Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _publ_contact_author_email QIANSOAL@USC.ES _publ_contact_author_name 'Prof Antonio Sousa' _journal_name_full 'J.Chem.Soc.,Dalton Trans.' _journal_coden_Cambridge 0186 loop_ _publ_author_name 'Antonio Sousa' 'Isabel Casanova' 'M. L. Duran' 'J. A. Garcia-Vazquez' 'J. Romero' A.Sousa-Pedrares data_[Zn(3-CF3-pyS)2(bipy)] _database_code_CSD 189578 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H14 F6 N4 S2 Zn' _chemical_formula_weight 577.86 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.261(4) _cell_length_b 13.050(7) _cell_length_c 13.345(7) _cell_angle_alpha 67.986(8) _cell_angle_beta 85.496(8) _cell_angle_gamma 82.258(8) _cell_volume 1321.0(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 877 _cell_measurement_theta_min 2.94 _cell_measurement_theta_max 25.68 _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.453 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 580 _exptl_absorpt_coefficient_mu 1.147 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.5924 _exptl_absorpt_correction_T_max 0.9449 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart-CCD-1000 BRUKER' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4500 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0681 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 24.71 _reflns_number_total 4500 _reflns_number_gt 2876 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER Smart' _computing_cell_refinement 'BRUKER Smart' _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1021P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4500 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0961 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1763 _refine_ls_wR_factor_gt 0.1491 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 Zn1 Zn 0.13370(7) 0.68190(5) 0.16499(5) 0.0583(3) Uani 1 1 d . . . S1 S 0.12354(16) 0.48915(11) 0.15882(13) 0.0650(4) Uani 1 1 d . . . S2 S -0.14508(18) 0.73671(11) 0.22428(12) 0.0665(4) Uani 1 1 d . . . F1 F 0.3340(6) 0.2422(3) 0.2465(4) 0.1112(13) Uani 1 1 d . . . F2 F 0.3369(6) 0.3139(4) 0.0763(4) 0.1149(14) Uani 1 1 d . . . F3 F 0.5557(5) 0.2369(4) 0.1553(6) 0.174(3) Uani 1 1 d . . . F4 F -0.4003(6) 0.6679(6) 0.4192(5) 0.160(2) Uani 1 1 d . . . F5 F -0.3533(8) 0.7045(7) 0.5550(5) 0.216(4) Uani 1 1 d . . . F6 F -0.3399(8) 0.8288(5) 0.3929(5) 0.173(3) Uani 1 1 d . . . N1 N 0.3678(5) 0.5873(3) 0.1721(4) 0.0598(11) Uani 1 1 d . . . N2 N 0.1069(6) 0.6500(4) 0.3422(4) 0.0700(13) Uani 1 1 d . . . N4 N 0.1054(5) 0.7757(3) -0.0045(3) 0.0551(10) Uani 1 1 d . . . N3 N 0.2389(5) 0.8380(3) 0.1351(4) 0.0603(11) Uani 1 1 d . . . C1 C 0.3299(6) 0.4916(4) 0.1657(4) 0.0532(12) Uani 1 1 d . . . C2 C 0.4573(7) 0.4084(4) 0.1664(5) 0.0670(15) Uani 1 1 d . . . C3 C 0.6156(7) 0.4262(6) 0.1744(6) 0.0861(19) Uani 1 1 d . . . H3 H 0.7001 0.3706 0.1763 0.103 Uiso 1 1 calc R . . C4 C 0.6522(7) 0.5241(6) 0.1795(6) 0.087(2) Uani 1 1 d . . . H4 H 0.7595 0.5365 0.1830 0.104 Uiso 1 1 calc R . . C5 C 0.5251(7) 0.6014(5) 0.1794(5) 0.0755(16) Uani 1 1 d . . . H5 H 0.5470 0.6673 0.1845 0.091 Uiso 1 1 calc R . . C6 C 0.4232(8) 0.3016(6) 0.1622(7) 0.091(2) Uani 1 1 d . . . C7 C -0.0515(7) 0.6877(4) 0.3473(5) 0.0633(14) Uani 1 1 d . . . C8 C -0.1278(9) 0.6824(6) 0.4461(5) 0.0836(18) Uani 1 1 d . . . C9 C -0.0341(12) 0.6379(7) 0.5366(6) 0.113(3) Uani 1 1 d . . . H9 H -0.0803 0.6333 0.6038 0.136 Uiso 1 1 calc R . . C10 C 0.1313(12) 0.5996(7) 0.5271(7) 0.119(3) Uani 1 1 d . . . H10 H 0.1960 0.5699 0.5876 0.143 Uiso 1 1 calc R . . C11 C 0.1942(9) 0.6063(6) 0.4302(7) 0.095(2) Uani 1 1 d . . . H11 H 0.3032 0.5794 0.4242 0.114 Uiso 1 1 calc R . . C12 C -0.3080(13) 0.7164(10) 0.4550(7) 0.130(3) Uani 1 1 d . . . C13 C 0.3067(8) 0.8649(5) 0.2097(5) 0.0787(17) Uani 1 1 d . . . H13 H 0.3170 0.8122 0.2795 0.094 Uiso 1 1 calc R . . C14 C 0.3609(8) 0.9661(5) 0.1872(6) 0.0820(18) Uani 1 1 d . . . H14 H 0.4090 0.9812 0.2401 0.098 Uiso 1 1 calc R . . C15 C 0.3428(8) 1.0444(5) 0.0853(6) 0.0820(18) Uani 1 1 d . . . H15 H 0.3779 1.1140 0.0678 0.098 Uiso 1 1 calc R . . C16 C 0.2722(7) 1.0189(4) 0.0094(5) 0.0711(16) Uani 1 1 d . . . H16 H 0.2579 1.0717 -0.0601 0.085 Uiso 1 1 calc R . . C17 C 0.2220(6) 0.9144(4) 0.0361(4) 0.0546(12) Uani 1 1 d . . . C18 C 0.1499(6) 0.8805(4) -0.0432(4) 0.0555(13) Uani 1 1 d . . . C19 C 0.1286(7) 0.9493(5) -0.1493(5) 0.0731(16) Uani 1 1 d . . . H19 H 0.1583 1.0211 -0.1745 0.088 Uiso 1 1 calc R . . C20 C 0.0617(8) 0.9098(6) -0.2187(5) 0.0843(18) Uani 1 1 d . . . H20 H 0.0465 0.9550 -0.2909 0.101 Uiso 1 1 calc R . . C21 C 0.0182(7) 0.8027(6) -0.1793(5) 0.0787(17) Uani 1 1 d . . . H21 H -0.0243 0.7742 -0.2247 0.094 Uiso 1 1 calc R . . C22 C 0.0394(6) 0.7395(5) -0.0720(5) 0.0648(14) Uani 1 1 d . . . H22 H 0.0065 0.6685 -0.0447 0.078 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 Zn1 0.0584(4) 0.0437(3) 0.0717(4) -0.0203(3) -0.0073(3) -0.0019(3) S1 0.0522(8) 0.0509(7) 0.0929(11) -0.0273(7) -0.0103(7) -0.0020(6) S2 0.0697(9) 0.0547(8) 0.0721(9) -0.0199(7) -0.0087(7) -0.0035(7) F1 0.132(4) 0.062(2) 0.136(4) -0.028(2) -0.014(3) -0.019(2) F2 0.140(4) 0.102(3) 0.131(4) -0.071(3) -0.011(3) -0.022(3) F3 0.089(3) 0.105(3) 0.372(9) -0.149(5) -0.008(4) 0.017(3) F4 0.097(4) 0.226(7) 0.157(5) -0.072(5) 0.010(3) -0.024(4) F5 0.184(6) 0.318(10) 0.107(4) -0.071(5) 0.033(4) 0.056(6) F6 0.175(6) 0.157(5) 0.162(5) -0.066(4) 0.001(4) 0.076(4) N1 0.056(3) 0.050(2) 0.071(3) -0.019(2) -0.009(2) -0.0060(19) N2 0.068(3) 0.051(2) 0.078(3) -0.009(2) -0.011(3) -0.004(2) N4 0.048(2) 0.049(2) 0.068(3) -0.024(2) -0.002(2) 0.0012(18) N3 0.062(3) 0.048(2) 0.071(3) -0.021(2) -0.008(2) -0.003(2) C1 0.051(3) 0.046(3) 0.060(3) -0.017(2) -0.006(2) -0.002(2) C2 0.060(3) 0.055(3) 0.090(4) -0.034(3) -0.006(3) 0.003(3) C3 0.055(4) 0.081(4) 0.131(6) -0.054(4) -0.012(4) 0.011(3) C4 0.055(4) 0.083(4) 0.132(6) -0.050(4) -0.014(4) 0.000(3) C5 0.067(4) 0.060(3) 0.102(5) -0.029(3) -0.015(3) -0.009(3) C6 0.072(4) 0.075(4) 0.141(7) -0.059(5) -0.018(5) 0.011(4) C7 0.075(4) 0.044(3) 0.068(4) -0.017(2) -0.003(3) -0.008(3) C8 0.095(5) 0.082(4) 0.071(4) -0.028(3) 0.000(4) -0.005(4) C9 0.154(8) 0.110(6) 0.070(5) -0.026(4) -0.006(5) -0.019(6) C10 0.127(7) 0.104(6) 0.103(7) -0.002(5) -0.060(6) -0.012(5) C11 0.093(5) 0.089(5) 0.086(5) -0.008(4) -0.018(4) -0.016(4) C12 0.132(9) 0.169(10) 0.082(6) -0.056(6) 0.006(6) 0.034(7) C13 0.105(5) 0.059(3) 0.075(4) -0.022(3) -0.022(4) -0.014(3) C14 0.085(4) 0.078(4) 0.099(5) -0.048(4) -0.010(4) -0.014(3) C15 0.086(4) 0.054(3) 0.113(5) -0.037(4) 0.000(4) -0.016(3) C16 0.077(4) 0.047(3) 0.086(4) -0.022(3) 0.000(3) -0.005(3) C17 0.046(3) 0.042(3) 0.070(3) -0.018(2) 0.001(2) 0.005(2) C18 0.045(3) 0.048(3) 0.072(4) -0.026(3) -0.001(2) 0.008(2) C19 0.079(4) 0.056(3) 0.074(4) -0.014(3) -0.006(3) 0.000(3) C20 0.084(4) 0.086(5) 0.070(4) -0.015(3) -0.018(3) -0.002(4) C21 0.071(4) 0.093(5) 0.082(5) -0.043(4) -0.012(3) -0.007(3) C22 0.054(3) 0.067(3) 0.080(4) -0.035(3) -0.007(3) -0.005(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 Zn1 N1 2.138(4) . ? Zn1 N4 2.144(4) . ? Zn1 N3 2.209(4) . ? Zn1 N2 2.241(5) . ? Zn1 S2 2.4770(19) . ? Zn1 S1 2.5602(19) . ? S1 C1 1.719(5) . ? S2 C7 1.727(6) . ? F1 C6 1.334(9) . ? F2 C6 1.344(8) . ? F3 C6 1.309(7) . ? F4 C12 1.275(12) . ? F5 C12 1.314(9) . ? F6 C12 1.388(12) . ? N1 C5 1.353(7) . ? N1 C1 1.362(6) . ? N2 C11 1.320(8) . ? N2 C7 1.340(7) . ? N4 C22 1.341(6) . ? N4 C18 1.360(6) . ? N3 C17 1.327(6) . ? N3 C13 1.353(7) . ? C1 C2 1.405(7) . ? C2 C3 1.378(8) . ? C2 C6 1.480(8) . ? C3 C4 1.380(8) . ? C4 C5 1.354(8) . ? C7 C8 1.397(8) . ? C8 C9 1.377(10) . ? C8 C12 1.503(11) . ? C9 C10 1.403(11) . ? C10 C11 1.331(11) . ? C13 C14 1.370(8) . ? C14 C15 1.365(9) . ? C15 C16 1.369(8) . ? C16 C17 1.388(7) . ? C17 C18 1.480(7) . ? C18 C19 1.373(8) . ? C19 C20 1.394(8) . ? C20 C21 1.383(9) . ? C21 C22 1.371(8) . ? 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 N1 Zn1 N4 103.56(16) . . ? N1 Zn1 N3 93.42(16) . . ? N4 Zn1 N3 75.13(16) . . ? N1 Zn1 N2 96.16(17) . . ? N4 Zn1 N2 156.20(16) . . ? N3 Zn1 N2 90.67(16) . . ? N1 Zn1 S2 158.59(13) . . ? N4 Zn1 S2 96.78(11) . . ? N3 Zn1 S2 98.25(12) . . ? N2 Zn1 S2 65.96(13) . . ? N1 Zn1 S1 65.97(12) . . ? N4 Zn1 S1 97.29(12) . . ? N3 Zn1 S1 156.15(12) . . ? N2 Zn1 S1 102.90(12) . . ? S2 Zn1 S1 105.15(5) . . ? C1 S1 Zn1 78.08(17) . . ? C7 S2 Zn1 81.1(2) . . ? C5 N1 C1 120.4(4) . . ? C5 N1 Zn1 137.0(4) . . ? C1 N1 Zn1 102.6(3) . . ? C11 N2 C7 121.0(6) . . ? C11 N2 Zn1 139.7(5) . . ? C7 N2 Zn1 99.3(3) . . ? C22 N4 C18 118.8(5) . . ? C22 N4 Zn1 124.1(4) . . ? C18 N4 Zn1 117.0(3) . . ? C17 N3 C13 118.1(5) . . ? C17 N3 Zn1 115.7(3) . . ? C13 N3 Zn1 126.0(4) . . ? N1 C1 C2 118.7(4) . . ? N1 C1 S1 113.3(3) . . ? C2 C1 S1 128.0(4) . . ? C3 C2 C1 118.9(5) . . ? C3 C2 C6 120.0(5) . . ? C1 C2 C6 121.1(5) . . ? C2 C3 C4 121.7(5) . . ? C5 C4 C3 117.1(5) . . ? N1 C5 C4 123.2(6) . . ? F3 C6 F1 107.1(6) . . ? F3 C6 F2 104.5(6) . . ? F1 C6 F2 103.8(6) . . ? F3 C6 C2 113.2(6) . . ? F1 C6 C2 113.9(6) . . ? F2 C6 C2 113.5(6) . . ? N2 C7 C8 120.6(5) . . ? N2 C7 S2 113.7(4) . . ? C8 C7 S2 125.7(5) . . ? C9 C8 C7 117.5(7) . . ? C9 C8 C12 120.9(7) . . ? C7 C8 C12 121.5(6) . . ? C8 C9 C10 119.8(8) . . ? C11 C10 C9 118.9(7) . . ? N2 C11 C10 122.2(7) . . ? F4 C12 F5 109.5(11) . . ? F4 C12 F6 105.3(9) . . ? F5 C12 F6 106.7(8) . . ? F4 C12 C8 115.3(8) . . ? F5 C12 C8 111.2(8) . . ? F6 C12 C8 108.4(9) . . ? N3 C13 C14 123.1(6) . . ? C15 C14 C13 118.5(6) . . ? C14 C15 C16 119.0(6) . . ? C15 C16 C17 120.0(6) . . ? N3 C17 C16 121.2(5) . . ? N3 C17 C18 116.2(4) . . ? C16 C17 C18 122.6(5) . . ? N4 C18 C19 121.4(5) . . ? N4 C18 C17 115.6(4) . . ? C19 C18 C17 122.9(5) . . ? C18 C19 C20 118.9(6) . . ? C21 C20 C19 119.5(6) . . ? C22 C21 C20 118.4(6) . . ? N4 C22 C21 122.8(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.727 _refine_diff_density_min -0.518 _refine_diff_density_rms 0.093 data_[Zn(5-CF3-pyS)2(bipy)] _database_code_CSD 189579 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H7 F3 N2 S Zn0.50' _chemical_formula_weight 288.93 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 6.5755(11) _cell_length_b 8.3861(14) _cell_length_c 20.449(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.060(3) _cell_angle_gamma 90.00 _cell_volume 1119.