# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address T.Calvet ; Centre Cient\'ific i Tecnol\`olic Universitat de Barcelona So\'e i Sabar\'is 1-3 E-08028 Barcelona Spain ; M.Font-Bardia ; Departament de Cristal.lografia Universitat de Barcelona Mart\'i i Franqu\`es, sn E-08028 Barcelona Spain ; M.Crespo ; Departament de Qu\'imica Inorg\`anica Universitat de Barcelona Mart\'i i Franqu\`es 1 E-08028-Barcelona Spain ; #TrackingRef '- MCPM50a1-om92a-om147a-pm47a.CIF' # 3. TITLE AND AUTHOR LIST _publ_section_title ; Biaryl formation in the synthesis of endo and exo-platinacycles ; _publ_contact_author_name 'Crespo, Margarita' _publ_contact_author_email margarita.crespo@qi.ub.es data_mcpm50a1 _database_code_depnum_ccdc_archive 'CCDC 822500' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H27 Br2 N Pt S' _chemical_formula_sum 'C25 H27 Br2 N Pt S' _chemical_formula_weight 728.45 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' Br Br -0.2901 2.4595 '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' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.039(4) _cell_length_b 10.075(6) _cell_length_c 12.819(5) _cell_angle_alpha 90.85(2) _cell_angle_beta 103.59(3) _cell_angle_gamma 90.42(3) _cell_volume 1260.0(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 260 _cell_measurement_theta_min 3 _cell_measurement_theta_max 31 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.920 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 8.834 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.40 _exptl_absorpt_correction_T_max 0.49 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'MAR345 with image plate detector' _diffrn_measurement_method 'phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13491 _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_sigmaI/netI 0.0433 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 32.29 _reflns_number_total 6984 _reflns_number_gt 6171 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MARXDS (Claudio Klein, 2005)' _computing_cell_refinement 'AUTOMAR (Claudio Klein, 2007)' _computing_data_reduction 'MARSCALE (Claudio Klein, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Brueggermann and Smith, 1990)' _computing_publication_material 'PLATON (Spek, 1990)' _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^)+(0.0447P)^2^+0.2738P] 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 SHELXL _refine_ls_extinction_coef 0.0109(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6984 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0358 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0934 _refine_ls_wR_factor_gt 0.0845 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.129 _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 Pt Pt 0.200793(14) 0.130232(14) 0.265606(10) 0.04905(7) Uani 1 1 d . . . Br1 Br -0.03346(5) 0.01134(5) 0.23292(4) 0.06544(12) Uani 1 1 d . . . Br2 Br 0.31066(7) 0.43876(6) 0.02497(5) 0.08672(17) Uani 1 1 d . . . S S 0.24871(13) 0.11267(12) 0.44729(9) 0.0593(2) Uani 1 1 d . . . N1 N 0.1744(4) 0.1548(3) 0.1056(3) 0.0528(7) Uani 1 1 d . . . C1 C 0.3814(4) 0.2216(4) 0.2806(3) 0.0481(7) Uani 1 1 d . . . C2 C 0.4068(5) 0.3507(4) 0.3249(3) 0.0544(8) Uani 1 1 d . . . H2 H 0.3387 0.3908 0.3522 0.065 Uiso 1 1 calc R . . C3 C 0.5265(6) 0.4210(5) 0.3303(4) 0.0685(11) Uani 1 1 d . . . C4 C 0.6327(6) 0.3546(6) 0.2929(4) 0.0752(13) Uani 1 1 d . . . H4 H 0.7171 0.3963 0.2984 0.090 Uiso 1 1 calc R . . C5 C 0.6089(6) 0.2283(6) 0.2484(4) 0.0704(12) Uani 1 1 d . . . H5 H 0.6783 0.1866 0.2239 0.085 Uiso 1 1 calc R . . C6 C 0.4833(5) 0.1605(4) 0.2388(3) 0.0548(9) Uani 1 1 d . . . C7 C 0.4681(5) 0.0332(4) 0.1819(3) 0.0569(9) Uani 1 1 d . . . C8 C 0.5687(6) -0.0629(5) 0.2100(4) 0.0723(12) Uani 1 1 d . . . H8 H 0.6411 -0.0478 0.2693 0.087 Uiso 1 1 calc R . . C9 C 0.5634(7) -0.1806(6) 0.1515(5) 0.0858(16) Uani 1 1 d . . . H9 H 0.6314 -0.2432 0.1735 0.103 Uiso 1 1 calc R . . C10 C 0.4597(6) -0.2071(5) 0.0616(5) 0.0749(13) Uani 1 1 d . . . H10 H 0.4578 -0.2855 0.0220 0.090 Uiso 1 1 calc R . . C11 C 0.3596(6) -0.1139(5) 0.0327(4) 0.0704(12) Uani 1 1 d . . . H11 H 0.2904 -0.1293 -0.0288 0.084 Uiso 1 1 calc R . . C12 C 0.3572(5) 0.0026(4) 0.0912(3) 0.0562(9) Uani 1 1 d . . . C13 C 0.2482(5) 0.0948(4) 0.0491(3) 0.0546(9) Uani 1 1 d . . . H13 H 0.2298 0.1123 -0.0239 0.066 Uiso 1 1 calc R . . C14 C 0.5461(8) 0.5605(7) 0.3744(5) 0.0965(19) Uani 1 1 d . . . H14A H 0.6356 0.5925 0.3717 0.145 Uiso 1 1 calc R . . H14B H 0.5377 0.5618 0.4475 0.145 Uiso 1 1 calc R . . H14C H 0.4777 0.6165 0.3323 0.145 Uiso 1 1 calc R . . C15 C 0.0667(5) 0.2468(5) 0.0528(4) 0.0663(11) Uani 1 1 d . . . H15A H -0.0223 0.2076 0.0512 0.080 Uiso 1 1 calc R . . H15B H 0.0730 0.2587 -0.0209 0.080 Uiso 1 1 calc R . . C16 C 0.0770(5) 0.3804(5) 0.1083(4) 0.0598(10) Uani 1 1 d . . . C17 C 0.1757(6) 0.4720(5) 0.1042(4) 0.0671(11) Uani 1 1 d . . . C18 C 0.0920(8) 0.6253(7) 0.2176(5) 0.0882(17) Uani 1 1 d . . . H18 H 0.0967 0.7064 0.2540 0.106 Uiso 1 1 calc R . . C19 C -0.0100(8) 0.5310(7) 0.2218(6) 0.0927(18) Uani 1 1 d . . . H19 H -0.0739 0.5503 0.2617 0.111 Uiso 1 1 calc R . . C20 C -0.0180(7) 0.4114(6) 0.1686(5) 0.0777(14) Uani 1 1 d . . . H20 H -0.0868 0.3507 0.1726 0.093 Uiso 1 1 calc R . . C21 C 0.1822(6) 0.5945(5) 0.1595(4) 0.0747(13) Uani 1 1 d . . . H21 H 0.2509 0.6553 0.1555 0.090 Uiso 1 1 calc R . . C22 C 0.0978(7) 0.1653(6) 0.4926(5) 0.0805(15) Uani 1 1 d . . . H22A H 0.0188 0.1136 0.4547 0.097 Uiso 1 1 calc R . . H22B H 0.1116 0.1481 0.5687 0.097 Uiso 1 1 calc R . . C23 C 0.0698(9) 0.3109(8) 0.4735(7) 0.107(2) Uani 1 1 d . . . H23A H -0.0112 0.3346 0.4966 0.161 Uiso 1 1 calc R . . H23B H 0.0566 0.3283 0.3983 0.161 Uiso 1 1 calc R . . H23C H 0.1463 0.3624 0.5133 0.161 Uiso 1 1 calc R . . C24 C 0.2368(6) -0.0659(5) 0.4726(4) 0.0711(12) Uani 1 1 d . . . H24A H 0.2411 -0.0790 0.5481 0.085 Uiso 1 1 calc R . . H24B H 0.1497 -0.1010 0.4316 0.085 Uiso 1 1 calc R . . C25 C 0.3529(8) -0.1399(7) 0.4410(6) 0.103(2) Uani 1 1 d . . . H25A H 0.3492 -0.2316 0.4595 0.154 Uiso 1 1 calc R . . H25B H 0.4391 -0.1017 0.4786 0.154 Uiso 1 1 calc R . . H25C H 0.3440 -0.1332 0.3651 0.154 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt 0.04596(10) 0.05433(10) 0.04721(9) 0.00140(6) 0.01171(7) -0.00123(6) Br1 0.0558(2) 0.0745(3) 0.0652(2) 0.0016(2) 0.0127(2) -0.00791(19) Br2 0.0835(4) 0.0859(4) 0.0957(4) 0.0047(3) 0.0311(3) -0.0030(3) S 0.0574(6) 0.0680(6) 0.0531(5) 0.0022(4) 0.0140(4) -0.0012(4) N1 0.0521(18) 0.0581(17) 0.0480(15) 0.0040(13) 0.0111(14) -0.0016(14) C1 0.0467(19) 0.0548(19) 0.0434(16) 0.0028(13) 0.0115(15) 0.0001(14) C2 0.056(2) 0.061(2) 0.0457(18) -0.0007(15) 0.0106(17) -0.0047(16) C3 0.065(3) 0.076(3) 0.064(3) -0.001(2) 0.015(2) -0.010(2) C4 0.064(3) 0.089(4) 0.070(3) -0.004(2) 0.012(2) -0.016(2) C5 0.060(3) 0.083(3) 0.070(3) -0.004(2) 0.017(2) -0.006(2) C6 0.053(2) 0.060(2) 0.0524(19) 0.0013(15) 0.0132(17) -0.0020(16) C7 0.054(2) 0.066(2) 0.053(2) 0.0017(16) 0.0171(18) -0.0023(17) C8 0.072(3) 0.077(3) 0.070(3) 0.008(2) 0.019(2) 0.003(2) C9 0.094(4) 0.083(4) 0.089(4) 0.010(3) 0.035(3) 0.011(3) C10 0.076(3) 0.069(3) 0.085(3) -0.002(2) 0.030(3) -0.004(2) C11 0.070(3) 0.070(3) 