# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _publ_contact_author_email fieldj@ukzn.ac.za _publ_contact_author_name 'John Field' _publ_author_name J.Field data_1_1st _database_code_depnum_ccdc_archive 'CCDC 857048' #TrackingRef '8518_web_deposit_cif_file_0_JohnField_1323158265.1_1st.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Pt{4'-(Ph)trpy}(NCS)]SbF6 (1): this crystal was obtained by allowing acetonitrile to escape from a single crystal of the solvate. It is the 1st determination of the crystal structure of 1. ; _chemical_name_common "[Pt{4'-(Ph)trpy}(NCS)]SbF6" _chemical_melting_point ? _chemical_formula_moiety 'C22 H15 N4 Pt S, F6 Sb' _chemical_formula_sum 'C22 H15 F6 N4 Pt S Sb' _chemical_formula_weight 798.28 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 _symmetry_space_group_name_Hall '-P 2yn' 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 9.6158(2) _cell_length_b 25.6118(7) _cell_length_c 10.3103(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.392(2) _cell_angle_gamma 90.00 _cell_volume 2523.41(11) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used >200 _cell_measurement_theta_min 4 _cell_measurement_theta_max 32 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.101 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 6.753 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0896 _exptl_absorpt_correction_T_max 0.3618 _exptl_absorpt_process_details 'Crysalis 170 RED' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur CCD' _diffrn_measurement_method 'omega 2 theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40442 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0370 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.64 _diffrn_reflns_theta_max 34.21 _reflns_number_total 9037 _reflns_number_gt 6857 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crysalis 170 CCD' _computing_cell_refinement 'Crysalis 170 CCD' _computing_data_reduction 'Crysalis 170 CCD' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-seed (Barbour, 2006)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.0289P)^2^+7.2219P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9037 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.0821 _refine_ls_wR_factor_gt 0.0783 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt 0.522908(16) 0.028163(6) 0.846366(15) 0.02481(5) Uani 1 1 d . . . Sb Sb 0.28494(4) 0.313182(12) 0.08804(3) 0.03697(8) Uani 1 1 d . . . S S 0.97074(17) 0.09528(8) 0.99925(16) 0.0661(5) Uani 1 1 d . . . F1 F 0.3729(5) 0.37837(13) 0.1113(4) 0.0719(12) Uani 1 1 d . . . F2 F 0.1140(4) 0.34615(18) 0.0531(5) 0.0843(14) Uani 1 1 d . . . F3 F 0.2034(4) 0.24729(13) 0.0618(4) 0.0665(10) Uani 1 1 d . . . F4 F 0.4613(3) 0.28178(13) 0.1205(4) 0.0571(9) Uani 1 1 d . . . F5 F 0.3110(4) 0.31612(14) -0.0901(3) 0.0610(9) Uani 1 1 d . . . F6 F 0.2630(5) 0.3096(2) 0.2641(4) 0.0859(13) Uani 1 1 d . . . N1 N 0.4287(4) 0.09882(13) 0.8306(3) 0.0258(7) Uani 1 1 d . . . N2 N 0.3357(4) 0.00634(13) 0.7844(3) 0.0218(6) Uani 1 1 d . . . N3 N 0.5565(4) -0.04954(15) 0.8392(3) 0.0264(7) Uani 1 1 d . . . N4 N 0.7192(4) 0.05157(15) 0.9114(4) 0.0312(8) Uani 1 1 d . . . C1 C 0.4900(6) 0.14567(19) 0.8543(5) 0.0379(11) Uani 1 1 d . . . H1 H 0.5872 0.1473 0.8833 0.045 Uiso 1 1 calc R . . C2 C 0.4134(6) 0.19156(19) 0.8370(5) 0.0425(12) Uani 1 1 d . . . H2 H 0.4584 0.2244 0.8521 0.051 Uiso 1 1 calc R . . C3 C 0.2716(6) 0.18928(19) 0.7977(5) 0.0412(11) Uani 1 1 d . . . H3 H 0.2174 0.2203 0.7869 0.049 Uiso 1 1 calc R . . C4 C 0.2091(5) 0.14045(17) 0.7741(4) 0.0325(9) Uani 1 1 d . . . H4 H 0.1116 0.1380 0.7474 0.039 Uiso 1 1 calc R . . C5 C 0.2884(5) 0.09627(16) 0.7895(4) 0.0265(8) Uani 1 1 d . . . C6 C 0.2345(4) 0.04279(16) 0.7630(4) 0.0250(8) Uani 1 1 d . . . C7 C 0.1012(4) 0.02809(16) 0.7164(4) 0.0236(7) Uani 1 1 d . . . H7 H 0.0299 0.0537 0.7015 0.028 Uiso 1 1 calc R . . C8 C 0.0692(4) -0.02505(16) 0.6902(4) 0.0230(7) Uani 1 1 d . . . C9 C 0.1788(4) -0.06131(16) 0.7155(4) 0.0250(8) Uani 1 1 d . . . H9 H 0.1616 -0.0974 0.6995 0.030 Uiso 1 1 calc R . . C10 C 0.3103(4) -0.04486(15) 0.7631(4) 0.0230(7) Uani 1 1 d . . . C11 C 0.4378(4) -0.07718(17) 0.7961(4) 0.0264(8) Uani 1 1 d . . . C12 C 0.4419(5) -0.13104(18) 0.7852(5) 0.0362(10) Uani 1 1 d . . . H12 H 0.3595 -0.1499 0.7549 0.043 Uiso 1 1 calc R . . C13 C 0.5663(6) -0.15715(19) 0.8186(5) 0.0417(12) Uani 1 1 d . . . H13 H 0.5702 -0.1941 0.8127 0.050 Uiso 1 1 calc R . . C14 C 0.6856(5) -0.12870(19) 0.8611(5) 0.0371(10) Uani 1 1 d . . . H14 H 0.7727 -0.1459 0.8825 0.045 Uiso 1 1 calc R . . C15 C 0.6764(4) -0.07559(18) 0.8717(4) 0.0281(8) Uani 1 1 d . . . H15 H 0.7579 -0.0565 0.9033 0.034 Uiso 1 1 calc R . . C16 C -0.0734(4) -0.04157(16) 0.6353(4) 0.0252(8) Uani 1 1 d . . . C17 C -0.1811(4) -0.00511(19) 0.6130(4) 0.0303(9) Uani 1 1 d . . . H17 H -0.1637 0.0305 0.6352 0.036 Uiso 1 1 calc R . . C18 C -0.3135(5) -0.0202(2) 0.5588(4) 0.0339(10) Uani 1 1 d . . . H18 H -0.3851 0.0053 0.5427 0.041 Uiso 1 1 calc R . . C19 C -0.3426(5) -0.0718(2) 0.5277(4) 0.0355(10) Uani 1 1 d . . . H19 H -0.4333 -0.0819 0.4902 0.043 Uiso 1 1 calc R . . C20 C -0.2370(6) -0.10857(19) 0.5522(5) 0.0390(11) Uani 1 1 d . . . H20 H -0.2562 -0.1442 0.5323 0.047 Uiso 1 1 calc R . . C21 C -0.1036(5) -0.09388(18) 0.6056(5) 0.0342(10) Uani 1 1 d . . . H21 H -0.0325 -0.1196 0.6220 0.041 Uiso 1 1 calc R . . C22 C 0.8208(5) 0.0691(2) 0.9463(5) 0.0356(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt 0.02233(7) 0.02919(8) 0.02270(7) -0.00254(6) 0.00160(5) -0.00266(6) Sb 0.03700(17) 0.02624(14) 0.04663(18) -0.00119(13) 0.00005(13) 0.00426(12) S 0.0381(7) 0.1064(14) 0.0513(8) 0.0083(9) -0.0063(6) -0.0321(8) F1 0.083(3) 0.0294(16) 0.100(3) -0.0146(18) -0.004(2) -0.0066(17) F2 0.052(2) 0.078(3) 0.120(4) 0.005(3) -0.002(2) 0.037(2) F3 0.055(2) 0.0411(18) 0.101(3) 0.0025(19) -0.002(2) -0.0118(16) F4 0.0404(18) 0.0483(19) 0.080(2) 0.0045(17) -0.0049(17) 0.0094(14) F5 0.082(3) 0.052(2) 0.0482(19) 0.0055(15) 0.0027(18) 0.0036(18) F6 0.093(3) 0.115(4) 0.053(2) -0.003(2) 0.020(2) 0.020(3) N1 0.0241(16) 0.0246(16) 0.0289(17) -0.0032(14) 0.0040(13) -0.0060(13) N2 0.0233(16) 0.0239(15) 0.0180(14) -0.0007(12) 0.0014(12) -0.0035(13) N3 0.0271(17) 0.0312(18) 0.0208(15) 0.0032(13) 0.0029(13) 0.0008(14) N4 0.033(2) 0.0313(19) 0.0292(18) -0.0063(15) 0.0044(15) -0.0013(16) C1 0.042(3) 0.033(2) 0.038(2) -0.010(2) 0.003(2) -0.006(2) C2 0.052(3) 0.026(2) 0.050(3) -0.007(2) 0.006(2) -0.009(2) C3 0.047(3) 0.029(2) 0.048(3) -0.008(2) 0.004(2) 0.005(2) C4 0.034(2) 0.029(2) 0.034(2) -0.0030(18) 0.0026(18) -0.0003(18) C5 0.030(2) 0.0234(18) 0.0253(18) -0.0047(15) 0.0018(16) -0.0056(16) C6 0.029(2) 0.0228(18) 0.0233(18) -0.0018(15) 0.0013(15) 0.0018(15) C7 0.0245(17) 0.0224(17) 0.0238(17) 0.0001(15) 0.0025(14) 0.0050(15) C8 0.0214(17) 0.0276(19) 0.0203(16) -0.0005(15) 0.0036(13) -0.0037(16) C9 0.0239(18) 0.0235(18) 0.0272(18) 0.0015(15) 0.0007(15) -0.0040(15) C10 0.0261(19) 0.0210(17) 0.0216(17) 0.0029(14) 0.0017(14) 0.0007(15) C11 0.0207(18) 0.035(2) 0.0228(18) 0.0022(16) -0.0009(14) 0.0011(16) C12 0.034(2) 0.029(2) 0.044(3) 0.003(2) -0.0007(19) -0.0019(19) C13 0.045(3) 0.026(2) 0.052(3) 0.006(2) -0.006(2) 0.003(2) C14 0.036(2) 0.036(2) 0.038(2) 0.009(2) -0.0014(19) 0.008(2) C15 0.0220(18) 0.037(2) 0.0243(18) 0.0030(17) -0.0009(14) 0.0010(17) C16 0.0246(18) 0.028(2) 0.0226(17) 0.0007(15) 0.0019(14) -0.0022(15) C17 0.023(2) 0.037(2) 0.030(2) -0.0022(18) -0.0005(16) -0.0025(17) C18 0.025(2) 0.045(3) 0.031(2) 0.0018(19) 0.0009(16) -0.0006(19) C19 0.025(2) 0.055(3) 0.025(2) -0.003(2) 0.0002(16) -0.010(2) C20 0.045(3) 0.033(2) 0.037(2) -0.0073(19) -0.001(2) -0.014(2) C21 0.035(2) 0.031(2) 0.036(2) -0.0047(18) 0.0013(18) -0.0022(18) C22 0.031(2) 0.044(3) 0.032(2) 0.004(2) 0.0049(18) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt N2 1.925(3) . ? Pt N3 2.019(4) . ? Pt N1 2.022(4) . ? Pt N4 2.023(4) . ? Sb F2 1.847(3) . ? Sb F6 1.853(4) . ? Sb F3 1.868(3) . ? Sb F4 1.873(3) . ? Sb F1 1.875(3) . ? Sb F5 1.882(4) . ? S C22 1.629(5) . ? N1 C1 1.347(6) . ? N1 C5 1.370(5) . ? N2 C10 1.347(5) . ? N2 C6 1.349(5) . ? N3 C15 1.342(5) . ? N3 C11 1.375(5) . ? N4 C22 1.098(6) . ? C1 C2 1.388(7) . ? C1 H1 0.9500 . ? C2 C3 1.380(8) . ? C2 H2 0.9500 . ? C3 C4 1.397(7) . ? C3 H3 0.9500 . ? C4 C5 1.364(6) . ? C4 H4 0.9500 . ? C5 C6 1.479(6) . ? C6 C7 1.371(6) . ? C7 C8 1.415(6) . ? C7 H7 0.9500 . ? C8 C9 1.408(6) . ? C8 C16 1.485(6) . ? C9 C10 1.371(5) . ? C9 H9 0.9500 . ? C10 C11 1.487(6) . ? C11 C12 1.385(6) . ? C12 C13 1.381(7) . ? C12 H12 0.9500 . ? C13 C14 1.388(7) . ? C13 H13 0.9500 . ? C14 C15 1.368(7) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.394(6) . ? C16 C21 1.397(6) . ? C17 C18 1.387(6) . ? C17 H17 0.9500 . ? C18 C19 1.380(7) . ? C18 H18 0.9500 . ? C19 C20 1.387(7) . ? C19 H19 0.9500 . ? C20 C21 1.390(7) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? 