# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 1145/200 #=============================================================================== data_global #=============================================================================== _audit_creation_date 18-07-98 # 1. SUBMISSION DETAILS _publ_contact_author ; Le Moustarder Soazig Laboratoire IMMO, universite d'Angers 2, Bd Lavoisier - 49045 Angers cedex France ; _publ_contact_author_phone (33)2-41-73-53-68 _publ_contact_author_fax (33)2-41-73-54-05 _publ_contact_author_email lemousta@univ-angers.fr _publ_requested_journal ' Journal of Materials Chemistry' _publ_requested_coeditor_name ; P. Hudhomme, C. Durand, N. Mercier, M.T. Azcondo,P. Delhaes, A. Riou, A. Gorgues ; #=============================================================== data_(D1)3.(ClO4)2 #(1) #=============================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C15H12O4S12Cl' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C15H12O4S12Cl' _chemical_formula_weight 676.48 _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 O 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 S 0.110 0.124 International_Tables_Vol_IV_Table_2.3.1 Cl 0.132 0.159 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 '' 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 11.953(4) _cell_length_b 14.701(2) _cell_length_c 13.917(4) _cell_angle_alpha 90 _cell_angle_beta 93.77(2) _cell_angle_gamma 90 _cell_volume 2440(1) _cell_formula_units_z 4 _cell_measurement_temperature 294 _cell_measurement_reflns_used 25 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; ? ; _exptl_crystal_description prism _exptl_crystal_colour 'black' _exptl_crystal_size_max 1.60 _exptl_crystal_size_mid 1.08 _exptl_crystal_size_min 0.71 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.86 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 1372 _exptl_absorpt_coefficient_mu 1.182 _exptl_absorpt_correction_type refined_empirical_(Walker_&_Stuart,_1983) _exptl_absorpt_correction_T_min 0.5334 _exptl_absorpt_correction_T_max 1.0000 #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 294 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device Enraf_Nonius_CAD4 _diffrn_measurement_method \q/2\q _diffrn_standards_number 3 _diffrn_standards_interval_count - _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -6 -4 -1 -3 -6 7 -5 7 -3 _diffrn_reflns_number 5719 _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 26.98 _reflns_number_total 5209 _reflns_number_observed 3910 _reflns_observed_criterion >3.0\s(I) _computing_data_collection 'CAD4_(Enraf-Nonius,_1994)' _computing_cell_refinement CAD4_(Enraf-Nonius,_1994) _computing_data_reduction 'process_MolEN_(Fair,_1990)' _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_MolEN_(Fair,_1990) _computing_molecular_graphics ? _computing_publication_material BTABLE_PTABLE_CIF_IN_MolEN_(Fair,_1990) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '4Fo^2^/(\s^2^(Fo^2^) + 0.0036 Fo^4^)' _refine_ls_hydrogen_treatment included_not_refined _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3910 _refine_ls_number_parameters 307 _refine_ls_number_restraints 32 _refine_ls_number_constraints 0 _refine_ls_abs_structure_details ; ? ; _refine_ls_R_factor_all 0.067 _refine_ls_R_factor_obs 0.051 _refine_ls_wR_factor_all 0.086 _refine_ls_wR_factor_obs 0.080 _refine_ls_goodness_of_fit_all 2.229 _refine_ls_goodness_of_fit_obs 2.122 _refine_ls_shift/esd_max 0.026 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 0.860 _refine_diff_density_min -1.459 #=============================================================================== # 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_occupancy _atom_site_thermal_displace_type _atom_site_type_symbol CL 0.2243(1) -0.36647(7) 0.97506(8) 0.0462(5) 1.000 Uij Cl S1A 0.3533(1) 0.8504(1) 0.2206(1) 0.0528(8) 0.750 Uij S S1B 0.2607(7) 0.8637(5) 0.2289(5) 0.097(4) 0.250 Uij S S2A 0.2967(1) 0.9363(1) 0.3226(1) 0.0517(8) 0.750 Uij S S2B 0.3984(6) 0.8961(4) 0.3144(5) 0.080(4) 0.250 Uij S S3 0.23858(9) 0.60774(8) 0.36570(7) 0.0409(5) 1.000 Uij S S4 0.3081(1) 0.71536(7) 0.53513(7) 0.0414(5) 1.000 Uij S S5 0.1558(1) 0.44721(8) 0.50689(7) 0.0426(5) 1.000 Uij S S6 0.2049(1) 0.56478(7) 0.67416(7) 0.0428(5) 1.000 Uij S S7 0.0741(1) 0.25774(8) 0.72956(9) 0.0513(6) 1.000 Uij S S8 0.0073(1) 0.35679(9) 0.81239(8) 0.0492(6) 1.000 Uij S S9 0.5364(1) 0.7138(1) 0.14001(9) 0.0589(7) 1.000 Uij S S10 0.5893(1) 0.5905(1) 0.0904(1) 0.0621(7) 1.000 Uij S S11 0.56191(9) 0.62544(7) 0.43888(8) 0.0400(5) 1.000 Uij S S12 0.4810(1) 0.45719(7) 0.34970(8) 0.0452(6) 1.000 Uij S O1 0.2769(4) -0.3783(3) 0.8865(3) 0.119(3) 1.000 Uij O O2 0.1130(4) -0.3895(5) 0.9557(5) 0.143(4) 1.000 Uij O O3 0.2377(5) -0.2750(3) 1.0100(3) 0.093(3) 1.000 Uij O O4 0.2697(6) -0.4209(4) 1.0469(4) 0.137(4) 1.000 Uij O C1 0.2648(4) 0.7511(3) 0.2410(3) 0.047(2) 1.000 Uij C C2 0.3436(4) 0.8701(3) 0.4298(3) 0.054(3) 1.000 Uij C C3 0.2729(3) 0.7214(3) 0.3448(3) 0.037(2) 1.000 Uij C C4 0.3055(3) 0.7728(3) 0.4248(3) 0.036(2) 1.000 Uij C C5 0.2478(3) 0.6159(3) 0.4916(3) 0.036(2) 1.000 Uij C C6 0.2066(3) 0.5504(3) 0.5500(3) 0.036(2) 1.000 Uij C C7 0.1144(3) 0.4068(3) 0.6189(3) 0.037(2) 1.000 Uij C C8 0.1358(3) 0.4606(3) 0.6938(3) 0.039(2) 1.000 Uij C C9 0.0609(4) 0.3153(3) 0.6144(3) 0.044(2) 1.000 Uij C C10 0.1118(4) 0.4450(3) 0.7980(3) 0.048(2) 1.000 Uij C C11 0.5985(4) 0.7048(3) 0.2650(3) 0.049(3) 1.000 Uij C C12 0.5131(4) 0.5167(3) 0.1653(3) 0.051(2) 1.000 Uij C C13 0.5594(3) 0.6199(3) 0.3129(3) 0.037(2) 1.000 Uij C C14 0.5239(3) 0.5417(3) 0.2716(3) 0.042(2) 1.000 Uij C C15 0.5099(4) 0.5176(3) 0.4548(3) 0.040(2) 1.000 Uij C H1 0.1803 0.4285 0.8329 0.0624 1.000 Uiso H H2 0.0850 0.5009 0.8248 0.0624 1.000 Uiso H H3 -0.0182 0.3207 0.5944 0.0574 1.000 Uiso H H4 0.0953 0.2787 0.5664 0.0574 1.000 Uiso H H5 0.5762 0.7564 0.3001 0.0658 1.000 Uiso H H6 0.6781 0.7034 0.2628 0.0658 1.000 Uiso H H7 0.5404 0.4562 0.1585 0.0677 1.000 Uiso H H8 0.4349 0.5180 0.1437 0.0677 1.000 Uiso 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 CL 0.0435(6) 0.0461(5) 0.0491(5) 0.0043(5) -0.0016(5) -0.0035(4) Cl S1A 0.0544(9) 0.0595(9) 0.0456(7) -0.0011(8) 0.0161(7) 0.0133(7) S S1B 0.096(5) 0.105(4) 0.091(4) 0.001(4) -0.008(4) 0.053(3) S S2A 0.059(1) 0.0444(7) 0.0528(8) 0.0105(7) 0.0053(8) 0.0129(6) S S2B 0.082(4) 0.069(3) 0.089(4) -0.019(3) 