# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2003 data_global _journal_coden_Cambridge 0440 #=============================================================================== _audit_creation_date 17-07-03 loop_ _publ_author_name 'Mir Wais Hosseini' 'De Cian,Andre' 'Sylvie Ferlay' 'Marielle Loi' 'Phillipe Turek' _publ_contact_author_name 'Dr Mir Wais Hosseini' _publ_contact_author_address ; Laboratoire de Chimie de Coordination Organique Universite Louis Pasteur Institut Le Bel, 4 Strasbourg F-67000 FRANCE ; _publ_contact_author_email HOSSEINI@CHIMIE.U-STRASBG.FR _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Molecular tectonics: structural and magnetic properties of a discrete Copper binuclear complex and a 1-D coordination network ; _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. OpenMoleN, Interactive Intelligent Structure solution (1997) Nonius B.V., Delft, The Netherlands. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. Walker, N. & Stuart, D. (1983). Acta Cryst., A39, 158-166. ; #=============================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. data_st397 _database_code_CSD 215577 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C26 H30 Cl10 Cu2 N2 S4' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C26 H30 Cl10 Cu2 N2 S4' _chemical_formula_weight 980.41 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 Cl ? 0.132 0.159 International_Tables_Vol_IV_Table_2.3.1 Cu ? 0.263 1.266 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 S ? 0.110 0.124 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' 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 9.7076(3) _cell_length_b 12.6420(3) _cell_length_c 16.1419(3) _cell_angle_alpha 90 _cell_angle_beta 98.468(2) _cell_angle_gamma 90 _cell_volume 1959.39(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used 5011 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 28.1 _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.66 _exptl_crystal_density_method none _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 2.003 _exptl_absorpt_correction_type refdelf_(Walker_&_Stuart,_1983) _exptl_absorpt_correction_T_min 0.9661 _exptl_absorpt_correction_T_max 1.1543 #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 5011 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 36. mm. Scan angle = 1.6 deg 1 scans of 60 sec per frame. Data collection was divided into 1 set(s) with the following starting angles and number of frames : Set 1 Theta = 6.30 Omega = 0.00 Kappa = 0.00 115 frames Friedel pairs were averaged. Internal R = 0.02 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5011 _diffrn_reflns_av_R_equivalents 0.020 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 28.06 _reflns_number_total 3962 _reflns_number_gt 3042 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3042 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.043 _refine_ls_R_factor_gt 0.029 _refine_ls_wR_factor_all 0.066 _refine_ls_wR_factor_ref 0.060 _refine_ls_goodness_of_fit_all 1.388 _refine_ls_goodness_of_fit_ref 1.260 _refine_ls_shift/su_max 0.005 