Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _publ_contact_author_name 'Professor John S. Field' _publ_contact_author_address ; School of Chemcical and Physical Sciences, University of Natal, Pietermaritzburg 3201 South Africa ; _publ_contact_author_email 'fieldj@nu.ac.za' loop_ _publ_author_name 'John S Field' 'Raymond J Haines' 'David R McMillin' 'Grant C Summerton' _journal_coden_Cambridge 186 _journal_name_full 'J Chemical Society Dalton Transactions' data_gs10 _database_code_CSD 168557 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Pt(4'(C6H4-CF3-o)trpy)Cl]SbF6' _chemical_formula_sum 'C22 H14 Cl F9 N3 Pt Sb' _chemical_formula_weight 843.64 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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P2(1)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.93(2) _cell_length_b 20.114(5) _cell_length_c 17.979(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.750(5) _cell_angle_gamma 90.00 _cell_volume 2462(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 2 _cell_measurement_theta_max 12 _exptl_crystal_description 'needle' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.95 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.276 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 6.967 _exptl_absorpt_correction_type 'psi-scans' _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 0.99 _exptl_absorpt_process_details ; Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166' ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius CAD4' _diffrn_measurement_method 'omega-2theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '60 minutes' _diffrn_standards_decay_% 0 _diffrn_reflns_number 4055 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0471 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 22.97 _reflns_number_total 3423 _reflns_number_gt 2504 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius CAD4' _computing_cell_refinement 'CELDIM, CAD4' _computing_data_reduction 'XCAD (McArdle, 2000)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP 3 (Farrugia, 2000)' _computing_publication_material 'ORTEP 3 (Farrugia, 2000)' _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3423 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0745 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1317 _refine_ls_wR_factor_gt 0.1160 _refine_ls_goodness_of_fit_ref 0.943 _refine_ls_restrained_S_all 0.943 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt 0.74991(6) 0.02907(2) 0.49460(2) 0.0439(2) Uani 1 1 d . . . Sb Sb 0.07891(14) 0.15069(5) 0.16154(5) 0.0674(3) Uani 1 1 d . . . Cl Cl 0.8122(5) 0.0621(2) 0.61845(17) 0.0688(9) Uani 1 1 d . . . F1 F 0.2111(13) -0.0700(6) 0.2019(5) 0.106(3) Uani 1 1 d . . . F2 F 0.3238(15) -0.1676(6) 0.2044(6) 0.126(4) Uani 1 1 d . . . F3 F 0.1130(13) -0.1358(5) 0.1102(5) 0.103(3) Uani 1 1 d . . . F4 F 0.109(3) 0.0723(6) 0.1134(9) 0.206(8) Uani 1 1 d . . . F5 F 0.049(2) 0.1000(8) 0.2453(6) 0.176(6) Uani 1 1 d . . . F6 F 0.026(3) 0.2241(6) 0.2081(9) 0.226(8) Uani 1 1 d . . . F7 F 0.078(2) 0.1951(7) 0.0765(7) 0.182(7) Uani 1 1 d . . . F8 F 0.334(2) 0.1537(12) 0.1864(15) 0.325(15) Uani 1 1 d . . . F9 F -0.191(2) 0.1398(9) 0.1347(10) 0.197(7) Uani 1 1 d . . . N1 N 0.7312(13) 0.1187(5) 0.4450(5) 0.050(2) Uani 1 1 d . . . N2 N 0.6971(12) 0.0011(5) 0.3900(5) 0.041(2) Uani 1 1 d . . . N3 N 0.7515(12) -0.0700(5) 0.5109(5) 0.046(2) Uani 1 1 d . . . C1 C 0.7526(17) 0.1789(6) 0.4784(7) 0.058(3) Uani 1 1 d . . . H1 H 0.7819 0.1818 0.5310 0.059(9) Uiso 1 1 calc R . . C2 C 0.7319(19) 0.2359(7) 0.4363(8) 0.069(4) Uani 1 1 d . . . H2 H 0.7381 0.2771 0.4601 0.059(9) Uiso 1 1 calc R . . C3 C 0.7021(19) 0.2323(7) 0.3598(7) 0.065(3) Uani 1 1 d . . . H3 H 0.6946 0.2711 0.3312 