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 81.34(14) . . ? N2 Pt N1 80.74(14) . . ? N3 Pt N1 162.07(14) . . ? N2 Pt N4 179.64(15) . . ? N3 Pt N4 99.02(15) . . ? N1 Pt N4 98.89(14) . . ? F2 Sb F6 91.0(2) . . ? F2 Sb F3 92.0(2) . . ? F6 Sb F3 90.3(2) . . ? F2 Sb F4 177.9(2) . . ? F6 Sb F4 90.18(19) . . ? F3 Sb F4 89.72(16) . . ? F2 Sb F1 89.8(2) . . ? F6 Sb F1 91.1(2) . . ? F3 Sb F1 177.73(19) . . ? F4 Sb F1 88.45(17) . . ? F2 Sb F5 90.2(2) . . ? F6 Sb F5 178.8(2) . . ? F3 Sb F5 89.65(18) . . ? F4 Sb F5 88.57(17) . . ? F1 Sb F5 88.96(18) . . ? C1 N1 C5 119.7(4) . . ? C1 N1 Pt 126.8(3) . . ? C5 N1 Pt 113.5(3) . . ? C10 N2 C6 122.2(3) . . ? C10 N2 Pt 118.8(3) . . ? C6 N2 Pt 119.0(3) . . ? C15 N3 C11 119.0(4) . . ? C15 N3 Pt 128.1(3) . . ? C11 N3 Pt 112.9(3) . . ? C22 N4 Pt 173.1(4) . . ? N1 C1 C2 121.0(5) . . ? N1 C1 H1 119.5 . . ? C2 C1 H1 119.5 . . ? C3 C2 C1 119.7(4) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 118.7(5) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C5 C4 C3 119.9(4) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 N1 121.0(4) . . ? C4 C5 C6 124.6(4) . . ? N1 C5 C6 114.5(4) . . ? N2 C6 C7 119.8(4) . . ? N2 C6 C5 112.3(4) . . ? C7 C6 C5 127.9(4) . . ? C6 C7 C8 120.4(4) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C9 C8 C7 117.2(3) . . ? C9 C8 C16 121.6(4) . . ? C7 C8 C16 121.3(4) . . ? C10 C9 C8 120.4(4) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? N2 C10 C9 120.0(4) . . ? N2 C10 C11 112.0(3) . . ? C9 C10 C11 127.9(4) . . ? N3 C11 C12 120.6(4) . . ? N3 C11 C10 114.9(4) . . ? C12 C11 C10 124.5(4) . . ? C13 C12 C11 119.6(4) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C12 C13 C14 119.2(5) . . ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4 . . ? C15 C14 C13 119.3(4) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? N3 C15 C14 122.4(4) . . ? N3 C15 H15 118.8 . . ? C14 C15 H15 118.8 . . ? C17 C16 C21 118.3(4) . . ? C17 C16 C8 120.6(4) . . ? C21 C16 C8 121.1(4) . . ? C18 C17 C16 120.7(4) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C19 C18 C17 120.9(4) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C18 C19 C20 118.8(4) . . ? C18 C19 H19 120.6 . . ? C20 C19 H19 120.6 . . ? C19 C20 C21 120.8(4) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C20 C21 C16 120.4(4) . . ? C20 C21 H21 119.8 . . ? C16 C21 H21 119.8 . . ? N4 C22 S 179.5(5) . . ? _diffrn_measured_fraction_theta_max 0.864 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.865 _refine_diff_density_min -1.509 _refine_diff_density_rms 0.197 # Attachment '8519_web_deposit_cif_file_1_JohnField_1323158265.1_2nd.cif' # B. P. Waldron MSc, University of KwaZulu-Natal, 2008 data_1_2nd _database_code_depnum_ccdc_archive 'CCDC 857049' #TrackingRef '8519_web_deposit_cif_file_1_JohnField_1323158265.1_2nd.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Pt{4'-(Ph)trpy}(NCS)]SbF6 (1): this crystal was obtained by allowing acetonitrile to escape from the single crystal of 1.MeCN obtained by exposing the single crystal 1_1st to aectonitrile vapours. As such it is the 2nd crystal strcuture determination of 1 using the original crystal. ; _chemical_name_common "[Pt{4'-(Ph)trpy}(NCS)]SbF6" _chemical_melting_point ? _chemical_formula_moiety 'C22 H15 N4 Pt S, F6 Sb' _chemical_formula_sum 'C22 H15 F6 N4 Pt S Sb' _chemical_formula_weight 798.28 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 _symmetry_space_group_name_Hall '-P 2yn' 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 9.6202(3) _cell_length_b 25.5918(10) _cell_length_c 10.3137(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.467(3) _cell_angle_gamma 90.00 _cell_volume 2523.06(16) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used >200 _cell_measurement_theta_min 4 _cell_measurement_theta_max 32 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.102 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 6.754 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0895 _exptl_absorpt_correction_T_max 0.3618 _exptl_absorpt_process_details 'Crysalis 170 RED' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur CCD' _diffrn_measurement_method 'omega 2 theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39798 _diffrn_reflns_av_R_equivalents 0.0682 _diffrn_reflns_av_sigmaI/netI 0.1196 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.64 _diffrn_reflns_theta_max 34.26 _reflns_number_total 9266 _reflns_number_gt 5163 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crysalis 170 CCD' _computing_cell_refinement 'Crysalis 170 CCD' _computing_data_reduction 'Crysalis 170 CCD' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-seed (Barbour, 2006)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.0289P)^2^+7.2219P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9266 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1264 _refine_ls_R_factor_gt 0.0598 _refine_ls_wR_factor_ref 0.1025 _refine_ls_wR_factor_gt 0.0942 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt 0.52251(3) 0.028243(10) 0.84629(2) 0.02780(7) Uani 1 1 d . . . Sb Sb 0.28439(5) 0.313433(18) 0.08859(5) 0.03958(13) Uani 1 1 d . . . S S 0.9708(2) 0.09449(11) 0.9986(2) 0.0663(7) Uani 1 1 d . . . F1 F 0.3730(5) 0.37834(17) 0.1119(5) 0.0752(16) Uani 1 1 d . . . F2 F 0.1133(5) 0.3466(2) 0.0530(6) 0.0853(18) Uani 1 1 d . . . F3 F 0.2026(5) 0.24759(18) 0.0627(6) 0.0722(15) Uani 1 1 d . . . F4 F 0.4601(4) 0.28173(18) 0.1212(5) 0.0625(13) Uani 1 1 d . . . F5 F 0.3112(5) 0.31608(18) -0.0888(5) 0.0649(13) Uani 1 1 d . . . F6 F 0.2618(6) 0.3101(2) 0.2638(5) 0.0887(17) Uani 1 1 d . . . N1 N 0.4302(5) 0.0992(2) 0.8307(5) 0.0266(11) Uani 1 1 d . . . N2 N 0.3354(5) 0.00616(19) 0.7840(5) 0.0221(10) Uani 1 1 d . . . N3 N 0.5569(5) -0.0493(2) 0.8387(5) 0.0273(12) Uani 1 1 d . . . N4 N 0.7166(5) 0.0516(2) 0.9119(5) 0.0322(12) Uani 1 1 d . . . C1 C 0.4893(8) 0.1459(3) 0.8528(7) 0.0410(18) Uani 1 1 d . . . H1 H 0.5868 0.1479 0.8803 0.049 Uiso 1 1 calc R . . C2 C 0.4129(8) 0.1913(3) 0.8369(7) 0.0424(18) Uani 1 1 d . . . H2 H 0.4577 0.2241 0.8531 0.051 Uiso 1 1 calc R . . C3 C 0.2719(8) 0.1892(3) 0.7976(7) 0.0413(17) Uani 1 1 d . . . H3 H 0.2182 0.2203 0.7862 0.050 Uiso 1 1 calc R . . C4 C 0.2095(7) 0.1410(3) 0.7750(6) 0.0339(15) Uani 1 1 d . . . H4 H 0.1117 0.1389 0.7491 0.041 Uiso 1 1 calc R . . C5 C 0.2876(6) 0.0963(2) 0.7895(6) 0.0243(13) Uani 1 1 d . . . C6 C 0.2351(7) 0.0429(2) 0.7622(6) 0.0254(13) Uani 1 1 d . . . C7 C 0.1011(6) 0.0278(2) 0.7158(5) 0.0248(12) Uani 1 1 d . . . H7 H 0.0295 0.0533 0.7003 0.030 Uiso 1 1 calc R . . C8 C 0.0698(6) -0.0254(2) 0.6910(5) 0.0229(12) Uani 1 1 d . . . C9 C 0.1788(6) -0.0612(2) 0.7160(6) 0.0247(13) Uani 1 1 d . . . H9 H 0.1617 -0.0973 0.7003 0.030 Uiso 1 1 calc R . . C10 C 0.3102(6) -0.0447(2) 0.7628(6) 0.0236(13) Uani 1 1 d . . . C11 C 0.4370(6) -0.0770(3) 0.7951(6) 0.0280(14) Uani 1 1 d . . . C12 C 0.4415(7) -0.1303(3) 0.7859(7) 0.0358(16) Uani 1 1 d . . . H12 H 0.3587 -0.1491 0.7572 0.043 Uiso 1 1 calc R . . C13 C 0.5656(7) -0.1570(3) 0.8181(7) 0.0436(19) Uani 1 1 d . . . H13 H 0.5693 -0.1939 0.8102 0.052 Uiso 1 1 calc R . . C14 C 0.6835(7) -0.1289(3) 0.8618(7) 0.0388(17) Uani 1 1 d . . . H14 H 0.7701 -0.1461 0.8854 0.047 Uiso 1 1 calc R . . C15 C 0.6743(6) -0.0759(3) 0.8707(6) 0.0295(14) Uani 1 1 d . . . H15 H 0.7563 -0.0570 0.9016 0.035 Uiso 1 1 calc R . . C16 C -0.0733(6) -0.0414(3) 0.6354(6) 0.0278(14) Uani 1 1 d . . . C17 C -0.1816(6) -0.0050(3) 0.6127(6) 0.0315(15) Uani 1 1 d . . . H17 H -0.1646 0.0307 0.6340 0.038 Uiso 1 1 calc R . . C18 C -0.3133(6) -0.0207(3) 0.5594(6) 0.0321(15) Uani 1 1 d . . . H18 H -0.3856 0.0046 0.5440 0.039 Uiso 1 1 calc R . . C19 C -0.3417(7) -0.0718(3) 0.5285(6) 0.0355(16) Uani 1 1 d . . . H19 H -0.4325 -0.0819 0.4912 0.043 Uiso 1 1 calc R . . C20 C -0.2366(8) -0.1088(3) 0.5522(7) 0.0426(18) Uani 1 1 d . . . H20 H -0.2555 -0.1445 0.5318 0.051 Uiso 1 1 calc R . . C21 C -0.1041(7) -0.0938(3) 0.6056(6) 0.0353(16) Uani 1 1 d . . . H21 H -0.0330 -0.1195 0.6223 0.042 Uiso 1 1 calc R . . C22 C 0.8218(6) 0.0686(3) 0.9462(6) 0.0333(15) 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 0.02259(11) 0.03381(13) 0.02631(12) -0.00297(12) -0.00029(8) -0.00266(12) Sb 0.0355(3) 0.0315(3) 0.0502(3) -0.0016(2) -0.0016(2) 0.0046(2) S 0.0338(10) 0.108(2) 0.0540(14) 0.0080(13) -0.0079(10) -0.0307(12) F1 0.082(4) 0.033(3) 0.106(4) -0.013(3) -0.006(3) -0.006(2) F2 0.051(3) 0.083(4) 0.119(5) -0.001(3) -0.004(3) 0.035(3) F3 0.055(3) 0.052(3) 0.107(4) 0.003(3) -0.003(3) -0.016(2) F4 0.039(3) 0.054(3) 0.091(4) 0.004(2) -0.005(2) 0.009(2) F5 0.079(3) 0.060(3) 0.054(3) 0.005(2) 0.000(3) 0.004(3) F6 0.090(4) 0.117(5) 0.063(4) -0.001(3) 0.022(3) 0.019(4) N1 0.025(3) 0.033(3) 0.022(3) -0.005(2) 0.004(2) -0.003(2) N2 0.017(2) 0.029(3) 0.020(3) -0.002(2) 0.0026(19) -0.003(2) N3 0.024(3) 0.037(3) 0.022(3) 0.005(2) 0.007(2) 0.000(2) N4 0.024(3) 0.036(3) 0.035(3) -0.006(2) 0.000(2) -0.005(2) C1 