0.023(3) 0.018(3) S S3 0.0410(6) 0.0461(5) 0.0361(5) 0.0013(5) -0.0015(4) -0.0015(4) S S4 0.0483(6) 0.0419(5) 0.0351(5) -0.0018(5) 0.0016(5) -0.0011(4) S S5 0.0469(6) 0.0446(5) 0.0370(5) -0.0018(5) 0.0006(5) -0.0035(4) S S6 0.0533(7) 0.0389(5) 0.0378(5) -0.0043(5) 0.0022(5) -0.0025(4) S S7 0.0542(7) 0.0454(6) 0.0549(6) -0.0019(5) 0.0054(6) 0.0067(5) S S8 0.0377(6) 0.0631(7) 0.0502(6) -0.0035(5) 0.0078(5) 0.0019(5) S S9 0.0499(7) 0.0650(8) 0.0628(7) 0.0020(6) 0.0095(6) 0.0105(6) S S10 0.0484(7) 0.0816(9) 0.0605(7) -0.0000(7) 0.0178(6) -0.0057(7) S S11 0.0347(5) 0.0338(5) 0.0545(6) -0.0002(4) -0.0030(5) -0.0075(4) S S12 0.0509(7) 0.0372(5) 0.0488(5) -0.0032(5) -0.0076(5) -0.0056(4) S O1 0.174(4) 0.095(3) 0.101(3) -0.022(3) 0.075(3) -0.029(2) O O2 0.046(3) 0.256(5) 0.250(5) -0.012(4) -0.015(3) -0.156(4) O O3 0.146(4) 0.055(2) 0.102(3) 0.003(3) 0.026(3) -0.023(2) O O4 0.209(5) 0.090(3) 0.136(4) 0.024(4) -0.052(4) 0.042(3) O C1 0.042(3) 0.062(3) 0.039(2) -0.005(2) -0.004(2) 0.011(2) C C2 0.065(3) 0.049(2) 0.051(2) -0.004(2) 0.008(2) 0.010(2) C C3 0.027(2) 0.050(2) 0.040(2) 0.004(2) 0.004(2) 0.007(2) C C4 0.029(2) 0.046(2) 0.036(2) -0.000(2) 0.002(2) 0.005(2) C C5 0.029(2) 0.042(2) 0.038(2) 0.003(2) 0.003(2) -0.000(2) C C6 0.034(2) 0.036(2) 0.038(2) 0.006(2) -0.003(2) 0.001(2) C C7 0.030(2) 0.042(2) 0.039(2) 0.005(2) 0.001(2) -0.000(2) C C8 0.032(2) 0.041(2) 0.045(2) 0.004(2) 0.001(2) 0.005(2) C C9 0.040(2) 0.046(2) 0.045(2) 0.001(2) 0.003(2) 0.000(2) C C10 0.051(3) 0.052(2) 0.041(2) -0.009(2) 0.001(2) -0.000(2) C C11 0.034(2) 0.050(2) 0.066(3) -0.001(2) 0.008(2) 0.004(2) C C12 0.047(3) 0.055(3) 0.053(2) -0.005(2) 0.008(2) -0.006(2) C C13 0.023(2) 0.040(2) 0.056(2) 0.004(2) 0.002(2) -0.003(2) C C14 0.028(2) 0.049(2) 0.054(2) 0.001(2) 0.000(2) -0.002(2) C C15 0.031(2) 0.036(2) 0.055(2) 0.004(2) -0.009(2) -0.003(2) C # 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 CL O1 1.430(5) . . ? CL O2 1.382(5) . . ? CL O3 1.435(4) . . ? CL O4 1.366(6) . . ? S1A S1B 1.137(8) . . ? S1A S2A 2.048(2) . . ? S1A S2B 1.534(7) . . ? S1A C1 1.836(5) . . ? S1B S2A 1.717(7) . . ? S1B S2B 2.02(1) . . ? S1B C1 1.665(9) . . ? S2A S2B 1.364(7) . . ? S2A C2 1.838(5) . . ? S2B C2 1.815(8) . . ? S3 C3 1.749(4) . . ? S3 C5 1.752(4) . . ? S4 C4 1.751(4) . . ? S4 C5 1.723(4) . . ? S5 C6 1.727(4) . . ? S5 C7 1.768(4) . . ? S6 C6 1.742(4) . . ? S6 C8 1.769(4) . . ? S7 S8 2.051(2) . . ? S7 C9 1.810(4) . . ? S8 C10 1.821(5) . . ? S9 S10 2.053(2) . . ? S9 C11 1.850(5) . . ? S10 C12 1.793(5) . . ? S11 C13 1.753(5) . . ? S11 C15 1.722(4) . . ? S12 C14 1.751(5) . . ? S12 C15 1.726(4) . . ? C1 C3 1.505(6) . . ? C2 C4 1.502(6) . . ? C3 C4 1.381(6) . . ? C5 C6 1.372(6) . . ? C7 C8 1.321(6) . . ? C7 C9 1.489(6) . . ? C8 C10 1.514(6) . . ? C11 C13 1.505(6) . . ? C12 C14 1.521(6) . . ? C13 C14 1.341(6) . . ? 