0.059(9) Uiso 1 1 calc R . . C4 C 0.6831(17) 0.1719(6) 0.3242(7) 0.054(3) Uani 1 1 d . . . H4 H 0.6593 0.1695 0.2717 0.059(9) Uiso 1 1 calc R . . C5 C 0.6991(15) 0.1160(6) 0.3660(6) 0.042(3) Uani 1 1 d . . . C6 C 0.6747(16) 0.0480(5) 0.3355(6) 0.042(3) Uani 1 1 d . . . C7 C 0.6353(15) 0.0281(6) 0.2610(6) 0.043(3) Uani 1 1 d . . . H7 H 0.6184 0.0596 0.2225 0.059(9) Uiso 1 1 calc R . . C8 C 0.6207(15) -0.0392(5) 0.2434(6) 0.040(3) Uani 1 1 d . . . C9 C 0.6456(15) -0.0848(6) 0.2999(5) 0.044(3) Uani 1 1 d . . . H9 H 0.6379 -0.1299 0.2883 0.059(9) Uiso 1 1 calc R . . C10 C 0.6830(15) -0.0641(6) 0.3757(6) 0.047(3) Uani 1 1 d . . . C11 C 0.7124(17) -0.1063(6) 0.4452(6) 0.051(3) Uani 1 1 d . . . C12 C 0.7071(19) -0.1738(6) 0.4456(7) 0.061(3) Uani 1 1 d . . . H12 H 0.6793 -0.1976 0.4005 0.059(9) Uiso 1 1 calc R . . C13 C 0.7440(19) -0.2065(7) 0.5145(8) 0.071(4) Uani 1 1 d . . . H13 H 0.7461 -0.2527 0.5160 0.059(9) Uiso 1 1 calc R . . C14 C 0.7778(19) -0.1705(8) 0.5812(7) 0.067(4) Uani 1 1 d . . . H14 H 0.7955 -0.1922 0.6277 0.059(9) Uiso 1 1 calc R . . C15 C 0.7848(17) -0.1038(7) 0.5781(6) 0.059(3) Uani 1 1 d . . . H15 H 0.8131 -0.0798 0.6231 0.059(9) Uiso 1 1 calc R . . C16 C 0.5932(17) -0.0581(5) 0.1605(6) 0.047(3) Uani 1 1 d . . . C17 C 0.738(2) -0.0387(7) 0.1231(7) 0.067(4) Uani 1 1 d . . . H17 H 0.8486 -0.0161 0.1481 0.059(9) Uiso 1 1 calc R . . C18 C 0.715(2) -0.0537(7) 0.0461(8) 0.070(4) Uani 1 1 d . . . H18 H 0.8126 -0.0391 0.0207 0.059(9) Uiso 1 1 calc R . . C19 C 0.570(2) -0.0861(7) 0.0074(6) 0.067(4) Uani 1 1 d . . . H19 H 0.5645 -0.0956 -0.0436 0.059(9) Uiso 1 1 calc R . . C20 C 0.427(2) -0.1057(6) 0.0440(7) 0.067(4) Uani 1 1 d . . . H20 H 0.3190 -0.1281 0.0167 0.059(9) Uiso 1 1 calc R . . C21 C 0.4328(19) -0.0938(5) 0.1229(6) 0.052(3) Uani 1 1 d . . . C22 C 0.270(2) -0.1154(8) 0.1592(8) 0.070(4) 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 Pt 0.0305(3) 0.0647(3) 0.0369(3) -0.0071(2) 0.00762(18) -0.0019(2) Sb 0.0729(6) 0.0793(6) 0.0484(5) 0.0079(4) 0.0073(4) 0.0039(5) Cl 0.0581(19) 0.104(3) 0.0433(16) -0.0193(17) 0.0072(14) -0.0013(19) F1 0.078(6) 0.162(9) 0.080(6) -0.043(6) 0.021(5) -0.041(6) F2 0.097(7) 0.138(9) 0.134(8) 0.069(8) -0.004(6) -0.023(7) F3 0.077(6) 0.128(8) 0.091(6) -0.021(6) -0.017(5) -0.028(6) F4 0.36(2) 0.111(10) 0.196(14) -0.021(9) 0.191(16) 0.021(12) F5 0.242(16) 0.218(14) 0.074(7) 0.056(8) 0.044(8) 0.056(12) F6 0.39(3) 0.107(9) 0.192(14) -0.064(10) 0.092(15) -0.026(12) F7 0.223(14) 0.202(14) 0.147(10) 0.114(10) 0.100(10) 0.093(12) F8 0.072(9) 0.36(3) 0.49(4) 0.15(3) -0.084(15) -0.033(14) F9 0.094(9) 0.275(19) 0.216(16) -0.008(14) 0.019(9) -0.037(11) N1 0.032(5) 0.067(7) 0.051(6) -0.013(5) 0.006(4) -0.006(5) N2 0.028(5) 0.049(5) 0.045(5) -0.009(5) 0.006(4) -0.003(4) N3 0.040(5) 0.062(6) 0.038(5) 0.001(4) 0.010(4) 0.006(5) C1 0.056(8) 0.055(8) 0.063(7) -0.029(7) 0.010(6) -0.008(6) C2 0.060(9) 0.072(10) 0.074(9) -0.013(8) 0.011(7) -0.010(7) C3 0.066(9) 0.061(9) 0.070(9) 0.004(7) 0.020(7) -0.001(7) C4 0.057(8) 0.049(8) 0.060(7) -0.005(6) 0.020(6) 0.005(6) C5 0.030(6) 0.052(7) 0.048(6) -0.001(5) 0.015(5) -0.001(5) C6 0.042(6) 0.042(7) 0.044(6) 0.000(5) 0.017(5) -0.001(5) C7 0.032(6) 0.053(7) 0.045(6) 0.003(5) 0.009(5) -0.004(5) C8 0.035(6) 0.047(7) 0.038(6) -0.005(5) 0.006(4) 0.005(5) C9 0.038(6) 0.048(6) 0.042(6) -0.008(6) 0.001(5) 0.013(5) C10 0.030(6) 0.057(8) 0.054(7) 0.002(6) 0.004(5) 0.003(5) C11 0.043(7) 0.065(9) 0.046(7) 0.000(6) 0.007(5) 0.003(6) C12 0.063(8) 0.058(8) 0.057(7) 0.007(6) -0.003(6) -0.010(6) C13 0.073(10) 0.060(9) 0.078(10) 0.023(7) 0.008(8) 0.005(7) C14 0.056(8) 0.090(11) 0.052(8) 0.016(8) 0.005(6) -0.003(7) C15 0.046(7) 0.092(11) 0.039(7) -0.010(7) 0.006(5) 0.002(7) C16 0.054(7) 0.044(6) 0.044(6) -0.006(5) 0.010(5) 0.009(6) C17 