Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Isamu Kinoshita' 'Kiyoshi Isobe' 'Kentaro Kimura' 'Sachiko Kubo' 'Riichi Miyamoto' 'Takanori Nishioka' 'Akio Sakata' 'L. James Wright' 'Toshihiro Yano' _publ_contact_author_name 'Prof Isamu Kinoshita' _publ_contact_author_address ; Department of Material Science Osaka City University 3-3-138 Sugimoto Sumiyoshi-ku Osaka 558-8585 JAPAN ; _publ_contact_author_email 'ISAMU@SCI.OSAKA-CU.AC.JP' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Design and synthesis of copper complexes of novel ligands based on the pyridine thiol group: novel structures and reactions relevant to bioloigical systems. ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan. Single Crystal Structure Analysis Software. Version 1.11. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; #------------------------------------------------------------------------------ data_[CuCl2(DPDS)]n _database_code_CSD 195987 _audit_creation_date 'Wed Oct 16 07:59:36 2002' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C10 H8 Cl2 Cu N2 S2 ' _chemical_formula_moiety 'C10 H8 Cl2 Cu N2 S2 ' _chemical_formula_weight 354.76 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P 31 ' _symmetry_Int_Tables_number 144 loop_ _symmetry_equiv_pos_as_xyz x,y,z -y,x-y,1/3+z -x+y,-x,2/3+z _cell_length_a 8.3704(9) _cell_length_b 8.3704 _cell_length_c 16.774(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 1017.8(2) _cell_formula_units_Z 3 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 29.1 _cell_measurement_theta_max 30.0 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'hexagonal' _exptl_crystal_colour 'purple' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.736 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 8.586 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.446 _exptl_absorpt_correction_T_max 0.999 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Cu K$B%((Ja' _diffrn_radiation_wavelength 1.5418 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method $B%((Jw-2$B%((Jq _diffrn_reflns_number 2352 _diffrn_reflns_av_R_equivalents 0.018 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 59.88 _diffrn_reflns_limit_h_min 12 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.09 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2016 _reflns_number_gt 2003 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0857 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 2016 _refine_ls_number_parameters 186 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[$B%((Js^2^(Fo^2^) + (0.0492P)^2^+1.2506P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0000 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^$B%((Jl^3^/sin(2$B%((Jq)]^-1/4^' _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack 0.09(3) _refine_diff_density_max 0.31 _refine_diff_density_min -0.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cu' 'Cu' -1.965 0.589 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Cl' 'Cl' 0.364 0.702 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'C' 'C' 0.018 0.009 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'N' 'N' 0.031 0.018 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'S' 'S' 0.333 0.557 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu(1) Cu -0.1856(1) 0.23207(9) -0.31088(4) 0.0367(2) Uani 1.00 d . . . Cl(1) Cl -0.4004(2) 0.2280(2) -0.22885(9) 0.0568(4) Uani 1.00 d . . . Cl(2) Cl 0.0372(2) 0.2335(2) -0.38607(8) 0.0531(3) Uani 1.00 d . . . S(1) S 0.1141(2) 0.4847(2) -0.19263(8) 0.0479(3) Uani 1.00 d . . . S(2) S -0.0328(2) 0.5021(2) -0.10008(8) 0.0569(4) Uani 1.00 d . . . N(1) N -0.0568(6) 0.5059(5) -0.3209(2) 0.0402(10) Uani 1.00 d . . . N(2) N 0.0447(5) 0.7189(6) 0.0202(2) 0.0367(9) Uani 1.00 d . . . C(1) C 0.0688(7) 0.6081(7) -0.2677(3) 0.045(1) Uani 1.00 d . . . C(2) C 0.1676(10) 0.7994(9) -0.2700(5) 0.063(2) Uani 1.00 d . . . C(3) C 0.126(1) 0.8844(10) -0.3312(6) 0.070(2) Uani 1.00 d . . . C(4) C -0.001(1) 0.781(1) -0.3860(5) 0.069(2) Uani 1.00 d . . . C(5) C -0.0927(10) 0.5907(9) -0.3805(4) 0.054(1) Uani 1.00 d . . . C(6) C 0.1283(7) 0.6865(7) -0.0399(3) 0.042(1) Uani 1.00 d . . . C(7) C 0.3203(7) 0.7834(9) -0.0467(4) 0.054(1) Uani 1.00 d . . . C(8) C 0.4182(9) 0.9115(9) 0.0087(4) 0.054(2) Uani 1.00 d . . . C(9) C 0.3319(8) 0.9434(9) 0.0720(4) 0.053(1) Uani 1.00 d . . . C(10) C 0.1437(7) 0.8417(8) 0.0753(3) 0.047(1) Uani 1.00 d . . . H(1) H 0.262(9) 0.871(9) -0.237(4) 0.0565(2) Uiso 1.00 calc . . . H(2) H 0.17(1) 0.99(1) -0.355(6) 0.1105(4) Uiso 1.00 calc . . . H(3) H -0.028(10) 0.82(1) -0.430(5) 0.0729(3) Uiso 1.00 calc . . . H(4) H -0.175(7) 0.522(7) -0.410(3) 0.0234(2) Uiso 1.00 calc . . . H(5) H 0.37(1) 0.75(1) -0.096(4) 0.0805(3) Uiso 1.00 calc . . . H(6) H 0.508(9) 0.966(8) 0.007(3) 0.0317(2) Uiso 1.00 calc . . . H(7) H 0.393(9) 1.020(8) 0.104(4) 0.0458(2) Uiso 1.00 calc . . . H(8) H 0.08(1) 0.86(1) 0.133(6) 0.1142(4) Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu(1) 0.0435(4) 0.0311(4) 0.0305(3) 0.0148(3) 0.0006(3) -0.0029(3) Cl(1) 0.0547(8) 0.0456(7) 0.0591(8) 0.0168(6) 0.0162(7) -0.0106(6) Cl(2) 0.0564(8) 0.0469(7) 0.0545(8) 0.0246(6) 0.0169(6) 0.0018(6) S(1) 0.0517(7) 0.0567(8) 0.0399(7) 0.0305(7) 0.0026(6) -0.0072(6) S(2) 0.0358(7) 0.0718(9) 0.0466(7) 0.0145(7) 0.0019(6) -0.0230(7) N(1) 0.046(2) 0.035(2) 0.040(2) 0.021(2) 0.006(2) 0.001(2) N(2) 0.032(2) 0.044(2) 0.033(2) 0.018(2) 0.001(2) 0.003(2) C(1) 0.046(3) 0.038(3) 0.049(3) 0.020(2) 0.005(2) -0.004(2) C(2) 0.061(4) 0.039(3) 0.080(5) 0.017(3) -0.003(3) -0.009(3) C(3) 0.069(4) 0.042(3) 0.096(6) 0.024(3) 0.012(4) 0.012(4) C(4) 0.078(5) 0.064(4) 0.076(5) 0.045(4) 0.018(4) 0.026(4) C(5) 0.063(4) 0.050(3) 0.050(3) 0.029(3) 0.001(3) 0.005(3) C(6) 0.040(3) 0.051(3) 0.032(2) 0.021(2) -0.002(2) 0.000(2) C(7) 0.028(3) 0.066(4) 0.058(4) 0.017(3) 0.003(3) -0.007(3) C(8) 0.027(3) 0.063(4) 0.061(4) 0.013(3) -0.005(3) 0.003(3) C(9) 0.048(3) 0.051(3) 0.055(4) 0.020(3) -0.018(3) -0.013(3) C(10) 0.042(3) 0.057(3) 0.036(3) 0.022(3) -0.004(2) -0.004(2) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL97' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu(1) Cl(1) 2.250(2) . . yes Cu(1) Cl(2) 2.246(2) . . yes Cu(1) N(1) 1.993(4) . . yes Cu(1) N(2) 2.007(4) . 3_454 yes S(1) S(2) 2.031(2) . . yes S(1) C(1) 1.786(7) . . yes S(2) C(6) 1.771(5) . . yes N(1) C(1) 1.316(6) . . yes N(1) C(5) 1.344(9) . . yes N(2) C(6) 1.331(8) . . yes N(2) C(10) 1.321(6) . . yes C(1) C(2) 1.388(8) . . yes C(2) C(3) 1.39(1) . . yes C(2) H(1) 0.904 . . no C(3) C(4) 1.35(1) . . yes C(3) H(2) 0.883 . . no C(4) C(5) 1.380(10) . . yes C(4) H(3) 0.899 . . no C(5) H(4) 0.804 . . no C(6) C(7) 1.396(7) . . yes C(7) C(8) 1.343(9) . . yes C(7) H(5) 0.984 . . no C(8) C(9) 1.38(1) . . yes C(8) H(6) 0.655 . . no C(9) C(10) 1.367(8) . . yes C(9) H(7) 0.798 . . no C(10) H(8) 1.167 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Cu(1) Cl(2) 176.43(7) . . . yes Cl(1) Cu(1) N(1) 92.1(2) . . . yes Cl(1) Cu(1) N(2) 89.6(1) . . 3_454 yes Cl(2) Cu(1) N(1) 88.6(1) . . . yes Cl(2) Cu(1) N(2) 90.0(1) . . 3_454 yes N(1) Cu(1) N(2) 173.7(2) . . 3_454 yes S(2) S(1) C(1) 100.7(2) . . . yes S(1) S(2) C(6) 105.9(2) . . . yes Cu(1) N(1) C(1) 119.2(4) . . . yes Cu(1) N(1) C(5) 122.3(3) . . . yes C(1) N(1) C(5) 118.5(5) . . . yes Cu(1) N(2) C(6) 118.2(3) 2_565 . . yes Cu(1) N(2) C(10) 121.8(4) 2_565 . . yes C(6) N(2) C(10) 120.0(4) . . . yes S(1) C(1) N(1) 115.7(4) . . . yes S(1) C(1) C(2) 120.7(5) . . . yes N(1) C(1) C(2) 123.5(6) . . . yes C(1) C(2) C(3) 117.1(6) . . . yes C(1) C(2) H(1) 124.3 . . . no C(3) C(2) H(1) 118.4 . . . no C(2) C(3) C(4) 119.6(7) . . . yes C(2) C(3) H(2) 141.2 . . . no C(4) C(3) H(2) 98.0 . . . no C(3) C(4) C(5) 120.2(8) . . . yes C(3) C(4) H(3) 125.4 . . . no C(5) C(4) H(3) 114.3 . . . no N(1) C(5) C(4) 121.0(6) . . . yes N(1) C(5) H(4) 114.6 . . . no C(4) C(5) H(4) 124.2 . . . no S(2) C(6) N(2) 111.2(3) . . . yes S(2) C(6) C(7) 127.9(5) . . . yes N(2) C(6) C(7) 120.8(5) . . . yes C(6) C(7) C(8) 118.3(6) . . . yes C(6) C(7) H(5) 113.5 . . . no C(8) C(7) H(5) 128.0 . . . no C(7) C(8) C(9) 121.0(6) . . . yes C(7) C(8) H(6) 123.4 . . . no C(9) C(8) H(6) 115.5 . . . no C(8) C(9) C(10) 117.5(5) . . . yes C(8) C(9) H(7) 119.3 . . . no C(10) C(9) H(7) 123.2 . . . no N(2) C(10) C(9) 122.4(6) . . . yes N(2) C(10) H(8) 122.6 . . . no C(9) C(10) H(8) 114.8 . . . no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cu(1) N(1) C(1) S(1) 1.7(6) . . . . yes Cu(1) N(1) C(1) C(2) 179.2(6) . . . . yes Cu(1) N(1) C(5) C(4) -179.8(6) . . . . yes Cl(1) Cu(1) N(1) C(1) 86.7(5) . . . . yes Cl(1) Cu(1) N(1) C(5) -93.7(5) . . . . yes Cl(2) Cu(1) N(1) C(1) -89.8(5) . . . . yes Cl(2) Cu(1) N(1) C(5) 89.7(5) . . . . yes S(1) S(2) C(6) N(2) 175.8(4) . . . . yes S(1) S(2) C(6) C(7) -8.7(7) . . . . yes S(1) C(1) N(1) C(5) -177.8(5) . . . . yes S(1) C(1) C(2) C(3) 178.7(6) . . . . yes S(2) S(1) C(1) N(1) -100.9(5) . . . . yes S(2) S(1) C(1) C(2) 81.5(6) . . . . yes S(2) C(6) N(2) C(10) 174.6(5) . . . . yes S(2) C(6) C(7) C(8) -175.7(6) . . . . yes N(1) C(1) C(2) C(3) 1(1) . . . . yes N(1) C(5) C(4) C(3) 0(1) . . . . yes N(2) C(6) C(7) C(8) 0(1) . . . . yes N(2) C(10) C(9) C(8) 0(1) . . . . yes C(1) S(1) S(2) C(6) -98.3(3) . . . . yes C(1) N(1) C(5) C(4) 0(1) . . . . yes C(1) C(2) C(3) C(4) -1(1) . . . . yes C(2) C(1) N(1) C(5) 0(1) . . . . yes C(2) C(3) C(4) C(5) 1(1) . . . . yes C(6) N(2) C(10) C(9) 2(1) . . . . yes C(6) C(7) C(8) C(9) 1(1) . . . . yes C(7) C(6) N(2) C(10) -1.3(9) . . . . yes C(7) C(8) C(9) C(10) 0(1) . . . . yes C(7) C(8) C(9) C(10) 0(1) . . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(2) C(3) 3.48(1) . 1_545 ? Cl(2) C(10) 3.555(5) . 2_664 ? S(2) C(3) 3.454(9) . 2_665 ? C(1) C(7) 3.581(10) . 3_564 ? C(2) C(6) 3.48(1) . 3_564 ? C(4) C(9) 3.57(1) . 3_464 ? C(4) C(10) 3.60(1) . 3_464 ? C(5) C(9) 3.49(1) . 3_464 ? C(5) C(8) 3.55(1) . 3_464 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #===END #------------------------------------------------------------------------------ data_[Cu(DPDS)Cl2] _database_code_CSD 195988 _audit_creation_date 'Wed Oct 16 07:44:48 2002' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C10 H8 Cl2 Cu N2 S2 ' _chemical_formula_moiety 'C10 H8 Cl2 Cu N2 S2 ' _chemical_formula_weight 354.76 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 7.530(1) _cell_length_b 8.2269(9) _cell_length_c 11.618(1) _cell_angle_alpha 87.87(1) _cell_angle_beta 73.02(1) _cell_angle_gamma 71.86(1) _cell_volume 653.0(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.8 _cell_measurement_theta_max 15.0 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.450 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.804 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 2.376 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.714 _exptl_absorpt_correction_T_max 0.998 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K$B%((Ja' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method $B%((Jw-2$B%((Jq _diffrn_reflns_number 4059 _diffrn_reflns_av_R_equivalents 0.007 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 30.00 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.69 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3812 _reflns_number_gt 3310 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0244 _refine_ls_wR_factor_ref 0.0631 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 3812 _refine_ls_number_parameters 186 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[$B%((Js^2^(Fo^2^) + (0.0284P)^2^+0.2622P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max -0.0010 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^$B%((Jl^3^/sin(2$B%((Jq)]^-1/4^' _refine_diff_density_max 0.31 _refine_diff_density_min -0.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cu' 'Cu' 0.320 1.265 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu(1) Cu 0.59305(3) -0.92683(3) -0.14845(2) 0.02631(6) Uani 1.00 d . . . Cl(1) Cl 0.91258(6) -1.05395(6) -0.17480(4) 0.03372(9) Uani 1.00 d . . . Cl(2) Cl 0.53618(6) -0.81320(5) 0.04514(4) 0.03170(9) Uani 1.00 d . . . S(1) S 0.64369(9) -0.68845(7) -0.42301(5) 0.0469(1) Uani 1.00 d . . . S(2) S 0.57382(7) -0.60272(6) -0.24830(5) 0.0400(1) Uani 1.00 d . . . N(1) N 0.6489(2) -1.0020(2) -0.3302(1) 0.0308(3) Uani 1.00 d . . . N(2) N 0.3275(2) -0.7697(2) -0.1488(1) 0.0273(3) Uani 1.00 d . . . C(1) C 0.6931(3) -0.9139(3) -0.4271(2) 0.0337(4) Uani 1.00 d . . . C(2) C 0.7740(4) -0.9904(3) -0.5436(2) 0.0487(5) Uani 1.00 d . . . C(3) C 0.8075(4) -1.1621(4) -0.5601(2) 0.0540(6) Uani 1.00 d . . . C(4) C 0.7590(4) -1.2542(3) -0.4610(2) 0.0497(5) Uani 1.00 d . . . C(5) C 0.6823(3) -1.1710(3) -0.3488(2) 0.0405(4) Uani 1.00 d . . . C(6) C 0.3327(3) -0.6168(2) -0.1920(2) 0.0317(3) Uani 1.00 d . . . C(7) C 0.1681(3) -0.4841(3) -0.1925(2) 0.0404(4) Uani 1.00 d . . . C(8) C -0.0123(3) -0.5114(3) -0.1474(2) 0.0414(4) Uani 1.00 d . . . C(9) C -0.0190(3) -0.6682(3) -0.1053(2) 0.0364(4) Uani 1.00 d . . . C(10) C 0.1532(3) -0.7955(2) -0.1064(2) 0.0310(3) Uani 1.00 d . . . H(1) H 0.805(4) -0.928(4) -0.601(3) 0.0700(1) Uiso 1.00 calc . . . H(2) H 0.864(4) -1.221(4) -0.636(3) 0.0657(1) Uiso 1.00 calc . . . H(3) H 0.777(4) -1.369(4) -0.469(2) 0.0631(1) Uiso 1.00 calc . . . H(4) H 0.652(4) -1.225(3) -0.282(2) 0.05300(9) Uiso 1.00 calc . . . H(5) H 0.176(3) -0.377(3) -0.218(2) 0.04909(8) Uiso 1.00 calc . . . H(6) H -0.122(4) -0.425(3) -0.145(2) 0.04747(8) Uiso 1.00 calc . . . H(7) H -0.130(3) -0.692(3) -0.078(2) 0.03741(7) Uiso 1.00 calc . . . H(8) H 0.153(3) -0.905(3) -0.079(2) 0.03276(7) Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu(1) 0.0250(1) 0.0259(1) 0.0238(1) -0.00364(7) -0.00576(7) 0.00189(7) Cl(1) 0.0259(2) 0.0346(2) 0.0336(2) -0.0033(2) -0.0049(2) 0.0015(2) Cl(2) 0.0323(2) 0.0330(2) 0.0271(2) -0.0095(2) -0.0053(2) -0.0005(2) S(1) 0.0530(3) 0.0395(3) 0.0410(3) -0.0155(2) -0.0036(2) 0.0148(2) S(2) 0.0368(2) 0.0328(2) 0.0509(3) -0.0152(2) -0.0094(2) 0.0043(2) N(1) 0.0341(7) 0.0319(7) 0.0244(6) -0.0099(6) -0.0062(5) 0.0023(6) N(2) 0.0277(6) 0.0254(6) 0.0273(6) -0.0061(5) -0.0087(5) 0.0030(5) C(1) 0.0307(8) 0.0395(9) 0.0280(8) -0.0111(7) -0.0047(6) 0.0052(7) C(2) 0.054(1) 0.059(1) 0.0267(9) -0.018(1) -0.0017(8) 0.0058(9) C(3) 0.060(1) 0.064(2) 0.0294(10) -0.014(1) -0.0041(9) -0.0109(10) C(4) 0.064(1) 0.043(1) 0.040(1) -0.017(1) -0.0100(10) -0.0080(9) C(5) 0.053(1) 0.0359(10) 0.0312(9) -0.0151(9) -0.0084(8) 0.0011(8) C(6) 0.0308(8) 0.0266(8) 0.0345(8) -0.0065(7) -0.0077(7) 0.0014(7) C(7) 0.0399(10) 0.0254(8) 0.048(1) -0.0011(7) -0.0115(8) 0.0037(8) C(8) 0.0329(9) 0.0360(10) 0.046(1) 0.0044(8) -0.0133(8) -0.0039(8) C(9) 0.0270(8) 0.046(1) 0.0339(9) -0.0086(8) -0.0077(7) -0.0029(8) C(10) 0.0311(8) 0.0343(9) 0.0280(8) -0.0104(7) -0.0094(6) 0.0033(7) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL97' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu(1) Cl(1) 2.2368(6) . . yes Cu(1) Cl(2) 2.3368(5) . . yes Cu(1) Cl(2) 2.7175(5) . 2_635 yes Cu(1) N(1) 2.106(2) . . yes Cu(1) N(2) 2.016(1) . . yes S(1) S(2) 2.0362(8) . . yes S(1) C(1) 1.774(2) . . yes S(2) C(6) 1.781(2) . . yes N(1) C(1) 1.332(2) . . yes N(1) C(5) 1.348(3) . . yes N(2) C(6) 1.344(2) . . yes N(2) C(10) 1.341(3) . . yes C(1) C(2) 1.393(3) . . yes C(2) C(3) 1.366(4) . . yes C(2) H(1) 0.845 . . no C(3) C(4) 1.377(3) . . yes C(3) H(2) 0.932 . . no C(4) C(5) 1.372(3) . . yes C(4) H(3) 0.913 . . no C(5) H(4) 0.886 . . no C(6) C(7) 1.374(3) . . yes C(7) C(8) 1.391(3) . . yes C(7) H(5) 0.937 . . no C(8) C(9) 1.373(3) . . yes C(8) H(6) 0.902 . . no C(9) C(10) 1.387(3) . . yes C(9) H(7) 0.882 . . no C(10) H(8) 0.947 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Cu(1) Cl(2) 93.69(2) . . . yes Cl(1) Cu(1) Cl(2) 98.04(2) . . 2_635 yes Cl(1) Cu(1) N(1) 86.68(4) . . . yes Cl(1) Cu(1) N(2) 166.29(5) . . . yes Cl(2) Cu(1) Cl(2) 88.26(2) . . 2_635 yes Cl(2) Cu(1) N(1) 173.31(5) . . . yes Cl(2) Cu(1) N(2) 88.82(4) . . . yes Cl(2) Cu(1) N(1) 98.31(5) 2_635 . . yes Cl(2) Cu(1) N(2) 95.51(5) 2_635 . . yes N(1) Cu(1) N(2) 89.28(6) . . . yes Cu(1) Cl(2) Cu(1) 91.74(2) . . 2_635 yes S(2) S(1) C(1) 108.19(7) . . . yes S(1) S(2) C(6) 100.40(7) . . . yes Cu(1) N(1) C(1) 128.0(1) . . . yes Cu(1) N(1) C(5) 113.3(1) . . . yes C(1) N(1) C(5) 117.2(2) . . . yes Cu(1) N(2) C(6) 112.8(1) . . . yes Cu(1) N(2) C(10) 128.7(1) . . . yes C(6) N(2) C(10) 118.4(1) . . . yes S(1) C(1) N(1) 124.1(1) . . . yes S(1) C(1) C(2) 113.2(2) . . . yes N(1) C(1) C(2) 122.6(2) . . . yes C(1) C(2) C(3) 119.1(2) . . . yes C(1) C(2) H(1) 117.6 . . . no C(3) C(2) H(1) 123.1 . . . no C(2) C(3) C(4) 118.9(2) . . . yes C(2) C(3) H(2) 122.9 . . . no C(4) C(3) H(2) 118.2 . . . no C(3) C(4) C(5) 118.8(2) . . . yes C(3) C(4) H(3) 121.3 . . . no C(5) C(4) H(3) 119.9 . . . no N(1) C(5) C(4) 123.3(2) . . . yes N(1) C(5) H(4) 114.1 . . . no C(4) C(5) H(4) 122.6 . . . no S(2) C(6) N(2) 113.4(1) . . . yes S(2) C(6) C(7) 123.2(2) . . . yes N(2) C(6) C(7) 123.4(2) . . . yes C(6) C(7) C(8) 117.9(2) . . . yes C(6) C(7) H(5) 121.2 . . . no C(8) C(7) H(5) 120.8 . . . no C(7) C(8) C(9) 119.2(2) . . . yes C(7) C(8) H(6) 119.3 . . . no C(9) C(8) H(6) 121.5 . . . no C(8) C(9) C(10) 119.6(2) . . . yes C(8) C(9) H(7) 122.4 . . . no C(10) C(9) H(7) 117.9 . . . no N(2) C(10) C(9) 121.5(2) . . . yes N(2) C(10) H(8) 117.0 . . . no C(9) C(10) H(8) 121.6 . . . no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cu(1) Cl(2) Cu(1) Cl(1) -93.48(2) . . 2_635 2_635 yes Cu(1) Cl(2) Cu(1) Cl(2) 0.0000(1) . . 2_635 2_635 yes Cu(1) Cl(2) Cu(1) N(1) 178.73(4) . . 2_635 2_635 yes Cu(1) Cl(2) Cu(1) N(2) 88.65(4) . . 2_635 2_635 yes Cu(1) Cl(2) Cu(1) Cl(1) 97.94(2) . 2_635 2_635 2_635 yes Cu(1) Cl(2) Cu(1) Cl(2) 0.0000(2) . 2_635 2_635 . yes Cu(1) Cl(2) Cu(1) N(1) -169.1(4) . 2_635 2_635 2_635 yes Cu(1) Cl(2) Cu(1) N(2) -95.55(5) . 2_635 2_635 2_635 yes Cu(1) N(1) C(1) S(1) -20.1(3) . . . . yes Cu(1) N(1) C(1) C(2) 163.6(2) . . . . yes Cu(1) N(1) C(5) C(4) -166.7(2) . . . . yes Cu(1) N(2) C(6) S(2) 5.0(2) . . . . yes Cu(1) N(2) C(6) C(7) -174.9(2) . . . . yes Cu(1) N(2) C(10) C(9) 175.0(1) . . . . yes Cl(1) Cu(1) N(1) C(1) -91.7(2) . . . . yes Cl(1) Cu(1) N(1) C(5) 73.6(1) . . . . yes Cl(1) Cu(1) N(2) C(6) -11.3(3) . . . . yes Cl(1) Cu(1) N(2) C(10) 172.8(1) . . . . yes Cl(2) Cu(1) Cl(2) Cu(1) 0.0000(1) . . 2_635 2_635 yes Cl(2) Cu(1) N(1) C(1) 1.6(5) . . . . yes Cl(2) Cu(1) N(1) C(5) 166.9(3) . . . . yes Cl(2) Cu(1) N(2) C(6) 89.5(1) . . . . yes Cl(2) Cu(1) N(2) C(10) -86.4(2) . . . . yes Cl(2) Cu(1) Cl(2) Cu(1) 0.0000(1) . 2_635 2_635 . yes Cl(2) Cu(1) N(1) C(1) -170.7(2) . 2_635 2_635 2_635 yes Cl(2) Cu(1) N(1) C(5) 24.1(2) . 2_635 2_635 2_635 yes Cl(2) Cu(1) N(2) C(6) -177.6(1) . 2_635 2_635 2_635 yes Cl(2) Cu(1) N(2) C(10) -1.7(2) . 