11' 120(3) . . ? Cl3 O12 O11' 59.3(16) . . ? O12 O10' O11 136(4) . . ? O12 O10' Cl3 69(2) . . ? O11 O10' Cl3 67(2) . . ? Cl3 O11' O12 57.7(17) . . ? Cl3 O11' O12' 51.3(15) . . ? O12 O11' O12' 91(2) . . ? O10 O12' Cl3 70(4) . . ? O10 O12' O11' 109(5) . . ? Cl3 O12' O11' 61.7(17) . . ? _diffrn_measured_fraction_theta_max 0.708 _diffrn_reflns_theta_full 25.56 _diffrn_measured_fraction_theta_full 0.708 _refine_diff_density_max 0.860 _refine_diff_density_min -2.009 _refine_diff_density_rms 0.250 #===END data_mar362 _database_code_CSD 178374 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Complex 2(ClO4)3.2Et2O.CH3CN' ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C80 H80 Cl3 N6 O12 P3 Pt3' _chemical_formula_sum 'C90 H85 Cl3 N7 O14 P3 Pt3' _chemical_formula_weight 2273.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 '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' 'O' 'O' 0.0106 0.0060 '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' _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 12.398(3) _cell_length_b 15.449(3) _cell_length_c 23.519(5) _cell_angle_alpha 82.20(3) _cell_angle_beta 89.42(3) _cell_angle_gamma 88.49(3) _cell_volume 4461.4(17) _cell_formula_units_Z 2 _cell_measurement_temperature 301(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.689 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2224 _exptl_absorpt_coefficient_mu 4.902 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 301(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28959 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0705 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 25.35 _reflns_number_total 14897 _reflns_number_gt 10556 _reflns_threshold_expression >2sigma(I) _computing_data_collection MarControl _computing_cell_refinement Scalepack _computing_data_reduction Denzo _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0738P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14897 _refine_ls_number_parameters 1000 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0629 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.1248 _refine_ls_wR_factor_gt 0.1120 _refine_ls_goodness_of_fit_ref 0.949 _refine_ls_restrained_S_all 0.951 _refine_ls_shift/su_max 0.007 _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 0.72142(3) 0.44137(2) 0.205574(14) 0.05308(10) Uani 1 1 d . . . Pt2 Pt 0.76448(2) 0.27084(2) 0.308589(13) 0.04798(10) Uani 1 1 d . . . Pt3 Pt 0.83383(2) 0.05521(2) 0.381141(13) 0.04874(10) Uani 1 1 d . . . P1 P 0.77895(15) 0.35778(14) 0.13994(9) 0.0480(5) Uani 1 1 d . . . P2 P 0.72316(15) 0.19740(13) 0.23512(8) 0.0443(4) Uani 1 1 d . . . P3 P 0.76999(15) 0.00392(13) 0.30270(8) 0.0464(5) Uani 1 1 d . . . N1 N 0.8688(6) 0.4730(4) 0.2472(3) 0.0603(18) Uani 1 1 d . . . N2 N 0.6656(6) 0.5221(5) 0.2606(3) 0.0652(19) Uani 1 1 d . . . N3 N 0.6146(5) 0.3260(4) 0.3400(3) 0.0601(18) Uani 1 1 d . . . N4 N 0.8115(6) 0.3267(4) 0.3776(3) 0.0603(18) Uani 1 1 d . . . N5 N 1.0072(5) 0.0334(5) 0.3704(3) 0.0594(17) Uani 1 1 d . . . N6 N 0.8949(6) 0.1040(4) 0.4490(3) 0.0533(16) Uani 1 1 d . . . C1 C 0.9692(7) 0.4463(6) 0.2386(4) 0.069(2) Uani 1 1 d . . . H1 H 0.9834 0.4127 0.2093 0.082 Uiso 1 1 calc R . . C2 C 1.0535(9) 0.4668(8) 0.2719(5) 0.092(3) Uani 1 1 d . . . H2 H 1.1237 0.4486 0.2645 0.110 Uiso 1 1 calc R . . C3 C 1.0325(11) 0.5138(8) 0.3156(5) 0.099(4) Uani 1 1 d . . . H3 H 1.0887 0.5270 0.3387 0.118 Uiso 1 1 calc R . . C4 C 0.9275(10) 0.5428(7) 0.3265(5) 0.086(3) Uani 1 1 d . . . H4 H 0.9121 0.5744 0.3567 0.103 Uiso 1 1 calc R . . C5 C 0.8478(8) 0.5224(6) 0.2904(4) 0.071(3) Uani 1 1 d . . . C6 C 0.7352(8) 0.5511(6) 0.2973(4) 0.070(2) Uani 1 1 d . . . C7 C 0.6951(13) 0.6053(8) 0.3358(5) 0.107(4) Uani 1 1 d . . . H7 H 0.7407 0.6253 0.3620 0.129 Uiso 1 1 calc R . . C8 C 0.5857(12) 0.6293(9) 0.3346(6) 0.113(4) Uani 1 1 d . . . H8 H 0.5586 0.6672 0.3591 0.136 Uiso 1 1 calc R . . C9 C 0.5187(10) 0.5973(7) 0.2975(5) 0.094(3) Uani 1 1 d . . . H9 H 0.4456 0.6127 0.2974 0.112 Uiso 1 1 calc R . . C10 C 0.5578(8) 0.5418(6) 0.2595(4) 0.068(2) Uani 1 1 d . . . C11 C 0.5003(8) 0.4966(6) 0.2193(4) 0.070(3) Uani 1 1 d . . . C12 C 0.5613(6) 0.4393(5) 0.1887(3) 0.056(2) Uani 1 1 d . . . C13 C 0.5041(7) 0.3880(6) 0.1550(4) 0.067(2) Uani 1 1 d . . . H13 H 0.5412 0.3491 0.1345 0.081 Uiso 1 1 calc R . . C14 C 0.3912(7) 0.3950(8) 0.1520(4) 0.081(3) Uani 1 1 d . . . H14 H 0.3543 0.3599 0.1301 0.097 Uiso 1 1 calc R . . C15 C 0.3343(9) 0.4530(9) 0.1811(5) 0.099(4) Uani 1 1 d . . . H15 H 0.2596 0.4584 0.1779 0.119 Uiso 1 1 calc R . . C16 C 0.3879(8) 0.5018(8) 0.2140(5) 0.083(3) Uani 1 1 d . . . H16 H 0.3490 0.5404 0.2340 0.100 Uiso 1 1 calc R . . C17 C 0.5158(7) 0.3302(5) 0.3161(4) 0.069(3) Uani 1 1 d . . . H17 H 0.5069 0.3081 0.2817 0.083 Uiso 1 1 calc R . . C18 C 0.4255(8) 0.3672(7) 0.3419(5) 0.088(3) Uani 1 1 d . . . H18 H 0.3580 0.3686 0.3249 0.106 Uiso 1 1 calc R . . C19 C 0.4390(10) 0.4006(8) 0.3917(6) 0.097(4) Uani 1 1 d . . . H19 H 0.3805 0.4248 0.4096 0.117 Uiso 1 1 calc R . . C20 C 0.5424(11) 0.3981(8) 0.4159(5) 0.102(4) Uani 1 1 d . . . H20 H 0.5525 0.4203 0.4503 0.123 Uiso 1 1 calc R . . C21 C 0.6285(9) 0.3630(6) 0.3890(4) 0.071(3) Uani 1 1 d . . . C22 C 0.7404(8) 0.3645(6) 0.4080(4) 0.067(2) Uani 1 1 d . . . C23 C 0.7737(11) 0.4034(7) 0.4546(4) 0.094(3) Uani 1 1 d . . . H23 H 0.7241 0.4299 0.4771 0.113 Uiso 1 1 calc R . . C24 C 0.8823(12) 0.4015(8) 0.4666(5) 0.101(4) Uani 1 1 d . . . H24 H 0.9067 0.4287 0.4968 0.122 Uiso 1 1 calc R . . C25 C 0.9541(10) 0.3604(7) 0.4348(4) 0.083(3) Uani 1 1 d . . . H25 H 1.0270 0.3581 0.4440 0.100 Uiso 1 1 calc R . . C26 C 0.9191(8) 0.3221(6) 0.3892(4) 0.068(2) Uani 1 1 d . . . C27 C 0.9826(7) 0.2784(6) 0.3482(4) 0.061(2) Uani 1 1 d . . . C28 C 0.9256(7) 0.2481(5) 0.3035(4) 0.056(2) Uani 1 1 d . . . C29 C 0.9916(6) 0.2134(6) 0.2630(4) 0.064(2) Uani 1 1 d . . . H29 H 0.9585 0.1925 0.2325 0.077 Uiso 1 1 calc R . . C30 C 1.1023(8) 0.2084(7) 0.2658(5) 0.083(3) Uani 1 1 d . . . H30 H 1.1423 0.1867 0.2370 0.100 Uiso 1 1 calc R . . C31 C 1.1525(8) 0.2355(7) 0.3110(6) 0.090(3) Uani 1 1 d . . . H31 H 1.2272 0.2302 0.3136 0.108 Uiso 1 1 calc R . . C32 C 1.0944(8) 0.2708(6) 0.3531(5) 0.079(3) Uani 1 1 d . . . H32 H 1.1292 0.2890 0.3841 0.095 Uiso 1 1 calc R . . C33 C 1.0607(7) -0.0026(6) 0.3296(4) 0.071(3) Uani 1 1 d . . . H33 H 1.0224 -0.0161 0.2983 0.085 Uiso 1 1 calc R . . C34 C 1.1711(8) -0.0206(7) 0.3319(5) 0.086(3) Uani 1 1 d . . . H34 H 1.2064 -0.0454 0.3027 0.103 Uiso 1 1 calc R . . C35 C 1.2273(8) -0.0005(7) 0.3792(5) 0.083(3) Uani 1 1 d . . . H35 H 1.3008 -0.0134 0.3828 0.099 Uiso 1 1 calc R . . C36 C 1.1733(7) 0.0381(6) 0.4199(5) 0.074(3) Uani 1 1 d . . . H36 H 1.2103 0.0527 0.4513 0.089 Uiso 1 1 calc R . . C37 C 1.0644(7) 0.0560(5) 0.4150(4) 0.062(2) Uani 1 1 d . . . C38 C 1.0026(8) 0.0988(5) 0.4574(4) 0.064(2) Uani 1 1 d . . . C39 C 1.0445(9) 0.1371(7) 0.5021(5) 0.083(3) Uani 1 1 d . . . H39 H 1.1184 0.1352 0.5087 0.099 Uiso 1 1 calc R . . C40 C 0.9744(10) 0.1784(7) 0.5366(4) 0.085(3) Uani 1 1 d . . . H40 H 1.0012 0.2053 0.5665 0.102 Uiso 1 1 calc R . . C41 C 0.8659(9) 0.1795(6) 0.5268(4) 0.077(3) Uani 1 1 d . . . H41 H 0.8188 0.2058 0.5507 0.092 Uiso 1 1 calc R . . C42 C 0.8262(8) 0.1424(5) 0.4823(4) 0.059(2) Uani 1 1 d . . . C43 C 0.7132(7) 0.1360(6) 0.4658(4) 0.062(2) Uani 1 1 d . . . C44 C 0.6938(6) 0.0923(5) 0.4186(3) 0.0530(19) Uani 1 1 d . . . C45 C 0.5890(7) 0.0812(6) 0.4060(4) 