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 0.613 _refine_diff_density_min -0.557 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol CU 0.67514(3) 0.04039(3) 0.37422(2) 0.0333(2) Uani ? ? Cu CL1 0.89852(8) 0.10955(7) 0.34222(5) 0.0486(4) Uani ? ? Cl CL2 0.53169(8) 0.17848(7) 0.34110(5) 0.0531(4) Uani ? ? Cl S1 0.61908(9) -0.03819(6) 0.24171(5) 0.0442(4) Uani ? ? S C1 0.4698(4) -0.1189(3) 0.2519(3) 0.067(2) Uani ? ? C C2 0.7553(4) -0.1348(2) 0.2599(2) 0.042(2) Uani ? ? C C3 0.7823(3) -0.1717(2) 0.3494(2) 0.032(1) Uani ? ? C C4 0.8423(3) -0.2681(2) 0.3695(2) 0.034(1) Uani ? ? C C5 0.8682(3) -0.3003(2) 0.4533(2) 0.032(1) Uani ? ? C C6 0.8306(3) -0.2312(2) 0.5130(2) 0.033(1) Uani ? ? C C7 0.7736(3) -0.1347(2) 0.4895(2) 0.030(1) Uani ? ? C N 0.7489(2) -0.1044(2) 0.4088(1) 0.030(1) Uani ? ? N C8 0.7362(3) -0.0610(2) 0.5563(2) 0.042(2) Uani ? ? C S2 0.67212(8) 0.06605(6) 0.51843(5) 0.0412(4) Uani ? ? S C9 0.8227(5) 0.1478(3) 0.5481(3) 0.084(2) Uani ? ? C C10 0.9358(3) -0.4037(2) 0.4772(2) 0.032(1) Uani ? ? C C11 1.0536(3) -0.4345(2) 0.4446(2) 0.041(1) Uani ? ? C C12 0.8820(3) -0.4701(2) 0.5327(2) 0.041(2) Uani ? ? C C13 0.4434(4) -0.4114(4) 0.3340(2) 0.068(2) Uani ? ? C CL3 0.2816(1) -0.36835(9) 0.28211(6) 0.0687(6) Uani ? ? Cl CL4 0.4812(1) -0.3472(1) 0.43136(7) 0.0938(8) Uani ? ? Cl CL5 0.4439(2) -0.5491(1) 0.34579(9) 0.1096(8) Uani ? ? Cl H1 0.3881 -0.0764 0.2435 0.0908 Uiso calc C1 H H2 0.4620 -0.1737 0.2112 0.0908 Uiso calc C1 H H3 0.4804 -0.1491 0.3064 0.0908 Uiso calc C1 H H4 0.8385 -0.1045 0.2459 0.0577 Uiso calc C2 H H5 0.7297 -0.1941 0.2249 0.0577 Uiso calc C2 H H6 0.8663 -0.3130 0.3267 0.0458 Uiso calc C4 H H7 0.8445 -0.2510 0.5704 0.0431 Uiso calc C6 H H8 0.8172 -0.0501 0.5962 0.0555 Uiso calc C8 H H9 0.6664 -0.0940 0.5827 0.0555 Uiso calc C8 H H10 0.8016 0.2187 0.5312 0.1114 Uiso calc C9 H H11 0.8486 0.1454 0.6072 0.1114 Uiso calc C9 H H12 0.8976 0.1226 0.5217 0.1114 Uiso calc C9 H H13 1.0908 -0.3895 0.4062 0.0532 Uiso calc C11 H H14 0.8008 -0.4500 0.5552 0.0535 Uiso calc C12 H H15 0.5140 -0.3937 0.3014 0.0866 Uiso calc C13 H 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 _atom_site_aniso_type_symbol CU 0.0391(2) 0.0237(2) 0.0398(2) 0.0034(1) 0.0042(1) 0.0038(1) Cu CL1 0.0439(4) 0.0518(4) 0.0506(4) -0.0058(3) 0.0138(3) 0.0021(3) Cl CL2 0.0525(4) 0.0394(4) 0.0724(5) 0.0157(3) 0.0151(3) 0.0181(3) Cl S1 0.0675(5) 0.0341(4) 0.0374(4) 0.0073(3) -0.0058(4) 0.0078(3) S C1 0.065(2) 0.065(2) 0.072(2) -0.004(2) -0.014(2) -0.004(2) C C2 0.066(2) 0.039(2) 0.029(1) 0.009(1) 0.007(1) 0.004(1) C C3 0.041(1) 0.028(1) 0.030(1) 0.003(1) 0.005(1) 0.000(1) C C4 0.047(1) 0.027(1) 0.030(1) 0.005(1) 0.005(1) -0.002(1) C C5 0.035(1) 0.026(1) 0.035(1) 0.002(1) 0.001(1) 0.001(1) C C6 0.040(1) 0.029(1) 0.029(1) 0.002(1) 0.003(1) 0.003(1) C C7 0.032(1) 0.027(1) 0.032(1) 0.000(1) 0.002(1) -0.002(1) C N 0.035(1) 0.026(1) 0.029(1) 0.0011(9) 0.0044(8) 0.0014(8) N C8 0.055(2) 0.037(1) 0.037(1) 0.011(1) 0.010(1) -0.001(1) C S2 0.0495(4) 0.0307(3) 0.0461(4) 0.0063(3) 0.0134(3) -0.0036(3) S C9 0.118(3) 0.071(2) 0.070(2) -0.053(2) 0.020(2) -0.023(2) C C10 0.037(1) 0.025(1) 0.035(1) 0.003(1) -0.000(1) 