2_635 2_635 2_635 yes S(1) S(2) C(6) N(2) 89.3(1) . . . . yes S(1) S(2) C(6) C(7) -90.7(2) . . . . yes S(1) C(1) N(1) C(5) 175.2(2) . . . . yes S(1) C(1) C(2) C(3) -175.9(2) . . . . yes S(2) S(1) C(1) N(1) 13.4(2) . . . . yes S(2) S(1) C(1) C(2) -169.9(2) . . . . yes S(2) C(6) N(2) C(10) -178.6(1) . . . . yes S(2) C(6) C(7) C(8) 179.2(2) . . . . yes N(1) Cu(1) N(2) C(6) -84.1(1) . . . . yes N(1) Cu(1) N(2) C(10) 100.0(2) . . . . yes N(1) C(1) C(2) C(3) 0.9(4) . . . . yes N(1) C(5) C(4) C(3) 1.0(4) . . . . yes N(2) Cu(1) N(1) C(1) 75.2(2) . . . . yes N(2) Cu(1) N(1) C(5) -119.5(2) . . . . yes N(2) C(6) C(7) C(8) -0.9(3) . . . . yes N(2) C(10) C(9) C(8) -0.6(3) . . . . yes C(1) S(1) S(2) C(6) -74.83(10) . . . . yes C(1) N(1) C(5) C(4) 0.3(4) . . . . yes C(1) C(2) C(3) C(4) 0.5(4) . . . . yes C(2) C(1) N(1) C(5) -1.2(3) . . . . yes C(2) C(3) C(4) C(5) -1.4(4) . . . . yes C(6) N(2) C(10) C(9) -0.7(3) . . . . yes C(6) C(7) C(8) C(9) -0.4(3) . . . . yes C(7) C(6) N(2) C(10) 1.5(3) . . . . yes C(7) C(8) C(9) C(10) 1.1(3) . . . . yes C(7) C(8) C(9) C(10) 1.1(3) . . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cu(1) Cl(2) 2.7175(5) . 2_635 ? Cl(1) C(10) 3.435(2) . 1_655 ? Cl(1) C(7) 3.442(2) . 1_645 ? Cl(1) C(2) 3.514(2) . 2_734 ? Cl(1) C(9) 3.527(3) . 1_655 ? C(7) C(9) 3.461(3) . 2_545 ? C(8) C(9) 3.436(3) . 2_545 ? C(8) C(8) 3.499(5) . 2_545 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #===END data_[Cu(DPDS)Br2] _database_code_CSD 195989 _audit_creation_date 'Wed Oct 16 07:36:04 2002' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C10 H8 Br2 Cu N2 S2 ' _chemical_formula_moiety 'C10 H8 Br2 Cu N2 S2 ' _chemical_formula_weight 443.66 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 13.241(2) _cell_length_b 7.499(1) _cell_length_c 14.093(1) _cell_angle_alpha 90 _cell_angle_beta 102.203(9) _cell_angle_gamma 90 _cell_volume 1367.7(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.6 _cell_measurement_theta_max 15.0 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.450 _exptl_crystal_size_mid 0.360 _exptl_crystal_size_min 0.150 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 2.155 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 7.740 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.386 _exptl_absorpt_correction_T_max 0.998 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K$B%((Ja' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method $B%((Jw-2$B%((Jq _diffrn_reflns_number 2233 _diffrn_reflns_av_R_equivalents 0.018 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 29.99 _diffrn_reflns_limit_h_min 12 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.04 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2004 _reflns_number_gt 1555 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0700 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 2004 _refine_ls_number_parameters 94 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[$B%((Js^2^(Fo^2^) + (0.0371P)^2^+0.2668P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max -0.0010 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^$B%((Jl^3^/sin(2$B%((Jq)]^-1/4^' _refine_diff_density_max 0.34 _refine_diff_density_min -0.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cu' 'Cu' 0.320 1.265 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Br' 'Br' -0.290 2.459 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br(1) Br 0.64786(2) 0.37971(4) 0.20101(2) 0.0494(1) Uani 1.00 d . . . Cu(1) Cu 0.5000 0.26540(6) 0.2500 0.0347(1) Uani 1.00 d S . . S(1) S 0.42165(5) -0.12993(9) 0.22186(5) 0.0413(2) Uani 1.00 d . . . N(1) N 0.4297(2) 0.1766(3) 0.1212(2) 0.0350(4) Uani 1.00 d . . . C(1) C 0.4046(2) 0.0031(3) 0.1152(2) 0.0336(5) Uani 1.00 d . . . C(2) C 0.3578(2) -0.0755(4) 0.0275(2) 0.0421(6) Uani 1.00 d . . . C(3) C 0.3348(2) 0.0290(5) -0.0547(2) 0.0478(7) Uani 1.00 d . . . C(4) C 0.3598(2) 0.2072(5) -0.0481(2) 0.0484(7) Uani 1.00 d . . . C(5) C 0.4088(2) 0.2753(4) 0.0399(2) 0.0425(6) Uani 1.00 d . . . H(1) H 0.336(3) -0.206(5) 0.027(3) 0.0644(1) Uiso 1.00 calc . . . H(2) H 0.304(2) -0.026(4) -0.113(3) 0.0540(1) Uiso 1.00 calc . . . H(3) H 0.345(3) 0.278(5) -0.096(3) 0.0624(1) Uiso 1.00 calc . . . H(4) H 0.434(2) 0.388(4) 0.052(2) 0.0466(1) Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br(1) 0.0446(2) 0.0530(2) 0.0515(2) -0.0111(1) 0.0120(1) 0.0005(1) Cu(1) 0.0364(2) 0.0367(2) 0.0300(2) 0.0000 0.0046(2) 0.0000 S(1) 0.0422(3) 0.0470(4) 0.0324(3) -0.0104(3) 0.0025(3) 0.0058(3) N(1) 0.0339(10) 0.042(1) 0.029(1) -0.0012(9) 0.0067(8) 0.0035(9) C(1) 0.029(1) 0.043(1) 0.028(1) -0.0023(10) 0.0051(9) -0.0002(10) C(2) 0.041(1) 0.048(1) 0.034(1) -0.002(1) 0.002(1) -0.004(1) C(3) 0.048(1) 0.067(2) 0.025(1) 0.007(1) 0.000(1) -0.006(1) C(4) 0.051(2) 0.064(2) 0.031(1) 0.011(1) 0.011(1) 0.009(1) C(5) 0.045(1) 0.048(2) 0.035(1) 0.003(1) 0.009(1) 0.006(1) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL97' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br(1) Cu(1) 2.3698(4) . . yes Cu(1) N(1) 1.973(2) . . yes Cu(1) N(1) 1.973(2) . 2_655 yes S(1) S(1) 2.059(1) . 2_655 yes S(1) C(1) 1.778(3) . . yes N(1) C(1) 1.341(3) . . yes N(1) C(5) 1.343(4) . . yes C(1) C(2) 1.392(3) . . yes C(2) C(3) 1.378(4) . . yes C(2) H(1) 1.022 . . no C(3) C(4) 1.376(5) . . yes C(3) H(2) 0.935 . . no C(4) C(5) 1.371(4) . . yes C(4) H(3) 0.854 . . no C(5) H(4) 0.915 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Br(1) Cu(1) Br(1) 137.59(3) . . 2_655 yes Br(1) Cu(1) N(1) 96.46(7) . . . yes Br(1) Cu(1) N(1) 97.58(7) . . 2_655 yes Br(1) Cu(1) N(1) 97.58(7) 2_655 . . yes Br(1) Cu(1) N(1) 96.46(7) 2_655 . 2_655 yes N(1) Cu(1) N(1) 140.5(1) . . 2_655 yes S(1) S(1) C(1) 105.26(9) 2_655 . . yes Cu(1) N(1) C(1) 116.6(2) . . . yes Cu(1) N(1) C(5) 124.8(2) . . . yes C(1) N(1) C(5) 118.6(2) . . . yes S(1) C(1) N(1) 120.4(2) . . . yes S(1) C(1) C(2) 117.8(2) . . . yes N(1) C(1) C(2) 121.6(2) . . . yes C(1) C(2) C(3) 119.0(3) . . . yes C(1) C(2) H(1) 119.0 . . . no C(3) C(2) H(1) 121.7 . . . no C(2) C(3) C(4) 119.2(3) . . . yes C(2) C(3) H(2) 118.2 . . . no C(4) C(3) H(2) 122.7 . . . no C(3) C(4) C(5) 119.0(3) . . . yes C(3) C(4) H(3) 122.7 . . . no C(5) C(4) H(3) 118.3 . . . no N(1) C(5) C(4) 122.6(3) . . . yes N(1) C(5) H(4) 110.9 . . . no C(4) C(5) H(4) 126.4 . . . no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Br(1) Cu(1) N(1) C(1) 123.6(2) . . . . yes Br(1) Cu(1) N(1) C(5) -54.1(2) . . . . yes Br(1) Cu(1) N(1) C(1) -96.6(2) . . 2_655 2_655 yes Br(1) Cu(1) N(1) C(5) 85.8(2) . . 2_655 2_655 yes Cu(1) N(1) C(1) S(1) 6.9(3) . . . . yes Cu(1) N(1) C(1) C(2) -177.9(2) . . . . yes Cu(1) N(1) C(5) C(4) 179.8(2) . . . . yes Cu(1) N(1) C(1) S(1) 6.9(3) . 2_655 2_655 2_655 yes Cu(1) N(1) C(1) C(2) -177.9(2) . 2_655 2_655 2_655 yes S(1) S(1) C(1) N(1) -63.3(2) . 2_655 2_655 2_655 yes S(1) S(1) C(1) C(2) 121.2(2) . 2_655 2_655 2_655 yes S(1) C(1) N(1) C(5) -175.3(2) . . . . yes S(1) C(1) C(2) C(3) 173.9(2) . . . . yes N(1) Cu(1) N(1) C(1) 13.3(2) . . 2_655 2_655 yes N(1) Cu(1) N(1) C(5) -164.4(2) . . 2_655 2_655 yes N(1) C(1) C(2) C(3) -1.5(4) . . . . yes N(1) C(5) C(4) C(3) -2.8(5) . . . . yes C(1) S(1) S(1) C(1) 108.9(2) . . 2_655 2_655 yes C(1) N(1) C(5) C(4) 2.2(4) . . . . yes C(1) C(2) C(3) C(4) 0.9(4) . . . . yes C(2) C(1) N(1) C(5) 0.0(4) . . . . yes C(2) C(3) C(4) C(5) 1.2(5) . . . . yes C(2) C(3) C(4) C(5) 1.2(5) . . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Br(1) S(1) 3.5754(9) . 5_555 ? S(1) C(4) 3.555(3) . 4_555 ? C(3) C(5) 3.589(4) . 7_555 ? C(4) C(4) 3.518(7) . 7_555 ? C(4) C(5) 3.585(4) . 7_555 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #===END data_[Cu(DPDS)Cl]n _database_code_CSD 195990 _audit_creation_date 'Wed Oct 16 07:27:30 2002' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C10 H8 Cl Cu N2 S2 ' _chemical_formula_moiety 'C10 H8 Cl Cu N2 S2 ' _chemical_formula_weight 319.31 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 7.933(3) _cell_length_b 15.061(2) _cell_length_c 10.383(2) _cell_angle_alpha 90 _cell_angle_beta 112.43(2) _cell_angle_gamma 90 _cell_volume 1146.6(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.6 _cell_measurement_theta_max 14.9 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.850 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 2.470 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.785 _exptl_absorpt_correction_T_max 1.000 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K$B%((Ja' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method $B%((Jw-2$B%((Jq _diffrn_reflns_number 3686 _diffrn_reflns_av_R_equivalents 0.018 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 29.99 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.50 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3338 _reflns_number_gt 2440 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0687 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 3388 _refine_ls_number_parameters 177 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[$B%((Js^2^(Fo^2^) + (0.0216P)^2^+0.5852P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0030 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^$B%((Jl^3^/sin(2$B%((Jq)]^-1/4^' _refine_diff_density_max 0.43 _refine_diff_density_min -0.