# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 #TrackingRef '- CoMQ.cif' #================================================= # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Professor Xiao-Ming Chen MOE Laboratory of bioinorganic and Synthetic Chemistry School of Chemistry and Chemical Engineering Sun Yst-Sen University Guangzhou 510275 P. R. China ; _publ_contact_author_phone 86-20-84113986 _publ_contact_author_fax 86-20-84112074 _publ_contact_author_email cxm@mail.sysu.edu.cn _publ_requested_coeditor_name ? _publ_contact_letter ; Dear Editor: Please consider this CIF as supplmentary data for a manuscript submitted to Angew. Chem. Int. Ed. Please note that the sample was measured at seven different temperatures. Thanks Xiao-Ming Chen ; #================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_coden_ASTM ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; A One-Dimensional Coordination Polymer Exhibiting Spin- Crossover and Semiconductor Behavior ; loop_ _publ_author_name _publ_author_address 'Wei Xue' ; MOE Laboratory of bioinorganic and Synthetic Chemistry School of Chemistry and Chemical Engineering Sun Yat-Sen University Guangzhou 510275 P. R. China ; 'Bao-Ying Wang' ; MOE Laboratory of bioinorganic and Synthetic Chemistry School of Chemistry and Chemical Engineering Sun Yat-Sen University Guangzhou 510275 P. R. China ; 'Jie Zhu' ; MOE Laboratory of bioinorganic and Synthetic Chemistry School of Chemistry and Chemical Engineering Sun Yat-Sen University Guangzhou 510275 P. R. China ; 'Wei-Xiong Zhang' ; MOE Laboratory of bioinorganic and Synthetic Chemistry School of Chemistry and Chemical Engineering Sun Yat-Sen University Guangzhou 510275 P. R. China ; 'Yue-Biao Zhang' ; MOE Laboratory of bioinorganic and Synthetic Chemistry School of Chemistry and Chemical Engineering Sun Yat-Sen University Guangzhou 510275 P. R. China ; ; Hai-Xia Zhao ; ; State Key Laboratory of Physical Chemistry of Solid Surface College of Chemistry and Chemical Engineering Xiamen University Xiamen 361005 P. R. China ; 'Xiao-Ming Chen' ; MOE Laboratory of bioinorganic and Synthetic Chemistry School of Chemistry and Chemical Engineering Sun Yat-Sen University Guangzhou 510275 P. R. China ; _publ_contact_author_name 'Professor Xiao-Ming Chen' #============================================================ data_1@112K _database_code_depnum_ccdc_archive 'CCDC 799875' #TrackingRef '- CoMQ.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common CoMQ _chemical_melting_point ? _chemical_formula_moiety 'C18 H12 Co N2 S2' _chemical_formula_sum 'C18 H12 Co N2 S2' _chemical_formula_weight 379.35 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' Co Co 0.3494 0.9721 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(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 3.6858(4) _cell_length_b 14.6127(15) _cell_length_c 12.8816(13) _cell_angle_alpha 90.00 _cell_angle_beta 93.1048(16) _cell_angle_gamma 90.00 _cell_volume 692.78(12) _cell_formula_units_Z 2 _cell_measurement_temperature 112(2) _cell_measurement_reflns_used 3445 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 26.0 _exptl_crystal_description needle-like _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.819 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 386 _exptl_absorpt_coefficient_mu 1.538 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.912 _exptl_absorpt_correction_T_max 0.926 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 112(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3445 _diffrn_reflns_av_R_equivalents 0.0159 _diffrn_reflns_av_sigmaI/netI 0.0188 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.99 _reflns_number_total 1349 _reflns_number_gt 1313 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART Bruker AXS Inc., 1998.' _computing_cell_refinement 'SAINT+ Ver. 6.22, Bruker AXS Inc., 2001.' _computing_data_reduction 'SAINT+ Ver. 6.22, Bruker AXS Inc., 2001.' _computing_structure_solution 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _computing_molecular_graphics 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _computing_publication_material 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0514P)^2^+0.4287P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1349 _refine_ls_number_parameters 106 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0279 _refine_ls_R_factor_gt 0.0274 _refine_ls_wR_factor_ref 0.0789 _refine_ls_wR_factor_gt 0.0784 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _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 Co1 Co 0.0000 0.5000 0.0000 0.01411(15) Uani 1 2 d S . . S1 S 0.43622(11) 0.44011(3) 0.11142(3) 0.01633(16) Uani 1 1 d . . . N1 N 0.0489(4) 0.61124(10) 0.08634(11) 0.0141(3) Uani 1 1 d . . . C8 C 0.3899(5) 0.51909(13) 0.21095(14) 0.0152(4) Uani 1 1 d . . . C4 C 0.1939(5) 0.67369(13) 0.25964(14) 0.0169(4) Uani 1 1 d . . . C9 C 0.2069(4) 0.60234(12) 0.18582(13) 0.0144(4) Uani 1 1 d . . . C5 C 0.3463(5) 0.65841(14) 0.36164(14) 0.0198(4) Uani 1 1 d . . . H5 H 0.3339 0.7039 0.4119 0.024 Uiso 1 1 calc R . . C7 C 0.5396(5) 0.50765(13) 0.31146(16) 0.0189(4) Uani 1 1 d . . . H7 H 0.6599 0.4535 0.3294 0.023 Uiso 1 1 calc R . . C3 C 0.0346(5) 0.75769(13) 0.22821(16) 0.0189(4) Uani 1 1 d . . . H3 H 0.0194 0.8057 0.2751 0.023 Uiso 1 1 calc R . . C1 C -0.0895(5) 0.69244(12) 0.05947(14) 