0.075(3) -0.007(2) 0.026(3) -0.007(2) C12 0.058(2) 0.060(2) 0.053(2) -0.0006(16) 0.0185(18) -0.0078(17) C13 0.055(2) 0.057(2) 0.0512(19) 0.0001(15) 0.0115(17) -0.0054(16) C14 0.107(5) 0.089(4) 0.091(4) -0.002(3) 0.020(4) -0.024(4) C15 0.062(3) 0.067(3) 0.065(3) 0.005(2) 0.007(2) -0.003(2) C16 0.055(2) 0.060(2) 0.063(2) 0.0072(18) 0.011(2) 0.0030(17) C17 0.067(3) 0.068(3) 0.065(3) 0.007(2) 0.013(2) 0.004(2) C18 0.095(5) 0.079(4) 0.091(4) 0.003(3) 0.023(4) 0.011(3) C19 0.100(5) 0.085(4) 0.098(4) 0.005(3) 0.034(4) 0.010(3) C20 0.076(4) 0.081(3) 0.080(3) 0.009(3) 0.024(3) 0.009(3) C21 0.081(4) 0.069(3) 0.073(3) 0.005(2) 0.015(3) 0.006(2) C22 0.079(4) 0.097(4) 0.070(3) -0.003(3) 0.026(3) 0.000(3) C23 0.103(6) 0.105(5) 0.119(6) -0.002(4) 0.038(5) 0.011(4) C24 0.070(3) 0.074(3) 0.069(3) 0.012(2) 0.014(2) 0.003(2) C25 0.094(5) 0.095(5) 0.117(6) 0.002(4) 0.021(4) 0.008(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt C1 1.994(4) . ? Pt N1 2.025(3) . ? Pt S 2.2746(14) . ? Pt Br1 2.5732(12) . ? Br2 C17 1.903(6) . ? S C22 1.825(6) . ? S C24 1.841(5) . ? N1 C13 1.297(6) . ? N1 C15 1.475(6) . ? C1 C6 1.403(6) . ? C1 C2 1.409(6) . ? C2 C3 1.378(7) . ? C2 H2 0.9300 . ? C3 C4 1.434(8) . ? C3 C14 1.501(8) . ? C4 C5 1.383(8) . ? C4 H4 0.9300 . ? C5 C6 1.408(7) . ? C5 H5 0.9300 . ? C6 C7 1.455(6) . ? C7 C8 1.393(7) . ? C7 C12 1.436(6) . ? C8 C9 1.387(8) . ? C8 H8 0.9300 . ? C9 C10 1.381(9) . ? C9 H9 0.9300 . ? C10 C11 1.370(8) . ? C10 H10 0.9300 . ? C11 C12 1.387(7) . ? C11 H11 0.9300 . ? C12 C13 1.450(6) . ? C13 H13 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.504(7) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.360(7) . ? C16 C20 1.396(8) . ? C17 C21 1.407(7) . ? C18 C21 1.336(9) . ? C18 C19 1.403(10) . ? C18 H18 0.9300 . ? C19 C20 1.368(9) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.509(9) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C25 1.518(9) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pt N1 86.22(15) . . ? C1 Pt S 88.60(11) . . ? N1 Pt S 174.82(10) . . ? C1 Pt Br1 176.24(10) . . ? N1 Pt Br1 90.09(11) . . ? S Pt Br1 95.09(4) . . ? C22 S C24 97.8(3) . . ? C22 S Pt 107.9(2) . . ? C24 S Pt 105.43(18) . . ? C13 N1 C15 119.6(4) . . ? C13 N1 Pt 123.0(3) . . ? C15 N1 Pt 117.4(3) . . ? C6 C1 C2 118.4(4) . . ? C6 C1 Pt 119.5(3) . . ? C2 C1 Pt 121.9(3) . . ? C3 C2 C1 123.9(4) . . ? C3 C2 H2 118.0 . . ? C1 C2 H2 118.0 . . ? C2 C3 C4 117.0(5) . . ? C2 C3 C14 121.8(5) . . ? C4 C3 C14 121.2(5) . . ? C5 C4 C3 119.6(5) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 122.4(5) . . ? C4 C5 H5 118.8 . . ? C6 C5 H5 118.8 . . ? C1 C6 C5 118.4(4) . . ? C1 C6 C7 125.0(4) . . ? C5 C6 C7 116.5(4) . . ? C8 C7 C12 116.6(4) . . ? C8 C7 C6 120.1(4) . . ? C12 C7 C6 123.2(4) . . ? C9 C8 C7 121.6(5) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C10 C9 C8 121.7(6) . . ? C10 C9 H9 119.2 . . ? C8 C9 H9 119.2 . . ? C11 C10 C9 117.7(5) . . ? C11 C10 H10 121.2 . . ? C9 C10 H10 121.2 . . ? C10 C11 C12 122.8(5) . . ? C10 C11 H11 118.6 . . ? C12 C11 H11 118.6 . . ? C11 C12 C7 119.6(5) . . ? C11 C12 C13 116.9(4) . . ? C7 C12 C13 123.1(4) . . ? N1 C13 C12 125.0(4) . . ? N1 C13 H13 117.5 . . ? C12 C13 H13 117.5 . . ? C3 C14 H14A 109.5 . . ? C3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 C16 112.9(4) . . ? N1 C15 H15A 109.0 . . ? C16 C15 H15A 109.0 . . ? N1 C15 H15B 109.0 . . ? C16 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? C17 C16 C20 118.1(5) . . ? C17 C16 C15 123.3(5) . . ? C20 C16 C15 118.5(5) . . ? C16 C17 C21 120.9(5) . . ? C16 C17 Br2 121.4(4) . . ? C21 C17 Br2 117.7(4) . . ? C21 C18 C19 117.6(6) . . ? C21 C18 H18 121.2 . . ? C19 C18 H18 121.2 . . ? C20 C19 C18 121.7(7) . . ? C20 C19 H19 119.1 . . ? C18 C19 H19 119.1 . . ? C19 C20 C16 120.1(6) . . ? C19 C20 H20 120.0 . . ? C16 C20 H20 120.0 . . ? C18 C21 C17 121.5(6) . . ? C18 C21 H21 119.2 . . ? C17 C21 H21 119.2 . . ? C23 C22 S 111.7(5) . . ? C23 C22 H22A 109.3 . . ? S C22 H22A 109.3 . . ? C23 C22 H22B 109.3 . . ? S C22 H22B 109.3 . . ? H22A C22 H22B 107.9 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 S 110.5(4) . . ? C25 C24 H24A 109.6 . . ? S C24 H24A 109.6 . . ? C25 C24 H24B 109.6 . . ? S C24 H24B 109.6 . . ? H24A C24 H24B 108.1 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.779 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.936 _refine_diff_density_max 1.250 _refine_diff_density_min -1.040 _refine_diff_density_rms 0.130 #===END data_mcom92a _database_code_depnum_ccdc_archive 'CCDC 822501' #TrackingRef '- MCPM50a1-om92a-om147a-pm47a.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H32 Br Cl N P Pt' _chemical_formula_sum 'C39 H32 Br Cl N P Pt' _chemical_formula_weight 856.08 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' Br Br -0.2901 2.4595 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P21/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 21.026(8) _cell_length_b 7.879(5) _cell_length_c 21.075(8) _cell_angle_alpha 90.00 _cell_angle_beta 108.56(2) _cell_angle_gamma 90.00 _cell_volume 3310(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 293 _cell_measurement_theta_min 3 _cell_measurement_theta_max 31 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.718 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 5.605 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.59 _exptl_absorpt_correction_T_max 0.76 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'MAR345 with image plate detector' _diffrn_measurement_method 'phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27088 _diffrn_reflns_av_R_equivalents 0.0748 _diffrn_reflns_av_sigmaI/netI 0.0985 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 32.29 _reflns_number_total 9183 _reflns_number_gt 7107 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MARXDS (Claudio Klein, 2005)' _computing_cell_refinement 'AUTOMAR (Claudio Klein, 2005)' _computing_data_reduction 'MARSCALE (Claudio Klein, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Brueggermann and Smith, 1990)' _computing_publication_material 'PLATON (Spek, 1990)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The displacement parameters of PT1-BR1 in the direction of the bond are restrained to be equal within an effective standard desviation ; _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^)+(0.0717P)^2^+1.3414P] 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 SHELXL _refine_ls_extinction_coef 0.0011(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9183 _refine_ls_number_parameters 399 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0696 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1659 _refine_ls_wR_factor_gt 0.1563 _refine_ls_goodness_of_fit_ref 1.090 _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 0.234027(11) 0.65631(2) 0.003071(10) 0.05640(10) Uani 1 1 d U . . Br1 Br 0.19112(4) 0.66956(8) 0.10091(4) 0.0761(2) Uani 1 1 d U . . P1 P 0.32753(7) 0.52170(16) 0.06393(7) 0.0541(3) Uani 1 1 d . . . Cl1 Cl 0.40592(12) 0.6786(2) -0.16438(11) 0.0875(5) Uani 1 1 d . . . N1 N 0.1454(3) 0.7542(6) -0.0633(2) 0.0667(11) Uani 1 1 d . . . C1 C -0.0690(5) 0.8580(10) -0.1491(5) 0.095(2) Uani 1 1 d . . . H1 H -0.0667 0.8220 -0.1065 0.115 