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 O1 CL O2 105.9(3) . . . ? O1 CL O3 111.1(3) . . . ? O1 CL O4 112.6(3) . . . ? O2 CL O3 112.3(4) . . . ? O2 CL O4 109.3(4) . . . ? O3 CL O4 105.7(3) . . . ? S1B S1A S2A 57.0(4) . . . ? S1B S1A S2B 97.3(4) . . . ? S1B S1A C1 63.1(4) . . . ? S2A S1A S2B 41.8(3) . . . ? S2A S1A C1 99.4(2) . . . ? S2B S1A C1 113.0(3) . . . ? S1A S1B S2A 89.3(5) . . . ? S1A S1B S2B 48.8(3) . . . ? S1A S1B C1 79.4(5) . . . ? S2A S1B S2B 41.8(3) . . . ? S2A S1B C1 122.5(4) . . . ? S2B S1B C1 99.1(4) . . . ? S1A S2A S1B 33.7(3) . . . ? S1A S2A S2B 48.5(3) . . . ? S1A S2A C2 98.0(2) . . . ? S1B S2A S2B 81.2(4) . . . ? S1B S2A C2 109.6(3) . . . ? S2B S2A C2 67.2(3) . . . ? S1A S2B S1B 33.9(3) . . . ? S1A S2B S2A 89.7(4) . . . ? S1A S2B C2 122.2(4) . . . ? S1B S2B S2A 57.0(3) . . . ? S1B S2B C2 98.3(4) . . . ? S2A S2B C2 69.0(3) . . . ? C3 S3 C5 95.8(2) . . . ? C4 S4 C5 96.8(2) . . . ? C6 S5 C7 95.8(2) . . . ? C6 S6 C8 94.8(2) . . . ? S8 S7 C9 98.7(2) . . . ? S7 S8 C10 98.5(2) . . . ? S10 S9 C11 98.0(2) . . . ? S9 S10 C12 99.2(2) . . . ? C13 S11 C15 95.9(2) . . . ? C14 S12 C15 96.3(2) . . . ? S1A C1 S1B 37.5(3) . . . ? S1A C1 C3 112.2(3) . . . ? S1B C1 C3 112.7(4) . . . ? S2A C2 S2B 43.8(2) . . . ? S2A C2 C4 113.0(3) . . . ? S2B C2 C4 106.6(4) . . . ? S3 C3 C1 115.8(3) . . . ? S3 C3 C4 116.4(3) . . . ? C1 C3 C4 127.7(4) . . . ? S4 C4 C2 115.5(3) . . . ? S4 C4 C3 115.6(3) . . . ? C2 C4 C3 128.8(4) . . . ? S3 C5 S4 114.0(2) . . . ? S3 C5 C6 122.9(3) . . . ? S4 C5 C6 123.0(3) . . . ? S5 C6 S6 115.1(2) . . . ? S5 C6 C5 122.8(3) . . . ? S6 C6 C5 122.1(3) . . . ? S5 C7 C8 116.3(3) . . . ? S5 C7 C9 114.3(3) . . . ? C8 C7 C9 129.4(4) . . . ? S6 C8 C7 117.7(3) . . . ? S6 C8 C10 113.5(3) . . . ? C7 C8 C10 128.8(4) . . . ? S7 C9 C7 111.9(3) . . . ? S8 C10 C8 112.8(3) . . . ? S9 C11 C13 111.0(3) . . . ? S10 C12 C14 113.9(3) . . . ? S11 C13 C11 114.8(3) . . . ? S11 C13 C14 116.9(3) . . . ? C11 C13 C14 128.3(4) . . . ? S12 C14 C12 115.0(3) . . . ? S12 C14 C13 116.0(3) . . . ? C12 C14 C13 128.9(4) . . . ? S11 C15 S12 114.8(2) . . . ? #===END#===END#===END#===END#===END#===END#===END#===END#===END#===END#===END data_(D1)3(BF4)2 #(2) #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C15H12BF4S12' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C15H12BF4S12' _chemical_formula_weight 663.84 _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 F ? 0.014 0.010 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 11.910(8) _cell_length_b 14.579(8) _cell_length_c 13.771(2) _cell_angle_alpha 90 _cell_angle_beta 94.28(2) _cell_angle_gamma 90 _cell_volume 2384(3) _cell_formula_units_z 4 _cell_measurement_temperature 294 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; ? ; _exptl_crystal_description prism _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.91 _exptl_crystal_size_mid 0.54 _exptl_crystal_size_min 0.51 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.85 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 1340 _exptl_absorpt_coefficient_mu 1.094 _exptl_absorpt_correction_type refined_empirical_(Walker_&_Stuart,_1983) _exptl_absorpt_correction_T_min 0.7034 _exptl_absorpt_correction_T_max 1.0000 #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 294 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device Enraf_Nonius_CAD4 _diffrn_measurement_method \q/2\q _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 7 -2 -1 5 -6 1 8 -1 _diffrn_reflns_number 4589 _diffrn_reflns_av_R_equivalents 0.031 