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cu' 'Cu' 0.320 1.265 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu(1) Cu 0.47956(4) 0.46325(2) 0.36262(3) 0.03712(9) Uani 1.00 d . . . Cl(1) Cl 0.27886(8) 0.44607(4) 0.48155(6) 0.0361(1) Uani 1.00 d . . . S(1) S 0.28538(9) 0.65206(4) 0.31993(6) 0.0355(1) Uani 1.00 d . . . S(2) S 0.19920(8) 0.77912(4) 0.26471(8) 0.0383(1) Uani 1.00 d . . . N(1) N 0.3409(3) 0.5235(1) 0.1723(2) 0.0301(4) Uani 1.00 d . . . N(2) N -0.1220(2) 0.8522(1) 0.1604(2) 0.0265(4) Uani 1.00 d . . . C(1) C 0.2475(3) 0.6000(2) 0.1578(2) 0.0291(5) Uani 1.00 d . . . C(2) C 0.1312(4) 0.6316(2) 0.0293(3) 0.0434(6) Uani 1.00 d . . . C(3) C 0.1122(4) 0.5837(2) -0.0885(3) 0.0475(7) Uani 1.00 d . . . C(4) C 0.2117(4) 0.5078(2) -0.0763(3) 0.0464(7) Uani 1.00 d . . . C(5) C 0.3224(4) 0.4795(2) 0.0545(3) 0.0386(6) Uani 1.00 d . . . C(6) C -0.0405(3) 0.7767(1) 0.2222(2) 0.0282(4) Uani 1.00 d . . . C(7) C -0.1332(4) 0.7063(2) 0.2493(3) 0.0402(6) Uani 1.00 d . . . C(8) C -0.3205(4) 0.7110(2) 0.2027(3) 0.0453(6) Uani 1.00 d . . . C(9) C -0.4086(3) 0.7859(2) 0.1326(3) 0.0394(6) Uani 1.00 d . . . C(10) C -0.3051(3) 0.8554(2) 0.1160(3) 0.0325(5) Uani 1.00 d . . . H(1) H 0.065(4) 0.681(2) 0.023(3) 0.0562(1) Uiso 1.00 calc . . . H(2) H 0.034(4) 0.602(2) -0.175(3) 0.0645(1) Uiso 1.00 calc . . . H(3) H 0.205(4) 0.479(2) -0.154(3) 0.0573(1) Uiso 1.00 calc . . . H(4) H 0.393(4) 0.424(2) 0.068(3) 0.0504(1) Uiso 1.00 calc . . . H(5) H -0.068(4) 0.656(2) 0.298(3) 0.04390(10) Uiso 1.00 calc . . . H(6) H -0.384(4) 0.666(2) 0.221(3) 0.0485(1) Uiso 1.00 calc . . . H(7) H -0.528(4) 0.795(2) 0.104(3) 0.0494(1) Uiso 1.00 calc . . . H(8) H -0.359(3) 0.907(2) 0.073(2) 0.03232(8) Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu(1) 0.0349(2) 0.0324(2) 0.0397(2) 0.0038(1) 0.0093(1) -0.0002(1) Cl(1) 0.0314(3) 0.0316(3) 0.0459(3) -0.0087(2) 0.0154(2) -0.0079(2) S(1) 0.0389(3) 0.0300(3) 0.0333(3) 0.0122(2) 0.0088(3) 0.0037(2) S(2) 0.0250(3) 0.0244(3) 0.0604(4) 0.0015(2) 0.0104(3) 0.0033(3) N(1) 0.0311(10) 0.0265(9) 0.0325(10) 0.0008(8) 0.0118(8) 0.0030(8) N(2) 0.0261(9) 0.0219(8) 0.0312(9) 0.0016(7) 0.0104(8) -0.0011(7) C(1) 0.024(1) 0.031(1) 0.032(1) 0.0032(9) 0.0108(9) 0.0063(9) C(2) 0.042(1) 0.051(2) 0.036(1) 0.018(1) 0.013(1) 0.012(1) C(3) 0.045(2) 0.065(2) 0.030(1) 0.008(1) 0.011(1) 0.009(1) C(4) 0.055(2) 0.051(2) 0.035(1) -0.001(1) 0.019(1) -0.002(1) C(5) 0.048(2) 0.030(1) 0.040(1) 0.001(1) 0.019(1) 0.001(1) C(6) 0.027(1) 0.0225(10) 0.034(1) -0.0006(8) 0.0103(9) -0.0021(8) C(7) 0.036(1) 0.027(1) 0.057(2) 0.0007(10) 0.016(1) 0.006(1) C(8) 0.038(1) 0.035(1) 0.070(2) -0.007(1) 0.028(1) 0.004(1) C(9) 0.026(1) 0.041(1) 0.053(2) 0.000(1) 0.016(1) -0.001(1) C(10) 0.030(1) 0.029(1) 0.040(1) 0.0039(9) 0.015(1) 0.0017(10) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL97' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu(1) Cl(1) 2.3721(9) . . yes Cu(1) Cl(1) 2.4061(7) . 3_666 yes Cu(1) N(1) 2.069(2) . . yes Cu(1) N(2) 2.082(2) . 2_545 yes S(1) S(2) 2.0394(8) . . yes S(1) C(1) 1.776(3) . . yes S(2) C(6) 1.781(2) . . yes N(1) C(1) 1.347(3) . . yes N(1) C(5) 1.349(3) . . yes N(2) C(6) 1.344(3) . . yes N(2) C(10) 1.347(3) . . yes C(1) C(2) 1.385(3) . . yes C(2) C(3) 1.378(4) . . yes C(2) H(1) 0.896 . . no C(3) C(4) 1.367(5) . . yes C(3) H(2) 0.913 . . no C(4) C(5) 1.374(4) . . yes C(4) H(3) 0.901 . . no C(5) H(4) 0.991 . . no C(6) C(7) 1.379(4) . . yes C(7) C(8) 1.378(4) . . yes C(7) H(5) 0.947 . . no C(8) C(9) 1.380(4) . . yes C(8) H(6) 0.902 . . no C(9) C(10) 1.381(4) . . yes C(9) H(7) 0.888 . . no C(10) H(8) 0.916 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Cu(1) Cl(1) 103.44(3) . . 3_666 yes Cl(1) Cu(1) N(1) 109.10(7) . . . yes Cl(1) Cu(1) N(2) 118.26(6) . . 2_545 yes Cl(1) Cu(1) N(1) 112.96(5) 3_666 . . yes Cl(1) Cu(1) N(2) 101.83(5) 3_666 . 2_545 yes N(1) Cu(1) N(2) 110.90(8) . . 2_545 yes Cu(1) Cl(1) Cu(1) 76.56(3) . . 3_666 yes S(2) S(1) C(1) 103.30(8) . . . yes S(1) S(2) C(6) 105.21(8) . . . yes Cu(1) N(1) C(1) 123.5(2) . . . yes Cu(1) N(1) C(5) 119.0(1) . . . yes C(1) N(1) C(5) 117.0(2) . . . yes Cu(1) N(2) C(6) 123.5(1) 2_555 . . yes Cu(1) N(2) C(10) 119.6(1) 2_555 . . yes C(6) N(2) C(10) 116.9(2) . . . yes S(1) C(1) N(1) 112.6(1) . . . yes S(1) C(1) C(2) 124.8(2) . . . yes N(1) C(1) C(2) 122.5(2) . . . yes C(1) C(2) C(3) 118.8(3) . . . yes C(1) C(2) H(1) 121.0 . . . no C(3) C(2) H(1) 120.1 . . . no C(2) C(3) C(4) 119.5(2) . . . yes C(2) C(3) H(2) 121.1 . . . no C(4) C(3) H(2) 119.4 . . . no C(3) C(4) C(5) 118.7(3) . . . yes C(3) C(4) H(3) 118.8 . . . no C(5) C(4) H(3) 122.6 . . . no N(1) C(5) C(4) 123.4(3) . . . yes N(1) C(5) H(4) 115.7 . . . no C(4) C(5) H(4) 120.9 . . . no S(2) C(6) N(2) 112.0(2) . . . yes S(2) C(6) C(7) 124.5(2) . . . yes N(2) C(6) C(7) 123.5(2) . . . yes C(6) C(7) C(8) 118.4(2) . . . yes C(6) C(7) H(5) 119.9 . . . no C(8) C(7) H(5) 121.6 . . . no C(7) C(8) C(9) 119.2(3) . . . yes C(7) C(8) H(6) 119.9 . . . no C(9) C(8) H(6) 120.9 . . . no C(8) C(9) C(10) 118.7(2) . . . yes C(8) C(9) H(7) 124.6 . . . no C(10) C(9) H(7) 116.4 . . . no N(2) C(10) C(9) 123.0(2) . . . yes N(2) C(10) H(8) 116.2 . . . no C(9) C(10) H(8) 120.8 . . . no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cu(1) Cl(1) Cu(1) Cl(1) 0.0000(1) . . 3_666 3_666 yes Cu(1) Cl(1) Cu(1) N(1) -117.82(7) . . 3_666 3_666 yes Cu(1) Cl(1) Cu(1) Cl(1) 0.0000(1) . 3_666 3_666 . yes Cu(1) Cl(1) Cu(1) N(1) 120.48(6) . 3_666 3_666 3_666 yes Cu(1) N(1) C(1) S(1) 9.2(3) . . . . yes Cu(1) N(1) C(1) C(2) -168.9(2) . . . . yes Cu(1) N(1) C(5) C(4) 170.4(2) . . . . yes Cl(1) Cu(1) Cl(1) Cu(1) 0.0 . . 3_666 3_666 yes Cl(1) Cu(1) N(1) C(1) 52.6(2) . . . . yes Cl(1) Cu(1) N(1) C(5) -118.7(2) . . . . yes Cl(1) Cu(1) Cl(1) Cu(1) 0.0000(1) . 3_666 3_666 . yes S(1) S(2) C(6) N(2) -169.1(1) . . . . yes S(1) S(2) C(6) C(7) 11.1(3) . . . . yes S(1) C(1) N(1) C(5) -179.3(2) . . . . yes S(1) C(1) C(2) C(3) -178.9(2) . . . . yes S(2) S(1) C(1) N(1) 162.5(2) . . . . yes S(2) S(1) C(1) C(2) -19.4(3) . . . . yes S(2) C(6) N(2) C(10) 176.0(2) . . . . yes S(2) C(6) C(7) C(8) -175.9(2) . . . . yes N(1) C(1) C(2) C(3) -1.1(4) . . . . yes N(1) C(5) C(4) C(3) -1.2(5) . . . . yes N(2) C(6) C(7) C(8) 4.3(4) . . . . yes N(2) C(10) C(9) C(8) 2.8(5) . . . . yes C(1) S(1) S(2) C(6) 85.0(1) . . . . yes C(1) N(1) C(5) C(4) -1.4(4) . . . . yes C(1) C(2) C(3) C(4) -1.7(5) . . . . yes C(2) C(1) N(1) C(5) 2.6(4) . . . . yes C(2) C(3) C(4) C(5) 2.8(5) . . . . yes C(6) N(2) C(10) C(9) 0.5(4) . . . . yes C(6) C(7) C(8) C(9) -0.8(5) . . . . yes C(7) C(6) N(2) C(10) -4.1(4) . . . . yes C(7) C(8) C(9) C(10) -2.5(5) . . . . yes C(7) C(8) C(9) C(10) -2.5(5) . . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(1) C(10) 3.470(3) . 4_565 ? Cl(1) N(2) 3.490(2) . 4_565 ? S(1) N(2) 3.325(2) . 4_565 ? S(1) C(10) 3.415(3) . 4_565 ? S(2) C(5) 3.592(3) . 2_555 ? N(2) C(5) 3.566(3) . 2_555 ? C(3) C(9) 3.451(4) . 4_564 ? C(3) C(10) 3.495(4) . 4_564 ? C(5) C(5) 3.470(7) . 3_665 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #===END data_[CuBr(PPT)]n _database_code_CSD 195991 _audit_creation_date 'Wed Oct 16 07:20:54 2002' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C10 H8 Br Cu N2 S ' _chemical_formula_moiety 'C10 H8 Br Cu N2 S ' _chemical_formula_weight 331.70 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 7.655(1) _cell_length_b 8.821(1) _cell_length_c 9.4081(9) _cell_angle_alpha 72.237(9) _cell_angle_beta 72.262(9) _cell_angle_gamma 67.494(10) _cell_volume 546.0(1) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.7 _cell_measurement_theta_max 15.0 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 2.018 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 5.825 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.732 _exptl_absorpt_correction_T_max 1.000 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K$B%((Ja' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method $B%((Jw-2$B%((Jq _diffrn_reflns_number 3374 _diffrn_reflns_av_R_equivalents 0.007 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 30.00 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 3.02 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3184 _reflns_number_gt 2587 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0737 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 3184 _refine_ls_number_parameters 168 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[$B%((Js^2^(Fo^2^) + (0.0316P)^2^+0.5423P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max -0.0010 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^$B%((Jl^3^/sin(2$B%((Jq)]^-1/4^' _refine_diff_density_max 0.86 _refine_diff_density_min -1.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cu' 'Cu' 0.320 1.265 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Br' 'Br' -0.290 2.459 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br(1) Br 0.72356(4) -0.90397(4) -0.45496(3) 0.03620(9) Uani 1.00 d . . . Cu(1) Cu 0.99401(5) -0.98416(5) -0.32842(4) 0.0397(1) Uani 1.00 d . . . S(1) S 1.0154(1) -0.83529(9) 0.09830(8) 0.0329(1) Uani 1.00 d . . . N(1) N 1.0450(3) -0.7672(3) -0.3176(3) 0.0313(4) Uani 1.00 d . . . N(2) N 0.7887(3) -0.7253(3) -0.1029(2) 0.0297(4) Uani 1.00 d . . . C(1) C 0.9449(4) -0.6730(3) -0.2146(3) 0.0301(5) Uani 1.00 d . . . C(2) C 0.9753(5) -0.5303(4) -0.2105(4) 0.0404(6) Uani 1.00 d . . . C(3) C 1.1237(5) -0.4830(4) -0.3201(4) 0.0439(7) Uani 1.00 d . . . C(4) C 1.2343(4) -0.5808(4) -0.4239(4) 0.0410(7) Uani 1.00 d . . . C(5) C 1.1914(4) -0.7197(4) -0.4211(3) 0.0379(6) Uani 1.00 d . . . C(6) C 0.8070(4) -0.7992(3) 0.0455(3) 0.0279(5) Uani 1.00 d . . . C(7) C 0.6456(4) -0.8450(4) 0.1447(3) 0.0373(6) Uani 1.00 d . . . C(8) C 0.4876(4) -0.8228(5) 0.0944(4) 0.0444(7) Uani 1.00 d . . . C(9) C 0.4791(5) -0.7507(5) -0.0588(4) 0.0501(8) Uani 1.00 d . . . C(10) C 0.6307(5) -0.7041(4) -0.1543(3) 0.0419(7) Uani 1.00 d . . . H(1) H 0.892(5) -0.469(4) -0.131(4) 0.0458(1) Uiso 1.00 calc . . . H(2) H 1.144(6) -0.380(5) -0.320(5) 0.0604(1) Uiso 1.00 calc . . . H(3) H 1.343(6) -0.553(5) -0.497(4) 0.0556(1) Uiso 1.00 calc . . . H(4) H 1.267(5) -0.785(4) -0.496(4) 0.0413(1) Uiso 1.00 calc . . . H(5) H 0.657(5) -0.892(4) 0.239(4) 0.0363(1) Uiso 1.00 calc . . . H(6) H 0.388(6) -0.855(5) 0.166(4) 0.0553(1) Uiso 1.00 calc . . . H(7) H 0.375(6) -0.730(5) -0.097(4) 0.0582(1) Uiso 1.00 calc . . . H(8) H 0.633(5) -0.656(4) -0.259(4) 0.0427(1) Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br(1) 0.0298(1) 0.0487(2) 0.0321(1) -0.0132(1) -0.0060(1) -0.0111(1) Cu(1) 0.0412(2) 0.0444(2) 0.0358(2) -0.0191(2) -0.0113(2) -0.0015(2) S(1) 0.0322(3) 0.0408(4) 0.0301(3) -0.0198(3) -0.0089(3) -0.0006(3) N(1) 0.032(1) 0.034(1) 0.029(1) -0.0157(9) -0.0024(9) -0.0046(9) N(2) 0.029(1) 0.035(1) 0.0242(10) -0.0138(9) -0.0042(8) -0.0028(9) C(1) 0.031(1) 0.031(1) 0.027(1) -0.013(1) -0.0060(10) -0.0011(10) C(2) 0.049(2) 0.033(1) 0.040(2) -0.017(1) -0.005(1) -0.009(1) C(3) 0.056(2) 0.035(2) 0.046(2) -0.026(1) -0.010(1) -0.002(1) C(4) 0.036(1) 0.043(2) 0.042(2) -0.023(1) -0.005(1) 0.003(1) C(5) 0.036(1) 0.041(2) 0.035(1) -0.018(1) 0.000(1) -0.006(1) C(6) 0.030(1) 0.029(1) 0.026(1) -0.0111(10) -0.0054(9) -0.0053(10) C(7) 0.033(1) 0.049(2) 0.029(1) -0.019(1) -0.005(1) -0.001(1) C(8) 0.031(1) 0.064(2) 0.038(2) -0.024(1) -0.003(1) -0.002(1) C(9) 0.034(1) 0.080(3) 0.040(2) -0.027(2) -0.011(1) -0.005(2) C(10) 0.039(1) 0.059(2) 0.030(1) -0.021(1) -0.011(1) -0.002(1) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL97' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br(1) Cu(1) 2.4638(6) . . yes Br(1) Cu(1) 2.5904(4) . 