0.0167(4) Uani 1 1 d . . . H1 H -0.1865 0.6999 -0.0082 0.020 Uiso 1 1 calc R . . C6 C 0.5113(5) 0.57686(15) 0.38612(14) 0.0212(4) Uani 1 1 d . . . H6 H 0.6066 0.5671 0.4535 0.025 Uiso 1 1 calc R . . C2 C -0.0975(5) 0.76727(13) 0.12714(15) 0.0194(4) Uani 1 1 d . . . H2 H -0.1917 0.8231 0.1038 0.023 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 Co1 0.0171(2) 0.0104(2) 0.0143(2) -0.00096(11) -0.00354(14) 0.00101(11) S1 0.0178(3) 0.0136(3) 0.0173(3) -0.00046(16) -0.00144(18) 0.00034(16) N1 0.0126(7) 0.0145(7) 0.0152(7) 0.0010(6) -0.0001(5) -0.0005(6) C8 0.0135(8) 0.0164(8) 0.0159(9) 0.0008(7) 0.0022(7) -0.0026(7) C4 0.0123(7) 0.0196(9) 0.0189(8) -0.0020(7) 0.0019(6) -0.0047(7) C9 0.0123(8) 0.0153(8) 0.0156(8) 0.0007(7) 0.0010(6) -0.0027(7) C5 0.0182(8) 0.0243(10) 0.0171(9) -0.0049(7) 0.0015(7) -0.0058(7) C7 0.0148(9) 0.0206(10) 0.0210(10) 0.0054(7) -0.0007(8) -0.0005(7) C3 0.0178(8) 0.0157(9) 0.0237(9) -0.0059(7) 0.0047(7) -0.0034(7) C1 0.0148(8) 0.0157(8) 0.0194(8) 0.0021(7) -0.0004(6) -0.0017(7) C6 0.0180(8) 0.0302(10) 0.0150(9) 0.0026(7) -0.0013(7) -0.0070(8) C2 0.0170(8) 0.0125(8) 0.0286(10) 0.0014(7) 0.0020(7) 0.0006(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 Co1 N1 1.9723(15) . ? Co1 N1 1.9723(15) 3_565 ? Co1 S1 2.2718(5) 3_565 ? Co1 S1 2.2718(5) . ? Co1 S1 2.7325(5) 1_455 ? Co1 S1 2.7325(5) 3_665 ? S1 C8 1.7404(19) . ? S1 Co1 2.7325(5) 1_655 ? N1 C1 1.330(2) . ? N1 C9 1.385(2) . ? C8 C7 1.390(3) . ? C8 C9 1.420(3) . ? C4 C3 1.411(3) . ? C4 C9 1.414(3) . ? C4 C5 1.418(3) . ? C5 C6 1.367(3) . ? C7 C6 1.403(3) . ? C3 C2 1.372(3) . ? C1 C2 1.400(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N1 180.00(9) . 3_565 ? N1 Co1 S1 94.51(4) . 3_565 ? N1 Co1 S1 85.49(5) 3_565 3_565 ? N1 Co1 S1 85.49(4) . . ? N1 Co1 S1 94.51(4) 3_565 . ? S1 Co1 S1 180.00(2) 3_565 . ? N1 Co1 S1 90.95(4) . 1_455 ? N1 Co1 S1 89.05(4) 3_565 1_455 ? S1 Co1 S1 85.577(16) 3_565 1_455 ? S1 Co1 S1 94.423(16) . 1_455 ? N1 Co1 S1 89.05(4) . 3_665 ? N1 Co1 S1 90.95(4) 3_565 3_665 ? S1 Co1 S1 94.423(16) 3_565 3_665 ? S1 Co1 S1 85.577(16) . 3_665 ? S1 Co1 S1 180.0 1_455 3_665 ? C8 S1 Co1 96.64(7) . . ? C8 S1 Co1 106.40(6) . 1_655 ? Co1 S1 Co1 94.423(16) . 1_655 ? C1 N1 C9 117.44(15) . . ? C1 N1 Co1 124.51(12) . . ? C9 N1 Co1 117.74(12) . . ? C7 C8 C9 118.38(17) . . ? C7 C8 S1 123.83(15) . . ? C9 C8 S1 117.68(14) . . ? C3 C4 C9 118.51(17) . . ? C3 C4 C5 122.73(18) . . ? C9 C4 C5 118.75(17) . . ? N1 C9 C4 121.69(16) . . ? N1 C9 C8 117.54(16) . . ? C4 C9 C8 120.76(16) . . ? C6 C5 C4 119.98(17) . . ? C8 C7 C6 120.75(17) . . ? C2 C3 C4 118.82(17) . . ? N1 C1 C2 123.75(17) . . ? C5 C6 C7 121.25(17) . . ? C3 C2 C1 119.52(17) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.605 _refine_diff_density_min -0.298 _refine_diff_density_rms 0.080 #=================================================END data_1@138K _database_code_depnum_ccdc_archive 'CCDC 799876' #TrackingRef '- CoMQ.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common CoMQ _chemical_melting_point ? _chemical_formula_moiety 'C18 H12 Co N2 S2' _chemical_formula_sum 'C18 H12 Co N2 S2' _chemical_formula_weight 379.35 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' Co Co 0.3494 0.9721 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(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 3.6896(4) _cell_length_b 14.6443(15) _cell_length_c 12.9107(13) _cell_angle_alpha 90.00 _cell_angle_beta 92.9027(16) _cell_angle_gamma 90.00 _cell_volume 696.69(13) _cell_formula_units_Z 2 _cell_measurement_temperature 138(2) _cell_measurement_reflns_used 3483 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 26.0 _exptl_crystal_description needle-like _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.808 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 386 _exptl_absorpt_coefficient_mu 1.529 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.912 _exptl_absorpt_correction_T_max 0.926 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 138(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3483 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 26.00 _reflns_number_total 1357 _reflns_number_gt 1304 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART Bruker AXS Inc., 1998.' _computing_cell_refinement 'SAINT+ Ver. 6.22, Bruker AXS Inc., 2001.' _computing_data_reduction 'SAINT+ Ver. 6.22, Bruker AXS Inc., 2001.' _computing_structure_solution 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _computing_molecular_graphics 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _computing_publication_material 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0605P)^2^+0.3237P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1357 _refine_ls_number_parameters 106 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0334 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0923 _refine_ls_wR_factor_gt 0.0915 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _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 Co1 Co 0.5000 0.5000 0.5000 0.01686(17) Uani 1 2 d S . . S1 S 0.05925(13) 0.55941(3) 0.38777(4) 0.01993(18) Uani 1 1 d . . . N1 N 0.4478(4) 0.38774(11) 0.41294(12) 0.0172(3) Uani 1 1 d . . . C7 C -0.0381(6) 0.49157(14) 0.18860(18) 0.0224(5) Uani 1 1 d . . . H7 H -0.1572 0.5457 0.1706 0.027 Uiso 1 1 calc R . . C8 C 0.1089(5) 0.48009(14) 0.28889(15) 0.0184(4) Uani 1 1 d . . . C4 C 0.3048(5) 