0.068(2) Uani 1 1 d . . . H45 H 0.5729 0.0499 0.3762 0.081 Uiso 1 1 calc R . . C46 C 0.5040(8) 0.1156(8) 0.4368(5) 0.089(3) Uani 1 1 d . . . H46 H 0.4328 0.1069 0.4273 0.107 Uiso 1 1 calc R . . C47 C 0.5258(10) 0.1618(8) 0.4806(5) 0.100(4) Uani 1 1 d . . . H47 H 0.4697 0.1862 0.5002 0.120 Uiso 1 1 calc R . . C48 C 0.6308(8) 0.1722(7) 0.4956(4) 0.079(3) Uani 1 1 d . . . H48 H 0.6464 0.2034 0.5255 0.095 Uiso 1 1 calc R . . C49 C 0.7811(6) 0.2393(5) 0.1642(3) 0.0519(19) Uani 1 1 d . . . C50 C 0.7822(6) 0.0852(5) 0.2386(3) 0.0494(18) Uani 1 1 d . . . C51 C 0.9161(6) 0.3811(6) 0.1139(4) 0.062(2) Uani 1 1 d . . . C52 C 0.9383(8) 0.4676(8) 0.0981(5) 0.090(3) Uani 1 1 d . . . H52 H 0.8869 0.5105 0.1039 0.108 Uiso 1 1 calc R . . C53 C 1.0403(11) 0.4921(11) 0.0728(5) 0.126(5) Uani 1 1 d . . . H53 H 1.0547 0.5501 0.0594 0.152 Uiso 1 1 calc R . . C54 C 1.1178(10) 0.4252(13) 0.0689(6) 0.131(6) Uani 1 1 d . . . H54 H 1.1869 0.4399 0.0559 0.158 Uiso 1 1 calc R . . C55 C 1.0948(10) 0.3399(11) 0.0834(6) 0.129(5) Uani 1 1 d . . . H55 H 1.1462 0.2967 0.0783 0.154 Uiso 1 1 calc R . . C56 C 0.9945(8) 0.3173(8) 0.1059(5) 0.097(4) Uani 1 1 d . . . H56 H 0.9790 0.2586 0.1159 0.116 Uiso 1 1 calc R . . C57 C 0.7109(6) 0.3718(6) 0.0712(3) 0.054(2) Uani 1 1 d . . . C58 C 0.7103(9) 0.3066(8) 0.0356(4) 0.090(3) Uani 1 1 d . . . H58 H 0.7394 0.2515 0.0484 0.108 Uiso 1 1 calc R . . C59 C 0.6663(11) 0.3237(10) -0.0191(5) 0.111(4) Uani 1 1 d . . . H59 H 0.6632 0.2792 -0.0420 0.134 Uiso 1 1 calc R . . C60 C 0.6274(9) 0.4060(11) -0.0395(5) 0.107(4) Uani 1 1 d . . . H60 H 0.5993 0.4171 -0.0764 0.128 Uiso 1 1 calc R . . C61 C 0.6296(7) 0.4720(9) -0.0059(5) 0.090(4) Uani 1 1 d . . . H61 H 0.6048 0.5280 -0.0201 0.108 Uiso 1 1 calc R . . C62 C 0.6687(7) 0.4545(7) 0.0487(4) 0.076(3) Uani 1 1 d . . . H62 H 0.6674 0.4990 0.0717 0.091 Uiso 1 1 calc R . . C63 C 0.5826(6) 0.1762(5) 0.2228(4) 0.059(2) Uani 1 1 d . . . C64 C 0.5181(7) 0.1557(6) 0.2698(5) 0.075(3) Uani 1 1 d . . . H64 H 0.5443 0.1593 0.3063 0.090 Uiso 1 1 calc R . . C65 C 0.4128(10) 0.1293(8) 0.2630(8) 0.113(5) Uani 1 1 d . . . H65 H 0.3705 0.1148 0.2956 0.136 Uiso 1 1 calc R . . C66 C 0.3707(11) 0.1241(9) 0.2126(10) 0.131(7) Uani 1 1 d . . . H66 H 0.2995 0.1079 0.2094 0.158 Uiso 1 1 calc R . . C67 C 0.4341(11) 0.1430(9) 0.1649(8) 0.125(6) Uani 1 1 d . . . H67 H 0.4059 0.1392 0.1289 0.151 Uiso 1 1 calc R . . C68 C 0.5406(8) 0.1681(7) 0.1696(5) 0.081(3) Uani 1 1 d . . . H68 H 0.5834 0.1793 0.1368 0.097 Uiso 1 1 calc R . . C69 C 0.6399(6) -0.0473(5) 0.3032(4) 0.054(2) Uani 1 1 d . . . C70 C 0.6063(7) -0.0996(6) 0.3521(4) 0.068(2) Uani 1 1 d . . . H70 H 0.6461 -0.1026 0.3857 0.081 Uiso 1 1 calc R . . C71 C 0.5145(8) -0.1472(6) 0.3516(5) 0.084(3) Uani 1 1 d . . . H71 H 0.4924 -0.1814 0.3851 0.101 Uiso 1 1 calc R . . C72 C 0.4556(9) -0.1455(7) 0.3036(6) 0.092(3) Uani 1 1 d . . . H72 H 0.3931 -0.1776 0.3040 0.110 Uiso 1 1 calc R . . C73 C 0.4888(8) -0.0959(7) 0.2543(5) 0.089(3) Uani 1 1 d . . . H73 H 0.4493 -0.0950 0.2208 0.107 Uiso 1 1 calc R . . C74 C 0.5803(7) -0.0472(6) 0.2538(4) 0.067(2) Uani 1 1 d . . . H74 H 0.6023 -0.0139 0.2199 0.081 Uiso 1 1 calc R . . C75 C 0.8521(6) -0.0866(5) 0.2830(3) 0.0512(19) Uani 1 1 d . . . C76 C 0.8764(7) -0.1552(5) 0.3263(4) 0.062(2) Uani 1 1 d . . . H76 H 0.8472 -0.1543 0.3628 0.074 Uiso 1 1 calc R . . C77 C 0.9416(8) -0.2229(6) 0.3159(5) 0.077(3) Uani 1 1 d . . . H77 H 0.9590 -0.2676 0.3453 0.093 Uiso 1 1 calc R . . C78 C 0.9817(10) -0.2249(8) 0.2619(6) 0.107(4) Uani 1 1 d . . . H78 H 1.0254 -0.2720 0.2545 0.128 Uiso 1 1 calc R . . C79 C 0.9592(10) -0.1602(7) 0.2188(5) 0.106(4) Uani 1 1 d . . . H79 H 0.9873 -0.1633 0.1823 0.127 Uiso 1 1 calc R . . C80 C 0.8950(8) -0.0895(7) 0.2286(4) 0.079(3) Uani 1 1 d . . . H80 H 0.8805 -0.0444 0.1991 0.095 Uiso 1 1 calc R . . Cl1 Cl 0.0852(3) 0.0593(2) 0.13378(15) 0.1060(10) Uani 1 1 d . . . Cl2 Cl 0.7491(2) 0.6811(2) 0.48107(11) 0.0874(8) Uani 1 1 d . . . Cl3 Cl 0.7523(2) 0.3467(2) 0.62881(12) 0.0882(8) Uani 1 1 d . . . O1 O 0.0683(9) -0.0142(8) 0.1034(5) 0.165(4) Uiso 1 1 d . . . O2 O 0.1537(10) 0.1190(8) 0.1049(5) 0.171(4) Uiso 1 1 d . . . O3 O 0.1312(9) 0.0237(8) 0.1896(6) 0.170(4) Uiso 1 1 d . . . O4 O -0.0184(8) 0.0973(7) 0.1446(4) 0.143(3) Uiso 1 1 d . . . O5 O 0.6545(8) 0.6403(7) 0.4709(5) 0.150(4) Uiso 1 1 d . . . O6 O 0.8476(12) 0.6442(11) 0.4575(7) 0.093(4) Uiso 0.50 1 d P . . O7 O 0.7617(11) 0.7021(11) 0.5366(6) 0.085(4) Uiso 0.50 1 d P . . O8 O 0.7263(15) 0.7613(14) 0.4448(9) 0.131(6) Uiso 0.50 1 d P . . O6' O 0.7878(16) 0.6389(15) 0.5320(9) 0.134(6) Uiso 0.50 1 d P . . O7' O 0.738(3) 0.773(2) 0.5049(16) 0.249(14) Uiso 0.50 1 d P . . O8' O 0.8236(16) 0.6977(14) 0.4385(9) 0.126(6) Uiso 0.50 1 d P . . O9 O 0.8563(7) 0.3465(6) 0.6055(4) 0.122(3) Uiso 1 1 d . . . O10 O 0.6847(15) 0.2885(14) 0.6071(8) 0.117(6) Uiso 0.50 1 d P . . O11 O 0.7451(13) 0.3288(13) 0.6901(8) 0.114(6) Uiso 0.50 1 d P . . O12 O 0.7393(13) 0.3923(13) 0.6761(8) 0.108(5) Uiso 0.50 1 d P . . O10' O 0.764(2) 0.244(2) 0.6517(14) 0.228(12) Uiso 0.50 1 d P . . O11' O 0.6592(14) 0.3456(13) 0.5945(8) 0.113(6) Uiso 0.50 1 d P . . O12' O 0.7278(19) 0.4399(17) 0.6143(11) 0.174(9) Uiso 0.50 1 d P . . N7 N 0.7166(14) 0.0517(12) 0.0960(8) 0.186(7) Uiso 1 1 d . . . C81 C 0.7662(16) 0.0250(14) 0.0701(9) 0.157(7) Uiso 1 1 d . . . C82 C 0.8299(19) -0.0390(17) 0.0417(11) 0.228(10) Uiso 1 1 d . . . O13 O 0.672(2) 0.1634(19) 0.8725(12) 0.361(12) Uiso 1 1 d . . . C83 C 0.723(3) 0.226(2) 0.8173(14) 0.276(13) Uiso 1 1 d . . . C84 C 0.805(3) 0.282(2) 0.8320(15) 0.306(15) Uiso 1 1 d . . . C85 C 0.628(4) 0.062(3) 0.9195(18) 0.36(2) Uiso 1 1 d . . . C86 C 0.528(5) 0.058(4) 0.938(2) 0.56(4) Uiso 1 1 d . . . O14 O 1.325(2) 0.2528(19) 0.9124(13) 0.205(11) Uiso 0.50 1 d PD . . C87 C 1.378(3) 0.269(3) 0.8562(14) 0.187(16) Uiso 0.50 1 d PD . . C89 C 1.339(3) 0.291(2) 0.9648(13) 0.196(16) Uiso 0.50 1 d PD . . C90 C 1.374(2) 0.2357(19) 1.0164(12) 0.122(9) Uiso 0.50 1 d PD . . C89' C 0.974(3) 0.247(3) 0.9380(17) 0.181(15) Uiso 0.50 1 d PD . . C90' C 0.964(4) 0.178(3) 0.9897(19) 0.23(2) Uiso 0.50 1 d PD . . C87' C 1.197(4) 0.249(4) 0.896(3) 0.31(3) Uiso 0.50 1 d PD . . C88 C 1.315(2) 0.228(2) 0.8137(13) 0.133(10) Uiso 0.50 1 d PD . . C88' C 1.279(4) 0.282(3) 0.8493(19) 0.187(15) Uiso 0.50 1 d PD . . O14' O 1.086(3) 0.266(3) 0.922(2) 0.34(2) Uiso 0.50 1 d PD . . 