0.071(9) 0.077(9) 0.052(7) 0.007(7) 0.009(7) 0.019(7) C18 0.078(10) 0.082(10) 0.055(8) 0.001(7) 0.026(7) 0.007(8) C19 0.103(11) 0.071(9) 0.028(6) -0.009(6) 0.015(7) 0.026(9) C20 0.088(10) 0.060(8) 0.042(7) -0.007(6) -0.016(7) -0.003(7) C21 0.071(8) 0.036(6) 0.045(6) -0.007(5) 0.003(6) 0.010(6) C22 0.061(9) 0.084(10) 0.055(8) -0.008(8) -0.011(7) -0.021(8) _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 N2 1.931(8) . ? Pt N1 2.004(10) . ? Pt N3 2.014(10) . ? Pt Cl 2.286(3) . ? Sb F8 1.742(14) . ? Sb F6 1.769(13) . ? Sb F7 1.770(9) . ? Sb F4 1.829(12) . ? Sb F9 1.853(15) . ? Sb F5 1.860(11) . ? F1 C22 1.306(17) . ? F2 C22 1.337(17) . ? F3 C22 1.332(15) . ? N1 C1 1.349(15) . ? N1 C5 1.397(13) . ? N2 C10 1.336(15) . ? N2 C6 1.349(14) . ? N3 C15 1.368(14) . ? N3 C11 1.372(14) . ? C1 C2 1.367(18) . ? C2 C3 1.355(17) . ? C3 C4 1.367(17) . ? C4 C5 1.346(15) . ? C5 C6 1.471(15) . ? C6 C7 1.376(15) . ? C7 C8 1.390(14) . ? C8 C9 1.355(14) . ? C8 C16 1.516(14) . ? C9 C10 1.403(15) . ? C10 C11 1.492(16) . ? C11 C12 1.358(17) . ? C12 C13 1.383(17) . ? C13 C14 1.383(19) . ? C14 C15 1.344(19) . ? C16 C17 1.366(18) . ? C16 C21 1.387(16) . ? C17 C18 1.397(18) . ? C18 C19 1.288(19) . ? C19 C20 1.348(19) . ? C20 C21 1.433(16) . ? C21 C22 1.471(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pt N1 81.1(4) . . ? N2 Pt N3 81.2(4) . . ? N1 Pt N3 162.3(3) . . ? N2 Pt Cl 179.9(3) . . ? N1 Pt Cl 99.0(3) . . ? N3 Pt Cl 98.7(3) . . ? F8 Sb F6 98.0(12) . . ? F8 Sb F7 92.4(9) . . ? F6 Sb F7 91.2(7) . . ? F8 Sb F4 87.1(11) . . ? F6 Sb F4 174.5(9) . . ? F7 Sb F4 90.5(7) . . ? F8 Sb F9 175.2(10) . . ? F6 Sb F9 86.2(10) . . ? F7 Sb F9 89.7(8) . . ? F4 Sb F9 88.6(8) . . ? F8 Sb F5 94.1(9) . . ? F6 Sb F5 90.6(7) . . ? F7 Sb F5 173.0(7) . . ? F4 Sb F5 87.1(6) . . ? F9 Sb F5 83.6(8) . . ? C1 N1 C5 118.1(11) . . ? C1 N1 Pt 128.1(8) . . ? C5 N1 Pt 113.7(7) . . ? C10 N2 C6 123.6(9) . . ? C10 N2 Pt 117.9(8) . . ? C6 N2 Pt 118.6(8) . . ? C15 N3 C11 118.0(11) . . ? C15 N3 Pt 128.0(8) . . ? C11 N3 Pt 114.0(7) . . ? N1 C1 C2 121.0(12) . . ? C3 C2 C1 119.9(13) . . ? C2 C3 C4 120.3(13) . . ? C5 C4 C3 119.4(11) . . ? C4 C5 N1 121.1(10) . . ? C4 C5 C6 125.2(10) . . ? N1 C5 C6 113.6(9) . . ? N2 C6 C7 118.6(10) . . ? N2 C6 C5 112.9(9) . . ? C7 C6 C5 128.5(10) . . ? C6 C7 C8 119.9(10) . . ? C9 C8 C7 119.7(10) . . ? C9 C8 C16 122.8(9) . . ? C7 C8 C16 117.3(9) . . ? C8 C9 C10 120.1(10) . . ? N2 C10 C9 118.2(10) . . ? N2 C10 C11 113.8(10) . . ? C9 C10 C11 128.1(11) . . ? C12 C11 N3 121.9(11) . . ? C12 C11 C10 125.0(11) . . ? N3 C11 C10 113.1(10) . . ? C11 C12 C13 118.7(12) . . ? C14 C13 C12 120.0(13) . . ? C15 C14 C13 119.3(12) . . ? C14 C15 N3 122.1(12) . . ? C17 C16 C21 120.3(11) . . ? C17 C16 C8 116.3(11) . . ? C21 C16 C8 123.4(10) . . ? C16 C17 C18 117.9(13) . . ? C19 C18 C17 125.3(14) . . ? C18 C19 C20 117.2(11) . . ? C19 C20 C21 123.1(13) . . ? C16 C21 C20 116.2(12) . . ? C16 C21 C22 123.2(10) . . ? C20 C21 C22 120.5(12) . . ? F1 C22 F3 107.4(13) . . ? F1 C22 F2 105.9(12) . . ? F3 C22 F2 105.1(12) . . ? F1 C22 C21 113.8(12) . . ? F3 C22 C21 113.4(12) . . ? F2 C22 C21 110.6(12) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 22.97 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.035 _refine_diff_density_min -1.075 _refine_diff_density_rms 0.186 data_gs06 _database_code_CSD 168558 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Pt(4'(C6H4-CH3-o)trpy)Cl]SbF6' _chemical_formula_sum 'C22 H17 Cl F6 N3 Pt Sb' _chemical_formula_weight 789.67 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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M 'Pna2(1)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 19.64(2) _cell_length_b 18.166(5) _cell_length_c 