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -2 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 24.97 _reflns_number_total 4474 _reflns_number_observed 3407 _reflns_observed_criterion >3.0\s(I) _computing_data_collection 'CAD4_(Enraf-Nonius,_1994)' _computing_cell_refinement CAD4_(Enraf-Nonius,_1994) _computing_data_reduction 'process_MolEN_(Fair,_1990)' _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_MolEN_(Fair,_1990) _computing_molecular_graphics 'Diamond package' _computing_publication_material BTABLE_PTABLE_CIF_IN_MolEN_(Fair,_1990) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme unit _refine_ls_hydrogen_treatment included_not_refined _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3407 _refine_ls_number_parameters 307 _refine_ls_number_restraints 48 _refine_ls_number_constraints 0 _refine_ls_abs_structure_details ; ? ; _refine_ls_R_factor_all 0.065 _refine_ls_R_factor_obs 0.048 _refine_ls_wR_factor_all 0.061 _refine_ls_wR_factor_obs 0.050 _refine_ls_goodness_of_fit_all 2.354 _refine_ls_goodness_of_fit_obs 2.012 _refine_ls_shift/esd_max 1.058 _refine_ls_shift/esd_mean 0.017 _refine_diff_density_max 0.712 _refine_diff_density_min -0.452 #=============================================================================== # 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_occupancy _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol S1A 0.7024(2) 0.0600(1) 0.6774(1) 0.0546(9) 0.860 Uij ? ? S S1B 0.607(2) 0.102(1) 0.692(2) 0.13(1) 0.140 Uij ? ? S S2A 0.6475(2) 0.1459(1) 0.7799(1) 0.0563(9) 0.860 Uij ? ? S S2B 0.741(2) 0.147(3) 0.772(2) 0.17(2) 0.140 Uij ? ? S S3 0.6892(1) 0.2806(1) 0.4642(1) 0.0443(7) 1.000 Uij ? ? S S4 0.7604(1) 0.3895(1) 0.6343(1) 0.0433(7) 1.000 Uij ? ? S S5 0.7931(1) 0.43207(9) 0.3252(1) 0.0444(7) 1.000 Uij ? ? S S6 0.8431(1) 0.5507(1) 0.4928(1) 0.0447(7) 1.000 Uij ? ? S S7 0.4934(1) -0.1394(1) 0.6883(1) 0.0507(8) 1.000 Uij ? ? S S8 0.4275(1) -0.2400(1) 0.7699(1) 0.0526(8) 1.000 Uij ? ? S S9 0.4635(1) 0.2860(1) 0.8609(1) 0.0572(8) 1.000 Uij ? ? S S10 0.4106(1) 0.4094(1) 0.9100(1) 0.0597(9) 1.000 Uij ? ? S S11 0.4376(1) 0.37409(9) 0.5611(1) 0.0382(6) 1.000 Uij ? ? S S12 0.5210(1) 0.54308(9) 0.6509(1) 0.0429(7) 1.000 Uij ? ? S F1 0.2583(4) 0.2217(3) 0.4927(3) 0.100(3) 1.000 Uij ? ? F F2 0.2167(5) 0.1242(4) 0.6086(3) 0.121(3) 1.000 Uij ? ? F F3 0.2330(6) 0.0788(4) 0.4610(4) 0.145(4) 1.000 Uij ? ? F F4 0.3819(4) 0.1188(5) 0.5491(4) 0.138(4) 1.000 Uij ? ? F C1 0.6553(5) 0.1253(4) 0.5698(4) 0.049(3) 1.000 Uij ? ? C C2 0.7356(5) 0.2469(4) 0.7595(4) 0.052(3) 1.000 Uij ? ? C C3 0.6924(4) 0.2240(4) 0.5760(4) 0.039(3) 1.000 Uij ? ? C C4 0.7251(4) 0.2745(4) 0.6544(4) 0.039(3) 1.000 Uij ? ? C C5 0.7508(4) 0.3811(4) 0.5096(4) 0.041(3) 1.000 Uij ? ? C C6 0.7911(4) 0.4463(4) 0.4500(4) 0.040(3) 1.000 Uij ? ? C C7 0.3630(4) -0.0351(4) 0.8054(4) 0.040(3) 1.000 Uij ? ? C C8 0.3856(4) -0.0900(4) 0.8820(4) 0.038(3) 1.000 Uij ? ? C C9 0.3889(5) -0.0518(4) 0.7016(4) 0.049(3) 1.000 Uij ? ? C C10 0.4389(4) -0.1825(4) 0.8850(4) 0.045(3) 1.000 Uij ? ? C C11 0.4029(4) 0.2955(4) 0.7382(4) 0.048(3) 1.000 Uij ? ? C C12 0.4889(5) 0.4826(4) 0.8349(4) 0.051(3) 1.000 Uij ? ? C C13 0.4409(4) 0.3795(4) 