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 950 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 26.35 _exptl_crystal_description Prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.715 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 580 _exptl_absorpt_coefficient_mu 1.353 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.7198 _exptl_absorpt_correction_T_max 0.8331 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart-CCD-1000 BRUKER' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2287 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0273 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 26.41 _reflns_number_total 2287 _reflns_number_gt 1667 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER Smart' _computing_cell_refinement 'BRUKER Smart' _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0410P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2287 _refine_ls_number_parameters 159 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0464 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0758 _refine_ls_wR_factor_gt 0.0697 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.985 _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 Zn1 Zn 1.0000 0.06797(4) 0.2500 0.04570(14) Uani 1 2 d S . . S1 S 0.73864(9) -0.07441(7) 0.19054(3) 0.05006(17) Uani 1 1 d . . . F1 F 1.1345(2) -0.2856(2) -0.07941(7) 0.0931(6) Uani 1 1 d . . . F2 F 1.3761(3) -0.1412(2) -0.03228(8) 0.0839(5) Uani 1 1 d . . . F3 F 1.3536(2) -0.38205(18) -0.00465(8) 0.0749(5) Uani 1 1 d . . . N1 N 1.0710(3) -0.0691(2) 0.12925(9) 0.0463(5) Uani 1 1 d . . . N2 N 0.8477(3) 0.2634(2) 0.28625(8) 0.0398(4) Uani 1 1 d . . . C1 C 0.8809(3) -0.1296(3) 0.12837(11) 0.0440(5) Uani 1 1 d . . . C2 C 0.8025(4) -0.2330(3) 0.07819(13) 0.0569(6) Uani 1 1 d . . . H2 H 0.6723 -0.2759 0.0785 0.068 Uiso 1 1 calc R . . C3 C 0.9140(4) -0.2717(3) 0.02892(13) 0.0579(7) Uani 1 1 d . . . H3 H 0.8604 -0.3400 -0.0047 0.070 Uiso 1 1 calc R . . C4 C 1.1089(3) -0.2082(3) 0.02924(11) 0.0463(5) Uani 1 1 d . . . C5 C 1.1787(3) -0.1094(3) 0.08083(12) 0.0480(6) Uani 1 1 d . . . H5 H 1.3102 -0.0679 0.0819 0.058 Uiso 1 1 calc R . . C6 C 1.2390(4) -0.2525(3) -0.02124(13) 0.0555(6) Uani 1 1 d . . . C7 C 0.6867(4) 0.2547(3) 0.32044(12) 0.0514(6) Uani 1 1 d . . . H7 H 0.6407 0.1547 0.3317 0.062 Uiso 1 1 calc R . . C8 C 0.5868(4) 0.3875(3) 0.33948(12) 0.0598(7) Uani 1 1 d . . . H8 H 0.4753 0.3777 0.3631 0.072 Uiso 1 1 calc R . . C9 C 0.6546(4) 0.5343(3) 0.32304(13) 0.0622(7) Uani 1 1 d . . . H9 H 0.5897 0.6259 0.3356 0.075 Uiso 1 1 calc R . . C10 C 0.8201(4) 0.5463(3) 0.28773(12) 0.0521(6) Uani 1 1 d . . . H10 H 0.8686 0.6455 0.2764 0.063 Uiso 1 1 calc R . . C11 C 0.9123(3) 0.4072(2) 0.26962(10) 0.0381(5) 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 Zn1 0.0437(2) 0.0300(2) 0.0624(3) 0.000 0.00224(17) 0.000 S1 0.0447(3) 0.0468(4) 0.0587(4) -0.0054(3) 0.0064(3) -0.0041(2) F1 0.0789(11) 0.1407(17) 0.0568(10) -0.0268(10) -0.0035(8) 0.0171(10) F2 0.0997(13) 0.0689(11) 0.0901(12) -0.0028(9) 0.0396(10) -0.0091(9) F3 0.0769(11) 0.0589(10) 0.0904(11) -0.0003(8) 0.0161(9) 0.0239(8) N1 0.0466(11) 0.0375(10) 0.0540(11) -0.0060(9) 0.0029(9) -0.0042(8) N2 0.0387(9) 0.0348(10) 0.0461(10) 0.0048(8) 0.0058(8) 0.0013(7) C1 0.0429(13) 0.0338(12) 0.0530(13) -0.0006(10) -0.0032(10) 0.0013(9) C2 0.0488(14) 0.0553(16) 0.0662(16) -0.0144(12) 0.0053(12) -0.0111(11) C3 0.0562(15) 0.0527(15) 0.0621(16) -0.0183(12) -0.0042(13) -0.0060(12) C4 0.0480(13) 0.0389(12) 0.0501(13) -0.0009(10) -0.0012(11) 0.0060(10) C5 0.0424(13) 0.0422(13) 0.0590(15) -0.0040(11) 0.0043(11) -0.0028(10) C6 0.0589(16) 0.0490(15) 0.0567(16) -0.0062(12) -0.0007(12) 0.0062(12) C7 0.0490(13) 0.0522(15) 0.0537(14) 0.0114(11) 0.0089(11) -0.0001(11) C8 0.0532(15) 0.073(2) 0.0554(15) 0.0020(13) 0.0175(12) 0.0138(13) C9 0.0671(18) 0.0555(17) 0.0654(17) -0.0140(13) 0.0132(14) 0.0150(13) C10 0.0607(16) 0.0356(13) 0.0604(15) -0.0075(10) 0.0090(12) 0.0026(10) C11 0.0397(12) 0.0343(12) 0.0394(11) -0.0014(9) 0.0008(9) 0.0013(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 Zn1 N2 2.1023(17) . ? Zn1 N2 2.1023(17) 2_755 ? Zn1 S1 2.3117(6) . ? Zn1 S1 2.3117(6) 2_755 ? S1 C1 1.731(2) . ? F1 C6 1.328(3) . ? F2 C6 1.336(3) . ? F3 C6 1.342(3) . ? N1 C5 1.330(3) . ? N1 C1 1.347(3) . ? N2 C11 1.336(2) . ? N2 C7 1.341(3) . ? C1 C2 1.393(3) . ? C2 C3 1.356(3) . ? C3 C4 1.387(3) . ? C4 C5 1.375(3) . ? C4 C6 1.467(3) . ? C7 C8 1.374(3) . ? C8 C9 1.365(4) . ? C9 C10 1.382(3) . ? C10 C11 1.386(3) . ? C11 C11 1.484(4) 2_755 ? 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 Zn1 N2 77.58(9) . 2_755 ? N2 Zn1 S1 103.45(5) . . ? N2 Zn1 S1 124.94(5) 2_755 . ? N2 Zn1 S1 124.94(5) . 2_755 ? N2 Zn1 S1 103.45(5) 2_755 2_755 ? S1 Zn1 S1 117.80(3) . 2_755 ? C1 S1 Zn1 95.18(7) . . ? C5 N1 C1 118.20(19) . . ? C11 N2 C7 118.55(18) . . ? C11 N2 Zn1 115.70(14) . . ? C7 N2 Zn1 125.61(14) . . ? N1 C1 C2 120.2(2) . . ? N1 C1 S1 118.29(16) . . ? C2 C1 S1 121.52(17) . . ? C3 C2 C1 120.8(2) . . ? C2 C3 C4 119.2(2) . . ? C5 C4 C3 117.1(2) . . ? C5 C4 C6 121.6(2) . . ? C3 C4 C6 121.2(2) . . ? N1 C5 C4 124.5(2) . . ? F1 C6 F2 106.3(2) . . ? F1 C6 F3 105.7(2) . . ? F2 C6 F3 103.8(2) . . ? F1 C6 C4 113.6(2) . . ? F2 C6 C4 113.9(2) . . ? F3 C6 C4 112.6(2) . . ? N2 C7 C8 122.6(2) . . ? C9 C8 C7 118.7(2) . . ? C8 C9 C10 119.7(2) . . ? C9 C10 C11 118.5(2) . . ? N2 C11 C10 121.9(2) . . ? N2 C11 C11 115.47(11) . 2_755 ? C10 C11 C11 122.61(14) . 2_755 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.276 _refine_diff_density_min -0.289 _refine_diff_density_rms 0.048 data_[Zn(3-CF3-pyS)2(phen)] _database_code_CSD 189580 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H17 F6 N5 S2 Zn' _chemical_formula_weight 642.94 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0734(17) _cell_length_b 11.1806(17) _cell_length_c 11.8543(18) _cell_angle_alpha 92.975(2) _cell_angle_beta 108.253(2) _cell_angle_gamma 102.908(2) _cell_volume 1346.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1999 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 27.81 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.585 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 1.135 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.5397 _exptl_absorpt_correction_T_max 0.7884 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart-CCD-1000 BRUKER' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6395 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0241 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 28.31 _reflns_number_total 6395 _reflns_number_gt 5097 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER Smart' _computing_cell_refinement 'BRUKER Smart' _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0386P)^2^+0.4618P] 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 6395 _refine_ls_number_parameters 362 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0460 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0856 _refine_ls_wR_factor_gt 0.0766 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 Zn1 Zn 0.93179(2) 0.657372(19) 0.66537(2) 0.04174(8) Uani 1 1 d . . . S1 S 0.84912(5) 0.42269(5) 0.60526(5) 0.04767(13) Uani 1 1 d . . . S2 S 1.17413(6) 0.69319(5) 0.74118(5) 0.05184(13) Uani 1 1 d . . . F1 F 0.63042(16) 0.17924(13) 0.63266(16) 0.0826(5) Uani 1 1 d . . . F2 F 0.58832(16) 0.22720(14) 0.45600(14) 0.0793(4) Uani 1 1 d . . . F3 F 0.43539(15) 0.18463(15) 0.5300(2) 0.1015(6) Uani 1 1 d . . . F4 F 1.4439(2) 0.6984(3) 1.12088(19) 0.1536(11) Uani 1 1 d . . . F5 F 1.4284(2) 0.7997(3) 0.9767(2) 0.1444(10) Uani 1 1 d . . . F6 F 1.3977(2) 0.6077(3) 0.9442(3) 0.1552(11) Uani 1 1 d . . . N1 N 0.73160(16) 0.57887(15) 0.66512(15) 0.0454(4) Uani 1 1 d . . . N2 N 1.01417(18) 0.66582(15) 0.86216(15) 0.0500(4) Uani 1 1 d . . . N3 N 0.91482(16) 0.84863(14) 0.68071(15) 0.0441(4) Uani 1 1 d . . . N4 N 0.87370(15) 0.69642(14) 0.48222(14) 0.0406(3) Uani 1 1 d . . . C1 C 0.71329(18) 0.45792(17) 0.62529(16) 0.0402(4) Uani 1 1 d . . . C2 C 0.58941(19) 0.37545(18) 0.60604(18) 0.0443(4) Uani 1 1 d . . . C3 C 0.4937(2) 0.4184(2) 0.6344(2) 0.0560(5) Uani 1 1 d . . . H3 H 0.4125 0.3643 0.6230 0.067 Uiso 1 1 calc R . . C4 C 0.5168(2) 0.5405(2) 0.6792(2) 0.0622(6) Uani 1 1 d . . . H4 H 0.4534 0.5697 0.7002 0.075 Uiso 1 1 calc R . . C5 C 0.6367(2) 0.6175(2) 0.6919(2) 0.0564(5) Uani 1 1 d . . . H5 H 0.6529 0.7006 0.7204 0.068 Uiso 1 1 calc R . . C6 C 0.5610(2) 0.2432(2) 0.5570(2) 0.0579(6) Uani 1 1 d . . . C7 C 1.1415(2) 0.67974(17) 0.87363(18) 0.0470(5) Uani 1 1 d . . . C8 C 1.2321(2) 0.6796(2) 0.9887(2) 0.0597(6) Uani 1 1 d . . . C9 C 1.1861(3) 0.6664(2) 1.0846(2) 0.0712(7) Uani 1 1 d . . . H9 H 1.2447 0.6661 1.1604 0.085 Uiso 1 1 calc R . . C10 C 1.0564(3) 0.6538(2) 1.0697(2) 0.0685(7) Uani 1 1 d . . . H10 H 1.0256 0.6454 1.1342 0.082 Uiso 1 1 calc R . . C11 C 0.9733(3) 0.6540(2) 0.9568(2) 0.0593(6) Uani 1 1 d . . . H11 H 0.8846 0.6455 0.9453 0.071 Uiso 1 1 calc R . . C12 C 1.3730(3) 0.6925(4) 1.0075(3) 0.0956(10) Uani 1 1 d . . . C13 C 0.9407(2) 0.9243(2) 0.7797(2) 0.0568(5) Uani 1 1 d . . . H13 H 0.9692 0.8956 0.8532 0.068 Uiso 1 1 calc R . . C14 C 0.9270(3) 1.0452(2) 0.7785(2) 0.0649(6) Uani 1 1 d . . . H14 H 0.9466 1.0956 0.8501 0.078 Uiso 1 1 calc R . . C15 C 0.8847(2) 1.0889(2) 0.6722(2) 0.0602(6) Uani 1 1 d . . . H15 H 0.8745 1.1692 0.6704 0.072 Uiso 1 1 calc R . . C16 C 0.85656(19) 1.01194(18) 0.5649(2) 0.0494(5) Uani 1 1 d . . . C17 C 0.87423(17) 0.89138(16) 0.57430(18) 0.0410(4) Uani 1 1 d . . . C18 C 0.85099(17) 0.80973(17) 0.46800(18) 0.0411(4) Uani 1 1 d . . . C19 C 0.80724(19) 0.8496(2) 0.3551(2) 0.0505(5) Uani 1 1 d . . . C20 C 0.7854(2) 0.7654(3) 0.2546(2) 0.0621(6) Uani 1 1 d . . . H20 H 0.7556 0.7872 0.1780 0.075 Uiso 1 1 calc R . . C21 C 0.8081(2) 0.6508(2) 0.2696(2) 0.0605(6) Uani 1 1 d . . . H21 H 0.7938 0.5944 0.2033 0.073 Uiso 1 1 calc R . . C22 C 0.8530(2) 0.6195(2) 0.38515(19) 0.0491(5) Uani 1 1 d . . . H22 H 0.8690 0.5418 0.3945 0.059 Uiso 1 1 calc R . . C23 C 0.8135(2) 1.0499(2) 0.4491(3) 0.0611(6) Uani 1 1 d . . . H23 H 0.8016 1.1294 0.4424 0.073 Uiso 1 1 calc R . . C24 C 0.7897(2) 0.9730(2) 0.3496(2) 0.0625(6) Uani 1 1 d . . . H24 H 0.7611 1.0002 0.2752 0.075 Uiso 1 1 calc R . . N1S N 1.7535(5) 0.9083(6) 0.9785(4) 0.198(3) Uani 1 1 d . . . C1S C 1.6732(5) 0.9288(5) 0.9067(4) 0.1249(16) Uani 1 1 d . . . C2S C 1.5646(5) 0.9535(4) 0.8128(4) 0.1367(16) Uani 1 1 d . . . H2S1 H 1.5391 1.0223 0.8418 0.205 Uiso 1 1 calc R . . H2S2 H 1.4915 0.8817 0.7896 0.205 Uiso 1 1 calc R . . H2S3 H 1.5913 0.9727 0.7448 0.205 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 Zn1 0.04334(13) 0.03593(12) 0.04334(13) 0.00886(9) 0.00957(9) 0.01102(9) S1 0.0407(3) 0.0418(3) 0.0639(3) 0.0129(2) 0.0195(2) 0.0128(2) S2 0.0535(3) 0.0528(3) 0.0458(3) 0.0113(2) 0.0114(2) 0.0130(2) F1 0.0855(11) 0.0515(8) 0.1031(12) 0.0274(8) 0.0155(9) 0.0213(7) F2 0.0878(11) 0.0638(9) 0.0763(10) -0.0107(7) 0.0203(8) 0.0138(8) F3 0.0475(8) 0.0664(10) 0.1700(19) -0.0117(10) 0.0289(10) -0.0095(7) F4 0.0814(13) 0.257(3) 0.0820(13) 0.0405(17) -0.0226(11) 0.0303(16) F5 0.0751(13) 0.186(3) 0.136(2) 0.0375(18) 0.0173(13) -0.0171(15) F6 0.0862(15) 0.218(3) 0.148(2) -0.025(2) 0.0011(14) 0.0787(18) N1 0.0462(9) 0.0412(8) 0.0474(9) 0.0078(7) 0.0123(7) 0.0125(7) N2 0.0608(11) 0.0402(9) 0.0456(10) 0.0103(7) 0.0118(8) 0.0138(8) N3 0.0482(9) 0.0347(8) 0.0501(9) 0.0088(7) 0.0162(7) 0.0117(7) N4 0.0367(8) 0.0417(8) 0.0439(9) 0.0083(7) 0.0129(7) 0.0112(6) C1 0.0387(9) 0.0419(10) 0.0396(10) 0.0135(8) 0.0099(8) 0.0119(8) C2 0.0380(10) 0.0462(10) 0.0454(11) 0.0128(8) 0.0085(8) 0.0106(8) C3 0.0427(11) 0.0630(14) 0.0654(14) 0.0173(11) 0.0199(10) 0.0147(10) C4 0.0587(14) 0.0712(16) 0.0705(15) 0.0152(12) 0.0310(12) 0.0291(12) C5 0.0628(14) 0.0537(12) 0.0570(13) 0.0066(10) 0.0196(11) 0.0241(11) C6 0.0424(11) 0.0493(12) 0.0742(16) 0.0094(11) 0.0121(11) 0.0065(9) C7 0.0553(12) 0.0338(9) 0.0436(11) 0.0061(8) 0.0064(9) 0.0093(8) C8 0.0633(14) 0.0542(13) 0.0460(12) 0.0081(10) 0.0003(10) 0.0093(11) C9 0.095(2) 0.0597(14) 0.0405(12) 0.0083(10) 0.0021(12) 0.0116(14) C10 0.102(2) 0.0527(13) 0.0495(13) 0.0075(10) 0.0272(14) 0.0145(13) C11 0.0749(16) 0.0460(12) 0.0599(14) 0.0090(10) 0.0265(12) 0.0149(11) C12 0.069(2) 0.126(3) 0.0680(19) 0.0155(19) -0.0060(15) 0.020(2) C13 0.0723(15) 0.0412(11) 0.0572(13) 0.0052(9) 0.0216(11) 0.0152(10) C14 0.0770(17) 0.0411(11) 0.0790(17) -0.0016(11) 0.0314(14) 0.0138(11) C15 0.0551(13) 0.0345(10) 0.0957(19) 0.0088(11) 0.0292(13) 0.0148(9) C16 0.0350(9) 0.0380(10) 0.0775(15) 0.0200(10) 0.0196(10) 0.0101(8) C17 0.0315(9) 0.0348(9) 0.0581(12) 0.0132(8) 0.0152(8) 0.0091(7) C18 0.0300(9) 0.0428(10) 0.0514(11) 0.0155(8) 0.0129(8) 0.0099(7) C19 0.0372(10) 0.0595(12) 0.0565(13) 0.0250(10) 0.0155(9) 0.0117(9) C20 0.0511(13) 0.0843(17) 0.0509(13) 0.0247(12) 0.0164(10) 0.0143(12) C21 0.0557(13) 0.0770(16) 0.0470(12) 0.0041(11) 0.0190(10) 0.0114(12) C22 0.0451(11) 0.0528(12) 0.0522(12) 0.0062(9) 0.0192(9) 0.0137(9) C23 0.0482(12) 0.0495(12) 0.0919(19) 0.0350(13) 0.0237(12) 0.0191(10) C24 0.0480(12) 0.0679(15) 0.0756(17) 0.0420(14) 0.0181(11) 0.0190(11) N1S 0.125(3) 0.341(8) 0.126(4) 0.103(4) 0.038(3) 0.043(4) C1S 0.125(4) 0.164(4) 0.077(2) 0.034(3) 0.039(2) 0.008(3) C2S 0.177(5) 0.127(4) 0.093(3) 0.023(3) 0.025(3) 0.039(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 Zn1 N4 2.1603(16) . ? Zn1 N3 2.1913(16) . ? Zn1 N1 2.1934(17) . ? Zn1 N2 2.2111(17) . ? Zn1 S2 2.4781(7) . ? Zn1 S1 2.5602(7) . ? S1 C1 1.718(2) . ? S2 C7 1.724(2) . ? F1 C6 1.337(3) . ? F2 C6 1.336(3) . ? F3 C6 1.326(3) . ? F4 C12 1.317(3) . ? F5 C12 1.343(4) . ? F6 C12 1.306(4) . ? N1 C5 1.337(3) . ? N1 C1 1.358(2) . ? N2 C11 1.337(3) . ? N2 C7 1.346(3) . ? N3 C13 1.324(3) . ? N3 C17 1.351(2) . ? N4 C22 1.327(3) . ? N4 C18 1.355(2) . ? C1 C2 1.415(3) . ? C2 C3 1.379(3) . ? C2 C6 1.487(3) . ? C3 C4 1.376(3) . ? C4 C5 1.370(3) . ? C7 C8 1.418(3) . ? C8 C9 1.385(4) . ? C8 C12 1.478(4) . ? C9 C10 1.365(4) . ? C10 C11 1.367(4) . ? C13 C14 1.394(3) . ? C14 C15 1.358(4) . ? C15 C16 1.405(3) . ? C16 C17 1.410(3) . ? C16 C23 1.426(3) . ? C17 C18 1.435(3) . ? C18 C19 1.406(3) . ? C19 C20 1.402(3) . ? C19 C24 1.437(3) . ? C20 C21 1.370(4) . ? C21 C22 1.396(3) . ? C23 C24 1.342(4) . ? N1S C1S 1.098(6) . ? C1S C2S 1.450(6) . ? 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 N4 Zn1 N3 76.18(6) . . ? N4 Zn1 N1 95.66(6) . . ? N3 Zn1 N1 93.63(6) . . ? N4 Zn1 N2 166.15(6) . . ? N3 Zn1 N2 91.79(6) . . ? N1 Zn1 N2 91.88(7) . . ? N4 Zn1 S2 108.25(4) . . ? N3 Zn1 S2 100.11(5) . . ? N1 Zn1 S2 154.62(5) . . ? N2 Zn1 S2 66.63(5) . . ? N4 Zn1 S1 93.55(4) . . ? N3 Zn1 S1 156.05(5) . . ? N1 Zn1 S1 65.52(4) . . ? N2 Zn1 S1 100.15(5) . . ? S2 Zn1 S1 103.669(19) . . ? C1 S1 Zn1 78.89(7) . . ? C7 S2 Zn1 80.03(7) . . ? C5 N1 C1 120.46(18) . . ? C5 N1 Zn1 138.33(15) . . ? C1 N1 Zn1 101.20(12) . . ? C11 N2 C7 121.2(2) . . ? C11 N2 Zn1 139.54(17) . . ? C7 N2 Zn1 99.05(13) . . ? C13 N3 C17 118.21(17) . . ? C13 N3 Zn1 127.90(14) . . ? C17 N3 Zn1 113.89(13) . . ? C22 N4 C18 118.45(17) . . ? C22 N4 Zn1 126.63(14) . . ? C18 N4 Zn1 114.84(13) . . ? N1 C1 C2 118.64(18) . . ? N1 C1 S1 114.22(14) . . ? C2 C1 S1 127.13(15) . . ? C3 C2 C1 119.3(2) . . ? C3 C2 C6 119.47(19) . . ? C1 C2 C6 121.26(19) . . ? C4 C3 C2 120.8(2) . . ? C5 C4 C3 117.6(2) . . ? N1 C5 C4 123.2(2) . . ? F3 C6 F2 105.3(2) . . ? F3 C6 F1 106.7(2) . . ? F2 C6 F1 105.2(2) . . ? F3 C6 C2 112.6(2) . . ? F2 C6 C2 113.55(19) . . ? F1 C6 C2 112.9(2) . . ? N2 C7 C8 118.4(2) . . ? N2 C7 S2 114.15(15) . . ? C8 C7 S2 127.40(19) . . ? C9 C8 C7 118.7(2) . . ? C9 C8 C12 120.0(2) . . ? C7 C8 C12 121.3(2) . . ? C10 C9 C8 121.2(2) . . ? C9 C10 C11 117.6(2) . . ? N2 C11 C10 122.8(3) . . ? F6 C12 F4 108.9(3) . . ? F6 C12 F5 104.4(4) . . ? F4 C12 F5 103.1(3) . . ? F6 C12 C8 114.8(3) . . ? F4 C12 C8 113.1(3) . . ? F5 C12 C8 111.7(3) . . ? N3 C13 C14 122.9(2) . . ? C15 C14 C13 119.6(2) . . ? C14 C15 C16 119.5(2) . . ? C15 C16 C17 117.2(2) . . ? C15 C16 C23 123.6(2) . . ? C17 C16 C23 119.1(2) . . ? N3 C17 C16 122.62(19) . . ? N3 C17 C18 117.56(16) . . ? C16 C17 C18 119.81(18) . . ? N4 C18 C19 122.94(19) . . ? N4 C18 C17 117.44(17) . . ? C19 C18 C17 119.62(18) . . ? C20 C19 C18 116.9(2) . . ? C20 C19 C24 124.3(2) . . ? C18 C19 C24 118.7(2) . . ? C21 C20 C19 119.8(2) . . ? C20 C21 C22 119.3(2) . . ? N4 C22 C21 122.5(2) . . ? C24 C23 C16 121.1(2) . . ? C23 C24 C19 121.6(2) . . ? N1S C1S C2S 178.4(6) . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 0.381 _refine_diff_density_min -0.273 _refine_diff_density_rms 0.047 data_[Cd2(5-CF3-pyS)4(DMF)]n _database_code_CSD 189581 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H19 Cd2 F12 N5 O S4' _chemical_formula_weight 1010.51 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' Cd Cd -0.8075 1.2024 '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 Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4195(16) _cell_length_b 12.4903(17) _cell_length_c 14.651(2) _cell_angle_alpha 64.648(4) _cell_angle_beta 69.447(4) _cell_angle_gamma 77.377(4) _cell_volume 1762.