2_734 yes Cu(1) S(1) 2.2622(7) . 2_735 yes Cu(1) N(1) 2.131(3) . . yes S(1) C(6) 1.700(3) . . yes N(1) C(1) 1.330(4) . . yes N(1) C(5) 1.350(4) . . yes N(2) C(1) 1.452(3) . . yes N(2) C(6) 1.374(3) . . yes N(2) C(10) 1.364(5) . . yes C(1) C(2) 1.377(5) . . yes C(2) C(3) 1.384(5) . . yes C(2) H(1) 0.973 . . no C(3) C(4) 1.366(5) . . yes C(3) H(2) 0.980 . . no C(4) C(5) 1.376(6) . . yes C(4) H(3) 0.961 . . no C(5) H(4) 0.954 . . no C(6) C(7) 1.418(4) . . yes C(7) C(8) 1.355(5) . . yes C(7) H(5) 0.872 . . no C(8) C(9) 1.397(5) . . yes C(8) H(6) 0.923 . . no C(9) C(10) 1.352(5) . . yes C(9) H(7) 0.907 . . no C(10) H(8) 0.942 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cu(1) Br(1) Cu(1) 81.35(2) . . 2_734 yes Br(1) Cu(1) Br(1) 98.65(2) . . 2_734 yes Br(1) Cu(1) S(1) 117.87(3) . . 2_735 yes Br(1) Cu(1) N(1) 110.82(6) . . . yes Br(1) Cu(1) S(1) 115.02(2) 2_734 . 2_735 yes Br(1) Cu(1) N(1) 102.68(6) 2_734 . . yes S(1) Cu(1) N(1) 110.35(7) 2_735 . . yes Cu(1) S(1) C(6) 106.51(9) 2_735 . . yes Cu(1) N(1) C(1) 125.2(2) . . . yes Cu(1) N(1) C(5) 118.8(2) . . . yes C(1) N(1) C(5) 116.0(3) . . . yes C(1) N(2) C(6) 120.2(3) . . . yes C(1) N(2) C(10) 117.0(2) . . . yes C(6) N(2) C(10) 122.8(2) . . . yes N(1) C(1) N(2) 115.7(3) . . . yes N(1) C(1) C(2) 125.0(3) . . . yes N(2) C(1) C(2) 119.2(2) . . . yes C(1) C(2) C(3) 117.6(3) . . . yes C(1) C(2) H(1) 118.4 . . . no C(3) C(2) H(1) 124.0 . . . no C(2) C(3) C(4) 118.8(4) . . . yes C(2) C(3) H(2) 118.1 . . . no C(4) C(3) H(2) 123.0 . . . no C(3) C(4) C(5) 119.6(3) . . . yes C(3) C(4) H(3) 119.5 . . . no C(5) C(4) H(3) 120.9 . . . no N(1) C(5) C(4) 122.9(3) . . . yes N(1) C(5) H(4) 118.0 . . . no C(4) C(5) H(4) 119.1 . . . no S(1) C(6) N(2) 120.2(2) . . . yes S(1) C(6) C(7) 124.4(2) . . . yes N(2) C(6) C(7) 115.4(3) . . . yes C(6) C(7) C(8) 122.0(3) . . . yes C(6) C(7) H(5) 115.4 . . . no C(8) C(7) H(5) 122.6 . . . no C(7) C(8) C(9) 120.1(3) . . . yes C(7) C(8) H(6) 117.1 . . . no C(9) C(8) H(6) 122.8 . . . no C(8) C(9) C(10) 118.7(4) . . . yes C(8) C(9) H(7) 123.1 . . . no C(10) C(9) H(7) 118.2 . . . no N(2) C(10) C(9) 121.1(3) . . . yes N(2) C(10) H(8) 117.0 . . . no C(9) C(10) H(8) 122.0 . . . no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Br(1) Cu(1) Br(1) Cu(1) 0.0 . . 2_734 2_734 yes Br(1) Cu(1) S(1) C(6) 177.7(1) . . 2_735 2_735 yes Br(1) Cu(1) N(1) C(1) 80.8(2) . . . . yes Br(1) Cu(1) N(1) C(5) -100.1(2) . . . . yes Br(1) Cu(1) Br(1) Cu(1) 0.0000(2) . 2_734 2_734 . yes Br(1) Cu(1) N(1) C(1) 174.7(2) . 2_734 2_734 2_734 yes Br(1) Cu(1) N(1) C(5) -4.4(2) . 2_734 2_734 2_734 yes Cu(1) Br(1) Cu(1) Br(1) 0.0000(2) . . 2_734 2_734 yes Cu(1) Br(1) Cu(1) N(1) 113.75(7) . . 2_734 2_734 yes Cu(1) Br(1) Cu(1) Br(1) 0.0000(2) . 2_734 2_734 . yes Cu(1) Br(1) Cu(1) N(1) -107.18(6) . 2_734 2_734 2_734 yes Cu(1) S(1) C(6) N(2) 165.3(2) . 2_735 2_735 2_735 yes Cu(1) S(1) C(6) C(7) -12.7(3) . 2_735 2_735 2_735 yes Cu(1) N(1) C(1) N(2) -0.4(3) . . . . yes Cu(1) N(1) C(1) C(2) -178.2(2) . . . . yes Cu(1) N(1) C(5) C(4) 179.5(2) . . . . yes S(1) Cu(1) N(1) C(1) 51.6(2) . 2_735 2_735 2_735 yes S(1) Cu(1) N(1) C(5) -127.5(2) . 2_735 2_735 2_735 yes S(1) C(6) N(2) C(1) -1.8(4) . . . . yes S(1) C(6) N(2) C(10) 175.2(2) . . . . yes S(1) C(6) C(7) C(8) -175.8(3) . . . . yes N(1) Cu(1) S(1) C(6) -53.6(1) . . 2_735 2_735 yes N(1) C(1) N(2) C(6) 107.1(3) . . . . yes N(1) C(1) N(2) C(10) -70.1(3) . . . . yes N(1) C(1) C(2) C(3) -1.4(5) . . . . yes N(1) C(5) C(4) C(3) -1.2(5) . . . . yes N(2) C(1) N(1) C(5) -179.6(2) . . . . yes N(2) C(1) C(2) C(3) -179.1(3) . . . . yes N(2) C(6) C(7) C(8) 2.3(5) . . . . yes N(2) C(10) C(9) C(8) -0.5(6) . . . . yes C(1) N(1) C(5) C(4) -1.3(4) . . . . yes C(1) N(2) C(6) C(7) 180.0(3) . . . . yes C(1) N(2) C(10) C(9) 179.3(3) . . . . yes C(1) C(2) C(3) C(4) -1.3(5) . . . . yes C(2) C(1) N(1) C(5) 2.7(4) . . . . yes C(2) C(1) N(2) C(6) -75.0(3) . . . . yes C(2) C(1) N(2) C(10) 107.8(4) . . . . yes C(2) C(3) C(4) C(5) 2.5(5) . . . . yes C(6) N(2) C(10) C(9) 2.2(5) . . . . yes C(6) C(7) C(8) C(9) -0.9(6) . . . . yes C(7) C(6) N(2) C(10) -3.0(4) . . . . yes C(7) C(8) C(9) C(10) -0.1(6) . . . . yes C(7) C(8) C(9) C(10) -0.1(6) . . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Br(1) Cu(1) 2.5904(4) . 2_734 ? C(3) C(5) 3.545(5) . 2_744 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #===END #------------------------------------------------------------------------------ data_PPT _database_code_CSD 195992 _audit_creation_date 'Wed Oct 16 07:06:08 2002' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C10 H8 N2 S ' _chemical_formula_moiety 'C10 H8 N2 S ' _chemical_formula_weight 188.25 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,-z _cell_length_a 6.655(1) _cell_length_b 6.641(2) _cell_length_c 10.4614(7) _cell_angle_alpha 90 _cell_angle_beta 99.288(8) _cell_angle_gamma 90 _cell_volume 456.3(1) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.2 _cell_measurement_theta_max 14.8 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.500 _exptl_crystal_size_min 0.480 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.370 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.303 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.970 _exptl_absorpt_correction_T_max 1.000 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K$B%((Ja' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method $B%((Jw-2$B%((Jq _diffrn_reflns_number 3104 _diffrn_reflns_av_R_equivalents 0.016 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 29.97 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.00 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2663 _reflns_number_gt 2433 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0286 _refine_ls_wR_factor_ref 0.0828 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 2663 _refine_ls_number_parameters 150 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[$B%((Js^2^(Fo^2^) + (0.0513P)^2^+0.0296P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0010 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^$B%((Jl^3^/sin(2$B%((Jq)]^-1/4^' _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack 0.29(7) _refine_diff_density_max 0.17 _refine_diff_density_min -0.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S(1) S -0.24935(4) 0.79859(8) 0.26004(3) 0.0478(1) Uani 1.00 d . . . N(1) N 0.2245(2) 0.5778(2) 0.1909(1) 0.0498(3) Uani 1.00 d . . . N(2) N 0.1482(1) 0.7874(2) 0.35554(9) 0.0386(2) Uani 1.00 d . . . C(1) C 0.1865(2) 0.7635(2) 0.2234(1) 0.0397(3) Uani 1.00 d . . . C(2) C 0.1906(3) 0.9324(3) 0.1469(2) 0.0508(3) Uani 1.00 d . . . C(3) C 0.2377(3) 0.9026(4) 0.0238(2) 0.0603(5) Uani 1.00 d . . . C(4) C 0.2783(3) 0.7107(3) -0.0136(2) 0.0601(5) Uani 1.00 d . . . C(5) C 0.2693(3) 0.5549(3) 0.0707(2) 0.0597(4) Uani 1.00 d . . . C(6) C -0.0484(2) 0.8031(2) 0.3801(1) 0.0368(2) Uani 1.00 d . . . C(7) C -0.0653(2) 0.8193(2) 0.5137(1) 0.0433(3) Uani 1.00 d . . . C(8) C 0.0999(2) 0.8204(3) 0.6086(1) 0.0472(3) Uani 1.00 d . . . C(9) C 0.2965(2) 0.8050(4) 0.5770(1) 0.0546(3) Uani 1.00 d . . . C(10) C 0.3156(2) 0.7888(4) 0.4505(1) 0.0505(3) Uani 1.00 d . . . H(1) H 0.167(3) 1.055(4) 0.183(2) 0.06493(8) Uiso 1.00 calc . . . H(2) H 0.229(4) 1.010(4) -0.037(2) 0.07932(9) Uiso 1.00 calc . . . H(3) H 0.315(4) 0.678(4) -0.099(2) 0.08310(9) Uiso 1.00 calc . . . H(4) H 0.286(4) 0.415(5) 0.049(3) 0.0953(1) Uiso 1.00 calc . . . H(5) H -0.206(3) 0.833(3) 0.536(2) 0.05472(6) Uiso 1.00 calc . . . H(6) H 0.088(2) 0.835(3) 0.698(2) 0.04345(5) Uiso 1.00 calc . . . H(7) H 0.407(3) 0.788(5) 0.641(2) 0.06922(7) Uiso 1.00 calc . . . H(8) H 0.441(2) 0.767(3) 0.417(2) 0.04481(5) Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S(1) 0.0382(1) 0.0659(2) 0.0396(2) 0.0015(2) 0.0077(1) 0.0016(2) N(1) 0.0535(7) 0.0550(7) 0.0439(6) -0.0037(6) 0.0170(5) -0.0068(6) N(2) 0.0381(4) 0.0475(5) 0.0313(4) -0.0007(6) 0.0090(3) -0.0002(5) C(1) 0.0343(5) 0.0542(8) 0.0318(5) -0.0012(5) 0.0087(4) -0.0001(5) C(2) 0.0527(8) 0.0581(8) 0.0439(7) 0.0028(7) 0.0148(6) 0.0068(7) C(3) 0.0541(9) 0.089(1) 0.0401(8) -0.0001(9) 0.0140(7) 0.0170(8) C(4) 0.0499(8) 0.097(1) 0.0359(7) -0.0044(8) 0.0142(6) -0.0093(7) C(5) 0.0616(10) 0.071(1) 0.0498(8) -0.0045(8) 0.0198(7) -0.0168(8) C(6) 0.0398(5) 0.0375(5) 0.0349(5) -0.0010(6) 0.0111(4) 0.0005(6) C(7) 0.0518(6) 0.0445(7) 0.0371(5) 0.0008(7) 0.0173(4) -0.0006(6) C(8) 0.0645(7) 0.0458(7) 0.0326(5) -0.0008(7) 0.0120(5) -0.0007(6) C(9) 