0.32586(14) 0.24013(15) 0.0203(4) Uani 1 1 d . . . C9 C 0.2911(5) 0.39683(13) 0.31378(14) 0.0170(4) Uani 1 1 d . . . C5 C 0.1541(6) 0.34128(15) 0.13843(16) 0.0240(4) Uani 1 1 d . . . H5 H 0.1668 0.2959 0.0883 0.029 Uiso 1 1 calc R . . C1 C 0.5871(5) 0.30694(13) 0.43974(16) 0.0203(4) Uani 1 1 d . . . H1 H 0.6840 0.2995 0.5071 0.024 Uiso 1 1 calc R . . C6 C -0.0094(6) 0.42262(16) 0.11407(16) 0.0248(5) Uani 1 1 d . . . H6 H -0.1036 0.4325 0.0468 0.030 Uiso 1 1 calc R . . C3 C 0.4640(6) 0.24192(14) 0.27153(18) 0.0230(4) Uani 1 1 d . . . H3 H 0.4789 0.1940 0.2247 0.028 Uiso 1 1 calc R . . C2 C 0.5959(5) 0.23231(14) 0.37192(17) 0.0235(4) Uani 1 1 d . . . H2 H 0.6907 0.1767 0.3950 0.028 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 Co1 0.0191(2) 0.0127(3) 0.0183(3) -0.00134(12) -0.00381(17) 0.00126(12) S1 0.0214(3) 0.0158(3) 0.0225(3) -0.00057(17) -0.0001(2) 0.00085(17) N1 0.0145(7) 0.0171(8) 0.0199(8) 0.0014(6) 0.0011(6) -0.0003(6) C7 0.0171(10) 0.0249(11) 0.0252(11) 0.0068(8) 0.0000(9) -0.0014(7) C8 0.0152(9) 0.0198(9) 0.0204(10) 0.0019(8) 0.0036(7) -0.0016(8) C4 0.0137(8) 0.0225(9) 0.0250(10) -0.0026(8) 0.0044(7) -0.0051(7) C9 0.0130(8) 0.0184(9) 0.0198(9) 0.0000(7) 0.0021(7) -0.0032(7) C5 0.0217(10) 0.0286(11) 0.0219(10) -0.0069(8) 0.0031(8) -0.0077(8) C1 0.0171(9) 0.0184(9) 0.0255(10) 0.0025(8) 0.0007(7) -0.0012(7) C6 0.0198(9) 0.0344(12) 0.0200(10) 0.0029(8) -0.0011(8) -0.0081(8) C3 0.0202(9) 0.0193(10) 0.0302(10) -0.0068(8) 0.0069(8) -0.0038(8) C2 0.0195(9) 0.0157(9) 0.0355(12) 0.0016(8) 0.0033(8) 0.0010(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 Co1 N1 1.9953(16) . ? Co1 N1 1.9953(16) 3_666 ? Co1 S1 2.2940(5) 3_666 ? Co1 S1 2.2940(5) . ? Co1 S1 2.7234(5) 3_566 ? Co1 S1 2.7234(5) 1_655 ? S1 C8 1.742(2) . ? S1 Co1 2.7234(5) 1_455 ? N1 C1 1.329(3) . ? N1 C9 1.384(3) . ? C7 C8 1.389(3) . ? C7 C6 1.402(3) . ? C8 C9 1.421(3) . ? C4 C9 1.411(3) . ? C4 C3 1.413(3) . ? C4 C5 1.418(3) . ? C5 C6 1.365(3) . ? C1 C2 1.402(3) . ? C3 C2 1.368(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N1 180.000(1) . 3_666 ? N1 Co1 S1 95.07(5) . 3_666 ? N1 Co1 S1 84.93(5) 3_666 3_666 ? N1 Co1 S1 84.93(5) . . ? N1 Co1 S1 95.07(5) 3_666 . ? S1 Co1 S1 180.0 3_666 . ? N1 Co1 S1 88.99(4) . 3_566 ? N1 Co1 S1 91.01(4) 3_666 3_566 ? S1 Co1 S1 94.286(18) 3_666 3_566 ? S1 Co1 S1 85.714(18) . 3_566 ? N1 Co1 S1 91.01(4) . 1_655 ? N1 Co1 S1 88.99(4) 3_666 1_655 ? S1 Co1 S1 85.714(18) 3_666 1_655 ? S1 Co1 S1 94.286(18) . 1_655 ? S1 Co1 S1 180.0 3_566 1_655 ? C8 S1 Co1 96.46(7) . . ? C8 S1 Co1 106.70(7) . 1_455 ? Co1 S1 Co1 94.286(18) . 1_455 ? C1 N1 C9 117.67(17) . . ? C1 N1 Co1 124.20(14) . . ? C9 N1 Co1 117.75(12) . . ? C8 C7 C6 120.87(19) . . ? C7 C8 C9 118.21(19) . . ? C7 C8 S1 123.50(16) . . ? C9 C8 S1 118.18(15) . . ? C9 C4 C3 118.42(19) . . ? C9 C4 C5 118.75(19) . . ? C3 C4 C5 122.82(19) . . ? N1 C9 C4 121.65(18) . . ? N1 C9 C8 117.54(17) . . ? C4 C9 C8 120.80(18) . . ? C6 C5 C4 120.02(19) . . ? N1 C1 C2 123.54(19) . . ? C5 C6 C7 121.21(19) . . ? C2 C3 C4 118.94(19) . . ? C3 C2 C1 119.55(19) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.658 _refine_diff_density_min -0.407 _refine_diff_density_rms 0.093 #=================================================END data_1@165K _database_code_depnum_ccdc_archive 'CCDC 799877' #TrackingRef '- CoMQ.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common CoMQ _chemical_melting_point ? _chemical_formula_moiety 'C18 H12 Co N2 S2' _chemical_formula_sum 'C18 H12 Co N2 S2' _chemical_formula_weight 379.35 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' Co Co 0.3494 0.9721 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(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 3.6911(4) _cell_length_b 14.6918(14) _cell_length_c 12.9593(12) _cell_angle_alpha 90.00 _cell_angle_beta 92.4986(15) _cell_angle_gamma 90.00 _cell_volume 702.10(12) _cell_formula_units_Z 2 _cell_measurement_temperature 165(2) _cell_measurement_reflns_used 3524 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 26.0 _exptl_crystal_description needle-like _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.794 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 386 _exptl_absorpt_coefficient_mu 1.518 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.913 _exptl_absorpt_correction_T_max 0.927 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 165(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3524 _diffrn_reflns_av_R_equivalents 0.0132 _diffrn_reflns_av_sigmaI/netI 0.0141 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 3 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 26.00 _reflns_number_total 1370 _reflns_number_gt 1316 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART Bruker AXS Inc., 1998.' _computing_cell_refinement 'SAINT+ Ver. 6.22, Bruker AXS Inc., 2001.' _computing_data_reduction 'SAINT+ Ver. 6.22, Bruker AXS Inc., 2001.' _computing_structure_solution 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _computing_molecular_graphics 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _computing_publication_material 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+0.4187P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1370 _refine_ls_number_parameters 106 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0276 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0764 _refine_ls_wR_factor_gt 