data_global #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; 'Zhang, Xian-Ming' School of Chemistry & Material Science Shanxi Normal University Linfen 041004 Shanxi Province P. R. China ; _publ_contact_author_phone '86-357-2051402' _publ_contact_author_fax '86-357-2051402' _publ_contact_author_email zhangxm@dns.sxtu.edu.cn _publ_requested_joiurnal 'J. Am. Chem. Soc.' _publ_requested_coeditor_name ? _publ_contact_letter ; Dear Sir or Madam: Please consider this CIF as a supplmentary data for a manuscript submitted to J. Am. Chem. Soc. Xian-Ming Zhang ; #================================================================= # 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_name_full ? _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 ; ? ; loop_ _publ_author_name _publ_author_address 'Zhang, Xian-Ming' ; School of Chemistry & Material Science Shanxi Normal University Linfen 041004 Shanxi Province P. R. China ; 'Fang, Rui-Qin' ; School of Chemistry & Material Science Shanxi Normal University Linfen 041004 Shanxi Province P. R. China ; 'Wu, Hai-Shun' ; School of Chemistry & Material Science Shanxi Normal University Linfen 041004 Shanxi Province P. R. China ; #====================================== data_a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H8 Cu3 N3 S2' _chemical_formula_weight 436.94 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I-42m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x, -y, -z' '-x, y, -z' 'y, x, z' '-y, -x, z' '-y, x, -z' 'y, -x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' '-y+1/2, x+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' _cell_length_a 10.2175(8) _cell_length_b 10.217 _cell_length_c 15.4618(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1614.17(19) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 62 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 26 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.798 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 4.162 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4612 _exptl_absorpt_correction_T_max 0.5052 _exptl_absorpt_process_details ? _exptl_special_details ; The C1 and N1 atoms from cyanide occupy same sites. ; _diffrn_ambient_temperature 295(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 'Bruker Apex CCD Diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 4365 _diffrn_reflns_av_R_equivalents 0.0255 _diffrn_reflns_av_sigmaI/netI 0.0268 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 27.47 _reflns_number_total 991 _reflns_number_gt 936 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0570P)^2^+3.5887P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(4) _refine_ls_number_reflns 991 _refine_ls_number_parameters 75 _refine_ls_number_restraints 55 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.0959 _refine_ls_wR_factor_gt 0.0942 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.147 _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 Cu1 Cu 0.5000 0.5000 0.16619(5) 0.0273(3) Uani 1 4 d S . . Cu2 Cu 0.5000 0.24037(6) 0.0000 0.0351(3) Uani 1 2 d S . . S1 S 0.37012(9) 0.37012(9) 0.07959(9) 0.0243(3) Uani 1 2 d S A . N1 N 0.5000 0.0568(6) 0.0000 0.079(3) Uani 0.50 2 d SP . . N2 N 0.1148(4) 0.1148(4) 0.2552(3) 0.0357(13) Uani 1 2 d SD . . C1 C 0.5000 0.0568(6) 0.0000 0.079(3) Uani 0.50 2 d SP . . C2 C 0.2709(4) 0.2709(4) 0.1468(4) 0.0265(12) Uani 1 2 d SDU . . C3 C 0.2768(10) 