0.0553(7) 0.0699(9) 0.0367(5) -0.003(1) 0.0015(5) -0.0029(9) C(10) 0.0404(5) 0.0711(9) 0.0395(6) -0.0009(9) 0.0050(4) 0.0003(9) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL97' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag S(1) C(6) 1.681(1) . . yes N(1) C(1) 1.315(2) . . yes N(1) C(5) 1.346(2) . . yes N(2) C(1) 1.454(2) . . yes N(2) C(6) 1.377(2) . . yes N(2) C(10) 1.367(1) . . yes C(1) C(2) 1.381(2) . . yes C(2) C(3) 1.388(3) . . yes C(2) H(1) 0.922 . . no C(3) C(4) 1.372(3) . . yes C(3) H(2) 0.949 . . no C(4) C(5) 1.368(3) . . yes C(4) H(3) 0.984 . . no C(5) H(4) 0.967 . . no C(6) C(7) 1.424(2) . . yes C(7) C(8) 1.357(2) . . yes C(7) H(5) 1.007 . . no C(8) C(9) 1.404(2) . . yes C(8) H(6) 0.959 . . no C(9) C(10) 1.355(2) . . yes C(9) H(7) 0.916 . . no C(10) H(8) 0.965 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(1) N(1) C(5) 115.4(1) . . . yes C(1) N(2) C(6) 120.19(9) . . . yes C(1) N(2) C(10) 116.4(1) . . . yes C(6) N(2) C(10) 123.4(1) . . . yes N(1) C(1) N(2) 114.8(1) . . . yes N(1) C(1) C(2) 126.1(1) . . . yes N(2) C(1) C(2) 119.0(1) . . . yes C(1) C(2) C(3) 116.8(2) . . . yes C(1) C(2) H(1) 117.5 . . . no C(3) C(2) H(1) 125.6 . . . no C(2) C(3) C(4) 118.8(2) . . . yes C(2) C(3) H(2) 121.1 . . . no C(4) C(3) H(2) 119.9 . . . no C(3) C(4) C(5) 119.2(2) . . . yes C(3) C(4) H(3) 123.5 . . . no C(5) C(4) H(3) 117.3 . . . no N(1) C(5) C(4) 123.8(2) . . . yes N(1) C(5) H(4) 112.4 . . . no C(4) C(5) H(4) 123.7 . . . no S(1) C(6) N(2) 121.64(8) . . . yes S(1) C(6) C(7) 123.71(9) . . . yes N(2) C(6) C(7) 114.63(9) . . . yes C(6) C(7) C(8) 122.4(1) . . . yes C(6) C(7) H(5) 117.6 . . . no C(8) C(7) H(5) 120.1 . . . no C(7) C(8) C(9) 120.2(1) . . . yes C(7) C(8) H(6) 122.0 . . . no C(9) C(8) H(6) 117.8 . . . no C(8) C(9) C(10) 118.3(1) . . . yes C(8) C(9) H(7) 120.6 . . . no C(10) C(9) H(7) 120.5 . . . no N(2) C(10) C(9) 121.1(1) . . . yes N(2) C(10) H(8) 112.6 . . . no C(9) C(10) H(8) 126.1 . . . no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S(1) C(6) N(2) C(1) -0.8(2) . . . . yes S(1) C(6) N(2) C(10) -179.5(2) . . . . yes S(1) C(6) C(7) C(8) 179.3(1) . . . . yes N(1) C(1) N(2) C(6) -100.1(2) . . . . yes N(1) C(1) N(2) C(10) 78.6(2) . . . . yes N(1) C(1) C(2) C(3) 0.6(2) . . . . yes N(1) C(5) C(4) C(3) -0.8(3) . . . . yes N(2) C(1) N(1) C(5) -177.1(1) . . . . yes N(2) C(1) C(2) C(3) 176.9(1) . . . . yes N(2) C(6) C(7) C(8) 0.4(2) . . . . yes N(2) C(10) C(9) C(8) 0.0(4) . . . . yes C(1) N(1) C(5) C(4) 0.8(3) . . . . yes C(1) N(2) C(6) C(7) 178.0(1) . . . . yes C(1) N(2) C(10) C(9) -178.3(2) . . . . yes C(1) C(2) C(3) C(4) -0.5(2) . . . . yes C(2) C(1) N(1) C(5) -0.7(2) . . . . yes C(2) C(1) N(2) C(6) 83.2(2) . . . . yes C(2) C(1) N(2) C(10) -98.1(2) . . . . yes C(2) C(3) C(4) C(5) 0.6(3) . . . . yes C(6) N(2) C(10) C(9) 0.4(3) . . . . yes C(6) C(7) C(8) C(9) -0.1(3) . . . . yes C(7) C(6) N(2) C(10) -0.6(2) . . . . yes C(7) C(8) C(9) C(10) -0.2(3) . . . . yes C(7) C(8) C(9) C(10) -0.2(3) . . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag S(1) C(8) 3.539(2) . 2_546 ? N(2) C(7) 3.476(2) . 2_546 ? N(2) C(8) 3.562(2) . 2_546 ? C(3) C(5) 3.508(3) . 2_555 ? C(6) C(8) 3.228(2) . 2_546 ? C(6) C(7) 3.444(2) . 2_546 ? C(6) C(8) 3.457(2) . 2_556 ? C(7) C(7) 3.4561(8) . 2_556 ? C(7) C(7) 3.4561(8) . 2_546 ? C(7) C(8) 3.546(2) . 2_546 ? C(7) C(8) 3.560(2) . 2_556 ? C(7) C(10) 3.583(3) . 2_556 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #===END data_[CuCl2(BPTM)2] _database_code_CSD 195993 _audit_creation_date 'Wed Oct 16 06:42:51 2002' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C11 H10 Cl2 Cu N2 S2 ' _chemical_formula_moiety 'C11 H10 Cl2 Cu N2 S2 ' _chemical_formula_weight 368.79 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 12.476(1) _cell_length_b 8.4932(9) _cell_length_c 13.1982(8) _cell_angle_alpha 90 _cell_angle_beta 99.004(6) _cell_angle_gamma 90 _cell_volume 1381.3(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.7 _cell_measurement_theta_max 15.0 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.070 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.773 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 2.250 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.960 _exptl_absorpt_correction_T_max 1.000 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K$B%((Ja' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method $B%((Jw-2$B%((Jq _diffrn_reflns_number 4461 _diffrn_reflns_av_R_equivalents 0.032 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 30.00 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.07 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 4027 _reflns_number_gt 2588 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.0978 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 4027 _refine_ls_number_parameters 203 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[$B%((Js^2^(Fo^2^) + (0.0283P)^2^+0.3649P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max -0.0010 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^$B%((Jl^3^/sin(2(J$B%((Jq)]^-1/4^' _refine_diff_density_max 0.39 _refine_diff_density_min -0.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cu' 'Cu' 0.320 1.265 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu(1) Cu 0.12444(3) -0.00065(5) 0.42589(3) 0.0284(1) Uani 1.00 d . . . Cl(1) Cl 0.28378(7) 0.1313(1) 0.44940(7) 0.0440(2) Uani 1.00 d . . . Cl(2) Cl -0.03429(6) -0.1396(1) 0.40268(6) 0.0325(2) Uani 1.00 d . . . S(1) S 0.09103(7) -0.0264(1) 0.16940(7) 0.0378(2) Uani 1.00 d . . . S(2) S 0.29627(8) 0.1761(1) 0.15680(6) 0.0354(2) Uani 1.00 d . . . N(1) N 0.0591(2) 0.1676(3) 0.3239(2) 0.0317(6) Uani 1.00 d . . . N(2) N 0.2992(2) 0.3225(3) -0.0149(2) 0.0283(5) Uani 1.00 d . . . C(1) C 0.0502(3) 0.1524(4) 0.2213(3) 0.0324(7) Uani 1.00 d . . . C(2) C 0.0065(3) 0.2702(5) 0.1549(3) 0.0487(10) Uani 1.00 d . . . C(3) C -0.0265(3) 0.4087(5) 0.1943(4) 0.052(1) Uani 1.00 d . . . C(4) C -0.0158(3) 0.4269(5) 0.2981(3) 0.0437(9) Uani 1.00 d . . . C(5) C 0.0273(3) 0.3052(4) 0.3604(3) 0.0382(8) Uani 1.00 d . . . C(6) C 0.2376(3) -0.0047(4) 0.1894(3) 0.0329(7) Uani 1.00 d . . . C(7) C 0.2689(3) 0.1854(4) 0.0227(2) 0.0275(6) Uani 1.00 d . . . C(8) C 0.2194(3) 0.0678(4) -0.0406(3) 0.0394(8) Uani 1.00 d . . . C(9) C 0.1976(3) 0.0957(5) -0.1449(3) 0.0411(9) Uani 1.00 d . . . C(10) C 0.2263(3) 0.2375(5) -0.1832(3) 0.0405(8) Uani 1.00 d . . . C(11) C 0.2768(3) 0.3468(4) -0.1162(3) 0.0351(7) Uani 1.00 d . . . H(1) H 0.003(3) 0.247(5) 0.081(3) 0.0491(1) Uiso 1.00 calc . . . H(2) H -0.050(4) 0.494(5) 0.150(3) 0.0761(2) Uiso 1.00 calc . . . H(3) H -0.039(3) 0.524(5) 0.332(3) 0.0579(2) Uiso 1.00 calc . . . H(4) H 0.034(3) 0.312(5) 0.426(3) 0.0533(2) Uiso 1.00 calc . . . H(5) H 0.264(3) -0.015(4) 0.256(3) 0.02171(10) Uiso 1.00 calc . . . H(6) H 0.262(2) -0.088(4) 0.152(2) 0.0197(1) Uiso 1.00 calc . . . H(7) H 0.200(3) -0.026(4) -0.014(3) 0.0395(1) Uiso 1.00 calc . . . H(8) H 0.170(3) 0.025(4) -0.187(3) 0.0373(1) Uiso 1.00 calc . . . H(9) H 0.213(3) 0.251(4) -0.250(3) 0.0320(1) Uiso 1.00 calc . . . H(10) H 0.300(3) 0.448(4) -0.137(3) 0.0369(1) Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu(1) 0.0290(2) 0.0256(2) 0.0286(2) 0.0008(2) -0.0016(1) 0.0037(2) Cl(1) 0.0375(5) 0.0385(5) 0.0518(5) -0.0084(4) -0.0065(4) 0.0115(4) Cl(2) 0.0304(4) 0.0327(4) 0.0326(4) -0.0010(3) -0.0004(3) -0.0020(3) S(1) 0.0374(5) 0.0367(5) 0.0389(5) -0.0036(4) 0.0043(4) -0.0024(4) S(2) 0.0491(5) 0.0289(4) 0.0279(4) -0.0090(4) 0.0052(4) -0.0031(3) N(1) 0.028(1) 0.029(1) 0.037(1) -0.001(1) 0.001(1) 0.005(1) N(2) 0.029(1) 0.029(1) 0.026(1) -0.003(1) 0.000(1) 0.000(1) C(1) 0.028(2) 0.034(2) 0.034(2) 0.002(1) 0.001(1) 0.008(1) C(2) 0.055(2) 0.048(2) 0.041(2) 0.007(2) 0.002(2) 0.015(2) C(3) 0.049(2) 0.044(2) 0.060(3) 0.014(2) 0.001(2) 0.021(2) C(4) 0.038(2) 0.034(2) 0.060(3) 0.008(2) 0.008(2) 0.005(2) C(5) 0.041(2) 0.035(2) 0.038(2) -0.001(2) 0.005(2) 0.003(2) C(6) 0.038(2) 0.029(2) 0.032(2) -0.001(2) 0.005(1) 0.003(1) C(7) 0.031(2) 0.025(1) 0.027(1) -0.002(1) 0.005(1) 0.000(1) C(8) 0.051(2) 0.034(2) 0.036(2) -0.017(2) 0.012(2) -0.008(2) C(9) 0.043(2) 0.049(2) 0.031(2) -0.018(2) 0.007(2) -0.016(2) C(10) 0.041(2) 0.053(2) 0.025(2) -0.005(2) -0.002(1) -0.003(2) C(11) 0.038(2) 0.037(2) 0.028(2) -0.006(2) -0.002(1) 0.004(1) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL97' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu(1) Cl(1) 2.261(1) . . yes Cu(1) Cl(2) 2.2842(9) . . yes Cu(1) N(1) 2.043(3) . . yes Cu(1) N(2) 2.047(3) . 2_545 yes S(1) C(1) 1.773(4) . . yes S(1) C(6) 1.815(4) . . yes S(2) C(6) 1.783(4) . . yes S(2) C(7) 1.751(3) . . yes N(1) C(1) 1.347(4) . . yes N(1) C(5) 1.347(5) . . yes N(2) C(7) 1.343(4) . . yes N(2) C(11) 1.339(4) . . yes C(1) C(2) 1.385(5) . . yes C(2) C(3) 1.375(6) . . yes C(2) H(1) 0.989 . . no C(3) C(4) 1.365(6) . . yes C(3) H(2) 0.949 . . no C(4) C(5) 1.377(5) . . yes C(4) H(3) 1.005 . . no C(5) H(4) 0.863 . . no C(6) H(5) 0.889 . . no C(6) H(6) 0.937 . . no C(7) C(8) 1.384(5) . . yes C(8) C(9) 1.381(5) . . yes C(8) H(7) 0.921 . . no C(9) C(10) 1.375(6) . . yes C(9) H(8) 0.852 . . no C(10) C(11) 1.366(5) . . yes C(10) H(9) 0.877 . . no C(11) H(10) 0.961 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Cu(1) Cl(2) 178.62(4) . . . yes Cl(1) Cu(1) N(1) 89.73(8) . . . yes Cl(1) Cu(1) N(2) 87.98(8) . . 2_545 yes Cl(2) Cu(1) N(1) 91.42(8) . . . yes Cl(2) Cu(1) N(2) 90.80(8) . . 2_545 yes N(1) Cu(1) N(2) 173.1(1) . . 