0.6877(4) 0.037(3) 1.000 Uij ? ? C C14 0.4786(4) 0.4584(4) 0.7290(4) 0.040(3) 1.000 Uij ? ? C C15 0.4893(4) 0.4823(3) 0.5452(4) 0.036(2) 1.000 Uij ? ? C B 0.2738(6) 0.1354(5) 0.5274(5) 0.048(3) 1.000 Uij ? ? B H1 0.3226 0.2963 0.7375 0.0632 0.860 Uiso calc C11 H H2 0.4238 0.2424 0.7013 0.0632 0.860 Uiso calc C11 H H3 0.5673 0.4800 0.8576 0.0671 0.860 Uiso calc C12 H H4 0.4641 0.5447 0.8422 0.0671 0.860 Uiso calc C12 H H5 0.9083 0.7189 0.4321 0.0608 1.000 Uiso calc ? H H6 1.0192 0.6739 0.4036 0.0608 1.000 Uiso calc ? H H7 0.9123 0.4968 0.1740 0.0642 1.000 Uiso calc ? H H8 0.8194 0.5716 0.1660 0.0642 1.000 Uiso calc ? H H9 0.5671 0.4799 0.8577 0.0665 1.000 Uiso calc C12 H H10 0.4639 0.5446 0.8421 0.0665 1.000 Uiso calc C12 H H11 0.3224 0.2964 0.7384 0.0637 1.000 Uiso calc C11 H H12 0.4232 0.2423 0.7020 0.0637 1.000 Uiso calc C11 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 S1A 0.059(1) 0.0483(9) 0.0570(9) 0.0117(8) 0.0072(8) 0.0145(8) S S1B 0.16(2) 0.08(1) 0.16(2) -0.01(1) 0.06(1) 0.02(1) S S2A 0.061(1) 0.062(1) 0.0470(8) -0.0012(9) 0.0160(8) 0.0139(8) S S2B 0.14(2) 0.31(3) 0.11(1) 0.06(2) 0.01(1) 0.08(2) S S3 0.0498(7) 0.0445(7) 0.0393(6) -0.0022(6) 0.0026(6) 0.0006(6) S S4 0.0418(7) 0.0484(7) 0.0402(6) 0.0015(6) 0.0003(6) -0.0009(6) S S5 0.0558(8) 0.0390(7) 0.0402(6) -0.0024(7) 0.0021(6) -0.0025(6) S S6 0.0482(7) 0.0468(7) 0.0396(6) -0.0030(7) 0.0009(6) -0.0044(6) S S7 0.0406(7) 0.0608(9) 0.0528(7) 0.0027(7) 0.0075(6) -0.0013(7) S S8 0.0552(8) 0.0444(7) 0.0594(8) 0.0021(7) 0.0068(7) -0.0058(7) S S9 0.0541(8) 0.0614(9) 0.0565(8) 0.0007(8) 0.0087(7) 0.0083(7) S S10 0.0504(8) 0.076(1) 0.0556(8) -0.0017(8) 0.0170(7) -0.0066(8) S S11 0.0349(6) 0.0328(6) 0.0487(7) -0.0014(6) -0.0027(6) -0.0051(6) S S12 0.0489(7) 0.0353(6) 0.0458(7) -0.0045(6) -0.0068(6) -0.0054(6) S F1 0.135(4) 0.063(2) 0.115(3) 0.000(3) 0.028(3) 0.023(2) F F2 0.155(4) 0.103(3) 0.110(3) 0.009(3) 0.066(3) 0.023(3) F F3 0.185(5) 0.112(4) 0.146(4) -0.016(4) -0.035(4) -0.061(3) F F4 0.053(3) 0.266(6) 0.188(5) 0.019(4) -0.006(3) 0.121(4) F C1 0.051(3) 0.045(3) 0.050(3) -0.003(3) 0.006(3) 0.012(3) C C2 0.048(3) 0.062(3) 0.046(3) -0.006(3) 0.001(3) 0.015(3) C C3 0.032(2) 0.048(3) 0.040(2) 0.006(2) 0.007(2) 0.009(2) C C4 0.029(2) 0.047(3) 0.043(3) 0.002(2) 0.003(2) 0.005(2) C C5 0.038(3) 0.043(3) 0.042(3) 0.005(2) 0.000(2) -0.000(2) C C6 0.038(3) 0.043(3) 0.039(2) 0.007(2) 0.001(2) -0.001(2) C C7 0.038(3) 0.041(3) 0.042(3) 0.000(2) -0.000(2) -0.002(2) C C8 0.031(2) 0.044(3) 0.041(3) -0.004(2) -0.001(2) -0.001(2) C C9 0.050(3) 0.052(3) 0.045(3) 0.007(3) 0.002(3) -0.000(3) C C10 0.035(3) 0.048(3) 0.052(3) -0.002(3) 0.001(2) 0.004(3) C C11 0.031(3) 0.051(3) 0.068(3) 0.000(3) 0.007(3) -0.003(3) C C12 0.044(3) 0.056(3) 0.055(3) 0.003(3) 0.002(3) -0.009(3) C C13 0.027(2) 0.040(3) 0.048(3) 0.002(2) 0.003(2) -0.002(2) C C14 0.028(2) 0.047(3) 0.048(3) 0.001(2) -0.001(2) -0.004(2) C C15 0.030(2) 0.032(2) 0.050(3) 0.004(2) -0.008(2) -0.006(2) C B 0.046(3) 0.044(3) 0.053(3) -0.002(3) 0.001(3) 0.001(3) B # 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 S1A S1B 1.32(2) . . ? S1A S2A 2.031(3) . . ? S1A S2B 1.85(3) . . ? S1A C1 1.814(6) . . ? S1B S2A 1.43(2) . . ? S1B S2B 1.99(3) . . ? S1B C1 1.85(2) . . ? S2A S2B 1.13(3) . . ? S2A C2 1.842(6) . . ? S2B C2 1.47(4) . . ? S3 C3 1.745(5) . . ? S3 C5 1.734(5) . . ? S4 C4 1.755(5) . . ? S4 C5 1.717(5) . . ? S5 C6 1.733(5) . . ? S5 C7 1.748(5) . 