0.0758 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _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 Co1 Co 0.0000 0.5000 0.0000 0.01917(14) Uani 1 2 d S . . S1 S 0.45122(12) 0.44165(3) 0.11382(4) 0.02263(15) Uani 1 1 d . . . N1 N 0.0581(4) 0.61451(10) 0.08841(11) 0.0195(3) Uani 1 1 d . . . C7 C 0.5376(5) 0.51018(14) 0.31137(16) 0.0250(4) Uani 1 1 d . . . H7 H 0.6557 0.4562 0.3293 0.030 Uiso 1 1 calc R . . C9 C 0.2130(4) 0.60493(12) 0.18662(13) 0.0194(4) Uani 1 1 d . . . C4 C 0.1969(5) 0.67539(13) 0.26050(15) 0.0225(4) Uani 1 1 d . . . C5 C 0.3440(5) 0.65985(14) 0.36174(15) 0.0268(4) Uani 1 1 d . . . H5 H 0.3303 0.7050 0.4118 0.032 Uiso 1 1 calc R . . C8 C 0.3956(5) 0.52174(13) 0.21148(14) 0.0203(4) Uani 1 1 d . . . C6 C 0.5060(5) 0.57863(16) 0.38582(15) 0.0281(4) Uani 1 1 d . . . H6 H 0.5970 0.5685 0.4529 0.034 Uiso 1 1 calc R . . C1 C -0.0834(5) 0.69473(13) 0.06239(15) 0.0229(4) Uani 1 1 d . . . H1 H -0.1815 0.7020 -0.0044 0.027 Uiso 1 1 calc R . . C2 C -0.0933(5) 0.76892(13) 0.12986(16) 0.0264(4) Uani 1 1 d . . . H2 H -0.1880 0.8244 0.1072 0.032 Uiso 1 1 calc R . . C3 C 0.0379(5) 0.75890(13) 0.22960(17) 0.0261(4) Uani 1 1 d . . . H3 H 0.0225 0.8066 0.2764 0.031 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 Co1 0.0224(2) 0.0146(2) 0.0200(2) -0.00209(12) -0.00515(14) 0.00169(12) S1 0.0252(3) 0.0179(2) 0.0248(3) -0.00040(17) 0.00043(19) 0.00110(16) N1 0.0178(7) 0.0197(7) 0.0210(7) 0.0022(6) 0.0009(6) 0.0007(6) C7 0.0200(9) 0.0281(10) 0.0268(10) 0.0062(8) 0.0002(8) -0.0015(7) C9 0.0165(8) 0.0204(9) 0.0213(8) 0.0006(7) 0.0025(6) -0.0031(7) C4 0.0168(8) 0.0245(9) 0.0266(9) -0.0030(8) 0.0043(7) -0.0053(7) C5 0.0233(9) 0.0327(11) 0.0245(9) -0.0071(8) 0.0031(7) -0.0078(8) C8 0.0177(8) 0.0216(8) 0.0217(9) 0.0013(7) 0.0033(7) -0.0014(7) C6 0.0230(9) 0.0396(11) 0.0214(9) 0.0022(8) -0.0004(7) -0.0081(8) C1 0.0192(8) 0.0212(9) 0.0283(9) 0.0037(7) 0.0011(7) -0.0012(7) C2 0.0227(9) 0.0173(9) 0.0393(11) 0.0008(8) 0.0034(8) 0.0007(7) C3 0.0230(9) 0.0209(9) 0.0348(10) -0.0071(8) 0.0072(8) -0.0034(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 Co1 N1 2.0414(15) . ? Co1 N1 2.0414(15) 3_565 ? Co1 S1 2.3389(5) 3_565 ? Co1 S1 2.3389(5) . ? Co1 S1 2.6971(5) 3_665 ? Co1 S1 2.6971(5) 1_455 ? S1 C8 1.7468(19) . ? S1 Co1 2.6971(5) 1_655 ? N1 C1 1.327(2) . ? N1 C9 1.380(2) . ? C7 C8 1.386(3) . ? C7 C6 1.402(3) . ? C9 C4 1.413(3) . ? C9 C8 1.426(3) . ? C4 C3 1.410(3) . ? C4 C5 1.416(3) . ? C5 C6 1.365(3) . ? C1 C2 1.399(3) . ? C2 C3 1.368(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N1 180.00(9) . 3_565 ? N1 Co1 S1 96.10(4) . 3_565 ? N1 Co1 S1 83.90(4) 3_565 3_565 ? N1 Co1 S1 83.90(4) . . ? N1 Co1 S1 96.10(4) 3_565 . ? S1 Co1 S1 180.00(2) 3_565 . ? N1 Co1 S1 88.97(4) . 3_665 ? N1 Co1 S1 91.03(4) 3_565 3_665 ? S1 Co1 S1 93.996(17) 3_565 3_665 ? S1 Co1 S1 86.004(17) . 3_665 ? N1 Co1 S1 91.03(4) . 1_455 ? N1 Co1 S1 88.97(4) 3_565 1_455 ? S1 Co1 S1 86.004(17) 3_565 1_455 ? S1 Co1 S1 93.996(17) . 1_455 ? S1 Co1 S1 180.0 3_665 1_455 ? C8 S1 Co1 96.14(7) . . ? C8 S1 Co1 107.27(6) . 1_655 ? Co1 S1 Co1 93.996(17) . 1_655 ? C1 N1 C9 117.89(16) . . ? C1 N1 Co1 123.98(13) . . ? C9 N1 Co1 117.57(12) . . ? C8 C7 C6 121.03(19) . . ? N1 C9 C4 121.49(17) . . ? N1 C9 C8 117.95(16) . . ? C4 C9 C8 120.55(17) . . ? C3 C4 C9 118.30(18) . . ? C3 C4 C5 122.77(18) . . ? C9 C4 C5 118.93(18) . . ? C6 C5 C4 119.95(18) . . ? C7 C8 C9 118.16(17) . . ? C7 C8 S1 122.86(15) . . ? C9 C8 S1 118.89(14) . . ? C5 C6 C7 121.24(19) . . ? N1 C1 C2 123.64(17) . . ? C3 C2 C1 119.26(18) . . ? C2 C3 C4 119.18(18) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.511 _refine_diff_density_min -0.259 _refine_diff_density_rms 0.072 #=================================================END data_1@192K _database_code_depnum_ccdc_archive 'CCDC 799878' #TrackingRef '- CoMQ.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common CoMQ _chemical_melting_point ? _chemical_formula_moiety 'C18 H12 Co N2 S2' _chemical_formula_sum 'C18 H12 Co N2 S2' _chemical_formula_weight 379.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(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 3.6947(3) _cell_length_b 14.7215(13) _cell_length_c 12.9900(12) _cell_angle_alpha 90.00 _cell_angle_beta 92.2964(14) _cell_angle_gamma 90.00 _cell_volume 705.98(11) _cell_formula_units_Z 2 _cell_measurement_temperature 192(2) _cell_measurement_reflns_used 3539 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 26.0 _exptl_crystal_description needle-like _exptl_crystal_colour black _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.785 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 386 _exptl_absorpt_coefficient_mu 1.509 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.913 _exptl_absorpt_correction_T_max 0.926 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 192(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3539 _diffrn_reflns_av_R_equivalents 0.0139 _diffrn_reflns_av_sigmaI/netI 0.0147 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.98 _reflns_number_total 1373 _reflns_number_gt 1334 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART Bruker AXS Inc., 1998.' _computing_cell_refinement 'SAINT+ Ver. 6.22, Bruker AXS Inc., 2001.' _computing_data_reduction 'SAINT+ Ver. 6.22, Bruker AXS Inc., 2001.' _computing_structure_solution 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _computing_molecular_graphics 