6.653(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2373(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 2 _cell_measurement_theta_max 12 _exptl_crystal_description 'needle' _exptl_crystal_colour 'red' _exptl_crystal_size_max 1.15 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.210 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 7.202 _exptl_absorpt_correction_type 'psi scans' _exptl_absorpt_correction_T_min 0.58 _exptl_absorpt_correction_T_max 0.99 _exptl_absorpt_process_details ; Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166' ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius CAD4' _diffrn_measurement_method 'omega 2 theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '60 minutes' _diffrn_standards_decay_% 0 _diffrn_reflns_number 2450 _diffrn_reflns_av_R_equivalents 0.0158 _diffrn_reflns_av_sigmaI/netI 0.0307 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 22.97 _reflns_number_total 2146 _reflns_number_gt 1727 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius CAD4' _computing_cell_refinement 'CELDIM, CAD4' _computing_data_reduction 'XCAD4 (McArdle, 2000)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP 3 (Farrugia, 2000)' _computing_publication_material 'ORTEP 3 (Farrugia, 2000)' _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.21(3) _refine_ls_number_reflns 2146 _refine_ls_number_parameters 182 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0533 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.1142 _refine_ls_wR_factor_gt 0.1013 _refine_ls_goodness_of_fit_ref 0.898 _refine_ls_restrained_S_all 0.898 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt 0.51243(2) 0.50563(2) 0.0000 0.0411(2) Uani 1 1 d . . . Sb Sb 0.71733(5) 0.20921(4) 0.0072(10) 0.0738(4) Uani 1 1 d . . . Cl Cl 0.49357(19) 0.38092(17) 0.004(2) 0.0641(12) Uani 1 1 d . . . F1 F 0.6461(6) 0.2706(6) 0.058(4) 0.118(8) Uani 1 1 d . . . F2 F 0.7912(6) 0.1503(6) -0.004(9) 0.190(10) Uani 1 1 d . . . F3 F 0.7656(13) 0.259(3) -0.200(7) 0.26(2) Uani 1 1 d . . . F4 F 0.7527(10) 0.2698(19) 0.180(5) 0.184(15) Uani 1 1 d . . . F5 F 0.6701(17) 0.1478(18) -0.152(6) 0.29(2) Uani 1 1 d . . . F6 F 0.6793(11) 0.1599(18) 0.213(4) 0.193(13) Uani 1 1 d . . . N1 N 0.4150(4) 0.5409(5) -0.005(4) 0.041(2) Uiso 1 1 d . . . N2 N 0.5287(4) 0.6099(5) 0.017(5) 0.041(2) Uiso 1 1 d . . . N3 N 0.6156(5) 0.5051(5) 0.009(8) 0.052(3) Uiso 1 1 d . . . C1 C 0.3583(6) 0.4989(6) -0.006(7) 0.054(4) Uiso 1 1 d . . . H1 H 0.3620 0.4479 -0.0063 0.079(13) Uiso 1 1 calc R . . C2 C 0.2979(7) 0.5303(7) -0.008(6) 0.057(4) Uiso 1 1 d . . . H2 H 0.2595 0.5009 -0.0239 0.079(13) Uiso 1 1 calc R . . C3 C 0.2896(7) 0.6057(7) 0.014(8) 0.063(4) Uiso 1 1 d . . . H3 H 0.2472 0.6264 0.0408 0.079(13) Uiso 1 1 calc R . . C4 C 0.3469(6) 0.6482(7) -0.005(6) 0.060(4) Uiso 1 1 d . . . H4 H 0.3430 0.6989 -0.0185 0.079(13) Uiso 1 1 calc R . . C5 C 0.4095(6) 0.6161(6) -0.003(6) 0.044(3) Uiso 1 1 d . . . C6 C 0.4755(5) 0.6563(6) 0.019(6) 0.045(3) Uiso 1 1 d . . . C7 C 0.4857(6) 0.7294(7) 0.040(3) 0.047(4) Uiso 1 1 d . . . H7 H 0.4486 0.7610 0.0457 0.079(13) Uiso 1 1 calc R . . C8 C 0.5506(7) 0.7575(7) 0.051(3) 0.058(4) Uiso 1 1 d . . . C9 C 0.6064(7) 0.7078(6) 0.041(3) 0.051(4) Uiso 1 1 d . . . H9 H 0.6505 0.7231 0.0699 0.079(13) Uiso 1 1 calc R . . C10 C 0.5926(6) 0.6350(6) -0.014(4) 0.043(3) Uiso 1 1 d . . . C11 C 0.6431(6) 0.5747(6) -0.005(6) 0.050(3) Uiso 1 1 d . . . C12 C 0.7108(7) 0.5836(7) 0.013(8) 0.060(3) Uiso 1 1 d . . . H12 H 0.7287 0.6301 0.0376 0.079(13) Uiso 1 1 calc R . . C13 C 0.7545(8) 0.5229(8) -0.007(7) 0.073(4) Uiso 1 1 d . . . H13 H 0.8015 0.5290 -0.0156 0.079(13) Uiso 1 1 calc R . . C14 C 0.7253(7) 0.4542(8) -0.013(5) 0.064(4) Uiso 1 1 d . . . H14 H 0.7522 0.4133 -0.0403 0.079(13) Uiso 1 1 calc R . . C15 C 0.6563(6) 0.4453(6) 0.022(5) 