Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'John S. Field' 'Jan-Andre Gertenbach' 'Raymond J. Haines' 'Lesibana P. Ledwaba' 'Ndoda T. Mashapa' 'David R. McMillin' 'Orde Q. Munro' 'Grant C. Summerton' _publ_contact_author_name 'Prof John S Field' _publ_contact_author_address ; School of Chemical and Physical Sciences University of Natal Private Bag X01 Pietermaritzburg 3201 SOUTH AFRICA ; _publ_contact_author_email 'FIELDJ@NU.AC.ZA' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Temperature dependence of the srystal structures and luminescence properties of [Pt{4'(o-Cl-ph)trpy}Cl]SbF6 (trpy = 2,2':6',2"-terpyridine) ; data_temdep180Kstructure _database_code_CSD 194846 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Pt{4'(o-Cl-Ph)trpy}Cl]SbF6 _chemical_formula_sum 'C21 H14 Cl2 F6 N3 Pt Sb' _chemical_formula_weight 810.09 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' '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' 'F' 'F' 0.0171 0.0103 '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 _symmetry_Int_Tables_number 14 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 6.787(2) _cell_length_b 18.804(12) _cell_length_c 18.221(8) _cell_angle_alpha 90.00 _cell_angle_beta 91.38(4) _cell_angle_gamma 90.00 _cell_volume 2324.7(19) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 3 _cell_measurement_theta_max 12 _exptl_crystal_description parallelpiped _exptl_crystal_colour orange _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.315 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 7.466 _exptl_absorpt_correction_type 'semi-empirical (psi scans)' _exptl_absorpt_correction_T_min 0.1049 _exptl_absorpt_correction_T_max 0.1797 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.70930 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'scintillation counter' _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 5568 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_av_sigmaI/netI 0.0241 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.25 _reflns_number_total 4066 _reflns_number_gt 3583 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nomius CAD4' _computing_cell_refinement 'CELDIM, CAD4' _computing_data_reduction 'XCAD4 (McArdle, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP 3 (Farrugia, 2000)' _computing_publication_material SHELXS-97 _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 4066 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0633 _refine_ls_R_factor_gt 0.0574 _refine_ls_wR_factor_ref 0.1885 _refine_ls_wR_factor_gt 0.1831 _refine_ls_goodness_of_fit_ref 1.642 _refine_ls_restrained_S_all 1.642 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt 0.75853(5) 0.01213(3) 0.99415(2) 0.0318(2) Uani 1 1 d . . . Cl1 Cl 0.7377(4) -0.00833(15) 1.11846(15) 0.0370(6) Uani 1 1 d . . . Cl2 Cl 0.5157(10) 0.0106(10) 0.6282(4) 0.405(14) Uani 1 1 d . . . N1 N 0.6964(12) -0.0855(6) 0.9582(4) 0.041(2) Uani 1 1 d . . . N2 N 0.7766(14) 0.0300(6) 0.8894(5) 0.041(2) Uani 1 1 d . . . N3 N 0.8243(13) 0.1168(5) 0.9965(4) 0.034(2) Uani 1 1 d . . . C1 C 0.6565(15) -0.1451(6) 0.9990(6) 0.039(2) Uani 1 1 d . . . H1 H 0.6594 -0.1417 1.0500 0.053(10) Uiso 1 1 calc R . . C2 C 0.6136(16) -0.2083(7) 0.9677(7) 0.045(3) Uani 1 1 d . . . H2 H 0.5847 -0.2472 0.9971 0.053(10) Uiso 1 1 calc R . . C3 C 0.6120(16) -0.2158(7) 0.8913(7) 0.048(3) Uani 1 1 d . . . H3 H 0.5857 -0.2595 0.8693 0.053(10) Uiso 1 1 calc R . . C4 C 0.6517(15) -0.1549(8) 0.8489(6) 0.052(3) Uani 1 1 d . . . H4 H 0.6447 -0.1577 0.7980 0.053(10) Uiso 1 1 calc R . . C5 C 0.6993(15) -0.0929(8) 0.8814(6) 0.046(3) Uani 1 1 d . . . C6 C 0.7461(15) -0.0266(6) 0.8447(6) 0.038(3) Uani 1 1 d . . . C7 C 0.7767(17) -0.0149(7) 0.7695(6) 0.044(3) Uani 1 1 d . . . H7 H 0.7635 -0.0527 0.7369 0.053(10) Uiso 1 1 calc R . . C8 C 0.8261(19) 0.0517(8) 0.7432(6) 0.056(4) Uani 1 1 d . . . C9 C 0.8422(19) 0.1049(7) 0.7925(6) 0.052(3) Uani 1 1 d . . . H9 H 0.8692 0.1506 0.7760 0.053(10) Uiso 1 1 calc R . . C10 C 0.8201(16) 0.0937(6) 0.8670(6) 0.039(3) Uani 1 1 d . . . C11 C 0.8497(15) 0.1462(7) 0.9275(6) 0.040(3) Uani 1 1 d . . . C12 C 0.8948(15) 0.2157(6) 0.9187(6) 0.038(2) Uani 1 1 d . . . H12 H 0.9101 0.2345 0.8720 0.053(10) Uiso 1 1 calc R . . C13 C 0.9182(17) 0.2589(7) 0.9803(6) 0.045(3) Uani 1 1 d . . . H13 H 0.9482 0.3068 0.9747 0.053(10) Uiso 1 1 calc R . . C14 C 0.8970(16) 0.2308(7) 1.0502(6) 0.045(3) Uani 1 1 d . . . H14 H 0.9123 0.2588 1.0920 0.053(10) Uiso 1 1 calc R . . C15 C 0.8506(14) 0.1570(7) 1.0547(5) 0.039(3) Uani 1 1 d . . . H15 H 0.8385 0.1366 1.1008 0.053(10) Uiso 1 1 calc R . . C16 C 0.870(3) 0.0627(9) 0.6634(6) 0.071(5) Uani 1 1 d . . . C17 C 1.040(4) 0.0924(7) 0.6426(7) 0.093(7) Uani 1 1 d . . . H17 H 1.1349 0.1043 0.6783 0.053(10) Uiso 1 1 calc R . . C18 C 1.078(5) 0.1056(9) 0.5700(11) 0.157(14) Uani 1 1 d . . . H18 H 1.1964 0.1265 0.5575 0.053(10) Uiso 1 1 calc R . . C19 C 0.946(6) 0.0890(9) 0.5177(10) 