# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Andy Hor' _publ_contact_author_email ANDYHOR@NUS.EDU.SG _publ_section_title ; Unexpected Selectivity Difference in Geometric-Isomerism Between N,S- and N,N-Heterocyclic Carbenes in Cyclometallated Pt(II) ; loop_ _publ_author_name T.S.A.Hor 'Han Vinh Huynh.' 'Lip Lin Koh.' 'Swee Kuan Yen.' 'David Young' # Attachment '9035-complex_2_H.cif' data_9035 _database_code_depnum_ccdc_archive 'CCDC 740228' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H19 Br N2 Pt S' _chemical_formula_weight 606.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.5378(6) _cell_length_b 10.4418(5) _cell_length_c 15.9889(7) _cell_angle_alpha 90.00 _cell_angle_beta 111.4260(10) _cell_angle_gamma 90.00 _cell_volume 1948.56(16) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6061 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 2.067 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 9.366 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.0988 _exptl_absorpt_correction_T_max 0.2121 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12114 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4449 _reflns_number_gt 4010 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+1.0066P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4449 _refine_ls_number_parameters 236 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0314 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0735 _refine_ls_wR_factor_gt 0.0693 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.003 _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 0.788564(12) 0.510627(14) 0.862632(10) 0.02337(7) Uani 1 1 d . . . Br1 Br 0.77437(4) 0.73795(4) 0.80569(3) 0.03528(11) Uani 1 1 d . . . S1 S 0.75165(9) 0.44182(11) 0.65640(7) 0.0305(2) Uani 1 1 d . . . N1 N 0.5903(3) 0.4103(3) 0.7124(2) 0.0236(6) Uani 1 1 d . . . N2 N 0.8680(3) 0.5544(4) 0.9983(2) 0.0288(7) Uani 1 1 d . . . C1 C 0.6989(3) 0.4517(4) 0.7419(3) 0.0256(8) Uani 1 1 d . . . C2 C 0.5438(3) 0.3718(4) 0.6223(2) 0.0259(8) Uani 1 1 d . . . C3 C 0.4340(3) 0.3263(4) 0.5764(3) 0.0293(8) Uani 1 1 d . . . H3 H 0.3807 0.3179 0.6049 0.035 Uiso 1 1 calc R . . C4 C 0.4056(4) 0.2934(4) 0.4863(3) 0.0353(10) Uani 1 1 d . . . H4 H 0.3311 0.2643 0.4530 0.042 Uiso 1 1 calc R . . C5 C 0.4849(4) 0.3027(4) 0.4450(3) 0.0355(9) Uani 1 1 d . . . H5 H 0.4639 0.2780 0.3846 0.043 Uiso 1 1 calc R . . C6 C 0.5944(4) 0.3475(4) 0.4909(3) 0.0313(9) Uani 1 1 d . . . H6 H 0.6478 0.3550 0.4624 0.038 Uiso 1 1 calc R . . C7 C 0.6230(3) 0.3812(4) 0.5802(3) 0.0276(8) Uani 1 1 d . . . C8 C 0.5242(3) 0.4079(4) 0.7718(3) 0.0268(8) Uani 1 1 d . . . H8A H 0.5759 0.3864 0.8328 0.032 Uiso 1 1 calc R . . H8B H 0.4663 0.3402 0.7515 0.032 Uiso 1 1 calc R . . C9 C 0.4649(4) 0.5339(4) 0.7744(4) 0.0374(10) Uani 1 1 d . . . H9A H 0.5219 0.6027 0.7926 0.045 Uiso 1 1 calc R . . H9B H 0.4101 0.5540 0.7141 0.045 Uiso 1 1 calc R . . C10 C 0.4031(5) 0.5273(5) 0.8389(4) 0.0442(12) Uani 1 1 d . . . H10A H 0.3439 0.4621 0.8192 0.066 Uiso 1 1 calc R . . H10B H 0.3683 0.6096 0.8410 0.066 Uiso 1 1 calc R . . H10C H 0.4570 0.5058 0.8984 0.066 Uiso 1 1 calc R . . C11 C 0.8816(4) 0.6723(5) 1.0344(3) 0.0396(11) Uani 1 1 d . . . H11 H 0.8679 0.7437 0.9962 0.047 Uiso 1 1 calc R . . C12 C 0.9151(4) 0.6921(6) 1.1263(3) 0.0483(13) Uani 1 1 d . . . H12 H 0.9230 0.7757 1.1495 0.058 Uiso 1 1 calc R . . C13 C 0.9360(4) 0.5903(6) 1.1817(3) 0.0568(15) Uani 1 1 d . . . H13 H 0.9580 0.6025 1.2440 0.068 Uiso 1 1 calc R . . C14 C 0.9251(5) 0.4677(6) 1.1466(3) 0.0488(13) Uani 1 1 d . . . H14 H 0.9411 0.3964 1.1850 0.059 Uiso 1 1 calc R . . C15 C 0.8905(3) 0.4505(5) 1.0543(3) 0.0332(9) Uani 1 1 d . . . C16 C 0.8711(3) 0.3272(4) 1.0064(3) 0.0299(9) Uani 1 1 d . . . C17 C 0.9066(4) 0.2105(5) 1.0498(3) 0.0392(10) Uani 1 1 d . . . H17 H 0.9430 0.2085 1.1126 0.047 Uiso 1 1 calc R . . C18 C 0.8892(4) 0.0984(5) 1.0019(4) 0.0441(12) Uani 1 1 d . . . H18 H 0.9122 0.0198 1.0318 0.053 Uiso 1 1 calc R . . C19 C 0.8377(4) 0.1020(5) 0.9095(4) 0.0437(11) Uani 1 1 d . . . H19 H 0.8262 0.0253 0.8766 0.052 Uiso 1 1 calc R . . C20 C 0.8023(3) 0.2184(4) 0.8641(3) 0.0321(9) Uani 1 1 d . . . H20 H 0.7672 0.2190 0.8012 0.039 Uiso 1 1 calc R . . C21 C 0.8187(3) 0.3342(4) 0.9119(3) 0.0287(8) 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 0.01962(10) 0.03005(10) 0.01960(10) -0.00192(5) 0.00618(7) -0.00041(5) Br1 0.0338(2) 0.0320(2) 0.0397(2) 0.00292(17) 0.01313(19) 0.00073(17) S1 0.0232(5) 0.0462(6) 0.0232(5) -0.0040(4) 0.0098(4) -0.0037(4) N1 0.0241(16) 0.0277(16) 0.0176(15) 0.0010(12) 0.0060(13) -0.0017(13) N2 0.0204(16) 0.042(2) 0.0230(17) -0.0056(15) 0.0071(14) -0.0011(15) C1 0.0219(19) 0.033(2) 0.0209(19) 0.0016(16) 0.0066(15) 0.0040(16) C2 0.027(2) 0.031(2) 0.0191(18) 0.0003(15) 0.0079(15) 0.0017(16) C3 0.029(2) 0.036(2) 0.025(2) -0.0009(16) 0.0126(17) -0.0063(17) C4 0.031(2) 0.040(2) 0.028(2) -0.0027(18) 0.0025(18) -0.0085(19) C5 0.032(2) 0.044(2) 0.025(2) -0.0059(18) 0.0043(18) -0.0026(19) C6 0.036(2) 0.035(2) 0.025(2) -0.0034(16) 0.0137(18) 0.0014(18) C7 0.024(2) 0.036(2) 0.0211(19) 0.0000(16) 0.0065(16) 0.0002(16) C8 0.026(2) 0.034(2) 0.0214(19) 