Uiso 1 1 calc R . . C2 C -0.1154(4) 0.7821(11) -0.2053(4) 0.090(2) Uani 1 1 d . . . H2 H -0.1454 0.7020 -0.1990 0.108 Uiso 1 1 calc R . . C3 C -0.1176(5) 0.8233(10) -0.2691(5) 0.090(2) Uani 1 1 d . . . C4 C -0.0720(4) 0.9397(10) -0.2777(4) 0.0844(19) Uani 1 1 d . . . H4 H -0.0705 0.9651 -0.3202 0.101 Uiso 1 1 calc R . . C5 C -0.0282(4) 1.0187(9) -0.2213(4) 0.0855(19) Uani 1 1 d . . . H5 H 0.0018 1.0989 -0.2274 0.103 Uiso 1 1 calc R . . C6 C -0.0273(4) 0.9827(9) -0.1562(4) 0.0821(18) Uani 1 1 d . . . C7 C 0.0197(3) 1.0734(8) -0.0978(3) 0.0690(14) Uani 1 1 d . . . C8 C 0.0133(5) 1.2476(11) -0.0928(5) 0.101(2) Uani 1 1 d . . . H8 H -0.0216 1.3039 -0.1243 0.121 Uiso 1 1 calc R . . C9 C 0.0579(6) 1.3387(9) -0.0422(5) 0.093(3) Uani 1 1 d . . . H9 H 0.0506 1.4540 -0.0381 0.112 Uiso 1 1 calc R . . C10 C 0.1138(5) 1.2611(11) 0.0032(4) 0.087(2) Uani 1 1 d . . . H10 H 0.1467 1.3242 0.0342 0.104 Uiso 1 1 calc R . . C11 C 0.1180(5) 1.0888(11) -0.0003(4) 0.088(2) Uani 1 1 d . . . H11 H 0.1534 1.0344 0.0313 0.106 Uiso 1 1 calc R . . C12 C 0.0730(3) 0.9913(8) -0.0477(3) 0.0679(14) Uani 1 1 d . . . C13 C 0.0810(4) 0.8031(8) -0.0479(3) 0.0692(14) Uani 1 1 d . . . H13A H 0.0425 0.7536 -0.0814 0.083 Uiso 1 1 calc R . . H13B H 0.0828 0.7578 -0.0046 0.083 Uiso 1 1 calc R . . C14 C 0.1454(4) 0.7681(8) -0.1228(3) 0.0719(15) Uani 1 1 d . . . H14 H 0.1072 0.8030 -0.1566 0.086 Uiso 1 1 calc R . . C15 C 0.2048(3) 0.7294(8) -0.1365(3) 0.0633(12) Uani 1 1 d . . . C16 C 0.2124(4) 0.7510(9) -0.2014(3) 0.0797(18) Uani 1 1 d . . . H16 H 0.1752 0.7780 -0.2378 0.096 Uiso 1 1 calc R . . C17 C 0.2735(4) 0.7325(9) -0.2101(4) 0.0806(17) Uani 1 1 d . . . H17 H 0.2791 0.7447 -0.2519 0.097 Uiso 1 1 calc R . . C18 C 0.3275(3) 0.6943(7) -0.1530(3) 0.0621(13) Uani 1 1 d . . . C19 C 0.3262(4) 0.6683(6) -0.0898(3) 0.0651(15) Uani 1 1 d . . . H19 H 0.3647 0.6444 -0.0543 0.078 Uiso 1 1 calc R . . C20 C 0.2624(3) 0.6801(6) -0.0820(3) 0.0536(11) Uani 1 1 d . . . C21 C -0.1671(5) 0.7378(12) -0.3299(4) 0.099(2) Uani 1 1 d . . . H21A H -0.1948 0.6602 -0.3153 0.148 Uiso 1 1 calc R . . H21B H -0.1428 0.6769 -0.3543 0.148 Uiso 1 1 calc R . . H21C H -0.1948 0.8224 -0.3583 0.148 Uiso 1 1 calc R . . C22 C 0.3182(3) 0.3904(7) 0.1312(2) 0.0539(11) Uani 1 1 d . . . C23 C 0.3310(3) 0.4582(8) 0.1962(3) 0.0656(13) Uani 1 1 d . . . H23 H 0.3466 0.5689 0.2053 0.079 Uiso 1 1 calc R . . C24 C 0.3205(4) 0.3593(8) 0.2462(4) 0.0767(18) Uani 1 1 d . . . H24 H 0.3284 0.4065 0.2885 0.092 Uiso 1 1 calc R . . C25 C 0.2990(4) 0.1957(9) 0.2358(4) 0.0780(17) Uani 1 1 d . . . H25 H 0.2942 0.1309 0.2709 0.094 Uiso 1 1 calc R . . C26 C 0.2839(5) 0.1249(11) 0.1706(5) 0.096(2) Uani 1 1 d . . . H26 H 0.2669 0.0154 0.1618 0.115 Uiso 1 1 calc R . . C27 C 0.2953(4) 0.2234(9) 0.1203(3) 0.0757(16) Uani 1 1 d . . . H27 H 0.2874 0.1760 0.0781 0.091 Uiso 1 1 calc R . . C28 C 0.3596(3) 0.3705(6) 0.0161(3) 0.0545(11) Uani 1 1 d . . . C29 C 0.4278(4) 0.3610(8) 0.0224(4) 0.0743(17) Uani 1 1 d . . . H29 H 0.4585 0.4355 0.0503 0.089 Uiso 1 1 calc R . . C30 C 0.4488(4) 0.2384(10) -0.0138(4) 0.0849(19) Uani 1 1 d . . . H30 H 0.4941 0.2295 -0.0095 0.102 Uiso 1 1 calc R . . C31 C 0.4026(4) 0.1281(9) -0.0568(4) 0.0801(19) Uani 1 1 d . . . H31 H 0.4171 0.0447 -0.0803 0.096 Uiso 1 1 calc R . . C32 C 0.3381(5) 0.1440(8) -0.0635(4) 0.083(2) Uani 1 1 d . . . H32 H 0.3075 0.0730 -0.0933 0.100 Uiso 1 1 calc R . . C33 C 0.3140(3) 0.2636(8) -0.0274(3) 0.0673(14) Uani 1 1 d . . . H33 H 0.2685 0.2708 -0.0326 0.081 Uiso 1 1 calc R . . C34 C 0.3956(3) 0.6664(6) 0.1058(3) 0.0588(12) Uani 1 1 d . . . C35 C 0.3888(4) 0.8370(7) 0.0904(4) 0.0727(17) Uani 1 1 d . . . H35 H 0.3501 0.8765 0.0585 0.087 Uiso 1 1 calc R . . C36 C 0.4398(4) 0.9503(8) 0.1223(4) 0.0768(17) Uani 1 1 d . . . H36 H 0.4356 1.0643 0.1103 0.092 Uiso 1 1 calc R . . C37 C 0.4964(4) 0.8956(10) 0.1714(4) 0.0768(17) Uani 1 1 d . . . H37 H 0.5293 0.9728 0.1939 0.092 Uiso 1 1 calc R . . C38 C 0.5042(4) 0.7233(9) 0.1871(3) 0.0751(16) Uani 1 1 d . . . H38 H 0.5432 0.6849 0.2190 0.090 Uiso 1 1 calc R . . C39 C 0.4536(3) 0.6084(9) 0.1552(3) 0.0710(15) Uani 1 1 d . . . H39 H 0.4583 0.4940 0.1666 0.085 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.05927(16) 0.05535(14) 0.05185(15) 0.00007(7) 0.01381(10) 0.00143(7) Br1 0.0783(5) 0.0847(4) 0.0649(4) -0.0007(3) 0.0224(3) 0.0060(3) P1 0.0583(7) 0.0528(6) 0.0483(6) 0.0001(5) 0.0132(5) 0.0008(5) Cl1 0.0853(12) 0.0927(11) 0.0894(13) 0.0033(9) 0.0349(10) 0.0031(9) N1 0.068(3) 0.068(3) 0.059(3) -0.001(2) 0.013(2) 0.002(2) C1 0.083(5) 0.113(6) 0.085(6) 0.002(4) 0.019(5) -0.003(4) C2 0.074(4) 0.104(5) 0.088(5) 0.002(4) 0.022(4) -0.007(4) C3 0.073(5) 0.096(5) 0.095(6) 0.002(4) 0.016(4) 0.000(4) C4 0.090(5) 0.088(4) 0.073(4) 0.005(4) 0.023(4) 0.014(4) C5 0.091(5) 0.087(4) 0.077(4) 0.001(4) 0.026(4) 0.003(4) C6 0.077(4) 0.088(4) 0.083(5) 0.000(4) 0.027(4) 0.002(3) C7 0.064(3) 0.069(3) 0.073(4) 0.006(3) 0.019(3) 0.009(3) C8 0.104(6) 0.089(5) 0.108(6) 0.002(5) 0.032(5) 0.015(5) C9 0.121(8) 0.065(4) 0.101(6) -0.007(4) 0.046(6) 0.001(4) C10 0.097(6) 0.084(5) 0.079(5) -0.011(4) 0.029(4) -0.009(4) C11 0.099(6) 0.084(4) 0.076(4) -0.003(4) 0.019(4) -0.001(4) C12 0.071(4) 0.069(3) 0.064(3) 0.001(3) 0.023(3) 0.006(3) C13 0.070(4) 0.072(3) 0.065(3) 0.004(3) 0.021(3) 0.001(3) C14 0.072(4) 0.072(4) 0.068(4) 0.009(3) 0.017(3) 0.000(3) C15 0.063(3) 0.066(3) 0.058(3) 0.003(2) 0.016(2) 0.000(3) C16 0.081(5) 0.084(4) 0.064(4) 0.006(3) 0.008(3) 0.002(4) C17 0.091(5) 0.076(4) 0.074(4) 0.006(3) 0.024(4) 0.009(4) C18 0.071(4) 0.057(3) 0.057(3) 0.003(2) 0.019(3) 0.002(2) C19 0.067(4) 0.060(3) 0.061(3) -0.001(2) 0.009(3) 0.003(2) C20 0.057(3) 0.050(2) 0.049(3) 0.0028(19) 0.010(2) 0.0004(19) C21 0.092(6) 0.105(6) 0.095(6) -0.009(5) 0.023(5) 0.002(5) C22 0.060(3) 0.055(2) 0.046(2) 0.007(2) 0.015(2) 0.004(2) C23 0.068(3) 0.071(3) 0.059(3) -0.003(3) 0.022(3) -0.002(3) C24 0.083(5) 0.084(4) 0.064(4) 0.009(3) 0.024(4) 0.002(3) C25 0.092(5) 0.077(4) 0.068(4) 0.013(3) 0.029(4) 0.003(4) C26 0.108(7) 0.083(4) 0.098(6) 0.004(4) 0.034(5) -0.012(4) C27 0.092(5) 0.068(3) 0.067(4) 0.002(3) 0.023(3) -0.002(3) C28 0.064(3) 0.050(2) 0.051(3) 0.0023(19) 0.019(2) 0.000(2) C29 0.081(5) 0.068(4) 0.075(4) -0.003(3) 0.026(4) 0.000(3) C30 0.095(5) 0.096(5) 0.069(4) 0.002(4) 0.032(4) 0.010(4) C31 0.093(5) 0.073(4) 0.078(4) 0.006(3) 0.033(4) 0.013(3) C32 0.089(5) 0.080(4) 0.078(5) -0.011(3) 0.023(4) -0.003(3) C33 0.072(4) 0.068(3) 0.062(3) -0.006(3) 0.022(3) 0.002(3) C34 0.059(3) 0.054(3) 0.060(3) -0.001(2) 0.014(2) -0.003(2) C35 0.077(4) 0.066(4) 0.072(4) -0.001(3) 0.020(4) -0.008(3) C36 0.086(5) 0.063(3) 0.078(4) -0.005(3) 0.022(4) -0.003(3) C37 0.082(5) 0.076(4) 0.071(4) -0.011(3) 0.024(3) -0.016(4) C38 0.075(4) 0.079(4) 0.064(3) 0.001(3) 0.012(3) 0.003(3) C39 0.072(4) 0.070(3) 0.066(3) -0.002(3) 0.014(3) -0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C20 2.071(6) . ? Pt1 N1 2.090(5) . ? Pt1 P1 2.2427(16) . ? Pt1 Br1 2.5021(12) . ? P1 C22 1.815(5) . ? P1 C28 1.822(6) . ? P1 C34 1.823(6) . ? Cl1 C18 1.746(7) . ? N1 C14 1.259(8) . ? N1 C13 1.537(9) . ? C1 C6 1.356(12) . ? C1 C2 1.406(12) . ? C1 H1 0.9300 . ? C2 C3 1.370(13) . ? C2 H2 0.9300 . ? C3 C4 1.380(12) . ? C3 C21 