0.144(15) Uani 1 1 d . . . H19 H 0.9735 0.0967 0.4686 0.053(10) Uiso 1 1 calc R . . C20 C 0.783(5) 0.062(2) 0.5361(11) 0.167(18) Uani 1 1 d . . . H20 H 0.6904 0.0527 0.4990 0.053(10) Uiso 1 1 calc R . . C21 C 0.733(3) 0.0470(16) 0.6078(8) 0.122(10) Uani 1 1 d . . . Sb Sb 0.39131(11) 0.28613(5) 0.79377(4) 0.0448(3) Uani 1 1 d . . . F1 F 0.6217(13) 0.3275(6) 0.8287(5) 0.091(3) Uani 1 1 d . . . F2 F 0.3622(17) 0.3627(5) 0.7309(5) 0.094(3) Uani 1 1 d . . . F3 F 0.4310(15) 0.2096(4) 0.8552(5) 0.082(3) Uani 1 1 d . . . F4 F 0.2503(16) 0.3305(5) 0.8677(5) 0.090(3) Uani 1 1 d . . . F5 F 0.5381(14) 0.2359(6) 0.7210(6) 0.086(3) Uani 1 1 d . . . F6 F 0.1626(14) 0.2438(7) 0.7574(5) 0.096(3) 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 0.0229(3) 0.0552(4) 0.0169(3) -0.00686(15) -0.00385(18) 0.01242(15) Cl1 0.0321(15) 0.0597(16) 0.0191(13) -0.0015(10) -0.0029(11) 0.0106(11) Cl2 0.050(3) 1.12(4) 0.046(3) -0.095(8) -0.025(3) 0.038(8) N1 0.019(4) 0.085(7) 0.020(4) -0.012(4) -0.005(3) 0.022(4) N2 0.030(5) 0.085(7) 0.009(4) -0.008(4) 0.002(3) 0.019(5) N3 0.031(5) 0.054(6) 0.018(4) 0.001(4) -0.001(3) 0.013(4) C1 0.032(6) 0.055(7) 0.029(5) 0.000(5) 0.000(4) 0.009(5) C2 0.028(6) 0.064(8) 0.043(6) -0.009(6) 0.004(5) 0.013(5) C3 0.033(6) 0.065(8) 0.045(7) -0.022(6) 0.009(5) -0.005(5) C4 0.026(5) 0.098(10) 0.032(6) -0.026(7) -0.003(5) 0.011(6) C5 0.020(5) 0.092(9) 0.027(5) -0.017(6) -0.003(4) 0.004(5) C6 0.022(5) 0.062(7) 0.028(6) -0.014(5) -0.009(4) 0.010(5) C7 0.028(6) 0.088(9) 0.017(6) -0.012(5) -0.004(4) 0.018(6) C8 0.053(7) 0.099(11) 0.014(5) 0.004(6) -0.006(5) 0.047(7) C9 0.065(8) 0.066(8) 0.024(6) -0.001(5) -0.014(5) 0.031(7) C10 0.036(6) 0.055(7) 0.026(5) 0.001(5) -0.007(4) 0.020(5) C11 0.028(5) 0.067(8) 0.025(5) 0.000(5) -0.005(4) 0.020(5) C12 0.037(6) 0.053(7) 0.023(5) 0.005(4) 0.007(4) 0.012(5) C13 0.040(6) 0.057(7) 0.038(6) -0.007(5) -0.003(5) 0.010(5) C14 0.034(6) 0.071(8) 0.030(6) -0.019(5) -0.008(5) 0.015(5) C15 0.030(5) 0.070(8) 0.016(5) -0.018(5) 0.000(4) 0.017(5) C16 0.117(13) 0.085(10) 0.009(5) 0.007(6) -0.004(7) 0.074(10) C17 0.21(2) 0.049(8) 0.023(7) -0.009(6) 0.028(10) -0.010(11) C18 0.36(4) 0.055(10) 0.064(13) -0.009(9) 0.080(19) -0.064(18) C19 0.37(5) 0.041(8) 0.019(7) 0.003(6) 0.021(16) 0.070(17) C20 0.22(3) 0.25(4) 0.029(11) -0.035(15) -0.035(14) 0.19(3) C21 0.097(14) 0.24(3) 0.024(8) -0.019(12) -0.013(8) 0.093(17) Sb 0.0440(5) 0.0669(6) 0.0231(4) 0.0090(3) -0.0063(3) 0.0000(4) F1 0.075(6) 0.123(8) 0.072(6) 0.019(6) -0.032(5) -0.040(6) F2 0.127(8) 0.105(7) 0.048(5) 0.038(5) -0.014(5) 0.022(6) F3 0.109(7) 0.065(5) 0.071(6) 0.034(4) -0.011(5) -0.005(5) F4 0.124(8) 0.097(7) 0.050(5) -0.015(5) 0.031(5) 0.011(6) F5 0.086(6) 0.097(7) 0.078(6) -0.007(6) 0.031(5) -0.012(6) F6 0.063(5) 0.163(10) 0.060(6) 0.005(6) -0.022(4) -0.029(6) _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 1.945(9) . ? Pt N1 1.991(11) . ? Pt N3 2.018(10) . ? Pt Cl1 2.305(3) . ? Cl2 C21 1.67(3) . ? N1 C1 1.377(15) . ? N1 C5 1.406(13) . ? N2 C10 1.302(16) . ? N2 C6 1.352(15) . ? N3 C15 1.311(13) . ? N3 C11 1.389(14) . ? C1 C2 1.347(17) . ? C2 C3 1.398(17) . ? C3 C4 1.412(19) . ? C4 C5 1.343(19) . ? C5 C6 1.455(18) . ? C6 C7 1.407(17) . ? C7 C8 1.38(2) . ? C8 C9 1.348(18) . ? C8 C16 1.505(16) . ? C9 C10 1.385(15) . ? C10 C11 1.490(15) . ? C11 C12 1.352(16) . ? C12 C13 1.391(16) . ? C13 C14 1.389(17) . ? C14 C15 1.425(17) . ? C16 C17 1.35(3) . ? C16 C21 1.39(2) . ? C17 C18 1.38(2) . ? C18 C19 1.33(4) . ? C19 C20 1.27(5) . ? C20 C21 1.39(3) . ? Sb F3 1.839(7) . ? Sb F1 1.846(8) . ? Sb F2 1.847(8) . ? Sb F6 1.853(9) . ? Sb F4 1.868(8) . ? Sb F5 1.925(10) . ? 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 81.6(4) . . ? N2 Pt N3 80.4(4) . . ? N1 Pt N3 162.0(3) . . ? N2 Pt Cl1 179.7(4) . . ? N1 Pt Cl1 98.8(3) . . ? N3 Pt Cl1 99.2(2) . . ? C1 N1 C5 117.7(11) . . ? C1 N1 Pt 128.0(7) . . ? C5 N1 Pt 114.3(9) . . ? C10 N2 C6 124.5(10) . . ? C10 N2 Pt 119.1(8) . . ? C6 N2 Pt 116.3(9) . . ? C15 N3 C11 119.0(11) . . ? C15 N3 Pt 127.3(8) . . ? C11 N3 Pt 113.7(7) . . ? C2 C1 N1 122.2(10) . . ? C1 C2 C3 120.5(12) . . ? C2 C3 C4 117.8(11) . . ? C5 C4 C3 120.7(11) . . ? C4 C5 N1 121.1(13) . . ? C4 C5 C6 126.4(11) . . ? N1 C5 C6 112.4(11) . . ? N2 C6 C7 116.1(12) . . ? N2 C6 C5 115.4(10) . . ? C7 C6 C5 128.4(11) . . ? C8 C7 C6 121.4(11) . . ? C9 C8 C7 117.1(11) . . ? C9 C8 C16 121.8(15) . . ? C7 C8 C16 120.9(13) . . ? C8 C9 C10 122.2(13) . . ? N2 C10 C9 118.5(11) . . ? N2 C10 C11 113.9(10) . . ? C9 C10 C11 127.5(12) . . ? C12 C11 N3 121.7(10) . . ? C12 C11 C10 125.4(10) . . ? N3 C11 C10 112.9(10) . . ? C11 C12 C13 119.4(11) . . ? C12 C13 C14 120.3(12) . . ? C13 C14 C15 116.8(10) . . ? N3 C15 C14 122.7(11) . . ? C17 C16 C21 116.6(15) . . ? C17 C16 C8 121.2(14) . . ? C21 C16 C8 122.1(18) . . ? C16 C17 C18 122(2) . . ? C19 C18 C17 121(3) . . ? C20 C19 C18 119(2) . . ? C19 C20 C21 125(3) . . ? C20 C21 C16 118(3) . . ? C20 C21 Cl2 122(2) . . ? C16 C21 Cl2 120.1(14) . . ? F3 Sb F1 90.6(4) . . ? F3 Sb F2 177.6(5) . . ? F1 Sb F2 87.8(5) . . ? F3 Sb F6 89.4(5) . . ? F1 Sb F6 179.0(5) . . ? F2 Sb F6 92.1(5) . . ? F3 Sb F4 88.9(5) . . ? F1 Sb F4 90.4(5) . . ? F2 Sb F4 92.9(5) . . ? F6 Sb F4 90.6(5) . . ? F3 Sb F5 87.9(5) . . ? F1 Sb F5 89.8(5) . . ? F2 Sb F5 90.3(5) . . ? F6 Sb F5 89.2(5) . . ? F4 Sb F5 176.8(4) . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 4.621 _refine_diff_density_min -4.675 _refine_diff_density_rms 0.273 data_temdep240Kstructure _database_code_CSD 194847 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Pt{4'(o-Cl-Ph)trpy}Cl]SbF6' _chemical_formula_sum 'C21 H14 Cl2 F6 N3 Pt Sb' _chemical_formula_weight 810.09 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' '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' 'F' 'F' 0.0171 0.0103 '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 _symmetry_Int_Tables_number 14 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 6.8182(10) _cell_length_b 18.863(5) _cell_length_c 18.276(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.004(15) _cell_angle_gamma 90.00 _cell_volume 2350.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 240(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 3 _cell_measurement_theta_max 12 _exptl_crystal_description parallelpiped _exptl_crystal_colour orange _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.289 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 7.385 _exptl_absorpt_correction_type 'semi-empirical (psi scans)' _exptl_absorpt_correction_T_min 0.1063 _exptl_absorpt_correction_T_max 0.1820 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 240(2) _diffrn_radiation_wavelength 0.70930 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'scintillation counter' _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 8909 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 24.91 _reflns_number_total 4116 _reflns_number_gt 3474 _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-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP 3 (Farrugia, 2000)' _computing_publication_material SHELXS-97 _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 4116 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0513 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.1394 _refine_ls_wR_factor_gt 0.1287 _refine_ls_goodness_of_fit_ref 1.167 _refine_ls_restrained_S_all 1.167 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.001 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 0.75699(4) 0.010806(19) 0.994746(15) 0.03911(17) Uani 1 1 d . . . Cl1 Cl 0.7373(3) -0.00962(12) 1.11870(12) 0.0497(5) Uani 1 1 d . . . Cl2 Cl 0.5109(9) 0.0093(7) 0.6305(3) 0.376(10) Uani 1 1 d . . . N1 N 0.6988(8) -0.0867(4) 0.9582(3) 0.0438(16) Uani 1 1 d . . . N2 N 0.7728(10) 0.0282(4) 0.8903(4) 0.0482(18) Uani 1 1 d . . . N3 N 0.8196(9) 0.1150(4) 0.9973(3) 0.0416(14) Uani 1 1 d . . . C1 C 0.6598(11) -0.1458(5) 0.9994(5) 0.0488(19) Uani 1 1 d . . . H1 H 0.6607 -0.1422 1.0507 0.074(8) Uiso 1 1 calc R . . C2 C 0.6201(14) -0.2089(6) 0.9679(6) 0.064(3) Uani 1 1 d . . . H2 H 0.5937 -0.2485 0.9976 0.074(8) Uiso 1 1 calc R . . C3 C 0.6179(14) -0.2162(5) 0.8918(5) 0.059(2) Uani 1 1 d . . . H3 H 0.5922 -0.2602 0.8697 0.074(8) Uiso 1 1 calc R . . C4 C 0.6552(11) -0.1555(6) 0.8494(5) 0.057(2) Uani 1 1 d . . . H4 H 0.6498 -0.1580 0.7981 0.074(8) Uiso 1 1 calc R . . C5 C 0.6995(10) -0.0927(5) 0.8832(4) 0.049(2) Uani 1 1 d . . . C6 C 0.7470(11) -0.0267(5) 0.8450(4) 0.0460(19) Uani 1 1 d . . . C7 C 0.7747(13) -0.0156(5) 0.7713(5) 0.053(2) Uani 1 1 d . . . H7 H 0.7611 -0.0537 0.7386 0.074(8) Uiso 1 1 calc R . . C8 C 0.8219(13) 0.0505(6) 0.7449(4) 0.060(3) Uani 1 1 d . . . C9 C 0.8394(13) 0.1050(5) 0.7940(4) 0.056(2) Uani 1 1 d . . . H9 H 0.8668 0.1510 0.7771 0.074(8) Uiso 1 1 calc R . . C10 C 0.8172(11) 0.0929(5) 0.8682(4) 0.0458(18) Uani 1 1 d . . . C11 C 0.8436(11) 0.1449(5) 0.9287(4) 0.0464(19) Uani 1 1 d . . . C12 C 0.8878(13) 0.2149(5) 0.9199(5) 0.055(2) Uani 1 1 d . . . H12 H 0.9019 0.2342 0.8728 0.074(8) Uiso 1 1 calc R . . C13 C 0.9116(13) 0.2572(5) 0.9813(5) 0.059(2) Uani 1 1 d . . . H13 H 0.9419 0.3056 0.9764 0.074(8) Uiso 1 1 calc R . . C14 C 0.8900(13) 0.2270(6) 1.0502(5) 0.061(2) Uani 1 1 d . . . H14 H 0.9059 0.2545 1.0927 0.074(8) Uiso 1 1 calc R . . C15 C 0.8450(11) 0.1561(5) 1.0550(4) 0.050(2) Uani 1 1 d . . . H15 H 0.8316 0.1359 1.1017 0.074(8) Uiso 1 1 calc R . . C16 C 0.864(2) 0.0629(6) 0.6656(4) 0.078(4) Uani 1 1 d . . . C17 C 1.035(2) 0.0906(5) 0.6453(6) 0.097(5) Uani 1 1 d . . . H17 H 1.1286 0.1009 0.6814 0.074(8) Uiso 1 1 calc R . . C18 C 1.080(4) 0.1051(7) 0.5719(9) 0.153(9) Uani 1 1 d . . . H18 H 1.2010 0.1258 0.5591 0.074(8) Uiso 1 1 calc R . . C19 C 0.943(4) 0.0880(7) 0.5191(8) 0.150(11) Uani 1 1 d . . . H19 H 0.9704 0.0959 0.4694 0.074(8) Uiso 1 1 calc R . . C20 C 0.778(4) 0.0612(14) 0.5387(8) 0.175(13) Uani 1 1 d . . . H20 H 0.6846 