0.0004(15) 0.0092(16) -0.0029(16) C9 0.040(3) 0.036(2) 0.044(3) 0.001(2) 0.025(2) 0.003(2) C10 0.048(3) 0.044(3) 0.053(3) -0.008(2) 0.034(3) 0.003(2) C11 0.025(2) 0.050(3) 0.040(3) -0.015(2) 0.009(2) -0.0011(19) C12 0.034(3) 0.067(3) 0.038(3) -0.025(2) 0.006(2) 0.003(2) C13 0.038(3) 0.098(4) 0.027(3) -0.023(3) 0.004(2) 0.005(3) C14 0.037(3) 0.081(4) 0.023(2) 0.004(2) 0.006(2) 0.008(3) C15 0.018(2) 0.055(3) 0.025(2) -0.0012(19) 0.0055(17) 0.0044(19) C16 0.0194(19) 0.042(2) 0.028(2) 0.0051(17) 0.0080(17) 0.0012(17) C17 0.026(2) 0.056(3) 0.036(2) 0.013(2) 0.0123(19) 0.007(2) C18 0.032(2) 0.046(3) 0.056(3) 0.022(2) 0.019(2) 0.009(2) C19 0.036(2) 0.038(2) 0.063(3) 0.001(2) 0.024(2) 0.004(2) C20 0.027(2) 0.031(2) 0.036(2) -0.0025(17) 0.0085(18) -0.0001(16) C21 0.0196(19) 0.038(2) 0.030(2) 0.0028(17) 0.0112(17) 0.0026(16) _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 C1 1.946(4) . ? Pt1 C21 1.985(4) . ? Pt1 N2 2.080(3) . ? Pt1 Br1 2.5252(5) . ? S1 C1 1.725(4) . ? S1 C7 1.747(4) . ? N1 C1 1.340(5) . ? N1 C2 1.401(5) . ? N1 C8 1.471(5) . ? N2 C11 1.344(6) . ? N2 C15 1.368(6) . ? C2 C3 1.386(5) . ? C2 C7 1.392(5) . ? C3 C4 1.395(6) . ? C3 H3 0.9400 . ? C4 C5 1.383(6) . ? C4 H4 0.9400 . ? C5 C6 1.380(6) . ? C5 H5 0.9400 . ? C6 C7 1.385(5) . ? C6 H6 0.9400 . ? C8 C9 1.519(6) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 C10 1.502(6) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 C12 1.387(6) . ? C11 H11 0.9400 . ? C12 C13 1.347(8) . ? C12 H12 0.9400 . ? C13 C14 1.385(8) . ? C13 H13 0.9400 . ? C14 C15 1.389(6) . ? C14 H14 0.9400 . ? C15 C16 1.472(6) . ? C16 C17 1.392(6) . ? C16 C21 1.413(6) . ? C17 C18 1.372(7) . ? C17 H17 0.9400 . ? C18 C19 1.379(7) . ? C18 H18 0.9400 . ? C19 C20 1.402(6) . ? C19 H19 0.9400 . ? C20 C21 1.404(6) . ? C20 H20 0.9400 . ? 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 C1 Pt1 C21 93.29(17) . . ? C1 Pt1 N2 170.87(15) . . ? C21 Pt1 N2 80.85(16) . . ? C1 Pt1 Br1 90.02(12) . . ? C21 Pt1 Br1 173.56(11) . . ? N2 Pt1 Br1 96.51(11) . . ? C1 S1 C7 92.89(19) . . ? C1 N1 C2 116.2(3) . . ? C1 N1 C8 121.2(3) . . ? C2 N1 C8 122.5(3) . . ? C11 N2 C15 118.8(4) . . ? C11 N2 Pt1 125.9(3) . . ? C15 N2 Pt1 114.4(3) . . ? N1 C1 S1 109.7(3) . . ? N1 C1 Pt1 126.6(3) . . ? S1 C1 Pt1 123.7(2) . . ? C3 C2 C7 120.9(3) . . ? C3 C2 N1 127.1(3) . . ? C7 C2 N1 112.0(3) . . ? C2 C3 C4 117.5(4) . . ? C2 C3 H3 121.3 . . ? C4 C3 H3 121.3 . . ? C5 C4 C3 121.2(4) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C6 C5 C4 121.3(4) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 C7 117.8(4) . . ? C5 C6 H6 121.1 . . ? C7 C6 H6 121.1 . . ? C6 C7 C2 121.3(4) . . ? C6 C7 S1 129.5(3) . . ? C2 C7 S1 109.2(3) . . ? N1 C8 C9 113.6(3) . . ? N1 C8 H8A 108.8 . . ? C9 C8 H8A 108.8 . . ? N1 C8 H8B 108.8 . . ? C9 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? C10 C9 C8 111.1(4) . . ? C10 C9 H9A 109.4 . . ? C8 C9 H9A 109.4 . . ? C10 C9 H9B 109.4 . . ? C8 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C11 C12 122.2(5) . . ? N2 C11 H11 118.9 . . ? C12 C11 H11 118.9 . . ? C13 C12 C11 119.3(5) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C12 C13 C14 119.7(5) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C13 C14 C15 119.8(5) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? N2 C15 C14 120.1(5) . . ? N2 C15 C16 113.5(4) . . ? C14 C15 C16 126.4(5) . . ? C17 C16 C21 121.1(4) . . ? C17 C16 C15 123.0(4) . . ? C21 C16 C15 115.8(4) . . ? C18 C17 C16 120.8(4) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C17 C18 C19 119.4(4) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C18 C19 C20 120.9(5) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C19 C20 C21 120.6(4) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C20 C21 C16 117.1(4) . . ? C20 C21 Pt1 127.9(3) . . ? C16 C21 Pt1 114.8(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.916 _refine_diff_density_min -1.702 _refine_diff_density_rms 0.151 # Attachment '9039a-complexH.cif' data_9039a _database_code_depnum_ccdc_archive 'CCDC 740229' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H19 Br N2 Pt S' _chemical_formula_weight 654.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.3286(15) _cell_length_b 8.8431(8) _cell_length_c 15.6141(14) _cell_angle_alpha 90.00 _cell_angle_beta 99.632(2) _cell_angle_gamma 90.00 _cell_volume 2222.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 4645 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 25.53 _exptl_crystal_description PLATE _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.956 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 8.218 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1376 _exptl_absorpt_correction_T_max 0.7346 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15309 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5101 _reflns_number_gt 4350 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0275P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5101 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0670 _refine_ls_wR_factor_gt 0.0643 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _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 