4_554 ? S6 C6 1.730(5) . . ? S6 C8 1.740(5) . 4_554 ? S7 S8 2.039(2) . . ? S7 C9 1.802(6) . . ? S8 C10 1.789(6) . . ? S9 S10 2.039(2) . . ? S9 C11 1.793(6) . . ? S10 C12 1.795(6) . . ? S11 C13 1.742(5) . . ? S11 C15 1.714(5) . . ? S12 C14 1.736(6) . . ? S12 C15 1.721(5) . . ? F1 F3 2.145(7) . . ? F1 B 1.355(8) . . ? F2 F3 2.160(8) . . ? F2 B 1.361(9) . . ? F3 F4 2.153(8) . . ? F3 B 1.299(9) . . ? F4 B 1.322(8) . . ? C1 C3 1.505(8) . . ? C2 C4 1.499(8) . . ? C3 C4 1.340(7) . . ? C5 C6 1.366(7) . . ? C7 C8 1.335(7) . . ? C7 C9 1.504(8) . . ? C8 C10 1.490(8) . . ? C11 C13 1.495(8) . . ? C12 C14 1.497(8) . . ? C13 C14 1.345(7) . . ? 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 S1B S1A S2A 44.4(9) . . . ? S1B S1A S2B 75(1) . . . ? S1B S1A C1 70.(1) . . . ? S2A S1A S2B 33.4(8) . . . ? S2A S1A C1 98.5(2) . . . ? S2B S1A C1 1041(1) . . . ? S1A S1B S2A 95(1) . . . ? S1A S1B S2B 64(1) . . . ? S1A S1B C1 67(1) . . . ? S2A S1B S2B 33.8(9) . . . ? S2A S1B C1 125(1) . . . ? S2B S1B C1 98(1) . . . ? S1A S2A S1B 40.4(9) . . . ? S1A S2A S2B 64(1) . . . ? S1A S2A C2 99.8(2) . . . ? S1B S2A S2B 101(1) . . . ? S1B S2A C2 113.1(9) . . . ? S2B S2A C2 52(1) . . . ? S1A S2B S1B 40.1(8) . . . ? S1A S2B S2A 82(1) . . . ? S1A S2B C2 126(1) . . . ? S1B S2B S2A 44(1) . . . ? S1B S2B C2 103(1) . . . ? S2A S2B C2 89(2) . . . ? C3 S3 C5 95.8(2) . . . ? C4 S4 C5 95.2(2) . . . ? C6 S5 C7 95.4(2) . . 4_554 ? C6 S6 C8 96.4(2) . . 4_554 ? S8 S7 C9 99.0(2) . . . ? S7 S8 C10 98.3(2) . . . ? S10 S9 C11 97.6(2) . . . ? S9 S10 C12 98.4(2) . . . ? C13 S11 C15 96.0(2) . . . ? C14 S12 C15 95.9(2) . . . ? F3 F1 B 35.2(3) . . . ? F3 F2 B 34.8(3) . . . ? F1 F3 F2 62.1(2) . . . ? F1 F3 F4 61.7(3) . . . ? F1 F3 B 37.0(4) . . . ? F2 F3 F4 61.0(3) . . . ? F2 F3 B 36.7(4) . . . ? F4 F3 B 35.1(4) . . . ? F3 F4 B 34.4(4) . . . ? S1A C1 S1B 42.3(7) . . . ? S1A C1 C3 112.6(4) . . . ? S1B C1 C3 103.7(7) . . . ? S2A C2 S2B 37(1) . . . ? S2A C2 C4 110.7(4) . . . ? S2B C2 C4 112.(1) . . . ? S3 C3 C1 114.5(4) . . . ? S3 C3 C4 115.9(4) . . . ? C1 C3 C4 129.6(5) . . . ? S4 C4 C2 113.9(4) . . . ? S4 C4 C3 117.2(4) . . . ? C2 C4 C3 128.9(5) . . . ? S3 C5 S4 114.5(3) . . . ? S3 C5 C6 122.0(4) . . . ? S4 C5 C6 123.4(4) . . . ? S5 C6 S6 114.3(3) . . . ? S5 C6 C5 122.9(4) . . . ? S6 C6 C5 122.7(4) . . . ? S5 C7 C8 117.5(4) . 4_455 . ? S5 C7 C9 114.9(4) . 4_455 . ? C8 C7 C9 127.6(5) . . . ? S6 C8 C7 116.1(4) . 4_455 . ? S6 C8 C10 115.2(4) . 4_455 . ? C7 C8 C10 128.6(5) . . . ? S7 C9 C7 113.8(4) . . . ? S8 C10 C8 113.3(4) . . . ? S9 C11 C13 112.8(4) . . . ? S10 C12 C14 114.4(4) . . . ? S11 C13 C11 116.3(4) . . . ? S11 C13 C14 116.3(4) . . . ? C11 C13 C14 127.4(5) . . . ? S12 C14 C12 115.5(4) . . . ? S12 C14 C13 116.7(4) . . . ? C12 C14 C13 127.8(5) . . . ? S11 C15 S12 115.1(3) . . . ? F1 B F2 109.7(6) . . . ? F1 B F3 107.9(6) . . . ? F1 B F4 110.8(6) . . . ? F2 B F3 108.6(6) . . . ? F2 B F4 109.3(6) . . . ? F3 B F4 110.5(6) . . . ? #===END#===END#===END#===END#===END#===END#===END#===END#===END#===END#===END data_D1.Cu(SCN)2 #(3) #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C12H4N2S10Cu' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C12H4N2S10Cu' _chemical_formula_weight 564.39 _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 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 Cu ? 