0.044(4) 0.037(4) 0.040(4) -0.009(3) -0.001(4) -0.003(3) C2 0.047(4) 0.029(4) 0.052(5) -0.005(3) 0.008(4) -0.007(3) C3 0.050(4) 0.032(4) 0.042(4) -0.007(3) 0.006(3) 0.004(3) C4 0.032(4) 0.039(4) 0.030(4) -0.002(3) 0.002(3) 0.000(3) C5 0.025(3) 0.029(3) 0.019(3) -0.004(2) 0.004(2) -0.004(3) C6 0.032(3) 0.023(3) 0.021(3) -0.001(2) 0.002(3) 0.000(3) C7 0.022(3) 0.031(3) 0.022(3) 0.000(3) 0.002(2) 0.002(3) C8 0.020(3) 0.036(3) 0.014(3) 0.000(3) 0.005(2) -0.006(3) C9 0.026(3) 0.023(3) 0.025(3) 0.001(2) 0.002(2) -0.005(3) C10 0.023(3) 0.022(3) 0.026(3) 0.005(2) 0.002(2) 0.000(2) C11 0.023(3) 0.040(4) 0.021(3) 0.002(3) 0.003(2) -0.004(3) C12 0.029(3) 0.033(4) 0.044(4) 0.007(3) -0.001(3) 0.000(3) C13 0.040(4) 0.033(4) 0.055(5) 0.006(3) -0.008(4) 0.006(3) C14 0.040(4) 0.042(4) 0.033(4) 0.009(3) -0.002(3) 0.009(3) C15 0.018(3) 0.043(4) 0.026(3) 0.006(3) -0.002(2) 0.001(3) C16 0.017(3) 0.039(4) 0.027(3) 0.004(3) 0.002(2) -0.002(3) C17 0.022(3) 0.041(4) 0.030(4) -0.004(3) 0.001(3) -0.005(3) C18 0.020(3) 0.042(4) 0.034(4) 0.001(3) 0.001(3) -0.002(3) C19 0.021(3) 0.057(5) 0.027(4) 0.004(3) -0.003(3) -0.007(3) C20 0.047(4) 0.048(4) 0.032(4) -0.017(3) 0.000(3) -0.020(4) C21 0.034(4) 0.039(4) 0.033(4) -0.003(3) 0.004(3) 0.001(3) C22 0.021(3) 0.046(4) 0.034(4) 0.006(3) 0.005(3) 0.000(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt N2 1.927(5) . ? Pt N4 2.004(5) . ? Pt N3 2.016(5) . ? Pt N1 2.020(5) . ? Sb F2 1.852(4) . ? Sb F6 1.846(5) . ? Sb F3 1.866(4) . ? Sb F4 1.871(4) . ? Sb F1 1.870(4) . ? Sb F5 1.878(5) . ? S C22 1.615(7) . ? N1 C1 1.332(8) . ? N1 C5 1.392(7) . ? N2 C10 1.338(7) . ? N2 C6 1.347(7) . ? N3 C15 1.328(7) . ? N3 C11 1.385(8) . ? N4 C22 1.122(8) . ? C1 C2 1.375(10) . ? C1 H1 0.9500 . ? C2 C3 1.372(10) . ? C2 H2 0.9500 . ? C3 C4 1.380(9) . ? C3 H3 0.9500 . ? C4 C5 1.368(9) . ? C4 H4 0.9500 . ? C5 C6 1.474(8) . ? C6 C7 1.378(8) . ? C7 C8 1.410(8) . ? C7 H7 0.9500 . ? C8 C9 1.395(8) . ? C8 C16 1.488(8) . ? C9 C10 1.368(8) . ? C9 H9 0.9500 . ? C10 C11 1.480(8) . ? C11 C12 1.367(9) . ? C12 C13 1.383(9) . ? C12 H12 0.9500 . ? C13 C14 1.376(10) . ? C13 H13 0.9500 . ? C14 C15 1.362(9) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.397(9) . ? C16 C21 1.401(9) . ? C17 C18 1.383(8) . ? C17 H17 0.9500 . ? C18 C19 1.367(9) . ? C18 H18 0.9500 . ? C19 C20 1.387(10) . ? C19 H19 0.9500 . ? C20 C21 1.385(9) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? 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 N4 179.6(2) . . ? N2 Pt N3 81.4(2) . . ? N4 Pt N3 99.0(2) . . ? N2 Pt N1 81.4(2) . . ? N4 Pt N1 98.2(2) . . ? N3 Pt N1 162.76(19) . . ? F2 Sb F6 90.9(3) . . ? F2 Sb F3 92.0(2) . . ? F6 Sb F3 90.2(3) . . ? F2 Sb F4 178.0(3) . . ? F6 Sb F4 90.4(2) . . ? F3 Sb F4 89.5(2) . . ? F2 Sb F1 90.0(2) . . ? F6 Sb F1 91.0(3) . . ? F3 Sb F1 177.6(2) . . ? F4 Sb F1 88.4(2) . . ? F2 Sb F5 90.4(2) . . ? F6 Sb F5 178.7(2) . . ? F3 Sb F5 89.7(2) . . ? F4 Sb F5 88.3(2) . . ? F1 Sb F5 89.0(2) . . ? C1 N1 C5 119.2(6) . . ? C1 N1 Pt 128.1(4) . . ? C5 N1 Pt 112.7(4) . . ? C10 N2 C6 122.6(5) . . ? C10 N2 Pt 119.0(4) . . ? C6 N2 Pt 118.4(4) . . ? C15 N3 C11 118.2(6) . . ? C15 N3 Pt 129.3(4) . . ? C11 N3 Pt 112.4(4) . . ? C22 N4 Pt 174.5(6) . . ? N1 C1 C2 121.7(7) . . ? N1 C1 H1 119.1 . . ? C2 C1 H1 119.1 . . ? C3 C2 C1 119.9(7) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 118.8(7) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C5 C4 C3 120.4(6) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 N1 119.9(5) . . ? C4 C5 C6 125.7(5) . . ? N1 C5 C6 114.4(5) . . ? N2 C6 C7 119.1(5) . . ? N2 C6 C5 113.0(5) . . ? C7 C6 C5 127.8(6) . . ? C6 C7 C8 120.4(5) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C9 C8 C7 117.3(5) . . ? C9 C8 C16 122.3(5) . . ? C7 C8 C16 120.3(5) . . ? C10 C9 C8 120.6(5) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? N2 C10 C9 120.0(5) . . ? N2 C10 C11 112.2(5) . . ? C9 C10 C11 127.8(6) . . ? C12 C11 N3 120.0(6) . . ? C12 C11 C10 125.0(6) . . ? N3 C11 C10 115.0(5) . . ? C11 C12 C13 120.6(6) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C14 C13 C12 118.5(7) . . ? C14 C13 H13 120.7 . . ? C12 C13 H13 120.7 . . ? C15 C14 C13 119.0(6) . . ? C15 C14 H14 120.5 . . ? C13 C14 H14 120.5 . . ? N3 C15 C14 123.6(6) . . ? N3 C15 H15 118.2 . . ? C14 C15 H15 118.2 . . ? C17 C16 C21 117.8(6) . . ? C17 C16 C8 121.4(6) . . ? C21 C16 C8 120.8(6) . . ? C18 C17 C16 120.4(6) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C19 C18 C17 121.4(6) . . ? C19 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? C18 C19 C20 119.4(6) . . ? C18 C19 H19 120.3 . . ? C20 C19 H19 120.3 . . ? C19 C20 C21 120.0(6) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C20 C21 C16 121.1(6) . . ? C20 C21 H21 119.5 . . ? C16 C21 H21 119.5 . . ? N4 C22 S 178.1(7) . . ? _diffrn_measured_fraction_theta_max 0.882 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 3.067 _refine_diff_density_min -1.230 _refine_diff_density_rms 0.183 # Attachment '8520_web_deposit_cif_file_2_JohnField_1323158265.1_3rd.cif' # B. P. Waldron MSc, University of KwaZulu-Natal, 2008 data_1_desacetone _database_code_depnum_ccdc_archive 'CCDC 857050' #TrackingRef '8520_web_deposit_cif_file_2_JohnField_1323158265.1_3rd.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; This is the crystal of [Pt{4'-(Ph)trpy}(NCS)]SbF6 (1) obtained after allowing acetone to escape from the single crystal of 1.(CH3)2CO obtained by direct crystallisation from acetone. It is the 3rd crystal structure determination of 1. ; _chemical_name_common "[Pt{4'-(Ph)trpy}(NCS)]SbF6" _chemical_melting_point ? _chemical_formula_moiety 'C22 H15 N4 Pt S, F6 Sb' _chemical_formula_sum 'C22 H15 F6 N4 Pt S Sb' _chemical_formula_weight 798.28 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 _symmetry_space_group_name_Hall '-P 2yn' 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 9.6020(8) _cell_length_b 25.593(2) _cell_length_c 10.2134(9) _cell_angle_alpha 90.00 _cell_angle_beta 96.301(7) _cell_angle_gamma 90.00 _cell_volume 2494.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used >200 _cell_measurement_theta_min 4 _cell_measurement_theta_max 32 _exptl_crystal_description 'irregular block' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.125 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 6.831 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2150 _exptl_absorpt_correction_T_max 0.5044 _exptl_absorpt_process_details 'Crysalis 170 RED' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur CCD' _diffrn_measurement_method 'omega 2 theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39592 _diffrn_reflns_av_R_equivalents 0.1478 _diffrn_reflns_av_sigmaI/netI 0.1910 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.65 _diffrn_reflns_theta_max 34.17 _reflns_number_total 9134 _reflns_number_gt 4578 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crysalis 170 CCD' _computing_cell_refinement 'Crysalis 170 CCD' _computing_data_reduction 'Crysalis 170 CCD' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-seed (Barbour, 2006)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.1011P)^2^+25.9945P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9134 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1663 _refine_ls_R_factor_gt 0.0844 _refine_ls_wR_factor_ref 0.2183 _refine_ls_wR_factor_gt 0.1927 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.961 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt 0.52321(5) 0.027854(19) 0.84612(4) 0.02095(13) Uani 1 1 d . . . Sb Sb 0.28762(9) 0.31324(3) 0.08846(9) 0.0285(2) Uani 1 1 d . . . S S 0.9711(4) 0.09531(19) 1.0000(4) 0.0474(11) Uani 1 1 d . . . F1 F 0.3730(10) 0.3787(3) 0.1126(10) 0.049(2) Uani 1 1 d . . . F2 F 0.1140(9) 0.3463(4) 0.0507(11) 0.058(3) Uani 1 1 d . . . F3 F 0.2061(9) 0.2481(3) 0.0646(10) 0.048(2) Uani 1 1 d . . . F4 F 0.4642(8) 0.2815(3) 0.1229(9) 0.039(2) Uani 1 1 d . . . F5 F 0.3150(10) 0.3162(3) -0.0906(8) 0.045(2) Uani 1 1 d . . . F6 F 0.2657(10) 0.3104(4) 0.2671(9) 0.058(3) Uani 1 1 d . . . N1 N 0.4319(10) 0.0986(4) 0.8308(9) 0.020(2) Uani 1 1 d . . . N2 N 0.3363(9) 0.0058(3) 0.7837(8) 0.0144(17) Uani 1 1 d . . . N3 N 0.5588(10) -0.0495(4) 0.8374(9) 0.023(2) Uani 1 1 d . . . N4 N 0.7190(10) 0.0516(4) 0.9087(10) 0.021(2) Uani 1 1 d . . . C1 C 0.4884(15) 0.1448(5) 0.8548(13) 0.033(3) Uani 1 1 d . . . H1 H 0.5851 0.1466 0.8864 0.039 Uiso 1 1 calc R . . C2 C 0.4152(15) 0.1905(5) 0.8366(14) 0.032(3) Uani 1 1 d . . . H2 H 0.4620 0.2232 0.8487 0.039 Uiso 1 1 calc R . . C3 C 0.2736(13) 0.1887(5) 0.8007(12) 0.025(2) Uani 1 1 d . . . H3 H 0.2204 0.2201 0.7920 0.030 Uiso 1 1 calc R . . C4 C 0.2086(13) 0.1407(5) 0.7772(11) 0.027(3) Uani 1 1 d . . . H4 H 0.1105 0.1387 0.7521 0.033 Uiso 1 1 calc R . . C5 C 0.2890(13) 0.0956(5) 0.7911(11) 0.023(2) Uani 1 1 d . . . C6 C 0.2352(12) 0.0430(4) 0.7640(10) 0.017(2) Uani 1 1 d . . . C7 C 0.1007(11) 0.0279(4) 0.7173(9) 