0.176241(10) 0.267420(16) 0.101016(9) 0.03690(6) Uani 1 1 d . . . Br1 Br 0.24875(3) 0.08075(5) 0.01728(3) 0.05495(13) Uani 1 1 d . . . S1 S 0.36089(8) 0.40001(14) 0.14741(8) 0.0577(3) Uani 1 1 d . . . N1 N 0.3009(2) 0.2627(3) 0.2634(2) 0.0399(8) Uani 1 1 d . . . N2 N 0.0601(2) 0.2429(3) 0.0249(2) 0.0394(8) Uani 1 1 d . . . C1 C 0.2800(3) 0.3018(4) 0.1792(3) 0.0407(9) Uani 1 1 d . . . C2 C 0.3798(3) 0.3090(5) 0.3050(3) 0.0458(10) Uani 1 1 d . . . C3 C 0.4151(3) 0.2847(5) 0.3909(3) 0.0601(12) Uani 1 1 d . . . H3 H 0.3874 0.2294 0.4280 0.072 Uiso 1 1 calc R . . C4 C 0.4924(4) 0.3452(8) 0.4194(4) 0.0810(16) Uani 1 1 d . . . H4 H 0.5169 0.3318 0.4772 0.097 Uiso 1 1 calc R . . C5 C 0.5349(4) 0.4254(8) 0.3647(5) 0.094(2) Uani 1 1 d . . . H5 H 0.5874 0.4638 0.3856 0.113 Uiso 1 1 calc R . . C6 C 0.4999(3) 0.4480(7) 0.2805(4) 0.0807(16) Uani 1 1 d . . . H6 H 0.5283 0.5022 0.2437 0.097 Uiso 1 1 calc R . . C7 C 0.4216(3) 0.3899(5) 0.2497(3) 0.0550(11) Uani 1 1 d . . . C8 C 0.2440(3) 0.1784(5) 0.3105(3) 0.0448(9) Uani 1 1 d . . . H8A H 0.1891 0.1756 0.2753 0.054 Uiso 1 1 calc R . . H8B H 0.2396 0.2313 0.3640 0.054 Uiso 1 1 calc R . . C1A C 0.2732(3) 0.0180(5) 0.3319(3) 0.0442(9) Uani 1 1 d . . . C2A C 0.2788(3) -0.0352(5) 0.4156(3) 0.0590(12) Uani 1 1 d . . . H2A H 0.2664 0.0282 0.4592 0.071 Uiso 1 1 calc R . . C3A C 0.3029(4) -0.1833(6) 0.4348(4) 0.0722(15) Uani 1 1 d . . . H3A H 0.3057 -0.2191 0.4913 0.087 Uiso 1 1 calc R . . C4A C 0.3225(4) -0.2774(6) 0.3720(4) 0.0722(16) Uani 1 1 d . . . H4A H 0.3397 -0.3760 0.3856 0.087 Uiso 1 1 calc R . . C5A C 0.3166(5) -0.2244(6) 0.2879(5) 0.0794(18) Uani 1 1 d . . . H5A H 0.3294 -0.2879 0.2446 0.095 Uiso 1 1 calc R . . C6A C 0.2917(3) -0.0769(5) 0.2680(3) 0.0607(13) Uani 1 1 d . . . H6A H 0.2873 -0.0421 0.2112 0.073 Uiso 1 1 calc R . . C11 C 0.0400(3) 0.1548(5) -0.0454(3) 0.0526(11) Uani 1 1 d . . . H11 H 0.0819 0.0998 -0.0647 0.063 Uiso 1 1 calc R . . C12 C -0.0395(3) 0.1419(5) -0.0903(3) 0.0637(13) Uani 1 1 d . . . H12 H -0.0509 0.0799 -0.1390 0.076 Uiso 1 1 calc R . . C13 C -0.1015(3) 0.2215(5) -0.0622(4) 0.0627(13) Uani 1 1 d . . . H13 H -0.1560 0.2138 -0.0909 0.075 Uiso 1 1 calc R . . C14 C -0.0819(3) 0.3137(5) 0.0095(3) 0.0534(11) Uani 1 1 d . . . H14 H -0.1236 0.3691 0.0290 0.064 Uiso 1 1 calc R . . C15 C -0.0013(3) 0.3246(5) 0.0528(3) 0.0427(9) Uani 1 1 d . . . C16 C 0.0272(3) 0.4184(4) 0.1285(2) 0.0406(9) Uani 1 1 d . . . C17 C -0.0258(3) 0.5128(5) 0.1660(3) 0.0530(11) Uani 1 1 d . . . H17 H -0.0821 0.5158 0.1429 0.064 Uiso 1 1 calc R . . C18 C 0.0047(3) 0.6008(5) 0.2361(3) 0.0609(13) Uani 1 1 d . . . H18 H -0.0309 0.6633 0.2607 0.073 Uiso 1 1 calc R . . C19 C 0.0877(3) 0.5966(5) 0.2701(3) 0.0598(12) Uani 1 1 d . . . H19 H 0.1082 0.6574 0.3174 0.072 Uiso 1 1 calc R . . C20 C 0.1416(3) 0.5027(4) 0.2348(3) 0.0488(10) Uani 1 1 d . . . H20 H 0.1977 0.5009 0.2589 0.059 Uiso 1 1 calc R . . C21 C 0.1124(2) 0.4114(4) 0.1635(2) 0.0379(8) 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 0.03624(10) 0.03599(9) 0.03780(10) 0.00170(6) 0.00428(7) -0.00008(6) Br1 0.0557(3) 0.0561(3) 0.0551(3) -0.0063(2) 0.0151(2) 0.0071(2) S1 0.0465(7) 0.0657(7) 0.0610(7) 0.0080(6) 0.0091(6) -0.0130(5) N1 0.0329(19) 0.0405(17) 0.0448(19) -0.0006(14) 0.0021(15) 0.0017(13) N2 0.041(2) 0.0372(17) 0.0383(18) 0.0035(13) 0.0006(15) -0.0030(14) C1 0.037(2) 0.0359(19) 0.049(2) -0.0013(17) 0.0072(18) 0.0010(16) C2 0.032(2) 0.046(2) 0.057(3) -0.010(2) 0.0007(19) 0.0050(18) C3 0.045(3) 0.070(3) 0.061(3) -0.009(2) -0.003(2) 0.005(2) C4 0.055(4) 0.109(5) 0.072(4) -0.010(4) -0.013(3) 0.001(3) C5 0.051(4) 0.121(5) 0.101(5) -0.025(4) -0.010(3) -0.019(3) C6 0.050(3) 0.093(4) 0.099(4) -0.008(4) 0.011(3) -0.023(3) C7 0.039(3) 0.056(3) 0.070(3) -0.005(2) 0.008(2) -0.006(2) C8 0.038(2) 0.051(2) 0.046(2) 0.0026(19) 0.0067(18) 0.0015(19) C1A 0.032(2) 0.049(2) 0.050(2) 0.0049(19) 0.0038(18) -0.0064(17) C2A 0.056(3) 0.063(3) 0.055(3) 0.013(2) 0.000(2) 0.004(2) C3A 0.070(4) 0.073(4) 0.072(4) 0.029(3) 0.005(3) -0.003(3) C4A 0.073(4) 0.051(3) 0.090(4) 0.014(3) 0.006(3) -0.002(2) C5A 0.100(5) 0.052(3) 0.090(5) -0.010(3) 0.028(4) -0.003(3) C6A 0.077(4) 0.049(3) 0.057(3) -0.002(2) 0.015(3) -0.010(2) C11 0.063(3) 0.047(2) 0.045(2) -0.003(2) 0.002(2) -0.003(2) C12 0.075(4) 0.058(3) 0.050(3) -0.002(2) -0.012(3) -0.015(3) C13 0.047(3) 0.070(3) 0.066(3) 0.015(3) -0.007(3) -0.015(2) C14 0.044(3) 0.060(3) 0.054(3) 0.014(2) 0.000(2) -0.003(2) C15 0.042(2) 0.041(2) 0.046(2) 0.0161(18) 0.0080(19) -0.0005(18) C16 0.043(2) 0.0369(19) 0.042(2) 0.0083(17) 0.0087(18) 0.0009(17) C17 0.047(3) 0.053(2) 0.060(3) 0.004(2) 0.011(2) 0.008(2) C18 0.062(3) 0.059(3) 0.065(3) -0.011(2) 0.022(3) 0.013(2) C19 0.072(4) 0.052(3) 0.054(3) -0.009(2) 0.008(3) 0.009(2) C20 0.051(3) 0.044(2) 0.049(2) -0.0030(19) 0.001(2) 0.0073(19) C21 0.038(2) 0.0323(18) 0.044(2) 0.0060(16) 0.0063(18) 0.0016(16) _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 C1 1.939(4) . ? Pt1 C21 2.000(4) . ? Pt1 N2 2.074(4) . ? Pt1 Br1 2.5208(5) . ? S1 C1 1.722(4) . ? S1 C7 1.736(5) . ? N1 C1 1.346(5) . ? N1 C2 1.403(5) . ? N1 C8 1.480(5) . ? N2 C11 1.342(5) . ? N2 C15 1.365(5) . ? C2 C3 1.385(7) . ? C2 