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _computing_publication_material 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0488P)^2^+0.3976P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1373 _refine_ls_number_parameters 106 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0277 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_ref 0.0767 _refine_ls_wR_factor_gt 0.0761 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 Co1 Co 0.5000 0.5000 0.5000 0.02136(14) Uani 1 2 d S . . S1 S 0.04387(12) 0.55782(3) 0.38531(3) 0.02403(15) Uani 1 1 d . . . N1 N 0.4389(4) 0.38433(10) 0.41092(11) 0.0209(3) Uani 1 1 d . . . C1 C 0.5815(5) 0.30454(13) 0.43661(15) 0.0246(4) Uani 1 1 d . . . H1 H 0.6801 0.2973 0.5031 0.029 Uiso 1 1 calc R . . C8 C 0.1027(5) 0.47731(13) 0.28843(14) 0.0218(4) Uani 1 1 d . . . C6 C -0.0043(5) 0.42067(16) 0.11427(15) 0.0311(4) Uani 1 1 d . . . H6 H -0.0943 0.4308 0.0474 0.037 Uiso 1 1 calc R . . C4 C 0.3022(5) 0.32397(13) 0.23919(14) 0.0248(4) Uani 1 1 d . . . C7 C -0.0367(5) 0.48896(14) 0.18857(16) 0.0272(4) Uani 1 1 d . . . H7 H -0.1535 0.5430 0.1706 0.033 Uiso 1 1 calc R . . C5 C 0.1565(5) 0.33962(14) 0.13823(15) 0.0298(4) Uani 1 1 d . . . H5 H 0.1706 0.2946 0.0883 0.036 Uiso 1 1 calc R . . C3 C 0.4608(5) 0.24066(13) 0.26991(16) 0.0281(4) Uani 1 1 d . . . H3 H 0.4761 0.1931 0.2231 0.034 Uiso 1 1 calc R . . C9 C 0.2847(4) 0.39433(12) 0.31313(13) 0.0208(4) Uani 1 1 d . . . C2 C 0.5918(5) 0.23041(13) 0.36915(16) 0.0287(4) Uani 1 1 d . . . H2 H 0.6865 0.1750 0.3916 0.034 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 Co1 0.0254(2) 0.0165(2) 0.0217(2) -0.00248(11) -0.00598(15) 0.00235(12) S1 0.0264(3) 0.0195(2) 0.0261(3) -0.00038(16) -0.00019(18) 0.00103(16) N1 0.0193(7) 0.0203(7) 0.0230(7) 0.0018(6) 0.0013(6) -0.0006(6) C1 0.0223(8) 0.0218(9) 0.0295(9) 0.0034(7) 0.0005(7) -0.0010(7) C8 0.0194(8) 0.0235(8) 0.0226(9) 0.0015(7) 0.0024(6) -0.0017(7) C6 0.0257(9) 0.0447(12) 0.0227(9) 0.0021(8) -0.0009(7) -0.0089(8) C4 0.0188(8) 0.0274(9) 0.0285(9) -0.0044(8) 0.0044(7) -0.0060(7) C7 0.0226(9) 0.0309(10) 0.0280(10) 0.0066(8) -0.0004(8) -0.0022(7) C5 0.0266(9) 0.0370(11) 0.0260(9) -0.0085(8) 0.0036(7) -0.0089(8) C3 0.0246(9) 0.0227(9) 0.0374(10) -0.0084(8) 0.0068(8) -0.0037(7) C9 0.0180(7) 0.0220(8) 0.0226(8) 0.0000(7) 0.0024(6) -0.0034(6) C2 0.0255(9) 0.0184(9) 0.0424(11) 0.0004(8) 0.0034(8) 0.0007(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 Co1 N1 2.0661(15) . ? Co1 N1 2.0661(15) 3_666 ? Co1 S1 2.3629(5) 3_666 ? Co1 S1 2.3629(5) . ? Co1 S1 2.6874(5) 3_566 ? Co1 S1 2.6874(5) 1_655 ? S1 C8 1.7486(19) . ? S1 Co1 2.6874(5) 1_455 ? N1 C1 1.325(2) . ? N1 C9 1.379(2) . ? C1 C2 1.401(3) . ? C8 C7 1.387(3) . ? C8 C9 1.425(3) . ? C6 C5 1.363(3) . ? C6 C7 1.402(3) . ? C4 C3 1.410(3) . ? C4 C9 1.416(3) . ? C4 C5 1.416(3) . ? C3 C2 1.367(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N1 180.000(1) . 3_666 ? N1 Co1 S1 96.62(4) . 3_666 ? N1 Co1 S1 83.38(4) 3_666 3_666 ? N1 Co1 S1 83.38(4) . . ? N1 Co1 S1 96.62(4) 3_666 . ? S1 Co1 S1 180.0 3_666 . ? N1 Co1 S1 88.97(4) . 3_566 ? N1 Co1 S1 91.03(4) 3_666 3_566 ? S1 Co1 S1 93.817(16) 3_666 3_566 ? S1 Co1 S1 86.183(16) . 3_566 ? N1 Co1 S1 91.03(4) . 1_655 ? N1 Co1 S1 88.97(4) 3_666 1_655 ? S1 Co1 S1 86.183(16) 3_666 1_655 ? S1 Co1 S1 93.817(16) . 1_655 ? S1 Co1 S1 180.0 3_566 1_655 ? C8 S1 Co1 95.94(6) . . ? C8 S1 Co1 107.55(6) . 1_455 ? Co1 S1 Co1 93.817(16) . 1_455 ? C1 N1 C9 118.17(16) . . ? C1 N1 Co1 123.81(12) . . ? C9 N1 Co1 117.37(11) . . ? N1 C1 C2 123.62(17) . . ? C7 C8 C9 118.09(17) . . ? C7 C8 S1 122.48(15) . . ? C9 C8 S1 119.36(14) . . ? C5 C6 C7 121.25(18) . . ? C3 C4 C9 118.30(17) . . ? C3 C4 C5 122.80(18) . . ? C9 C4 C5 118.90(18) . . ? C8 C7 C6 121.10(19) . . ? C6 C5 C4 119.98(18) . . ? C2 C3 C4 119.35(17) . . ? N1 C9 C4 121.23(16) . . ? N1 C9 C8 118.21(16) . . ? C4 C9 C8 120.55(16) . . ? C3 C2 C1 119.11(18) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.511 _refine_diff_density_min -0.254 _refine_diff_density_rms 0.068 #=================================================END data_1@218K _database_code_depnum_ccdc_archive 'CCDC 799879' #TrackingRef '- CoMQ.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common CoMQ _chemical_melting_point ? _chemical_formula_moiety 'C18 H12 Co N2 S2' _chemical_formula_sum 'C18 H12 Co N2 S2' _chemical_formula_weight 379.35 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' Co Co 0.3494 0.9721 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(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 3.6988(3) _cell_length_b 14.7379(12) _cell_length_c 13.0078(11) _cell_angle_alpha 90.00 _cell_angle_beta 92.2308(13) _cell_angle_gamma 90.00 _cell_volume 708.55(10) _cell_formula_units_Z 2 _cell_measurement_temperature 218(2) _cell_measurement_reflns_used 3570 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 26.0 _exptl_crystal_description needle-like _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.778 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 386 _exptl_absorpt_coefficient_mu 1.504 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.914 _exptl_absorpt_correction_T_max 0.926 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 218(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3570 _diffrn_reflns_av_R_equivalents 0.0140 _diffrn_reflns_av_sigmaI/netI 