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.904 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 1.539 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.5017 _exptl_absorpt_correction_T_max 0.7484 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33971 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 30.58 _reflns_number_total 10697 _reflns_number_gt 7627 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0399P)^2^+0.6024P] 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 10697 _refine_ls_number_parameters 462 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0552 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0866 _refine_ls_wR_factor_gt 0.0758 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _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 Cd1 Cd 0.860024(17) 0.508292(16) 0.125674(15) 0.03587(6) Uani 1 1 d . . . Cd2 Cd 0.645171(18) 0.434378(17) 0.411285(15) 0.03932(6) Uani 1 1 d . . . S1 S 1.11691(7) 0.57336(6) 0.02101(6) 0.04179(15) Uani 1 1 d . . . S2 S 0.70398(7) 0.30966(6) 0.29245(6) 0.04359(16) Uani 1 1 d . . . S3 S 0.80922(7) 0.59263(6) 0.28046(6) 0.04052(15) Uani 1 1 d . . . S4 S 0.56961(7) 0.45328(6) 0.61601(6) 0.04352(16) Uani 1 1 d . . . F1 F 0.6808(3) 1.0138(3) -0.0592(3) 0.1405(14) Uani 1 1 d . . . F2 F 0.8135(4) 1.0851(3) -0.1992(3) 0.1591(18) Uani 1 1 d . . . F3 F 0.8186(6) 1.1030(4) -0.0679(6) 0.268(4) Uani 1 1 d . . . F4 F 1.3035(3) 0.1387(4) 0.1937(3) 0.1406(15) Uani 1 1 d . . . F5 F 1.2883(3) 0.2133(3) 0.2990(4) 0.1320(13) Uani 1 1 d . . . F6 F 1.2547(3) 0.0362(3) 0.3560(3) 0.1302(13) Uani 1 1 d . . . F7 F 1.1387(4) 0.1425(2) 0.5370(3) 0.1218(13) Uani 1 1 d . . . F8 F 1.2289(3) 0.2733(3) 0.5351(3) 0.1203(11) Uani 1 1 d . . . F9 F 1.0636(3) 0.2172(3) 0.6510(2) 0.1184(11) Uani 1 1 d . . . F10 F 0.4720(4) -0.0474(3) 0.6174(3) 0.1340(14) Uani 1 1 d . . . F11 F 0.2919(3) -0.0006(2) 0.7044(3) 0.1187(11) Uani 1 1 d . . . F12 F 0.4255(3) -0.1015(2) 0.7801(2) 0.1015(9) Uani 1 1 d . . . N1 N 0.9061(2) 0.7076(2) 0.01185(17) 0.0402(5) Uani 1 1 d . . . N2 N 0.9478(2) 0.32658(19) 0.23081(17) 0.0386(5) Uani 1 1 d . . . N3 N 0.8564(2) 0.3979(2) 0.43492(18) 0.0406(5) Uani 1 1 d . . . N4 N 0.5555(2) 0.2786(2) 0.56584(18) 0.0398(5) Uani 1 1 d . . . N5 N 0.4674(3) 0.5724(3) 0.0991(3) 0.0708(9) Uani 1 1 d . . . O1 O 0.6608(2) 0.6004(2) 0.08889(19) 0.0552(5) Uani 1 1 d . . . C1 C 1.0318(3) 0.7098(2) -0.0210(2) 0.0385(6) Uani 1 1 d . . . C2 C 1.0876(3) 0.8170(3) -0.0833(3) 0.0534(8) Uani 1 1 d . . . H2 H 1.1745 0.8177 -0.1071 0.064 Uiso 1 1 calc R . . C3 C 1.0134(4) 0.9207(3) -0.1090(3) 0.0633(9) Uani 1 1 d . . . H3 H 1.0493 0.9927 -0.1501 0.076 Uiso 1 1 calc R . . C4 C 0.8842(4) 0.9178(3) -0.0733(3) 0.0577(8) Uani 1 1 d . . . C5 C 0.8346(3) 0.8099(3) -0.0142(2) 0.0500(7) Uani 1 1 d . . . H5 H 0.7479 0.8077 0.0088 0.060 Uiso 1 1 calc R . . C6 C 0.8019(5) 1.0295(4) -0.0989(4) 0.0907(15) Uani 1 1 d . . . C7 C 0.8555(3) 0.2543(2) 0.2973(2) 0.0375(6) Uani 1 1 d . . . C8 C 0.8845(3) 0.1381(2) 0.3635(2) 0.0492(7) Uani 1 1 d . . . H8 H 0.8209 0.0881 0.4096 0.059 Uiso 1 1 calc R . . C9 C 1.0073(3) 0.0989(3) 0.3595(3) 0.0553(8) Uani 1 1 d . . . H9 H 1.0279 0.0214 0.4018 0.066 Uiso 1 1 calc R . . C10 C 1.1007(3) 0.1756(3) 0.2921(2) 0.0485(7) Uani 1 1 d . . . C11 C 1.0662(3) 0.2881(3) 0.2294(2) 0.0439(6) Uani 1 1 d . . . H11 H 1.1285 0.3397 0.1840 0.053 Uiso 1 1 calc R . . C12 C 1.2358(4) 0.1397(4) 0.2842(3) 0.0703(10) Uani 1 1 d . . . C13 C 0.9073(2) 0.4958(2) 0.3552(2) 0.0363(5) Uani 1 1 d . . . C14 C 1.0297(3) 0.5178(3) 0.3363(2) 0.0461(7) Uani 1 1 d . . . H14 H 1.0636 0.5861 0.2813 0.055 Uiso 1 1 calc R . . C15 C 1.0999(3) 0.4371(3) 0.4000(3) 0.0508(7) Uani 1 1 d . . . H15 H 1.1816 0.4508 0.3888 0.061 Uiso 1 1 calc R . . C16 C 1.0477(3) 0.3355(3) 0.4808(2) 0.0464(7) Uani 1 1 d . . . C17 C 0.9257(3) 0.3199(3) 0.4955(2) 0.0458(7) Uani 1 1 d . . . H17 H 0.8901 0.2521 0.5501 0.055 Uiso 1 1 calc R . . C18 C 1.1209(4) 0.2431(3) 0.5490(3) 0.0617(9) Uani 1 1 d . . . C19 C 0.5282(3) 0.3127(2) 0.6469(2) 0.0402(6) Uani 1 1 d . . . C20 C 0.4680(3) 0.2381(3) 0.7488(2) 0.0576(8) Uani 1 1 d . . . H20 H 0.4525 0.2598 0.8056 0.069 Uiso 1 1 calc R . . C21 C 0.4318(3) 0.1316(3) 0.7645(3) 0.0605(9) Uani 1 1 d . . . H21 H 0.3909 0.0813 0.8321 0.073 Uiso 1 1 calc R . . C22 C 0.4562(3) 0.1003(3) 0.6802(2) 0.0477(7) Uani 1 1 d . . . C23 C 0.5198(3) 0.1756(3) 0.5818(2) 0.0453(6) Uani 1 1 d . . . H23 H 0.5386 0.1540 0.5245 0.054 Uiso 1 1 calc R . . C24 C 0.4117(4) -0.0104(3) 0.6940(3) 0.0625(9) Uani 1 1 d . . . C25 C 0.5761(3) 0.5387(3) 0.1170(3) 0.0555(8) Uani 1 1 d . . . H25 H 0.5905 0.4582 0.1558 0.067 Uiso 1 1 calc R . . C26 C 0.4361(7) 0.6954(6) 0.0419(8) 0.172(4) Uani 1 1 d . . . H26A H 0.3766 0.7289 0.0898 0.258 Uiso 1 1 calc R . . H26B H 0.4001 0.7021 -0.0108 0.258 Uiso 1 1 calc R . . H26C H 0.5105 0.7374 0.0083 0.258 Uiso 1 1 calc R . . C27 C 0.3721(5) 0.4880(7) 0.1456(4) 0.137(3) Uani 1 1 d . . . H27A H 0.3485 0.4839 0.0905 0.205 Uiso 1 1 calc R . . H27B H 0.2999 0.5137 0.1919 0.205 Uiso 1 1 calc R . . H27C H 0.4053 0.4110 0.1850 0.205 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 Cd1 0.03120(10) 0.03295(9) 0.03533(10) -0.00735(7) -0.00918(8) -0.00006(7) Cd2 0.03099(10) 0.03693(10) 0.03965(11) -0.01139(8) -0.00151(8) -0.00454(7) S1 0.0394(4) 0.0427(3) 0.0413(4) -0.0114(3) -0.0150(3) -0.0040(3) S2 0.0408(4) 0.0427(4) 0.0468(4) -0.0195(3) -0.0111(3) -0.0005(3) S3 0.0381(4) 0.0379(3) 0.0421(4) -0.0140(3) -0.0094(3) -0.0032(3) S4 0.0354(4) 0.0440(4) 0.0505(4) -0.0200(3) -0.0104(3) -0.0017(3) F1 0.097(2) 0.098(2) 0.152(3) -0.023(2) -0.014(2) 0.0451(19) F2 0.149(3) 0.099(2) 0.126(3) 0.023(2) -0.033(2) 0.037(2) F3 0.340(7) 0.146(4) 0.530(11) -0.245(6) -0.337(8) 0.167(5) F4 0.0569(16) 0.251(5) 0.106(2) -0.090(3) -0.0229(16) 0.046(2) F5 0.0756(19) 0.132(3) 0.222(4) -0.082(3) -0.075(2) 0.0107(18) F6 0.0786(18) 0.098(2) 0.158(3) 0.0050(19) -0.0591(19) 0.0279(15) F7 0.190(3) 0.0590(14) 0.167(3) -0.0540(17) -0.129(3) 0.0438(18) F8 0.100(2) 0.096(2) 0.167(3) -0.0068(19) -0.096(2) -0.0083(16) F9 0.132(3) 0.126(2) 0.0695(17) -0.0119(16) -0.0498(17) 0.024(2) F10 0.183(3) 0.105(2) 0.115(2) -0.0595(19) 0.025(2) -0.088(2) F11 0.0751(17) 0.0768(17) 0.198(3) -0.0180(19) -0.067(2) -0.0209(13) F12 0.131(2) 0.0468(12) 0.114(2) 0.0070(13) -0.0587(19) -0.0235(13) N1 0.0382(12) 0.0405(12) 0.0349(11) -0.0113(9) -0.0059(9) -0.0045(9) N2 0.0390(12) 0.0334(11) 0.0363(11) -0.0098(9) -0.0082(9) -0.0015(9) N3 0.0385(12) 0.0432(12) 0.0363(12) -0.0129(10) -0.0065(10) -0.0085(10) N4 0.0360(12) 0.0377(11) 0.0374(12) -0.0112(9) -0.0036(9) -0.0059(9) N5 0.0378(15) 0.113(3) 0.0676(19) -0.0401(19) -0.0221(14) 0.0053(16) O1 0.0393(12) 0.0523(12) 0.0706(15) -0.0195(11) -0.0201(11) 0.0010(10) C1 0.0422(15) 0.0401(13) 0.0320(13) -0.0140(11) -0.0077(11) -0.0063(11) C2 0.0473(17) 0.0464(16) 0.0590(19) -0.0170(14) -0.0038(14) -0.0163(13) C3 0.074(2) 0.0370(16) 0.062(2) -0.0108(14) -0.0070(18) -0.0124(15) C4 0.069(2) 0.0406(16) 0.0507(18) -0.0147(14) -0.0129(16) 0.0061(15) C5 0.0470(17) 0.0493(16) 0.0455(16) -0.0179(13) -0.0100(13) 0.0055(13) C6 0.097(4) 0.050(2) 0.103(4) -0.025(2) -0.025(3) 0.020(2) C7 0.0413(15) 0.0347(12) 0.0348(13) -0.0147(10) -0.0092(11) -0.0001(11) C8 0.0530(18) 0.0338(13) 0.0471(16) -0.0065(12) -0.0106(14) -0.0031(12) C9 0.067(2) 0.0372(14) 0.0501(18) -0.0071(13) -0.0236(16) 0.0086(14) C10 0.0460(17) 0.0479(16) 0.0482(17) -0.0178(13) -0.0178(14) 0.0080(13) C11 0.0430(16) 0.0434(15) 0.0395(14) -0.0128(12) -0.0105(12) -0.0014(12) C12 0.056(2) 0.073(2) 0.076(3) -0.026(2) -0.029(2) 0.0161(19) C13 0.0341(13) 0.0387(13) 0.0375(13) -0.0184(11) -0.0071(11) -0.0035(10) C14 0.0371(15) 0.0452(15) 0.0494(16) -0.0134(13) -0.0065(12) -0.0110(12) C15 0.0373(15) 0.0571(18) 0.0611(19) -0.0239(15) -0.0153(14) -0.0059(13) C16 0.0511(17) 0.0452(15) 0.0521(17) -0.0232(13) -0.0222(14) 0.0000(13) C17 0.0519(17) 0.0416(14) 0.0420(15) -0.0130(12) -0.0127(13) -0.0080(12) C18 0.069(2) 0.0542(19) 0.070(2) -0.0221(17) -0.038(2) 0.0047(17) C19 0.0322(13) 0.0402(13) 0.0395(14) -0.0107(11) -0.0092(11) 0.0016(10) C20 0.070(2) 0.0539(18) 0.0373(16) -0.0151(14) -0.0056(15) -0.0037(16) C21 0.064(2) 0.0498(18) 0.0407(16) -0.0025(13) 0.0002(15) -0.0103(15) C22 0.0404(15) 0.0400(14) 0.0494(17) -0.0068(12) -0.0088(13) -0.0071(12) C23 0.0442(16) 0.0422(15) 0.0441(15) -0.0147(12) -0.0080(13) -0.0054(12) C24 0.058(2) 0.0504(18) 0.067(2) -0.0060(16) -0.0158(17) -0.0201(16) C25 0.0406(17) 0.066(2) 0.0541(19) -0.0126(16) -0.0207(14) -0.0040(15) C26 0.145(6) 0.127(5) 0.302(11) -0.100(7) -0.162(8) 0.078(5) C27 0.067(3) 0.244(8) 0.091(4) -0.029(4) -0.023(3) -0.073(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N2 2.371(2) . ? Cd1 N1 2.378(2) . ? Cd1 O1 2.444(2) . ? Cd1 S1 2.6627(8) 2_765 ? Cd1 S3 2.7284(8) . ? Cd1 S1 2.9041(8) . ? Cd1 S2 2.9975(8) . ? Cd2 N4 2.331(2) . ? Cd2 N3 2.473(2) . ? Cd2 S4 2.6170(8) 2_666 ? Cd2 S3 2.6350(8) . ? Cd2 S2 2.6370(8) . ? Cd2 S4 2.9150(9) . ? S1 C1 1.739(3) . ? S1 Cd1 2.6627(8) 2_765 ? S2 C7 1.731(3) . ? S3 C13 1.747(3) . ? S4 C19 1.745(3) . ? S4 Cd2 2.6170(8) 2_666 ? F1 C6 1.322(6) . ? F2 C6 1.300(6) . ? F3 C6 1.255(6) . ? F4 C12 1.284(5) . ? F5 C12 1.324(5) . ? F6 C12 1.303(5) . ? F7 C18 1.306(4) . ? F8 C18 1.291(5) . ? F9 C18 1.326(5) . ? F10 C24 1.307(5) . ? F11 C24 1.305(4) . ? F12 C24 1.320(4) . ? N1 C5 1.338(4) . ? N1 C1 1.347(4) . ? N2 C11 1.329(4) . ? N2 C7 1.348(4) . ? N3 C17 1.334(4) . ? N3 C13 1.345(3) . ? N4 C23 1.334(4) . ? N4 C19 1.343(4) . ? N5 C25 1.301(4) . ? N5 C26 1.434(7) . ? N5 C27 1.457(6) . ? O1 C25 1.214(4) . ? C1 C2 1.396(4) . ? C2 C3 1.365(5) . ? C3 C4 1.384(5) . ? C4 C5 1.370(5) . ? C4 C6 1.482(5) . ? C7 C8 1.402(4) . ? C8 C9 1.370(5) . ? C9 C10 1.388(5) . ? C10 C11 1.371(4) . ? C10 C12 1.487(5) . ? C13 C14 1.391(4) . ? C14 C15 1.377(4) . ? C15 C16 1.384(5) . ? C16 C17 1.377(4) . ? C16 C18 1.486(4) . ? C19 C20 1.392(4) . ? C20 C21 1.380(5) . ? C21 C22 1.371(5) . ? C22 C23 1.376(4) . ? C22 C24 1.486(5) . ? 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 Cd1 N1 142.05(8) . . ? N2 Cd1 O1 140.59(8) . . ? N1 Cd1 O1 77.09(8) . . ? N2 Cd1 S1 92.57(6) . 2_765 ? N1 Cd1 S1 98.21(6) . 2_765 ? O1 Cd1 S1 82.93(6) . 