C7 1.385(6) . ? C3 C4 1.376(7) . ? C3 H3 0.9300 . ? C4 C5 1.382(8) . ? C4 H4 0.9300 . ? C5 C6 1.358(8) . ? C5 H5 0.9300 . ? C6 C7 1.387(7) . ? C6 H6 0.9300 . ? C8 C1A 1.516(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C1A C6A 1.375(6) . ? C1A C2A 1.378(6) . ? C2A C3A 1.386(7) . ? C2A H2A 0.9300 . ? C3A C4A 1.365(9) . ? C3A H3A 0.9300 . ? C4A C5A 1.381(9) . ? C4A H4A 0.9300 . ? C5A C6A 1.386(7) . ? C5A H5A 0.9300 . ? C6A H6A 0.9300 . ? C11 C12 1.373(6) . ? C11 H11 0.9300 . ? C12 C13 1.364(7) . ? C12 H12 0.9300 . ? C13 C14 1.378(7) . ? C13 H13 0.9300 . ? C14 C15 1.379(6) . ? C14 H14 0.9300 . ? C15 C16 1.456(6) . ? C16 C17 1.399(5) . ? C16 C21 1.408(5) . ? C17 C18 1.367(6) . ? C17 H17 0.9300 . ? C18 C19 1.372(7) . ? C18 H18 0.9300 . ? C19 C20 1.389(6) . ? C19 H19 0.9300 . ? C20 C21 1.393(5) . ? C20 H20 0.9300 . ? 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 C1 Pt1 C21 93.71(16) . . ? C1 Pt1 N2 174.76(14) . . ? C21 Pt1 N2 81.08(15) . . ? C1 Pt1 Br1 89.58(11) . . ? C21 Pt1 Br1 176.65(11) . . ? N2 Pt1 Br1 95.62(9) . . ? C1 S1 C7 93.2(2) . . ? C1 N1 C2 116.1(3) . . ? C1 N1 C8 122.5(4) . . ? C2 N1 C8 121.4(4) . . ? C11 N2 C15 118.4(4) . . ? C11 N2 Pt1 127.2(3) . . ? C15 N2 Pt1 114.3(3) . . ? N1 C1 S1 109.2(3) . . ? N1 C1 Pt1 128.8(3) . . ? S1 C1 Pt1 121.9(2) . . ? C3 C2 C7 121.0(4) . . ? C3 C2 N1 127.1(4) . . ? C7 C2 N1 111.9(4) . . ? C4 C3 C2 117.6(5) . . ? C4 C3 H3 121.2 . . ? C2 C3 H3 121.2 . . ? C3 C4 C5 121.8(6) . . ? C3 C4 H4 119.1 . . ? C5 C4 H4 119.1 . . ? C6 C5 C4 120.1(5) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C7 119.6(6) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C2 C7 C6 119.8(5) . . ? C2 C7 S1 109.6(3) . . ? C6 C7 S1 130.6(4) . . ? N1 C8 C1A 112.3(3) . . ? N1 C8 H8A 109.1 . . ? C1A C8 H8A 109.1 . . ? N1 C8 H8B 109.1 . . ? C1A C8 H8B 109.1 . . ? H8A C8 H8B 107.9 . . ? C6A C1A C2A 119.5(4) . . ? C6A C1A C8 120.7(4) . . ? C2A C1A C8 119.8(4) . . ? C1A C2A C3A 119.9(5) . . ? C1A C2A H2A 120.0 . . ? C3A C2A H2A 120.0 . . ? C4A C3A C2A 120.8(5) . . ? C4A C3A H3A 119.6 . . ? C2A C3A H3A 119.6 . . ? C3A C4A C5A 119.3(5) . . ? C3A C4A H4A 120.4 . . ? C5A C4A H4A 120.4 . . ? C4A C5A C6A 120.3(5) . . ? C4A C5A H5A 119.9 . . ? C6A C5A H5A 119.9 . . ? C1A C6A C5A 120.2(5) . . ? C1A C6A H6A 119.9 . . ? C5A C6A H6A 119.9 . . ? N2 C11 C12 123.2(4) . . ? N2 C11 H11 118.4 . . ? C12 C11 H11 118.4 . . ? C13 C12 C11 118.8(5) . . ? C13 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? C12 C13 C14 118.9(5) . . ? C12 C13 H13 120.5 . . ? C14 C13 H13 120.5 . . ? C13 C14 C15 120.8(5) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? N2 C15 C14 119.9(4) . . ? N2 C15 C16 114.1(4) . . ? C14 C15 C16 126.0(4) . . ? C17 C16 C21 120.2(4) . . ? C17 C16 C15 122.9(4) . . ? C21 C16 C15 116.8(3) . . ? C18 C17 C16 120.5(4) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C17 C18 C19 119.8(4) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C18 C19 C20 120.9(5) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C19 C20 C21 120.6(4) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C20 C21 C16 118.0(3) . . ? C20 C21 Pt1 128.5(3) . . ? C16 C21 Pt1 113.6(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.387 _refine_diff_density_min -0.585 _refine_diff_density_rms 0.111 # Attachment '9048-complex_3H.cif' data_9048 _database_code_depnum_ccdc_archive 'CCDC 740230' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H26 Br N3 Pt' _chemical_formula_weight 727.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.4351(9) _cell_length_b 33.749(3) _cell_length_c 13.2500(10) _cell_angle_alpha 90.00 _cell_angle_beta 100.230(2) _cell_angle_gamma 90.00 _cell_volume 5472.2(7) _cell_formula_units_Z 8 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 4128 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 20.58 _exptl_crystal_description BLOCK _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.766 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2816 _exptl_absorpt_coefficient_mu 6.614 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1878 _exptl_absorpt_correction_T_max 0.7778 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38238 _diffrn_reflns_av_R_equivalents 0.0751 _diffrn_reflns_av_sigmaI/netI 0.0955 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 27.50 _reflns_number_total 12572 _reflns_number_gt 7482 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0384P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12572 _refine_ls_number_parameters 667 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1010 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1097 _refine_ls_wR_factor_gt 0.0953 _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_restrained_S_all 0.937 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.46129(2) 0.629964(9) 0.00630(2) 0.04551(9) Uani 1 1 d . . . Pt2 Pt 0.03127(2) 0.651182(9) 0.39399(2) 0.04995(10) Uani 1 1 d . . . Br1 Br 0.39939(6) 0.57362(2) -0.10468(6) 0.0643(2) Uani 1 1 d . . . Br4 Br -0.12758(7) 0.64939(3) 0.25674(7) 0.0820(3) Uani 1 1 d . . . N1 N 0.7038(4) 0.61685(18) -0.0008(5) 0.0510(15) Uani 1 1 d . . . N2 N 0.6387(4) 0.56828(18) 