1.526(12) . ? C4 C5 1.397(10) . ? C4 H4 0.9300 . ? C5 C6 1.395(10) . ? C5 H5 0.9300 . ? C6 C7 1.493(10) . ? C7 C8 1.387(11) . ? C7 C12 1.427(9) . ? C8 C9 1.377(13) . ? C8 H8 0.9300 . ? C9 C10 1.398(13) . ? C9 H9 0.9300 . ? C10 C11 1.364(12) . ? C10 H10 0.9300 . ? C11 C12 1.372(10) . ? C11 H11 0.9300 . ? C12 C13 1.493(8) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.402(9) . ? C14 H14 0.9300 . ? C15 C20 1.433(8) . ? C15 C16 1.435(9) . ? C16 C17 1.363(10) . ? C16 H16 0.9300 . ? C17 C18 1.399(10) . ? C17 H17 0.9300 . ? C18 C19 1.355(9) . ? C19 C20 1.406(10) . ? C19 H19 0.9300 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C27 1.395(8) . ? C22 C23 1.414(8) . ? C23 C24 1.385(9) . ? C23 H23 0.9300 . ? C24 C25 1.361(9) . ? C24 H24 0.9300 . ? C25 C26 1.421(11) . ? C25 H25 0.9300 . ? C26 C27 1.395(11) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C33 1.381(8) . ? C28 C29 1.401(10) . ? C29 C30 1.386(10) . ? C29 H29 0.9300 . ? C30 C31 1.399(12) . ? C30 H30 0.9300 . ? C31 C32 1.325(13) . ? C31 H31 0.9300 . ? C32 C33 1.404(10) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C35 1.380(7) . ? C34 C39 1.404(9) . ? C35 C36 1.393(10) . ? C35 H35 0.9300 . ? C36 C37 1.373(10) . ? C36 H36 0.9300 . ? C37 C38 1.394(10) . ? C37 H37 0.9300 . ? C38 C39 1.395(10) . ? C38 H38 0.9300 . ? C39 H39 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 C20 Pt1 N1 80.1(2) . . ? C20 Pt1 P1 95.53(16) . . ? N1 Pt1 P1 172.00(14) . . ? C20 Pt1 Br1 171.39(14) . . ? N1 Pt1 Br1 93.27(15) . . ? P1 Pt1 Br1 91.65(5) . . ? C22 P1 C28 102.1(3) . . ? C22 P1 C34 104.0(3) . . ? C28 P1 C34 107.8(3) . . ? C22 P1 Pt1 115.03(19) . . ? C28 P1 Pt1 113.8(2) . . ? C34 P1 Pt1 113.05(19) . . ? C14 N1 C13 117.9(5) . . ? C14 N1 Pt1 114.5(5) . . ? C13 N1 Pt1 127.5(4) . . ? C6 C1 C2 121.1(9) . . ? C6 C1 H1 119.5 . . ? C2 C1 H1 119.5 . . ? C3 C2 C1 121.5(9) . . ? C3 C2 H2 119.3 . . ? C1 C2 H2 119.3 . . ? C2 C3 C4 118.6(8) . . ? C2 C3 C21 121.3(8) . . ? C4 C3 C21 120.0(9) . . ? C3 C4 C5 118.9(8) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C6 C5 C4 123.0(8) . . ? C6 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? C1 C6 C5 116.7(8) . . ? C1 C6 C7 122.5(8) . . ? C5 C6 C7 120.8(7) . . ? C8 C7 C12 117.7(6) . . ? C8 C7 C6 118.8(6) . . ? C12 C7 C6 123.4(6) . . ? C9 C8 C7 121.1(8) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C8 C9 C10 121.3(7) . . ? C8 C9 H9 119.4 . . ? C10 C9 H9 119.4 . . ? C11 C10 C9 117.0(7) . . ? C11 C10 H10 121.5 . . ? C9 C10 H10 121.5 . . ? C10 C11 C12 123.7(8) . . ? C10 C11 H11 118.1 . . ? C12 C11 H11 118.1 . . ? C11 C12 C7 118.8(6) . . ? C11 C12 C13 120.5(7) . . ? C7 C12 C13 120.7(6) . . ? C12 C13 N1 110.9(5) . . ? C12 C13 H13A 109.5 . . ? N1 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? N1 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? N1 C14 C15 118.1(6) . . ? N1 C14 H14 121.0 . . ? C15 C14 H14 121.0 . . ? C14 C15 C20 118.3(6) . . ? C14 C15 C16 123.2(6) . . ? C20 C15 C16 118.3(6) . . ? C17 C16 C15 120.8(6) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C16 C17 C18 116.5(7) . . ? C16 C17 H17 121.7 . . ? C18 C17 H17 121.7 . . ? C19 C18 C17 127.9(7) . . ? C19 C18 Cl1 116.0(5) . . ? C17 C18 Cl1 116.0(5) . . ? C18 C19 C20 115.0(6) . . ? C18 C19 H19 122.5 . . ? C20 C19 H19 122.5 . . ? C19 C20 C15 121.3(5) . . ? C19 C20 Pt1 130.1(4) . . ? C15 C20 Pt1 108.4(4) . . ? C3 C21 H21A 109.5 . . ? C3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C27 C22 C23 117.7(5) . . ? C27 C22 P1 121.8(4) . . ? C23 C22 P1 120.4(4) . . ? C24 C23 C22 119.9(6) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C25 C24 C23 122.4(7) . . ? C25 C24 H24 118.8 . . ? C23 C24 H24 118.8 . . ? C24 C25 C26 119.2(7) . . ? C24 C25 H25 120.4 . . ? C26 C25 H25 120.4 . . ? C27 C26 C25 118.5(7) . . ? C27 C26 H26 120.7 . . ? C25 C26 H26 120.7 . . ? C26 C27 C22 122.2(7) . . ? C26 C27 H27 118.9 . . ? C22 C27 H27 118.9 . . ? C33 C28 C29 120.2(5) . . ? C33 C28 P1 117.7(5) . . ? C29 C28 P1 122.1(5) . . ? C30 C29 C28 118.7(7) . . ? C30 C29 H29 120.6 . . ? C28 C29 H29 120.6 . . ? C29 C30 C31 120.8(8) . . ? C29 C30 H30 119.6 . . ? C31 C30 H30 119.6 . . ? C32 C31 C30 119.1(7) . . ? C32 C31 H31 120.5 . . ? C30 C31 H31 120.5 . . ? C31 C32 C33 122.6(8) . . ? C31 C32 H32 118.7 . . ? C33 C32 H32 118.7 . . ? C28 C33 C32 118.4(7) . . ? C28 C33 H33 120.8 . . ? C32 C33 H33 120.8 . . ? C35 C34 C39 119.5(6) . . ? C35 C34 P1 119.3(5) . . ? C39 C34 P1 121.2(4) . . ? C34 C35 C36 120.3(7) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C37 C36 C35 120.8(6) . . ? C37 C36 H36 119.6 . . ? C35 C36 H36 119.6 . . ? C36 C37 C38 119.5(7) . . ? C36 C37 H37 120.3 . . ? C38 C37 H37 120.3 . . ? C37 C38 C39 120.2(7) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C38 C39 C34 119.6(6) . . ? C38 C39 H39 120.2 . . ? C34 C39 H39 120.2 . . ? _diffrn_measured_fraction_theta_max 0.780 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 2.829 _refine_diff_density_min -0.909 _refine_diff_density_rms 0.165 #===END data_mcom147a _database_code_depnum_ccdc_archive 'CCDC 822502' #TrackingRef '- MCPM50a1-om92a-om147a-pm47a.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H35 Br N P Pt' _chemical_formula_sum 'C40 H35 Br N P Pt' _chemical_formula_weight 835.66 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.683(5) _cell_length_b 9.885(4) _cell_length_c 17.635(7) _cell_angle_alpha 85.59(2) _cell_angle_beta 82.01(2) _cell_angle_gamma 82.75(2) _cell_volume 1655.2(13) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6255 _cell_measurement_theta_min 3 _cell_measurement_theta_max 31 _exptl_crystal_description prism _exptl_crystal_colour ? _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.677 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 820 _exptl_absorpt_coefficient_mu 5.523 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.52 _exptl_absorpt_correction_T_max 0.58 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'MAR345 with image plate detector' _diffrn_measurement_method 'phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16162 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_sigmaI/netI 0.0144 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 32.33 _reflns_number_total 8611 _reflns_number_gt 8046 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MARXDS (Claudio Klein, 2005)' _computing_cell_refinement 'AUTOMAR (Claudio Klein, 2007)' _computing_data_reduction 'MARSCALE (Claudio Klein, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Brueggermann and Smith, 1990)' _computing_publication_material 'PLATON (Spek, 1990)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The displacement parameters of Pt-Br, Pt-Br in the direction of the bond are restrained to be equal within an effective standard desviation ; _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^)+(0.0592P)^2^+0.2478P] 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 SHELXL _refine_ls_extinction_coef 0.0030(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8611 _refine_ls_number_parameters 400 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0927 _refine_ls_wR_factor_gt 0.0888 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_restrained_S_all 1.126 _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 Pt Pt 0.171119(11) 0.192664(10) 0.274313(5) 0.04389(6) Uani 1 1 d U . . Br Br 0.36058(5) 0.03604(4) 0.20397(2) 0.06173(10) Uani 1 1 d U . . P P 0.11163(9) 0.30748(8) 0.16635(4) 0.04462(16) Uani 1 1 d . . . N N 0.2127(3) 0.0928(3) 0.37920(15) 0.0443(5) Uani 1 1 d U . . C1 C 0.0220(4) 0.3027(4) 0.34654(16) 0.0465(6) Uani 1 1 d . . . C2 C -0.0816(4) 0.4006(4) 0.3328(2) 0.0572(8) Uani 1 1 d . . . H2 H -0.0935 0.4272 0.2821 0.069 Uiso 1 1 calc R . . C3 C -0.1725(4) 0.4642(4) 0.3912(2) 0.0569(8) Uani 1 1 d . . . H3 H -0.2429 0.5322 0.3793 0.068 Uiso 1 1 calc R . . C4 C -0.1576(4) 0.4257(4) 0.4676(2) 0.0598(8) Uani 1 1 d . . . H4 H -0.2162 0.4709 0.5064 0.072 Uiso 1 1 calc R . . C5 C -0.0573(4) 0.3214(4) 0.48642(18) 0.0539(7) Uani 1 1 d . . . C6 C 0.0323(3) 0.2603(3) 0.42494(16) 0.0459(6) Uani 1 1 d . . . C7 C 0.1353(4) 0.1461(4) 0.43783(18) 0.0509(7) Uani 1 1 d . . . H7 H 0.1462 0.1110 0.4874 0.061 Uiso 1 1 calc R . . C8 C 0.3139(4) -0.0278(3) 0.3917(2) 0.0537(7) Uani 1 1 d . . . H8A H 0.3111 -0.0914 0.3528 0.064 Uiso 1 1 calc R . . H8B H 0.2851 -0.0725 0.4412 0.064 Uiso 1 1 calc R . . C9 C 0.4618(4) 0.0029(4) 0.38923(19) 0.0545(7) Uani 1 1 d . . . C10 C 0.4906(5) 0.1276(5) 0.4140(2) 0.0694(10) Uani 1 1 d . . . H10 H 0.4161 0.1903 0.4326 0.083 Uiso 1 1 calc R . . C11 C 0.6243(7) 0.1587(6) 0.4114(3) 0.0871(16) Uani 1 1 d . . . H11 H 0.6406 0.2418 0.4277 0.105 Uiso 1 1 calc R . . C12 C 0.7354(6) 0.0656(7) 0.3845(3) 0.0918(19) Uani 1 1 d . . . H12 H 0.8270 0.0865 0.3820 0.110 Uiso 1 1 calc R . . C13 C 0.7108(5) -0.0590(6) 0.3610(2) 0.0747(12) Uani 1 1 d . . . H13 H 0.7866 -0.1210 0.3432 0.090 Uiso 1 1 calc R . . C14 C 0.5756(4) -0.0929(4) 0.3635(2) 0.0566(8) Uani 1 1 d . . . C15 C 0.5558(4) -0.2265(4) 0.3364(2) 0.0563(8) Uani 1 1 d . . . C16 C 0.4754(4) -0.3188(4) 0.3810(2) 0.0619(9) Uani 1 1 d . . . H16 H 0.4308 -0.2959 0.4292 0.074 Uiso 1 1 calc R . . C17 C 0.4616(4) -0.4433(4) 0.3542(3) 0.0657(9) Uani 1 1 d . . . H17 H 0.4063 -0.5022 0.3848 0.079 Uiso 1 1 calc R . . C18 C 0.5275(5) -0.4837(4) 0.2830(2) 0.0680(10) Uani 1 1 d . . . C19 C 0.6084(5) -0.3918(5) 0.2395(2) 0.0720(11) Uani 1 1 d . . . H19 H 0.6539 -0.4152 0.1915 0.086 Uiso 1 1 calc R . . C20 C 0.6230(5) -0.2665(5) 0.2656(2) 0.0733(11) Uani 1 1 d . . . H20 H 0.6788 -0.2081 0.2351 0.088 Uiso 1 1 calc R . . C21 C -0.0461(5) 0.2807(5) 0.5695(2) 0.0662(10) Uani 1 1 d . . . H21A H 0.0156 0.1972 0.5734 0.099 Uiso 1 1 calc R . . H21B H -0.1375 0.2676 0.5960 0.099 Uiso 1 1 calc R . . H21C H -0.0094 0.3515 0.5923 0.099 Uiso 1 1 calc R . . C22 C 0.5160(6) -0.6208(5) 0.2561(4) 0.0898(15) Uani 1 1 d . . . H22A H 0.5142 -0.6136 0.2016 0.135 Uiso 1 1 calc R . . H22B H 0.4312 -0.6536 0.2813 0.135 Uiso 1 1 calc R . . H22C H 0.5953 -0.6834 0.2680 0.135 Uiso 1 1 calc R . . C23 C -0.0484(4) 0.2602(3) 0.13885(18) 0.0494(6) Uani 1 1 d . . . C24 C -0.0918(5) 0.3016(5) 0.0671(2) 0.0700(11) Uani 1 1 d . . . H24 H -0.0368 0.3535 0.0316 0.084 Uiso 1 1 calc R . . C25 C -0.2162(5) 0.2655(5) 0.0489(3) 0.0749(11) Uani 1 1 d . . . H25 H -0.2452 0.2965 0.0019 0.090 Uiso 1 1 calc R . . C26 C -0.2987(5) 0.1843(4) 0.0992(3) 0.0690(10) Uani 1 1 d . . . H26 H -0.3827 0.1615 0.0866 0.083 Uiso 1 1 calc R . . C27 C -0.2534(5) 0.1389(4) 0.1675(3) 0.0653(9) Uani 1 1 d . . . H27 H -0.3062 0.0819 0.2009 0.078 Uiso 1 1 calc R . . C28 C -0.1303(4) 0.1752(3) 0.1886(2) 0.0548(7) Uani 1 1 d . . . H28 H -0.1025 0.1430 0.2357 0.066 Uiso 1 1 calc R . . C29 C 0.0899(4) 0.4934(3) 0.17141(17) 0.0484(6) Uani 1 1 d . . . C30 C -0.0107(4) 0.5816(4) 0.1370(2) 0.0597(8) Uani 1 1 d . . . H30 H -0.0741 0.5469 0.1108 0.072 Uiso 1 1 calc R . . C31 C -0.0156(5) 0.7231(5) 0.1423(3) 0.0750(12) Uani 1 1 d . . . H31 H -0.0843 0.7821 0.1207 0.090 Uiso 1 1 calc R . . C32 C 0.0794(6) 0.7745(5) 0.1787(3) 0.0785(13) Uani 1 1 d . . . H32 H 0.0761 0.8687 0.1806 0.094 Uiso 1 1 calc R . . C33 C 0.1796(6) 0.6910(4) 0.2127(3) 0.0772(12) Uani 1 1 d . . . H33 H 0.2437 0.7274 0.2376 0.093 Uiso 1 1 calc R . . C34 C 0.1838(5) 0.5480(4) 0.2091(2) 0.0647(9) Uani 1 1 d . . . H34 H 0.2509 0.4899 0.2325 0.078 Uiso 1 1 calc R . . C35 C 0.2333(4) 0.2824(3) 0.07794(17) 0.0495(6) Uani 1 1 d . . . C36 C 0.3194(5) 0.3771(4) 0.0459(2) 0.0637(9) Uani 1 1 d . . . H36 H 0.3153 0.4591 0.0692 0.076 Uiso 1 1 calc R . . C37 C 0.4130(6) 0.3539(6) -0.0205(3) 0.0813(13) Uani 1 1 d . . . H37 H 0.4679 0.4213 -0.0421 0.098 Uiso 1 1 calc R . . C38 C 0.4242(6) 0.2333(6) -0.0539(2) 0.0781(12) Uani 1 1 d . . . H38 H 0.4877 0.2167 -0.0978 0.094 Uiso 1 1 calc R . . C39 C 0.3417(7) 0.1370(5) -0.0225(3) 0.0830(14) Uani 1 1 d . . . H39 H 0.3495 0.0538 -0.0449 0.100 Uiso 1 1 calc R . . C40 C 0.2461(6) 0.1604(4) 0.0425(2) 0.0717(11) Uani 1 1 d . . . H40 H 0.1898 0.0933 0.0626 0.086 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt 0.04894(9) 0.04205(8) 0.04075(8) -0.00006(5) -0.00737(5) -0.00537(5) Br 0.0652(2) 0.0603(2) 0.05470(19) -0.00444(15) -0.00296(15) 0.00684(15) P 0.0531(5) 0.0437(4) 0.0377(3) 0.0013(3) -0.0076(3) -0.0085(3) N 0.0531(15) 0.0425(12) 0.0383(10) 0.0017(8) -0.0098(9) -0.0078(9) C1 0.0495(17) 0.0570(17) 0.0350(12) -0.0016(11) -0.0018(10) -0.0184(12) C2 0.057(2) 0.062(2) 0.0506(17) -0.0058(15) -0.0039(14) -0.0025(14) C3 0.0486(19) 0.0573(19) 0.0606(19) -0.0025(14) -0.0006(13) 0.0018(13) C4 0.057(2) 0.063(2) 0.0565(19) -0.0156(16) 0.0061(14) -0.0061(14) C5 0.058(2) 0.0616(19) 0.0433(15) -0.0090(13) 0.0008(12) -0.0151(14) C6 0.0550(18) 0.0491(15) 0.0342(12) 0.0031(10) -0.0090(10) -0.0086(11) C7 0.059(2) 0.0547(17) 0.0390(14) 0.0025(12) -0.0082(12) -0.0087(13) C8 0.056(2) 0.0462(16) 0.0583(18) 0.0060(13) -0.0106(13) -0.0052(12) C9 0.062(2) 0.0558(18) 0.0477(15) 0.0141(13) -0.0164(13) -0.0140(14) C10 0.082(3) 0.066(2) 0.067(2) 0.0075(18) -0.025(2) -0.0240(19) C11 0.103(4) 0.098(4) 0.074(3) 0.013(3) -0.032(3) -0.053(3) C12 0.075(4) 0.148(5) 0.064(2) 0.031(3) -0.031(2) -0.055(3) C13 0.057(3) 0.107(4) 0.063(2) 0.023(2) -0.0204(17) -0.026(2) C14 0.053(2) 0.068(2) 0.0486(16) 0.0155(14) -0.0149(13) -0.0084(14) C15 0.0441(18) 0.065(2) 0.0536(17) 0.0076(15) -0.0020(12) 0.0037(13) C16 0.059(2) 0.060(2) 0.0591(19) 0.0068(15) 0.0038(15) 0.0026(14) C17 0.059(2) 0.059(2) 0.073(2) 0.0030(17) 0.0018(17) -0.0018(15) C18 0.066(2) 0.065(2) 0.066(2) 0.0053(17) -0.0114(17) 0.0169(17) C19 0.070(3) 0.084(3) 0.0527(19) 0.0017(18) -0.0028(16) 0.018(2) C20 0.073(3) 0.089(3) 0.0515(19) 0.0212(19) -0.0005(16) -0.008(2) C21 0.071(3) 0.086(3) 0.0417(16) -0.0054(16) -0.0048(15) -0.0111(19) C22 0.098(4) 0.069(3) 0.100(4) -0.020(3) -0.021(3) 0.018(2) C23 0.0529(18) 0.0499(16) 0.0474(15) 0.0051(12) -0.0128(12) -0.0120(12) C24 0.085(3) 0.081(3) 0.0492(18) 0.0097(17) -0.0218(17) -0.025(2) C25 0.080(3) 0.082(3) 0.071(2) -0.002(2) -0.036(2) -0.011(2) C26 0.071(3) 0.061(2) 0.082(3) -0.0140(19) -0.024(2) -0.0138(17) C27 0.068(3) 0.058(2) 0.074(2) -0.0076(17) -0.0082(18) -0.0200(16) C28 0.064(2) 0.0501(17) 0.0526(17) 0.0011(13) -0.0133(14) -0.0103(13) C29 0.0554(18) 0.0441(14) 0.0432(14) 0.0020(11) -0.0038(11) -0.0020(11) C30 0.064(2) 0.0542(18) 0.0583(19) 0.0078(14) -0.0109(15) 0.0005(14) C31 0.077(3) 0.059(2) 0.079(3) 0.0135(19) -0.006(2) 0.0114(18) C32 