0.052(4) Uiso 1 1 d . . . H15 H 0.6384 0.3993 0.0533 0.079(13) Uiso 1 1 calc R . . C16 C 0.5636(8) 0.8383(8) 0.082(3) 0.056(4) Uiso 1 1 d . . . C21 C 0.5444(12) 0.8733(13) 0.252(4) 0.087(7) Uiso 1 1 d . . . C20 C 0.5583(15) 0.9488(17) 0.281(5) 0.126(10) Uiso 1 1 d . . . H20 H 0.5471 0.9734 0.3989 0.079(13) Uiso 1 1 calc R . . C19 C 0.5889(13) 0.9827(13) 0.126(4) 0.090(7) Uiso 1 1 d . . . H19 H 0.5958 1.0330 0.1405 0.079(13) Uiso 1 1 calc R . . C18 C 0.6097(9) 0.9552(10) -0.038(4) 0.085(7) Uiso 1 1 d . . . H18 H 0.6318 0.9834 -0.1346 0.079(13) Uiso 1 1 calc R . . C17 C 0.5968(9) 0.8763(10) -0.065(3) 0.081(6) Uiso 1 1 d . . . H17 H 0.6112 0.8525 -0.1812 0.079(13) Uiso 1 1 calc R . . C22 C 0.5087(12) 0.8335(16) 0.420(5) 0.137(11) Uiso 1 1 d . . . H22A H 0.4981 0.8677 0.5253 0.079(13) Uiso 1 1 calc R . . H22B H 0.5378 0.7955 0.4712 0.079(13) Uiso 1 1 calc R . . H22C H 0.4674 0.8120 0.3697 0.079(13) 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 0.0644(3) 0.0302(3) 0.0289(3) -0.0003(10) 0.0036(14) -0.00241(18) Sb 0.0919(7) 0.0405(5) 0.0890(8) -0.002(2) -0.003(2) 0.0224(4) Cl 0.101(3) 0.0324(15) 0.059(3) -0.016(6) -0.025(6) -0.0047(15) F1 0.105(7) 0.099(7) 0.15(2) -0.018(11) 0.010(11) 0.046(6) F2 0.120(8) 0.099(8) 0.35(3) -0.08(3) -0.03(3) 0.063(7) F3 0.16(2) 0.33(5) 0.28(5) 0.15(4) 0.09(3) 0.13(3) F4 0.104(12) 0.27(3) 0.18(3) -0.16(2) -0.015(14) -0.041(17) F5 0.22(2) 0.21(2) 0.43(6) -0.17(3) 0.14(3) -0.14(2) F6 0.123(14) 0.29(3) 0.16(2) 0.17(2) 0.030(15) 0.008(18) _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 N2 1.924(9) . ? Pt N1 2.019(9) . ? Pt N3 2.027(11) . ? Pt Cl 2.296(3) . ? Sb F4 1.74(2) . ? Sb F5 1.80(3) . ? Sb F6 1.798(18) . ? Sb F2 1.805(9) . ? Sb F1 1.820(10) . ? Sb F3 1.91(4) . ? N1 C1 1.349(15) . ? N1 C5 1.370(13) . ? N2 C6 1.343(13) . ? N2 C10 1.351(15) . ? N3 C15 1.353(15) . ? N3 C11 1.378(14) . ? C1 C2 1.317(18) . ? C2 C3 1.388(19) . ? C3 C4 1.370(18) . ? C4 C5 1.360(17) . ? C5 C6 1.497(15) . ? C6 C7 1.348(17) . ? C7 C8 1.374(18) . ? C8 C9 1.421(17) . ? C8 C16 1.50(2) . ? C9 C10 1.399(17) . ? C10 C11 1.477(15) . ? C11 C12 1.345(18) . ? C12 C13 1.40(2) . ? C13 C14 1.374(19) . ? C14 C15 1.38(2) . ? C16 C21 1.35(3) . ? C16 C17 1.36(2) . ? C21 C20 1.41(3) . ? C21 C22 1.50(4) . ? C20 C19 1.34(4) . ? C19 C18 1.26(4) . ? C18 C17 1.47(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pt N1 81.2(3) . . ? N2 Pt N3 80.6(4) . . ? N1 Pt N3 161.7(3) . . ? N2 Pt Cl 176.0(12) . . ? N1 Pt Cl 99.2(3) . . ? N3 Pt Cl 99.0(2) . . ? F4 Sb F5 172.0(13) . . ? F4 Sb F6 88.7(17) . . ? F5 Sb F6 85.7(12) . . ? F4 Sb F2 94.7(13) . . ? F5 Sb F2 91.3(16) . . ? F6 Sb F2 94.0(18) . . ? F4 Sb F1 78.2(11) . . ? F5 Sb F1 95.3(13) . . ? F6 Sb F1 81.1(11) . . ? F2 Sb F1 171.4(19) . . ? F4 Sb F3 88.7(14) . . ? F5 Sb F3 97(2) . . ? F6 Sb F3 174.7(12) . . ? F2 Sb F3 81.6(16) . . ? F1 Sb F3 102.9(11) . . ? C1 N1 C5 119.9(9) . . ? C1 N1 Pt 127.0(7) . . ? C5 N1 Pt 113.0(7) . . ? C6 N2 C10 120.8(10) . . ? C6 N2 Pt 119.3(7) . . ? C10 N2 Pt 118.6(8) . . ? C15 N3 C11 120.7(10) . . ? C15 N3 Pt 126.6(8) . . ? C11 N3 Pt 112.7(8) . . ? C2 C1 N1 119.9(11) . . ? C1 C2 C3 122.1(14) . . ? C4 C3 C2 116.8(15) . . ? C5 C4 C3 120.0(12) . . ? C4 C5 N1 119.9(10) . . ? C4 C5 C6 125.1(11) . . ? N1 C5 C6 114.8(10) . . ? N2 C6 C7 120.3(10) . . ? N2 C6 C5 111.5(10) . . ? C7 C6 C5 128.3(10) . . ? C6 C7 C8 120.6(12) . . ? C7 C8 C9 118.4(12) . . ? C7 C8 C16 121.8(13) . . ? C9 C8 C16 119.7(12) . . ? C10 C9 C8 117.6(12) . . ? N2 C10 C9 117.3(13) . . ? N2 C10 C11 111.5(10) . . ? C9 C10 C11 124.0(13) . . ? C12 C11 N3 119.5(12) . . ? C12 C11 C10 125.3(11) . . ? N3 C11 C10 114.8(10) . . ? C11 C12 C13 120.2(15) . . ? C14 C13 C12 117.5(14) . . ? C13 C14 C15 120.7(14) . . ? N3 C15 C14 118.3(13) . . ? C21 C16 C17 