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 0.0647(2) 0.04391(19) 0.0513(2) -0.00869(15) 0.00400(14) -0.00337(14) Pt2 0.05644(19) 0.04270(18) 0.04503(18) -0.00747(14) 0.00609(12) 0.00000(12) Pt3 0.05679(19) 0.04617(19) 0.04378(18) -0.00803(14) -0.00001(12) -0.00118(13) P1 0.0494(11) 0.0485(12) 0.0460(12) -0.0055(10) 0.0031(8) -0.0054(8) P2 0.0432(10) 0.0449(12) 0.0446(11) -0.0066(9) 0.0046(8) -0.0001(8) P3 0.0544(11) 0.0425(11) 0.0431(11) -0.0092(9) 0.0008(8) 0.0009(8) N1 0.075(5) 0.050(4) 0.056(4) -0.006(4) -0.003(3) -0.013(3) N2 0.090(5) 0.050(4) 0.056(5) -0.009(4) 0.002(4) -0.003(4) N3 0.062(4) 0.054(4) 0.064(5) -0.011(4) 0.016(3) 0.004(3) N4 0.091(5) 0.047(4) 0.043(4) -0.007(3) 0.007(4) -0.004(4) N5 0.066(4) 0.053(4) 0.060(4) -0.013(4) -0.004(3) -0.002(3) N6 0.071(4) 0.045(4) 0.044(4) -0.003(3) -0.003(3) -0.004(3) C1 0.070(6) 0.065(6) 0.071(6) -0.003(5) -0.004(4) -0.016(5) C2 0.092(8) 0.084(8) 0.094(8) 0.010(7) -0.025(6) -0.031(6) C3 0.123(10) 0.085(8) 0.089(8) -0.003(7) -0.035(7) -0.050(7) C4 0.109(9) 0.064(7) 0.088(8) -0.023(6) -0.017(6) -0.023(6) C5 0.105(8) 0.043(5) 0.064(6) 0.001(5) -0.011(5) -0.017(5) C6 0.098(7) 0.052(6) 0.064(6) -0.015(5) 0.005(5) -0.006(5) C7 0.194(14) 0.073(8) 0.062(7) -0.034(6) 0.006(8) -0.023(8) C8 0.140(12) 0.113(11) 0.093(10) -0.042(8) 0.019(8) 0.025(9) C9 0.115(9) 0.079(8) 0.090(8) -0.028(7) 0.017(7) 0.018(6) C10 0.084(7) 0.054(6) 0.067(6) -0.007(5) 0.010(5) 0.009(5) C11 0.077(6) 0.066(6) 0.063(6) 0.002(5) 0.012(5) 0.008(5) C12 0.061(5) 0.054(5) 0.053(5) -0.008(4) 0.004(4) 0.005(4) C13 0.067(6) 0.074(7) 0.060(6) -0.004(5) 0.003(4) -0.007(4) C14 0.057(6) 0.110(9) 0.073(7) -0.007(6) 0.005(4) 0.001(5) C15 0.073(7) 0.133(11) 0.088(8) -0.008(8) 0.001(6) 0.020(7) C16 0.079(7) 0.097(8) 0.070(7) -0.005(6) 0.013(5) 0.023(6) C17 0.078(6) 0.044(5) 0.083(7) -0.004(5) 0.030(5) 0.007(4) C18 0.077(7) 0.072(7) 0.110(9) 0.004(7) 0.040(6) 0.007(5) C19 0.092(8) 0.097(9) 0.098(9) -0.008(7) 0.043(7) 0.023(6) C20 0.143(11) 0.083(8) 0.083(8) -0.026(6) 0.036(8) 0.016(7) C21 0.109(8) 0.058(6) 0.047(5) -0.009(5) 0.025(5) 0.008(5) C22 0.101(7) 0.051(5) 0.051(5) -0.012(4) 0.012(5) -0.001(5) C23 0.144(11) 0.080(8) 0.062(7) -0.024(6) 0.015(7) -0.002(7) C24 0.158(12) 0.076(8) 0.071(8) -0.011(6) -0.020(8) -0.030(8) C25 0.111(8) 0.075(7) 0.066(7) -0.015(6) -0.015(6) -0.012(6) C26 0.088(7) 0.055(6) 0.058(6) 0.001(5) -0.018(5) -0.014(5) C27 0.063(5) 0.050(5) 0.068(6) -0.003(4) -0.005(4) -0.005(4) C28 0.070(5) 0.044(5) 0.056(5) -0.009(4) -0.004(4) -0.003(4) C29 0.048(5) 0.066(6) 0.080(6) -0.021(5) 0.005(4) 0.001(4) C30 0.064(6) 0.073(7) 0.115(9) -0.024(6) 0.002(5) 0.003(5) C31 0.063(7) 0.081(8) 0.128(10) -0.018(7) -0.012(6) -0.005(5) C32 0.074(7) 0.063(6) 0.099(8) 0.001(6) -0.033(6) -0.014(5) C33 0.056(6) 0.082(7) 0.078(7) -0.022(6) 0.004(4) -0.006(4) C34 0.068(7) 0.087(8) 0.101(9) -0.006(7) 0.009(6) -0.001(5) C35 0.064(6) 0.076(7) 0.104(9) 0.004(6) -0.002(6) 0.000(5) C36 0.063(6) 0.069(7) 0.088(7) 0.001(6) -0.022(5) -0.014(5) C37 0.070(6) 0.046(5) 0.069(6) 0.000(5) -0.011(4) -0.010(4) C38 0.091(7) 0.044(5) 0.058(6) -0.001(4) -0.015(5) -0.010(4) C39 0.083(7) 0.073(7) 0.089(8) 0.004(6) -0.033(6) -0.011(5) C40 0.123(9) 0.070(7) 0.064(7) -0.017(6) -0.024(6) -0.011(6) C41 0.110(8) 0.066(7) 0.056(6) -0.013(5) -0.004(5) 0.002(5) C42 0.094(6) 0.037(5) 0.046(5) -0.006(4) -0.003(4) -0.007(4) C43 0.080(6) 0.054(5) 0.049(5) -0.002(4) 0.010(4) 0.003(4) C44 0.068(5) 0.045(5) 0.046(5) -0.009(4) 0.003(4) 0.001(4) C45 0.074(6) 0.065(6) 0.065(6) -0.014(5) 0.006(4) -0.002(4) C46 0.077(7) 0.109(9) 0.086(8) -0.037(7) 0.016(5) 0.004(6) C47 0.099(9) 0.117(10) 0.086(8) -0.033(7) 0.027(6) 0.021(7) C48 0.092(8) 0.073(7) 0.076(7) -0.025(6) 0.019(5) -0.003(5) C49 0.069(5) 0.038(4) 0.046(5) 0.001(4) 0.007(4) 0.003(3) C50 0.061(5) 0.042(4) 0.046(4) -0.008(4) 0.008(3) 0.004(3) C51 0.051(5) 0.080(7) 0.055(5) -0.004(5) 0.003(4) -0.022(4) C52 0.075(7) 0.099(9) 0.093(8) 0.003(7) 0.010(5) -0.035(6) C53 0.113(11) 0.152(14) 0.105(10) 0.027(10) 0.007(8) -0.076(10) C54 0.067(9) 0.21(2) 0.111(11) 0.007(11) 0.008(7) -0.045(10) C55 0.086(9) 0.143(13) 0.155(13) -0.016(11) 0.058(8) -0.014(8) C56 0.077(7) 0.113(10) 0.102(9) -0.017(7) 0.039(6) -0.024(6) C57 0.059(5) 0.058(5) 0.042(5) -0.003(4) 0.002(3) 0.007(4) C58 0.108(8) 0.102(9) 0.057(6) -0.002(6) -0.006(5) 0.011(6) C59 0.155(12) 0.125(12) 0.056(7) -0.013(7) -0.020(7) -0.010(9) C60 0.097(9) 0.164(15) 0.055(7) 0.008(9) -0.009(6) -0.032(9) C61 0.064(6) 0.125(11) 0.065(7) 0.040(7) -0.005(5) 0.003(6) C62 0.059(6) 0.091(8) 0.075(7) -0.004(6) 0.010(4) 0.005(5) C63 0.053(5) 0.052(5) 0.071(6) -0.011(4) 0.002(4) 0.004(4) C64 0.063(6) 0.054(6) 0.106(8) -0.002(5) 0.024(5) 0.002(4) C65 0.062(8) 0.085(9) 0.196(16) -0.026(10) 0.031(8) -0.015(6) C66 0.048(8) 0.095(10) 0.26(2) -0.044(12) -0.017(10) 0.000(6) C67 0.083(10) 0.104(10) 0.202(17) -0.067(11) -0.075(10) 0.021(7) C68 0.070(6) 0.081(7) 0.095(8) -0.024(6) -0.018(5) 0.007(5) C69 0.060(5) 0.046(5) 0.055(5) -0.007(4) 0.006(4) 0.003(4) C70 0.068(6) 0.063(6) 0.073(6) -0.014(5) 0.014(4) -0.006(4) C71 0.082(7) 0.060(6) 0.108(9) -0.006(6) 0.030(6) -0.018(5) C72 0.075(7) 0.070(7) 0.132(11) -0.013(7) 0.007(7) -0.021(5) C73 0.081(7) 0.074(7) 0.113(9) -0.010(7) -0.027(6) -0.020(5) C74 0.068(6) 0.050(5) 0.085(7) -0.010(5) -0.008(5) -0.009(4) C75 0.063(5) 0.038(4) 0.054(5) -0.009(4) 0.001(4) 0.000(3) C76 0.077(6) 0.048(5) 0.060(6) -0.004(4) -0.001(4) 0.002(4) C77 0.096(7) 0.052(6) 0.081(7) -0.005(5) 0.004(5) 0.013(5) C78 0.117(9) 0.075(8) 0.129(11) -0.026(8) 0.014(8) 0.042(7) C79 0.153(11) 0.071(7) 0.087(8) 0.002(6) 0.036(7) 0.052(7) C80 0.101(7) 0.067(7) 0.070(7) -0.012(5) 0.008(5) 0.024(5) Cl1 0.094(2) 0.118(3) 0.110(2) -0.033(2) 0.0234(17) -0.0079(17) Cl2 0.0713(16) 0.125(3) 0.0669(16) -0.0130(16) -0.0001(12) -0.0183(14) Cl3 0.0713(16) 0.111(2) 0.093(2) -0.0482(18) 0.0181(13) -0.0181(14) _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 N2 2.021(7) . ? Pt1 C12 2.030(8) . ? Pt1 N1 2.179(7) . ? Pt1 P1 2.243(2) . ? Pt2 C28 2.024(8) . ? Pt2 N4 2.037(7) . ? Pt2 N3 2.187(6) . ? Pt2 P2 2.262(2) . ? Pt3 N6 2.018(7) . ? Pt3 C44 2.043(8) . ? Pt3 N5 2.184(7) . ? Pt3 P3 2.262(2) . ? P1 C57 1.814(8) . ? P1 C51 1.829(8) . ? P1 C49 1.842(8) . ? P2 C63 1.816(8) . ? P2 C49 1.851(8) . ? P2 C50 1.855(8) . ? P3 C69 1.815(8) . ? P3 C75 1.817(8) . ? P3 C50 1.835(8) . ? N1 C1 1.323(11) . ? N1 C5 1.370(12) . ? N2 C6 1.353(11) . ? N2 C10 1.363(11) . ? N3 C17 1.349(11) . ? N3 C21 1.367(11) . ? N4 C22 1.304(11) . ? N4 C26 1.362(11) . ? N5 C33 1.334(11) . ? N5 C37 1.362(11) . ? N6 C42 1.332(11) . ? N6 C38 1.350(11) . ? C1 C2 1.382(13) . ? C2 C3 1.356(16) . ? C3 C4 1.398(16) . ? C4 C5 1.379(13) . ? C5 C6 1.467(13) . ? C6 C7 1.394(14) . ? C7 C8 1.396(17) . ? C8 C9 1.360(16) . ? C9 C10 1.394(13) . ? C10 C11 1.452(14) . ? C11 C16 1.399(13) . ? C11 C12 1.414(12) . ? C12 C13 1.406(12) . ? C13 C14 1.402(12) . ? C14 C15 1.375(15) . ? C15 C16 1.344(15) . ? C17 C18 1.411(12) . ? C18 C19 1.358(16) . ? C19 C20 1.405(16) . ? C20 C21 1.374(13) . ? C21 C22 1.464(14) . ? C22 C23 1.391(14) . ? C23 C24 1.377(16) . ? C24 C25 1.356(16) . ? C25 C26 1.372(13) . ? C26 C27 1.464(13) . ? C27 C32 1.393(12) . ? C27 C28 1.410(11) . ? C28 C29 1.401(11) . ? C29 C30 1.374(12) . ? C30 C31 1.356(15) . ? C31 C32 1.381(15) . ? C33 C34 1.390(12) . ? C34 C35 1.393(15) . ? C35 C36 1.357(14) . ? C36 C37 1.373(12) . ? C37 C38 1.469(13) . ? C38 C39 1.386(13) . ? C39 C40 1.385(15) . ? C40 C41 1.367(14) . ? C41 C42 1.361(12) . ? C42 C43 1.468(12) . ? C43 C48 1.381(12) . ? C43 C44 1.401(11) . ? C44 C45 1.356(11) . ? C45 C46 1.407(12) . ? C46 C47 1.362(15) . ? C47 C48 1.371(14) . ? C51 C52 1.372(13) . ? C51 C56 1.396(14) . ? C52 C53 1.429(14) . ? C53 C54 1.40(2) . ? C54 C55 1.35(2) . ? C55 C56 1.381(14) . ? C57 C58 1.395(13) . ? C57 C62 1.406(12) . ? C58 C59 1.392(14) . ? C59 C60 1.373(18) . ? C60 C61 1.374(17) . ? C61 C62 1.366(13) . ? C63 C64 1.365(12) . ? C63 C68 1.382(13) . ? C64 C65 1.395(14) . ? C65 C66 1.31(2) . ? C66 C67 1.37(2) . ? C67 C68 1.395(15) . ? C69 C70 1.380(11) . ? C69 C74 1.384(12) . ? C70 C71 1.372(12) . ? C71 C72 1.348(15) . ? C72 C73 1.367(15) . ? C73 C74 1.376(12) . ? C75 C80 1.385(12) . ? C75 C76 1.395(11) . ? C76 C77 1.353(12) . ? C77 C78 1.365(15) . ? C78 C79 1.348(15) . ? C79 C80 1.378(13) . ? Cl1 O2 1.376(12) . ? Cl1 O4 1.434(10) . ? Cl1 O1 1.441(12) . ? Cl1 O3 1.468(12) . ? Cl2 O8' 1.36(2) . ? Cl2 O6' 1.37(2) . ? Cl2 O5 1.384(11) . ? Cl2 O7 1.400(15) . ? Cl2 O8 1.43(2) . ? Cl2 O6 1.469(16) . ? Cl2 O7' 1.60(4) . ? Cl3 O9 1.396(9) . ? Cl3 O10 1.396(19) . ? Cl3 O12 1.401(18) . ? Cl3 O11' 1.417(18) . ? Cl3 O11 1.432(18) . ? Cl3 O12' 1.46(3) . ? Cl3 O10' 1.60(3) . ? O6 O8' 0.93(2) . ? O7 O6' 1.04(2) . ? O7 O7' 1.27(4) . ? O8 O7' 1.46(4) . ? O8 O8' 1.55(3) . ? O10 O11' 0.94(2) . ? O10 O10' 1.53(3) . ? O11 O12 0.99(2) . ? O11 O10' 1.69(4) . ? O12 O12' 1.54(3) . ? N7 C81 0.98(2) . ? C81 C82 1.48(3) . ? O13 C83 1.64(3) . ? O13 C85 1.88(4) . ? C83 C84 1.42(4) . ? C85 C86 1.32(7) . ? O14 C89 1.451(19) . ? O14 C87 1.468(19) . ? O14 C88' 1.59(5) . ? O14 C87' 1.64(6) . ? C87 C88' 1.25(5) . ? C87 C88 1.494(19) . ? C89 C90 1.448(19) . ? C89' O14' 1.450(19) . ? C89' C90' 1.514(19) . ? C87' O14' 1.53(2) . ? C87' C88' 1.55(2) . ? C88 C88' 1.32(5) . ? 