2_765 ? N2 Cd1 S3 89.87(6) . . ? N1 Cd1 S3 83.24(6) . . ? O1 Cd1 S3 91.60(6) . . ? S1 Cd1 S3 173.85(2) 2_765 . ? N2 Cd1 S1 85.60(6) . . ? N1 Cd1 S1 58.61(6) . . ? O1 Cd1 S1 133.10(6) . . ? S1 Cd1 S1 88.52(2) 2_765 . ? S3 Cd1 S1 97.29(2) . . ? N2 Cd1 S2 57.35(6) . . ? N1 Cd1 S2 157.21(6) . . ? O1 Cd1 S2 83.51(6) . . ? S1 Cd1 S2 91.07(2) 2_765 . ? S3 Cd1 S2 85.49(2) . . ? S1 Cd1 S2 142.90(2) . . ? N4 Cd2 N3 96.58(8) . . ? N4 Cd2 S4 94.77(6) . 2_666 ? N3 Cd2 S4 159.47(6) . 2_666 ? N4 Cd2 S3 156.98(6) . . ? N3 Cd2 S3 61.78(5) . . ? S4 Cd2 S3 103.78(3) 2_666 . ? N4 Cd2 S2 94.06(6) . . ? N3 Cd2 S2 93.91(6) . . ? S4 Cd2 S2 102.30(2) 2_666 . ? S3 Cd2 S2 95.15(3) . . ? N4 Cd2 S4 59.04(6) . . ? N3 Cd2 S4 82.47(5) . . ? S4 Cd2 S4 88.82(2) 2_666 . ? S3 Cd2 S4 107.24(2) . . ? S2 Cd2 S4 151.94(2) . . ? C1 S1 Cd1 102.21(9) . 2_765 ? C1 S1 Cd1 78.06(9) . . ? Cd1 S1 Cd1 91.48(2) 2_765 . ? C7 S2 Cd2 100.75(9) . . ? C7 S2 Cd1 76.37(9) . . ? Cd2 S2 Cd1 86.07(2) . . ? C13 S3 Cd2 83.56(9) . . ? C13 S3 Cd1 101.59(9) . . ? Cd2 S3 Cd1 91.87(2) . . ? C19 S4 Cd2 95.52(9) . 2_666 ? C19 S4 Cd2 76.49(10) . . ? Cd2 S4 Cd2 91.18(2) 2_666 . ? C5 N1 C1 119.2(3) . . ? C5 N1 Cd1 133.2(2) . . ? C1 N1 Cd1 107.22(17) . . ? C11 N2 C7 119.8(2) . . ? C11 N2 Cd1 130.97(19) . . ? C7 N2 Cd1 109.15(17) . . ? C17 N3 C13 119.1(2) . . ? C17 N3 Cd2 141.98(19) . . ? C13 N3 Cd2 98.97(17) . . ? C23 N4 C19 120.2(2) . . ? C23 N4 Cd2 131.52(19) . . ? C19 N4 Cd2 107.94(17) . . ? C25 N5 C26 120.1(4) . . ? C25 N5 C27 120.4(4) . . ? C26 N5 C27 119.3(4) . . ? C25 O1 Cd1 119.6(2) . . ? N1 C1 C2 120.7(3) . . ? N1 C1 S1 116.0(2) . . ? C2 C1 S1 123.3(2) . . ? C3 C2 C1 119.4(3) . . ? C2 C3 C4 119.5(3) . . ? C5 C4 C3 118.6(3) . . ? C5 C4 C6 121.0(4) . . ? C3 C4 C6 120.3(4) . . ? N1 C5 C4 122.6(3) . . ? F3 C6 F2 106.7(5) . . ? F3 C6 F1 106.0(5) . . ? F2 C6 F1 101.8(5) . . ? F3 C6 C4 113.8(5) . . ? F2 C6 C4 113.6(4) . . ? F1 C6 C4 113.9(4) . . ? N2 C7 C8 120.1(3) . . ? N2 C7 S2 117.10(19) . . ? C8 C7 S2 122.7(2) . . ? C9 C8 C7 119.4(3) . . ? C8 C9 C10 119.6(3) . . ? C11 C10 C9 118.2(3) . . ? C11 C10 C12 119.1(3) . . ? C9 C10 C12 122.6(3) . . ? N2 C11 C10 122.9(3) . . ? F4 C12 F6 108.0(4) . . ? F4 C12 F5 104.5(4) . . ? F6 C12 F5 104.3(4) . . ? F4 C12 C10 114.0(3) . . ? F6 C12 C10 113.0(4) . . ? F5 C12 C10 112.3(3) . . ? N3 C13 C14 121.2(3) . . ? N3 C13 S3 115.7(2) . . ? C14 C13 S3 123.1(2) . . ? C15 C14 C13 119.2(3) . . ? C14 C15 C16 119.4(3) . . ? C17 C16 C15 118.3(3) . . ? C17 C16 C18 120.0(3) . . ? C15 C16 C18 121.7(3) . . ? N3 C17 C16 122.8(3) . . ? F8 C18 F7 107.9(3) . . ? F8 C18 F9 103.9(3) . . ? F7 C18 F9 105.3(4) . . ? F8 C18 C16 114.2(3) . . ? F7 C18 C16 112.2(3) . . ? F9 C18 C16 112.7(3) . . ? N4 C19 C20 120.1(3) . . ? N4 C19 S4 116.5(2) . . ? C20 C19 S4 123.4(2) . . ? C21 C20 C19 119.2(3) . . ? C22 C21 C20 119.8(3) . . ? C21 C22 C23 118.5(3) . . ? C21 C22 C24 120.9(3) . . ? C23 C22 C24 120.6(3) . . ? N4 C23 C22 122.1(3) . . ? F11 C24 F10 108.0(4) . . ? F11 C24 F12 104.2(3) . . ? F10 C24 F12 104.4(3) . . ? F11 C24 C22 112.8(3) . . ? F10 C24 C22 113.6(3) . . ? F12 C24 C22 113.0(3) . . ? O1 C25 N5 127.4(4) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 30.58 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.745 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.085 data_[Cd(3-CF3-pyS)2(DMF)]2 _database_code_CSD 189582 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H13 Cd F6 N3 O S2' _chemical_formula_weight 541.80 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.1086(17) _cell_length_b 11.338(2) _cell_length_c 12.460(3) _cell_angle_alpha 109.534(5) _cell_angle_beta 105.748(5) _cell_angle_gamma 96.928(5) _cell_volume 1010.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.781 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 532 _exptl_absorpt_coefficient_mu 1.351 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.6717 _exptl_absorpt_correction_T_max 0.9355 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18110 _diffrn_reflns_av_R_equivalents 0.0647 _diffrn_reflns_av_sigmaI/netI 0.1240 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 30.65 _reflns_number_total 6166 _reflns_number_gt 3012 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0209P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6166 _refine_ls_number_parameters 255 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1157 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0686 _refine_ls_wR_factor_gt 0.0551 _refine_ls_goodness_of_fit_ref 0.819 _refine_ls_restrained_S_all 0.819 _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 Cd1 Cd 0.99688(3) 0.93000(2) 0.61735(2) 0.03712(8) Uani 1 1 d . . . S1 S 1.28866(11) 0.87894(8) 0.70135(8) 0.0458(2) Uani 1 1 d . . . S2 S 0.92896(11) 0.82999(8) 0.36101(7) 0.0383(2) Uani 1 1 d . . . N1 N 0.9882(4) 0.7194(3) 0.6333(2) 0.0424(7) Uani 1 1 d . . . N2 N 0.7123(3) 0.8607(2) 0.4838(2) 0.0361(6) Uani 1 1 d . . . N3 N 0.8883(4) 1.1201(3) 0.9563(3) 0.0608(9) Uani 1 1 d . . . O1 O 0.8721(3) 0.9915(3) 0.7705(2) 0.0593(7) Uani 1 1 d . . . F1 F 1.5106(4) 0.7224(3) 0.8371(3) 0.1160(10) Uani 1 1 d . . . F2 F 1.4943(4) 0.6609(3) 0.6544(3) 0.1190(11) Uani 1 1 d . . . F3 F 1.4573(4) 0.5237(3) 0.7281(3) 0.1378(13) Uani 1 1 d . . . F4 F 0.6298(3) 0.8049(2) 0.11426(19) 0.0829(7) Uani 1 1 d . . . F5 F 0.6465(3) 0.6233(2) 0.12348(19) 0.0878(8) Uani 1 1 d . . . F6 F 0.3960(3) 0.6638(3) 0.0674(2) 0.1022(9) Uani 1 1 d . . . C1 C 1.1629(4) 0.7315(3) 0.6739(3) 0.0375(8) Uani 1 1 d . . . C2 C 1.2298(5) 0.6275(3) 0.6911(3) 0.0469(9) Uani 1 1 d . . . C3 C 1.1139(6) 0.5193(4) 0.6727(4) 0.0652(11) Uani 1 1 d . . . H3 H 1.1561 0.4511 0.6866 0.078 Uiso 1 1 calc R . . C4 C 0.9367(6) 0.5099(4) 0.6342(4) 0.0706(12) Uani 1 1 d . . . H4 H 0.8573 0.4363 0.6218 0.085 Uiso 1 1 calc R . . C5 C 0.8790(5) 0.6112(4) 0.6142(3) 0.0589(10) Uani 1 1 d . . . H5 H 0.7582 0.6045 0.5860 0.071 Uiso 1 1 calc R . . C6 C 1.4208(6) 0.6346(5) 0.7272(5) 0.0736(13) Uani 1 1 d . . . C7 C 0.7174(4) 0.8177(3) 0.3715(3) 0.0348(7) Uani 1 1 d . . . C8 C 0.5596(4) 0.7658(3) 0.2727(3) 0.0420(8) Uani 1 1 d . . . C9 C 0.4023(5) 0.7622(3) 0.2963(4) 0.0572(10) Uani 1 1 d . . . H9 H 0.2962 0.7285 0.2324 0.069 Uiso 1 1 calc R . . C10 C 0.4010(5) 0.8072(4) 0.4117(4) 0.0592(11) Uani 1 1 d . . . H10 H 0.2952 0.8052 0.4275 0.071 Uiso 1 1 calc R . . C11 C 0.5581(5) 0.8553(3) 0.5036(3) 0.0485(9) Uani 1 1 d . . . H11 H 0.5580 0.8855 0.5827 0.058 Uiso 1 1 calc R . . C12 C 0.5592(5) 0.7148(4) 0.1454(3) 0.0613(11) Uani 1 1 d . . . C13 C 0.9417(5) 1.0867(4) 0.8629(4) 0.0603(11) Uani 1 1 d . . . H13 H 1.0417 1.1404 0.8675 0.072 Uiso 1 1 calc R . . C14 C 0.9850(7) 1.2340(5) 1.0621(4) 0.1123(19) Uani 1 1 d . . . H14A H 1.0759 1.2805 1.0459 0.168 Uiso 1 1 calc R . . H14B H 1.0372 1.2097 1.1281 0.168 Uiso 1 1 calc R . . H14C H 0.9062 1.2875 1.0829 0.168 Uiso 1 1 calc R . . C15 C 0.7381(6) 1.0438(5) 0.9606(4) 0.0883(15) Uani 1 1 d . . . H15A H 0.6477 1.0910 0.9635 0.133 Uiso 1 1 calc R . . H15B H 0.7714 1.0237 1.0313 0.133 Uiso 1 1 calc R . . H15C H 0.6946 0.9655 0.8899 0.133 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 Cd1 0.04004(15) 0.03957(14) 0.03467(13) 0.01586(11) 0.01364(11) 0.01222(11) S1 0.0409(5) 0.0441(5) 0.0548(6) 0.0243(5) 0.0132(4) 0.0095(4) S2 0.0423(5) 0.0354(5) 0.0396(5) 0.0139(4) 0.0167(4) 0.0125(4) N1 0.0444(18) 0.0411(17) 0.0401(16) 0.0111(14) 0.0176(14) 0.0098(14) N2 0.0368(16) 0.0338(15) 0.0393(16) 0.0142(13) 0.0145(13) 0.0087(12) N3 0.068(2) 0.084(2) 0.0326(18) 0.0166(18) 0.0228(17) 0.028(2) O1 0.0671(18) 0.0641(17) 0.0411(15) 0.0094(14) 0.0262(14) 0.0077(14) F1 0.0728(19) 0.139(3) 0.119(3) 0.056(2) -0.0047(18) 0.0305(18) F2 0.096(2) 0.165(3) 0.182(3) 0.114(3) 0.096(2) 0.084(2) F3 0.116(2) 0.107(2) 0.246(4) 0.111(3) 0.068(3) 0.078(2) F4 0.1063(19) 0.0835(18) 0.0498(14) 0.0293(13) 0.0148(13) 0.0049(15) F5 0.116(2) 0.0718(16) 0.0544(14) 0.0023(13) 0.0174(14) 0.0348(16) F6 0.0718(17) 0.125(2) 0.0561(15) 0.0113(15) -0.0182(14) -0.0060(15) C1 0.045(2) 0.043(2) 0.0294(17) 0.0140(15) 0.0185(16) 0.0134(16) C2 0.063(3) 0.041(2) 0.049(2) 0.0215(18) 0.0266(19) 0.0201(19) C3 0.090(3) 0.045(2) 0.074(3) 0.030(2) 0.038(3) 0.022(2) C4 0.088(4) 0.039(2) 0.082(3) 0.020(2) 0.037(3) -0.006(2) C5 0.056(3) 0.051(3) 0.060(3) 0.011(2) 0.023(2) -0.001(2) C6 0.070(3) 0.073(3) 0.101(4) 0.053(3) 0.031(3) 0.040(3) C7 0.0369(19) 0.0267(17) 0.0397(19) 0.0140(15) 0.0095(16) 0.0079(14) C8 0.043(2) 0.0358(19) 0.040(2) 0.0136(16) 0.0050(17) 0.0073(16) C9 0.039(2) 0.050(2) 0.068(3) 0.021(2) 0.002(2) 0.0032(18) C10 0.038(2) 0.061(3) 0.083(3) 0.028(2) 0.026(2) 0.0122(19) C11 0.052(2) 0.047(2) 0.058(2) 0.0223(19) 0.030(2) 0.0174(18) C12 0.059(3) 0.056(3) 0.045(2) 0.010(2) -0.003(2) 0.003(2) C13 0.067(3) 0.073(3) 0.045(2) 0.024(2) 0.022(2) 0.018(2) C14 0.120(4) 0.127(5) 0.054(3) -0.001(3) 0.025(3) 0.013(4) C15 0.075(3) 0.127(4) 0.078(3) 0.045(3) 0.037(3) 0.031(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 Cd1 N2 2.305(3) . ? Cd1 O1 2.341(2) . ? Cd1 N1 2.455(3) . ? Cd1 S1 2.5336(10) . ? Cd1 S2 2.6204(10) 2_776 ? Cd1 S2 2.8746(10) . ? S1 C1 1.723(3) . ? S2 C7 1.748(3) . ? S2 Cd1 2.6204(10) 2_776 ? N1 C5 1.332(4) . ? N1 C1 1.342(4) . ? N2 C7 1.334(4) . ? N2 C11 1.337(4) . ? N3 C13 1.304(4) . ? N3 C15 1.431(5) . ? N3 C14 1.441(5) . ? O1 C13 1.216(4) . ? F1 C6 1.330(5) . ? F2 C6 1.304(5) . ? F3 C6 1.328(4) . ? F4 C12 1.329(4) . ? F5 C12 1.321(4) . ? F6 C12 1.331(4) . ? C1 C2 1.411(4) . ? C2 C3 1.363(5) . ? C2 C6 1.475(5) . ? C3 C4 1.365(5) . ? C4 C5 1.364(5) . ? C7 C8 1.406(4) . ? C8 C9 1.383(5) . ? C8 C12 1.494(5) . ? C9 C10 1.360(5) . ? C10 C11 1.362(5) . ? 