2_545 yes C(1) S(1) C(6) 101.5(2) . . . yes C(6) S(2) C(7) 105.1(2) . . . yes Cu(1) N(1) C(1) 123.8(2) . . . yes Cu(1) N(1) C(5) 118.7(2) . . . yes C(1) N(1) C(5) 117.4(3) . . . yes Cu(1) N(2) C(7) 123.8(2) 2_555 . . yes Cu(1) N(2) C(11) 117.8(2) 2_555 . . yes C(7) N(2) C(11) 118.4(3) . . . yes S(1) C(1) N(1) 119.1(2) . . . yes S(1) C(1) C(2) 118.8(3) . . . yes N(1) C(1) C(2) 122.0(3) . . . yes C(1) C(2) C(3) 119.3(4) . . . yes C(1) C(2) H(1) 115.6 . . . no C(3) C(2) H(1) 125.1 . . . no C(2) C(3) C(4) 119.2(4) . . . yes C(2) C(3) H(2) 119.8 . . . no C(4) C(3) H(2) 120.7 . . . no C(3) C(4) C(5) 118.9(4) . . . yes C(3) C(4) H(3) 123.4 . . . no C(5) C(4) H(3) 117.7 . . . no N(1) C(5) C(4) 123.1(4) . . . yes N(1) C(5) H(4) 115.7 . . . no C(4) C(5) H(4) 121.2 . . . no S(1) C(6) S(2) 119.7(2) . . . yes S(1) C(6) H(5) 110.4 . . . no S(1) C(6) H(6) 104.7 . . . no S(2) C(6) H(5) 102.5 . . . no S(2) C(6) H(6) 109.9 . . . no H(5) C(6) H(6) 109.6 . . . no S(2) C(7) N(2) 113.0(2) . . . yes S(2) C(7) C(8) 125.1(3) . . . yes N(2) C(7) C(8) 121.9(3) . . . yes C(7) C(8) C(9) 118.5(3) . . . yes C(7) C(8) H(7) 120.6 . . . no C(9) C(8) H(7) 120.8 . . . no C(8) C(9) C(10) 119.7(3) . . . yes C(8) C(9) H(8) 121.2 . . . no C(10) C(9) H(8) 119.0 . . . no C(9) C(10) C(11) 118.5(3) . . . yes C(9) C(10) H(9) 117.8 . . . no C(11) C(10) H(9) 123.7 . . . no N(2) C(11) C(10) 123.0(3) . . . yes N(2) C(11) H(10) 113.5 . . . no C(10) C(11) H(10) 123.4 . . . no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cu(1) N(1) C(1) S(1) 3.1(4) . . . . yes Cu(1) N(1) C(1) C(2) -179.3(3) . . . . yes Cu(1) N(1) C(5) C(4) 178.8(3) . . . . yes Cu(1) N(2) C(7) S(2) 2.6(3) . 2_545 2_545 2_545 yes Cu(1) N(2) C(7) C(8) -178.7(3) . 2_545 2_545 2_545 yes Cu(1) N(2) C(11) C(10) 179.9(3) . 2_545 2_545 2_545 yes Cl(1) Cu(1) N(1) C(1) 98.3(3) . . . . yes Cl(1) Cu(1) N(1) C(5) -78.5(3) . . . . yes Cl(1) Cu(1) N(2) C(7) -104.5(3) . . 2_545 2_545 yes Cl(1) Cu(1) N(2) C(11) 74.4(2) . . 2_545 2_545 yes Cl(2) Cu(1) N(1) C(1) -80.9(3) . . . . yes Cl(2) Cu(1) N(1) C(5) 102.3(3) . . . . yes Cl(2) Cu(1) N(2) C(7) 74.8(3) . . 2_545 2_545 yes Cl(2) Cu(1) N(2) C(11) -106.3(2) . . 2_545 2_545 yes S(1) C(1) N(1) C(5) 180.0(3) . . . . yes S(1) C(1) C(2) C(3) 179.3(3) . . . . yes S(1) C(6) S(2) C(7) -68.8(2) . . . . yes S(2) C(6) S(1) C(1) -46.1(2) . . . . yes S(2) C(7) N(2) C(11) -176.3(2) . . . . yes S(2) C(7) C(8) C(9) 176.4(3) . . . . yes N(1) Cu(1) N(2) C(7) -33.8(10) . . 2_545 2_545 yes N(1) Cu(1) N(2) C(11) 145.1(8) . . 2_545 2_545 yes N(1) C(1) S(1) C(6) -78.1(3) . . . . yes N(1) C(1) C(2) C(3) 1.7(6) . . . . yes N(1) C(5) C(4) C(3) -0.4(6) . . . . yes N(2) C(7) S(2) C(6) 174.2(2) . . . . yes N(2) C(7) C(8) C(9) -2.2(5) . . . . yes N(2) C(11) C(10) C(9) -0.4(6) . . . . yes C(1) N(1) C(5) C(4) 1.8(5) . . . . yes C(1) C(2) C(3) C(4) -0.3(6) . . . . yes C(2) C(1) S(1) C(6) 104.2(3) . . . . yes C(2) C(1) N(1) C(5) -2.4(5) . . . . yes C(2) C(3) C(4) C(5) -0.4(6) . . . . yes C(6) S(2) C(7) C(8) -4.4(4) . . . . yes C(7) N(2) C(11) C(10) -1.1(5) . . . . yes C(7) C(8) C(9) C(10) 0.6(6) . . . . yes C(8) C(7) N(2) C(11) 2.4(5) . . . . yes C(8) C(9) C(10) C(11) 0.6(6) . . . . yes C(8) C(9) C(10) C(11) 0.6(6) . . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cu(1) Cl(2) 2.9324(9) . 3_556 ? Cl(1) C(6) 3.582(4) . 2_555 ? Cl(2) C(11) 3.408(4) . 4_455 ? Cl(2) C(5) 3.417(4) . 3_556 ? Cl(2) Cl(2) 3.502(2) . 3_556 ? Cl(2) C(10) 3.556(4) . 3_555 ? S(2) C(6) 3.452(4) . 2_555 ? C(4) C(6) 3.498(5) . 2_555 ? C(4) C(10) 3.552(6) . 4_455 ? C(5) C(11) 3.439(5) . 4_455 ? C(5) C(6) 3.500(5) . 2_555 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #===END #------------------------------------------------------------------------------ data__tptm-Cu3 _database_code_CSD 195994 _audit_creation_date 'Mon Aug 5 18:01:45 2002' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C18 H15 Cu F6 N4 P S3 ' _chemical_formula_moiety 'C18 H15 Cu F6 N4 P S3 ' _chemical_formula_weight 592.03 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/a 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,-z -x,-y,-z 1/2+x,1/2-y,z _cell_length_a 14.414(2) _cell_length_b 10.132(2) _cell_length_c 15.605(2) _cell_angle_alpha 90 _cell_angle_beta 91.534(4) _cell_angle_gamma 90 _cell_volume 2278.4(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 8046 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 193.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'Chip' _exptl_crystal_colour 'purple' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.020 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.726 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.368 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.696 _exptl_absorpt_correction_T_max 0.973 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K$B%((Ja' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method $B%((Jw _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 22495 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.48 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5117 _reflns_number_gt 3700 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.1054 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 5117 _refine_ls_number_parameters 358 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[$B%((Js^2^(Fo^2^) + (0.0496P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0000 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^$B%(l^3^/sin(2$B%((Jq)]^-1/4^' _refine_diff_density_max 0.87 _refine_diff_density_min -0.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Cu' 'Cu' 0.320 1.265 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu(1) Cu 0.11005(3) 0.20477(4) 0.22399(2) 0.0239(1) Uani 1.00 d . . . S(1) S 0.14640(6) -0.04125(8) 0.11123(5) 0.0289(2) Uani 1.00 d . . . S(2) S -0.02985(6) 0.10306(9) 0.08679(5) 0.0308(2) Uani 1.00 d . . . S(3) S 0.14369(7) 0.22016(8) 0.02862(5) 0.0328(2) Uani 1.00 d . . . P(1) P 0.09608(7) -0.2342(1) 0.41169(6) 0.0410(2) Uani 1.00 d . . . F(1) F 0.1354(2) -0.0894(3) 0.4247(2) 0.0648(7) Uani 1.00 d . . . F(2) F 0.0544(2) -0.1945(3) 0.3196(2) 0.0811(9) Uani 1.00 d . . . F(3) F 0.0559(2) -0.3806(3) 0.3972(2) 0.0623(7) Uani 1.00 d . . . F(4) F 0.1885(2) -0.2786(4) 0.3720(3) 0.109(1) Uani 1.00 d . . . F(5) F 0.1343(3) -0.2731(3) 0.5038(2) 0.091(1) Uani 1.00 d . . . F(6) F 0.0023(2) -0.1878(3) 0.4527(2) 0.0788(9) Uani 1.00 d . . . N(1) N 0.2308(2) 0.0940(3) 0.2374(2) 0.0255(6) Uani 1.00 d . . . N(2) N -0.0130(2) 0.1122(3) 0.2573(2) 0.0243(6) Uani 1.00 d . . . N(3) N 0.1075(2) 0.3823(3) 0.1579(2) 0.0239(6) Uani 1.00 d . . . N(4) N 0.1277(2) 0.2914(3) 0.3405(2) 0.0313(6) Uani 1.00 d . . . C(1) C 0.0924(2) 0.1183(3) 0.1092(2) 0.0241(7) Uani 1.00 d . . . C(2) C 0.2334(2) -0.0167(3) 0.1908(2) 0.0245(7) Uani 1.00 d . . . C(3) C 0.3019(3) -0.1113(4) 0.2027(2) 0.0330(8) Uani 1.00 d . . . C(4) C 0.3707(3) -0.0898(4) 0.2633(2) 0.0390(9) Uani 1.00 d . . . C(5) C 0.3711(3) 0.0264(4) 0.3088(2) 0.0378(9) Uani 1.00 d . . . C(6) C 0.3008(2) 0.1140(4) 0.2953(2) 0.0326(8) Uani 1.00 d . . . C(7) C -0.0677(2) 0.0715(3) 0.1912(2) 0.0268(7) Uani 1.00 d . . . C(8) C -0.1515(3) 0.0078(4) 0.2027(3) 0.0375(9) Uani 1.00 d . . . C(9) C -0.1794(3) -0.0164(4) 0.2846(3) 0.0412(9) Uani 1.00 d . . . C(10) C -0.1234(3) 0.0241(4) 0.3528(3) 0.0379(9) Uani 1.00 d . . . C(11) C -0.0410(2) 0.0868(4) 0.3370(2) 0.0300(7) Uani 1.00 d . . . C(12) C 0.1237(2) 0.3762(3) 0.0737(2) 0.0254(7) Uani 1.00 d . . . C(13) C 0.1261(3) 0.4888(4) 0.0221(2) 0.0318(8) Uani 1.00 d . . . C(14) C 0.1120(3) 0.6097(4) 0.0592(2) 0.0382(9) Uani 1.00 d . . . C(15) C 0.0942(3) 0.6163(4) 0.1453(2) 0.0359(8) Uani 1.00 d . . . C(16) C 0.0924(2) 0.5018(3) 0.1920(2) 0.0279(7) Uani 1.00 d . . . C(17) C 0.1390(2) 0.3318(3) 0.4077(2) 0.0284(7) Uani 1.00 d . . . C(18) C 0.1532(4) 0.3840(6) 0.4936(3) 0.044(1) Uani 1.00 d . . . H(1) H 0.298(2) -0.180(4) 0.175(2) 0.0260(1) Uiso 1.00 calc . . . H(2) H 0.411(3) -0.151(4) 0.268(2) 0.0450(2) Uiso 1.00 calc . . . H(3) H 0.413(3) 0.044(4) 0.349(2) 0.0382(1) Uiso 1.00 calc . . . H(4) H 0.295(3) 0.191(4) 0.327(2) 0.0388(1) Uiso 1.00 calc . . . H(5) H -0.188(3) -0.020(4) 0.154(3) 0.0483(1) Uiso 1.00 calc . . . H(6) H -0.238(3) -0.061(4) 0.295(2) 0.0353(1) Uiso 1.00 calc . . . H(7) H -0.140(3) 0.006(4) 0.405(3) 0.0488(2) Uiso 1.00 calc . . . H(8) H 0.000(2) 0.114(3) 0.381(2) 0.0198(1) Uiso 1.00 calc . . . H(9) H 0.138(2) 0.474(4) -0.034(2) 0.0318(1) Uiso 1.00 calc . . . H(10) H 0.118(2) 0.688(4) 0.023(2) 0.0317(1) Uiso 1.00 calc . . . H(11) H 0.081(3) 0.686(4) 0.169(2) 0.0390(1) Uiso 1.00 calc . . . H(12) H 0.084(2) 0.500(4) 0.246(2) 0.0306(1) Uiso 1.00 calc . . . H(13) H 0.188(4) 0.329(6) 0.528(3) 0.0782(2) Uiso 1.00 calc . . . H(14) H 0.104(4) 0.395(6) 0.514(4) 0.0990(3) Uiso 1.00 calc . . . H(15) H 0.190(4) 0.452(6) 0.489(4) 0.0941(3) Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu(1) 0.0318(2) 0.0209(2) 0.0188(2) -0.0011(2) -0.0007(1) -0.0020(2) S(1) 0.0394(5) 0.0181(4) 0.0289(4) 0.0016(3) -0.0069(3) -0.0033(3) S(2) 0.0343(5) 0.0355(5) 0.0224(4) 0.0004(4) -0.0071(3) 0.0007(3) S(3) 0.0523(6) 0.0223(4) 0.0244(4) 0.0014(4) 0.0117(4) -0.0003(3) P(1) 0.0383(6) 0.0469(6) 0.0377(5) 0.0028(5) -0.0018(4) -0.0122(5) F(1) 0.066(2) 0.050(2) 0.077(2) -0.005(1) -0.013(1) -0.012(1) F(2) 0.117(3) 0.077(2) 0.047(2) -0.003(2) -0.018(2) -0.006(1) F(3) 0.070(2) 0.048(2) 0.068(2) -0.008(1) -0.017(1) -0.009(1) F(4) 0.060(2) 0.100(3) 0.169(3) 0.006(2) 0.042(2) -0.061(3) F(5) 0.154(3) 0.060(2) 0.056(2) 0.012(2) -0.046(2) -0.001(1) F(6) 0.063(2) 0.078(2) 0.096(2) 0.012(2) 0.025(2) -0.006(2) N(1) 0.027(1) 0.026(1) 0.023(1) 0.000(1) -0.002(1) 0.000(1) N(2) 0.027(1) 0.024(1) 0.022(1) 0.003(1) 0.000(1) 0.002(1) N(3) 0.028(1) 0.019(1) 