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 N2 Pt1 C12 80.7(3) . . ? N2 Pt1 N1 77.8(3) . . ? C12 Pt1 N1 158.4(3) . . ? N2 Pt1 P1 176.4(2) . . ? C12 Pt1 P1 97.5(2) . . ? N1 Pt1 P1 104.1(2) . . ? C28 Pt2 N4 81.0(3) . . ? C28 Pt2 N3 156.8(3) . . ? N4 Pt2 N3 76.1(3) . . ? C28 Pt2 P2 95.1(2) . . ? N4 Pt2 P2 174.3(2) . . ? N3 Pt2 P2 108.0(2) . . ? N6 Pt3 C44 80.3(3) . . ? N6 Pt3 N5 77.7(3) . . ? C44 Pt3 N5 158.0(3) . . ? N6 Pt3 P3 177.70(19) . . ? C44 Pt3 P3 101.2(2) . . ? N5 Pt3 P3 100.86(19) . . ? C57 P1 C51 98.4(4) . . ? C57 P1 C49 105.4(4) . . ? C51 P1 C49 104.7(4) . . ? C57 P1 Pt1 117.6(3) . . ? C51 P1 Pt1 113.6(3) . . ? C49 P1 Pt1 115.2(3) . . ? C63 P2 C49 106.2(4) . . ? C63 P2 C50 100.2(4) . . ? C49 P2 C50 96.1(3) . . ? C63 P2 Pt2 118.8(3) . . ? C49 P2 Pt2 116.3(3) . . ? C50 P2 Pt2 115.9(3) . . ? C69 P3 C75 97.8(4) . . ? C69 P3 C50 109.7(4) . . ? C75 P3 C50 101.8(3) . . ? C69 P3 Pt3 121.7(3) . . ? C75 P3 Pt3 112.2(3) . . ? C50 P3 Pt3 111.1(3) . . ? C1 N1 C5 119.1(8) . . ? C1 N1 Pt1 128.9(6) . . ? C5 N1 Pt1 111.8(6) . . ? C6 N2 C10 123.8(8) . . ? C6 N2 Pt1 119.1(6) . . ? C10 N2 Pt1 117.1(6) . . ? C17 N3 C21 118.7(7) . . ? C17 N3 Pt2 128.3(6) . . ? C21 N3 Pt2 112.9(6) . . ? C22 N4 C26 123.5(8) . . ? C22 N4 Pt2 120.3(7) . . ? C26 N4 Pt2 116.3(6) . . ? C33 N5 C37 118.2(8) . . ? C33 N5 Pt3 129.6(6) . . ? C37 N5 Pt3 112.0(6) . . ? C42 N6 C38 123.5(7) . . ? C42 N6 Pt3 117.6(6) . . ? C38 N6 Pt3 118.9(6) . . ? N1 C1 C2 121.9(10) . . ? C3 C2 C1 119.1(11) . . ? C2 C3 C4 120.9(10) . . ? C5 C4 C3 117.0(11) . . ? N1 C5 C4 122.0(10) . . ? N1 C5 C6 116.6(8) . . ? C4 C5 C6 121.4(10) . . ? N2 C6 C7 118.4(11) . . ? N2 C6 C5 114.4(8) . . ? C7 C6 C5 127.2(10) . . ? C6 C7 C8 119.4(12) . . ? C9 C8 C7 119.9(11) . . ? C8 C9 C10 121.0(12) . . ? N2 C10 C9 117.4(10) . . ? N2 C10 C11 112.6(8) . . ? C9 C10 C11 130.0(10) . . ? C16 C11 C12 119.8(10) . . ? C16 C11 C10 122.6(9) . . ? C12 C11 C10 117.3(8) . . ? C13 C12 C11 117.2(8) . . ? C13 C12 Pt1 130.5(7) . . ? C11 C12 Pt1 112.1(7) . . ? C14 C13 C12 120.4(9) . . ? C15 C14 C13 121.1(11) . . ? C16 C15 C14 119.2(11) . . ? C15 C16 C11 122.3(11) . . ? N3 C17 C18 122.0(10) . . ? C19 C18 C17 118.9(11) . . ? C18 C19 C20 119.1(10) . . ? C21 C20 C19 120.1(11) . . ? N3 C21 C20 121.0(11) . . ? N3 C21 C22 114.9(8) . . ? C20 C21 C22 124.1(10) . . ? N4 C22 C23 119.7(10) . . ? N4 C22 C21 115.6(8) . . ? C23 C22 C21 124.6(10) . . ? C24 C23 C22 118.2(11) . . ? C25 C24 C23 120.7(11) . . ? C24 C25 C26 120.0(11) . . ? N4 C26 C25 118.0(10) . . ? N4 C26 C27 113.2(8) . . ? C25 C26 C27 128.9(10) . . ? C32 C27 C28 123.0(9) . . ? C32 C27 C26 120.1(9) . . ? C28 C27 C26 116.9(8) . . ? C29 C28 C27 114.1(8) . . ? C29 C28 Pt2 133.0(6) . . ? C27 C28 Pt2 112.7(6) . . ? C30 C29 C28 123.9(9) . . ? C31 C30 C29 119.4(11) . . ? C30 C31 C32 121.1(10) . . ? C31 C32 C27 118.5(10) . . ? N5 C33 C34 122.8(9) . . ? C33 C34 C35 118.0(10) . . ? C36 C35 C34 119.1(10) . . ? C35 C36 C37 120.5(10) . . ? N5 C37 C36 121.3(9) . . ? N5 C37 C38 116.1(8) . . ? C36 C37 C38 122.6(9) . . ? N6 C38 C39 118.5(9) . . ? N6 C38 C37 115.0(8) . . ? C39 C38 C37 126.5(10) . . ? C40 C39 C38 118.9(10) . . ? C41 C40 C39 119.8(10) . . ? C42 C41 C40 120.6(10) . . ? N6 C42 C41 118.8(9) . . ? N6 C42 C43 113.0(7) . . ? C41 C42 C43 128.2(9) . . ? C48 C43 C44 122.3(9) . . ? C48 C43 C42 120.9(9) . . ? C44 C43 C42 116.8(7) . . ? C45 C44 C43 116.6(8) . . ? C45 C44 Pt3 131.5(6) . . ? C43 C44 Pt3 112.0(6) . . ? C44 C45 C46 121.8(9) . . ? C47 C46 C45 120.0(10) . . ? C46 C47 C48 119.7(10) . . ? C47 C48 C43 119.4(10) . . ? P1 C49 P2 119.6(4) . . ? P3 C50 P2 122.2(4) . . ? C52 C51 C56 119.4(9) . . ? C52 C51 P1 116.1(8) . . ? C56 C51 P1 124.3(7) . . ? C51 C52 C53 120.3(12) . . ? C54 C53 C52 117.4(13) . . ? C55 C54 C53 121.8(12) . . ? C54 C55 C56 119.7(14) . . ? C55 C56 C51 121.0(12) . . ? C58 C57 C62 117.0(8) . . ? C58 C57 P1 122.8(7) . . ? C62 C57 P1 119.6(7) . . ? C59 C58 C57 120.4(11) . . ? C60 C59 C58 120.3(13) . . ? C59 C60 C61 120.5(11) . . ? C62 C61 C60 119.3(11) . . ? C61 C62 C57 122.4(11) . . ? C64 C63 C68 117.9(9) . . ? C64 C63 P2 117.5(7) . . ? C68 C63 P2 124.0(7) . . ? C63 C64 C65 119.8(12) . . ? C66 C65 C64 123.0(15) . . ? C65 C66 C67 118.3(14) . . ? C66 C67 C68 120.9(14) . . ? C63 C68 C67 120.1(12) . . ? C70 C69 C74 117.8(8) . . ? C70 C69 P3 119.3(7) . . ? C74 C69 P3 122.1(7) . . ? C71 C70 C69 120.5(10) . . ? C72 C71 C70 121.4(10) . . ? C71 C72 C73 119.1(10) . . ? C72 C73 C74 120.5(10) . . ? C73 C74 C69 120.6(9) . . ? C80 C75 C76 118.8(8) . . ? C80 C75 P3 124.0(7) . . ? C76 C75 P3 117.2(6) . . ? C77 C76 C75 121.0(9) . . ? C76 C77 C78 119.1(10) . . ? C79 C78 C77 121.6(10) . . ? C78 C79 C80 120.3(10) . . ? C79 C80 C75 119.2(9) . . ? O2 Cl1 O4 112.4(7) . . ? O2 Cl1 O1 112.5(7) . . ? O4 Cl1 O1 107.8(6) . . ? O2 Cl1 O3 110.0(7) . . ? O4 Cl1 O3 107.2(6) . . ? O1 Cl1 O3 106.6(7) . . ? O8' Cl2 O6' 115.5(12) . . ? O8' Cl2 O5 120.1(10) . . ? O6' Cl2 O5 106.0(10) . . ? O8' Cl2 O7 123.9(10) . . ? O6' Cl2 O7 44.1(9) . . ? O5 Cl2 O7 116.1(7) . . ? O8' Cl2 O8 67.7(11) . . ? O6' Cl2 O8 148.9(13) . . ? O5 Cl2 O8 96.9(9) . . ? O7 Cl2 O8 106.8(11) . . ? O8' Cl2 O6 38.1(9) . . ? O6' Cl2 O6 83.3(11) . . ? O5 Cl2 O6 115.4(8) . . ? O7 Cl2 O6 113.5(8) . . ? O8 Cl2 O6 105.8(10) . . ? O8' Cl2 O7' 102.1(15) . . ? O6' Cl2 O7' 93.1(15) . . ? O5 Cl2 O7' 117.1(12) . . ? O7 Cl2 O7' 49.6(13) . . ? O8 Cl2 O7' 57.2(14) . . ? O6 Cl2 O7' 126.1(13) . . ? O9 Cl3 O10 113.0(9) . . ? O9 Cl3 O12 115.3(8) . . ? O10 Cl3 O12 130.6(10) . . ? O9 Cl3 O11' 122.0(8) . . ? O10 Cl3 O11' 39.0(9) . . ? O12 Cl3 O11' 114.9(10) . . ? O9 Cl3 O11 116.0(8) . . ? O10 Cl3 O11 106.7(11) . . ? O12 Cl3 O11 40.9(9) . . ? O11' Cl3 O11 120.7(10) . . ? O9 Cl3 O12' 97.7(10) . . ? O10 Cl3 O12' 117.7(13) . . ? O12 Cl3 O12' 65.3(11) . . ? O11' Cl3 O12' 78.6(12) . . ? O11 Cl3 O12' 105.9(13) . . ? O9 Cl3 O10' 90.7(12) . . ? O10 Cl3 O10' 60.8(12) . . ? O12 Cl3 O10' 108.6(14) . . ? O11' Cl3 O10' 99.3(13) . . ? O11 Cl3 O10' 67.6(13) . . ? O12' Cl3 O10' 171.2(16) . . ? O8' O6 Cl2 64.5(17) . . ? O6' O7 O7' 138(3) . . ? O6' O7 Cl2 66.3(15) . . ? O7' O7 Cl2 73.4(19) . . ? Cl2 O8 O7' 67.3(18) . . ? Cl2 O8 O8' 54.0(10) . . ? O7' O8 O8' 100(2) . . ? O7 O6' Cl2 69.6(15) . . ? O7 O7' O8 112(3) . . ? O7 O7' Cl2 57.0(17) . . ? O8 O7' Cl2 55.5(16) . . ? O6 O8' Cl2 77.4(18) . . ? O6 O8' O8 136(2) . . ? Cl2 O8' O8 58.3(11) . . ? O11' O10 Cl3 71.7(18) . . ? O11' O10 O10' 137(3) . . ? Cl3 O10 O10' 66.3(15) . . ? O12 O11 Cl3 67.8(16) . . ? O12 O11 O10' 129(2) . . ? Cl3 O11 O10' 61.0(13) . . ? O11 O12 Cl3 71.2(17) . . ? O11 O12 O12' 130(2) . . ? Cl3 O12 O12' 59.1(12) . . ? O10 O10' Cl3 52.9(13) . . ? O10 O10' O11 