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 Cd1 O1 86.41(9) . . ? N2 Cd1 N1 91.48(9) . . ? O1 Cd1 N1 89.33(9) . . ? N2 Cd1 S1 148.99(7) . . ? O1 Cd1 S1 108.51(7) . . ? N1 Cd1 S1 62.57(7) . . ? N2 Cd1 S2 100.83(6) . 2_776 ? O1 Cd1 S2 89.55(7) . 2_776 ? N1 Cd1 S2 167.55(7) . 2_776 ? S1 Cd1 S2 106.17(3) . 2_776 ? N2 Cd1 S2 59.24(7) . . ? O1 Cd1 S2 145.47(7) . . ? N1 Cd1 S2 94.56(6) . . ? S1 Cd1 S2 103.65(3) . . ? S2 Cd1 S2 93.39(3) 2_776 . ? C1 S1 Cd1 85.16(11) . . ? C7 S2 Cd1 100.10(10) . 2_776 ? C7 S2 Cd1 77.07(11) . . ? Cd1 S2 Cd1 86.61(3) 2_776 . ? C5 N1 C1 119.8(3) . . ? C5 N1 Cd1 143.0(3) . . ? C1 N1 Cd1 97.2(2) . . ? C7 N2 C11 120.5(3) . . ? C7 N2 Cd1 108.76(19) . . ? C11 N2 Cd1 130.7(2) . . ? C13 N3 C15 122.1(4) . . ? C13 N3 C14 120.5(4) . . ? C15 N3 C14 117.3(4) . . ? C13 O1 Cd1 122.5(3) . . ? N1 C1 C2 119.8(3) . . ? N1 C1 S1 114.9(2) . . ? C2 C1 S1 125.3(3) . . ? C3 C2 C1 118.6(4) . . ? C3 C2 C6 120.3(4) . . ? C1 C2 C6 121.0(3) . . ? C2 C3 C4 120.7(4) . . ? C5 C4 C3 118.3(4) . . ? N1 C5 C4 122.8(4) . . ? F2 C6 F3 104.7(4) . . ? F2 C6 F1 106.3(4) . . ? F3 C6 F1 106.0(4) . . ? F2 C6 C2 113.4(4) . . ? F3 C6 C2 112.3(4) . . ? F1 C6 C2 113.4(4) . . ? N2 C7 C8 120.0(3) . . ? N2 C7 S2 114.9(2) . . ? C8 C7 S2 125.1(3) . . ? C9 C8 C7 118.0(3) . . ? C9 C8 C12 120.2(3) . . ? C7 C8 C12 121.7(3) . . ? C10 C9 C8 120.8(3) . . ? C9 C10 C11 118.4(3) . . ? N2 C11 C10 122.3(3) . . ? F5 C12 F4 106.2(4) . . ? F5 C12 F6 106.1(3) . . ? F4 C12 F6 106.4(3) . . ? F5 C12 C8 113.3(3) . . ? F4 C12 C8 113.0(3) . . ? F6 C12 C8 111.3(4) . . ? O1 C13 N3 125.7(4) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 30.65 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.518 _refine_diff_density_min -0.575 _refine_diff_density_rms 0.091 data_[Cd(3-CF3-pyS)2(bipy)] _database_code_CSD 189583 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H17 Cd F6 N5 S2' _chemical_formula_weight 665.95 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 2(1)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.680(3) _cell_length_b 9.7564(18) _cell_length_c 20.410(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.684(3) _cell_angle_gamma 90.00 _cell_volume 2723.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 954 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 27.57 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.624 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 1.019 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.6092 _exptl_absorpt_correction_T_max 0.7363 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart-CCD-1000 BRUKER' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6377 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0243 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 28.25 _reflns_number_total 6377 _reflns_number_gt 4949 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER Smart' _computing_cell_refinement 'BRUKER Smart' _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0307P)^2^+0.9963P] 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 6377 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0437 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0762 _refine_ls_wR_factor_gt 0.0693 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 Cd1 Cd 0.806649(14) 0.772574(18) 0.050526(9) 0.05481(7) Uani 1 1 d . . . S1 S 0.86112(5) 0.88877(7) -0.05699(3) 0.06392(17) Uani 1 1 d . . . S2 S 0.66105(5) 0.86529(8) 0.11175(4) 0.06908(19) Uani 1 1 d . . . F1 F 0.8101(3) 1.0150(3) -0.19357(12) 0.1590(13) Uani 1 1 d . . . F2 F 0.8911(2) 0.8342(4) -0.21118(13) 0.1559(12) Uani 1 1 d . . . F3 F 0.7635(3) 0.8759(4) -0.26833(11) 0.1858(16) Uani 1 1 d . . . F4 F 0.56192(16) 1.1133(2) 0.17990(11) 0.1115(7) Uani 1 1 d . . . F5 F 0.56077(17) 0.9462(3) 0.24684(12) 0.1219(8) Uani 1 1 d . . . F6 F 0.59914(19) 1.1451(3) 0.28068(11) 0.1257(8) Uani 1 1 d . . . N1 N 0.70975(16) 0.7254(2) -0.05265(10) 0.0594(5) Uani 1 1 d . . . N2 N 0.83804(17) 0.9270(2) 0.15095(11) 0.0645(5) Uani 1 1 d . . . N3 N 0.79565(17) 0.5352(2) 0.07290(11) 0.0647(5) Uani 1 1 d . . . N4 N 0.96213(15) 0.6792(2) 0.07259(10) 0.0581(5) Uani 1 1 d . . . C1 C 0.76362(18) 0.8025(2) -0.09355(12) 0.0532(5) Uani 1 1 d . . . C2 C 0.7388(2) 0.8068(3) -0.16032(14) 0.0674(7) Uani 1 1 d . . . C3 C 0.6574(2) 0.7346(3) -0.18278(16) 0.0798(9) Uani 1 1 d . . . H3 H 0.6400 0.7377 -0.2269 0.096 Uiso 1 1 calc R . . C4 C 0.6032(2) 0.6594(3) -0.14053(18) 0.0823(9) Uani 1 1 d . . . H4 H 0.5484 0.6111 -0.1549 0.099 Uiso 1 1 calc R . . C5 C 0.6321(2) 0.6571(3) -0.07564(16) 0.0740(8) Uani 1 1 d . . . H5 H 0.5957 0.6054 -0.0464 0.089 Uiso 1 1 calc R . . C6 C 0.7987(4) 0.8853(6) -0.20790(18) 0.1119(14) Uani 1 1 d . . . C7 C 0.7425(2) 0.9473(2) 0.16352(11) 0.0565(6) Uani 1 1 d . . . C8 C 0.7148(2) 1.0316(3) 0.21642(13) 0.0659(7) Uani 1 1 d . . . C9 C 0.7865(3) 1.0920(4) 0.25453(15) 0.0873(10) Uani 1 1 d . . . H9 H 0.7694 1.1486 0.2892 0.105 Uiso 1 1 calc R . . C10 C 0.8834(3) 1.0686(4) 0.24122(18) 0.0988(11) Uani 1 1 d . . . H10 H 0.9326 1.1074 0.2670 0.119 Uiso 1 1 calc R . . C11 C 0.9057(3) 0.9866(4) 0.18901(18) 0.0879(9) Uani 1 1 d . . . H11 H 0.9712 0.9718 0.1796 0.106 Uiso 1 1 calc R . . C12 C 0.6103(3) 1.0579(4) 0.23050(16) 0.0868(10) Uani 1 1 d . . . C13 C 0.7108(2) 0.4686(4) 0.07217(16) 0.0848(9) Uani 1 1 d . . . H13 H 0.6532 0.5189 0.0687 0.102 Uiso 1 1 calc R . . C14 C 0.7049(3) 0.3276(4) 0.07639(19) 0.1012(12) Uani 1 1 d . . . H14 H 0.6447 0.2833 0.0761 0.121 Uiso 1 1 calc R . . C15 C 0.7899(4) 0.2552(4) 0.0810(2) 0.1066(14) Uani 1 1 d . . . H15 H 0.7881 0.1599 0.0827 0.128 Uiso 1 1 calc R . . C16 C 0.8778(3) 0.3216(3) 0.08328(16) 0.0857(9) Uani 1 1 d . . . H16 H 0.9358 0.2725 0.0873 0.103 Uiso 1 1 calc R . . C17 C 0.8790(2) 0.4641(3) 0.07950(12) 0.0599(6) Uani 1 1 d . . . C18 C 0.97106(19) 0.5444(3) 0.08256(11) 0.0561(6) Uani 1 1 d . . . C19 C 1.0617(2) 0.4862(3) 0.09630(14) 0.0794(9) Uani 1 1 d . . . H19 H 1.0679 0.3921 0.1023 0.095 Uiso 1 1 calc R . . C20 C 1.1421(3) 0.5704(4) 0.10084(17) 0.0922(11) Uani 1 1 d . . . H20 H 1.2031 0.5331 0.1107 0.111 Uiso 1 1 calc R . . C21 C 1.1332(2) 0.7070(4) 0.09113(17) 0.0862(9) Uani 1 1 d . . . H21 H 1.1873 0.7645 0.0942 0.103 Uiso 1 1 calc R . . C22 C 1.0421(2) 0.7580(3) 0.07665(16) 0.0762(8) Uani 1 1 d . . . H22 H 1.0356 0.8516 0.0693 0.091 Uiso 1 1 calc R . . N1S N 0.4530(4) 0.6649(5) 0.0632(3) 0.167(2) Uani 1 1 d . . . C1S C 0.4288(3) 0.7723(6) 0.0708(3) 0.135(2) Uani 1 1 d . . . C2S C 0.4030(4) 0.9139(6) 0.0744(4) 0.216(4) Uani 1 1 d . . . H2S1 H 0.4559 0.9687 0.0585 0.324 Uiso 1 1 calc R . . H2S2 H 0.3900 0.9379 0.1190 0.324 Uiso 1 1 calc R . . H2S3 H 0.3456 0.9303 0.0480 0.324 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 Cd1 0.06439(12) 0.04642(10) 0.05358(11) -0.00049(8) -0.00072(8) 0.00756(8) S1 0.0700(4) 0.0600(4) 0.0616(4) 0.0086(3) -0.0084(3) -0.0123(3) S2 0.0633(4) 0.0764(5) 0.0675(4) -0.0177(3) -0.0037(3) 0.0094(3) F1 0.251(3) 0.120(2) 0.1055(18) 0.0518(16) -0.0216(19) -0.070(2) F2 0.136(2) 0.226(4) 0.1063(19) 0.000(2) 0.0430(17) -0.049(2) F3 0.228(3) 0.267(4) 0.0619(14) 0.0448(18) -0.0324(17) -0.103(3) F4 0.1081(15) 0.1311(18) 0.0956(15) -0.0024(13) 0.0185(12) 0.0513(13) F5 0.1254(17) 0.1137(18) 0.1278(18) -0.0055(14) 0.0550(14) -0.0166(14) F6 0.161(2) 0.1243(19) 0.0934(15) -0.0410(13) 0.0458(14) 0.0162(16) N1 0.0657(13) 0.0503(11) 0.0621(13) -0.0054(10) 0.0009(10) -0.0015(10) N2 0.0688(14) 0.0594(13) 0.0652(14) -0.0063(10) -0.0084(11) 0.0076(10) N3 0.0716(14) 0.0562(13) 0.0662(14) 0.0058(10) -0.0015(11) -0.0014(11) N4 0.0657(13) 0.0521(12) 0.0564(12) 0.0018(9) 0.0003(10) 0.0066(10) C1 0.0580(14) 0.0447(13) 0.0570(14) -0.0015(10) -0.0013(11) 0.0063(10) C2 0.0762(18) 0.0684(17) 0.0575(16) 0.0008(13) -0.0068(13) 0.0023(14) C3 0.085(2) 0.088(2) 0.0655(18) -0.0117(16) -0.0190(16) 0.0051(17) C4 0.0686(18) 0.083(2) 0.095(2) -0.0194(18) -0.0126(17) -0.0107(16) C5 0.0658(17) 0.0676(19) 0.089(2) -0.0096(15) 0.0071(15) -0.0093(14) C6 0.139(4) 0.139(4) 0.058(2) 0.016(2) -0.012(2) -0.038(3) C7 0.0744(16) 0.0477(13) 0.0474(13) 0.0030(10) -0.0004(11) 0.0084(11) C8 0.093(2) 0.0571(16) 0.0473(14) -0.0017(11) 0.0067(13) 0.0037(14) C9 0.125(3) 0.079(2) 0.0571(18) -0.0135(15) 0.0008(18) -0.004(2) C10 0.110(3) 0.101(3) 0.085(2) -0.020(2) -0.024(2) -0.016(2) C11 0.078(2) 0.089(2) 0.097(2) -0.0135(19) -0.0174(18) 0.0017(17) C12 0.114(3) 0.082(2) 0.0648(19) -0.0092(16) 0.0235(19) 0.015(2) C13 0.083(2) 0.084(2) 0.087(2) 0.0148(17) -0.0020(17) -0.0115(17) C14 0.120(3) 0.084(3) 0.100(3) 0.020(2) 0.000(2) -0.037(2) C15 0.163(4) 0.056(2) 0.101(3) 0.0217(18) 0.004(3) -0.020(2) C16 0.124(3) 0.0516(16) 0.082(2) 0.0151(15) -0.0001(19) 0.0059(18) C17 0.0860(18) 0.0485(14) 0.0452(13) 0.0042(10) -0.0005(12) 0.0075(13) C18 0.0749(16) 0.0524(14) 0.0409(12) -0.0036(10) -0.0013(11) 0.0147(12) C19 0.099(2) 0.0684(19) 0.0711(19) -0.0131(14) -0.0158(16) 0.0300(17) C20 0.076(2) 0.113(3) 0.087(2) -0.027(2) -0.0176(17) 0.029(2) C21 0.071(2) 0.098(3) 0.090(2) -0.0203(19) -0.0048(16) -0.0015(18) C22 0.077(2) 0.0646(19) 0.087(2) -0.0037(14) -0.0025(16) -0.0010(14) N1S 0.150(4) 0.107(3) 0.243(6) -0.032(4) -0.021(4) -0.029(3) C1S 0.088(3) 0.109(4) 0.209(6) -0.043(4) -0.013(3) -0.018(3) C2S 0.104(4) 0.141(5) 0.401(11) -0.098(6) -0.047(5) 0.028(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 Cd1 N4 2.353(2) . ? Cd1 N3 2.366(2) . ? Cd1 N1 2.517(2) . ? Cd1 S2 2.5311(8) . ? Cd1 N2 2.576(2) . ? Cd1 S1 2.5875(8) . ? S1 C1 1.738(3) . ? S2 C7 1.724(3) . ? F1 C6 1.308(5) . ? F2 C6 1.362(6) . ? F3 C6 1.322(4) . ? F4 C12 1.334(4) . ? F5 C12 1.328(4) . ? F6 C12 1.342(4) . ? N1 C5 1.335(3) . ? N1 C1 1.349(3) . ? N2 C11 1.335(4) . ? N2 C7 1.349(3) . ? N3 C13 1.330(4) . ? N3 C17 1.339(3) . ? N4 C18 1.336(3) . ? N4 C22 1.339(4) . ? C1 C2 1.401(4) . ? C2 C3 1.390(4) . ? C2 C6 1.490(5) . ? C3 C4 1.359(5) . ? C4 C5 1.378(4) . ? C7 C8 1.413(4) . ? C8 C9 1.377(4) . ? C8 C12 1.484(5) . ? C9 C10 1.376(5) . ? C10 C11 1.370(5) . ? C13 C14 1.381(5) . ? C14 C15 1.363(6) . ? C15 C16 1.366(6) . ? C16 C17 1.393(4) . ? C17 C18 1.484(4) . ? C18 C19 1.389(4) . ? C19 C20 1.375(5) . ? C20 C21 1.352(5) . ? C21 C22 1.371(5) . ? N1S C1S 1.111(6) . ? C1S C2S 1.428(8) . ? 