0.0147 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.99 _reflns_number_total 1386 _reflns_number_gt 1338 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART Bruker AXS Inc., 1998.' _computing_cell_refinement 'SAINT+ Ver. 6.22, Bruker AXS Inc., 2001.' _computing_data_reduction 'SAINT+ Ver. 6.22, Bruker AXS Inc., 2001.' _computing_structure_solution 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _computing_molecular_graphics 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _computing_publication_material 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0471P)^2^+0.4079P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1386 _refine_ls_number_parameters 106 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0274 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0757 _refine_ls_wR_factor_gt 0.0751 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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 Co1 Co 1.0000 0.5000 0.5000 0.02327(14) Uani 1 2 d S . . S1 S 0.54294(12) 0.55761(3) 0.38499(3) 0.02519(15) Uani 1 1 d . . . N1 N 0.9380(4) 0.38386(10) 0.41057(11) 0.0222(3) Uani 1 1 d . . . C8 C 0.6026(5) 0.47692(13) 0.28843(14) 0.0231(4) Uani 1 1 d . . . C7 C 0.4641(5) 0.48864(14) 0.18872(16) 0.0293(4) Uani 1 1 d . . . H7 H 0.3478 0.5426 0.1708 0.035 Uiso 1 1 calc R . . C9 C 0.7839(4) 0.39398(12) 0.31311(13) 0.0219(4) Uani 1 1 d . . . C5 C 0.6567(5) 0.33945(15) 0.13847(15) 0.0323(4) Uani 1 1 d . . . H5 H 0.6706 0.2945 0.0886 0.039 Uiso 1 1 calc R . . C4 C 0.8017(5) 0.32377(13) 0.23923(14) 0.0263(4) Uani 1 1 d . . . C1 C 1.0807(5) 0.30429(13) 0.43615(15) 0.0263(4) Uani 1 1 d . . . H1 H 1.1797 0.2971 0.5025 0.032 Uiso 1 1 calc R . . C2 C 1.0906(5) 0.23038(13) 0.36873(16) 0.0308(4) Uani 1 1 d . . . H2 H 1.1852 0.1750 0.3910 0.037 Uiso 1 1 calc R . . C6 C 0.4966(5) 0.42046(16) 0.11454(15) 0.0337(5) Uani 1 1 d . . . H6 H 0.4072 0.4307 0.0477 0.040 Uiso 1 1 calc R . . C3 C 0.9598(5) 0.24068(13) 0.26990(17) 0.0305(4) Uani 1 1 d . . . H3 H 0.9749 0.1932 0.2232 0.037 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 Co1 0.0279(2) 0.0177(2) 0.0235(2) -0.00287(12) -0.00680(15) 0.00301(12) S1 0.0272(3) 0.0207(2) 0.0275(3) -0.00018(16) -0.00058(18) 0.00116(16) N1 0.0208(7) 0.0213(7) 0.0244(7) 0.0015(6) 0.0011(6) -0.0003(6) C8 0.0205(8) 0.0254(9) 0.0237(9) 0.0011(7) 0.0028(6) -0.0019(7) C7 0.0250(9) 0.0337(10) 0.0289(10) 0.0067(8) -0.0010(8) -0.0024(7) C9 0.0191(8) 0.0234(8) 0.0235(8) 0.0000(7) 0.0024(6) -0.0040(6) C5 0.0292(9) 0.0403(11) 0.0275(9) -0.0093(8) 0.0039(7) -0.0100(8) C4 0.0205(8) 0.0292(9) 0.0295(9) -0.0056(8) 0.0048(7) -0.0066(7) C1 0.0242(8) 0.0225(9) 0.0321(9) 0.0034(7) 0.0006(7) -0.0011(7) C2 0.0277(9) 0.0197(9) 0.0450(11) -0.0001(8) 0.0033(8) 0.0009(7) C6 0.0284(9) 0.0488(12) 0.0236(9) 0.0025(8) -0.0012(7) -0.0098(9) C3 0.0269(9) 0.0245(9) 0.0406(11) -0.0096(8) 0.0068(8) -0.0039(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 Co1 N1 2.0772(15) . ? Co1 N1 2.0772(15) 3_766 ? Co1 S1 2.3707(5) . ? Co1 S1 2.3707(5) 3_766 ? Co1 S1 2.6881(5) 1_655 ? Co1 S1 2.6881(5) 3_666 ? S1 C8 1.7499(19) . ? S1 Co1 2.6881(5) 1_455 ? N1 C1 1.323(2) . ? N1 C9 1.378(2) . ? C8 C7 1.387(3) . ? C8 C9 1.425(3) . ? C7 C6 1.402(3) . ? C9 C4 1.416(3) . ? C5 C6 1.363(3) . ? C5 C4 1.416(3) . ? C4 C3 1.408(3) . ? C1 C2 1.400(3) . ? C2 C3 1.364(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N1 180.00(8) . 3_766 ? N1 Co1 S1 83.18(4) . . ? N1 Co1 S1 96.82(4) 3_766 . ? N1 Co1 S1 96.82(4) . 3_766 ? N1 Co1 S1 83.18(4) 3_766 3_766 ? S1 Co1 S1 180.0 . 3_766 ? N1 Co1 S1 90.98(4) . 1_655 ? N1 Co1 S1 89.02(4) 3_766 1_655 ? S1 Co1 S1 93.758(16) . 1_655 ? S1 Co1 S1 86.243(16) 3_766 1_655 ? N1 Co1 S1 89.02(4) . 3_666 ? N1 Co1 S1 90.98(4) 3_766 3_666 ? S1 Co1 S1 86.242(16) . 3_666 ? S1 Co1 S1 93.757(16) 3_766 3_666 ? S1 Co1 S1 180.0 1_655 3_666 ? C8 S1 Co1 95.90(6) . . ? C8 S1 Co1 107.62(6) . 1_455 ? Co1 S1 Co1 93.758(16) . 1_455 ? C1 N1 C9 118.30(16) . . ? C1 N1 Co1 123.73(12) . . ? C9 N1 Co1 117.30(12) . . ? C7 C8 C9 118.11(17) . . ? C7 C8 S1 122.31(15) . . ? C9 C8 S1 119.51(14) . . ? C8 C7 C6 121.08(19) . . ? N1 C9 C4 121.13(16) . . ? N1 C9 C8 118.33(16) . . ? C4 C9 C8 120.54(16) . . ? C6 C5 C4 120.00(18) . . ? C3 C4 C9 118.25(17) . . ? C3 C4 C5 122.85(18) . . ? C9 C4 C5 118.89(18) . . ? N1 C1 C2 123.51(18) . . ? C3 C2 C1 119.13(18) . . ? C5 C6 C7 121.25(19) . . ? C2 C3 C4 119.46(18) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.495 _refine_diff_density_min -0.225 _refine_diff_density_rms 0.065 #=================================================END data_1@245K _database_code_depnum_ccdc_archive 'CCDC 799880' #TrackingRef '- CoMQ.