0.103(4) 0.051(2) 0.077(3) -0.0049(19) -0.001(2) -0.006(2) C33 0.112(4) 0.0431(18) 0.081(3) -0.0035(17) -0.021(2) -0.018(2) C34 0.083(3) 0.0438(17) 0.070(2) -0.0047(15) -0.0201(19) -0.0071(15) C35 0.0614(19) 0.0487(16) 0.0379(13) -0.0015(11) -0.0065(12) -0.0056(12) C36 0.073(3) 0.063(2) 0.0528(18) -0.0059(15) 0.0086(16) -0.0163(16) C37 0.084(3) 0.092(3) 0.065(2) -0.015(2) 0.016(2) -0.021(2) C38 0.086(3) 0.094(3) 0.0466(19) -0.0086(19) 0.0045(18) 0.009(2) C39 0.121(4) 0.067(3) 0.060(2) -0.016(2) -0.008(2) -0.001(3) C40 0.097(3) 0.060(2) 0.059(2) -0.0106(17) -0.004(2) -0.017(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 Pt C1 2.048(3) . ? Pt N 2.094(3) . ? Pt P 2.2477(11) . ? Pt Br 2.4994(10) . ? P C23 1.811(3) . ? P C29 1.831(3) . ? P C35 1.832(3) . ? N C7 1.295(4) . ? N C8 1.468(4) . ? C1 C2 1.337(5) . ? C1 C6 1.427(4) . ? C2 C3 1.393(5) . ? C2 H2 0.9300 . ? C3 C4 1.393(6) . ? C3 H3 0.9300 . ? C4 C5 1.379(6) . ? C4 H4 0.9300 . ? C5 C6 1.414(5) . ? C5 C21 1.504(5) . ? C6 C7 1.435(5) . ? C7 H7 0.9300 . ? C8 C9 1.495(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C14 1.407(6) . ? C9 C10 1.411(6) . ? C10 C11 1.362(7) . ? C10 H10 0.9300 . ? C11 C12 1.380(9) . ? C11 H11 0.9300 . ? C12 C13 1.387(8) . ? C12 H12 0.9300 . ? C13 C14 1.386(6) . ? C13 H13 0.9300 . ? C14 C15 1.482(6) . ? C15 C20 1.388(6) . ? C15 C16 1.397(5) . ? C16 C17 1.381(6) . ? C16 H16 0.9300 . ? C17 C18 1.390(6) . ? C17 H17 0.9300 . ? C18 C19 1.390(7) . ? C18 C22 1.492(7) . ? C19 C20 1.384(7) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C28 1.402(5) . ? C23 C24 1.404(5) . ? C24 C25 1.383(6) . ? C24 H24 0.9300 . ? C25 C26 1.387(7) . ? C25 H25 0.9300 . ? C26 C27 1.364(7) . ? C26 H26 0.9300 . ? C27 C28 1.392(5) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C34 1.381(5) . ? C29 C30 1.394(5) . ? C30 C31 1.404(6) . ? C30 H30 0.9300 . ? C31 C32 1.361(8) . ? C31 H31 0.9300 . ? C32 C33 1.365(8) . ? C32 H32 0.9300 . ? C33 C34 1.415(5) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C36 1.369(5) . ? C35 C40 1.385(5) . ? C36 C37 1.393(5) . ? C36 H36 0.9300 . ? C37 C38 1.356(7) . ? C37 H37 0.9300 . ? C38 C39 1.356(8) . ? C38 H38 0.9300 . ? C39 C40 1.384(7) . ? C39 H39 0.9300 . ? C40 H40 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 Pt N 80.67(12) . . ? C1 Pt P 95.15(10) . . ? N Pt P 175.73(8) . . ? C1 Pt Br 171.28(9) . . ? N Pt Br 90.65(8) . . ? P Pt Br 93.52(4) . . ? C23 P C29 107.53(16) . . ? C23 P C35 101.36(16) . . ? C29 P C35 102.49(15) . . ? C23 P Pt 112.72(11) . . ? C29 P Pt 113.80(11) . . ? C35 P Pt 117.61(12) . . ? C7 N C8 119.1(3) . . ? C7 N Pt 113.3(2) . . ? C8 N Pt 127.6(2) . . ? C2 C1 C6 116.8(3) . . ? C2 C1 Pt 131.7(2) . . ? C6 C1 Pt 111.4(3) . . ? C1 C2 C3 122.6(4) . . ? C1 C2 H2 118.7 . . ? C3 C2 H2 118.7 . . ? C2 C3 C4 119.9(4) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 120.9(3) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 116.9(3) . . ? C4 C5 C21 119.4(3) . . ? C6 C5 C21 123.7(4) . . ? C5 C6 C1 122.7(3) . . ? C5 C6 C7 121.5(3) . . ? C1 C6 C7 115.7(3) . . ? N C7 C6 118.8(3) . . ? N C7 H7 120.6 . . ? C6 C7 H7 120.6 . . ? N C8 C9 114.3(3) . . ? N C8 H8A 108.7 . . ? C9 C8 H8A 108.7 . . ? N C8 H8B 108.7 . . ? C9 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? C14 C9 C10 118.4(4) . . ? C14 C9 C8 120.8(3) . . ? C10 C9 C8 120.8(4) . . ? C11 C10 C9 121.9(5) . . ? C11 C10 H10 119.1 . . ? C9 C10 H10 119.1 . . ? C10 C11 C12 119.4(5) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? C11 C12 C13 120.1(5) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C14 C13 C12 121.3(5) . . ? C14 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? C13 C14 C9 118.7(4) . . ? C13 C14 C15 118.9(4) . . ? C9 C14 C15 122.3(3) . . ? C20 C15 C16 117.5(4) . . ? C20 C15 C14 119.9(4) . . ? C16 C15 C14 122.6(3) . . ? C17 C16 C15 120.8(4) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C16 C17 C18 122.1(4) . . ? C16 C17 H17 119.0 . . ? C18 C17 H17 119.0 . . ? C17 C18 C19 116.6(4) . . ? C17 C18 C22 121.5(5) . . ? C19 C18 C22 121.8(4) . . ? C20 C19 C18 121.8(4) . . ? C20 C19 H19 119.1 . . ? C18 C19 H19 119.1 . . ? C19 C20 C15 121.1(4) . . ? C19 C20 H20 119.4 . . ? C15 C20 H20 119.4 . . ? C5 C21 H21A 109.5 . . ? C5 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C5 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C28 C23 C24 117.8(3) . . ? C28 C23 P 120.1(2) . . ? C24 C23 P 122.1(3) . . ? C25 C24 C23 120.2(4) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 121.6(4) . . ? C24 C25 H25 119.2 . . ? C26 C25 H25 119.2 . . ? C27 C26 C25 118.2(4) . . ? C27 C26 H26 120.9 . . ? C25 C26 H26 120.9 . . ? C26 C27 C28 122.0(4) . . ? C26 C27 H27 119.0 . . ? C28 C27 H27 119.0 . . ? C27 C28 C23 120.1(3) . . ? C27 C28 H28 120.0 . . ? C23 C28 H28 120.0 . . ? C34 C29 C30 118.9(3) . . ? C34 C29 P 116.9(3) . . ? C30 C29 P 124.1(3) . . ? C29 C30 C31 119.6(4) . . ? C29 C30 H30 120.2 . . ? C31 C30 H30 120.2 . . ? C32 C31 C30 120.4(4) . . ? C32 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? C31 C32 C33 121.5(4) . . ? C31 C32 H32 119.3 . . ? C33 C32 H32 119.3 . . ? C32 C33 C34 118.6(4) . . ? C32 C33 H33 120.7 . . ? C34 C33 H33 120.7 . . ? C29 C34 C33 121.0(4) . . ? C29 C34 H34 119.5 . . ? C33 C34 H34 119.5 . . ? C36 C35 C40 117.0(3) . . ? C36 C35 P 123.1(3) . . ? C40 C35 P 119.9(3) . . ? C35 C36 C37 121.7(4) . . ? C35 C36 H36 119.1 . . ? C37 C36 H36 119.1 . . ? C38 C37 C36 120.1(4) . . ? C38 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? C37 C38 C39 119.1(4) . . ? C37 C38 H38 120.4 . . ? C39 C38 H38 120.4 . . ? C38 C39 C40 121.1(4) . . ? C38 C39 H39 119.4 . . ? C40 C39 H39 119.4 . . ? C39 C40 C35 120.8(4) . . ? C39 C40 H40 119.6 . . ? C35 C40 H40 119.6 . . ? _diffrn_measured_fraction_theta_max 0.730 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.926 _refine_diff_density_max 2.138 _refine_diff_density_min -1.164 _refine_diff_density_rms 0.141 #===END data_mcpm47a _database_code_depnum_ccdc_archive 'CCDC 822503' #TrackingRef '- MCPM50a1-om92a-om147a-pm47a.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H31 Br F2 N P Pt, 0.5(C H2 Cl2), (H2 O)' _chemical_formula_sum 'C39.50 H34 Br Cl F2 N O P Pt' _chemical_formula_weight 918.10 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.508(4) _cell_length_b 11.237(4) _cell_length_c 18.529(6) _cell_angle_alpha 81.01(3) _cell_angle_beta 82.46(2) _cell_angle_gamma 76.34(3) _cell_volume 1890.8(12) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 385 _cell_measurement_theta_min 3 _cell_measurement_theta_max 31 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.613 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 898 _exptl_absorpt_coefficient_mu 4.920 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.59 _exptl_absorpt_correction_T_max 0.71 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 16933 _diffrn_reflns_av_R_equivalents 0.0587 _diffrn_reflns_av_sigmaI/netI 0.0955 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 32.52 _reflns_number_total 9453 _reflns_number_gt 8399 _reflns_threshold_expression >2sigma(I) _computing_data_collection MARXDS _computing_cell_refinement AUTOMAR _computing_data_reduction MARSCALE _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Brueggermann and Smith, 1990)' _computing_publication_material 'PLATON (Spek, 1990)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The displacement parameters of Pt-Br, Pt-Br in the direction of the bond are restrained to be equal within an effective standard desviation ; _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^)+(0.0810P)^2^+2.0463P] 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 SHELXL _refine_ls_extinction_coef 0.0191(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9453 _refine_ls_number_parameters 453 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1526 _refine_ls_wR_factor_gt 0.1440 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.085 _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 Pt Pt 0.653077(19) 0.817114(17) 0.742198(9) 0.04196(10) Uani 1 1 d U . . Br Br 0.87781(7) 0.66983(7) 0.69838(4) 0.05953(17) Uani 1 1 d U . . P P 0.59576(15) 0.68905(14) 0.84112(7) 0.0417(3) Uani 1 1 d . . . N1 N 0.6909(5) 0.9370(4) 0.6498(2) 0.0369(8) Uani 1 1 d . . . F1 F 0.8789(5) 1.1077(4) 0.5666(2) 0.0645(10) Uani 1 1 d . . . F2 F 0.6389(6) 0.8724(5) 0.4593(3) 0.0797(13) Uani 1 1 d . . . C1 C 0.4874(6) 0.9636(5) 0.7635(3) 0.0402(9) Uani 1 1 d . . . C2 C 0.3710(7) 0.9650(5) 0.8097(3) 0.0479(11) Uani 1 1 d . . . H2 H 0.3590 0.8928 0.8397 0.057 Uiso 1 1 calc R . . C3 C 0.2622(6) 1.0758(6) 0.8148(3) 0.0489(12) Uani 1 1 d . . . H3 H 0.1778 1.0739 0.8462 0.059 Uiso 1 1 calc R . . C4 C 0.2803(7) 1.1866(6) 0.7736(3) 0.0514(12) Uani 1 1 d . . . H4 H 0.2091 1.2588 0.7770 0.062 Uiso 1 1 calc R . . C5 C 0.4130(6) 1.1865(5) 0.7254(3) 0.0431(10) Uani 1 1 d . . . C6 C 0.5098(6) 1.0733(5) 0.7206(3) 0.0441(10) Uani 1 1 d . . . C7 C 0.4370(7) 1.3047(6) 0.6836(3) 0.0513(12) Uani 1 1 d . . . C8 C 0.5544(8) 1.3482(7) 0.6884(4) 0.0601(15) Uani 1 1 d . . . H8 H 0.6242 1.3032 0.7188 0.072 Uiso 1 1 calc R . . C9 C 0.5735(9) 1.4587(8) 0.6487(5) 0.0712(18) Uani 1 1 d . . . H9 H 0.6571 1.4858 0.6525 0.085 Uiso 1 1 calc R . . C10 C 0.4746(8) 1.5291(7) 0.6045(4) 0.0613(15) Uani 1 1 d . . . C11 C 0.3524(9) 1.4866(8) 0.6004(4) 0.0686(18) Uani 1 1 d . . . H11 H 0.2834 1.5325 0.5697 0.082 Uiso 1 1 calc R . . C12 C 0.3291(9) 1.3787(7) 0.6402(4) 0.0641(16) Uani 1 1 d . . . H12 H 0.2429 1.3541 0.6387 0.077 Uiso 1 1 calc R . . C13 C 0.5047(12) 1.6540(9) 0.5642(6) 0.089(3) Uani 1 1 d . . . H13A H 0.4303 1.6917 0.5322 0.133 Uiso 1 1 calc R . . H13B H 0.5977 1.6396 0.5359 0.133 Uiso 1 1 calc R . . H13C H 0.5046 1.7078 0.5997 0.133 Uiso 1 1 calc R . . C14 C 0.6402(7) 1.0673(5) 0.6628(3) 0.0489(11) Uani 1 1 d . . . H14A H 0.6123 1.1193 0.6178 0.059 Uiso 1 1 calc R . . H14B H 0.7169 1.0957 0.6802 0.059 Uiso 1 1 calc R . . C15 C 0.7286(7) 0.9108(6) 0.5869(3) 0.0519(12) Uani 1 1 d . . . H15 H 0.7422 0.8273 0.5829 0.062 Uiso 1 1 calc R . . C16 C 0.7560(7) 0.9891(6) 0.5166(3) 0.0518(12) Uani 1 1 d . . . C17 C 0.8336(7) 1.0815(6) 0.5067(3) 0.0521(12) Uani 1 1 d . . . C18 C 0.8715(8) 1.1397(7) 0.4393(4) 0.0637(16) Uani 1 1 d . . . H18 H 0.9243 1.2009 0.4344 0.076 Uiso 1 1 calc R . . C19 C 0.8284(9) 1.1047(8) 0.3771(4) 0.073(2) Uani 1 1 d . . . H19 H 0.8576 1.1408 0.3306 0.087 Uiso 1 1 calc R . . C20 C 0.7474(10) 1.0220(8) 0.3832(4) 0.074(2) Uani 1 1 d . . . H20 H 0.7118 1.0056 0.3423 0.089 Uiso 1 1 calc R . . C21 C 0.7171(7) 0.9609(7) 0.4519(3) 0.0562(14) Uani 1 1 d . . . C22 C 0.5520(6) 0.7558(5) 0.9273(3) 0.0445(10) Uani 1 1 d . . . C23 C 0.4375(7) 0.7381(7) 0.9776(3) 0.0549(13) Uani 1 1 d . . . H23 H 0.3714 0.6950 0.9678 0.066 Uiso 1 1 calc R . . C24 C 0.4220(8) 0.7856(7) 1.0437(4) 0.0648(17) Uani 1 1 d . . . H24 H 0.3446 0.7731 1.0781 0.078 Uiso 1 1 calc R . . C25 C 0.5169(9) 0.8505(8) 1.0602(4) 0.0675(17) Uani 1 1 d . . . H25 H 0.5031 0.8822 1.1047 0.081 Uiso 1 1 calc R . . C26 C 0.6313(8) 0.8674(7) 1.0104(4) 0.0613(15) Uani 1 1 d . . . H26 H 0.6987 0.9085 1.0210 0.074 Uiso 1 1 calc R . . C27 C 0.6458(8) 0.8225(6) 0.9438(4) 0.0572(14) Uani 1 1 d . . . H27 H 0.7214 0.8377 0.9089 0.069 Uiso 1 1 calc R . . C28 C 0.4439(6) 0.6240(5) 0.8296(3) 0.0439(10) Uani 1 1 d . . . C29 C 0.4123(7) 0.5259(7) 0.8791(4) 0.0574(14) Uani 1 1 d . . . H29 H 0.4675 0.4942 0.9184 0.069 Uiso 1 1 calc R . . C30 C 0.2948(7) 0.4742(7) 0.8691(4) 0.0568(14) Uani 1 1 d . . . H30 H 0.2731 0.4069 0.9010 0.068 Uiso 1 1 calc R . . C31 C 0.2136(7) 0.5259(7) 0.8113(4) 0.0593(15) Uani 1 1 d . . . H31 H 0.1339 0.4947 0.8058 0.071 Uiso 1 1 calc R . . C32 C 0.2459(8) 0.6201(7) 0.7626(4) 0.0595(15) Uani 1 1 d . . . H32 H 0.1906 0.6508 0.7232 0.071 Uiso 1 1 calc R . . C33 C 0.3604(6) 0.6714(5) 0.7705(3) 0.0460(11) Uani 1 1 d . . . H33 H 0.3819 0.7369 0.7370 0.055 Uiso 1 1 calc R . . C34 C 0.7333(6) 0.5482(6) 0.8652(3) 0.0467(11) Uani 1 1 d . . . C35 C 0.8060(8) 0.5301(7) 0.9288(4) 0.0639(16) Uani 1 1 d . . . H35 H 0.7859 0.5905 0.9600 0.077 Uiso 1 1 calc R . . C36 C 0.9061(11) 0.4232(10) 0.9441(6) 0.085(2) Uani 1 1 d . . . H36 H 0.9561 0.4115 0.9855 0.102 Uiso 1 1 calc R . . C37 C 0.9343(10) 0.3319(8) 0.8987(5) 0.076(2) Uani 1 1 d . . . H37 H 0.9982 0.2570 0.9110 0.092 Uiso 1 1 calc R . . C38 C 0.8688(9) 0.3523(8) 0.8371(5) 0.0689(18) Uani 1 1 d . . . H38 H 0.8933 0.2930 0.8051 0.083 Uiso 1 1 calc R . . C39 C 0.7671(8) 0.4576(7) 0.8196(4) 0.0604(15) Uani 1 1 d . . . H39 H 0.7208 0.4682 0.7770 0.072 Uiso 1 1 calc R . . Cl1 Cl 0.8761(4) 1.0221(4) 0.8159(2) 0.0706(9) Uani 0.50 1 d P . . Cl2 Cl 1.0435(5) 0.8400(5) 0.9141(2) 0.0789(11) Uani 0.50 1 d P . . C1W C 0.9977(10) 0.8912(9) 0.8243(6) 0.0397(19) Uani 0.50 1 d P . . H1W1 H 1.0852 0.9012 0.7927 0.048 Uiso 0.50 1 calc PR . . H1W2 H 0.9606 0.8283 0.8072 0.048 Uiso 0.50 1 calc PR . . O1W O 0.9512(10) 0.6478(9) 0.4860(5) 0.057(2) Uani 0.50 1 d P . . O2W O 1.0301(15) 0.7330(14) 0.3375(7) 0.088(4) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt 0.04360(14) 0.04208(16) 0.03947(13) -0.00237(8) -0.00331(7) -0.01030(8) Br 0.0554(3) 0.0587(4) 0.0588(4) -0.0020(3) -0.0008(3) -0.0076(3) P 0.0440(7) 0.0427(8) 0.0383(6) -0.0021(5) -0.0047(5) -0.0113(5) N1 0.041(2) 0.037(2) 0.0329(17) -0.0012(14) -0.0037(14) -0.0123(15) F1 0.068(2) 0.067(3) 0.061(2) -0.0082(18) -0.0029(18) -0.0216(18) F2 0.096(3) 0.085(4) 0.066(3) -0.009(2) -0.012(2) -0.035(3) C1 0.044(2) 0.034(3) 0.044(2) -0.0038(18) -0.0101(18) -0.0078(17) C2 0.056(3) 0.039(3) 0.049(3) -0.001(2) -0.014(2) -0.009(2) C3 0.044(3) 0.051(3) 0.052(3) -0.012(2) -0.002(2) -0.009(2) C4 0.053(3) 0.050(3) 0.052(3) -0.009(2) -0.002(2) -0.013(2) C5 0.046(3) 0.040(3) 0.044(2) -0.0071(19) -0.0031(19) -0.0092(18) C6 0.046(3) 0.046(3) 0.040(2) -0.0056(19) -0.0037(18) -0.0092(19) C7 0.057(3) 0.046(3) 0.050(3) -0.005(2) -0.007(2) -0.011(2) C8 0.064(4) 0.053(4) 0.063(4) -0.005(3) -0.012(3) -0.013(3) C9 0.073(5) 0.065(5) 0.078(5) -0.011(4) -0.002(4) -0.023(3) C10 0.070(4) 0.048(4) 0.064(4) -0.010(3) -0.002(3) -0.010(3) C11 0.071(4) 0.072(5) 0.060(4) -0.001(3) -0.010(3) -0.013(3) C12 0.070(4) 0.058(4) 0.064(4) -0.004(3) -0.011(3) -0.015(3) C13 0.100(7) 0.079(7) 0.083(6) -0.006(5) -0.001(5) -0.019(5) C14 0.054(3) 0.042(3) 0.051(3) -0.004(2) -0.003(2) -0.014(2) C15 0.056(3) 0.051(4) 0.050(3) -0.006(2) -0.003(2) -0.017(2) C16 0.052(3) 0.051(4) 0.051(3) 0.000(2) -0.006(2) -0.012(2) C17 