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 N4 Cd1 N3 69.10(8) . . ? N4 Cd1 N1 123.73(7) . . ? N3 Cd1 N1 87.05(7) . . ? N4 Cd1 S2 139.37(5) . . ? N3 Cd1 S2 101.68(6) . . ? N1 Cd1 S2 93.94(5) . . ? N4 Cd1 N2 86.13(7) . . ? N3 Cd1 N2 115.43(8) . . ? N1 Cd1 N2 148.61(7) . . ? S2 Cd1 N2 61.50(5) . . ? N4 Cd1 S1 93.63(5) . . ? N3 Cd1 S1 127.75(6) . . ? N1 Cd1 S1 61.61(5) . . ? S2 Cd1 S1 119.89(3) . . ? N2 Cd1 S1 111.82(6) . . ? C1 S1 Cd1 85.68(9) . . ? C7 S2 Cd1 87.79(9) . . ? C5 N1 C1 120.0(2) . . ? C5 N1 Cd1 142.6(2) . . ? C1 N1 Cd1 97.46(15) . . ? C11 N2 C7 119.5(3) . . ? C11 N2 Cd1 145.7(2) . . ? C7 N2 Cd1 94.85(15) . . ? C13 N3 C17 119.3(3) . . ? C13 N3 Cd1 122.3(2) . . ? C17 N3 Cd1 118.05(17) . . ? C18 N4 C22 118.9(2) . . ? C18 N4 Cd1 119.42(17) . . ? C22 N4 Cd1 121.72(19) . . ? N1 C1 C2 119.4(2) . . ? N1 C1 S1 115.23(19) . . ? C2 C1 S1 125.4(2) . . ? C3 C2 C1 119.3(3) . . ? C3 C2 C6 119.3(3) . . ? C1 C2 C6 121.3(3) . . ? C4 C3 C2 120.3(3) . . ? C3 C4 C5 117.8(3) . . ? N1 C5 C4 123.2(3) . . ? F1 C6 F3 108.5(4) . . ? F1 C6 F2 104.9(4) . . ? F3 C6 F2 104.9(4) . . ? F1 C6 C2 114.6(4) . . ? F3 C6 C2 112.1(4) . . ? F2 C6 C2 111.2(4) . . ? N2 C7 C8 120.0(2) . . ? N2 C7 S2 115.85(18) . . ? C8 C7 S2 124.1(2) . . ? C9 C8 C7 119.0(3) . . ? C9 C8 C12 119.9(3) . . ? C7 C8 C12 121.1(3) . . ? C10 C9 C8 119.9(3) . . ? C11 C10 C9 118.3(3) . . ? N2 C11 C10 123.2(3) . . ? F5 C12 F4 106.0(3) . . ? F5 C12 F6 105.4(3) . . ? F4 C12 F6 105.9(3) . . ? F5 C12 C8 113.7(3) . . ? F4 C12 C8 113.0(3) . . ? F6 C12 C8 112.1(3) . . ? N3 C13 C14 122.6(3) . . ? C15 C14 C13 118.0(4) . . ? C14 C15 C16 120.4(3) . . ? C15 C16 C17 118.8(4) . . ? N3 C17 C16 120.8(3) . . ? N3 C17 C18 116.9(2) . . ? C16 C17 C18 122.3(3) . . ? N4 C18 C19 120.8(3) . . ? N4 C18 C17 115.9(2) . . ? C19 C18 C17 123.2(3) . . ? C20 C19 C18 118.8(3) . . ? C21 C20 C19 120.5(3) . . ? C20 C21 C22 118.0(3) . . ? N4 C22 C21 123.0(3) . . ? N1S C1S C2S 173.9(8) . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 28.25 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 0.245 _refine_diff_density_min -0.392 _refine_diff_density_rms 0.056 data_[Hg(3-CF3-pyS)2] _database_code_CSD 189584 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H6 F6 Hg N2 S2' _chemical_formula_weight 556.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 7.5788(15) _cell_length_b 18.800(4) _cell_length_c 21.479(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3060.5(11) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1016 _cell_measurement_theta_min 2.365 _cell_measurement_theta_max 26.32 _exptl_crystal_description Prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.417 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064 _exptl_absorpt_coefficient_mu 10.392 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.1138 _exptl_absorpt_correction_T_max 0.3944 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart-CCD-1000 BRUKER' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18043 _diffrn_reflns_av_R_equivalents 0.0699 _diffrn_reflns_av_sigmaI/netI 0.0482 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 26.39 _reflns_number_total 3136 _reflns_number_gt 1913 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER Smart' _computing_cell_refinement 'BRUKER Smart' _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0218P)^2^+0.6578P] 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 3136 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0691 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0695 _refine_ls_wR_factor_gt 0.0567 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 Hg1 Hg 0.23861(3) 0.228956(14) 0.280010(10) 0.03922(10) Uani 1 1 d . . . S1 S 0.3947(2) 0.14450(10) 0.21886(7) 0.0411(4) Uani 1 1 d . . . S2 S 0.1515(2) 0.30097(10) 0.36485(8) 0.0462(5) Uani 1 1 d . . . N1 N 0.1899(7) 0.2256(3) 0.1515(3) 0.0492(15) Uani 1 1 d . . . N2 N 0.0450(8) 0.3539(3) 0.2582(2) 0.0468(15) Uani 1 1 d . . . F1 F 0.6554(6) 0.1105(3) 0.1103(2) 0.0866(16) Uani 1 1 d . . . F2 F 0.5419(7) 0.0773(3) 0.0246(2) 0.0896(16) Uani 1 1 d . . . F3 F 0.4583(7) 0.0303(3) 0.1098(2) 0.0881(16) Uani 1 1 d . . . F4 F 0.1687(8) 0.4485(3) 0.4325(2) 0.0938(17) Uani 1 1 d . . . F5 F -0.0775(8) 0.3998(3) 0.4477(2) 0.109(2) Uani 1 1 d . . . F6 F -0.0644(9) 0.5103(3) 0.4267(2) 0.120(2) Uani 1 1 d . . . C1 C 0.3096(8) 0.1745(4) 0.1473(3) 0.0418(18) Uani 1 1 d . . . C2 C 0.3651(8) 0.1481(4) 0.0896(3) 0.0429(17) Uani 1 1 d . . . C3 C 0.2898(9) 0.1745(4) 0.0364(3) 0.057(2) Uani 1 1 d . . . H3 H 0.3232 0.1569 -0.0023 0.069 Uiso 1 1 calc R . . C4 C 0.1647(11) 0.2271(5) 0.0407(3) 0.080(3) Uani 1 1 d . . . H4 H 0.1109 0.2456 0.0053 0.096 Uiso 1 1 calc R . . C5 C 0.1221(10) 0.2514(5) 0.0988(4) 0.077(3) Uani 1 1 d . . . H5 H 0.0407 0.2882 0.1018 0.092 Uiso 1 1 calc R . . C6 C 0.5035(11) 0.0923(5) 0.0827(3) 0.060(2) Uani 1 1 d . . . C7 C 0.0537(8) 0.3673(4) 0.3190(3) 0.0385(16) Uani 1 1 d . . . C8 C -0.0098(9) 0.4309(4) 0.3447(3) 0.0467(18) Uani 1 1 d . . . C9 C -0.0837(9) 0.4806(4) 0.3058(4) 0.055(2) Uani 1 1 d . . . H9 H -0.1291 0.5227 0.3219 0.066 Uiso 1 1 calc R . . C10 C -0.0900(11) 0.4678(5) 0.2435(4) 0.061(2) Uani 1 1 d . . . H10 H -0.1382 0.5011 0.2163 0.073 Uiso 1 1 calc R . . C11 C -0.0239(10) 0.4053(5) 0.2221(3) 0.057(2) Uani 1 1 d . . . H11 H -0.0265 0.3974 0.1793 0.068 Uiso 1 1 calc R . . C12 C 0.0017(14) 0.4470(5) 0.4125(4) 0.073(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.04366(16) 0.03693(16) 0.03708(12) -0.00178(12) 0.00278(13) 0.00249(14) S1 0.0389(9) 0.0423(11) 0.0421(8) -0.0033(9) 0.0025(8) 0.0010(8) S2 0.0543(11) 0.0412(11) 0.0431(9) -0.0017(9) 0.0041(8) 0.0046(10) N1 0.044(3) 0.050(4) 0.054(3) 0.002(3) 0.004(3) 0.015(3) N2 0.055(4) 0.034(3) 0.051(3) -0.005(3) -0.002(3) -0.009(3) F1 0.045(3) 0.101(4) 0.114(4) -0.049(3) -0.005(3) 0.020(3) F2 0.116(4) 0.090(4) 0.063(3) -0.027(3) 0.022(3) 0.035(3) F3 0.110(4) 0.059(4) 0.095(4) 0.002(3) 0.010(3) 0.018(3) F4 0.111(4) 0.093(4) 0.077(3) -0.031(3) -0.030(3) 0.013(4) F5 0.145(5) 0.118(5) 0.064(3) -0.009(3) 0.043(3) -0.008(4) F6 0.173(6) 0.097(5) 0.088(4) -0.043(3) -0.014(4) 0.076(4) C1 0.033(4) 0.048(5) 0.044(4) -0.008(4) 0.004(3) -0.003(3) C2 0.038(4) 0.048(5) 0.043(4) -0.006(4) -0.001(3) -0.002(4) C3 0.054(5) 0.067(6) 0.051(4) -0.005(4) 0.003(3) 0.001(4) C4 0.068(5) 0.122(9) 0.050(5) 0.007(6) -0.007(4) 0.024(6) C5 0.070(6) 0.092(8) 0.069(5) 0.009(5) 0.008(4) 0.041(5) C6 0.067(6) 0.059(6) 0.053(5) -0.017(5) 0.000(4) 0.007(5) C7 0.029(3) 0.036(4) 0.050(4) -0.007(4) 0.009(3) -0.011(3) C8 0.040(4) 0.043(5) 0.057(4) -0.005(4) 0.003(3) 0.002(4) C9 0.045(5) 0.042(5) 0.078(5) -0.003(5) 0.004(4) 0.002(4) C10 0.056(5) 0.056(6) 0.071(5) 0.020(5) -0.019(4) -0.007(5) C11 0.059(5) 0.062(6) 0.050(4) -0.004(5) -0.005(4) -0.018(5) C12 0.087(7) 0.060(7) 0.072(6) -0.020(5) -0.004(5) 0.020(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 S2 2.3642(18) . ? Hg1 S1 2.3761(17) . ? Hg1 N1 2.786(6) . ? Hg1 N2 2.808(6) . ? S1 C1 1.760(7) . ? S2 C7 1.752(7) . ? N1 C1 1.324(8) . ? N1 C5 1.333(8) . ? N2 C7 1.333(7) . ? N2 C11 1.345(9) . ? F1 C6 1.338(8) . ? F2 C6 1.312(7) . ? F3 C6 1.346(9) . ? F4 C12 1.337(10) . ? F5 C12 1.312(10) . ? F6 C12 1.327(9) . ? C1 C2 1.400(8) . ? C2 C3 1.370(9) . ? C2 C6 1.491(10) . ? C3 C4 1.374(10) . ? C4 C5 1.369(9) . ? C7 C8 1.402(9) . ? C8 C9 1.373(9) . ? C8 C12 1.490(10) . ? C9 C10 1.360(10) . ? C10 C11 1.359(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Hg1 S1 161.41(6) . . ? S2 Hg1 N1 137.70(13) . . ? S1 Hg1 N1 60.21(12) . . ? S2 Hg1 N2 60.26(11) . . ? S1 Hg1 N2 136.60(11) . . ? N1 Hg1 N2 77.54(16) . . ? C1 S1 Hg1 94.9(2) . . ? C7 S2 Hg1 95.3(2) . . ? C1 N1 C5 118.0(6) . . ? C1 N1 Hg1 89.6(4) . . ? C5 N1 Hg1 152.1(5) . . ? C7 N2 C11 116.7(7) . . ? C7 N2 Hg1 88.2(4) . . ? C11 N2 Hg1 154.2(5) . . ? N1 C1 C2 121.6(6) . . ? N1 C1 S1 115.1(5) . . ? C2 C1 S1 123.3(6) . . ? C3 C2 C1 118.9(7) . . ? C3 C2 C6 117.8(6) . . ? C1 C2 C6 123.3(6) . . ? C2 C3 C4 119.6(7) . . ? C5 C4 C3 117.6(7) . . ? N1 C5 C4 124.2(8) . . ? F2 C6 F1 106.5(7) . . ? F2 C6 F3 106.3(7) . . ? F1 C6 F3 104.4(7) . . ? F2 C6 C2 113.6(7) . . ? F1 C6 C2 112.5(7) . . ? F3 C6 C2 112.8(7) . . ? N2 C7 C8 122.0(7) . . ? N2 C7 S2 115.9(5) . . ? C8 C7 S2 122.1(5) . . ? C9 C8 C7 118.9(7) . . ? C9 C8 C12 118.6(7) . . ? C7 C8 C12 122.5(7) . . ? C10 C9 C8 119.5(8) . . ? C11 C10 C9 118.2(8) . . ? N2 C11 C10 124.7(7) . . ? F5 C12 F6 107.6(8) . . ? F5 C12 F4 105.1(8) . . ? F6 C12 F4 105.3(8) . . ? F5 C12 C8 113.5(8) . . ? F6 C12 C8 112.7(8) . . ? F4 C12 C8 112.0(7) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.653 _refine_diff_density_min -0.869 _refine_diff_density_rms 0.131 data_[Hg(5-CF3-pyS)2] _database_code_CSD 189585 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H6 F6 Hg N2 S2' _chemical_formula_weight 556.90 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' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.639(6) _cell_length_b 15.075(6) _cell_length_c 6.934(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.085(8) _cell_angle_gamma 90.00 _cell_volume 1529.