0.000(1) C C11 0.048(2) 0.031(1) 0.045(1) 0.003(1) 0.014(1) 0.009(1) C C12 0.047(2) 0.034(2) 0.044(1) 0.006(1) 0.010(1) 0.005(1) C C13 0.059(2) 0.081(3) 0.065(2) 0.003(2) 0.026(2) 0.007(2) C CL3 0.0626(5) 0.0920(7) 0.0564(5) -0.0035(5) 0.0111(4) -0.0035(5) Cl CL4 0.0856(7) 0.138(1) 0.0701(6) -0.0030(8) -0.0074(6) -0.0038(7) Cl CL5 0.1199(8) 0.0798(8) 0.1378(9) 0.0211(7) 0.0723(6) 0.0231(6) Cl # 10. MOLECULAR GEOMETRY 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 CL1 2.4624(9) . . ? CU CL2 2.2480(8) . . ? CU S1 2.3485(9) . . ? CU N 2.014(2) . . ? CU S2 2.3549(8) . . ? S1 C1 1.799(5) . . ? S1 C2 1.792(3) . . ? C2 C3 1.504(4) . . ? C3 C4 1.369(4) . . ? C3 N 1.357(4) . . ? C4 C5 1.399(4) . . ? C5 C6 1.388(4) . . ? C5 C10 1.488(4) . . ? C6 C7 1.370(4) . . ? C7 N 1.346(4) . . ? C7 C8 1.509(4) . . ? C8 S2 1.796(3) . . ? S2 C9 1.797(4) . . ? C10 C11 1.383(4) . . ? C10 C12 1.385(4) . . ? C11 C12 1.383(4) . 3_746 ? C13 CL3 1.755(4) . . ? C13 CL4 1.759(5) . . ? C13 CL5 1.751(5) . . ? 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 ? ? ? ? ? ? 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 CL1 CU CL2 102.02(3) . . . ? CL1 CU S1 93.00(3) . . . ? CL1 CU N 95.33(7) . . . ? CL1 CU S2 107.34(3) . . . ? CL2 CU S1 93.42(3) . . . ? CL2 CU N 162.57(7) . . . ? CL2 CU S2 91.75(3) . . . ? S1 CU N 83.87(7) . . . ? S1 CU S2 157.47(4) . . . ? N CU S2 84.65(7) . . . ? C1 S1 C2 100.6(2) . . . ? S1 C2 C3 112.9(2) . . . ? C2 C3 C4 120.8(3) . . . ? C2 C3 N 117.3(2) . . . ? C4 C3 N 121.9(2) . . . ? C3 C4 C5 119.9(3) . . . ? C4 C5 C6 117.4(3) . . . ? C4 C5 C10 121.0(2) . . . ? C6 C5 C10 121.6(2) . . . ? C5 C6 C7 120.3(3) . . . ? C6 C7 N 121.9(2) . . . ? C6 C7 C8 118.9(2) . . . ? N C7 C8 119.2(2) . . . ? C3 N C7 118.6(2) . . . ? C7 C8 S2 114.7(2) . . . ? C8 S2 C9 101.3(2) . . . ? C5 C10 C11 120.4(3) . . . ? C5 C10 C12 120.4(3) . . . ? C11 C10 C12 119.2(3) . . . ? C10 C11 C12 120.7(3) . . 3_746 ? C10 C12 C11 120.1(3) . . 3_746 ? CL3 C13 CL4 109.8(2) . . . ? CL3 C13 CL5 110.4(3) . . . ? CL4 C13 CL5 111.4(2) . . . ? _diffrn_measured_fraction_theta_max 0.799 _diffrn_reflns_theta_full 28.06 _diffrn_measured_fraction_theta_full 0.799 data_st468 _database_code_CSD 215578 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C24 H28 B2 Cl2 Cu2 F8 N2 S4' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H28 B2 Cl2 Cu2 F8 N2 S4' _chemical_formula_weight 844.36 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 B ? 0.000 0.001 International_Tables_Vol_IV_Table_2.3.1 Cl ? 0.132 0.159 International_Tables_Vol_IV_Table_2.3.1 Cu ? 0.263 1.266 International_Tables_Vol_IV_Table_2.3.1 F ? 0.014 0.010 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 S ? 0.110 0.124 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' 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 32.475(3) _cell_length_b 13.496(2) _cell_length_c 8.7380(5) _cell_angle_alpha 90 _cell_angle_beta 96.335(6) _cell_angle_gamma 90 _cell_volume 3806.