89(2) . . ? Cl3 O10' O11 51.4(12) . . ? O10 O11' Cl3 69.3(17) . . ? Cl3 O12' O12 55.5(12) . . ? N7 C81 C82 163(3) . . ? C83 O13 C85 160(3) . . ? C84 C83 O13 114(3) . . ? C86 C85 O13 119(5) . . ? C89 O14 C87 132(3) . . ? C89 O14 C88' 138(3) . . ? C87 O14 C88' 48(2) . . ? C89 O14 C87' 112(3) . . ? C87 O14 C87' 104(3) . . ? C88' O14 C87' 57.1(15) . . ? C88' C87 O14 71(3) . . ? C88' C87 C88 57(2) . . ? O14 C87 C88 109(3) . . ? C90 C89 O14 120(3) . . ? O14' C89' C90' 113(4) . . ? O14' C87' C88' 145(6) . . ? O14' C87' O14 139(5) . . ? C88' C87' O14 60(3) . . ? C88' C88 C87 52(2) . . ? C87 C88' C88 71(3) . . ? C87 C88' C87' 122(4) . . ? C88 C88' C87' 119(4) . . ? C87 C88' O14 61(2) . . ? C88 C88' O14 111(3) . . ? C87' C88' O14 63(3) . . ? C89' O14' C87' 156(5) . . ? _diffrn_measured_fraction_theta_max 0.912 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.912 _refine_diff_density_max 1.402 _refine_diff_density_min -2.173 _refine_diff_density_rms 0.203 #===END data_mar128 _database_code_CSD 178375 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Complex 4(ClO4)3.1.5Et2O.CH3CN' ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C82 H74 Cl3 N7 O13.50 P3 Pt3 S3' _chemical_formula_weight 2254.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.134(3) _cell_length_b 13.463(3) _cell_length_c 25.340(5) _cell_angle_alpha 79.99(3) _cell_angle_beta 86.05(3) _cell_angle_gamma 70.32(3) _cell_volume 4154.5(14) _cell_formula_units_Z 2 _cell_measurement_temperature 301(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.802 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2202 _exptl_absorpt_coefficient_mu 5.335 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 301(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24391 _diffrn_reflns_av_R_equivalents 0.0624 _diffrn_reflns_av_sigmaI/netI 0.0936 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.61 _reflns_number_total 13020 _reflns_number_gt 8788 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1016P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13020 _refine_ls_number_parameters 950 _refine_ls_number_restraints 64 _refine_ls_R_factor_all 0.0862 _refine_ls_R_factor_gt 0.0580 _refine_ls_wR_factor_ref 0.1698 _refine_ls_wR_factor_gt 0.1516 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.978 _refine_ls_shift/su_max 0.024 _refine_ls_shift/su_mean 0.002 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 0.51948(3) 0.43398(3) 0.157872(17) 0.04570(14) Uani 1 1 d . . . Pt2 Pt 0.63677(4) 0.17983(3) 0.19861(2) 0.05514(16) Uani 1 1 d . . . Pt3 Pt 0.75606(4) -0.05921(3) 0.27594(2) 0.05540(16) Uani 1 1 d . . . S1 S 0.7827(3) 0.5375(3) 0.20519(18) 0.0835(11) Uani 1 1 d . . . S2 S 0.4724(4) 0.0586(3) 0.08912(18) 0.0996(14) Uani 1 1 d . . . S3 S 1.0679(3) -0.0089(3) 0.3007(2) 0.1041(15) Uani 1 1 d . . . P1 P 0.3819(2) 0.4382(2) 0.21620(12) 0.0458(7) Uani 1 1 d . . . P2 P 0.5371(2) 0.2175(2) 0.27265(12) 0.0526(7) Uani 1 1 d . . . P3 P 0.6216(2) -0.0188(2) 0.33682(12) 0.0519(7) Uani 1 1 d . . . N1 N 0.6416(7) 0.4345(6) 0.1041(4) 0.053(2) Uani 1 1 d . . . N2 N 0.4729(7) 0.3825(6) 0.0907(4) 0.050(2) Uani 1 1 d . . . N3 N 0.7152(10) 0.1336(8) 0.1301(4) 0.066(3) Uani 1 1 d . . . N4 N 0.7854(8) 0.2162(8) 0.2003(5) 0.073(3) Uani 1 1 d . . . N5 N 0.8735(8) -0.0968(7) 0.2201(5) 0.065(3) Uani 1 1 d . . . N6 N 0.6826(8) -0.1187(7) 0.2231(4) 0.058(3) Uani 1 1 d . . . C1 C 0.3827(10) 0.3565(9) 0.0842(5) 0.061(3) Uani 1 1 d . . . H1 H 0.3325 0.3609 0.1122 0.073 Uiso 1 1 calc R . . C2 C 0.3628(13) 0.3247(11) 0.0390(6) 0.079(4) Uani 1 1 d . . . H2 H 0.3014 0.3063 0.0362 0.094 Uiso 1 1 calc R . . C3 C 0.4356(13) 0.3207(11) -0.0015(6) 0.083(4) Uani 1 1 d . . . H3 H 0.4222 0.3017 -0.0332 0.099 Uiso 1 1 calc R . . C4 C 0.5247(12) 0.3426(10) 0.0024(5) 0.071(4) Uani 1 1 d . . . H4 H 0.5743 0.3366 -0.0259 0.086 Uiso 1 1 calc R . . C5 C 0.5450(9) 0.3751(8) 0.0491(5) 0.056(3) Uani 1 1 d . . . C6 C 0.6397(10) 0.4033(9) 0.0566(5) 0.060(3) Uani 1 1 d . . . C7 C 0.7273(13) 0.4033(12) 0.0226(7) 0.093(5) Uani 1 1 d . . . H7 H 0.7291 0.3822 -0.0106 0.111 Uiso 1 1 calc R . . C8 C 0.8072(13) 0.4315(14) 0.0352(8) 0.099(5) Uani 1 1 d . . . H8 H 0.8658 0.4266 0.0118 0.119 Uiso 1 1 calc R . . C9 C 0.8054(10) 0.4678(12) 0.0820(7) 0.084(4) Uani 1 1 d . . . H9 H 0.8597 0.4924 0.0902 0.101 Uiso 1 1 calc R . . C10 C 0.7211(10) 0.4671(9) 0.1170(6) 0.065(3) Uani 1 1 d . . . C11 C 0.7007(9) 0.4974(9) 0.1697(6) 0.060(3) Uani 1 1 d . . . C12 C 0.6106(10) 0.4871(8) 0.2013(5) 0.061(3) Uani 1 1 d . . . C13 C 0.6134(11) 0.5138(9) 0.2520(6) 0.068(3) Uani 1 1 d . . . H13 H 0.5607 0.5123 0.2784 0.082 Uiso 1 1 calc R . . C14 C 0.7015(11) 0.5422(10) 0.2589(7) 0.083(4) Uani 1 1 d . . . H14 H 0.7149 0.5622 0.2904 0.099 Uiso 1 1 calc R . . C15 C 0.8150(12) 0.2624(10) 0.2386(7) 0.084(4) Uani 1 1 d . . . H15 H 0.7651 0.2938 0.2637 0.101 Uiso 1 1 calc R . . C16 C 0.9220(12) 0.2607(12) 0.2386(9) 0.109(6) Uani 1 1 d . . . H16 H 0.9465 0.2836 0.2663 0.130 Uiso 1 1 calc R . . C17 C 0.9911(14) 0.2247(14) 0.1973(12) 0.144(11) Uani 1 1 d . . . H17 H 1.0604 0.2291 0.1959 0.173 Uiso 1 1 calc R . . C18 C 0.9598(12) 0.1828(13) 0.1584(9) 0.110(7) Uani 1 1 d . . . H18 H 1.0083 0.1567 0.1316 0.131 Uiso 1 1 calc R . . C19 C 0.8567(13) 0.1794(10) 0.1591(8) 0.090(5) Uani 1 1 d . . . C20 C 0.8178(14) 0.1405(12) 0.1208(7) 0.090(5) Uani 1 1 d . . . C21 C 0.8674(19) 0.1061(15) 0.0736(8) 0.140(10) Uani 1 1 d . . . H21 H 0.9370 0.1071 0.0649 0.168 Uiso 1 1 calc R . . C22 C 0.815(2) 0.0714(16) 0.0406(7) 0.133(10) Uani 1 1 d . . . H22 H 0.8493 0.0528 0.0085 0.160 Uiso 1 1 calc R . . C23 C 0.7154(17) 0.0621(13) 0.0519(7) 0.111(6) Uani 1 1 d . . . H23 H 0.6823 0.0341 0.0297 0.133 Uiso 1 1 calc R . . C24 C 0.6671(14) 0.0970(12) 0.0981(6) 0.087(5) Uani 1 1 d . . . C25 C 0.5617(13) 0.0987(10) 0.1195(6) 0.081(4) Uani 1 1 d . . . C26 C 0.5227(12) 0.1301(9) 0.1685(5) 0.069(4) Uani 1 1 d . . . C27 C 0.4184(10) 0.1207(9) 0.1813(6) 0.072(4) Uani 1 1 d . . . H27 H 0.3807 0.1373 0.2128 0.087 Uiso 1 1 calc R . . C28 C 0.3805(12) 0.0854(10) 0.1428(6) 0.081(4) Uani 1 1 d . . . H28 H 0.3132 0.0761 0.1445 0.097 Uiso 1 1 calc R . . C29 C 0.5871(10) -0.1337(10) 0.2250(5) 0.062(3) Uani 1 1 d . . . H29 H 0.5416 -0.1132 0.2538 0.074 Uiso 1 1 calc R . . C30 C 0.5507(12) -0.1762(11) 0.1886(6) 0.079(4) Uani 1 1 d . . . H30 H 0.4833 -0.1855 0.1922 0.095 Uiso 1 1 calc R . . C31 C 0.6209(11) -0.2059(10) 0.1444(5) 0.064(3) Uani 1 1 d . . . H31 H 0.5998 -0.2348 0.1179 0.076 Uiso 1 1 calc R . . C32 C 0.7106(14) -0.1931(10) 0.1414(6) 0.084(5) Uani 1 1 d . . . H32 H 0.7553 -0.2132 0.1122 0.101 Uiso 1 1 calc R . . C33 C 0.7484(11) -0.1496(10) 0.1798(5) 0.070(4) Uani 1 1 d . . . C34 C 0.8519(9) -0.1344(9) 0.1782(5) 0.062(3) Uani 1 1 d . . . C35 C 0.9329(13) -0.1594(11) 0.1370(7) 0.088(4) Uani 1 1 d . . . H35 H 0.9224 -0.1848 0.1066 0.106 Uiso 1 1 calc R . . C36 C 1.0304(15) -0.1422(14) 0.1466(9) 0.114(7) Uani 1 1 d . . . H36 H 1.0866 -0.1592 0.1218 0.137 Uiso 1 1 calc R . . C37 C 1.0462(12) -0.1035(13) 0.1886(8) 0.101(6) Uani 1 1 d . . . H37 H 1.1118 -0.0936 0.1925 0.122 Uiso 1 1 calc R . . C38 C 0.9658(11) -0.0777(9) 0.2265(7) 0.076(4) Uani 1 1 d . . . C39 C 0.9667(11) -0.0432(11) 0.2753(7) 0.081(4) Uani 1 1 d . . . C40 C 0.8753(10) -0.0232(9) 0.3100(6) 0.067(3) Uani 1 1 d . . . C41 C 0.8954(13) 0.0125(11) 0.3550(7) 0.091(5) Uani 1 1 d . . . H41 H 0.8455 0.0289 0.3827 0.109 Uiso 1 1 calc R . . C42 C 0.9944(13) 