0.025(1) -0.001(1) 0.003(1) 0.000(1) N(4) 0.038(2) 0.031(2) 0.025(1) 0.000(1) 0.000(1) -0.002(1) C(1) 0.036(2) 0.018(2) 0.018(1) 0.000(1) -0.001(1) -0.001(1) C(2) 0.029(2) 0.023(2) 0.021(2) 0.000(1) 0.002(1) 0.004(1) C(3) 0.039(2) 0.028(2) 0.032(2) 0.007(2) 0.006(1) 0.003(2) C(4) 0.035(2) 0.045(2) 0.037(2) 0.013(2) 0.003(2) 0.013(2) C(5) 0.030(2) 0.054(3) 0.030(2) 0.004(2) -0.006(1) 0.005(2) C(6) 0.034(2) 0.037(2) 0.027(2) -0.002(2) -0.003(1) -0.002(2) C(7) 0.030(2) 0.022(2) 0.028(2) 0.004(1) 0.001(1) 0.001(1) C(8) 0.028(2) 0.038(2) 0.046(2) -0.002(2) -0.001(2) -0.002(2) C(9) 0.030(2) 0.043(2) 0.051(2) -0.003(2) 0.007(2) 0.002(2) C(10) 0.038(2) 0.038(2) 0.038(2) 0.004(2) 0.013(2) 0.006(2) C(11) 0.033(2) 0.031(2) 0.026(2) 0.001(2) 0.000(1) 0.000(1) C(12) 0.029(2) 0.021(2) 0.026(2) 0.000(1) 0.002(1) 0.000(1) C(13) 0.043(2) 0.028(2) 0.025(2) 0.000(2) 0.005(1) 0.005(1) C(14) 0.051(2) 0.022(2) 0.041(2) -0.002(2) 0.004(2) 0.009(2) C(15) 0.050(2) 0.019(2) 0.039(2) 0.003(2) 0.006(2) -0.003(2) C(16) 0.031(2) 0.024(2) 0.029(2) 0.001(1) 0.004(1) -0.003(1) C(17) 0.026(2) 0.031(2) 0.028(2) 0.000(1) 0.001(1) 0.001(1) C(18) 0.043(3) 0.061(3) 0.027(2) 0.000(2) -0.006(2) -0.011(2) #------------------------------------------------------------------------------ _computing_data_collection 'CRYSTALCLEAR' _computing_cell_refinement 'CRYSTALCLEAR' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL97' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu(1) N(1) 2.077(3) . . yes Cu(1) N(2) 2.084(3) . . yes Cu(1) N(3) 2.074(3) . . yes Cu(1) N(4) 2.028(3) . . yes Cu(1) C(1) 2.004(3) . . yes S(1) C(1) 1.794(3) . . yes S(1) C(2) 1.759(3) . . yes S(2) C(1) 1.794(3) . . yes S(2) C(7) 1.762(3) . . yes S(3) C(1) 1.801(3) . . yes S(3) C(12) 1.758(3) . . yes P(1) F(1) 1.584(3) . . yes P(1) F(2) 1.595(3) . . yes P(1) F(3) 1.607(3) . . yes P(1) F(4) 1.551(4) . . yes P(1) F(5) 1.576(3) . . yes P(1) F(6) 1.583(3) . . yes N(1) C(2) 1.338(4) . . yes N(1) C(6) 1.352(4) . . yes N(2) C(7) 1.346(4) . . yes N(2) C(11) 1.343(4) . . yes N(3) C(12) 1.342(4) . . yes N(3) C(16) 1.342(4) . . yes N(4) C(17) 1.135(4) . . yes C(2) C(3) 1.385(5) . . yes C(3) C(4) 1.369(5) . . yes C(4) C(5) 1.374(6) . . yes C(5) C(6) 1.359(5) . . yes C(7) C(8) 1.385(5) . . yes C(8) C(9) 1.372(6) . . yes C(9) C(10) 1.381(6) . . yes C(10) C(11) 1.375(5) . . yes C(12) C(13) 1.397(5) . . yes C(13) C(14) 1.372(5) . . yes C(14) C(15) 1.377(5) . . yes C(15) C(16) 1.371(5) . . yes C(17) C(18) 1.450(5) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Cu(1) N(2) 116.6(1) . . . yes N(1) Cu(1) N(3) 121.5(1) . . . yes N(1) Cu(1) N(4) 93.4(1) . . . yes N(1) Cu(1) C(1) 86.5(1) . . . yes N(2) Cu(1) N(3) 120.7(1) . . . yes N(2) Cu(1) N(4) 93.4(1) . . . yes N(2) Cu(1) C(1) 86.4(1) . . . yes N(3) Cu(1) N(4) 94.0(1) . . . yes N(3) Cu(1) C(1) 86.3(1) . . . yes N(4) Cu(1) C(1) 179.7(1) . . . yes C(1) S(1) C(2) 100.7(1) . . . yes C(1) S(2) C(7) 99.3(1) . . . yes C(1) S(3) C(12) 99.3(1) . . . yes F(1) P(1) F(2) 90.4(2) . . . yes F(1) P(1) F(3) 179.2(2) . . . yes F(1) P(1) F(4) 90.7(2) . . . yes F(1) P(1) F(5) 90.0(2) . . . yes F(1) P(1) F(6) 88.8(2) . . . yes F(2) P(1) F(3) 88.9(2) . . . yes F(2) P(1) F(4) 91.2(2) . . . yes F(2) P(1) F(5) 178.3(2) . . . yes F(2) P(1) F(6) 89.1(2) . . . yes F(3) P(1) F(4) 89.2(2) . . . yes F(3) P(1) F(5) 90.8(2) . . . yes F(3) P(1) F(6) 91.3(2) . . . yes F(4) P(1) F(5) 90.5(2) . . . yes F(4) P(1) F(6) 179.4(2) . . . yes F(5) P(1) F(6) 89.3(2) . . . yes Cu(1) N(1) C(2) 115.7(2) . . . yes Cu(1) N(1) C(6) 126.5(2) . . . yes C(2) N(1) C(6) 117.2(3) . . . yes Cu(1) N(2) C(7) 115.6(2) . . . yes Cu(1) N(2) C(11) 126.6(2) . . . yes C(7) N(2) C(11) 117.8(3) . . . yes Cu(1) N(3) C(12) 116.5(2) . . . yes Cu(1) N(3) C(16) 125.9(2) . . . yes C(12) N(3) C(16) 117.6(3) . . . yes Cu(1) N(4) C(17) 175.5(3) . . . yes Cu(1) C(1) S(1) 109.5(1) . . . yes Cu(1) C(1) S(2) 108.2(2) . . . yes Cu(1) C(1) S(3) 109.2(2) . . . yes S(1) C(1) S(2) 110.4(2) . . . yes S(1) C(1) S(3) 110.0(2) . . . yes S(2) C(1) S(3) 109.4(2) . . . yes S(1) C(2) N(1) 118.2(2) . . . yes S(1) C(2) C(3) 119.3(3) . . . yes N(1) C(2) C(3) 122.5(3) . . . yes C(2) C(3) C(4) 118.9(3) . . . yes C(3) C(4) C(5) 119.1(4) . . . yes C(4) C(5) C(6) 119.1(3) . . . yes N(1) C(6) C(5) 123.1(3) . . . yes S(2) C(7) N(2) 117.6(2) . . . yes S(2) C(7) C(8) 119.8(3) . . . yes N(2) C(7) C(8) 122.6(3) . . . yes C(7) C(8) C(9) 118.8(3) . . . yes C(8) C(9) C(10) 119.0(4) . . . yes C(9) C(10) C(11) 119.3(4) . . . yes N(2) C(11) C(10) 122.5(3) . . . yes S(3) C(12) N(3) 117.9(2) . . . yes S(3) C(12) C(13) 119.8(2) . . . yes N(3) C(12) C(13) 122.3(3) . . . yes C(12) C(13) C(14) 118.7(3) . . . yes C(13) C(14) C(15) 119.2(3) . . . yes C(14) C(15) C(16) 119.0(3) . . . yes N(3) C(16) C(15) 123.2(3) . . . yes N(4) C(17) C(18) 179.8(4) . . . yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cu(1) N(1) C(2) S(1) 10.9(3) . . . . yes Cu(1) N(1) C(2) C(3) -169.3(3) . . . . yes Cu(1) N(1) C(6) C(5) 169.9(3) . . . . yes Cu(1) N(2) C(7) S(2) -0.8(3) . . . . yes Cu(1) N(2) C(7) C(8) 179.7(3) . . . . yes Cu(1) N(2) C(11) C(10) -179.5(3) . . . . yes Cu(1) N(3) C(12) S(3) 0.8(3) . . . . yes Cu(1) N(3) C(12) C(13) -178.4(3) . . . . yes Cu(1) N(3) C(16) C(15) 178.0(3) . . . . yes Cu(1) N(4) C(17) C(18) -155(98) . . . . yes Cu(1) C(1) S(1) C(2) -27.0(2) . . . . yes Cu(1) C(1) S(2) C(7) -35.5(2) . . . . yes Cu(1) C(1) S(3) C(12) -32.5(2) . . . . yes S(1) C(1) Cu(1) N(1) 28.1(2) . . . . yes S(1) C(1) Cu(1) N(2) -88.9(2) . . . . yes S(1) C(1) Cu(1) N(3) 150.0(2) . . . . yes S(1) C(1) Cu(1) N(4) -41(23) . . . . yes S(1) C(1) S(2) C(7) 84.3(2) . . . . yes S(1) C(1) S(3) C(12) -152.8(2) . . . . yes S(1) C(2) N(1) C(6) -176.9(2) . . . . yes S(1) C(2) C(3) C(4) 178.4(3) . . . . yes S(2) C(1) Cu(1) N(1) 148.5(2) . . . . yes S(2) C(1) Cu(1) N(2) 31.5(2) . . . . yes S(2) C(1) Cu(1) N(3) -89.6(2) . . . . yes S(2) C(1) Cu(1) N(4) 79(23) . . . . yes S(2) C(1) S(1) C(2) -146.0(2) . . . . yes S(2) C(1) S(3) C(12) 85.7(2) . . . . yes S(2) C(7) N(2) C(11) -179.1(2) . . . . yes S(2) C(7) C(8) C(9) 179.7(3) . . . . yes S(3) C(1) Cu(1) N(1) -92.5(2) . . . . yes S(3) C(1) Cu(1) N(2) 150.5(2) . . . . yes S(3) C(1) Cu(1) N(3) 29.4(2) . . . . yes S(3) C(1) Cu(1) N(4) -161(22) . . . . yes S(3) C(1) S(1) C(2) 93.1(2) . . . . yes S(3) C(1) S(2) C(7) -154.4(2) . . . . yes S(3) C(12) N(3) C(16) 179.9(2) . . . . yes S(3) C(12) C(13) C(14) -178.8(3) . . . . yes N(1) Cu(1) N(2) C(7) -103.6(2) . . . . yes N(1) Cu(1) N(2) C(11) 74.5(3) . . . . yes N(1) Cu(1) N(3) C(12) 64.6(2) . . . . yes N(1) Cu(1) N(3) C(16) -114.4(3) . . . . yes N(1) Cu(1) N(4) C(17) -45(3) . . . . yes N(1) C(2) S(1) C(1) 10.3(3) . . . . yes N(1) C(2) C(3) C(4) -1.3(5) . . . . yes N(1) C(6) C(5) C(4) -1.6(6) . . . . yes N(2) Cu(1) N(1) C(2) 60.2(2) . . . . yes N(2) Cu(1) N(1) C(6) -111.1(3) . . . . yes N(2) Cu(1) N(3) C(12) -102.6(2) . . . . yes N(2) Cu(1) N(3) C(16) 78.4(3) . . . . yes N(2) Cu(1) N(4) C(17) 71(3) . . . . yes N(2) C(7) S(2) C(1) 23.3(3) . . . . yes N(2) C(7) C(8) C(9) -0.8(5) . . . . yes N(2) C(11) C(10) C(9) 0.9(6) . . . . yes N(3) Cu(1) N(1) C(2) -107.5(2) . . . . yes N(3) Cu(1) N(1) C(6) 81.2(3) . . . . yes N(3) Cu(1) N(2) C(7) 64.2(3) . . . . yes N(3) Cu(1) N(2) C(11) -117.7(3) . . . . yes N(3) Cu(1) N(4) C(17) -167(3) . . . . yes N(3) C(12) S(3) C(1) 20.2(3) . . . . yes N(3) C(12) C(13) C(14) 0.5(5) . . . . yes N(3) C(16) C(15) C(14) 0.2(6) . . . . yes N(4) Cu(1) N(1) C(2) 155.7(2) . . . . yes N(4) Cu(1) N(1) C(6) -15.6(3) . . . . yes N(4) Cu(1) N(2) C(7) 160.9(2) . . . . yes N(4) Cu(1) N(2) C(11) -21.0(3) . . . . yes N(4) Cu(1) N(3) C(12) 161.1(2) . . . . yes N(4) Cu(1) N(3) C(16) -17.9(3) . . . . yes C(1) Cu(1) N(1) C(2) -24.0(2) . . . . yes C(1) Cu(1) N(1) C(6) 164.7(3) . . . . yes C(1) Cu(1) N(2) C(7) -19.3(2) . . . . yes C(1) Cu(1) N(2) C(11) 158.8(3) . . . . yes C(1) Cu(1) N(3) C(12) -19.0(2) . . . . yes C(1) Cu(1) N(3) C(16) 162.0(3) . . . . yes C(1) Cu(1) N(4) C(17) 24(24) . . . . yes C(1) S(1) C(2) C(3) -169.5(3) . . . . yes C(1) S(2) C(7) C(8) -157.2(3) . . . . yes C(1) S(3) C(12) C(13) -160.5(3) . . . . yes C(2) N(1) C(6) C(5) -1.3(5) . . . . yes C(2) C(3) C(4) C(5) -1.7(6) . . . . yes C(3) C(2) N(1) C(6) 2.8(5) . . . . yes C(3) C(4) C(5) C(6) 3.1(6) . . . . yes C(7) N(2) C(11) C(10) -1.4(5) . . . . yes C(7) C(8) C(9) C(10) 0.3(6) . . . . yes C(8) C(7) N(2) C(11) 1.4(5) . . . . yes C(8) C(9) C(10) C(11) -0.3(6) . . . . yes C(12) N(3) C(16) C(15) -1.0(5) . . . . yes C(12) C(13) C(14) C(15) -1.3(6) . . . . yes C(13) C(12) N(3) C(16) 0.7(5) . . . . yes C(13) C(14) C(15) C(16) 1.0(6) . . . . yes C(13) C(14) C(15) C(16) 1.0(6) . . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag S(1) S(2) 3.533(1) . 3_555 ? S(1) C(15) 3.593(4) . 1_545 ? S(2) S(2) 3.545(2) . 3_555 ? F(1) C(18) 3.283(6) . 2_546 ? F(1) C(10) 3.544(5) . 3_556 ? F(2) C(15) 3.389(5) . 1_545 ? F(2) C(4) 3.526(5) . 4_445 ? F(3) C(18) 3.132(6) . 1_545 ? F(3) C(17) 3.153(4) . 1_545 ? F(3) C(5) 3.313(5) . 4_445 ? F(3) C(4) 3.359(5) . 4_445 ? F(3) C(16) 3.470(4) . 1_545 ? F(3) C(18) 3.502(6) . 3_556 ? F(3) N(4) 3.599(4) . 1_545 ? F(4) C(9) 3.153(6) . 4_545 ? F(4) C(18) 3.473(6) . 2_546 ? F(5) C(10) 3.379(5) . 3_556 ? F(5) C(11) 3.424(5) . 3_556 ? F(5) C(6) 3.442(4) . 2_546 ? F(5) C(18) 3.450(7) . 2_546 ? F(5) C(18) 3.489(6) . 1_545 ? F(5) C(5) 3.563(5) . 2_546 ? F(6) C(18) 3.127(6) . 3_556 ? F(6) C(17) 3.356(4) . 3_556 ? F(6) C(11) 3.469(4) . 3_556 ? C(4) C(16) 3.526(5) . 4_555 ? C(5) C(18) 3.431(6) . 2_546 ? C(9) C(16) 3.560(5) . 4_455 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------