0.0794(4) 0.0509(15) Uani 1 1 d . . . N3 N 0.5019(4) 0.68042(17) 0.0864(4) 0.0459(14) Uani 1 1 d . . . N4 N 0.1634(5) 0.6086(2) 0.2522(4) 0.0541(16) Uani 1 1 d . . . N5 N 0.0832(4) 0.5672(2) 0.3359(5) 0.0570(16) Uani 1 1 d . . . N6 N 0.1555(5) 0.65479(19) 0.5151(5) 0.0549(16) Uani 1 1 d . . . C1 C 0.6121(5) 0.6033(2) 0.0335(5) 0.0468(17) Uani 1 1 d . . . C2 C 0.7878(5) 0.5893(3) 0.0207(6) 0.055(2) Uani 1 1 d . . . C3 C 0.8946(7) 0.5889(3) 0.0042(6) 0.079(3) Uani 1 1 d . . . H3 H 0.9234 0.6098 -0.0284 0.095 Uiso 1 1 calc R . . C4 C 0.9571(7) 0.5557(4) 0.0390(8) 0.090(3) Uani 1 1 d . . . H4 H 1.0287 0.5539 0.0279 0.107 Uiso 1 1 calc R . . C5 C 0.9144(8) 0.5254(4) 0.0896(7) 0.090(3) Uani 1 1 d . . . H5 H 0.9590 0.5039 0.1121 0.108 Uiso 1 1 calc R . . C6 C 0.8099(7) 0.5254(3) 0.1085(6) 0.074(3) Uani 1 1 d . . . H6 H 0.7817 0.5047 0.1421 0.089 Uiso 1 1 calc R . . C7 C 0.7481(6) 0.5593(3) 0.0730(6) 0.057(2) Uani 1 1 d . . . C8 C 0.7122(6) 0.6530(2) -0.0572(6) 0.061(2) Uani 1 1 d . . . H8A H 0.7774 0.6670 -0.0250 0.073 Uiso 1 1 calc R . . H8B H 0.6499 0.6696 -0.0516 0.073 Uiso 1 1 calc R . . C9 C 0.7169(6) 0.6475(2) -0.1685(6) 0.057(2) Uani 1 1 d . . . C10 C 0.6455(7) 0.6230(3) -0.2307(8) 0.082(3) Uani 1 1 d . . . H10 H 0.5937 0.6088 -0.2027 0.099 Uiso 1 1 calc R . . C11 C 0.6491(8) 0.6190(4) -0.3336(9) 0.104(4) Uani 1 1 d . . . H11 H 0.6020 0.6015 -0.3740 0.124 Uiso 1 1 calc R . . C12 C 0.7217(9) 0.6406(4) -0.3758(8) 0.098(4) Uani 1 1 d . . . H12 H 0.7220 0.6388 -0.4458 0.118 Uiso 1 1 calc R . . C13 C 0.7932(9) 0.6646(3) -0.3175(9) 0.095(3) Uani 1 1 d . . . H13 H 0.8443 0.6786 -0.3468 0.114 Uiso 1 1 calc R . . C14 C 0.7910(7) 0.6687(3) -0.2129(8) 0.078(3) Uani 1 1 d . . . H14 H 0.8399 0.6857 -0.1732 0.094 Uiso 1 1 calc R . . C15 C 0.5667(6) 0.5438(2) 0.1262(6) 0.065(2) Uani 1 1 d . . . H15A H 0.5653 0.5175 0.0964 0.078 Uiso 1 1 calc R . . H15B H 0.4934 0.5545 0.1095 0.078 Uiso 1 1 calc R . . C16 C 0.5970(6) 0.5401(2) 0.2408(6) 0.058(2) Uani 1 1 d . . . C17 C 0.5527(7) 0.5088(3) 0.2892(7) 0.077(3) Uani 1 1 d . . . H17 H 0.5081 0.4904 0.2496 0.092 Uiso 1 1 calc R . . C18 C 0.5735(9) 0.5047(4) 0.3939(9) 0.110(4) Uani 1 1 d . . . H18 H 0.5439 0.4836 0.4248 0.132 Uiso 1 1 calc R . . C19 C 0.6388(11) 0.5322(5) 0.4530(9) 0.130(5) Uani 1 1 d . . . H19 H 0.6526 0.5301 0.5241 0.156 Uiso 1 1 calc R . . C20 C 0.6826(8) 0.5622(4) 0.4058(9) 0.113(4) Uani 1 1 d . . . H20 H 0.7280 0.5803 0.4455 0.135 Uiso 1 1 calc R . . C21 C 0.6619(7) 0.5668(3) 0.2998(7) 0.078(3) Uani 1 1 d . . . H21 H 0.6921 0.5879 0.2696 0.094 Uiso 1 1 calc R . . C22 C 0.5999(6) 0.6884(2) 0.1417(6) 0.060(2) Uani 1 1 d . . . H22 H 0.6526 0.6685 0.1508 0.072 Uiso 1 1 calc R . . C23 C 0.6270(7) 0.7254(3) 0.1866(6) 0.071(2) Uani 1 1 d . . . H23 H 0.6962 0.7300 0.2247 0.085 Uiso 1 1 calc R . . C24 C 0.5489(7) 0.7546(3) 0.1731(7) 0.080(3) Uani 1 1 d . . . H24 H 0.5660 0.7799 0.1993 0.096 Uiso 1 1 calc R . . C25 C 0.4449(6) 0.7465(3) 0.1206(6) 0.067(2) Uani 1 1 d . . . H25 H 0.3909 0.7658 0.1140 0.081 Uiso 1 1 calc R . . C26 C 0.4211(5) 0.7088(2) 0.0772(5) 0.0487(18) Uani 1 1 d . . . C27 C 0.3165(5) 0.6961(2) 0.0190(5) 0.0490(18) Uani 1 1 d . . . C28 C 0.2229(6) 0.7204(3) 0.0052(7) 0.069(2) Uani 1 1 d . . . H28 H 0.2262 0.7459 0.0319 0.083 Uiso 1 1 calc R . . C29 C 0.1269(6) 0.7057(3) -0.0481(7) 0.073(3) Uani 1 1 d . . . H29 H 0.0643 0.7213 -0.0571 0.088 Uiso 1 1 calc R . . C30 C 0.1218(6) 0.6688(3) -0.0880(6) 0.068(2) Uani 1 1 d . . . H30 H 0.0560 0.6596 -0.1252 0.082 Uiso 1 1 calc R . . C31 C 0.2133(6) 0.6441(2) -0.0744(6) 0.058(2) Uani 1 1 d . . . H31 H 0.2075 0.6184 -0.1002 0.069 Uiso 1 1 calc R . . C32 C 0.3139(5) 0.6580(2) -0.0220(5) 0.0447(17) Uani 1 1 d . . . C33 C 0.0962(5) 0.6064(3) 0.3213(5) 0.0529(19) Uani 1 1 d . . . C34 C 0.1941(6) 0.5710(3) 0.2221(6) 0.056(2) Uani 1 1 d . . . C35 C 0.2583(6) 0.5588(3) 0.1519(6) 0.073(3) Uani 1 1 d . . . H35 H 0.2923 0.5765 0.1140 0.088 Uiso 1 1 calc R . . C36 C 0.2677(8) 0.5183(4) 0.1427(9) 0.099(4) Uani 1 1 d . . . H36 H 0.3097 0.5086 0.0967 0.119 Uiso 1 1 calc R . . C37 C 0.2188(8) 0.4916(3) 0.1976(9) 0.097(4) Uani 1 1 d . . . H37 H 0.2281 0.4646 0.1877 0.117 Uiso 1 1 calc R . . C38 C 0.1548(7) 0.5041(3) 0.2685(8) 0.083(3) Uani 1 1 d . . . H38 H 0.1219 0.4862 0.3070 0.099 Uiso 1 1 calc R . . C39 C 0.1433(6) 0.5443(3) 0.2780(6) 0.059(2) Uani 1 1 d . . . C40 C 0.2000(6) 0.6462(2) 0.2138(6) 0.063(2) Uani 1 1 d . . . H40A H 0.1415 0.6655 0.2099 0.076 Uiso 1 1 calc R . . H40B H 0.2140 0.6421 0.1448 0.076 Uiso 1 1 calc R . . C41 C 0.3016(7) 0.6629(3) 0.2793(6) 0.062(2) Uani 1 1 d . . . C42 C 0.3012(9) 0.7002(3) 0.3138(7) 0.089(3) Uani 1 1 d . . . H42 H 0.2372 0.7151 0.2994 0.107 Uiso 1 1 calc R . . C43 C 0.3947(13) 0.7173(4) 0.3709(9) 0.118(4) Uani 1 1 d . . . H43 H 0.3952 0.7437 0.3907 0.142 Uiso 1 1 calc R . . C44 C 0.4859(10) 0.6941(5) 0.3970(9) 0.113(4) Uani 1 1 d . . . H44 H 0.5482 0.7046 0.4374 0.136 Uiso 1 1 calc R . . C45 C 0.4860(8) 0.6564(4) 0.3647(8) 0.107(4) Uani 1 1 d . . . H45 H 0.5485 0.6409 0.3820 0.129 Uiso 1 1 calc R . . C46 C 0.3935(8) 0.6406(3) 0.3060(7) 0.087(3) Uani 1 1 d . . . H46 H 0.3938 0.6144 0.2843 0.105 Uiso 1 1 