0.0155(19) Uani 1 1 d . . . H7 H 0.0290 0.0535 0.7033 0.019 Uiso 1 1 calc R . . C8 C 0.0682(11) -0.0251(4) 0.6902(10) 0.017(2) Uani 1 1 d . . . C9 C 0.1772(11) -0.0616(4) 0.7158(11) 0.018(2) Uani 1 1 d . . . H9 H 0.1596 -0.0978 0.7022 0.022 Uiso 1 1 calc R . . C10 C 0.3098(12) -0.0445(4) 0.7605(11) 0.017(2) Uani 1 1 d . . . C11 C 0.4379(11) -0.0777(5) 0.7944(11) 0.019(2) Uani 1 1 d . . . C12 C 0.4419(14) -0.1301(5) 0.7840(12) 0.031(3) Uani 1 1 d . . . H12 H 0.3589 -0.1487 0.7538 0.037 Uiso 1 1 calc R . . C13 C 0.5676(14) -0.1576(5) 0.8174(13) 0.030(3) Uani 1 1 d . . . H13 H 0.5713 -0.1946 0.8114 0.036 Uiso 1 1 calc R . . C14 C 0.6844(14) -0.1288(5) 0.8588(12) 0.027(3) Uani 1 1 d . . . H14 H 0.7723 -0.1456 0.8795 0.033 Uiso 1 1 calc R . . C15 C 0.6737(13) -0.0757(5) 0.8700(11) 0.022(2) Uani 1 1 d . . . H15 H 0.7550 -0.0568 0.9037 0.026 Uiso 1 1 calc R . . C16 C -0.0727(12) -0.0413(5) 0.6331(12) 0.022(2) Uani 1 1 d . . . C17 C -0.1819(12) -0.0043(5) 0.6125(11) 0.023(2) Uani 1 1 d . . . H17 H -0.1653 0.0313 0.6360 0.028 Uiso 1 1 calc R . . C18 C -0.3141(12) -0.0204(5) 0.5575(11) 0.025(3) Uani 1 1 d . . . H18 H -0.3865 0.0048 0.5404 0.030 Uiso 1 1 calc R . . C19 C -0.3419(12) -0.0717(5) 0.5276(11) 0.024(3) Uani 1 1 d . . . H19 H -0.4335 -0.0817 0.4916 0.029 Uiso 1 1 calc R . . C20 C -0.2394(13) -0.1088(5) 0.5489(12) 0.027(3) Uani 1 1 d . . . H20 H -0.2596 -0.1443 0.5277 0.032 Uiso 1 1 calc R . . C21 C -0.1025(13) -0.0938(5) 0.6029(12) 0.024(3) Uani 1 1 d . . . H21 H -0.0311 -0.1194 0.6186 0.029 Uiso 1 1 calc R . . C22 C 0.8214(12) 0.0687(5) 0.9466(12) 0.023(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt 0.0163(2) 0.0250(2) 0.0208(2) -0.00142(19) -0.00140(14) -0.00152(19) Sb 0.0237(4) 0.0239(4) 0.0365(5) -0.0010(3) -0.0024(3) 0.0030(3) S 0.0250(17) 0.077(3) 0.039(2) 0.0065(19) -0.0060(15) -0.0240(18) F1 0.052(6) 0.029(5) 0.066(6) -0.006(4) 0.001(5) -0.007(4) F2 0.027(5) 0.046(6) 0.098(8) 0.003(5) -0.010(5) 0.019(4) F3 0.040(5) 0.040(5) 0.064(6) 0.009(4) 0.005(4) 0.002(4) F4 0.021(4) 0.034(5) 0.059(5) -0.001(4) -0.009(4) 0.007(3) F5 0.060(6) 0.037(5) 0.037(5) 0.004(4) 0.005(4) -0.001(4) F6 0.052(6) 0.085(8) 0.038(5) -0.002(5) 0.013(4) 0.005(5) N1 0.019(5) 0.029(5) 0.013(4) -0.009(4) 0.010(4) -0.010(4) N2 0.015(4) 0.013(4) 0.015(4) -0.005(3) 0.003(3) 0.000(3) N3 0.015(4) 0.041(6) 0.013(4) -0.010(4) 0.005(4) 0.000(4) N4 0.019(5) 0.017(5) 0.027(5) -0.010(4) 0.004(4) -0.001(4) C1 0.032(7) 0.031(7) 0.035(7) -0.013(6) 0.003(6) 0.000(6) C2 0.038(8) 0.015(6) 0.044(8) -0.001(5) 0.005(6) -0.004(5) C3 0.031(6) 0.015(6) 0.027(6) 0.002(4) -0.003(5) 0.002(5) C4 0.024(6) 0.037(7) 0.019(6) 0.001(5) -0.004(5) 0.001(5) C5 0.024(6) 0.029(7) 0.017(5) -0.002(4) -0.004(4) -0.008(5) C6 0.022(5) 0.014(5) 0.015(5) -0.005(4) -0.003(4) 0.002(4) C7 0.018(5) 0.017(5) 0.012(4) -0.001(4) 0.003(4) 0.003(4) C8 0.016(5) 0.021(5) 0.015(5) -0.001(4) 0.002(4) -0.002(4) C9 0.015(5) 0.016(5) 0.024(5) -0.002(4) 0.001(4) 0.006(4) C10 0.021(5) 0.007(4) 0.022(5) 0.005(4) 0.003(4) 0.006(4) C11 0.010(5) 0.023(6) 0.026(6) 0.004(4) 0.001(4) -0.003(4) C12 0.029(7) 0.036(8) 0.025(6) -0.003(5) -0.007(5) -0.004(6) C13 0.039(7) 0.014(6) 0.034(7) 0.004(5) -0.006(6) 0.004(5) C14 0.028(6) 0.028(7) 0.024(6) 0.006(5) -0.007(5) -0.001(5) C15 0.021(5) 0.025(6) 0.018(5) 0.002(4) -0.003(4) -0.006(5) C16 0.016(5) 0.023(6) 0.027(6) 0.011(4) 0.001(4) -0.003(4) C17 0.017(5) 0.028(7) 0.024(6) 0.001(5) -0.003(4) -0.003(5) C18 0.016(5) 0.035(7) 0.022(6) 0.001(5) -0.002(4) -0.002(5) C19 0.015(5) 0.044(8) 0.012(5) -0.004(5) 0.001(4) -0.010(5) C20 0.031(7) 0.023(6) 0.023(6) -0.009(5) -0.006(5) -0.002(5) C21 0.022(6) 0.027(6) 0.024(6) 0.000(5) 0.003(5) 0.011(5) C22 0.017(6) 0.026(6) 0.025(6) 0.004(5) 0.001(4) -0.001(5) _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 1.923(9) . ? Pt N1 2.009(10) . ? Pt N4 2.012(10) . ? Pt N3 2.013(11) . ? Sb F3 1.848(9) . ? Sb F6 1.861(9) . ? Sb F1 1.870(8) . ? Sb F2 1.871(8) . ? Sb F5 1.878(8) . ? Sb F4 1.879(7) . ? S C22 1.630(12) . ? N1 C1 1.315(16) . ? N1 C5 1.389(15) . ? N2 C10 1.327(14) . ? N2 C6 1.359(14) . ? N3 C15 1.303(15) . ? N3 C11 1.396(14) . ? N4 C22 1.107(14) . ? C1 C2 1.367(18) . ? C1 H1 0.9500 . ? C2 C3 1.369(18) . ? C2 H2 0.9500 . ? C3 C4 1.387(17) . ? C3 H3 0.9500 . ? C4 C5 1.387(18) . ? C4 H4 0.9500 . ? C5 C6 1.458(16) . ? C6 C7 1.382(15) . ? C7 C8 1.412(15) . ? C7 H7 0.9500 . ? C8 C9 1.405(15) . ? C8 C16 1.473(16) . ? C9 C10 1.376(15) . ? C9 H9 0.9500 . ? C10 C11 1.504(15) . ? C11 C12 1.346(18) . ? C12 C13 1.406(18) . ? C12 H12 0.9500 . ? C13 C14 1.370(18) . ? C13 H13 0.9500 . ? C14 C15 1.367(17) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C21 1.401(17) . ? C16 C17 1.412(17) . ? C17 C18 1.393(16) . ? C17 H17 0.9500 . ? C18 C19 1.368(17) . ? C18 H18 0.9500 . ? C19 C20 1.367(18) . ? C19 H19 0.9500 . ? C20 C21 1.422(17) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? 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 81.7(4) . . ? N2 Pt N4 179.1(4) . . ? N1 Pt N4 97.9(4) . . ? N2 Pt N3 81.5(4) . . ? N1 Pt N3 163.1(4) . . ? N4 Pt N3 98.8(4) . . ? F3 Sb F6 90.1(5) . . ? F3 Sb F1 179.1(4) . . ? F6 Sb F1 90.0(5) . . ? F3 Sb F2 91.5(4) . . ? F6 Sb F2 91.5(5) . . ? F1 Sb F2 89.5(4) . . ? F3 Sb F5 90.6(4) . . ? F6 Sb F5 178.5(4) . . ? F1 Sb F5 89.2(4) . . ? F2 Sb F5 89.9(5) . . ? F3 Sb F4 89.7(4) . . ? F6 Sb F4 89.8(4) . . ? F1 Sb F4 89.4(4) . . ? F2 Sb F4 178.3(4) . . ? F5 Sb F4 88.8(4) . . ? C1 N1 C5 118.5(11) . . ? C1 N1 Pt 129.0(9) . . ? C5 N1 Pt 112.5(8) . . ? C10 N2 C6 122.2(9) . . ? C10 N2 Pt 119.8(7) . . ? C6 N2 Pt 117.9(7) . . ? C15 N3 C11 117.8(11) . . ? C15 N3 Pt 129.6(9) . . ? C11 N3 Pt 112.5(8) . . ? C22 N4 Pt 173.7(10) . . ? N1 C1 C2 123.3(13) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C1 C2 C3 119.2(12) . . ? C1 C2 H2 120.4 . . ? C3 C2 H2 120.4 . . ? C2 C3 C4 119.4(11) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 119.0(11) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C4 C5 N1 120.4(11) . . ? C4 C5 C6 124.6(11) . . ? N1 C5 C6 115.0(11) . . ? N2 C6 C7 118.7(10) . . ? N2 C6 C5 112.8(10) . . ? C7 C6 C5 128.5(10) . . ? C6 C7 C8 121.0(10) . . ? C6 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? C9 C8 C7 117.2(10) . . ? C9 C8 C16 121.3(10) . . ? C7 C8 C16 121.4(10) . . ? C10 C9 C8 119.6(10) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? N2 C10 C9 121.3(10) . . ? N2 C10 C11 111.8(10) . . ? C9 C10 C11 126.8(10) . . ? C12 C11 N3 120.6(11) . . ? C12 C11 C10 125.1(10) . . ? N3 C11 C10 114.2(10) . . ? C11 C12 C13 120.7(12) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C14 C13 C12 117.2(12) . . ? C14 C13 H13 121.4 . . ? C12 C13 H13 121.4 . . ? C15 C14 C13 119.6(12) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? N3 C15 C14 124.0(11) . . ? N3 C15 H15 118.0 . . ? C14 C15 H15 118.0 . . ? C21 C16 C17 118.7(11) . . ? C21 C16 C8 120.9(11) . . ? C17 C16 C8 120.3(11) . . ? C18 C17 C16 119.4(12) . . ? C18 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? C19 C18 C17 121.4(12) . . ? C19 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? C20 C19 C18 120.8(11) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C19 C20 C21 119.6(11) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C16 C21 C20 120.1(11) . . ? C16 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? N4 C22 S 178.4(12) . . ? _diffrn_measured_fraction_theta_max 0.886 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 3.448 _refine_diff_density_min -3.369 _refine_diff_density_rms 0.396 # Attachment '8521_web_deposit_cif_file_3_JohnField_1323158265.1MeCN.cif' # B. P. Waldron MSc, University of KwaZulu-Natal, 2008 data_1mecn_2nd _database_code_depnum_ccdc_archive 'CCDC 857051' #TrackingRef '8521_web_deposit_cif_file_3_JohnField_1323158265.1MeCN.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Pt{4'-(Ph)trpy}(NCS)]SbF6.MeCN (1.MeCN) This crystal was obtained by exposing the single crystal of 1_1st to vapours of acetonitrile. ; _chemical_name_common "[Pt{4'-(Ph)trpy}(NCS)]SbF6.CH3CN" _chemical_melting_point ? _chemical_formula_moiety 'C22 H15 N4 Pt S, F6 Sb, C2 H3 N' _chemical_formula_sum 'C24 H18 F6 N5 Pt S Sb' _chemical_formula_weight 839.33 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 _symmetry_space_group_name_Hall '-P 2yn' 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 9.9301(2) _cell_length_b 25.7960(9) _cell_length_c 10.347(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.060(2) _cell_angle_gamma 90.00 _cell_volume 2609.