119.7(17) . . ? C21 C16 C8 121.7(17) . . ? C17 C16 C8 118.5(16) . . ? C16 C21 C20 121(2) . . ? C16 C21 C22 122(2) . . ? C20 C21 C22 117(2) . . ? C19 C20 C21 115(3) . . ? C18 C19 C20 129(3) . . ? C19 C18 C17 116(2) . . ? C16 C17 C18 119(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 22.97 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.993 _refine_diff_density_min -0.608 _refine_diff_density_rms 0.137 data_gs11 _database_code_CSD 168559 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Pt{4'(C6H4-CH3-o)trpy}Cl]BF4' _chemical_formula_sum 'C22 H17 B Cl F4 N3 Pt' _chemical_formula_weight 640.73 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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P2(1)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.87(2) _cell_length_b 19.489(5) _cell_length_c 16.500(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.923(5) _cell_angle_gamma 90.00 _cell_volume 2161(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 2 _cell_measurement_theta_max 12 _exptl_crystal_description 'needle' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.95 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.969 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 6.664 _exptl_absorpt_correction_type 'Psi-scans' _exptl_absorpt_correction_T_min 0.64 _exptl_absorpt_correction_T_max 0.99 _exptl_absorpt_process_details ; Walker, N. & stuart, D. (1983) Acta. Cryst. A39, 158-166. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius CAD4' _diffrn_measurement_method 'omega-2theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '60 minutes' _diffrn_standards_decay_% 0 _diffrn_reflns_number 3589 _diffrn_reflns_av_R_equivalents 0.0219 _diffrn_reflns_av_sigmaI/netI 0.0391 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 22.97 _reflns_number_total 2996 _reflns_number_gt 2208 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius CAD4' _computing_cell_refinement 'CELDIM, CAD4' _computing_data_reduction 'XCAD (McArdle, 2000)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP 3 (Farrugia, 2000)' _computing_publication_material 'ORTEP 3 (Farrugia, 2000)' _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2996 _refine_ls_number_parameters 281 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0713 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1395 _refine_ls_wR_factor_gt 0.1233 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.986 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt 0.24327(5) 0.03483(3) 0.00650(2) 0.0609(2) Uani 1 1 d . . . Cl Cl 0.2947(5) 0.0695(3) 0.1421(2) 0.0945(12) Uani 1 1 d . . . N1 N 0.2724(11) -0.0677(6) 0.0249(6) 0.060(3) Uani 1 1 d . . . N2 N 0.2027(11) 0.0047(5) -0.1075(5) 0.057(2) Uani 1 1 d . . . N3 N 0.2035(12) 0.1280(5) -0.0486(6) 0.068(3) Uani 1 1 d . . . C1 C 0.3140(16) -0.1013(9) 0.0995(8) 0.077(4) Uani 1 1 d . . . H1 H 0.3332 -0.0771 0.1491 0.095(11) Uiso 1 1 calc R . . C2 C 0.3262(19) -0.1705(10) 0.0990(10) 0.094(5) Uani 1 1 d . . . H2 H 0.3503 -0.1940 0.1491 0.095(11) Uiso 1 1 calc R . . C3 C 0.305(2) -0.2063(8) 0.0284(10) 0.088(4) Uani 1 1 d . . . H3 H 0.3159 -0.2539 0.0305 0.095(11) Uiso 1 1 calc R . . C4 C 0.2663(17) -0.1735(7) -0.0476(8) 0.076(3) Uani 1 1 d . . . H4 H 0.2507 -0.1976 -0.0972 0.095(11) Uiso 1 1 calc R . . C5 C 0.2523(13) -0.1024(7) -0.0458(7) 0.057(3) Uani 1 1 d . . . C6 C 0.2087(14) -0.0618(6) -0.1234(7) 0.054(3) Uani 1 1 d . . . C7 C 0.1809(14) -0.0836(6) -0.2040(6) 0.059(3) Uani 1 1 d . . . H7 H 0.1774 -0.1303 -0.2160 0.095(11) Uiso 1 1 calc R . . C8 C 0.1578(14) -0.0357(5) -0.2677(6) 0.051(2) Uani 1 1 d . . . C9 C 0.1522(15) 0.0337(6) -0.2489(7) 0.063(3) Uani 1 1 d . . . H9 H 0.1335 0.0661 -0.2913 0.095(11) Uiso 1 1 calc R . . C10 C 0.1744(14) 0.0552(6) -0.1670(7) 