0.0525 0.5019 0.074(8) Uiso 1 1 calc R . . C21 C 0.726(3) 0.0439(12) 0.6107(7) 0.133(7) Uani 1 1 d . . . Sb Sb 0.38188(10) 0.28703(4) 0.79478(3) 0.0625(2) Uani 1 1 d . . . F1 F 0.6093(14) 0.3290(6) 0.8311(6) 0.158(4) Uani 1 1 d . . . F2 F 0.3586(16) 0.3631(5) 0.7320(5) 0.139(3) Uani 1 1 d . . . F3 F 0.4184(16) 0.2108(4) 0.8543(5) 0.137(3) Uani 1 1 d . . . F4 F 0.2418(16) 0.3314(5) 0.8674(5) 0.142(3) Uani 1 1 d . . . F5 F 0.5323(14) 0.2385(5) 0.7238(6) 0.136(3) Uani 1 1 d . . . F6 F 0.1562(13) 0.2456(6) 0.7584(5) 0.139(3) 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 0.0274(2) 0.0649(3) 0.0251(2) -0.00473(11) -0.00195(14) 0.01203(11) Cl1 0.0392(12) 0.0828(15) 0.0269(10) 0.0002(8) -0.0018(8) 0.0098(9) Cl2 0.081(4) 0.98(3) 0.065(3) -0.064(6) -0.036(3) 0.019(7) N1 0.023(3) 0.074(4) 0.034(3) -0.012(3) -0.007(2) 0.011(3) N2 0.033(4) 0.087(5) 0.025(3) -0.005(3) -0.001(3) 0.017(3) N3 0.033(3) 0.061(4) 0.031(3) -0.005(3) -0.002(2) 0.016(3) C1 0.035(4) 0.067(5) 0.045(5) -0.001(4) 0.004(3) 0.004(4) C2 0.046(5) 0.082(7) 0.063(6) 0.002(5) 0.002(5) 0.009(4) C3 0.059(5) 0.063(5) 0.054(5) -0.016(4) 0.005(4) -0.002(4) C4 0.035(4) 0.094(7) 0.042(5) -0.025(5) -0.002(3) 0.004(4) C5 0.024(3) 0.085(6) 0.039(4) -0.010(4) 0.000(3) 0.003(4) C6 0.030(4) 0.075(5) 0.032(4) -0.005(4) -0.004(3) 0.013(4) C7 0.043(5) 0.087(6) 0.031(4) -0.006(4) -0.009(4) 0.016(4) C8 0.059(5) 0.096(7) 0.024(4) 0.010(4) -0.002(4) 0.043(5) C9 0.062(5) 0.069(6) 0.036(4) 0.003(4) -0.007(4) 0.021(4) C10 0.044(4) 0.065(5) 0.029(4) 0.002(3) -0.001(3) 0.020(4) C11 0.037(4) 0.071(5) 0.032(4) 0.000(4) 0.000(3) 0.012(4) C12 0.051(5) 0.075(6) 0.039(5) 0.001(4) 0.000(4) 0.009(4) C13 0.051(5) 0.069(6) 0.058(6) -0.006(4) 0.000(4) 0.014(4) C14 0.047(5) 0.084(7) 0.050(5) -0.022(5) -0.010(4) 0.013(4) C15 0.036(4) 0.078(6) 0.036(4) -0.023(4) -0.003(3) 0.016(4) C16 0.126(10) 0.089(7) 0.020(4) 0.009(4) 0.000(5) 0.062(7) C17 0.187(15) 0.057(6) 0.046(6) 0.000(5) 0.043(8) 0.010(8) C18 0.30(3) 0.074(9) 0.089(11) -0.007(8) 0.086(14) -0.044(13) C19 0.35(3) 0.058(7) 0.037(7) -0.003(6) 0.033(12) 0.059(13) C20 0.24(3) 0.25(3) 0.030(7) -0.010(11) -0.018(11) 0.16(2) C21 0.121(13) 0.23(2) 0.045(7) -0.011(10) -0.010(7) 0.071(13) Sb 0.0601(4) 0.0905(5) 0.0368(4) 0.0198(3) -0.0062(3) -0.0073(3) F1 0.131(7) 0.203(10) 0.139(8) 0.065(7) -0.073(6) -0.091(7) F2 0.189(9) 0.133(7) 0.095(6) 0.064(5) -0.040(6) -0.018(6) F3 0.186(9) 0.116(6) 0.109(6) 0.068(5) -0.007(6) 0.005(6) F4 0.186(9) 0.143(8) 0.097(6) -0.029(6) 0.046(6) 0.006(7) F5 0.134(7) 0.134(7) 0.140(7) 0.006(6) 0.064(6) -0.002(6) F6 0.100(6) 0.218(10) 0.099(6) 0.008(7) -0.033(5) -0.046(6) _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 1.941(7) . ? Pt N1 1.996(7) . ? Pt N3 2.012(7) . ? Pt Cl1 2.302(2) . ? Cl2 C21 1.65(2) . ? N1 C1 1.371(11) . ? N1 C5 1.376(10) . ? N2 C10 1.321(11) . ? N2 C6 1.336(12) . ? N3 C15 1.321(10) . ? N3 C11 1.383(10) . ? C1 C2 1.349(13) . ? C2 C3 1.399(14) . ? C3 C4 1.406(14) . ? C4 C5 1.370(13) . ? C5 C6 1.463(13) . ? C6 C7 1.376(12) . ? C7 C8 1.375(14) . ? C8 C9 1.369(13) . ? C8 C16 1.496(12) . ? C9 C10 1.383(11) . ? C10 C11 1.490(11) . ? C11 C12 1.364(12) . ? C12 C13 1.386(13) . ? C13 C14 1.389(13) . ? C14 C15 1.375(14) . ? C16 C17 1.329(18) . ? C16 C21 1.421(19) . ? C17 C18 1.403(17) . ? C18 C19 1.38(3) . ? C19 C20 1.29(3) . ? C20 C21 1.40(2) . ? Sb F3 1.819(7) . ? Sb F6 1.849(8) . ? Sb F2 1.845(7) . ? Sb F4 1.837(8) . ? Sb F1 1.864(7) . ? Sb F5 1.891(10) . ? 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 80.6(3) . . ? N2 Pt N3 81.1(3) . . ? N1 Pt N3 161.8(2) . . ? N2 Pt Cl1 179.8(2) . . ? N1 Pt Cl1 99.41(19) . . ? N3 Pt Cl1 98.82(18) . . ? C1 N1 C5 118.7(7) . . ? C1 N1 Pt 127.2(5) . . ? C5 N1 Pt 114.1(6) . . ? C10 N2 C6 123.9(7) . . ? C10 N2 Pt 118.0(6) . . ? C6 N2 Pt 118.1(7) . . ? C15 N3 C11 117.9(8) . . ? C15 N3 Pt 128.3(6) . . ? C11 N3 Pt 113.7(5) . . ? C2 C1 N1 121.5(8) . . ? C1 C2 C3 120.9(10) . . ? C4 C3 C2 117.8(9) . . ? C5 C4 C3 119.7(8) . . ? C4 C5 N1 121.3(9) . . ? C4 C5 C6 124.7(8) . . ? N1 C5 C6 114.0(8) . . ? N2 C6 C7 118.0(9) . . ? N2 C6 C5 113.1(7) . . ? C7 C6 C5 128.8(8) . . ? C6 C7 C8 120.9(9) . . ? C7 C8 C9 118.1(8) . . ? C7 C8 C16 121.8(9) . . ? C9 C8 C16 120.1(10) . . ? C10 C9 C8 120.6(9) . . ? N2 C10 C9 118.5(8) . . ? N2 C10 C11 114.2(7) . . ? C9 C10 C11 127.3(9) . . ? C12 C11 N3 121.8(8) . . ? C12 C11 C10 125.2(8) . . ? N3 C11 C10 113.0(8) . . ? C11 C12 C13 119.2(9) . . ? C12 C13 C14 119.0(9) . . ? C15 C14 C13 118.7(8) . . ? N3 C15 C14 123.3(9) . . ? C17 C16 C21 118.8(11) . . ? C17 C16 C8 120.0(11) . . ? C21 C16 C8 121.1(13) . . ? C16 C17 C18 122.5(16) . . ? C17 C18 C19 118.1(18) . . ? C20 C19 C18 119.4(15) . . ? C19 C20 C21 125(2) . . ? C20 C21 C16 116(2) . . ? C20 C21 Cl2 121.6(16) . . ? C16 C21 Cl2 122.4(11) . . ? F3 Sb F6 89.7(5) . . ? F3 Sb F2 176.7(5) . . ? F6 Sb F2 91.9(5) . . ? F3 Sb F4 90.0(5) . . ? F6 Sb F4 91.1(5) . . ? F2 Sb F4 92.9(5) . . ? F3 Sb F1 