calc R . . C47 C 0.0020(6) 0.5514(3) 0.3955(6) 0.067(2) Uani 1 1 d . . . H47A H -0.0100 0.5235 0.3798 0.081 Uiso 1 1 calc R . . H47B H -0.0670 0.5650 0.3747 0.081 Uiso 1 1 calc R . . C48 C 0.0383(6) 0.5562(3) 0.5095(6) 0.059(2) Uani 1 1 d . . . C49 C -0.0218(7) 0.5786(3) 0.5668(7) 0.074(3) Uani 1 1 d . . . H49 H -0.0859 0.5910 0.5353 0.088 Uiso 1 1 calc R . . C50 C 0.0143(9) 0.5826(3) 0.6728(8) 0.095(3) Uani 1 1 d . . . H50 H -0.0265 0.5972 0.7120 0.114 Uiso 1 1 calc R . . C51 C 0.1089(10) 0.5650(4) 0.7182(8) 0.097(3) Uani 1 1 d . . . H51 H 0.1332 0.5677 0.7884 0.116 Uiso 1 1 calc R . . C52 C 0.1684(8) 0.5433(3) 0.6598(8) 0.088(3) Uani 1 1 d . . . H52 H 0.2331 0.5314 0.6914 0.105 Uiso 1 1 calc R . . C53 C 0.1354(7) 0.5388(3) 0.5583(7) 0.071(2) Uani 1 1 d . . . H53 H 0.1775 0.5241 0.5205 0.085 Uiso 1 1 calc R . . C54 C 0.2474(7) 0.6318(3) 0.5266(7) 0.068(2) Uani 1 1 d . . . H54 H 0.2567 0.6146 0.4740 0.082 Uiso 1 1 calc R . . C55 C 0.3257(7) 0.6332(3) 0.6127(8) 0.080(3) Uani 1 1 d . . . H55 H 0.3871 0.6170 0.6189 0.096 Uiso 1 1 calc R . . C56 C 0.3129(8) 0.6584(3) 0.6891(8) 0.088(3) Uani 1 1 d . . . H56 H 0.3659 0.6597 0.7482 0.106 Uiso 1 1 calc R . . C57 C 0.2203(8) 0.6824(3) 0.6793(6) 0.077(3) Uani 1 1 d . . . H57 H 0.2108 0.6999 0.7313 0.092 Uiso 1 1 calc R . . C58 C 0.1433(6) 0.6798(3) 0.5908(6) 0.059(2) Uani 1 1 d . . . C59 C 0.0408(7) 0.7033(2) 0.5688(7) 0.065(2) Uani 1 1 d . . . C60 C 0.0140(8) 0.7336(3) 0.6334(7) 0.083(3) Uani 1 1 d . . . H60 H 0.0614 0.7399 0.6938 0.099 Uiso 1 1 calc R . . C61 C -0.0813(10) 0.7534(3) 0.6067(10) 0.100(4) Uani 1 1 d . . . H61 H -0.1000 0.7729 0.6502 0.120 Uiso 1 1 calc R . . C62 C -0.1496(9) 0.7455(3) 0.5183(10) 0.099(3) Uani 1 1 d . . . H62 H -0.2145 0.7596 0.5016 0.118 Uiso 1 1 calc R . . C63 C -0.1244(7) 0.7164(3) 0.4514(7) 0.073(3) Uani 1 1 d . . . H63 H -0.1724 0.7114 0.3905 0.088 Uiso 1 1 calc R . . C64 C -0.0264(6) 0.6946(2) 0.4756(6) 0.054(2) 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 0.03881(15) 0.04133(18) 0.05455(18) 0.00134(14) 0.00332(11) 0.00417(12) Pt2 0.04638(17) 0.0493(2) 0.05454(19) 0.00677(15) 0.01007(13) -0.00008(13) Br1 0.0602(5) 0.0493(5) 0.0779(6) -0.0105(4) -0.0029(4) 0.0036(4) Br4 0.0636(6) 0.0828(7) 0.0888(7) 0.0100(5) -0.0158(4) 0.0015(5) N1 0.042(3) 0.044(4) 0.067(4) -0.001(3) 0.012(3) 0.004(3) N2 0.041(3) 0.040(4) 0.067(4) 0.001(3) -0.003(3) 0.008(3) N3 0.044(3) 0.042(4) 0.052(4) -0.001(3) 0.010(3) 0.003(3) N4 0.054(4) 0.063(5) 0.045(4) -0.001(3) 0.007(3) -0.002(3) N5 0.047(4) 0.060(5) 0.061(4) 0.004(4) 0.001(3) -0.010(3) N6 0.063(4) 0.048(4) 0.055(4) 0.009(3) 0.014(3) -0.009(3) C1 0.044(4) 0.044(5) 0.052(4) -0.003(4) 0.006(3) -0.003(3) C2 0.036(4) 0.064(6) 0.060(5) -0.012(4) -0.003(3) 0.006(4) C3 0.059(6) 0.102(8) 0.075(6) -0.019(6) 0.008(4) 0.001(5) C4 0.047(5) 0.124(11) 0.093(7) -0.034(7) -0.001(5) 0.034(6) C5 0.077(7) 0.110(10) 0.073(7) -0.007(6) -0.010(5) 0.029(6) C6 0.066(6) 0.071(7) 0.078(6) -0.009(5) -0.010(4) 0.024(5) C7 0.050(5) 0.060(6) 0.057(5) -0.009(4) -0.004(4) 0.010(4) C8 0.063(5) 0.040(5) 0.081(6) -0.008(4) 0.019(4) -0.006(4) C9 0.047(4) 0.055(5) 0.073(6) 0.007(4) 0.020(4) 0.009(4) C10 0.076(6) 0.091(8) 0.086(7) -0.011(6) 0.029(5) -0.014(5) C11 0.071(7) 0.136(11) 0.103(9) -0.036(8) 0.013(6) -0.018(6) C12 0.092(8) 0.136(12) 0.068(7) -0.002(7) 0.017(6) 0.016(7) C13 0.110(9) 0.085(8) 0.097(8) 0.030(7) 0.044(7) 0.007(6) C14 0.073(6) 0.074(7) 0.090(7) 0.005(5) 0.023(5) -0.014(5) C15 0.066(5) 0.044(5) 0.082(6) 0.014(4) 0.007(4) -0.002(4) C16 0.050(5) 0.056(6) 0.065(5) -0.006(4) 0.007(4) 0.009(4) C17 0.066(6) 0.083(8) 0.081(7) 0.002(6) 0.010(5) 0.000(5) C18 0.109(9) 0.151(13) 0.076(8) 0.012(8) 0.033(7) 0.008(8) C19 0.107(10) 0.221(19) 0.065(8) -0.021(10) 0.022(7) 0.016(10) C20 0.073(7) 0.171(14) 0.092(9) -0.053(9) 0.008(6) -0.002(7) C21 0.070(6) 0.080(7) 0.082(7) -0.020(6) 0.006(5) -0.003(5) C22 0.042(4) 0.061(6) 0.074(5) -0.013(4) 0.000(4) -0.001(4) C23 0.064(6) 0.072(7) 0.072(6) -0.008(5) 0.001(4) -0.006(5) C24 0.091(7) 0.058(7) 0.089(7) -0.023(5) 0.014(5) -0.005(5) C25 0.065(6) 0.060(6) 0.075(6) -0.022(5) 0.009(4) 0.004(4) C26 0.043(4) 0.044(5) 0.059(5) -0.002(4) 0.009(3) 0.000(3) C27 0.045(4) 0.053(5) 0.051(4) 0.002(4) 0.015(3) 0.013(3) C28 0.051(5) 0.062(6) 0.098(7) -0.009(5) 0.019(4) 0.003(4) C29 0.042(5) 0.085(7) 0.091(7) -0.001(6) 0.007(4) 0.025(4) C30 0.037(4) 0.083(7) 0.081(6) -0.004(5) 0.002(4) 0.003(4) C31 0.044(4) 0.062(6) 0.066(5) -0.003(4) 0.006(4) 0.001(4) C32 0.039(4) 0.052(5) 0.045(4) 0.005(3) 0.013(3) 0.010(3) C33 0.042(4) 0.066(6) 0.048(4) 0.009(4) 0.001(3) -0.008(4) C34 0.053(5) 0.059(6) 0.053(5) -0.004(4) -0.001(4) -0.001(4) C35 0.047(5) 0.101(8) 0.069(6) -0.034(5) 0.003(4) 0.008(5) C36 0.072(7) 0.107(11) 0.112(9) -0.047(8) -0.002(6) 0.014(6) C37 0.077(7) 0.074(8) 0.127(10) -0.032(7) -0.018(6) 0.011(6) C38 0.077(6) 0.066(7) 0.097(7) -0.020(6) -0.005(5) -0.002(5) C39 0.050(5) 0.059(6) 0.062(5) -0.011(5) -0.006(4) -0.001(4) C40 0.069(5) 0.059(6) 0.065(5) 0.019(4) 0.022(4) 0.000(4) C41 0.060(5) 0.073(7) 0.057(5) 0.005(5) 0.020(4) -0.010(4) C42 0.105(8) 0.076(8) 0.084(7) -0.015(6) 0.007(6) 0.009(6) C43 0.167(13) 0.083(10) 