0.054(3) Uani 1 1 d . . . C11 C 0.1705(15) 0.1231(6) -0.1341(7) 0.059(3) Uani 1 1 d . . . C12 C 0.1414(17) 0.1805(7) -0.1788(9) 0.082(4) Uani 1 1 d . . . H12 H 0.1253 0.1772 -0.2360 0.095(11) Uiso 1 1 calc R . . C13 C 0.134(2) 0.2458(8) -0.1439(11) 0.100(5) Uani 1 1 d . . . H13 H 0.1048 0.2851 -0.1761 0.095(11) Uiso 1 1 calc R . . C14 C 0.173(2) 0.2479(8) -0.0567(10) 0.095(5) Uani 1 1 d . . . H14 H 0.1756 0.2899 -0.0297 0.095(11) Uiso 1 1 calc R . . C15 C 0.2060(16) 0.1891(7) -0.0114(8) 0.073(4) Uani 1 1 d . . . H15 H 0.2309 0.1914 0.0461 0.095(11) Uiso 1 1 calc R . . C16 C 0.1395(19) -0.0554(5) -0.3572(7) 0.067(3) Uani 1 1 d D . . C17 C 0.2888(19) -0.0386(6) -0.3954(7) 0.079(4) Uani 1 1 d D . . H17 H 0.3991 -0.0144 -0.3674 0.095(11) Uiso 1 1 calc R . . C18 C 0.274(3) -0.0587(9) -0.4791(9) 0.109(6) Uani 1 1 d D . . H18 H 0.3779 -0.0488 -0.5054 0.095(11) Uiso 1 1 calc R . . C19 C 0.112(3) -0.0918(7) -0.5215(8) 0.095(5) Uani 1 1 d D . . H19 H 0.1026 -0.1037 -0.5768 0.095(11) Uiso 1 1 calc R . . C20 C -0.033(3) -0.1071(7) -0.4829(8) 0.098(5) Uani 1 1 d D . . H20 H -0.1440 -0.1299 -0.5123 0.095(11) Uiso 1 1 calc R . . C21 C -0.027(2) -0.0906(7) -0.3996(8) 0.084(4) Uani 1 1 d D . . C22 C -0.193(2) -0.1098(9) -0.3566(10) 0.125(6) Uani 1 1 d D . . H22A H -0.2953 -0.1338 -0.3947 0.095(11) Uiso 1 1 calc R . . H22B H -0.2484 -0.0689 -0.3377 0.095(11) Uiso 1 1 calc R . . H22C H -0.1422 -0.1388 -0.3101 0.095(11) Uiso 1 1 calc R . . B B 0.548(3) 0.1818(11) 0.6693(13) 0.105(6) Uiso 1 1 d . . . F1A F 0.534(4) 0.2009(14) 0.5921(16) 0.155(10) Uiso 0.50 1 d P . . F2A F 0.590(5) 0.2412(17) 0.7073(19) 0.204(12) Uiso 0.50 1 d P . . F3A F 0.665(3) 0.1303(11) 0.7060(13) 0.139(7) Uiso 0.50 1 d P . . F4A F 0.353(4) 0.1692(14) 0.6696(17) 0.187(10) Uiso 0.50 1 d P . . F1B F 0.510(4) 0.1267(12) 0.7054(15) 0.152(8) Uiso 0.50 1 d P . . F2B F 0.475(3) 0.1702(11) 0.5839(12) 0.110(6) Uiso 0.50 1 d P . . F3B F 0.727(3) 0.2069(12) 0.6677(14) 0.151(7) Uiso 0.50 1 d P . . F4B F 0.461(3) 0.2367(9) 0.7100(11) 0.105(5) Uiso 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 0.0335(3) 0.0952(4) 0.0554(3) -0.0059(2) 0.0121(2) -0.0070(2) Cl 0.0616(19) 0.157(4) 0.0665(19) -0.024(2) 0.0162(15) -0.007(2) N1 0.030(5) 0.098(7) 0.052(5) 0.018(5) 0.010(4) -0.002(4) N2 0.034(4) 0.082(7) 0.056(5) 0.009(5) 0.014(4) -0.002(5) N3 0.034(5) 0.089(8) 0.081(7) -0.023(6) 0.015(4) -0.011(5) C1 0.042(6) 0.116(13) 0.077(9) 0.016(9) 0.019(6) -0.002(8) C2 0.059(8) 0.136(15) 0.089(11) 0.035(11) 0.019(7) 0.004(9) C3 0.087(9) 0.077(10) 0.097(10) 0.044(9) 0.013(8) 0.018(8) C4 0.075(8) 0.088(10) 0.066(8) 0.014(7) 0.019(6) 0.013(7) C5 0.027(5) 0.079(9) 0.064(7) 0.033(7) 0.010(5) 0.002(5) C6 0.042(6) 0.054(7) 0.062(7) -0.004(6) 0.005(5) 0.005(5) C7 0.050(6) 0.064(7) 0.063(7) 0.001(6) 0.013(5) -0.007(5) C8 0.045(6) 0.054(6) 0.054(6) -0.001(5) 0.008(5) 0.007(5) C9 0.062(7) 0.066(8) 0.059(6) -0.003(6) 0.011(5) -0.001(6) C10 0.037(5) 0.055(7) 0.071(7) -0.010(6) 0.012(5) -0.007(5) C11 0.050(6) 0.062(8) 0.068(7) 0.002(6) 0.019(5) -0.003(5) C12 0.071(8) 0.083(10) 0.099(10) -0.019(8) 0.033(7) -0.004(7) C13 0.101(11) 0.081(10) 0.133(14) -0.016(9) 0.060(10) 0.000(8) C14 0.091(9) 0.075(10) 0.137(14) -0.044(10) 0.065(10) -0.028(8) C15 0.056(7) 0.066(9) 0.099(10) -0.029(8) 0.025(7) -0.018(6) C16 0.085(8) 0.057(7) 0.053(6) 0.007(5) 0.001(6) 0.019(6) C17 0.089(9) 0.087(9) 0.063(7) 0.006(7) 0.019(7) 0.000(7) C18 0.159(17) 0.115(13) 0.066(9) 0.007(9) 0.052(10) 0.013(11) C19 0.174(17) 0.060(9) 0.048(7) 0.010(7) 0.013(10) 0.032(10) C20 0.142(14) 0.084(11) 0.052(8) -0.017(7) -0.019(8) 0.031(9) C21 0.089(9) 0.070(9) 0.081(9) -0.014(7) -0.010(7) 0.010(7) C22 0.071(9) 0.157(17) 0.138(14) -0.052(12) -0.003(10) -0.014(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt N2 1.935(9) . ? Pt N3 2.025(11) . ? Pt N1 2.025(11) . ? Pt Cl 2.293(3) . ? N1 C5 1.331(16) . ? N1 C1 1.371(15) . ? N2 C6 1.324(14) . ? N2 C10 1.374(15) . ? N3 C15 1.337(15) . ? N3 C11 1.385(14) . ? C1 C2 1.352(19) . ? C2 C3 1.34(2) . ? C3 C4 1.384(19) . ? C4 C5 1.389(17) . ? C5 C6 1.482(15) . ? C6 C7 1.372(14) . ? C7 C8 1.391(14) . ? C8 C9 1.390(13) . ? C8 C16 1.505(14) . ? C9 C10 1.392(15) . ? C10 C11 1.434(15) . ? C11 C12 1.332(16) . ? C12 C13 1.402(17) . ? C13 C14 1.41(2) . ? C14 C15 1.361(19) . ? C16 C17 1.351(17) . ? C16 C21 1.391(17) . ? C17 C18 1.419(17) . ? C18 C19 1.35(2) . ? C19 C20 1.32(2) . ? C20 C21 1.403(17) . ? C21 C22 1.512(19) . ? B F1B 1.28(3) . ? B F1A 1.31(3) . ? B F2A 1.32(3) . ? B F3B 1.33(3) . ? B F3A 1.35(3) . ? B F4A 1.36(3) . ? B F2B 1.41(3) . ? B F4B 1.45(3) . ? F1A F2B 0.72(3) . ? F1A F3B 1.63(3) . ? F2A F4B 0.90(3) . ? F2A F3B 1.42(4) . ? F3A F1B 1.07(3) . ? F3A F3B 1.71(3) . ? F4A F1B 1.39(3) . ? F4A F4B 1.59(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pt N3 81.7(4) . . ? N2 Pt N1 80.6(4) . . ? N3 Pt N1 162.3(4) . . ? N2 Pt Cl 179.2(3) . . ? N3 Pt Cl 98.8(3) . . ? N1 Pt Cl 98.8(3) . . ? C5 N1 C1 120.6(12) . . ? C5 N1 Pt 112.4(7) . . ? C1 N1 Pt 126.9(10) . . ? C6 N2 C10 124.3(9) . . ? C6 N2 Pt 119.0(7) . . ? C10 N2 Pt 116.6(8) . . ? C15 N3 C11 120.9(12) . . ? C15 N3 Pt 127.2(9) . . ? C11 N3 Pt 111.9(8) . . ? C2 C1 N1 118.1(14) . . ? C3 C2 C1 122.0(14) . . ? C2 C3 C4 120.9(14) . . ? C3 C4 C5 116.3(13) . . ? N1 C5 C4 122.0(10) . . ? N1 C5 C6 116.8(11) . . ? C4 C5 C6 121.1(12) . . ? N2 C6 C7 119.5(10) . . ? N2 C6 C5 111.2(10) . . ? C7 C6 C5 129.4(11) . . ? C6 C7 C8 119.7(11) . . ? C9 C8 C7 119.3(10) . . ? C9 C8 C16 117.9(9) . . ? C7 C8 C16 122.9(9) . . ? C8 C9 C10 120.4(10) . . ? N2 C10 C9 116.7(10) . . ? N2 C10 C11 113.6(10) . . ? C9 C10 C11 129.6(11) . . ? C12 C11 N3 118.6(11) . . ? C12 C11 C10 125.4(11) . . ? N3 C11 C10 116.0(10) . . ? C11 C12 C13 123.3(14) . . ? C12 C13 C14 115.4(15) . . ? C15 C14 C13 120.8(13) . . ? N3 C15 C14 120.8(13) . . ? C17 C16 C21 120.6(12) . . ? C17 C16 C8 118.6(11) . . ? C21 C16 C8 120.9(11) . . ? C16 C17 C18 118.6(14) . . ? C19 C18 C17 121.5(15) . . ? C20 C19 C18 118.6(14) . . ? C19 C20 C21 123.3(15) . . ? C16 C21 C20 117.4(14) . . ? C16 C21 C22 120.5(12) . . ? C20 C21 C22 122.1(14) . . ? F1B B F1A 135(3) . . ? F1B B F2A 124(3) . . ? F1A B F2A 100(2) . . ? F1B B F3B 127(2) . . ? F1A B F3B 76.0(19) . . ? F2A B F3B 64.6(19) . . ? F1B B F3A 47.9(15) . . ? F1A B F3A 124(2) . . ? F2A B F3A 113(2) . . ? F3B B F3A 79.2(17) . . ? F1B B F4A 63.4(17) . . ? F1A B F4A 100(2) . . ? F2A B F4A 106(2) . . ? F3B B F4A 169(3) . . ? F3A B F4A 111(2) . . ? F1B B F2B 105(2) . . ? F1A B F2B 30.2(14) . . ? F2A B F2B 128(2) . . ? F3B B F2B 100(2) . . ? F3A B F2B 113(2) . . ? F4A B F2B 80.3(18) . . ? F1B B F4B 105(2) . . ? F1A B F4B 107(2) . . ? F2A B F4B 37.6(15) . . ? F3B B F4B 102(2) . . ? F3A B F4B 127(2) . . ? F4A B F4B 68.6(16) . . ? F2B B F4B 119.0(18) . . ? F2B F1A B 83(3) . . ? F2B F1A F3B 123(4) . . ? B F1A F3B 52.5(15) . . ? F4B F2A B 79(3) . . ? F4B F2A F3B 137(4) . . ? B F2A F3B 58.1(19) . . ? F1B F3A B 62.7(18) . . ? F1B F3A F3B 112(2) . . ? B F3A F3B 50.0(13) . . ? B F4A F1B 55.5(17) . . ? B F4A F4B 58.5(15) . . ? F1B F4A F4B 94(2) . . ? F3A F1B B 69(2) . . ? F3A F1B F4A 131(3) . . ? B F1B F4A 61.1(18) . . ? F1A F2B B 67(3) . . ? B F3B F2A 57.3(17) . . ? B F3B F1A 51.4(14) . . ? F2A F3B F1A 82.7(19) . . ? B F3B F3A 50.9(14) . . ? F2A F3B F3A 90(2) . . ? F1A F3B F3A 89.6(17) . . ? F2A F4B B 63(2) . . ? F2A F4B F4A 116(3) . . ? B F4B F4A 52.9(14) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 22.97 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.882 _refine_diff_density_min -1.133 _refine_diff_density_rms 0.148