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used >200 _cell_measurement_theta_min 4 _cell_measurement_theta_max 32 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.136 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 6.537 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0943 _exptl_absorpt_correction_T_max 0.3744 _exptl_absorpt_process_details 'Crysalis 170 RED' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur CCD' _diffrn_measurement_method 'omega 2 theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38184 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_sigmaI/netI 0.0602 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 34.00 _reflns_number_total 8961 _reflns_number_gt 5626 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crysalis 170 CCD' _computing_cell_refinement 'Crysalis 170 CCD' _computing_data_reduction 'Crysalis 170 CCD' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-seed (Barbour, 2006)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.0500P)^2^+88.7041P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8961 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1427 _refine_ls_R_factor_gt 0.0803 _refine_ls_wR_factor_ref 0.2107 _refine_ls_wR_factor_gt 0.1776 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt 0.51795(4) 0.026982(18) 0.84777(4) 0.03062(13) Uani 1 1 d . . . Sb Sb 0.78089(12) 0.18238(4) 0.59453(12) 0.0539(3) Uani 1 1 d . . . S S 0.9740(4) 0.0843(2) 0.9950(4) 0.0611(11) Uani 1 1 d . . . F1 F 0.8263(13) 0.1862(4) 0.4228(11) 0.081(3) Uani 1 1 d . . . F2 F 0.7211(13) 0.2507(4) 0.5806(15) 0.095(4) Uani 1 1 d . . . F3 F 0.9531(11) 0.2096(5) 0.6654(13) 0.085(4) Uani 1 1 d . . . F4 F 0.8617(15) 0.1182(5) 0.6109(16) 0.110(5) Uani 1 1 d . . . F5 F 0.736(2) 0.1775(7) 0.7583(16) 0.141(7) Uani 1 1 d . . . F6 F 0.636(3) 0.1587(5) 0.5287(15) 0.159(9) Uani 1 1 d . . . N1 N 0.4248(10) 0.0959(4) 0.8361(9) 0.032(2) Uani 1 1 d . . . N2 N 0.3339(8) 0.0047(3) 0.7833(7) 0.0191(15) Uani 1 1 d . . . N3 N 0.5551(10) -0.0494(4) 0.8360(9) 0.0302(19) Uani 1 1 d . . . N4 N 0.7090(9) 0.0505(4) 0.9146(8) 0.0259(18) Uani 1 1 d . . . N5 N 0.688(4) 0.2247(14) 1.062(3) 0.179(15) Uani 1 1 d . . . C1 C 0.4789(13) 0.1429(5) 0.8666(14) 0.042(3) Uani 1 1 d . . . H1 H 0.5743 0.1452 0.8992 0.050 Uiso 1 1 calc R . . C2 C 0.4039(15) 0.1874(5) 0.8532(15) 0.045(3) Uani 1 1 d . . . H2 H 0.4484 0.2198 0.8723 0.054 Uiso 1 1 calc R . . C3 C 0.2628(15) 0.1860(5) 0.8118(13) 0.042(3) Uani 1 1 d . . . H3 H 0.2089 0.2167 0.8037 0.051 Uiso 1 1 calc R . . C4 C 0.2050(12) 0.1373(5) 0.7830(12) 0.034(2) Uani 1 1 d . . . H4 H 0.1090 0.1343 0.7549 0.041 Uiso 1 1 calc R . . C5 C 0.2845(11) 0.0937(4) 0.7947(11) 0.028(2) Uani 1 1 d . . . C6 C 0.2337(11) 0.0403(4) 0.7635(10) 0.027(2) Uani 1 1 d . . . C7 C 0.1003(10) 0.0253(5) 0.7157(9) 0.0260(19) Uani 1 1 d . . . H7 H 0.0298 0.0505 0.7003 0.031 Uiso 1 1 calc R . . C8 C 0.0690(9) -0.0274(4) 0.6900(8) 0.0208(17) Uani 1 1 d . . . C9 C 0.1764(11) -0.0628(5) 0.7134(11) 0.031(2) Uani 1 1 d . . . H9 H 0.1592 -0.0987 0.6971 0.037 Uiso 1 1 calc R . . C10 C 0.3081(11) -0.0459(4) 0.7604(10) 0.028(2) Uani 1 1 d . . . C11 C 0.4352(11) -0.0777(5) 0.7918(11) 0.033(2) Uani 1 1 d . . . C12 C 0.4411(14) -0.1305(6) 0.7818(14) 0.045(3) Uani 1 1 d . . . H12 H 0.3599 -0.1497 0.7522 0.054 Uiso 1 1 calc R . . C13 C 0.5652(16) -0.1564(6) 0.8148(15) 0.050(3) Uani 1 1 d . . . H13 H 0.5697 -0.1931 0.8094 0.060 Uiso 1 1 calc R . . C14 C 0.6808(15) -0.1276(6) 0.8551(13) 0.045(3) Uani 1 1 d . . . H14 H 0.7675 -0.1441 0.8741 0.054 Uiso 1 1 calc R . . C15 C 0.6707(12) -0.0748(5) 0.8679(10) 0.033(2) Uani 1 1 d . . . H15 H 0.7512 -0.0558 0.9014 0.040 Uiso 1 1 calc R . . C16 C -0.0712(11) -0.0439(4) 0.6341(10) 0.027(2) Uani 1 1 d . . . C17 C -0.1808(12) -0.0083(5) 0.6156(13) 0.038(3) Uani 1 1 d . . . H17 H -0.1633 0.0267 0.6413 0.045 Uiso 1 1 calc R . . C18 C -0.3113(12) -0.0225(5) 0.5621(11) 0.034(2) Uani 1 1 d . . . H18 H -0.3826 0.0026 0.5500 0.041 Uiso 1 1 calc R . . C19 C -0.3391(13) -0.0741(6) 0.5251(11) 0.041(3) Uani 1 1 d . . . H19 H -0.4298 -0.0844 0.4890 0.049 Uiso 1 1 calc R . . C20 C -0.2370(14) -0.1094(6) 0.5407(11) 0.044(3) Uani 1 1 d . . . H20 H -0.2562 -0.1443 0.5146 0.053 Uiso 1 1 calc R . . C21 C -0.1025(14) -0.0949(5) 0.5953(12) 0.038(3) Uani 1 1 d . . . H21 H -0.0319 -0.1202 0.6059 0.046 Uiso 1 1 calc R . . C22 C 0.8179(12) 0.0647(5) 0.9438(11) 0.034(2) Uani 1 1 d . . . C23 C 0.792(3) 0.2281(12) 1.040(3) 0.125(12) Uani 1 1 d . . . C24 C 0.914(4) 0.2286(18) 1.020(6) 0.25(3) Uani 1 1 d . . . H241 H 0.9228 0.2047 0.9486 0.376 Uiso 1 1 calc R . . H242 H 0.9750 0.2177 1.1003 0.376 Uiso 1 1 calc R . . H243 H 0.9378 0.2637 0.9964 0.376 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 0.02499(18) 0.0359(2) 0.0307(2) -0.0009(2) 0.00428(13) -0.00058(19) Sb 0.0599(6) 0.0370(5) 0.0664(7) 0.0100(5) 0.0156(5) 0.0064(4) S 0.0305(16) 0.096(3) 0.055(2) 0.006(2) 0.0030(15) -0.0202(19) F1 0.096(8) 0.075(7) 0.075(7) 0.005(6) 0.019(6) -0.016(6) F2 0.091(9) 0.049(6) 0.143(12) -0.006(7) 0.009(8) 0.008(6) F3 0.055(6) 0.081(8) 0.111(10) -0.004(7) -0.009(6) -0.007(5) F4 0.122(11) 0.061(7) 0.151(13) 0.039(8) 0.033(10) 0.037(7) F5 0.183(17) 0.155(15) 0.106(11) 0.007(10) 0.079(12) -0.036(13) F6 0.32(3) 0.066(8) 0.089(10) -0.004(8) 0.024(13) 0.069(13) N1 0.028(4) 0.043(6) 0.026(4) 0.005(4) 0.012(4) 0.001(4) N2 0.023(4) 0.029(4) 0.006(3) 0.001(3) 0.003(3) -0.003(3) N3 0.035(5) 0.031(5) 0.026(4) 0.003(4) 0.011(4) 0.003(4) N4 0.023(4) 0.038(5) 0.018(4) -0.005(4) 0.007(3) -0.003(4) N5 0.16(3) 0.21(3) 0.18(3) -0.10(3) 0.06(2) -0.10(3) C1 0.035(6) 0.042(7) 0.053(8) -0.009(6) 0.020(6) -0.009(5) C2 0.049(8) 0.030(6) 0.056(8) -0.009(6) 0.012(6) -0.012(6) C3 0.053(8) 0.034(6) 0.043(7) -0.002(6) 0.019(6) -0.004(6) C4 0.030(5) 0.035(6) 0.035(6) -0.005(5) 0.001(4) 0.002(5) C5 0.023(5) 0.035(6) 0.027(5) 0.000(4) 0.007(4) -0.003(4) C6 0.032(5) 0.027(5) 0.023(4) -0.001(4) 0.009(4) 0.000(4) C7 0.019(4) 0.037(6) 0.022(4) 0.001(4) 0.003(3) 0.003(4) C8 0.015(3) 0.031(5) 0.016(4) -0.005(4) 0.003(3) -0.002(4) C9 0.028(5) 0.032(6) 0.032(5) 0.000(5) 0.003(4) -0.002(4) C10 0.032(5) 0.027(5) 0.025(5) 0.009(4) 0.007(4) 0.003(4) C11 0.021(5) 0.051(7) 0.024(5) 0.002(5) -0.007(4) 0.003(5) C12 0.037(6) 0.046(8) 0.048(7) 0.005(6) 0.000(6) 0.005(6) C13 0.054(8) 0.035(7) 0.058(9) 0.003(6) 0.001(7) 0.012(6) C14 0.049(8) 0.044(7) 0.040(7) 0.011(6) 0.002(6) 0.010(6) C15 0.035(6) 0.045(7) 0.017(4) 0.003(5) -0.001(4) 0.000(5) C16 0.029(5) 0.034(5) 0.018(4) 0.003(4) 0.006(4) 0.001(4) C17 0.027(5) 0.043(7) 0.041(6) 0.000(5) 0.000(5) 0.000(5) C18 0.030(5) 0.048(7) 0.025(5) 0.000(5) 0.004(4) -0.003(5) C19 0.035(6) 0.060(9) 0.025(5) -0.001(5) -0.001(4) -0.015(6) C20 0.048(7) 0.060(9) 0.021(5) 0.001(5) -0.003(5) -0.014(7) C21 0.043(7) 0.038(7) 0.034(6) -0.010(5) 0.007(5) -0.005(5) C22 0.035(6) 0.036(6) 0.029(5) 0.003(5) 0.004(4) -0.001(5) C23 0.094(19) 0.13(2) 0.16(3) -0.07(2) 0.036(19) -0.073(19) C24 0.11(3) 0.20(4) 0.45(9) -0.19(5) 0.08(4) -0.06(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt N2 1.920(8) . ? Pt N4 1.996(9) . ? Pt N1 1.998(10) . ? Pt N3 2.013(10) . ? Sb F6 1.60(2) . ? Sb F5 1.831(14) . ? Sb F4 1.834(11) . ? Sb F2 1.858(11) . ? Sb F3 1.876(10) . ? Sb F1 1.910(12) . ? S C22 1.629(13) . ? N1 C1 1.340(16) . ? N1 C5 1.386(14) . ? N2 C6 1.344(14) . ? N2 C10 1.344(14) . ? N3 C15 1.313(15) . ? N3 C11 1.403(15) . ? N4 C22 1.132(14) . ? N5 C23 1.11(4) . ? C1 C2 1.364(19) . ? C1 H1 0.9500 . ? C2 C3 1.39(2) . ? C2 H2 0.9500 . ? C3 C4 1.393(18) . ? C3 H3 0.9500 . ? C4 C5 1.368(16) . ? C4 H4 0.9500 . ? C5 C6 1.482(15) . ? C6 C7 1.386(14) . ? C7 C8 1.409(15) . ? C7 H7 0.9500 . ? C8 C9 1.393(15) . ? C8 C16 1.474(14) . ? C9 C10 1.383(15) . ? C9 H9 0.9500 . ? C10 C11 1.492(15) . ? C11 C12 1.369(19) . ? C12 C13 1.390(19) . ? C12 H12 0.9500 . ? C13 C14 1.37(2) . ? C13 H13 0.9500 . ? C14 C15 1.374(19) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C21 1.394(17) . ? C16 C17 1.412(16) . ? C17 C18 1.367(16) . ? C17 H17 0.9500 . ? C18 C19 1.401(19) . ? C18 H18 0.9500 . ? C19 C20 1.35(2) . ? C19 H19 0.9500 . ? C20 C21 1.407(18) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C23 C24 1.25(4) . ? C24 H241 0.9800 . ? C24 H242 0.9800 . ? C24 H243 0.9800 . ? 