90.5(4) . . ? F6 Sb F1 179.8(5) . . ? F2 Sb F1 87.9(4) . . ? F4 Sb F1 88.9(5) . . ? F3 Sb F5 87.3(5) . . ? F6 Sb F5 90.0(5) . . ? F2 Sb F5 89.8(5) . . ? F4 Sb F5 177.0(5) . . ? F1 Sb F5 90.0(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.91 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.602 _refine_diff_density_min -2.176 _refine_diff_density_rms 0.184 data_temdep260Kstructure _database_code_CSD 194848 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Pt{4'(o-Cl-Ph)trpy)Cl]SbF6 _chemical_formula_sum 'C21 H14 Cl2 F6 N3 Pt Sb' _chemical_formula_weight 810.09 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' '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' 'F' 'F' 0.0171 0.0103 '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 _symmetry_Int_Tables_number 14 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 6.8209(10) _cell_length_b 18.889(4) _cell_length_c 18.302(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.050(10) _cell_angle_gamma 90.00 _cell_volume 2358.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 260(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 3 _cell_measurement_theta_max 12 _exptl_crystal_description parallelpiped _exptl_crystal_colour orange _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.282 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 7.361 _exptl_absorpt_correction_type 'semi-empirical (psi scans)' _exptl_absorpt_correction_T_min 0.1068 _exptl_absorpt_correction_T_max 0.1826 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 260(2) _diffrn_radiation_wavelength 0.70930 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'scintillation counter' _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_% ? _diffrn_reflns_number 5879 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.0322 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 24.93 _reflns_number_total 4132 _reflns_number_gt 3233 _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-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP 3 (Farrugia 2000)' _computing_publication_material 'SHELXS-97' _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 4132 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0564 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.1288 _refine_ls_wR_factor_gt 0.1197 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _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 0.75630(4) 0.010224(19) 0.994996(15) 0.04201(15) Uani 1 1 d . . . Cl1 Cl 0.7372(4) -0.01061(13) 1.11875(12) 0.0546(6) Uani 1 1 d . . . Cl2 Cl 0.5071(9) 0.0101(7) 0.6314(3) 0.356(9) Uani 1 1 d . . . N1 N 0.6995(9) -0.0883(4) 0.9585(3) 0.0469(17) Uani 1 1 d . . . N2 N 0.7715(11) 0.0281(4) 0.8907(4) 0.0497(18) Uani 1 1 d . . . N3 N 0.8183(9) 0.1146(4) 0.9978(3) 0.0423(15) Uani 1 1 d . . . C1 C 0.6606(12) -0.1462(5) 0.9994(5) 0.053(2) Uani 1 1 d . . . H1 H 0.6592 -0.1427 1.0501 0.084(10) Uiso 1 1 calc R . . C2 C 0.6241(15) -0.2086(6) 0.9673(6) 0.066(3) Uani 1 1 d . . . H2 H 0.6009 -0.2481 0.9964 0.084(10) Uiso 1 1 calc R . . C3 C 0.6197(15) -0.2163(6) 0.8909(6) 0.067(3) Uani 1 1 d . . . H3 H 0.5917 -0.2595 0.8689 0.084(10) Uiso 1 1 calc R . . C4 C 0.6593(13) -0.1560(6) 0.8499(5) 0.061(2) Uani 1 1 d . . . H4 H 0.6576 -0.1582 0.7992 0.084(10) Uiso 1 1 calc R . . C5 C 0.7006(11) -0.0937(5) 0.8839(4) 0.047(2) Uani 1 1 d . . . C6 C 0.7467(12) -0.0278(5) 0.8448(4) 0.047(2) Uani 1 1 d . . . C7 C 0.7713(13) -0.0174(5) 0.7710(5) 0.055(2) Uani 1 1 d . . . H7 H 0.7553 -0.0547 0.7384 0.084(10) Uiso 1 1 calc R . . C8 C 0.8208(15) 0.0506(6) 0.7456(4) 0.062(3) Uani 1 1 d . . . C9 C 0.8416(14) 0.1065(6) 0.7941(4) 0.059(2) Uani 1 1 d . . . H9 H 0.8712 0.1518 0.7775 0.084(10) Uiso 1 1 calc R . . C10 C 0.8165(12) 0.0928(5) 0.8687(4) 0.0456(19) Uani 1 1 d . . . C11 C 0.8409(11) 0.1439(5) 0.9291(4) 0.047(2) Uani 1 1 d . . . C12 C 0.8858(14) 0.2141(5) 0.9211(5) 0.057(2) Uani 1 1 d . . . H12 H 0.9028 0.2334 0.8748 0.084(10) Uiso 1 1 calc R . . C13 C 0.9056(14) 0.2557(6) 0.9823(6) 0.063(2) Uani 1 1 d . . . H13 H 0.9316 0.3038 0.9776 0.084(10) Uiso 1 1 calc R . . C14 C 0.8866(14) 0.2257(6) 1.0504(5) 0.061(3) Uani 1 1 d . . . H14 H 0.9044 0.2529 1.0923 0.084(10) Uiso 1 1 calc R . . C15 C 0.8412(11) 0.1556(5) 1.0555(4) 0.052(2) Uani 1 1 d . . . H15 H 0.8257 0.1358 1.1017 0.084(10) Uiso 1 1 calc R . . C16 C 0.860(2) 0.0628(6) 0.6662(5) 0.082(4) Uani 1 1 d . . . C17 C 1.042(3) 0.0925(6) 0.6477(6) 0.102(5) Uani 1 1 d . . . H17 H 1.1333 0.1038 0.6835 0.084(10) Uiso 1 1 calc R . . C18 C 1.081(4) 0.1047(8) 0.5737(9) 0.180(12) Uani 1 1 d . . . H18 H 1.2015 0.1241 0.5606 0.084(10) Uiso 1 1 calc R . . C19 C 0.949(5) 0.0891(9) 0.5205(9) 0.184(14) Uani 1 1 d . . . H19 H 0.9785 0.0985 0.4718 0.084(10) Uiso 1 1 calc R . . C20 C 0.775(4) 0.0597(13) 0.5388(7) 0.178(13) Uani 1 1 d . . . H20 H 0.6869 0.0492 0.5014 0.084(10) Uiso 1 1 calc R . . C21 C 0.718(3) 0.0439(12) 0.6120(7) 0.136(7) Uani 1 1 d . . . Sb