0.103(9) -0.033(7) 0.018(9) -0.027(9) C44 0.090(9) 0.146(14) 0.098(9) -0.027(9) 0.005(7) -0.030(8) C45 0.071(7) 0.149(13) 0.097(8) -0.035(8) 0.004(6) 0.011(7) C46 0.064(6) 0.094(8) 0.105(8) -0.027(6) 0.017(5) -0.009(5) C47 0.062(5) 0.062(6) 0.075(6) 0.020(5) 0.005(4) -0.015(4) C48 0.060(5) 0.058(6) 0.055(5) 0.010(4) 0.004(4) -0.016(4) C49 0.067(6) 0.085(8) 0.068(6) 0.005(5) 0.010(5) -0.012(5) C50 0.118(9) 0.074(8) 0.095(8) -0.001(6) 0.028(7) -0.010(6) C51 0.111(9) 0.092(9) 0.079(7) 0.008(7) -0.004(7) -0.027(7) C52 0.070(7) 0.100(9) 0.087(8) 0.023(6) -0.005(6) -0.012(5) C53 0.066(6) 0.074(7) 0.070(6) 0.017(5) 0.008(4) 0.002(4) C54 0.074(6) 0.060(6) 0.071(6) 0.012(5) 0.014(5) 0.001(5) C55 0.068(6) 0.087(8) 0.081(7) 0.010(6) 0.000(5) 0.003(5) C56 0.077(7) 0.102(9) 0.080(7) 0.026(6) -0.003(5) -0.025(6) C57 0.088(7) 0.091(8) 0.052(5) -0.001(5) 0.014(5) -0.038(6) C58 0.071(6) 0.059(6) 0.050(5) -0.004(4) 0.020(4) -0.017(4) C59 0.083(6) 0.050(6) 0.069(6) -0.009(4) 0.035(5) -0.013(4) C60 0.088(7) 0.070(7) 0.095(7) -0.017(6) 0.031(6) -0.011(5) C61 0.128(10) 0.059(7) 0.133(10) -0.022(7) 0.077(8) -0.003(7) C62 0.099(8) 0.069(8) 0.140(10) 0.020(8) 0.057(8) 0.020(6) C63 0.081(6) 0.054(6) 0.093(7) 0.011(5) 0.037(5) 0.020(5) C64 0.068(5) 0.049(5) 0.051(5) 0.015(4) 0.023(4) 0.002(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N3 2.022(6) . ? Pt1 C32 2.037(6) . ? Pt1 C1 2.053(7) . ? Pt1 Br1 2.4431(9) . ? Pt2 N6 2.024(6) . ? Pt2 C64 2.025(8) . ? Pt2 C33 2.035(8) . ? Pt2 Br4 2.4366(9) . ? N1 C1 1.377(8) . ? N1 C2 1.391(9) . ? N1 C8 1.444(9) . ? N2 C1 1.344(9) . ? N2 C7 1.411(8) . ? N2 C15 1.437(9) . ? N3 C22 1.334(8) . ? N3 C26 1.379(8) . ? N4 C33 1.346(8) . ? N4 C34 1.402(10) . ? N4 C40 1.470(9) . ? N5 C33 1.351(9) . ? N5 C39 1.396(9) . ? N5 C47 1.487(9) . ? N6 C58 1.341(9) . ? N6 C54 1.367(10) . ? C2 C7 1.367(11) . ? C2 C3 1.384(10) . ? C3 C4 1.396(13) . ? C3 H3 0.9300 . ? C4 C5 1.380(14) . ? C4 H4 0.9300 . ? C5 C6 1.366(12) . ? C5 H5 0.9300 . ? C6 C7 1.412(11) . ? C6 H6 0.9300 . ? C8 C9 1.498(11) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.377(11) . ? C9 C14 1.377(11) . ? C10 C11 1.380(12) . ? C10 H10 0.9300 . ? C11 C12 1.357(14) . ? C11 H11 0.9300 . ? C12 C13 1.340(14) . ? C12 H12 0.9300 . ? C13 C14 1.398(12) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C16 1.504(10) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C21 1.360(11) . ? C16 C17 1.398(11) . ? C17 C18 1.372(13) . ? C17 H17 0.9300 . ? C18 C19 1.382(16) . ? C18 H18 0.9300 . ? C19 C20 1.354(17) . ? C19 H19 0.9300 . ? C20 C21 1.390(13) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.396(11) . ? C22 H22 0.9300 . ? C23 C24 1.375(12) . ? C23 H23 0.9300 . ? C24 C25 1.384(10) . ? C24 H24 0.9300 . ? C25 C26 1.404(10) . ? C25 H25 0.9300 . ? C26 C27 1.454(9) . ? C27 C32 1.394(10) . ? C27 C28 1.409(10) . ? C28 C29 1.368(11) . ? C28 H28 0.9300 . ? C29 C30 1.350(11) . ? C29 H29 0.9300 . ? C30 C31 1.395(10) . ? C30 H30 0.9300 . ? C31 C32 1.399(10) . ? C31 H31 0.9300 . ? C34 C39 1.387(11) . ? C34 C35 1.393(10) . ? C35 C36 1.379(13) . ? C35 H35 0.9300 . ? C36 C37 1.367(14) . ? C36 H36 0.9300 . ? C37 C38 1.401(13) . ? C37 H37 0.9300 . ? C38 C39 1.372(11) . ? C38 H38 0.9300 . ? C40 C41 1.509(11) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.342(12) . ? C41 C46 1.361(12) . ? C42 C43 1.394(14) . ? C42 H42 0.9300 . ? C43 C44 1.369(15) . ? C43 H43 0.9300 . ? C44 C45 1.344(16) . ? C44 H44 0.9300 . ? C45 C46 1.376(13) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C47 C48 1.506(10) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 C49 1.383(11) . ? C48 C53 1.393(10) . ? C49 C50 1.403(12) . ? C49 H49 0.9300 . ? C50 C51 1.359(14) . ? C50 H50 0.9300 . ? C51 C52 1.373(14) . ? C51 H51 0.9300 . ? C52 C53 1.344(12) . ? C52 H52 0.9300 . ? C53 H53 0.9300 . ? C54 C55 1.362(11) . ? C54 H54 0.9300 . ? C55 C56 1.353(13) . ? C55 H55 0.9300 . ? C56 C57 1.396(13) . ? C56 H56 0.9300 . ? C57 C58 1.379(11) . ? C57 H57 0.9300 . ? C58 C59 1.485(11) . ? C59 C64 1.394(11) . ? C59 C60 1.412(11) . ? C60 C61 1.352(13) . ? C60 H60 0.9300 . ? C61 C62 1.346(14) . ? C61 H61 0.9300 . ? C62 C63 1.393(13) . ? C62 H62 0.9300 . ? C63 C64 1.413(10) . ? C63 H63 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Pt1 C32 80.7(3) . . ? N3 Pt1 C1 98.1(2) . . ? C32 Pt1 C1 178.2(3) . . ? N3 Pt1 Br1 173.60(16) . . ? C32 Pt1 Br1 94.2(2) . . ? C1 Pt1 Br1 86.86(19) . . ? N6 Pt2 C64 80.0(3) . . ? N6 Pt2 C33 96.2(3) . . ? C64 Pt2 C33 175.9(3) . . ? N6 Pt2 Br4 175.41(19) . . ? C64 Pt2 Br4 95.7(2) . . ? C33 Pt2 Br4 88.03(19) . . ? C1 N1 C2 110.3(7) . . ? C1 N1 C8 126.2(6) . . ? C2 N1 C8 123.4(6) . . ? C1 N2 C7 108.9(6) . . ? C1 N2 C15 125.5(6) . . ? C7 N2 C15 125.6(6) . . ? C22 N3 C26 119.2(6) . . ? C22 N3 Pt1 125.3(5) . . ? C26 N3 Pt1 115.4(5) . . ? C33 N4 C34 112.1(7) . . ? C33 N4 C40 123.4(7) . . ? C34 N4 C40 124.4(6) . . ? C33 N5 C39 111.9(6) . . ? C33 N5 C47 122.5(7) . . ? C39 N5 C47 125.0(7) . . ? C58 N6 C54 118.5(7) . . ? C58 N6 Pt2 117.3(5) . . ? C54 N6 Pt2 124.0(6) . . ? N2 C1 N1 106.8(6) . . ? N2 C1 Pt1 127.4(5) . . ? N1 C1 Pt1 125.5(5) . . ? C7 C2 C3 121.2(8) . . ? C7 C2 N1 105.8(6) . . ? C3 C2 