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 294 _cell_measurement_reflns_used 9265 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 27.5 _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.47 _exptl_crystal_density_method none _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 1.534 _exptl_absorpt_correction_type refdelf_(Walker_&_Stuart,_1983) _exptl_absorpt_correction_T_min 0.8875 _exptl_absorpt_correction_T_max 1.2211 #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 294 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 9265 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 35. mm. Scan angle = 2.0 deg 1 scans of 100 sec per frame. Data collection was divided into 2 set(s) with the following starting angles and number of frames : Set 1 Theta = 8.09 Omega = -114.50 Kappa = 180.00 72 frames Set 2 Theta = -5.70 Kappa = -111.90 Phi = -163.90 15 frames Friedel pairs were averaged. Internal R = 0.03 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 9265 _diffrn_reflns_av_R_equivalents 0.030 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.54 _reflns_number_total 4406 _reflns_number_gt 2330 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2330 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.117 _refine_ls_R_factor_gt 0.056 _refine_ls_wR_factor_all 0.196 _refine_ls_wR_factor_ref 0.094 _refine_ls_goodness_of_fit_all 1.218 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_shift/su_max 0.014 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 0.441 _refine_diff_density_min -0.280 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol CU 0.29341(3) 0.24120(7) 0.1338(1) 0.0386(5) Uani ? ? Cu CL 0.23347(6) 0.3135(2) 0.1733(2) 0.043(1) Uani ? ? Cl S1 0.32004(7) 0.3856(2) 0.0380(3) 0.048(1) Uani ? ? S C1 0.3607(3) 0.3242(7) -0.047(1) 0.056(5) Uani ? ? C C2 0.3745(3) 0.2275(6) 0.028(1) 0.041(4) Uani ? ? C N 0.3479(2) 0.1808(5) 0.1118(7) 0.032(3) Uani ? ? N C3 0.3583(2) 0.0916(6) 0.1737(9) 0.034(4) Uani ? ? C C4 0.3290(3) 0.0443(7) 0.275(1) 0.045(4) Uani ? ? C S2 0.27644(6) 0.0886(2) 0.2304(2) 0.039(1) Uani ? ? S C5 0.3458(5) 0.443(1) 0.207(1) 0.091(9) Uani ? ? C C6 0.2596(3) 0.1087(9) 0.418(1) 0.069(6) Uani ? ? C C7 0.4122(3) 0.1859(7) 0.003(1) 0.047(5) Uani ? ? C C8 0.4233(3) 0.0920(7) 0.063(1) 0.041(4) Uani ? ? C C9 0.3953(3) 0.0446(6) 0.149(1) 0.040(4) Uani ? ? C C10 0.4630(2) 0.0445(7) 0.031(1) 0.044(5) Uani ? ? C C11 0.4657(3) -0.0561(8) 0.019(1) 0.059(6) Uani ? ? C C12 0.4973(3) 0.1006(8) 0.013(1) 0.065(6) Uani ? ? C B 0.3729(5) 0.260(1) 0.537(2) 0.083(9) Uani ? ? B F1 0.3818(6) 0.3389(9) 0.606(1) 0.22(1) Uani ? ? F F2 0.3325(3) 0.2788(9) 0.452(1) 0.170(9) Uani ? ? F F3 0.3682(4) 0.1831(7) 0.628(1) 0.134(7) Uani ? ? F F4 0.3965(3) 0.2436(7) 0.422(1) 0.131(7) Uani ? ? F H1 0.3839 0.3673 -0.0414 0.0710 Uiso calc C1 H H2 0.3513 0.3115 -0.1523 0.0710 Uiso calc C1 H H3 0.3381 0.0592 0.3792 0.0574 Uiso calc C4 H H4 0.3294 -0.0254 0.2600 0.0574 Uiso calc C4 H H5 0.3261 0.4776 0.2595 0.1305 Uiso calc C5 H H6 0.3590 0.3936 0.2726 0.1305 Uiso calc C5 H H7 0.3660 0.4881 0.1779 0.1305 Uiso calc C5 H H8 0.2319 0.1324 0.4061 0.0875 Uiso calc C6 H H9 0.2610 0.0480 0.4732 0.0875 Uiso calc C6 H H10 0.2771 0.1562 0.4723 0.0875 Uiso calc C6 H H11 0.4307 0.2213 -0.0539 0.0611 Uiso calc C7 H H12 0.4014 -0.0195 0.1907 0.0535 Uiso calc C9 H H13 0.4423 -0.0961 0.0324 0.0826 Uiso calc C11 H H14 0.4959 0.1707 0.0214 0.0917 Uiso calc C12 H 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 _atom_site_aniso_type_symbol CU 0.0368(4) 0.0325(5) 0.0479(5) 0.0096(4) 0.0154(4) 0.0061(5) Cu CL 0.042(1) 0.044(1) 0.042(1) 0.0149(9) 0.0130(8) -0.0012(9) Cl S1 0.050(1) 0.037(1) 0.060(1) 0.011(1) 0.0196(9) 0.011(1) S C1 0.049(5) 0.050(5) 0.069(5) 0.009(4) 0.029(4) 0.021(4) C C2 0.039(4) 0.037(4) 0.047(4) 0.007(4) 0.008(3) 0.004(4) C N 0.033(3) 0.029(3) 0.035(3) 0.004(3) 0.008(3) 0.000(3) N C3 0.035(4) 0.029(4) 0.039(4) 0.008(3) 0.003(3) -0.000(3) C C4 0.044(4) 0.042(5) 0.048(5) 0.011(4) 0.013(4) 0.011(4) C S2 0.038(1) 0.036(1) 0.043(1) 0.0034(9) 0.0081(8) 0.0035(9) S C5 0.17(1) 0.062(7) 0.075(8) -0.038(8) 0.017(8) -0.018(6) C C6 0.070(6) 0.079(7) 0.059(5) 0.013(5) 0.034(4) 0.023(5) C C7 0.036(4) 0.047(5) 0.061(5) 0.004(4) 0.016(4) 0.007(4) C C8 0.035(4) 0.041(5) 0.049(5) 0.006(4) 0.007(3) -0.004(4) C C9 0.038(4) 0.034(4) 0.051(5) 0.007(4) 0.001(4) 0.001(4) C C10 0.028(4) 0.050(5) 0.060(5) 0.010(4) 0.006(4) -0.000(5) C C11 0.038(5) 0.051(6) 0.104(7) 0.004(5) 0.019(5) -0.005(6) C C12 0.051(5) 0.044(6) 0.121(8) 0.009(5) 0.027(5) -0.004(6) C B 0.12(1) 0.057(8) 0.087(9) 0.025(7) 0.023(8) -0.020(7) B F1 0.66(3) 0.123(7) 0.126(6) -0.13(1) 0.14(1) -0.069(6) F F2 0.124(7) 0.166(9) 0.24(1) 0.027(7) 0.052(7) 0.076(8) F F3 0.22(1) 0.089(6) 0.122(6) 0.037(7) 0.028(6) 0.033(5) F F4 0.152(7) 0.150(8) 0.097(5) 0.051(6) 0.023(5) -0.020(5) F # 10. MOLECULAR GEOMETRY 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 CL 2.237(2) . . ? CU S1 2.326(3) . . ? CU N 1.975(6) . . ? CU S2 2.316(2) . . ? S1 C1 1.789(9) . . ? S1 C5 1.79(1) . . ? C1 C2 1.51(1) . . ? C2 N 1.35(1) . . ? C2 C7 1.38(1) . . ? N C3 1.35(1) . . ? C3 C4 1.51(1) . . ? C3 C9 1.39(1) . . ? C4 S2 1.808(9) . . ? S2 C6 1.80(1) . . ? C7 C8 1.40(1) . . ? C8 C9 1.40(1) . . ? C8 C10 1.49(1) . . ? C10 C11 1.37(1) . . ? C10 C12 1.38(1) . . ? C11 C12 1.40(1) . 3_655 ? B F1 1.24(2) . . ? B F2 1.45(2) . . ? B F3 1.33(2) . . ? B F4 1.35(2) . . ? 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 ? ? ? ? ? ? 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 CU S1 93.19(9) . . . ? CL CU N 176.3(2) . . . ? CL CU S2 94.84(9) . . . ? S1 CU N 86.4(2) . . . ? S1 CU S2 171.79(9) . . . ? N CU S2 85.5(2) . . . ? C1 S1 C5 104.1(7) . . . ? S1 C1 C2 114.6(6) . . . ? C1 C2 N 117.7(7) . . . ? C1 C2 C7 120.5(8) . . . ? N C2 C7 121.7(8) . . . ? C2 N C3 119.2(7) . . . ? N C3 C4 117.8(7) . . . ? N C3 C9 121.7(8) . . . ? C4 C3 C9 120.4(8) . . . ? C3 C4 S2 112.1(6) . . . ? C4 S2 C6 103.2(5) . . . ? C2 C7 C8 120.3(8) . . . ? C7 C8 C9 117.2(8) . . . ? C7 C8 C10 120.9(8) . . . ? C9 C8 C10 122.0(8) . . . ? C3 C9 C8 119.9(8) . . . ? C8 C10 C11 120.4(9) . . . ? C8 C10 C12 121.0(9) . . . ? C11 C10 C12 118.6(9) . . . ? C10 C11 C12 120(1) . . 3_655 ? C10 C12 C11 120(1) . . 3_655 ? F1 B F2 104(1) . . . ? F1 B F3 114(1) . . . ? F1 B F4 112(1) . . . ? F2 B F3 106(1) . . . ? F2 B F4 101(1) . . . ? F3 B F4 115(1) . . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.963