0.0209(12) 0.3544(7) 0.095(5) Uani 1 1 d . . . H42 H 1.0196 0.0421 0.3825 0.114 Uiso 1 1 calc R . . C43 C 0.2536(8) 0.4742(8) 0.1806(4) 0.050(3) Uani 1 1 d . . . C44 C 0.1813(10) 0.4184(10) 0.1912(6) 0.077(4) Uani 1 1 d . . . H44 H 0.1944 0.3591 0.2180 0.092 Uiso 1 1 calc R . . C45 C 0.0881(12) 0.4538(13) 0.1603(8) 0.110(6) Uani 1 1 d . . . H45 H 0.0377 0.4184 0.1676 0.132 Uiso 1 1 calc R . . C46 C 0.0683(12) 0.5401(13) 0.1192(8) 0.106(6) Uani 1 1 d . . . H46 H 0.0085 0.5592 0.0974 0.127 Uiso 1 1 calc R . . C47 C 0.1378(9) 0.5959(9) 0.1116(5) 0.063(3) Uani 1 1 d . . . H47 H 0.1231 0.6568 0.0856 0.076 Uiso 1 1 calc R . . C48 C 0.2302(9) 0.5642(9) 0.1417(5) 0.057(3) Uani 1 1 d . . . H48 H 0.2771 0.6036 0.1357 0.069 Uiso 1 1 calc R . . C49 C 0.3382(9) 0.5415(9) 0.2596(5) 0.053(3) Uani 1 1 d . . . C50 C 0.3535(10) 0.6377(8) 0.2437(5) 0.060(3) Uani 1 1 d . . . H50 H 0.3940 0.6480 0.2129 0.072 Uiso 1 1 calc R . . C51 C 0.3088(13) 0.7201(11) 0.2731(6) 0.084(4) Uani 1 1 d . . . H51 H 0.3209 0.7849 0.2627 0.101 Uiso 1 1 calc R . . C52 C 0.2476(14) 0.7063(12) 0.3171(7) 0.092(5) Uani 1 1 d . . . H52 H 0.2203 0.7610 0.3374 0.110 Uiso 1 1 calc R . . C53 C 0.2259(12) 0.6158(13) 0.3318(6) 0.090(5) Uani 1 1 d . . . H53 H 0.1799 0.6095 0.3609 0.108 Uiso 1 1 calc R . . C54 C 0.2724(10) 0.5291(11) 0.3035(6) 0.078(4) Uani 1 1 d . . . H54 H 0.2590 0.4649 0.3141 0.093 Uiso 1 1 calc R . . C55 C 0.4009(8) 0.3081(7) 0.2578(5) 0.053(3) Uani 1 1 d . . . H55A H 0.3639 0.3209 0.2917 0.064 Uiso 1 1 calc R . . H55B H 0.3641 0.2711 0.2405 0.064 Uiso 1 1 calc R . . C56 C 0.5834(11) 0.2675(9) 0.3250(5) 0.066(3) Uani 1 1 d . . . C57 C 0.5109(13) 0.3438(11) 0.3528(6) 0.087(4) Uani 1 1 d . . . H57 H 0.4377 0.3714 0.3446 0.104 Uiso 1 1 calc R . . C58 C 0.5526(17) 0.3774(13) 0.3939(7) 0.106(6) Uani 1 1 d . . . H58 H 0.5065 0.4302 0.4119 0.127 Uiso 1 1 calc R . . C59 C 0.6566(17) 0.3353(13) 0.4074(7) 0.106(6) Uani 1 1 d . . . H59 H 0.6824 0.3586 0.4346 0.127 Uiso 1 1 calc R . . C60 C 0.7248(13) 0.2577(13) 0.3813(7) 0.104(6) Uani 1 1 d . . . H60 H 0.7972 0.2283 0.3908 0.124 Uiso 1 1 calc R . . C61 C 0.6880(11) 0.2222(11) 0.3408(6) 0.077(4) Uani 1 1 d . . . H61 H 0.7349 0.1674 0.3243 0.093 Uiso 1 1 calc R . . C62 C 0.5086(8) 0.0991(7) 0.3101(4) 0.049(3) Uani 1 1 d . . . H62A H 0.4613 0.1218 0.3400 0.059 Uiso 1 1 calc R . . H62B H 0.4680 0.0766 0.2867 0.059 Uiso 1 1 calc R . . C63 C 0.5587(9) -0.1210(9) 0.3540(4) 0.052(3) Uani 1 1 d . . . C64 C 0.4529(11) -0.1002(10) 0.3659(5) 0.070(4) Uani 1 1 d . . . H64 H 0.4084 -0.0291 0.3613 0.084 Uiso 1 1 calc R . . C65 C 0.4069(13) -0.1768(12) 0.3844(7) 0.097(5) Uani 1 1 d . . . H65 H 0.3334 -0.1581 0.3925 0.117 Uiso 1 1 calc R . . C66 C 0.4701(16) -0.2800(14) 0.3906(7) 0.102(5) Uani 1 1 d . . . H66 H 0.4400 -0.3330 0.4038 0.122 Uiso 1 1 calc R . . C67 C 0.5808(17) -0.3090(10) 0.3776(7) 0.104(6) Uani 1 1 d . . . H67 H 0.6247 -0.3803 0.3812 0.125 Uiso 1 1 calc R . . C68 C 0.6214(12) -0.2277(10) 0.3594(6) 0.080(4) Uani 1 1 d . . . H68 H 0.6944 -0.2451 0.3503 0.096 Uiso 1 1 calc R . . C69 C 0.6464(10) -0.0064(10) 0.4044(5) 0.062(3) Uani 1 1 d . . . C70 C 0.7295(12) -0.0864(12) 0.4322(6) 0.083(4) Uani 1 1 d . . . H70 H 0.7753 -0.1406 0.4149 0.100 Uiso 1 1 calc R . . C71 C 0.7448(17) -0.0864(16) 0.4854(7) 0.114(6) Uani 1 1 d . . . H71 H 0.8011 -0.1403 0.5041 0.137 Uiso 1 1 calc R . . C72 C 0.6773(17) -0.0073(17) 0.5105(7) 0.110(6) Uani 1 1 d . . . H72 H 0.6869 -0.0080 0.5466 0.131 Uiso 1 1 calc R . . C73 C 0.5997(16) 0.0692(15) 0.4845(7) 0.109(6) Uani 1 1 d . . . H73 H 0.5554 0.1239 0.5020 0.131 Uiso 1 1 calc R . . C74 C 0.5820(12) 0.0704(11) 0.4312(5) 0.077(4) Uani 1 1 d . . . H74 H 0.5248 0.1249 0.4135 0.093 Uiso 1 1 calc R . . Cl1 Cl 0.3312(3) 0.8195(3) 0.10030(14) 0.0794(10) Uani 1 1 d . . . Cl2 Cl 0.1905(3) 0.2086(4) 0.3463(2) 0.1059(14) Uani 1 1 d D . . Cl3 Cl 1.1142(3) 0.2413(4) 0.00983(17) 0.0915(11) Uani 1 1 d D . . O1 O 0.2553(8) 0.7908(7) 0.0739(4) 0.088(3) Uiso 1 1 d . . . O2 O 0.2899(9) 0.8612(9) 0.1481(5) 0.117(4) Uiso 1 1 d . . . O3 O 0.3847(9) 0.8806(8) 0.0652(4) 0.104(3) Uiso 1 1 d . . . O4 O 0.4199(9) 0.7209(9) 0.1188(5) 0.107(3) Uiso 1 1 d . . . O5 O 0.2874(15) 0.208(2) 0.3722(9) 0.101(7) Uiso 0.50 1 d PD . . O6 O 0.185(2) 0.1070(16) 0.3746(11) 0.136(9) Uiso 0.50 1 d PD . . O7 O 0.2354(19) 0.1692(18) 0.2958(7) 0.113(7) Uiso 0.50 1 d PD . . O8 O 0.141(3) 0.3104(18) 0.3136(12) 0.167(13) Uiso 0.50 1 d PD . . O5' O 0.1171(18) 0.193(2) 0.3905(8) 0.125(8) Uiso 0.50 1 d PD . . O6' O 0.244(4) 0.0978(19) 0.340(2) 0.24(2) Uiso 0.50 1 d PD . . O7' O 0.2519(19) 0.2645(19) 0.3674(9) 0.108(8) Uiso 0.50 1 d PD . . O8' O 0.093(2) 0.266(3) 0.3172(15) 0.196(15) Uiso 0.50 1 d PD . . O9 O 1.2222(12) 0.1931(16) -0.0101(8) 0.091(6) Uiso 0.50 1 d PD . . O10 O 1.0360(16) 0.2017(19) -0.0082(9) 0.096(7) Uiso 0.50 1 d PD . . O11 O 1.113(2) 0.273(2) 0.0609(7) 0.125(8) Uiso 0.50 1 d PD . . O12 O 1.083(4) 0.3548(16) -0.0139(18) 0.203(17) Uiso 0.50 1 d PD . . O9' O 1.148(3) 0.164(2) 0.0565(10) 0.175(12) Uiso 0.50 1 d PD . . O10' O 1.179(3) 0.276(3) -0.0332(10) 0.170(12) Uiso 0.50 1 d PD . . O11' O 1.076(3) 0.346(2) 0.0290(18) 0.184(14) Uiso 0.50 1 d PD . . O12' O 1.018(2) 0.257(3) -0.0195(13) 0.168(14) Uiso 0.50 1 d PD . . N7 N 0.308(3) 0.470(3) 0.4787(14) 0.281(14) Uiso 1 1 d D . . C75 C 0.292(4) 0.380(3) 0.479(2) 0.32(2) Uiso 1 1 d D . . C76 C 0.322(11) 0.259(4) 0.497(5) 0.92(11) Uiso 1 1 d D . . O13 O 0.903(2) 0.582(2) 0.3287(14) 0.315(13) Uiso 1 1 d D . . C77 C 0.944(3) 0.674(3) 0.3094(14) 0.271(18) Uiso 1 1 d D . . C78 C 0.976(2) 0.628(2) 0.2591(12) 0.186(11) Uiso 1 1 d D . . C79 C 0.922(8) 0.568(5) 0.3875(17) 0.68(8) Uiso 1 1 d D . . C80 C 0.913(4) 0.456(4) 0.397(2) 0.36(3) Uiso 1 1 d D . . O14 O 0.0000 0.0000 0.5000 0.43(3) Uiso 1 2 d SD . . C81 C 0.087(3) -0.116(3) 0.4891(19) 0.31(2) Uiso 1 1 d D . . C82 C 0.094(4) -0.215(3) 0.4670(18) 0.31(2) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0382(2) 0.0461(2) 0.0543(3) -0.00419(18) -0.00153(18) -0.01766(18) Pt2 0.0521(3) 0.0466(3) 0.0608(3) -0.00109(19) 0.0028(2) -0.0131(2) Pt3 0.0491(3) 0.0519(3) 0.0604(3) -0.0042(2) 0.0002(2) -0.0130(2) S1 0.062(2) 0.082(2) 0.116(3) -0.005(2) -0.022(2) -0.0381(19) S2 0.127(4) 0.079(3) 0.092(3) -0.023(2) -0.036(3) -0.023(3) S3 0.061(2) 0.079(3) 0.171(5) -0.007(3) -0.022(3) -0.023(2) P1 0.0394(15) 0.0473(15) 0.0512(18) -0.0033(12) -0.0021(12) -0.0167(12) P2 0.0508(17) 0.0504(17) 0.0548(19) -0.0012(13) -0.0032(14) -0.0173(14) P3 0.0543(17) 0.0512(17) 0.0482(18) -0.0028(13) -0.0011(14) -0.0172(14) N1 0.049(6) 0.041(5) 0.067(7) 0.006(4) -0.016(5) -0.017(4) N2 0.046(5) 0.034(5) 0.068(7) -0.005(4) -0.005(5) -0.010(4) N3 0.084(8) 0.050(6) 0.057(7) -0.006(5) -0.003(6) -0.013(6) N4 0.052(6) 0.055(6) 0.098(9) 0.022(6) 0.005(6) -0.018(5) N5 0.052(6) 0.045(6) 0.086(8) -0.004(5) 0.003(6) -0.003(5) N6 0.066(7) 0.047(5) 0.048(6) 0.002(4) -0.001(5) -0.005(5) C1 0.057(8) 0.062(7) 0.066(9) -0.010(6) -0.004(6) -0.023(6) C2 0.084(10) 0.077(9) 0.083(11) -0.029(8) -0.009(9) -0.028(8) C3 0.098(12) 0.094(11) 0.065(10) -0.032(8) -0.017(9) -0.030(9) C4 0.084(10) 0.086(9) 0.044(8) -0.017(6) -0.001(7) -0.025(8) C5 0.053(7) 0.044(7) 0.059(8) 0.005(5) -0.007(6) -0.005(5) C6 0.050(7) 0.043(7) 0.076(10) -0.002(6) -0.001(6) -0.004(5) C7 0.080(11) 0.103(12) 0.083(11) -0.013(9) 0.040(9) -0.023(9) C8 0.065(10) 0.121(13) 0.117(16) -0.018(11) 0.029(10) -0.046(10) C9 0.048(8) 0.118(12) 0.092(12) -0.013(9) 