Sb 0.37749(11) 0.28781(5) 0.79520(4) 0.0704(3) Uani 1 1 d . . . F1 F 0.5995(16) 0.3317(7) 0.8333(6) 0.183(5) Uani 1 1 d . . . F2 F 0.3592(18) 0.3630(6) 0.7319(5) 0.160(4) Uani 1 1 d . . . F3 F 0.4114(17) 0.2119(5) 0.8550(5) 0.155(4) Uani 1 1 d . . . F4 F 0.2378(16) 0.3310(6) 0.8670(6) 0.156(4) Uani 1 1 d . . . F5 F 0.5263(16) 0.2384(6) 0.7240(6) 0.161(4) Uani 1 1 d . . . F6 F 0.1519(15) 0.2467(7) 0.7586(6) 0.163(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 0.0290(2) 0.0689(3) 0.0281(2) -0.00361(13) -0.00180(13) 0.01206(14) Cl1 0.0438(13) 0.0898(17) 0.0304(10) 0.0009(9) -0.0018(9) 0.0112(10) Cl2 0.096(4) 0.90(3) 0.069(3) -0.041(6) -0.039(3) -0.003(7) N1 0.024(3) 0.080(5) 0.037(3) -0.011(3) -0.006(3) 0.011(3) N2 0.040(4) 0.081(5) 0.028(3) -0.002(3) -0.002(3) 0.014(4) N3 0.027(3) 0.063(4) 0.037(3) -0.003(3) -0.003(3) 0.012(3) C1 0.032(4) 0.082(7) 0.045(5) -0.004(5) 0.002(4) 0.009(4) C2 0.049(5) 0.092(8) 0.059(6) 0.001(5) 0.003(5) 0.007(5) C3 0.056(6) 0.070(7) 0.075(7) -0.017(5) -0.004(5) 0.001(5) C4 0.043(5) 0.093(8) 0.046(5) -0.014(5) -0.004(4) -0.001(5) C5 0.025(4) 0.077(6) 0.039(4) -0.005(4) -0.001(3) 0.007(4) C6 0.031(4) 0.072(6) 0.038(4) -0.008(4) -0.006(3) 0.009(4) C7 0.050(5) 0.083(7) 0.033(4) -0.012(4) -0.005(4) 0.011(5) C8 0.075(7) 0.086(7) 0.026(4) 0.005(4) -0.002(4) 0.036(5) C9 0.060(6) 0.082(7) 0.034(4) 0.006(4) 0.000(4) 0.025(5) C10 0.039(4) 0.066(6) 0.032(4) 0.002(4) -0.003(3) 0.013(4) C11 0.036(4) 0.073(6) 0.033(4) -0.003(4) -0.002(3) 0.016(4) C12 0.055(5) 0.075(7) 0.043(5) 0.000(4) -0.004(4) 0.014(5) C13 0.055(6) 0.062(6) 0.073(6) -0.004(5) 0.002(5) 0.006(5) C14 0.056(6) 0.079(7) 0.049(5) -0.015(5) -0.003(4) 0.012(5) C15 0.032(4) 0.083(7) 0.040(4) -0.023(4) -0.004(3) 0.010(4) C16 0.138(11) 0.087(8) 0.022(4) 0.007(4) 0.002(6) 0.060(8) C17 0.189(16) 0.063(7) 0.054(7) 0.007(5) 0.044(9) 0.018(9) C18 0.37(4) 0.081(10) 0.085(11) 0.009(8) 0.109(17) -0.038(15) C19 0.43(4) 0.078(10) 0.041(8) 0.011(7) 0.065(15) 0.092(17) C20 0.29(3) 0.22(3) 0.019(6) -0.001(9) -0.005(11) 0.14(2) C21 0.134(14) 0.23(2) 0.039(6) -0.006(9) -0.001(7) 0.080(14) Sb 0.0662(5) 0.1030(6) 0.0418(4) 0.0248(3) -0.0069(3) -0.0111(4) F1 0.150(9) 0.240(13) 0.158(9) 0.070(9) -0.075(7) -0.097(9) F2 0.214(11) 0.156(8) 0.110(7) 0.075(6) -0.051(7) -0.027(8) F3 0.200(11) 0.144(8) 0.120(7) 0.077(6) -0.007(7) 0.000(7) F4 0.179(10) 0.151(9) 0.139(8) -0.031(7) 0.037(7) 0.015(8) F5 0.170(10) 0.166(10) 0.149(8) 0.011(7) 0.082(8) 0.000(8) F6 0.131(8) 0.220(11) 0.137(8) 0.020(8) -0.063(6) -0.065(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 1.941(7) . ? Pt N1 2.014(8) . ? Pt N3 2.017(7) . ? Pt Cl1 2.303(2) . ? Cl2 C21 1.61(2) . ? N1 C1 1.351(12) . ? N1 C5 1.370(10) . ? N2 C10 1.323(12) . ? N2 C6 1.359(12) . ? N3 C15 1.319(10) . ? N3 C11 1.382(10) . ? C1 C2 1.341(14) . ? C2 C3 1.405(14) . ? C3 C4 1.391(14) . ? C4 C5 1.360(13) . ? C5 C6 1.470(13) . ? C6 C7 1.376(12) . ? C7 C8 1.407(14) . ? C8 C9 1.388(13) . ? C8 C16 1.496(12) . ? C9 C10 1.401(11) . ? C10 C11 1.476(11) . ? C11 C12 1.370(13) . ? C12 C13 1.374(13) . ? C13 C14 1.376(14) . ? C14 C15 1.363(14) . ? C16 C17 1.400(19) . ? C16 C21 1.43(2) . ? C17 C18 1.400(17) . ? C18 C19 1.36(3) . ? C19 C20 1.36(4) . ? C20 C21 1.43(2) . ? Sb F4 1.817(9) . ? Sb F3 1.818(8) . ? Sb F2 1.837(8) . ? Sb F6 1.849(9) . ? Sb F1 1.861(9) . ? Sb F5 1.898(11) . ? 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(3) . . ? N2 Pt N3 81.0(3) . . ? N1 Pt N3 162.1(3) . . ? N2 Pt Cl1 179.8(2) . . ? N1 Pt Cl1 99.0(2) . . ? N3 Pt Cl1 98.87(19) . . ? C1 N1 C5 119.6(8) . . ? C1 N1 Pt 127.0(6) . . ? C5 N1 Pt 113.4(6) . . ? C10 N2 C6 123.9(7) . . ? C10 N2 Pt 118.2(6) . . ? C6 N2 Pt 117.8(7) . . ? C15 N3 C11 118.7(8) . . ? C15 N3 Pt 128.2(6) . . ? C11 N3 Pt 113.0(5) . . ? C2 C1 N1 120.4(8) . . ? C1 C2 C3 122.0(10) . . ? C4 C3 C2 116.7(10) . . ? C5 C4 C3 120.1(9) . . ? C4 C5 N1 121.3(9) . . ? C4 C5 C6 123.7(8) . . ? N1 C5 C6 115.1(8) . . ? N2 C6 C7 118.8(9) . . ? N2 C6 C5 112.5(7) . . ? C7 C6 C5 128.7(9) . . ? C6 C7 C8 119.0(9) . . ? C9 C8 C7 120.5(8) . . ? C9 C8 C16 119.0(10) . . ? C7 C8 C16 120.4(9) . . ? C8 C9 C10 118.1(10) . . ? N2 C10 C9 119.8(8) . . ? N2 C10 C11 113.7(7) . . ? C9 C10 C11 126.5(9) . . ? C12 C11 N3 120.6(8) . . ? C12 C11 C10 125.3(8) . . ? N3 C11 C10 114.0(8) . . ? C11 C12 C13 119.2(9) . . ? C12 C13 C14 119.6(10) . . ? C15 C14 C13 118.9(9) . . ? N3 C15 C14 122.9(9) . . ? C17 C16 C21 122.1(11) . . ? C17 C16 C8 117.2(11) . . ? C21 C16 C8 120.8(13) . . ? C18 C17 C16 118.1(17) . . ? C19 C18 C17 122(2) . . ? C20 C19 C18 119.6(15) . . ? C19 C20 C21 124(2) . . ? C20 C21 C16 114.4(19) . . ? C20 C21 Cl2 122.2(16) . . ? C16 C21 Cl2 123.4(11) . . ? F4 Sb F3 89.1(5) . . ? F4 Sb F2 94.2(5) . . ? F3 Sb F2 176.1(5) . . ? F4 Sb F6 90.8(6) . . ? F3 Sb F6 89.6(5) . . ? F2 Sb F6 92.3(5) . . ? F4 Sb F1 87.5(6) . . ? F3 Sb F1 91.3(5) . . ? F2 Sb F1 86.9(5) . . ? F6 Sb F1 178.1(6) . . ? F4 Sb F5 176.7(5) . . ? F3 Sb F5 