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 N4 179.7(4) . . ? N2 Pt N1 81.0(4) . . ? N4 Pt N1 98.8(4) . . ? N2 Pt N3 81.9(4) . . ? N4 Pt N3 98.4(4) . . ? N1 Pt N3 162.8(4) . . ? F6 Sb F5 91.2(9) . . ? F6 Sb F4 92.3(7) . . ? F5 Sb F4 91.5(8) . . ? F6 Sb F2 94.5(6) . . ? F5 Sb F2 90.6(8) . . ? F4 Sb F2 172.8(6) . . ? F6 Sb F3 177.7(7) . . ? F5 Sb F3 91.1(7) . . ? F4 Sb F3 87.0(6) . . ? F2 Sb F3 86.1(6) . . ? F6 Sb F1 87.9(7) . . ? F5 Sb F1 178.9(7) . . ? F4 Sb F1 87.8(6) . . ? F2 Sb F1 90.2(6) . . ? F3 Sb F1 89.8(6) . . ? C1 N1 C5 116.8(11) . . ? C1 N1 Pt 128.9(9) . . ? C5 N1 Pt 114.3(8) . . ? C6 N2 C10 121.6(9) . . ? C6 N2 Pt 118.9(7) . . ? C10 N2 Pt 119.5(7) . . ? C15 N3 C11 118.5(10) . . ? C15 N3 Pt 129.4(9) . . ? C11 N3 Pt 112.0(8) . . ? C22 N4 Pt 175.2(9) . . ? N1 C1 C2 123.3(12) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C1 C2 C3 120.9(12) . . ? C1 C2 H2 119.6 . . ? C3 C2 H2 119.6 . . ? C2 C3 C4 116.3(12) . . ? C2 C3 H3 121.8 . . ? C4 C3 H3 121.8 . . ? C5 C4 C3 120.9(12) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C4 C5 N1 121.8(11) . . ? C4 C5 C6 125.1(10) . . ? N1 C5 C6 113.1(10) . . ? N2 C6 C7 120.0(10) . . ? N2 C6 C5 112.7(9) . . ? C7 C6 C5 127.3(10) . . ? C6 C7 C8 120.2(9) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C9 C8 C7 117.6(9) . . ? C9 C8 C16 121.4(10) . . ? C7 C8 C16 121.0(9) . . ? C10 C9 C8 120.2(10) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? N2 C10 C9 120.5(10) . . ? N2 C10 C11 111.5(10) . . ? C9 C10 C11 128.0(11) . . ? C12 C11 N3 119.8(10) . . ? C12 C11 C10 125.2(11) . . ? N3 C11 C10 115.0(11) . . ? C11 C12 C13 120.5(13) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C14 C13 C12 118.3(14) . . ? C14 C13 H13 120.8 . . ? C12 C13 H13 120.8 . . ? C13 C14 C15 119.7(13) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? N3 C15 C14 123.1(12) . . ? N3 C15 H15 118.5 . . ? C14 C15 H15 118.5 . . ? C21 C16 C17 116.6(11) . . ? C21 C16 C8 122.2(10) . . ? C17 C16 C8 121.2(10) . . ? C18 C17 C16 122.3(13) . . ? C18 C17 H17 118.8 . . ? C16 C17 H17 118.8 . . ? C17 C18 C19 119.5(12) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? C20 C19 C18 120.0(12) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C21 120.6(13) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C16 C21 C20 120.9(13) . . ? C16 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? N4 C22 S 176.5(11) . . ? N5 C23 C24 175(6) . . ? C23 C24 H241 109.5 . . ? C23 C24 H242 109.5 . . ? H241 C24 H242 109.5 . . ? C23 C24 H243 109.5 . . ? H241 C24 H243 109.5 . . ? H242 C24 H243 109.5 . . ? _diffrn_measured_fraction_theta_max 0.840 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 5.662 _refine_diff_density_min -4.631 _refine_diff_density_rms 0.284 # Attachment '8522_web_deposit_cif_file_4_JohnField_1323158265.1meoh.cif' # B. P. Waldron MSc, University of KwaZulu-Natal, 2008 data_1MeOH _database_code_depnum_ccdc_archive 'CCDC 857052' #TrackingRef '8522_web_deposit_cif_file_4_JohnField_1323158265.1meoh.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Pt{4'-(Ph)trpy}(NCS)]SbF6.CH3OH. This crystal was obtained by exposing a single crystal of [Pt{4'-(Ph)trpy}(NCS)]SbF6 (1) to vapours of methanol. ; _chemical_name_common "[Pt{4'-(Ph)trpy}(NCS)]SbF6.CH3OH" _chemical_melting_point ? _chemical_formula_moiety 'C22 H15 N4 Pt S, F6 Sb, C H4 O' _chemical_formula_sum 'C23 H19 F6 N4 O Pt S Sb' _chemical_formula_weight 830.32 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' O O 0.0106 0.0060 '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' S S 0.1246 0.1234 '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 _symmetry_space_group_name_Hall '-P 2yn' 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 9.7239(3) _cell_length_b 25.4860(7) _cell_length_c 10.4632(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.004(2) _cell_angle_gamma 90.00 _cell_volume 2567.76(13) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used >200 _cell_measurement_theta_min 4 _cell_measurement_theta_max 32 _exptl_crystal_description 'irregular block' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.148 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 6.644 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1029 _exptl_absorpt_correction_T_max 0.3703 _exptl_absorpt_process_details 'Crysalis RED 170' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur CCD' _diffrn_measurement_method 'omega 2 theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41513 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0521 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 34.22 _reflns_number_total 9434 _reflns_number_gt 6588 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crysalis CCD 170' _computing_cell_refinement 'Crysalis CCD 170' _computing_data_reduction 'Crysalis CCD 170' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-seed (Barbour, 2005)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.0419P)^2^+4.3222P] 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 9434 _refine_ls_number_parameters 339 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0655 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0862 _refine_ls_wR_factor_gt 0.0810 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt 0.521876(15) 0.024009(6) 0.852856(14) 0.02224(5) Uani 1 1 d . . . Sb Sb 0.77910(3) 0.182952(12) 0.61030(3) 0.03430(8) Uani 1 1 d . . . S S 0.97898(13) 0.08480(6) 0.99873(14) 0.0476(3) Uani 1 1 d . . . F1 F 0.8138(5) 0.18849(14) 0.4387(3) 0.0702(11) Uani 1 1 d . . . F2 F 0.9532(3) 0.21394(14) 0.6615(4) 0.0654(11) Uani 1 1 d . . . F3 F 0.8683(5) 0.11800(13) 0.6201(4) 0.0763(12) Uani 1 1 d . . . F4 F 0.6108(4) 0.15157(17) 0.5590(5) 0.0961(16) Uani 1 1 d . . . F5 F 0.7016(4) 0.24946(13) 0.5998(5) 0.0751(12) Uani 1 1 d . . . F6 F 0.7519(6) 0.1769(2) 0.7800(4) 0.0992(16) Uani 1 1 d . . . O O 0.2883(8) 0.3184(3) 0.5922(7) 0.113(2) Uani 1 1 d D . . N1 N 0.4279(3) 0.09432(13) 0.8509(3) 0.0237(7) Uani 1 1 d . . . N2 N 0.3364(3) 0.00211(13) 0.7863(3) 0.0215(6) Uani 1 1 d . . . N3 N 0.5574(4) -0.05314(14) 0.8303(3) 0.0246(7) Uani 1 1 d . . . N4 N 0.7167(4) 0.04708(14) 0.9199(3) 0.0277(7) Uani 1 1 d . . . C1 C 0.4853(5) 0.14124(17) 0.8864(4) 0.0295(9) Uani 1 1 d . . . H1 H 0.5818 0.1431 0.9175 0.035 Uiso 1 1 calc R . . C2 C 0.4069(5) 0.18674(18) 0.8784(5) 0.0362(10) Uani 1 1 d . . . H2 H 0.4496 0.2194 0.9031 0.043 Uiso 1 1 calc R . . C3 C 0.2672(5) 0.18454(17) 0.8348(5) 0.0343(10) Uani 1 1 d . . . H3 H 0.2124 0.2155 0.8303 0.041 Uiso 1 1 calc R . . C4 C 0.2067(4) 0.13645(16) 0.7973(4) 0.0280(8) Uani 1 1 d . . . H4 H 0.1103 0.1345 0.7660 0.034 Uiso 1 1 calc R . . C5 C 0.2867(4) 0.09188(16) 0.8056(4) 0.0245(8) Uani 1 1 d . . . C6 C 0.2345(4) 0.03896(15) 0.7689(4) 0.0223(7) Uani 1 1 d . . . C7 C 0.1021(4) 0.02453(15) 0.7184(4) 0.0230(7) Uani 1 1 d . . . H7 H 0.0309 0.0503 0.7047 0.028 Uiso 1 1 calc R . . C8 C 0.0713(4) -0.02827(15) 0.6866(4) 0.0219(7) Uani 1 1 d . . . C9 C 0.1811(4) -0.06462(16) 0.7072(4) 0.0246(8) Uani 1 1 d . . . H9 H 0.1641 -0.1005 0.6866 0.030 Uiso 1 1 calc R . . C10 C 0.3125(4) -0.04861(15) 0.7570(4) 0.0212(7) Uani 1 1 d . . . C11 C 0.4396(4) -0.08117(16) 0.7830(4) 0.0245(8) Uani 1 1 d . . . C12 C 0.4461(5) -0.13402(17) 0.7623(4) 0.0308(9) Uani 1 1 d . . . H12 H 0.3644 -0.1531 0.7309 0.037 Uiso 1 1 calc R . . C13 C 0.5729(5) -0.15951(18) 0.7875(5) 0.0358(10) Uani 1 1 d . . . H13 H 0.5789 -0.1961 0.7724 0.043 Uiso 1 1 calc R . . C14 C 0.6895(5) -0.13156(18) 0.8344(5) 0.0336(10) Uani 1 1 d . . . H14 H 0.7768 -0.1487 0.8523 0.040 Uiso 1 1 calc R . . C15 C 0.6796(4) -0.07821(16) 0.8556(4) 0.0266(8) Uani 1 1 d . . . H15 H 0.7605 -0.0590 0.8885 0.032 Uiso 1 1 calc R . . C16 C -0.0708(4) -0.04448(16) 0.6285(4) 0.0231(8) Uani 1 1 d . . . C17 C -0.1789(4) -0.00801(18) 0.6138(5) 0.0310(9) Uani 1 1 d . . . H17 H -0.1618 0.0270 0.6427 0.037 Uiso 1 1 calc R . . C18 C -0.3112(4) -0.02251(18) 0.5573(5) 0.0331(9) Uani 1 1 d . . . H18 H -0.3833 0.0029 0.5470 0.040 Uiso 1 1 calc R . . C19 C -0.3398(5) -0.07366(19) 0.5158(4) 0.0339(10) Uani 1 1 d . . . H19 H -0.4305 -0.0835 0.4777 0.041 Uiso 1 1 calc R . . C20 C -0.2327(5) -0.10982(19) 0.5313(5) 0.0360(10) Uani 1 1 d . . . H20 H -0.2505 -0.1450 0.5035 0.043 Uiso 1 1 calc R . . C21 C -0.0997(5) -0.09579(18) 0.5866(4) 0.0330(9) Uani 1 1 d . . . H21 H -0.0279 -0.1213 0.5961 0.040 Uiso 1 1 calc R . . C22 C 0.8241(5) 0.06228(18) 0.9515(4) 0.0307(9) Uani 1 1 d . . . C23 C 0.3122(14) 0.2671(4) 0.5589(11) 0.139(5) Uani 1 1 d D . . H231 H 0.2321 0.2454 0.5720 0.209 Uiso 1 1 calc R . . H232 H 0.3953 0.2539 0.6130 0.209 Uiso 1 1 calc R . . H233 H 0.3260 0.2655 0.4679 0.209 Uiso 1 1 calc R . . H24 H 0.359(11) 0.339(3) 0.553(13) 0.22(7) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt 0.01659(7) 0.02663(8) 0.02306(7) -0.00037(6) 0.00118(5) -0.00202(6) Sb 0.03751(17) 0.02575(14) 0.03904(16) 0.00145(12) 0.00325(13) -0.00182(12) S 0.0229(6) 0.0675(9) 0.0503(7) 0.0037(7) -0.0020(5) -0.0133(6) F1 0.101(3) 0.063(2) 0.0473(19) -0.0006(17) 0.013(2) -0.015(2) F2 0.0384(18) 0.053(2) 0.100(3) -0.0108(19) -0.0075(19) -0.0068(15) F3 0.089(3) 0.0322(17) 0.109(3) 0.0109(19) 0.021(3) 0.0136(18) F4 0.060(3) 0.073(3) 0.145(4) 0.001(3) -0.019(3) -0.038(2) F5 0.051(2) 0.0414(19) 0.130(4) -0.006(2) 0.004(2) 0.0119(16) F6 0.118(4) 0.134(4) 0.052(2) 0.008(2) 0.033(3) -0.013(3) O 0.110(5) 0.115(5) 0.130(6) 0.025(4) 0.069(5) 0.028(4) N1 0.0215(16) 0.0248(16) 0.0247(16) -0.0011(13) 0.0031(13) -0.0027(13) N2 0.0156(15) 0.0255(16) 0.0224(15) 0.0001(13) -0.0007(12) -0.0016(12) N3 0.0215(16) 0.0303(18) 0.0215(15) 0.0006(13) 0.0012(13) 0.0046(13) N4 0.0226(18) 0.0270(17) 0.0323(18) -0.0022(14) -0.0002(15) -0.0011(14) C1 0.029(2) 0.030(2) 0.030(2) -0.0036(17) 0.0035(17) -0.0056(17) C2 0.037(3) 0.026(2) 0.045(3) -0.0068(19) 0.004(2) -0.0060(18) C3 0.037(2) 0.025(2) 0.040(2) -0.0033(18) 0.002(2) -0.0002(18) C4 0.026(2) 0.027(2) 0.030(2) -0.0008(16) -0.0022(17) 0.0009(16) C5 0.0211(19) 0.0270(19) 0.0250(18) -0.0008(15) 