0.008(8) -0.038(8) C10 0.048(7) 0.062(8) 0.075(10) 0.012(6) -0.007(6) -0.015(6) C11 0.049(7) 0.047(7) 0.087(10) 0.000(6) -0.008(6) -0.023(5) C12 0.058(7) 0.036(6) 0.087(10) -0.007(6) -0.013(7) -0.011(5) C13 0.071(9) 0.072(8) 0.074(10) -0.019(7) -0.016(7) -0.033(7) C14 0.069(9) 0.077(9) 0.104(12) -0.022(8) -0.041(8) -0.014(7) C15 0.071(10) 0.060(8) 0.127(14) -0.014(8) -0.014(9) -0.028(7) C16 0.054(9) 0.081(11) 0.19(2) -0.001(11) -0.010(11) -0.027(8) C17 0.050(10) 0.072(12) 0.29(3) 0.031(14) 0.017(15) -0.030(9) C18 0.045(9) 0.087(12) 0.20(2) -0.020(12) 0.023(11) -0.029(8) C19 0.071(10) 0.044(8) 0.132(15) 0.000(8) 0.039(10) -0.007(7) C20 0.096(13) 0.063(9) 0.087(12) 0.012(8) 0.029(10) -0.013(9) C21 0.16(2) 0.113(15) 0.072(13) 0.015(11) 0.068(14) 0.026(13) C22 0.17(2) 0.117(15) 0.047(11) 0.003(10) 0.038(14) 0.018(14) C23 0.129(16) 0.101(13) 0.065(11) -0.005(9) 0.011(11) 0.006(11) C24 0.094(12) 0.076(10) 0.062(10) 0.008(7) 0.011(9) -0.001(9) C25 0.105(12) 0.047(8) 0.078(11) -0.013(6) -0.027(9) -0.003(7) C26 0.096(10) 0.039(7) 0.059(8) -0.007(5) -0.018(7) -0.004(6) C27 0.054(8) 0.061(8) 0.106(12) -0.013(7) -0.017(7) -0.022(6) C28 0.080(10) 0.063(8) 0.108(12) -0.009(7) -0.036(9) -0.030(7) C29 0.065(8) 0.083(9) 0.045(7) -0.012(6) -0.010(6) -0.031(7) C30 0.082(10) 0.081(9) 0.070(10) -0.009(7) -0.006(8) -0.022(8) C31 0.059(8) 0.077(9) 0.056(8) -0.023(6) -0.019(7) -0.014(7) C32 0.108(13) 0.054(8) 0.063(9) -0.013(6) -0.003(9) 0.012(8) C33 0.074(9) 0.066(8) 0.060(9) 0.001(6) 0.002(7) -0.018(7) C34 0.042(7) 0.047(7) 0.078(9) -0.005(6) 0.001(6) 0.004(5) C35 0.083(11) 0.084(10) 0.092(12) -0.020(8) 0.018(9) -0.020(8) C36 0.095(14) 0.093(13) 0.146(19) -0.026(12) 0.052(13) -0.026(10) C37 0.057(9) 0.085(11) 0.154(18) -0.030(11) 0.037(11) -0.015(8) C38 0.062(9) 0.044(7) 0.115(13) -0.004(7) 0.008(8) -0.013(6) C39 0.068(9) 0.065(9) 0.105(13) 0.004(8) -0.013(8) -0.020(7) C40 0.047(7) 0.047(7) 0.102(11) -0.004(6) -0.004(7) -0.013(6) C41 0.081(11) 0.086(10) 0.115(14) -0.005(9) -0.031(9) -0.041(8) C42 0.089(11) 0.096(11) 0.111(14) -0.002(9) -0.051(10) -0.040(9) C43 0.037(6) 0.048(6) 0.062(7) -0.001(5) -0.003(5) -0.015(5) C44 0.067(8) 0.075(8) 0.091(11) 0.024(7) -0.019(8) -0.041(7) C45 0.069(10) 0.129(13) 0.145(17) 0.021(12) -0.029(10) -0.066(10) C46 0.061(9) 0.121(13) 0.136(16) 0.021(11) -0.039(10) -0.043(9) C47 0.051(7) 0.058(7) 0.077(9) 0.004(6) -0.015(6) -0.017(6) C48 0.047(7) 0.059(7) 0.070(8) -0.007(6) -0.012(6) -0.023(5) C49 0.044(6) 0.059(7) 0.051(7) -0.011(5) -0.005(5) -0.009(5) C50 0.068(8) 0.041(6) 0.073(9) 0.001(5) -0.008(6) -0.026(6) C51 0.107(12) 0.079(10) 0.081(11) -0.029(8) 0.005(9) -0.042(9) C52 0.112(13) 0.068(10) 0.092(12) -0.029(8) -0.002(10) -0.017(9) C53 0.083(10) 0.113(13) 0.069(10) -0.035(9) 0.024(8) -0.022(9) C54 0.067(9) 0.080(9) 0.084(11) -0.017(7) 0.004(8) -0.021(7) C55 0.053(7) 0.045(6) 0.063(8) -0.006(5) 0.004(6) -0.021(5) C56 0.079(9) 0.056(7) 0.067(9) -0.007(6) -0.002(7) -0.030(7) C57 0.101(11) 0.085(10) 0.071(10) -0.015(8) -0.014(8) -0.023(9) C58 0.153(18) 0.094(12) 0.085(12) -0.028(9) -0.018(12) -0.048(12) C59 0.158(18) 0.095(12) 0.081(12) -0.015(9) -0.054(12) -0.051(12) C60 0.094(12) 0.100(12) 0.125(15) -0.035(11) -0.053(11) -0.023(10) C61 0.066(9) 0.071(9) 0.098(11) -0.003(7) -0.008(8) -0.029(7) C62 0.056(7) 0.048(6) 0.041(6) 0.001(4) -0.005(5) -0.017(5) C63 0.061(7) 0.058(7) 0.044(7) -0.005(5) 0.001(5) -0.029(6) C64 0.078(9) 0.063(8) 0.080(10) -0.011(6) -0.001(7) -0.038(7) C65 0.087(11) 0.074(10) 0.140(15) -0.023(9) 0.032(10) -0.042(9) C66 0.134(16) 0.099(13) 0.100(13) -0.007(9) 0.013(11) -0.080(12) C67 0.162(18) 0.037(8) 0.104(13) 0.000(7) 0.003(12) -0.028(10) C68 0.084(10) 0.066(9) 0.087(11) -0.010(7) -0.013(8) -0.020(8) C69 0.065(8) 0.069(8) 0.052(8) -0.001(6) -0.008(6) -0.028(7) C70 0.089(10) 0.090(10) 0.075(11) -0.007(8) -0.006(8) -0.038(9) C71 0.155(18) 0.127(15) 0.056(11) 0.016(10) -0.039(11) -0.048(13) C72 0.137(16) 0.136(17) 0.063(11) -0.006(11) -0.029(11) -0.054(14) C73 0.135(16) 0.113(13) 0.069(12) -0.023(10) 0.006(11) -0.025(12) C74 0.095(11) 0.078(9) 0.055(9) -0.001(7) -0.001(8) -0.029(8) Cl1 0.089(2) 0.101(3) 0.067(2) -0.0144(18) 0.0048(18) -0.056(2) Cl2 0.079(3) 0.124(3) 0.115(4) 0.012(3) -0.007(2) -0.048(2) Cl3 0.076(2) 0.131(3) 0.082(3) -0.027(2) 0.000(2) -0.047(2) _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 2.033(10) . ? Pt1 C12 2.046(12) . ? Pt1 N2 2.142(9) . ? Pt1 P1 2.246(3) . ? Pt2 N3 2.041(11) . ? Pt2 C26 2.070(14) . ? Pt2 N4 2.171(11) . ? Pt2 P2 2.244(3) . ? Pt3 N5 2.015(10) . ? Pt3 C40 2.068(13) . ? Pt3 N6 2.106(11) . ? Pt3 P3 2.250(3) . ? S1 C14 1.667(17) . ? S1 C11 1.718(13) . ? S2 C25 1.718(16) . ? S2 C28 1.758(17) . ? S3 C42 1.640(18) . ? S3 C39 1.741(16) . ? P1 C55 1.827(10) . ? P1 C49 1.839(11) . ? P1 C43 1.843(11) . ? P2 C56 1.813(13) . ? P2 C55 1.815(10) . ? P2 C62 1.846(10) . ? P3 C63 1.809(11) . ? P3 C69 1.812(13) . ? P3 C62 1.833(10) . ? N1 C10 1.339(15) . ? N1 C6 1.346(16) . ? N2 C5 1.362(14) . ? N2 C1 1.371(14) . ? N3 C24 1.31(2) . ? N3 C20 1.383(19) . ? N4 C15 1.380(18) . ? N4 C19 1.395(18) . ? N5 C34 1.336(16) . ? N5 C38 1.346(17) . ? N6 C29 1.331(15) . ? N6 C33 1.382(16) . ? C1 C2 1.361(18) . ? C2 C3 1.35(2) . ? C3 C4 1.313(18) . ? C4 C5 1.402(17) . ? C5 C6 1.450(16) . ? C6 C7 1.390(18) . ? C7 C8 1.30(2) . ? C8 C9 1.36(2) . ? C9 C10 1.372(17) . ? C10 C11 1.445(19) . ? C11 C12 1.416(17) . ? C12 C13 1.400(17) . ? C13 C14 1.367(17) . ? C15 C16 1.398(19) . ? C16 C17 1.38(3) . ? C17 C18 1.36(3) . ? C18 C19 1.37(2) . ? C19 C20 1.38(2) . ? C20 C21 1.40(2) . ? C21 C22 1.35(3) . ? C22 C23 1.37(3) . ? C23 C24 1.37(2) . ? C24 C25 1.45(2) . ? C25 C26 1.391(19) . ? C26 C27 1.427(18) . ? C27 C28 1.346(18) . ? C29 C30 1.357(18) . ? C30 C31 1.425(19) . ? C31 C32 1.242(19) . ? C32 C33 1.42(2) . ? C33 C34 1.438(18) . ? C34 C35 1.437(18) . ? C35 C36 1.42(2) . ? C36 C37 1.32(2) . ? C37 C38 1.38(2) . ? C38 C39 1.40(2) . ? C39 C40 1.415(19) . ? C40 C41 1.38(2) . ? C41 C42 1.342(19) . ? C43 C48 1.383(14) . ? C43 C44 1.384(15) . ? C44 C45 1.394(18) . ? C45 C46 1.38(2) . ? C46 C47 1.350(17) . ? C47 C48 1.378(15) . ? C49 C50 1.365(14) . ? C49 C54 1.381(17) . ? C50 C51 1.387(17) . ? C51 C52 1.35(2) . ? C52 C53 1.328(19) . ? C53 C54 1.416(18) . ? C56 C61 1.358(17) . ? C56 C57 1.400(18) . ? C57 C58 1.41(2) . ? C58 C59 1.33(2) . ? C59 C60 1.36(2) . ? C60 C61 1.38(2) . ? C63 C64 1.345(16) . ? C63 C68 1.382(16) . ? C64 C65 1.364(17) . ? C65 C66 1.35(2) . ? C66 C67 1.40(2) . ? C67 C68 1.371(19) . ? C69 C74 1.349(17) . ? C69 C70 1.377(17) . ? C70 C71 1.38(2) . ? C71 C72 1.36(2) . ? C72 C73 1.30(2) . ? C73 C74 1.38(2) . ? Cl1 O3 1.417(11) . ? Cl1 O2 1.420(12) . ? Cl1 O1 1.426(10) . ? Cl1 O4 1.468(11) . ? Cl2 O8' 1.431(16) . ? Cl2 O8 1.438(15) . ? Cl2 O6 1.453(15) . ? Cl2 O6' 1.454(16) . ? Cl2 O7' 1.454(14) . ? Cl2 O5' 1.459(14) . ? Cl2 O5 1.469(14) . ? Cl2 O7 1.479(14) . ? Cl3 O9' 1.418(16) . ? Cl3 O11 1.425(14) . ? Cl3 O10 1.437(13) . ? Cl3 O9 1.444(13) . ? Cl3 O10' 1.445(15) . ? Cl3 O12' 1.449(15) . ? Cl3 O12 1.469(16) . ? Cl3 O11' 1.485(15) . ? O5 O7' 0.74(3) . ? O6 O6' 1.13(5) . ? O6 O5' 1.31(3) . ? O7 O6' 1.32(5) . ? O8 O8' 1.00(4) . ? O9 O10' 1.14(3) . ? O10 O12' 0.72(4) . ? O11 O11' 1.15(4) . ? O11 O9' 1.40(3) . ? O12 O11' 1.07(5) . ? O12 O10' 1.46(4) . ? N7 C75 1.297(19) . ? C75 C76 1.53(2) . ? O13 C79 1.50(2) . ? O13 C77 1.504(19) . ? C77 C78 1.485(19) . ? C79 C80 1.53(2) . ? O14 C81 1.65(3) . ? O14 C81 1.65(3) 2_556 ? C81 C82 1.51(3) . ? 