0.053(3) 0.050(3) 0.052(3) -0.004(2) -0.003(2) -0.011(2) C18 0.066(4) 0.059(4) 0.063(4) -0.001(3) -0.001(3) -0.014(3) C19 0.073(5) 0.076(6) 0.061(4) 0.008(3) -0.003(3) -0.013(4) C20 0.090(6) 0.076(6) 0.053(4) -0.001(3) -0.010(3) -0.016(4) C21 0.062(4) 0.058(4) 0.047(3) -0.003(2) -0.005(2) -0.013(3) C22 0.044(3) 0.051(3) 0.039(2) -0.006(2) -0.0013(18) -0.013(2) C23 0.053(3) 0.063(4) 0.049(3) -0.006(3) 0.001(2) -0.015(2) C24 0.068(4) 0.072(5) 0.054(3) -0.010(3) 0.005(3) -0.019(3) C25 0.076(5) 0.067(5) 0.061(4) -0.014(3) -0.008(3) -0.014(3) C26 0.068(4) 0.062(4) 0.058(3) -0.011(3) -0.009(3) -0.018(3) C27 0.063(4) 0.057(4) 0.055(3) -0.010(3) -0.004(3) -0.019(3) C28 0.044(3) 0.043(3) 0.046(2) -0.003(2) -0.0046(19) -0.0145(19) C29 0.053(3) 0.059(4) 0.058(3) 0.003(3) -0.007(3) -0.016(3) C30 0.060(3) 0.057(4) 0.055(3) -0.002(3) -0.001(3) -0.021(3) C31 0.056(3) 0.057(4) 0.069(4) -0.007(3) -0.011(3) -0.020(3) C32 0.059(4) 0.061(4) 0.058(3) -0.008(3) -0.010(3) -0.012(3) C33 0.049(3) 0.042(3) 0.047(2) -0.002(2) -0.009(2) -0.010(2) C34 0.045(3) 0.048(3) 0.045(3) -0.003(2) -0.0014(19) -0.010(2) C35 0.066(4) 0.062(4) 0.058(4) -0.005(3) -0.011(3) -0.004(3) C36 0.083(6) 0.080(7) 0.086(6) 0.004(5) -0.019(5) -0.008(4) C37 0.071(5) 0.063(5) 0.086(6) 0.000(4) 0.000(4) -0.008(3) C38 0.071(4) 0.058(4) 0.070(4) -0.003(3) 0.005(3) -0.008(3) C39 0.062(4) 0.061(4) 0.057(3) -0.010(3) -0.005(3) -0.012(3) Cl1 0.069(2) 0.058(2) 0.087(2) 0.0076(16) -0.0243(17) -0.0195(15) Cl2 0.068(2) 0.094(3) 0.070(2) 0.0166(19) -0.0109(16) -0.0260(19) C1W 0.034(4) 0.039(5) 0.048(5) -0.010(4) 0.002(3) -0.014(3) O1W 0.061(5) 0.052(5) 0.061(5) -0.009(4) -0.007(4) -0.019(4) O2W 0.084(8) 0.109(11) 0.078(7) -0.024(7) -0.005(6) -0.030(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 Pt C1 2.041(5) . ? Pt N1 2.055(4) . ? Pt P 2.2386(16) . ? Pt Br 2.5017(13) . ? P C28 1.814(5) . ? P C22 1.827(5) . ? P C34 1.836(6) . ? N1 C15 1.232(7) . ? N1 C14 1.477(7) . ? F1 C17 1.337(8) . ? F2 C21 1.357(8) . ? C1 C2 1.306(8) . ? C1 C6 1.404(8) . ? C2 C3 1.425(8) . ? C2 H2 0.9300 . ? C3 C4 1.390(9) . ? C3 H3 0.9300 . ? C4 C5 1.447(9) . ? C4 H4 0.9300 . ? C5 C6 1.391(8) . ? C5 C7 1.480(9) . ? C6 C14 1.523(8) . ? C7 C8 1.338(10) . ? C7 C12 1.412(10) . ? C8 C9 1.379(11) . ? C8 H8 0.9300 . ? C9 C10 1.352(11) . ? C9 H9 0.9300 . ? C10 C11 1.372(11) . ? C10 C13 1.554(12) . ? C11 C12 1.366(11) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.484(9) . ? C15 H15 0.9300 . ? C16 C17 1.387(9) . ? C16 C21 1.402(9) . ? C17 C18 1.361(9) . ? C18 C19 1.412(12) . ? C18 H18 0.9300 . ? C19 C20 1.324(12) . ? C19 H19 0.9300 . ? C20 C21 1.378(10) . ? C20 H20 0.9300 . ? C22 C23 1.368(8) . ? C22 C27 1.382(8) . ? C23 C24 1.387(9) . ? C23 H23 0.9300 . ? C24 C25 1.375(11) . ? C24 H24 0.9300 . ? C25 C26 1.360(11) . ? C25 H25 0.9300 . ? C26 C27 1.383(9) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.384(8) . ? C28 C33 1.399(8) . ? C29 C30 1.420(9) . ? C29 H29 0.9300 . ? C30 C31 1.375(10) . ? C30 H30 0.9300 . ? C31 C32 1.347(10) . ? C31 H31 0.9300 . ? C32 C33 1.381(8) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C39 1.378(9) . ? C34 C35 1.406(9) . ? C35 C36 1.362(12) . ? C35 H35 0.9300 . ? C36 C37 1.383(14) . ? C36 H36 0.9300 . ? C37 C38 1.334(12) . ? C37 H37 0.9300 . ? C38 C39 1.365(11) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? Cl1 C1W 1.642(11) . ? Cl2 C1W 1.751(11) . ? C1W H1W1 0.9700 . ? C1W H1W2 0.9700 . ? 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 Pt N1 81.4(2) . . ? C1 Pt P 96.14(16) . . ? N1 Pt P 176.01(11) . . ? C1 Pt Br 168.25(16) . . ? N1 Pt Br 87.53(12) . . ? P Pt Br 95.16(5) . . ? C28 P C22 107.0(2) . . ? C28 P C34 101.0(3) . . ? C22 P C34 102.5(3) . . ? C28 P Pt 112.25(19) . . ? C22 P Pt 115.5(2) . . ? C34 P Pt 117.09(18) . . ? C15 N1 C14 120.4(5) . . ? C15 N1 Pt 126.7(4) . . ? C14 N1 Pt 111.9(3) . . ? C2 C1 C6 120.0(5) . . ? C2 C1 Pt 128.5(4) . . ? C6 C1 Pt 111.5(4) . . ? C1 C2 C3 120.8(6) . . ? C1 C2 H2 119.6 . . ? C3 C2 H2 119.6 . . ? C4 C3 C2 121.1(6) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 118.1(6) . . ? C3 C4 H4 121.0 . . ? C5 C4 H4 121.0 . . ? C6 C5 C4 117.2(6) . . ? C6 C5 C7 124.0(5) . . ? C4 C5 C7 118.9(6) . . ? C5 C6 C1 122.7(5) . . ? C5 C6 C14 118.3(5) . . ? C1 C6 C14 118.9(5) . . ? C8 C7 C12 118.1(7) . . ? C8 C7 C5 122.3(6) . . ? C12 C7 C5 119.5(6) . . ? C7 C8 C9 120.9(7) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C10 C9 C8 122.2(8) . . ? C10 C9 H9 118.9 . . ? C8 C9 H9 118.9 . . ? C9 C10 C11 117.3(8) . . ? C9 C10 C13 117.9(8) . . ? C11 C10 C13 124.7(8) . . ? C12 C11 C10 121.8(8) . . ? C12 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? C11 C12 C7 119.6(7) . . ? C11 C12 H12 120.2 . . ? C7 C12 H12 120.2 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N1 C14 C6 107.0(4) . . ? N1 C14 H14A 110.3 . . ? C6 C14 H14A 110.3 . . ? N1 C14 H14B 110.3 . . ? C6 C14 H14B 110.3 . . ? H14A C14 H14B 108.6 . . ? N1 C15 C16 131.3(6) . . ? N1 C15 H15 114.4 . . ? C16 C15 H15 114.4 . . ? C17 C16 C21 114.9(6) . . ? C17 C16 C15 125.5(6) . . ? C21 C16 C15 119.1(6) . . ? F1 C17 C18 119.9(6) . . ? F1 C17 C16 117.0(5) . . ? C18 C17 C16 122.9(6) . . ? C17 C18 C19 118.2(7) . . ? C17 C18 H18 120.9 . . ? C19 C18 H18 120.9 . . ? C20 C19 C18 121.7(7) . . ? C20 C19 H19 119.1 . . ? C18 C19 H19 119.1 . . ? C19 C20 C21 118.2(8) . . ? C19 C20 H20 120.9 . . ? C21 C20 H20 120.9 . . ? F2 C21 C20 119.4(6) . . ? F2 C21 C16 116.8(6) . . ? C20 C21 C16 123.7(7) . . ? C23 C22 C27 118.5(5) . . ? C23 C22 P 124.1(5) . . ? C27 C22 P 117.3(4) . . ? C22 C23 C24 118.8(6) . . ? C22 C23 H23 120.6 . . ? C24 C23 H23 120.6 . . ? C25 C24 C23 122.4(7) . . ? C25 C24 H24 118.8 . . ? C23 C24 H24 118.8 . . ? C26 C25 C24 118.9(7) . . ? C26 C25 H25 120.5 . . ? C24 C25 H25 120.5 . . ? C25 C26 C27 119.0(7) . . ? C25 C26 H26 120.5 . . ? C27 C26 H26 120.5 . . ? C22 C27 C26 122.3(6) . . ? C22 C27 H27 118.8 . . ? C26 C27 H27 118.8 . . ? C29 C28 C33 120.1(5) . . ? C29 C28 P 119.5(4) . . ? C33 C28 P 120.4(4) . . ? C28 C29 C30 119.3(6) . . ? C28 C29 H29 120.4 . . ? C30 C29 H29 120.4 . . ? C31 C30 C29 118.5(6) . . ? C31 C30 H30 120.7 . . ? C29 C30 H30 120.7 . . ? C32 C31 C30 122.1(6) . . ? C32 C31 H31 119.0 . . ? C30 C31 H31 119.0 . . ? C31 C32 C33 120.6(6) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? C32 C33 C28 119.4(6) . . ? C32 C33 H33 120.3 . . ? C28 C33 H33 120.3 . . ? C39 C34 C35 118.9(6) . . ? C39 C34 P 119.1(5) . . ? C35 C34 P 122.0(5) . . ? C36 C35 C34 119.3(8) . . ? C36 C35 H35 120.4 . . ? C34 C35 H35 120.4 . . ? C35 C36 C37 120.6(9) . . ? C35 C36 H36 119.7 . . ? C37 C36 H36 119.7 . . ? C38 C37 C36 119.4(8) . . ? C38 C37 H37 120.3 . . ? C36 C37 H37 120.3 . . ? C37 C38 C39 122.1(8) . . ? C37 C38 H38 119.0 . . ? C39 C38 H38 119.0 . . ? C38 C39 C34 119.6(7) . . ? C38 C39 H39 120.2 . . ? C34 C39 H39 120.2 . . ? Cl1 C1W Cl2 113.9(6) . . ? Cl1 C1W H1W1 108.8 . . ? Cl2 C1W H1W1 108.8 . . ? Cl1 C1W H1W2 108.8 . . ? Cl2 C1W H1W2 108.8 . . ? H1W1 C1W H1W2 107.7 . . ? _diffrn_measured_fraction_theta_max 0.690 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.880 _refine_diff_density_max 2.114 _refine_diff_density_min -1.466 _refine_diff_density_rms 0.294 #===END