0.2768(10) 0.2366(7) 0.072(5) Uani 0.50 2 d SPDU A 1 H3 H 0.3342 0.3342 0.2636 0.086 Uiso 0.50 2 calc SPR A 1 C4 C 0.1961(9) 0.1961(9) 0.2855(10) 0.075(6) Uani 0.50 2 d SPDU A 1 H4 H 0.2024 0.2024 0.3454 0.090 Uiso 0.50 2 calc SPR A 1 C5 C 0.1073(11) 0.1073(11) 0.1728(8) 0.073(5) Uani 0.50 2 d SPDU A 1 H5 H 0.0480 0.0480 0.1494 0.088 Uiso 0.50 2 calc SPR A 1 C6 C 0.1812(7) 0.1812(7) 0.1160(9) 0.065(5) Uani 0.50 2 d SPDU A 1 H6 H 0.1705 0.1705 0.0567 0.078 Uiso 0.50 2 calc SPR A 1 C3' C 0.1535(11) 0.3137(13) 0.1756(9) 0.095(5) Uani 0.50 1 d PDU A 2 H3' H 0.1207 0.3955 0.1606 0.114 Uiso 0.50 1 calc PR A 2 C4' C 0.0844(12) 0.2285(11) 0.2290(8) 0.098(5) Uani 0.50 1 d PDU A 2 H4' H 0.0040 0.2595 0.2484 0.118 Uiso 0.50 1 calc PR A 2 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 Cu1 0.0273(3) 0.0273(3) 0.0274(5) 0.000 0.000 0.0025(6) Cu2 0.0347(4) 0.0231(3) 0.0476(5) 0.000 0.0101(5) 0.000 S1 0.0228(4) 0.0228(4) 0.0273(7) 0.0047(4) 0.0047(4) -0.0045(5) N1 0.061(4) 0.027(3) 0.151(8) 0.000 0.002(9) 0.000 N2 0.0351(19) 0.0351(19) 0.037(3) 0.0101(16) 0.0101(16) -0.008(3) C1 0.061(4) 0.027(3) 0.151(8) 0.000 0.002(9) 0.000 C2 0.0252(17) 0.0252(17) 0.029(3) 0.0053(15) 0.0053(15) -0.006(2) C3 0.082(7) 0.082(7) 0.052(8) -0.012(5) -0.012(5) -0.030(8) C4 0.087(7) 0.087(7) 0.051(8) 0.015(5) 0.015(5) -0.025(8) C5 0.082(6) 0.082(6) 0.055(8) 0.004(5) 0.004(5) -0.043(8) C6 0.078(6) 0.078(6) 0.040(7) -0.004(4) -0.004(4) -0.044(7) C3' 0.094(9) 0.072(8) 0.120(9) 0.049(7) 0.065(7) 0.019(7) C4' 0.079(8) 0.078(8) 0.138(10) 0.041(8) 0.073(7) 0.028(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 Cu1 N2 2.056(5) 12 ? Cu1 N2 2.056(5) 11 ? Cu1 S1 2.3055(15) . ? Cu1 S1 2.3055(15) 2_665 ? Cu2 N1 1.876(6) . ? Cu2 S1 2.2434(8) . ? Cu2 S1 2.2434(8) 4_655 ? S1 C2 1.771(5) . ? S1 Cu2 2.2434(8) 5 ? N1 C1 1.160(12) 2_655 ? N1 N1 1.160(12) 2_655 ? N2 C4 1.264(12) . ? N2 C4' 1.268(11) . ? N2 C4' 1.268(11) 5 ? N2 C5 1.279(12) . ? N2 Cu1 2.056(5) 11_455 ? C2 C3' 1.352(9) . ? C2 C3' 1.352(9) 5 ? C2 C6 1.380(9) . ? C2 C3 1.391(10) . ? C3 C4 1.390(10) . ? C5 C6 1.383(10) . ? C3' C4' 1.392(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu1 N2 107.5(3) 12 11 ? N2 Cu1 S1 110.08(8) 12 . ? N2 Cu1 S1 110.08(8) 11 . ? N2 Cu1 S1 110.08(8) 12 2_665 ? N2 Cu1 S1 110.08(8) 11 2_665 ? S1 Cu1 S1 108.98(8) . 2_665 ? N1 Cu2 S1 126.22(4) . . ? N1 Cu2 S1 126.22(4) . 4_655 ? S1 Cu2 S1 107.55(7) . 4_655 ? C2 S1 Cu2 108.80(9) . 5 ? C2 S1 Cu2 108.80(9) . . ? Cu2 S1 Cu2 113.47(6) 5 . ? C2 S1 Cu1 108.57(19) . . ? Cu2 S1 Cu1 108.56(4) 5 . ? Cu2 S1 Cu1 108.56(4) . . ? C1 N1 N1 0.0 2_655 2_655 ? C1 N1 Cu2 180.0 2_655 . ? N1 N1 Cu2 180.0 2_655 . ? C4 N2 C4' 71.2(8) . . ? C4 N2 C4' 71.2(8) . 5 ? C4' N2 C4' 110.2(11) . 5 ? C4 N2 C5 116.6(11) . . ? C4' N2 C5 73.9(8) . . ? C4' N2 C5 73.9(8) 5 . ? C4 N2 Cu1 122.0(8) . 11_455 ? C4' N2 Cu1 124.8(6) . 11_455 ? C4' N2 Cu1 124.8(6) 5 11_455 ? C5 N2 Cu1 121.4(8) . 11_455 ? C3' C2 C3' 117.7(11) . 5 ? C3' C2 C6 74.9(7) . . ? C3' C2 C6 74.9(7) 5 . ? C3' C2 C3 72.3(7) . . ? C3' C2 C3 72.3(7) 5 . ? C6 C2 C3 113.7(10) . . ? C3' C2 S1 121.1(5) . . ? C3' C2 S1 121.1(5) 5 . ? C6 C2 S1 123.9(7) . . ? C3 C2 S1 122.4(7) . . ? C4 C3 C2 119.5(13) . . ? N2 C4 C3 125.3(14) . . ? N2 C5 C6 124.6(14) . . ? C2 C6 C5 120.4(13) . . ? C2 C3' C4' 116.3(11) . . ? N2 C4' C3' 129.6(11) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.633 _refine_diff_density_min -0.397 _refine_diff_density_rms 0.101