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 C12 80.9(5) . . ? N1 Pt1 N2 76.9(4) . . ? C12 Pt1 N2 157.8(5) . . ? N1 Pt1 P1 178.3(2) . . ? C12 Pt1 P1 99.1(4) . . ? N2 Pt1 P1 103.0(3) . . ? N3 Pt2 C26 80.6(5) . . ? N3 Pt2 N4 76.8(5) . . ? C26 Pt2 N4 157.4(5) . . ? N3 Pt2 P2 172.4(4) . . ? C26 Pt2 P2 92.2(4) . . ? N4 Pt2 P2 110.4(4) . . ? N5 Pt3 C40 80.6(5) . . ? N5 Pt3 N6 78.8(4) . . ? C40 Pt3 N6 159.1(5) . . ? N5 Pt3 P3 178.2(4) . . ? C40 Pt3 P3 101.1(4) . . ? N6 Pt3 P3 99.4(3) . . ? C14 S1 C11 92.2(6) . . ? C25 S2 C28 90.6(7) . . ? C42 S3 C39 90.9(8) . . ? C55 P1 C49 108.5(5) . . ? C55 P1 C43 106.5(5) . . ? C49 P1 C43 97.7(5) . . ? C55 P1 Pt1 111.9(4) . . ? C49 P1 Pt1 119.9(4) . . ? C43 P1 Pt1 110.8(4) . . ? C56 P2 C55 105.3(6) . . ? C56 P2 C62 102.1(5) . . ? C55 P2 C62 100.8(5) . . ? C56 P2 Pt2 121.7(5) . . ? C55 P2 Pt2 112.8(4) . . ? C62 P2 Pt2 111.7(4) . . ? C63 P3 C69 97.7(5) . . ? C63 P3 C62 102.7(5) . . ? C69 P3 C62 107.9(6) . . ? C63 P3 Pt3 112.8(4) . . ? C69 P3 Pt3 121.9(4) . . ? C62 P3 Pt3 111.5(4) . . ? C10 N1 C6 122.1(11) . . ? C10 N1 Pt1 118.6(9) . . ? C6 N1 Pt1 119.2(8) . . ? C5 N2 C1 116.8(10) . . ? C5 N2 Pt1 113.8(8) . . ? C1 N2 Pt1 129.4(8) . . ? C24 N3 C20 123.8(14) . . ? C24 N3 Pt2 118.6(11) . . ? C20 N3 Pt2 117.6(11) . . ? C15 N4 C19 120.8(14) . . ? C15 N4 Pt2 126.8(10) . . ? C19 N4 Pt2 112.2(11) . . ? C34 N5 C38 125.0(12) . . ? C34 N5 Pt3 117.3(9) . . ? C38 N5 Pt3 117.6(10) . . ? C29 N6 C33 116.0(11) . . ? C29 N6 Pt3 131.6(8) . . ? C33 N6 Pt3 112.4(9) . . ? C2 C1 N2 123.5(13) . . ? C3 C2 C1 117.4(14) . . ? C4 C3 C2 122.3(14) . . ? C3 C4 C5 120.0(13) . . ? N2 C5 C4 119.9(12) . . ? N2 C5 C6 116.0(11) . . ? C4 C5 C6 124.1(12) . . ? N1 C6 C7 115.8(13) . . ? N1 C6 C5 114.1(11) . . ? C7 C6 C5 130.0(14) . . ? C8 C7 C6 122.9(17) . . ? C7 C8 C9 120.6(15) . . ? C8 C9 C10 118.0(14) . . ? N1 C10 C9 120.4(14) . . ? N1 C10 C11 109.9(11) . . ? C9 C10 C11 129.7(13) . . ? C12 C11 C10 121.8(11) . . ? C12 C11 S1 110.6(10) . . ? C10 C11 S1 127.3(10) . . ? C13 C12 C11 110.9(11) . . ? C13 C12 Pt1 140.4(10) . . ? C11 C12 Pt1 108.7(9) . . ? C14 C13 C12 113.0(13) . . ? C13 C14 S1 113.2(12) . . ? N4 C15 C16 118.3(16) . . ? C17 C16 C15 120(2) . . ? C18 C17 C16 121.3(17) . . ? C17 C18 C19 119.8(19) . . ? C18 C19 C20 123.5(17) . . ? C18 C19 N4 119.7(19) . . ? C20 C19 N4 116.8(15) . . ? C19 C20 N3 116.1(14) . . ? C19 C20 C21 129(2) . . ? N3 C20 C21 115(2) . . ? C22 C21 C20 121(2) . . ? C21 C22 C23 123.1(19) . . ? C22 C23 C24 116(2) . . ? N3 C24 C23 122.1(18) . . ? N3 C24 C25 110.1(13) . . ? C23 C24 C25 128(2) . . ? C26 C25 C24 123.1(14) . . ? C26 C25 S2 112.2(13) . . ? C24 C25 S2 124.6(13) . . ? C25 C26 C27 112.0(13) . . ? C25 C26 Pt2 107.4(11) . . ? C27 C26 Pt2 140.5(10) . . ? C28 C27 C26 112.8(14) . . ? C27 C28 S2 112.4(12) . . ? N6 C29 C30 125.6(13) . . ? C29 C30 C31 116.5(14) . . ? C32 C31 C30 119.6(13) . . ? C31 C32 C33 123.5(14) . . ? N6 C33 C32 118.9(13) . . ? N6 C33 C34 115.8(13) . . ? C32 C33 C34 125.4(14) . . ? N5 C34 C35 118.8(13) . . ? N5 C34 C33 115.6(11) . . ? C35 C34 C33 125.6(14) . . ? C36 C35 C34 114.2(15) . . ? C37 C36 C35 124.1(17) . . ? C36 C37 C38 120.1(17) . . ? N5 C38 C37 117.8(16) . . ? N5 C38 C39 111.8(13) . . ? C37 C38 C39 130.1(16) . . ? C38 C39 C40 121.7(14) . . ? C38 C39 S3 128.1(12) . . ? C40 C39 S3 110.0(12) . . ? C41 C40 C39 110.7(13) . . ? C41 C40 Pt3 141.3(11) . . ? C39 C40 Pt3 108.0(11) . . ? C42 C41 C40 113.0(17) . . ? C41 C42 S3 115.3(13) . . ? C48 C43 C44 119.7(10) . . ? C48 C43 P1 116.1(8) . . ? C44 C43 P1 124.3(9) . . ? C43 C44 C45 117.9(12) . . ? C46 C45 C44 122.1(13) . . ? C47 C46 C45 118.5(14) . . ? C46 C47 C48 121.1(12) . . ? C47 C48 C43 120.6(11) . . ? C50 C49 C54 119.4(11) . . ? C50 C49 P1 120.3(9) . . ? C54 C49 P1 119.2(10) . . ? C49 C50 C51 120.2(12) . . ? C52 C51 C50 120.0(13) . . ? C53 C52 C51 121.1(14) . . ? C52 C53 C54 120.3(14) . . ? C49 C54 C53 118.8(13) . . ? P2 C55 P1 119.3(6) . . ? C61 C56 C57 119.9(14) . . ? C61 C56 P2 118.9(11) . . ? C57 C56 P2 120.9(11) . . ? C56 C57 C58 117.7(15) . . ? C59 C58 C57 121.6(17) . . ? C58 C59 C60 119.6(15) . . ? C59 C60 C61 121.1(15) . . ? C56 C61 C60 120.0(15) . . ? P3 C62 P2 119.2(6) . . ? C64 C63 C68 116.2(12) . . ? C64 C63 P3 123.7(9) . . ? C68 C63 P3 120.0(10) . . ? C63 C64 C65 124.1(13) . . ? C66 C65 C64 118.6(15) . . ? C65 C66 C67 121.1(14) . . ? C68 C67 C66 117.0(14) . . ? C67 C68 C63 123.0(15) . . ? C74 C69 C70 117.7(13) . . ? C74 C69 P3 124.1(10) . . ? C70 C69 P3 117.9(11) . . ? C69 C70 C71 120.2(15) . . ? C72 C71 C70 119.7(17) . . ? C73 C72 C71 120.6(17) . . ? C72 C73 C74 120.7(17) . . ? C69 C74 C73 121.1(14) . . ? O3 Cl1 O2 114.5(7) . . ? O3 Cl1 O1 113.3(6) . . ? O2 Cl1 O1 113.5(7) . . ? O3 Cl1 O4 102.7(7) . . ? O2 Cl1 O4 104.0(7) . . ? O1 Cl1 O4 107.5(6) . . ? O8' Cl2 O8 40.6(18) . . ? O8' Cl2 O6 110(2) . . ? O8 Cl2 O6 150(2) . . ? O8' Cl2 O6' 117(3) . . ? O8 Cl2 O6' 139(3) . . ? O6 Cl2 O6' 46(2) . . ? O8' Cl2 O7' 121(2) . . ? O8 Cl2 O7' 83.9(18) . . ? O6 Cl2 O7' 121.2(16) . . ? O6' Cl2 O7' 119(2) . . ? O8' Cl2 O5' 84.2(19) . . ? O8 Cl2 O5' 109.0(18) . . ? O6 Cl2 O5' 53.5(13) . . ? O6' Cl2 O5' 99(2) . . ? O7' Cl2 O5' 103.1(15) . . ? O8' Cl2 O5 150(2) . . ? O8 Cl2 O5 110.4(18) . . ? O6 Cl2 O5 98.0(15) . . ? O6' Cl2 O5 90(2) . . ? O7' Cl2 O5 29.3(11) . . ? O5' Cl2 O5 104.8(14) . . ? O8' Cl2 O7 86.2(19) . . ? O8 Cl2 O7 86.4(17) . . ? O6 Cl2 O7 95.9(16) . . ? O6' Cl2 O7 53(2) . . ? O7' Cl2 O7 113.8(14) . . ? O5' Cl2 O7 141.4(14) . . ? O5 Cl2 O7 102.2(13) . . ? O9' Cl3 O11 58.9(15) . . ? O9' Cl3 O10 98.1(17) . . ? O11 Cl3 O10 125.4(14) . . ? O9' Cl3 O9 85.1(16) . . ? O11 Cl3 O9 112.8(14) . . ? O10 Cl3 O9 113.3(13) . . ? O9' Cl3 O10' 129(2) . . ? O11 Cl3 O10' 119.3(17) . . ? O10 Cl3 O10' 113.2(17) . . ? O9 Cl3 O10' 46.6(14) . . ? O9' Cl3 O12' 124(2) . . ? O11 Cl3 O12' 123.9(18) . . ? O10 Cl3 O12' 28.7(15) . . ? O9 Cl3 O12' 123.2(17) . . ? O10' Cl3 O12' 100(2) . . ? O9' Cl3 O12 147(2) . . ? O11 Cl3 O12 88(2) . . ? O10 Cl3 O12 106(2) . . ? O9 Cl3 O12 105.2(19) . . ? O10' Cl3 O12 60.2(19) . . ? O12' Cl3 O12 78(2) . . ? O9' Cl3 O11' 105(2) . . ? O11 Cl3 O11' 46.5(16) . . ? O10 Cl3 O11' 118.8(18) . . ? O9 Cl3 O11' 124.3(17) . . ? O10' Cl3 O11' 94(2) . . ? O12' Cl3 O11' 96(2) . . ? O12 Cl3 O11' 42.6(19) . . ? O7' O5 Cl2 74.2(15) . . ? O6' O6 O5' 130.4(19) . . ? O6' O6 Cl2 67.1(14) . . ? O5' O6 Cl2 63.5(10) . . ? O6' O7 Cl2 62.3(12) . . ? O8' O8 Cl2 69.3(14) . . ? O6 O5' Cl2 63.0(10) . . ? O6 O6' O7 125(3) . . ? O6 O6' Cl2 67.0(14) . . ? O7 O6' Cl2 64.2(13) . . ? O5 O7' Cl2 76.5(15) . . ? O8 O8' Cl2 70.1(14) . . ? O10' O9 Cl3 66.7(11) . . ? O12' O10 Cl3 76.6(17) . . ? O11' O11 O9' 129.5(18) . . ? O11' O11 Cl3 69.4(13) . . ? O9' O11 Cl3 60.3(10) . . ? O11' O12 O10' 114(3) . . ? O11' O12 Cl3 69.5(14) . . ? O10' O12 Cl3 59.1(11) . . ? O11 O9' Cl3 60.8(10) . . ? O9 O10' Cl3 66.7(11) . . ? O9 O10' O12 125.0(19) . . ? Cl3 O10' O12 60.7(12) . . ? O12 O11' O11 130(2) . . ? O12 O11' Cl3 67.9(13) . . ? O11 O11' Cl3 64.0(11) . . ? O10 O12' Cl3 74.7(16) . . ? N7 C75 C76 151(8) . . ? C79 O13 C77 100(3) . . ? C78 C77 O13 87(2) . . ? O13 C79 C80 93(4) . . ? C81 O14 C81 180(3) . 2_556 ? C82 C81 O14 142(4) . . ? _diffrn_measured_fraction_theta_max 0.832 _diffrn_reflns_theta_full 25.61 _diffrn_measured_fraction_theta_full 0.832 _refine_diff_density_max 1.602 _refine_diff_density_min -3.232 _refine_diff_density_rms 0.342 #===END