N1 132.9(8) . . ? C2 C3 C4 116.6(10) . . ? C2 C3 H3 121.7 . . ? C4 C3 H3 121.7 . . ? C5 C4 C3 121.1(9) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C6 C5 C4 123.4(10) . . ? C6 C5 H5 118.3 . . ? C4 C5 H5 118.3 . . ? C5 C6 C7 114.7(9) . . ? C5 C6 H6 122.6 . . ? C7 C6 H6 122.6 . . ? C2 C7 N2 108.1(7) . . ? C2 C7 C6 123.0(8) . . ? N2 C7 C6 128.9(8) . . ? N1 C8 C9 115.1(6) . . ? N1 C8 H8A 108.5 . . ? C9 C8 H8A 108.5 . . ? N1 C8 H8B 108.5 . . ? C9 C8 H8B 108.5 . . ? H8A C8 H8B 107.5 . . ? C10 C9 C14 117.7(8) . . ? C10 C9 C8 122.0(7) . . ? C14 C9 C8 120.2(8) . . ? C9 C10 C11 121.4(9) . . ? C9 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? C12 C11 C10 119.7(10) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C13 C12 C11 120.6(10) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C14 120.2(10) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C9 C14 C13 120.3(9) . . ? C9 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? N2 C15 C16 114.9(7) . . ? N2 C15 H15A 108.5 . . ? C16 C15 H15A 108.5 . . ? N2 C15 H15B 108.5 . . ? C16 C15 H15B 108.5 . . ? H15A C15 H15B 107.5 . . ? C21 C16 C17 118.6(8) . . ? C21 C16 C15 122.8(8) . . ? C17 C16 C15 118.5(8) . . ? C18 C17 C16 121.4(10) . . ? C18 C17 H17 119.3 . . ? C16 C17 H17 119.3 . . ? C17 C18 C19 119.5(12) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C20 C19 C18 119.0(12) . . ? C20 C19 H19 120.5 . . ? C18 C19 H19 120.5 . . ? C19 C20 C21 122.2(12) . . ? C19 C20 H20 118.9 . . ? C21 C20 H20 118.9 . . ? C16 C21 C20 119.4(10) . . ? C16 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? N3 C22 C23 122.9(7) . . ? N3 C22 H22 118.6 . . ? C23 C22 H22 118.6 . . ? C24 C23 C22 118.4(8) . . ? C24 C23 H23 120.8 . . ? C22 C23 H23 120.8 . . ? C23 C24 C25 119.8(9) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C24 C25 C26 119.8(8) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? N3 C26 C25 119.7(7) . . ? N3 C26 C27 114.3(7) . . ? C25 C26 C27 126.0(7) . . ? C32 C27 C28 121.6(7) . . ? C32 C27 C26 115.8(6) . . ? C28 C27 C26 122.6(7) . . ? C29 C28 C27 118.7(8) . . ? C29 C28 H28 120.6 . . ? C27 C28 H28 120.6 . . ? C30 C29 C28 120.9(7) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C29 C30 C31 121.3(8) . . ? C29 C30 H30 119.3 . . ? C31 C30 H30 119.3 . . ? C30 C31 C32 120.0(8) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C27 C32 C31 117.4(6) . . ? C27 C32 Pt1 113.5(5) . . ? C31 C32 Pt1 129.1(6) . . ? N4 C33 N5 104.8(7) . . ? N4 C33 Pt2 128.8(6) . . ? N5 C33 Pt2 126.3(5) . . ? C39 C34 C35 122.2(9) . . ? C39 C34 N4 105.3(7) . . ? C35 C34 N4 132.6(8) . . ? C36 C35 C34 114.9(10) . . ? C36 C35 H35 122.6 . . ? C34 C35 H35 122.6 . . ? C37 C36 C35 123.7(10) . . ? C37 C36 H36 118.2 . . ? C35 C36 H36 118.2 . . ? C36 C37 C38 121.1(11) . . ? C36 C37 H37 119.4 . . ? C38 C37 H37 119.4 . . ? C39 C38 C37 116.2(10) . . ? C39 C38 H38 121.9 . . ? C37 C38 H38 121.9 . . ? C38 C39 C34 122.0(8) . . ? C38 C39 N5 132.2(9) . . ? C34 C39 N5 105.8(7) . . ? N4 C40 C41 113.7(6) . . ? N4 C40 H40A 108.8 . . ? C41 C40 H40A 108.8 . . ? N4 C40 H40B 108.8 . . ? C41 C40 H40B 108.8 . . ? H40A C40 H40B 107.7 . . ? C42 C41 C46 119.0(9) . . ? C42 C41 C40 119.5(9) . . ? C46 C41 C40 121.5(9) . . ? C41 C42 C43 121.3(11) . . ? C41 C42 H42 119.4 . . ? C43 C42 H42 119.4 . . ? C44 C43 C42 118.4(12) . . ? C44 C43 H43 120.8 . . ? C42 C43 H43 120.8 . . ? C45 C44 C43 120.5(12) . . ? C45 C44 H44 119.8 . . ? C43 C44 H44 119.7 . . ? C44 C45 C46 119.9(11) . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C41 C46 C45 120.8(11) . . ? C41 C46 H46 119.6 . . ? C45 C46 H46 119.6 . . ? N5 C47 C48 112.5(6) . . ? N5 C47 H47A 109.1 . . ? C48 C47 H47A 109.1 . . ? N5 C47 H47B 109.1 . . ? C48 C47 H47B 109.1 . . ? H47A C47 H47B 107.8 . . ? C49 C48 C53 119.0(8) . . ? C49 C48 C47 120.9(8) . . ? C53 C48 C47 120.1(8) . . ? C48 C49 C50 119.6(9) . . ? C48 C49 H49 120.2 . . ? C50 C49 H49 120.2 . . ? C51 C50 C49 120.0(10) . . ? C51 C50 H50 120.0 . . ? C49 C50 H50 120.0 . . ? C50 C51 C52 119.6(10) . . ? C50 C51 H51 120.2 . . ? C52 C51 H51 120.2 . . ? C53 C52 C51 121.6(10) . . ? C53 C52 H52 119.2 . . ? C51 C52 H52 119.2 . . ? C52 C53 C48 120.2(9) . . ? C52 C53 H53 119.9 . . ? C48 C53 H53 119.9 . . ? C55 C54 N6 122.2(9) . . ? C55 C54 H54 118.9 . . ? N6 C54 H54 118.9 . . ? C56 C55 C54 119.2(9) . . ? C56 C55 H55 120.4 . . ? C54 C55 H55 120.4 . . ? C55 C56 C57 120.0(9) . . ? C55 C56 H56 120.0 . . ? C57 C56 H56 120.0 . . ? C58 C57 C56 118.7(9) . . ? C58 C57 H57 120.7 . . ? C56 C57 H57 120.7 . . ? N6 C58 C57 121.5(8) . . ? N6 C58 C59 113.4(7) . . ? C57 C58 C59 125.1(8) . . ? C64 C59 C60 121.5(9) . . ? C64 C59 C58 114.8(7) . . ? C60 C59 C58 123.7(9) . . ? C61 C60 C59 119.4(10) . . ? C61 C60 H60 120.3 . . ? C59 C60 H60 120.3 . . ? C62 C61 C60 121.1(10) . . ? C62 C61 H61 119.4 . . ? C60 C61 H61 119.4 . . ? C61 C62 C63 121.0(11) . . ? C61 C62 H62 119.5 . . ? C63 C62 H62 119.5 . . ? C62 C63 C64 120.4(10) . . ? C62 C63 H63 119.8 . . ? C64 C63 H63 119.8 . . ? C59 C64 C63 116.6(8) . . ? C59 C64 Pt2 114.4(6) . . ? C63 C64 Pt2 129.0(7) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.444 _refine_diff_density_min -0.821 _refine_diff_density_rms 0.132