0.0017(15) -0.0031(15) C6 0.0215(19) 0.0247(18) 0.0205(17) -0.0001(14) 0.0025(15) 0.0009(14) C7 0.0167(16) 0.0246(18) 0.0271(18) 0.0005(16) 0.0013(14) 0.0024(15) C8 0.0152(16) 0.0278(19) 0.0223(16) 0.0004(15) 0.0014(14) -0.0017(14) C9 0.0201(18) 0.0253(19) 0.0272(19) 0.0011(15) -0.0007(16) -0.0015(15) C10 0.0209(18) 0.0200(18) 0.0221(17) 0.0006(14) 0.0008(15) 0.0010(14) C11 0.0194(18) 0.028(2) 0.0253(18) 0.0024(15) -0.0005(15) -0.0004(14) C12 0.027(2) 0.029(2) 0.035(2) 0.0045(18) -0.0017(18) -0.0014(16) C13 0.036(2) 0.025(2) 0.044(3) 0.0040(19) -0.001(2) 0.0048(18) C14 0.029(2) 0.031(2) 0.040(2) 0.0100(19) 0.0011(19) 0.0076(17) C15 0.0202(19) 0.031(2) 0.0264(19) 0.0041(16) -0.0030(16) 0.0008(15) C16 0.0172(17) 0.031(2) 0.0218(17) 0.0017(15) 0.0032(14) -0.0008(15) C17 0.020(2) 0.034(2) 0.038(2) -0.0014(18) -0.0014(18) -0.0041(16) C18 0.0174(18) 0.042(2) 0.039(2) 0.003(2) -0.0006(17) -0.0003(18) C19 0.022(2) 0.049(3) 0.030(2) 0.0008(19) 0.0012(17) -0.0100(19) C20 0.033(2) 0.038(2) 0.036(2) -0.0066(19) 0.003(2) -0.0124(19) C21 0.028(2) 0.033(2) 0.036(2) -0.0052(18) 0.0000(19) -0.0033(18) C22 0.026(2) 0.035(2) 0.032(2) 0.0006(18) 0.0060(18) 0.0013(17) C23 0.207(14) 0.092(7) 0.133(9) 0.058(7) 0.074(9) 0.059(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 1.923(3) . ? Pt N1 2.010(3) . ? Pt N4 2.014(3) . ? Pt N3 2.016(3) . ? Sb F4 1.834(4) . ? Sb F6 1.838(4) . ? Sb F5 1.852(3) . ? Sb F3 1.865(3) . ? Sb F2 1.877(3) . ? Sb F1 1.878(4) . ? S C22 1.623(5) . ? O C23 1.383(11) . ? O H24 0.99(7) . ? N1 C1 1.350(5) . ? N1 C5 1.390(5) . ? N2 C10 1.342(5) . ? N2 C6 1.359(5) . ? N3 C15 1.343(5) . ? N3 C11 1.382(5) . ? N4 C22 1.120(5) . ? C1 C2 1.384(6) . ? C1 H1 0.9500 . ? C2 C3 1.373(7) . ? C2 H2 0.9500 . ? C3 C4 1.392(6) . ? C3 H3 0.9500 . ? C4 C5 1.373(6) . ? C4 H4 0.9500 . ? C5 C6 1.473(5) . ? C6 C7 1.372(5) . ? C7 C8 1.408(5) . ? C7 H7 0.9500 . ? C8 C9 1.407(5) . ? C8 C16 1.489(5) . ? C9 C10 1.373(5) . ? C9 H9 0.9500 . ? C10 C11 1.482(5) . ? C11 C12 1.367(6) . ? C12 C13 1.386(6) . ? C12 H12 0.9500 . ? C13 C14 1.371(7) . ? C13 H13 0.9500 . ? C14 C15 1.383(6) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C21 1.395(6) . ? C16 C17 1.396(6) . ? C17 C18 1.389(6) . ? C17 H17 0.9500 . ? C18 C19 1.390(6) . ? C18 H18 0.9500 . ? C19 C20 1.383(7) . ? C19 H19 0.9500 . ? C20 C21 1.388(6) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C23 H231 0.9800 . ? C23 H232 0.9800 . ? C23 H233 0.9800 . ? 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 81.54(14) . . ? N2 Pt N4 179.18(14) . . ? N1 Pt N4 98.49(14) . . ? N2 Pt N3 80.90(14) . . ? N1 Pt N3 162.41(13) . . ? N4 Pt N3 99.06(14) . . ? F4 Sb F6 90.2(2) . . ? F4 Sb F5 92.45(19) . . ? F6 Sb F5 91.3(2) . . ? F4 Sb F3 91.0(2) . . ? F6 Sb F3 90.0(2) . . ? F5 Sb F3 176.26(18) . . ? F4 Sb F2 178.9(2) . . ? F6 Sb F2 90.3(2) . . ? F5 Sb F2 88.57(16) . . ? F3 Sb F2 87.92(17) . . ? F4 Sb F1 91.4(2) . . ? F6 Sb F1 177.9(2) . . ? F5 Sb F1 90.02(19) . . ? F3 Sb F1 88.58(19) . . ? F2 Sb F1 88.07(18) . . ? C23 O H24 104(6) . . ? C1 N1 C5 119.0(4) . . ? C1 N1 Pt 128.1(3) . . ? C5 N1 Pt 112.9(3) . . ? C10 N2 C6 122.4(3) . . ? C10 N2 Pt 119.1(3) . . ? C6 N2 Pt 118.5(3) . . ? C15 N3 C11 119.4(4) . . ? C15 N3 Pt 127.0(3) . . ? C11 N3 Pt 113.5(3) . . ? C22 N4 Pt 175.7(4) . . ? N1 C1 C2 121.5(4) . . ? N1 C1 H1 119.3 . . ? C2 C1 H1 119.3 . . ? C3 C2 C1 119.8(4) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 119.3(4) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 119.8(4) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 N1 120.6(4) . . ? C4 C5 C6 124.7(4) . . ? N1 C5 C6 114.7(3) . . ? N2 C6 C7 119.6(4) . . ? N2 C6 C5 112.3(3) . . ? C7 C6 C5 128.1(4) . . ? C6 C7 C8 120.3(4) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C9 C8 C7 117.5(3) . . ? C9 C8 C16 121.4(3) . . ? C7 C8 C16 121.1(3) . . ? C10 C9 C8 120.6(4) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? N2 C10 C9 119.7(4) . . ? N2 C10 C11 112.6(3) . . ? C9 C10 C11 127.7(4) . . ? C12 C11 N3 120.8(4) . . ? C12 C11 C10 125.3(4) . . ? N3 C11 C10 113.9(3) . . ? C11 C12 C13 119.4(4) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? C14 C13 C12 119.6(4) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C13 C14 C15 119.7(4) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? N3 C15 C14 121.1(4) . . ? N3 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C21 C16 C17 118.3(4) . . ? C21 C16 C8 121.6(4) . . ? C17 C16 C8 120.1(4) . . ? C18 C17 C16 120.6(4) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C17 C18 C19 121.0(4) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C20 C19 C18 118.3(4) . . ? C20 C19 H19 120.9 . . ? C18 C19 H19 120.9 . . ? C19 C20 C21 121.3(4) . . ? C19 C20 H20 119.3 . . ? C21 C20 H20 119.3 . . ? C20 C21 C16 120.5(4) . . ? C20 C21 H21 119.7 . . ? C16 C21 H21 119.7 . . ? N4 C22 S 179.2(5) . . ? O C23 H231 109.5 . . ? O C23 H232 109.5 . . ? H231 C23 H232 109.5 . . ? O C23 H233 109.5 . . ? H231 C23 H233 109.5 . . ? H232 C23 H233 109.5 . . ? _diffrn_measured_fraction_theta_max 0.885 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 3.020 _refine_diff_density_min -2.299 _refine_diff_density_rms 0.165 # Attachment '8523_web_deposit_cif_file_5_JohnField_1323158265.1Me2CO.cif' # B. P. Waldron MSc, University of KwaZulu-Natal, 2008 data_1.acetone _database_code_depnum_ccdc_archive 'CCDC 857053' #TrackingRef '8523_web_deposit_cif_file_5_JohnField_1323158265.1Me2CO.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; This is a crystal of [Pt{4'-(Ph)trpy}(NCS)]SbF6.(CH3)2CO obtained directly by crystallisation from an acetone solution of 1. ; _chemical_name_common "[Pt{4'-(Ph)trpy}(NCS)]SbF6.(CH3)2CO" _chemical_melting_point ? _chemical_formula_moiety 'C22 H15 N4 Pt S, C3 H6 O, F6 Sb' _chemical_formula_sum 'C25 H21 F6 N4 O Pt S Sb' _chemical_formula_weight 856.36 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' O O 0.0106 0.0060 '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_space_group_name_Hall '-P 2yn' 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 9.7859(3) _cell_length_b 25.3897(8) _cell_length_c 10.9182(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.355(3) _cell_angle_gamma 90.00 _cell_volume 2683.96(15) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used >200 _cell_measurement_theta_min 4 _cell_measurement_theta_max 32 _exptl_crystal_description 'irregular block' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.119 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 6.360 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2337 _exptl_absorpt_correction_T_max 0.5290 _exptl_absorpt_process_details 'Crysalis RED 170' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur CCD' _diffrn_measurement_method 'omega 2 theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28462 _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 26.11 _reflns_number_total 5291 _reflns_number_gt 5224 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crysalis CCD 170' _computing_cell_refinement 'Crysalis CCD 170' _computing_data_reduction 'Crysalis CCD 170' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Hg IUCr' _computing_publication_material 'CIFTAB (Sheldrick, 1997' _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^)+(0.0000P)^2^+85.6442P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5291 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0878 _refine_ls_R_factor_gt 0.0865 _refine_ls_wR_factor_ref 0.1643 _refine_ls_wR_factor_gt 0.1639 _refine_ls_goodness_of_fit_ref 1.532 _refine_ls_restrained_S_all 1.532 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt 0.51679(5) 0.02952(2) 0.86104(5) 0.02173(16) Uani 1 1 d . . . Sb Sb 0.23242(11) 0.32952(4) 1.08658(10) 0.0308(3) Uani 1 1 d . . . S S 0.9759(4) 0.0834(2) 1.0092(5) 0.0483(12) Uani 1 1 d . . . F1 F 0.0890(15) 0.2985(6) 0.9794(13) 0.085(5) Uani 1 1 d . . . F2 F 0.2812(16) 0.2644(5) 1.1490(12) 0.078(4) Uani 1 1 d . . . F3 F 0.3402(14) 0.3210(5) 0.9607(12) 0.068(4) Uani 1 1 d . . . F4 F 0.3755(13) 0.3631(6) 1.1857(14) 0.085(5) Uani 1 1 d . . . F5 F 0.1784(13) 0.3955(4) 1.0181(11) 0.059(3) Uani 1 1 d . . . F6 F 0.1152(17) 0.3383(6) 1.2021(14) 0.092(5) Uani 1 1 d . . . O O 0.181(2) 0.2754(11) 0.617(2) 0.125(9) Uani 1 1 d . . . N1 N 0.4189(12) 0.0992(5) 0.8682(11) 0.022(2) Uani 1 1 d . . . N2 N 0.3337(10) 0.0072(4) 0.7914(10) 0.017(2) Uani 1 1 d . . . N3 N 0.5573(11) -0.0470(6) 0.8293(10) 0.028(3) Uani 1 1 d . . . N4 N 0.7086(12) 0.0528(5) 0.9312(12) 0.028(3) Uani 1 1 d . . . C1 C 0.4719(16) 0.1448(6) 0.9124(14) 0.030(3) Uani 1 1 d . . . H1 H 0.5671 0.1467 0.9453 0.036 Uiso 1 1 calc R . . C2 C 0.3918(18) 0.1891(7) 0.9112(16) 0.038(4) Uani 1 1 d . . . H2 H 0.4314 0.2209 0.9461 0.046 Uiso 1 1 calc R . . C3 C 0.2563(17) 0.1883(6) 0.8608(16) 0.035(4) Uani 1 1 d . . . H3 H 0.2022 0.2195 0.8561 0.041 Uiso 1 1 calc R . . C4 C 0.1988(16) 0.1410(6) 0.8167(14) 0.028(3) Uani 1 1 d . . . H4 H 