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common CoMQ _chemical_melting_point ? _chemical_formula_moiety 'C18 H12 Co N2 S2' _chemical_formula_sum 'C18 H12 Co N2 S2' _chemical_formula_weight 379.35 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' Co Co 0.3494 0.9721 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(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 3.7060(4) _cell_length_b 14.7577(14) _cell_length_c 13.0266(13) _cell_angle_alpha 90.00 _cell_angle_beta 92.2066(15) _cell_angle_gamma 90.00 _cell_volume 711.92(12) _cell_formula_units_Z 2 _cell_measurement_temperature 245(2) _cell_measurement_reflns_used 3552 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 26.0 _exptl_crystal_description needle-like _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.770 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 386 _exptl_absorpt_coefficient_mu 1.497 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.914 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 245(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3552 _diffrn_reflns_av_R_equivalents 0.0128 _diffrn_reflns_av_sigmaI/netI 0.0142 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.98 _reflns_number_total 1385 _reflns_number_gt 1332 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART Bruker AXS Inc., 1998.' _computing_cell_refinement 'SAINT+ Ver. 6.22, Bruker AXS Inc., 2001.' _computing_data_reduction 'SAINT+ Ver. 6.22, Bruker AXS Inc., 2001.' _computing_structure_solution 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _computing_molecular_graphics 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _computing_publication_material 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+0.3193P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1385 _refine_ls_number_parameters 106 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0274 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0760 _refine_ls_wR_factor_gt 0.0755 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _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 Co1 Co 0.5000 0.5000 0.0000 0.02600(14) Uani 1 2 d S . . S1 S 0.95686(12) 0.44250(3) 0.11521(3) 0.02744(15) Uani 1 1 d . . . N1 N 0.5626(4) 0.61632(10) 0.08951(11) 0.0240(3) Uani 1 1 d . . . C8 C 0.8968(5) 0.52325(13) 0.21146(14) 0.0251(4) Uani 1 1 d . . . C9 C 0.7165(4) 0.60614(12) 0.18691(13) 0.0241(3) Uani 1 1 d . . . C5 C 0.8432(5) 0.66053(15) 0.36136(15) 0.0353(4) Uani 1 1 d . . . H5 H 0.8288 0.7054 0.4112 0.042 Uiso 1 1 calc R . . C4 C 0.6989(5) 0.67629(13) 0.26066(14) 0.0288(4) Uani 1 1 d . . . C1 C 0.4197(5) 0.69581(12) 0.06412(15) 0.0287(4) Uani 1 1 d . . . H1 H 0.3204 0.7030 -0.0020 0.034 Uiso 1 1 calc R . . C7 C 1.0351(5) 0.51164(14) 0.31114(16) 0.0324(4) Uani 1 1 d . . . H7 H 1.1512 0.4577 0.3291 0.039 Uiso 1 1 calc R . . C2 C 0.4099(5) 0.76965(13) 0.13133(16) 0.0337(4) Uani 1 1 d . . . H2 H 0.3156 0.8250 0.1091 0.040 Uiso 1 1 calc R . . C3 C 0.5407(5) 0.75929(13) 0.23006(17) 0.0341(4) Uani 1 1 d . . . H3 H 0.5255 0.8067 0.2768 0.041 Uiso 1 1 calc R . . C6 C 1.0027(5) 0.57984(17) 0.38514(15) 0.0374(5) Uani 1 1 d . . . H6 H 1.0921 0.5697 0.4518 0.045 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 Co1 0.0311(2) 0.0200(2) 0.0262(2) -0.00341(12) -0.00774(15) 0.00356(12) S1 0.0290(2) 0.0230(2) 0.0301(3) -0.00023(16) -0.00123(18) 0.00129(16) N1 0.0226(7) 0.0225(7) 0.0270(7) 0.0012(6) 0.0008(6) -0.0005(6) C8 0.0219(8) 0.0275(8) 0.0260(9) 0.0012(7) 0.0025(6) -0.0026(7) C9 0.0206(7) 0.0257(8) 0.0261(8) -0.0007(7) 0.0026(6) -0.0046(6) C5 0.0314(9) 0.0451(12) 0.0296(9) -0.0103(8) 0.0030(7) -0.0099(8) C4 0.0224(8) 0.0323(9) 0.0320(9) -0.0065(8) 0.0049(7) -0.0069(7) C1 0.0264(8) 0.0254(9) 0.0343(9) 0.0032(7) 0.0000(7) -0.0005(7) C7 0.0272(9) 0.0382(11) 0.0315(10) 0.0069(8) -0.0011(8) -0.0035(7) C2 0.0303(9) 0.0216(9) 0.0493(12) -0.0013(8) 0.0032(8) 0.0011(7) C3 0.0306(9) 0.0276(9) 0.0446(11) -0.0115(8) 0.0077(8) -0.0044(7) C6 0.0319(9) 0.0543(13) 0.0258(9) 0.0016(8) -0.0017(7) -0.0112(9) _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 Co1 N1 2.0831(15) 3_665 ? Co1 N1 2.0831(15) . ? Co1 S1 2.3756(5) . ? Co1 S1 2.3756(5) 3_665 ? Co1 S1 2.6939(5) 1_455 ? Co1 S1 2.6939(5) 3_765 ? S1 C8 1.7501(19) . ? S1 Co1 2.6939(5) 1_655 ? N1 C1 1.324(2) . ? N1 C9 1.379(2) . ? C8 C7 1.388(3) . ? C8 C9 1.424(3) . ? C9 C4 1.416(2) . ? C5 C6 1.360(3) . ? C5 C4 1.417(3) . ? C4 C3 1.409(3) . ? C1 C2 1.399(3) . ? C7 C6 1.402(3) . ? C2 C3 1.366(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N1 180.00(8) 3_665 . ? N1 Co1 S1 96.93(4) 3_665 . ? N1 Co1 S1 83.07(4) . . ? N1 Co1 S1 83.07(4) 3_665 3_665 ? N1 Co1 S1 96.93(4) . 3_665 ? S1 Co1 S1 180.0 . 3_665 ? N1 Co1 S1 89.02(4) 3_665 1_455 ? N1 Co1 S1 90.98(4) . 1_455 ? S1 Co1 S1 93.735(16) . 1_455 ? S1 Co1 S1 86.265(16) 3_665 1_455 ? N1 Co1 S1 90.98(4) 3_665 3_765 ? N1 Co1 S1 89.02(4) . 3_765 ? S1 Co1 S1 86.265(16) . 3_765 ? S1 Co1 S1 93.735(16) 3_665 3_765 ? S1 Co1 S1 180.000(17) 1_455 3_765 ? C8 S1 Co1 95.86(6) . . ? C8 S1 Co1 107.64(6) . 1_655 ? Co1 S1 Co1 93.735(16) . 1_655 ? C1 N1 C9 118.28(15) . . ? C1 N1 Co1 123.75(12) . . ? C9 N1 Co1 117.28(11) . . ? C7 C8 C9 117.98(17) . . ? C7 C8 S1 122.24(15) . . ? C9 C8 S1 119.70(13) . . ? N1 C9 C4 121.10(16) . . ? N1 C9 C8 118.29(15) . . ? C4 C9 C8 120.61(16) . . ? C6 C5 C4 120.00(18) . . ? C3 C4 C9 118.25(17) . . ? C3 C4 C5 122.88(18) . . ? C9 C4 C5 118.87(18) . . ? N1 C1 C2 123.61(17) . . ? C8 C7 C6 121.08(19) . . ? C3 C2 C1 119.04(18) . . ? C2 C3 C4 119.51(17) . . ? C5 C6 C7 121.33(18) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.462 _refine_diff_density_min -0.212 _refine_diff_density_rms 0.064 #=================================================END data_1@272K _database_code_depnum_ccdc_archive 'CCDC 799881' #TrackingRef '- CoMQ.