87.6(5) . . ? F2 Sb F5 89.1(5) . . ? F6 Sb F5 89.4(5) . . ? F1 Sb F5 92.3(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.93 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.425 _refine_diff_density_min -1.803 _refine_diff_density_rms 0.177 data_temdep295Kstructure _database_code_CSD 194849 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Pt{4'(o-Cl-Ph)trpy}Cl]SbF6 _chemical_formula_sum 'C21 H14 Cl2 F6 N3 Pt Sb' _chemical_formula_weight 810.09 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' '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' 'F' 'F' 0.0171 0.0103 '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 _symmetry_Int_Tables_number 14 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 6.8440(10) _cell_length_b 18.965(2) _cell_length_c 18.333(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.050(10) _cell_angle_gamma 90.00 _cell_volume 2379.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 3 _cell_measurement_theta_max 12 _exptl_crystal_description paralellpiped _exptl_crystal_colour orange _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.261 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 7.294 _exptl_absorpt_correction_type 'semi-empirical (psi scans)' _exptl_absorpt_correction_T_min 0.1080 _exptl_absorpt_correction_T_max 0.1845 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.70930 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'scintillation counter' _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 5764 _diffrn_reflns_av_R_equivalents 0.0163 _diffrn_reflns_av_sigmaI/netI 0.0273 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 24.92 _reflns_number_total 4174 _reflns_number_gt 3290 _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-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP 3 (Farrugia 2000)' _computing_publication_material 'SHELXS-97' _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 4174 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.1166 _refine_ls_wR_factor_gt 0.1079 _refine_ls_goodness_of_fit_ref 0.910 _refine_ls_restrained_S_all 0.910 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt 0.75512(3) 0.009123(16) 0.995358(12) 0.04583(14) Uani 1 1 d . . . Cl1 Cl 0.7365(3) -0.01183(12) 1.11867(11) 0.0622(5) Uani 1 1 d . . . Cl2 Cl 0.5072(9) 0.0077(5) 0.6326(3) 0.308(6) Uani 1 1 d . . . N1 N 0.7014(7) -0.0890(3) 0.9585(3) 0.0515(14) Uani 1 1 d . . . N2 N 0.7706(9) 0.0273(4) 0.8916(3) 0.0510(15) Uani 1 1 d . . . N3 N 0.8152(8) 0.1133(3) 0.9982(3) 0.0461(13) Uani 1 1 d . . . C1 C 0.6647(10) -0.1468(4) 0.9985(4) 0.0578(19) Uani 1 1 d . . . H1 H 0.6654 -0.1434 1.0491 0.074(7) Uiso 1 1 calc R . . C2 C 0.6267(12) -0.2101(5) 0.9670(5) 0.067(2) Uani 1 1 d . . . H2 H 0.6009 -0.2494 0.9957 0.074(7) Uiso 1 1 calc R . . C3 C 0.6265(12) -0.2158(5) 0.8919(5) 0.067(2) Uani 1 1 d . . . H3 H 0.6023 -0.2590 0.8698 0.074(7) Uiso 1 1 calc R . . C4 C 0.6628(11) -0.1564(5) 0.8496(4) 0.064(2) Uani 1 1 d . . . H4 H 0.6615 -0.1592 0.7990 0.074(7) Uiso 1 1 calc R . . C5 C 0.7004(9) -0.0939(4) 0.8838(4) 0.0517(17) Uani 1 1 d . . . C6 C 0.7461(10) -0.0284(4) 0.8458(4) 0.0506(16) Uani 1 1 d . . . C7 C 0.7697(11) -0.0170(4) 0.7727(4) 0.0571(18) Uani 1 1 d . . . H7 H 0.7546 -0.0541 0.7400 0.074(7) Uiso 1 1 calc R . . C8 C 0.8159(12) 0.0499(5) 0.7469(4) 0.066(2) Uani 1 1 d . . . C9 C 0.8365(12) 0.1056(4) 0.7958(4) 0.0609(19) Uani 1 1 d . . . H9 H 0.8651 0.1508 0.7793 0.074(7) Uiso 1 1 calc R . . C10 C 0.8134(10) 0.0921(4) 0.8692(3) 0.0502(16) Uani 1 1 d . . . C11 C 0.8379(10) 0.1428(4) 0.9301(4) 0.0510(16) Uani 1 1 d . . . C12 C 0.8797(12) 0.2129(5) 0.9224(4) 0.065(2) Uani 1 1 d . . . H12 H 0.8940 0.2324 0.8761 0.074(7) Uiso 1 1 calc R . . C13 C 0.9004(12) 0.2541(5) 0.9830(5) 0.070(2) Uani 1 1 d . . . H13 H 0.9267 0.3020 0.9784 0.074(7) Uiso 1 1 calc R . . C14 C 0.8819(13) 0.2242(5) 1.0504(5) 0.072(2) Uani 1 1 d . . . H14 H 0.8994 0.2514 1.0921 0.074(7) Uiso 1 1 calc R . . C15 C 0.8380(10) 0.1546(4) 1.0564(4) 0.0581(19) Uani 1 1 d . . . H15 H 0.8233 0.1351 1.1027 0.074(7) Uiso 1 1 calc R . . C16 C 0.8625(18) 0.0639(5) 0.6677(4) 0.088(3) Uani 1 1 d . . . C17 C 1.042(2) 0.0922(5) 0.6495(5) 0.111(5) Uani 1 1 d . . . H17 H 1.1351 0.1028 0.6848 0.074(7) Uiso 1 1 calc R . . C18 C 1.077(3) 0.1042(7) 0.5744(8) 0.168(8) Uani 1 1 d . . . H18 H 1.1962 0.1229 0.5594 0.074(7) Uiso 1 1 calc R . . C19 C 0.934(4) 0.0881(8) 0.5227(8) 0.183(12) Uani 1 1 d . . . H19 H 0.9582 0.0971 0.4737 0.074(7) Uiso 1 1 calc R . . C20 C 0.770(3) 0.0615(11) 0.5412(7) 0.180(10) Uani 1 1 d . . . H20 H 0.6801 0.0518 0.5046 0.074(7) Uiso 1 1 calc R . . C21 C 0.718(2) 0.0456(9) 0.6141(6) 0.130(5) Uani 1 1 d . . . Sb Sb 0.37010(10) 0.28899(4) 0.79630(3) 0.0840(3) Uani 1 1 d . . . F1 F 0.5876(17) 0.3320(8) 0.8348(6) 0.228(6) Uani 1 1 d . . . F2 F 0.3591(17) 0.3612(5) 0.7324(5) 0.189(4) Uani 1 1 d . . . F3 F 0.4034(16) 0.2135(5) 0.8545(5) 0.190(4) Uani 1 1 d . . . F4 F 0.2299(17) 