0.1038 0.1394 0.7830 0.033 Uiso 1 1 calc R . . C5 C 0.2794(14) 0.0960(6) 0.8213(14) 0.026(3) Uani 1 1 d . . . C6 C 0.2321(14) 0.0437(5) 0.7782(12) 0.020(3) Uani 1 1 d . . . C7 C 0.0999(14) 0.0294(6) 0.7237(13) 0.025(3) Uani 1 1 d . . . H7 H 0.0279 0.0548 0.7115 0.030 Uiso 1 1 calc R . . C8 C 0.0749(13) -0.0223(6) 0.6877(14) 0.024(3) Uani 1 1 d . . . C9 C 0.1820(15) -0.0594(6) 0.7057(12) 0.022(3) Uani 1 1 d . . . H9 H 0.1654 -0.0951 0.6824 0.026 Uiso 1 1 calc R . . C10 C 0.3128(13) -0.0430(5) 0.7582(12) 0.016(3) Uani 1 1 d . . . C11 C 0.4410(14) -0.0742(6) 0.7821(13) 0.022(3) Uani 1 1 d . . . C12 C 0.4488(15) -0.1278(6) 0.7573(13) 0.026(3) Uani 1 1 d . . . H12 H 0.3685 -0.1469 0.7236 0.031 Uiso 1 1 calc R . . C13 C 0.5725(16) -0.1525(6) 0.7821(14) 0.031(3) Uani 1 1 d . . . H13 H 0.5779 -0.1894 0.7693 0.037 Uiso 1 1 calc R . . C14 C 0.6924(17) -0.1244(7) 0.8262(16) 0.038(4) Uani 1 1 d . . . H14 H 0.7800 -0.1412 0.8395 0.045 Uiso 1 1 calc R . . C15 C 0.6787(14) -0.0716(7) 0.8496(13) 0.031(4) Uani 1 1 d . . . H15 H 0.7587 -0.0520 0.8813 0.038 Uiso 1 1 calc R . . C16 C -0.0662(13) -0.0391(5) 0.6255(12) 0.018(3) Uani 1 1 d . . . C17 C -0.1805(14) -0.0054(7) 0.6188(16) 0.035(4) Uani 1 1 d . . . H17 H -0.1699 0.0286 0.6553 0.042 Uiso 1 1 calc R . . C18 C -0.3071(14) -0.0210(6) 0.5601(17) 0.033(4) Uani 1 1 d . . . H18 H -0.3822 0.0030 0.5537 0.040 Uiso 1 1 calc R . . C19 C -0.3287(16) -0.0706(7) 0.5101(16) 0.037(4) Uani 1 1 d . . . H19 H -0.4173 -0.0806 0.4692 0.044 Uiso 1 1 calc R . . C20 C -0.2217(17) -0.1050(8) 0.5199(16) 0.043(4) Uani 1 1 d . . . H20 H -0.2364 -0.1399 0.4891 0.052 Uiso 1 1 calc R . . C21 C -0.0893(17) -0.0896(7) 0.5752(16) 0.037(4) Uani 1 1 d . . . H21 H -0.0145 -0.1136 0.5785 0.044 Uiso 1 1 calc R . . C22 C 0.8166(16) 0.0653(6) 0.9617(15) 0.028(3) Uani 1 1 d . . . C23 C 0.292(3) 0.2761(10) 0.583(2) 0.071(7) Uani 1 1 d . . . C24 C 0.416(3) 0.2867(11) 0.669(2) 0.078(7) Uani 1 1 d . . . H241 H 0.4270 0.3248 0.6810 0.117 Uiso 1 1 calc R . . H242 H 0.4965 0.2727 0.6352 0.117 Uiso 1 1 calc R . . H243 H 0.4095 0.2697 0.7483 0.117 Uiso 1 1 calc R . . C25 C 0.302(3) 0.2657(13) 0.452(2) 0.100(11) Uani 1 1 d . . . H251 H 0.2145 0.2504 0.4118 0.150 Uiso 1 1 calc R . . H252 H 0.3773 0.2410 0.4466 0.150 Uiso 1 1 calc R . . H253 H 0.3193 0.2988 0.4110 0.150 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 0.0130(2) 0.0287(3) 0.0225(3) 0.0007(2) -0.00067(18) -0.0018(2) Sb 0.0327(6) 0.0290(6) 0.0314(6) -0.0034(4) 0.0068(4) -0.0043(4) S 0.022(2) 0.063(3) 0.058(3) 0.005(2) -0.0037(19) -0.015(2) F1 0.077(9) 0.086(10) 0.081(10) 0.005(8) -0.026(8) -0.034(8) F2 0.110(11) 0.057(8) 0.068(9) 0.021(7) 0.019(8) 0.040(8) F3 0.090(9) 0.055(7) 0.073(8) -0.005(6) 0.053(8) 0.001(7) F4 0.054(8) 0.091(10) 0.096(11) -0.031(8) -0.035(7) -0.003(7) F5 0.070(8) 0.036(6) 0.069(8) 0.003(6) -0.004(6) 0.004(6) F6 0.110(12) 0.092(11) 0.093(11) -0.003(9) 0.075(10) 0.011(9) O 0.078(13) 0.21(3) 0.088(15) 0.009(16) 0.019(11) 0.075(16) N1 0.027(6) 0.020(6) 0.020(6) -0.002(5) 0.007(5) -0.005(5) N2 0.009(5) 0.021(6) 0.022(6) 0.001(5) 0.002(4) 0.001(4) N3 0.012(5) 0.056(9) 0.014(6) 0.001(5) -0.003(4) 0.006(5) N4 0.012(6) 0.035(7) 0.034(7) 0.000(6) -0.003(5) 0.001(5) C1 0.025(8) 0.041(9) 0.023(8) 0.000(7) 0.000(6) -0.006(7) C2 0.044(10) 0.030(9) 0.042(10) 0.001(7) 0.011(8) -0.011(8) C3 0.032(8) 0.020(8) 0.051(10) -0.002(7) 0.004(7) 0.003(6) C4 0.028(8) 0.024(8) 0.031(8) 0.009(6) 0.004(6) -0.001(6) C5 0.021(7) 0.027(8) 0.029(8) 0.007(6) 0.001(6) -0.004(6) C6 0.028(7) 0.008(6) 0.023(7) -0.002(5) 0.000(6) 0.003(5) C7 0.019(7) 0.025(7) 0.031(8) -0.008(7) 0.000(6) 0.005(6) C8 0.013(6) 0.025(8) 0.031(8) 0.002(6) -0.006(5) 0.000(6) C9 0.029(7) 0.021(7) 0.015(6) -0.005(5) -0.003(5) 0.003(6) C10 0.021(6) 0.004(6) 0.021(7) 0.003(5) 0.001(5) 0.003(5) C11 0.019(7) 0.025(7) 0.024(7) 0.004(6) 0.012(6) 0.001(6) C12 0.027(8) 0.030(8) 0.019(7) 0.001(6) -0.006(6) -0.004(6) C13 0.030(8) 0.028(8) 0.032(8) 0.008(7) -0.009(6) 0.007(7) C14 0.029(8) 0.042(10) 0.040(10) 0.007(8) 0.001(7) 0.018(7) C15 0.012(7) 0.060(11) 0.020(7) 0.006(7) -0.006(5) 0.002(7) C16 0.017(6) 0.019(7) 0.020(7) -0.005(5) 0.003(5) -0.004(5) C17 0.007(7) 0.043(10) 0.052(10) 0.008(8) -0.004(6) -0.002(6) C18 0.012(7) 0.020(8) 0.067(12) 0.006(7) 0.003(7) 0.003(6) C19 0.026(8) 0.040(10) 0.039(9) 0.015(8) -0.012(7) -0.014(7) C20 0.032(9) 0.054(12) 0.039(10) -0.005(9) -0.008(7) -0.012(8) C21 0.033(9) 0.031(9) 0.044(10) -0.013(8) 0.001(7) 0.002(7) C22 0.027(8) 0.021(7) 0.039(9) -0.004(7) 0.013(7) 0.001(6) C23 0.084(17) 0.077(17) 0.054(13) 0.004(12) 0.015(12) 0.057(14) C24 0.090(19) 0.089(19) 0.055(14) 0.015(13) 0.010(13) 0.010(15) C25 0.12(2) 0.12(3) 0.058(16) -0.009(16) 0.011(16) 0.06(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt N2 1.927(10) . ? Pt N4 2.010(12) . ? Pt N1 2.018(12) . ? Pt N3 2.024(14) . ? Sb F2 1.824(12) . ? Sb F6 1.838(12) . ? Sb F4 1.849(12) . ? Sb F3 1.862(11) . ? Sb F1 1.866(12) . ? Sb F5 1.879(11) . ? S C22 1.636(16) . ? O C23 1.20(3) . ? N1 C1 1.331(19) . ? N1 C5 1.389(18) . ? N2 C10 1.333(16) . ? N2 C6 1.352(17) . ? N3 C15 1.332(18) . ? N3 C11 1.366(18) . ? N4 C22 1.107(19) . ? C1 C2 1.37(2) . ? C1 H1 0.9500 . ? C2 C3 1.36(2) . ? C2 H2 0.9500 . ? C3 C4 1.38(2) . ? C3 H3 0.9500 . ? C4 C5 1.39(2) . ? C4 H4 0.9500 . ? C5 C6 1.460(19) . ? C6 C7 1.391(19) . ? C7 C8 1.38(2) . ? C7 H7 0.9500 . ? C8 C9 1.402(19) . ? C8 C16 1.510(18) . ? C9 C10 1.387(18) . ? C9 H9 0.9500 . ? C10 C11 1.476(18) . ? C11 C12 1.39(2) . ? C12 C13 1.35(2) . ? C12 H12 0.9500 . ? C13 C14 1.40(2) . ? C13 H13 0.9500 . ? C14 C15 1.37(2) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C21 1.40(2) . ? C16 C17 1.40(2) . ? C17 C18 1.37(2) . ? C17 H17 0.9500 . ? C18 C19 1.38(2) . ? C18 H18 0.9500 . ? C19 C20 1.36(3) . ? C19 H19 0.9500 . ? C20 C21 1.40(2) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C23 C24 1.45(4) . ? C23 C25 1.47(3) . ? C24 H241 0.9800 . ? C24 H242 0.9800 . ? C24 H243 0.9800 . ? C25 H251 0.9800 . ? C25 H252 0.9800 . ? C25 H253 0.9800 . ? 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 N4 179.1(5) . . ? N2 Pt N1 81.6(5) . . ? N4 Pt N1 98.6(5) . . ? N2 Pt N3 81.0(5) . . ? N4 Pt N3 98.8(5) . . ? N1 Pt N3 162.6(5) . . ? F2 Sb F6 90.5(7) . . ? F2 Sb F4 93.7(7) . . ? F6 Sb F4 92.1(8) . . ? F2 Sb F3 91.5(6) . . ? F6 Sb F3 175.9(7) . . ? F4 Sb F3 91.3(7) . . ? F2 Sb F1 89.1(7) . . ? F6 Sb F1 89.6(8) . . ? F4 Sb F1 176.7(7) . . ? F3 Sb F1 86.8(7) . . ? F2 Sb F5 178.2(6) . . ? F6 Sb F5 89.8(6) . . ? F4 Sb F5 88.1(6) . . ? F3 Sb F5 88.1(6) . . ? F1 Sb F5 89.1(6) . . ? C1 N1 C5 119.6(13) . . ? C1 N1 Pt 128.0(10) . . ? C5 N1 Pt 112.4(9) . . ? C10 N2 C6 123.0(11) . . ? C10 N2 Pt 119.1(9) . . ? C6 N2 Pt 117.9(9) . . ? C15 N3 C11 120.0(14) . . ? C15 N3 Pt 127.9(11) . . ? C11 N3 Pt 112.2(9) . . ? C22 N4 Pt 175.1(13) . . ? N1 C1 C2 121.3(14) . . ? N1 C1 H1 119.3 . . ? C2 C1 H1 119.3 . . ? C3 C2 C1 120.9(16) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C2 C3 C4 118.6(15) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C3 C4 C5 120.2(14) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C4 C5 N1 119.3(13) . . ? C4 C5 C6 125.8(13) . . ? N1 C5 C6 114.9(13) . . ? N2 C6 C7 119.4(12) . . ? N2 C6 C5 113.2(12) . . ? C7 C6 C5 127.3(13) . . ? C8 C7 C6 119.0(13) . . ? C8 C7 H7 120.5 . . ? C6 C7 H7 120.5 . . ? C7 C8 C9 120.0(12) . . ? C7 C8 C16 120.6(12) . . ? C9 C8 C16 119.3(12) . . ? C10 C9 C8 118.9(13) . . ? C10 C9 H9 120.6 . . ? C8 C9 H9 120.6 . . ? N2 C10 C9 119.7(12) . . ? N2 C10 C11 111.9(11) . . ? C9 C10 C11 128.4(12) . . ? N3 C11 C12 120.1(13) . . ? N3 C11 C10 115.8(12) . . ? C12 C11 C10 124.1(13) . . ? C13 C12 C11 119.0(14) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C12 C13 C14 121.0(15) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C15 C14 C13 117.5(14) . . ? C15 C14 H14 121.2 . . ? C13 C14 H14 121.2 . . ? N3 C15 C14 122.3(15) . . ? N3 C15 H15 118.8 . . ? C14 C15 H15 118.8 . . ? C21 C16 C17 117.2(13) . . ? C21 C16 C8 121.4(13) . . ? C17 C16 C8 121.4(13) . . ? C18 C17 C16 120.5(16) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C17 C18 C19 121.9(15) . . ? C17 C18 H18 119.1 . . ? C19 C18 H18 119.1 . . ? C20 C19 C18 119.0(15) . . ? C20 C19 H19 120.5 . . ? C18 C19 H19 120.5 . . ? C19 C20 C21 120.5(17) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C16 C21 C20 120.8(16) . . ? C16 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? N4 C22 S 179.0(17) . . ? O C23 C24 121(2) . . ? O C23 C25 120(3) . . ? C24 C23 C25 120(2) . . ? C23 C24 H241 109.5 . . ? C23 C24 H242 109.5 . . ? H241 C24 H242 109.5 . . ? C23 C24 H243 109.5 . . ? H241 C24 H243 109.5 . . ? H242 C24 H243 109.5 . . ? C23 C25 H251 109.5 . . ? C23 C25 H252 109.5 . . ? H251 C25 H252 109.5 . . ? C23 C25 H253 109.5 . . ? H251 C25 H253 109.5 . . ? H252 C25 H253 109.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.362 _refine_diff_density_min -3.001 _refine_diff_density_rms 0.236