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common CoMQ _chemical_melting_point ? _chemical_formula_moiety 'C18 H12 Co N2 S2' _chemical_formula_sum 'C18 H12 Co N2 S2' _chemical_formula_weight 379.35 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' Co Co 0.3494 0.9721 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(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 3.7109(4) _cell_length_b 14.7647(14) _cell_length_c 13.0315(13) _cell_angle_alpha 90.00 _cell_angle_beta 92.1943(15) _cell_angle_gamma 90.00 _cell_volume 713.48(12) _cell_formula_units_Z 2 _cell_measurement_temperature 272(2) _cell_measurement_reflns_used 3853 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 26.0 _exptl_crystal_description needle-like _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.766 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 386 _exptl_absorpt_coefficient_mu 1.493 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.914 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 272(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3583 _diffrn_reflns_av_R_equivalents 0.0137 _diffrn_reflns_av_sigmaI/netI 0.0146 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.98 _reflns_number_total 1384 _reflns_number_gt 1320 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART Bruker AXS Inc., 1998.' _computing_cell_refinement 'SAINT+ Ver. 6.22, Bruker AXS Inc., 2001.' _computing_data_reduction 'SAINT+ Ver. 6.22, Bruker AXS Inc., 2001.' _computing_structure_solution 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _computing_molecular_graphics 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _computing_publication_material 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0610P)^2^+0.2135P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1384 _refine_ls_number_parameters 106 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0287 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0851 _refine_ls_wR_factor_gt 0.0836 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 Co1 Co 1.0000 0.5000 0.5000 0.02871(16) Uani 1 2 d S . . S1 S 0.54385(12) 0.55744(3) 0.38466(3) 0.02962(17) Uani 1 1 d . . . N1 N 0.9375(4) 0.38361(10) 0.41047(11) 0.0256(3) Uani 1 1 d . . . C4 C 0.8010(5) 0.32367(13) 0.23951(14) 0.0314(4) Uani 1 1 d . . . C8 C 0.6034(5) 0.47664(13) 0.28857(14) 0.0276(4) Uani 1 1 d . . . C1 C 1.0799(5) 0.30409(13) 0.43570(15) 0.0310(4) Uani 1 1 d . . . H1 H 1.1794 0.2969 0.5018 0.037 Uiso 1 1 calc R . . C9 C 0.7836(4) 0.39385(12) 0.31315(13) 0.0258(4) Uani 1 1 d . . . C5 C 0.6565(5) 0.33940(15) 0.13887(15) 0.0385(5) Uani 1 1 d . . . H5 H 0.6704 0.2945 0.0891 0.046 Uiso 1 1 calc R . . C3 C 0.9585(5) 0.24076(13) 0.26996(17) 0.0370(4) Uani 1 1 d . . . H3 H 0.9734 0.1934 0.2232 0.044 Uiso 1 1 calc R . . C7 C 0.4658(6) 0.48807(15) 0.18907(16) 0.0351(4) Uani 1 1 d . . . H7 H 0.3501 0.5420 0.1711 0.042 Uiso 1 1 calc R . . C6 C 0.4974(5) 0.42018(18) 0.11506(14) 0.0406(5) Uani 1 1 d . . . H6 H 0.4081 0.4304 0.0484 0.049 Uiso 1 1 calc R . . C2 C 1.0892(5) 0.23034(13) 0.36860(16) 0.0370(4) Uani 1 1 d . . . H2 H 1.1829 0.1750 0.3908 0.044 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 Co1 0.0349(2) 0.0219(2) 0.0286(2) -0.00382(11) -0.00868(16) 0.00433(12) S1 0.0311(3) 0.0249(3) 0.0326(3) -0.00014(16) -0.00145(19) 0.00153(16) N1 0.0249(7) 0.0241(7) 0.0279(7) 0.0009(6) -0.0002(6) -0.0012(6) C4 0.0246(8) 0.0354(9) 0.0344(9) -0.0075(8) 0.0051(7) -0.0082(7) C8 0.0245(8) 0.0304(9) 0.0279(9) 0.0014(8) 0.0026(6) -0.0031(7) C1 0.0294(8) 0.0261(9) 0.0375(9) 0.0030(7) 0.0003(7) -0.0008(7) C9 0.0222(7) 0.0273(9) 0.0282(8) -0.0011(7) 0.0028(6) -0.0053(6) C5 0.0351(9) 0.0497(12) 0.0307(9) -0.0114(9) 0.0033(7) -0.0114(9) C3 0.0334(10) 0.0297(10) 0.0484(11) -0.0125(8) 0.0082(8) -0.0045(8) C7 0.0307(10) 0.0414(11) 0.0330(10) 0.0081(8) -0.0017(8) -0.0036(8) C6 0.0359(10) 0.0589(13) 0.0267(9) 0.0015(9) -0.0027(7) -0.0119(9) C2 0.0336(9) 0.0235(9) 0.0539(12) -0.0020(8) 0.0032(8) 0.0011(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 Co1 N1 2.0850(15) . ? Co1 N1 2.0850(15) 3_766 ? Co1 S1 2.3768(5) . ? Co1 S1 2.3768(5) 3_766 ? Co1 S1 2.6989(5) 1_655 ? Co1 S1 2.6989(5) 3_666 ? S1 C8 1.7497(19) . ? S1 Co1 2.6989(5) 1_455 ? N1 C1 1.324(2) . ? N1 C9 1.379(2) . ? C4 C3 1.407(3) . ? C4 C9 1.415(3) . ? C4 C5 1.417(3) . ? C8 C7 1.385(3) . ? C8 C9 1.424(3) . ? C1 C2 1.398(3) . ? C5 C6 1.361(4) . ? C3 C2 1.365(3) . ? C7 C6 1.399(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N1 180.00(8) . 3_766 ? N1 Co1 S1 83.05(4) . . ? N1 Co1 S1 96.95(4) 3_766 . ? N1 Co1 S1 96.95(4) . 3_766 ? N1 Co1 S1 83.05(4) 3_766 3_766 ? S1 Co1 S1 180.0 . 3_766 ? N1 Co1 S1 90.97(4) . 1_655 ? N1 Co1 S1 89.03(4) 3_766 1_655 ? S1 Co1 S1 93.745(16) . 1_655 ? S1 Co1 S1 86.255(16) 3_766 1_655 ? N1 Co1 S1 89.03(4) . 3_666 ? N1 Co1 S1 90.97(4) 3_766 3_666 ? S1 Co1 S1 86.255(16) . 3_666 ? S1 Co1 S1 93.745(16) 3_766 3_666 ? S1 Co1 S1 180.0 1_655 3_666 ? C8 S1 Co1 95.91(6) . . ? C8 S1 Co1 107.57(6) . 1_455 ? Co1 S1 Co1 93.745(16) . 1_455 ? C1 N1 C9 118.23(15) . . ? C1 N1 Co1 123.86(12) . . ? C9 N1 Co1 117.22(11) . . ? C3 C4 C9 118.36(18) . . ? C3 C4 C5 122.82(18) . . ? C9 C4 C5 118.82(18) . . ? C7 C8 C9 117.92(18) . . ? C7 C8 S1 122.32(16) . . ? C9 C8 S1 119.69(13) . . ? N1 C1 C2 123.69(17) . . ? N1 C9 C4 121.00(16) . . ? N1 C9 C8 118.39(15) . . ? C4 C9 C8 120.60(16) . . ? C6 C5 C4 120.01(18) . . ? C2 C3 C4 119.49(18) . . ? C8 C7 C6 121.4(2) . . ? C5 C6 C7 121.17(19) . . ? C3 C2 C1 119.01(18) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.645 _refine_diff_density_min -0.177 _refine_diff_density_rms 0.066 #=================================================END