0.3302(6) 0.8662(6) 0.198(4) Uani 1 1 d . . . F5 F 0.5220(17) 0.2400(6) 0.7269(7) 0.214(6) Uani 1 1 d . . . F6 F 0.1485(14) 0.2485(6) 0.7596(6) 0.187(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 0.0336(2) 0.0726(2) 0.03123(18) -0.00195(11) -0.00091(12) 0.01172(11) Cl1 0.0507(11) 0.1032(15) 0.0327(9) 0.0029(8) -0.0004(8) 0.0119(9) Cl2 0.135(4) 0.70(2) 0.090(3) -0.013(5) -0.051(3) -0.035(6) N1 0.032(3) 0.088(4) 0.035(3) -0.006(3) -0.001(2) 0.012(3) N2 0.043(3) 0.079(4) 0.032(3) -0.005(3) -0.003(2) 0.015(3) N3 0.032(3) 0.064(4) 0.042(3) -0.007(2) -0.001(2) 0.014(2) C1 0.039(4) 0.078(6) 0.056(4) 0.008(4) 0.002(3) 0.008(4) C2 0.050(4) 0.081(6) 0.071(5) 0.008(4) 0.005(4) 0.003(4) C3 0.062(5) 0.074(5) 0.066(5) -0.010(4) 0.004(4) -0.001(4) C4 0.051(4) 0.093(6) 0.050(4) -0.020(4) 0.006(3) -0.005(4) C5 0.033(3) 0.076(5) 0.046(4) 0.003(3) -0.003(3) 0.006(3) C6 0.037(3) 0.070(4) 0.046(4) -0.003(3) -0.008(3) 0.011(3) C7 0.061(5) 0.075(5) 0.036(4) -0.007(3) -0.001(3) 0.014(4) C8 0.072(5) 0.093(6) 0.034(4) -0.001(4) -0.003(3) 0.032(4) C9 0.067(5) 0.071(5) 0.044(4) 0.006(3) 0.003(3) 0.018(4) C10 0.042(4) 0.075(5) 0.034(3) 0.000(3) -0.004(3) 0.008(3) C11 0.047(4) 0.061(4) 0.045(4) -0.003(3) -0.003(3) 0.012(3) C12 0.059(5) 0.083(6) 0.053(4) -0.001(4) 0.006(4) 0.006(4) C13 0.064(5) 0.071(5) 0.074(5) -0.010(4) 0.005(4) 0.005(4) C14 0.068(5) 0.094(7) 0.054(5) -0.020(4) 0.000(4) 0.005(5) C15 0.044(4) 0.083(5) 0.047(4) -0.017(4) -0.005(3) 0.011(4) C16 0.146(10) 0.084(6) 0.032(4) 0.008(4) -0.002(5) 0.039(6) C17 0.197(14) 0.070(6) 0.066(6) 0.019(5) 0.061(8) 0.007(7) C18 0.31(3) 0.092(9) 0.103(11) 0.020(8) 0.105(14) -0.006(12) C19 0.41(4) 0.086(9) 0.049(7) 0.018(6) 0.060(13) 0.076(15) C20 0.29(3) 0.22(2) 0.029(6) 0.015(8) -0.003(10) 0.083(19) C21 0.169(14) 0.161(12) 0.059(6) 0.009(7) -0.022(8) 0.037(11) Sb 0.0772(4) 0.1252(6) 0.0496(3) 0.0351(3) -0.0073(3) -0.0162(4) F1 0.188(9) 0.309(14) 0.188(10) 0.052(10) -0.090(8) -0.105(10) F2 0.254(11) 0.184(8) 0.128(6) 0.088(6) -0.044(7) -0.041(8) F3 0.243(12) 0.189(9) 0.139(7) 0.093(7) -0.003(7) -0.004(8) F4 0.227(11) 0.174(9) 0.194(10) -0.041(8) 0.063(8) 0.015(8) F5 0.254(13) 0.201(11) 0.187(10) 0.028(8) 0.124(10) 0.008(10) F6 0.134(7) 0.242(11) 0.185(9) 0.030(8) -0.069(6) -0.078(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 N2 1.935(6) . ? Pt N1 2.013(6) . ? Pt N3 2.018(6) . ? Pt Cl1 2.299(2) . ? Cl2 C21 1.648(18) . ? N1 C1 1.344(10) . ? N1 C5 1.372(8) . ? N2 C10 1.329(10) . ? N2 C6 1.360(10) . ? N3 C15 1.333(9) . ? N3 C11 1.378(9) . ? C1 C2 1.358(11) . ? C2 C3 1.379(12) . ? C3 C4 1.390(12) . ? C4 C5 1.364(11) . ? C5 C6 1.459(10) . ? C6 C7 1.367(10) . ? C7 C8 1.389(12) . ? C8 C9 1.392(11) . ? C8 C16 1.512(11) . ? C9 C10 1.380(9) . ? C10 C11 1.482(10) . ? C11 C12 1.369(11) . ? C12 C13 1.365(12) . ? C13 C14 1.367(12) . ? C14 C15 1.358(12) . ? C16 C17 1.382(16) . ? C16 C21 1.436(17) . ? C17 C18 1.416(15) . ? C18 C19 1.40(3) . ? C19 C20 1.27(3) . ? C20 C21 1.417(18) . ? Sb F4 1.783(9) . ? Sb F3 1.799(7) . ? Sb F2 1.804(7) . ? Sb F6 1.828(8) . ? Sb F1 1.838(9) . ? Sb F5 1.888(11) . ? 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(3) . . ? N2 Pt N3 80.8(3) . . ? N1 Pt N3 161.9(2) . . ? N2 Pt Cl1 179.7(2) . . ? N1 Pt Cl1 99.23(16) . . ? N3 Pt Cl1 98.91(16) . . ? C1 N1 C5 119.2(7) . . ? C1 N1 Pt 127.3(5) . . ? C5 N1 Pt 113.5(5) . . ? C10 N2 C6 123.6(6) . . ? C10 N2 Pt 118.8(5) . . ? C6 N2 Pt 117.5(6) . . ? C15 N3 C11 118.3(7) . . ? C15 N3 Pt 128.3(5) . . ? C11 N3 Pt 113.4(4) . . ? N1 C1 C2 121.7(7) . . ? C1 C2 C3 119.5(8) . . ? C2 C3 C4 119.6(8) . . ? C5 C4 C3 118.8(7) . . ? C4 C5 N1 121.2(7) . . ? C4 C5 C6 124.1(7) . . ? N1 C5 C6 114.7(7) . . ? N2 C6 C7 118.0(7) . . ? N2 C6 C5 113.1(6) . . ? C7 C6 C5 128.9(7) . . ? C6 C7 C8 120.2(7) . . ? C7 C8 C9 119.9(7) . . ? C7 C8 C16 122.4(7) . . ? C9 C8 C16 117.6(8) . . ? C10 C9 C8 118.4(8) . . ? N2 C10 C9 119.9(7) . . ? N2 C10 C11 113.0(6) . . ? C9 C10 C11 127.0(7) . . ? C12 C11 N3 120.8(7) . . ? C12 C11 C10 125.2(7) . . ? N3 C11 C10 114.0(6) . . ? C13 C12 C11 119.6(8) . . ? C12 C13 C14 119.3(9) . . ? C15 C14 C13 119.8(8) . . ? N3 C15 C14 122.2(8) . . ? C17 C16 C21 122.7(10) . . ? C17 C16 C8 119.2(9) . . ? C21 C16 C8 118.0(11) . . ? C16 C17 C18 116.7(14) . . ? C19 C18 C17 120.3(17) . . ? C20 C19 C18 121.6(14) . . ? C19 C20 C21 123.9(19) . . ? C20 C21 C16 114.8(16) . . ? C20 C21 Cl2 120.6(14) . . ? C16 C21 Cl2 124.5(10) . . ? F4 Sb F3 89.5(5) . . ? F4 Sb F2 96.4(6) . . ? F3 Sb F2 173.8(5) . . ? F4 Sb F6 90.1(6) . . ? F3 Sb F6 89.3(5) . . ? F2 Sb F6 92.6(5) . . ? F4 Sb F1 88.0(6) . . ? F3 Sb F1 91.4(5) . . ? F2 Sb F1 86.9(5) . . ? F6 Sb F1 178.0(6) . . ? F4 Sb F5 176.0(5) . . ? F3 Sb F5 86.5(5) . . ? F2 Sb F5 87.6(5) . . ? F6 Sb F5 90.2(5) . . ? F1 Sb F5 91.8(6) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.92 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.193 _refine_diff_density_min -1.520 _refine_diff_density_rms 0.151