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 810 _cell_measurement_theta_min 3.10 _cell_measurement_theta_max 26.29 _exptl_crystal_description Needle _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.419 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 10.398 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.0576 _exptl_absorpt_correction_T_max 0.6812 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart-CCD-1000 BRUKER' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6620 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_sigmaI/netI 0.0671 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 3 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 26.43 _reflns_number_total 3124 _reflns_number_gt 1974 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER Smart' _computing_cell_refinement 'BRUKER Smart' _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0810P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3124 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0789 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1372 _refine_ls_wR_factor_gt 0.1218 _refine_ls_goodness_of_fit_ref 0.926 _refine_ls_restrained_S_all 0.926 _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 Hg1 Hg 0.35957(3) 0.21148(3) 0.19798(6) 0.05086(19) Uani 1 1 d . . . S1 S 0.2651(2) 0.3314(2) 0.2742(4) 0.0520(7) Uani 1 1 d . . . S2 S 0.4563(3) 0.0950(2) 0.1277(5) 0.0630(9) Uani 1 1 d . . . N1 N 0.1754(7) 0.1784(6) 0.2705(12) 0.045(2) Uani 1 1 d . . . N2 N 0.5169(6) 0.1589(6) 0.4696(14) 0.053(2) Uani 1 1 d . . . F1 F -0.1357(19) 0.141(2) 0.195(6) 0.106(12) Uani 0.50 1 d P . . F2 F -0.053(2) 0.031(2) 0.199(7) 0.109(13) Uani 0.50 1 d P . . F3 F -0.087(4) 0.083(4) 0.452(9) 0.123(18) Uani 0.50 1 d P . . F1A F -0.067(4) 0.041(4) 0.407(10) 0.18(4) Uani 0.50 1 d P . . F2A F -0.149(3) 0.144(3) 0.304(8) 0.16(2) Uani 0.50 1 d P . . F3A F -0.073(4) 0.058(4) 0.105(5) 0.15(2) Uani 0.50 1 d P . . F4 F 0.723(3) 0.047(3) 0.916(7) 0.15(3) Uani 0.50 1 d P . . F5 F 0.8059(14) 0.132(4) 0.752(5) 0.130(18) Uani 0.50 1 d P . . F6 F 0.693(4) 0.185(3) 0.922(7) 0.17(3) Uani 0.50 1 d P . . F4A F 0.771(2) 0.176(3) 0.783(5) 0.120(12) Uani 0.50 1 d P . . F5A F 0.682(2) 0.140(3) 0.961(3) 0.098(12) Uani 0.50 1 d P . . F6A F 0.762(3) 0.046(2) 0.846(7) 0.13(2) Uani 0.50 1 d P . . C1 C 0.1657(7) 0.2671(7) 0.2802(13) 0.040(2) Uani 1 1 d . . . C2 C 0.0800(8) 0.3076(7) 0.2955(16) 0.048(3) Uani 1 1 d . . . H2 H 0.0750 0.3689 0.3032 0.057 Uiso 1 1 calc R . . C3 C 0.0022(8) 0.2538(9) 0.2991(15) 0.050(3) Uani 1 1 d . . . H3 H -0.0554 0.2789 0.3109 0.061 Uiso 1 1 calc R . . C4 C 0.0121(8) 0.1622(7) 0.2848(15) 0.048(3) Uani 1 1 d . . . C5 C 0.1012(9) 0.1290(8) 0.2703(16) 0.053(3) Uani 1 1 d . . . H5 H 0.1083 0.0679 0.2597 0.064 Uiso 1 1 calc R . . C6 C -0.0698(11) 0.1044(10) 0.278(2) 0.073(4) Uani 1 1 d . . . C7 C 0.5313(7) 0.0998(7) 0.3310(15) 0.040(2) Uani 1 1 d . . . C8 C 0.6025(9) 0.0408(8) 0.3415(17) 0.060(3) Uani 1 1 d . . . H8 H 0.6099 -0.0012 0.2451 0.072 Uiso 1 1 calc R . . C9 C 0.6627(8) 0.0453(8) 0.4980(17) 0.059(3) Uani 1 1 d . . . H9 H 0.7117 0.0060 0.5084 0.071 Uiso 1 1 calc R . . C10 C 0.6506(8) 0.1078(7) 0.6392(15) 0.048(3) Uani 1 1 d . . . C11 C 0.5748(8) 0.1620(8) 0.6206(16) 0.051(3) Uani 1 1 d . . . H11 H 0.5639 0.2024 0.7184 0.062 Uiso 1 1 calc R . . C12 C 0.7172(9) 0.1169(9) 0.808(2) 0.061(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.0522(3) 0.0560(3) 0.0436(3) 0.0004(2) -0.00962(19) 0.0013(2) S1 0.0547(18) 0.0491(16) 0.0513(16) -0.0049(13) -0.0080(14) -0.0041(14) S2 0.071(2) 0.0645(19) 0.0521(17) -0.0107(15) -0.0188(16) 0.0108(17) N1 0.055(6) 0.040(4) 0.039(5) 0.001(4) -0.008(4) 0.006(5) N2 0.042(5) 0.055(6) 0.060(6) -0.008(5) -0.009(5) 0.013(5) F1 0.050(15) 0.094(16) 0.17(3) 0.02(2) -0.071(18) 0.006(15) F2 0.10(2) 0.065(15) 0.16(3) -0.06(2) 0.06(3) -0.039(14) F3 0.077(19) 0.18(5) 0.11(2) 0.04(3) 0.017(18) -0.05(3) F1A 0.13(5) 0.16(5) 0.24(8) 0.14(5) -0.09(5) -0.09(4) F2A 0.08(2) 0.14(3) 0.27(6) -0.01(4) 0.08(3) -0.032(19) F3A 0.15(3) 0.19(5) 0.11(2) -0.02(2) -0.02(2) -0.10(3) F4 0.10(3) 0.19(5) 0.14(3) 0.11(3) -0.08(2) -0.08(3) F5 0.021(10) 0.28(5) 0.087(15) -0.03(2) -0.015(11) 0.006(17) F6 0.20(5) 0.15(3) 0.15(4) -0.10(3) -0.13(4) 0.10(3) F4A 0.055(16) 0.19(3) 0.12(2) 0.02(2) -0.016(18) -0.08(2) F5A 0.096(16) 0.17(3) 0.029(9) -0.010(15) -0.004(9) 0.06(2) F6A 0.13(4) 0.11(3) 0.14(4) -0.05(3) -0.10(3) 0.06(3) C1 0.042(6) 0.050(6) 0.027(5) 0.001(4) -0.006(4) -0.004(5) C2 0.048(7) 0.049(7) 0.045(6) -0.006(5) -0.008(5) 0.005(5) C3 0.043(6) 0.065(7) 0.043(6) -0.007(6) 0.000(5) 0.018(6) C4 0.051(7) 0.051(7) 0.041(6) 0.006(5) 0.000(5) 0.002(6) C5 0.073(8) 0.041(6) 0.045(6) 0.001(5) -0.003(6) 0.000(6) C6 0.077(11) 0.071(10) 0.071(10) 0.009(8) 0.014(9) -0.018(8) C7 0.030(5) 0.046(6) 0.045(6) 0.004(5) 0.007(5) 0.004(5) C8 0.066(8) 0.062(8) 0.052(7) -0.013(6) -0.010(6) 0.006(7) C9 0.054(7) 0.066(8) 0.056(7) -0.007(6) -0.002(6) 0.019(6) C10 0.043(6) 0.057(7) 0.042(6) 0.001(5) -0.003(5) 0.001(5) C11 0.045(7) 0.055(7) 0.053(7) -0.012(6) -0.013(6) 0.007(6) C12 0.049(8) 0.071(9) 0.062(9) -0.008(7) -0.011(7) 0.002(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 S2 2.319(3) . ? Hg1 S1 2.348(3) . ? Hg1 N1 2.805(10) . ? Hg1 N2 3.027(9) . ? S1 C1 1.750(11) . ? S2 C7 1.756(11) . ? N1 C5 1.317(15) . ? N1 C1 1.347(14) . ? N2 C11 1.324(13) . ? N2 C7 1.333(13) . ? F1 F2A 0.78(5) . ? F1 C6 1.24(3) . ? F1 F3A 1.68(6) . ? F2 F3A 0.82(5) . ? F2 C6 1.27(3) . ? F2 F1A 1.47(7) . ? F3 F1A 0.77(9) . ? F3 C6 1.28(5) . ? F3 F2A 1.63(7) . ? F1A C6 1.31(5) . ? F2A C6 1.32(4) . ? F3A C6 1.38(4) . ? F4 F6A 0.77(6) . ? F4 C12 1.29(4) . ? F4 F5A 1.55(6) . ? F5 F4A 0.87(5) . ? F5 C12 1.39(3) . ? F5 F6A 1.59(5) . ? F6 F5A 0.75(6) . ? F6 C12 1.35(4) . ? F6 F4A 1.53(6) . ? F4A C12 1.20(3) . ? F5A C12 1.24(3) . ? F6A C12 1.28(3) . ? C1 C2 1.402(16) . ? C2 C3 1.398(17) . ? C3 C4 1.392(17) . ? C4 C5 1.404(16) . ? C4 C6 1.482(18) . ? C7 C8 1.371(15) . ? C8 C9 1.375(15) . ? C9 C10 1.375(15) . ? C10 C11 1.380(15) . ? C10 C12 1.503(15) . ? 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 S2 Hg1 S1 178.36(11) . . ? S2 Hg1 N1 120.1(2) . . ? S1 Hg1 N1 61.2(2) . . ? S2 Hg1 N2 58.38(19) . . ? S1 Hg1 N2 120.18(19) . . ? N1 Hg1 N2 123.8(3) . . ? C1 S1 Hg1 94.4(4) . . ? C7 S2 Hg1 99.7(4) . . ? C5 N1 C1 118.2(10) . . ? C5 N1 Hg1 153.9(8) . . ? C1 N1 Hg1 86.4(7) . . ? C11 N2 C7 118.8(9) . . ? C11 N2 Hg1 159.0(7) . . ? C7 N2 Hg1 82.1(6) . . ? F2A F1 C6 78(4) . . ? F2A F1 F3A 124(6) . . ? C6 F1 F3A 54.2(18) . . ? F3A F2 C6 80(5) . . ? F3A F2 F1A 131(6) . . ? C6 F2 F1A 56(2) . . ? F1A F3 C6 74(8) . . ? F1A F3 F2A 115(10) . . ? C6 F3 F2A 52(3) . . ? F3 F1A C6 71(7) . . ? F3 F1A F2 124(9) . . ? C6 F1A F2 54(3) . . ? F1 F2A C6 66(4) . . ? F1 F2A F3 115(6) . . ? C6 F2A F3 50(2) . . ? F2 F3A C6 65(4) . . ? F2 F3A F1 106(5) . . ? C6 F3A F1 46.4(19) . . ? F6A F4 C12 72(4) . . ? F6A F4 F5A 117(6) . . ? C12 F4 F5A 51(2) . . ? F4A F5 C12 59(2) . . ? F4A F5 F6A 106(4) . . ? C12 F5 F6A 50.1(17) . . ? F5A F6 C12 65(4) . . ? F5A F6 F4A 109(5) . . ? C12 F6 F4A 49(2) . . ? F5 F4A C12 82(4) . . ? F5 F4A F6 133(5) . . ? C12 F4A F6 58(2) . . ? F6 F5A C12 81(5) . . ? F6 F5A F4 131(6) . . ? C12 F5A F4 53.6(19) . . ? F4 F6A C12 74(5) . . ? F4 F6A F5 124(6) . . ? C12 F6A F5 56.6(19) . . ? N1 C1 C2 122.2(10) . . ? N1 C1 S1 117.3(8) . . ? C2 C1 S1 120.5(8) . . ? C3 C2 C1 118.7(11) . . ? C4 C3 C2 119.1(11) . . ? C3 C4 C5 117.3(11) . . ? C3 C4 C6 119.9(12) . . ? C5 C4 C6 122.7(12) . . ? N1 C5 C4 124.5(11) . . ? F1 C6 F2 111(3) . . ? F1 C6 F3 112(3) . . ? F2 C6 F3 104(3) . . ? F1 C6 F1A 130(3) . . ? F2 C6 F1A 70(3) . . ? F3 C6 F1A 35(4) . . ? F1 C6 F2A 36(2) . . ? F2 C6 F2A 130(3) . . ? F3 C6 F2A 77(3) . . ? F1A C6 F2A 104(4) . . ? F1 C6 F3A 79(3) . . ? F2 C6 F3A 36(2) . . ? F3 C6 F3A 133(3) . . ? F1A C6 F3A 103(4) . . ? F2A C6 F3A 110(3) . . ? F1 C6 C4 111.8(19) . . ? F2 C6 C4 110.9(18) . . ? F3 C6 C4 108(3) . . ? F1A C6 C4 114(3) . . ? F2A C6 C4 116(2) . . ? F3A C6 C4 109(2) . . ? N2 C7 C8 122.3(10) . . ? N2 C7 S2 119.8(7) . . ? C8 C7 S2 117.9(8) . . ? C7 C8 C9 118.4(11) . . ? C8 C9 C10 120.0(11) . . ? C9 C10 C11 117.6(10) . . ? C9 C10 C12 121.3(10) . . ? C11 C10 C12 121.0(11) . . ? N2 C11 C10 122.8(10) . . ? F4A C12 F5A 102(3) . . ? F4A C12 F6A 108(3) . . ? F5A C12 F6A 106(3) . . ? F4A C12 F4 131(2) . . ? F5A C12 F4 75(3) . . ? F6A C12 F4 35(3) . . ? F4A C12 F6 73(3) . . ? F5A C12 F6 33(3) . . ? F6A C12 F6 131(3) . . ? F4 C12 F6 107(3) . . ? F4A C12 F5 38(3) . . ? F5A C12 F5 128(3) . . ? F6A C12 F5 73(2) . . ? F4 C12 F5 105(3) . . ? F6 C12 F5 108(3) . . ? F4A C12 C10 111.3(19) . . ? F5A C12 C10 114.3(18) . . ? F6A C12 C10 113.6(18) . . ? F4 C12 C10 114(2) . . ? F6 C12 C10 111(2) . . ? F5 C12 C10 112.7(18) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.43 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.847 _refine_diff_density_min -2.113 _refine_diff_density_rms 0.198