0.263 1.266 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 5.417(7) _cell_length_b 17.75(1) _cell_length_c 20.71(1) _cell_angle_alpha 90 _cell_angle_beta 96.94(2) _cell_angle_gamma 90 _cell_volume 1976(4) _cell_formula_units_z 4 _cell_measurement_temperature 294 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; ? ; _exptl_crystal_description plate _exptl_crystal_colour 'BLACK' _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.87 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 1116 _exptl_absorpt_coefficient_mu 2.108 _exptl_absorpt_correction_type refined_empirical_(Walker_&_Stuart,_1983) _exptl_absorpt_correction_T_min 0.4374 _exptl_absorpt_correction_T_max 1.0000 #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 294 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device Enraf_Nonius_CAD4 _diffrn_measurement_method \q/2\q _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 180 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 -8 2 -2 0 10 -1 -4 5 _diffrn_reflns_number 4040 _diffrn_reflns_av_R_equivalents 0.064 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3639 _reflns_number_observed 1353 _reflns_observed_criterion >3.0\s(I) _computing_data_collection 'CAD4_(Enraf-Nonius,_1994)' _computing_cell_refinement CAD4_(Enraf-Nonius,_1994) _computing_data_reduction 'process_MolEN_(Fair,_1990)' _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_MolEN_(Fair,_1990) _computing_molecular_graphics ? _computing_publication_material BTABLE_PTABLE_CIF_IN_MolEN_(Fair,_1990) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '4Fo^2^/(\s^2^(Fo^2^) + 0.0036 Fo^4^)' _refine_ls_hydrogen_treatment included_not_refined _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1353 _refine_ls_number_parameters 174 _refine_ls_number_restraints 16 _refine_ls_number_constraints 0 _refine_ls_abs_structure_details ; ? ; _refine_ls_R_factor_all 0.203 _refine_ls_R_factor_obs 0.056 _refine_ls_wR_factor_all 0.352 _refine_ls_wR_factor_obs 0.069 _refine_ls_goodness_of_fit_all ***** _refine_ls_goodness_of_fit_obs 1.418 _refine_ls_shift/esd_max 0.029 _refine_ls_shift/esd_mean 0.002 _refine_diff_density_max 3.044 _refine_diff_density_min -3.347 #=============================================================================== # 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_occupancy _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol CU1 0.1865(3) 0.3719(1) 0.79119(9) 0.062(1) 1.000 Uij ? ? Cu S1a -1.1609(7) 0.1812(2) 0.5727(2) 0.039(2) 0.800 Uij ? ? S S1b -1.139(4) 0.079(1) 0.559(1) 0.09(1) 0.200 Uij ? ? S S2a -0.9846(8) 0.1034(2) 0.5217(2) 0.046(2) 0.800 Uij ? ? S S2b -1.055(5) 0.183(1) 0.545(1) 0.11(1) 0.200 Uij ? ? S S3 -0.4599(6) 0.0466(2) 0.6883(2) 0.040(2) 1.000 Uij ? ? S S4 -0.4981(6) 0.2057(2) 0.7107(2) 0.037(2) 1.000 Uij ? ? S S5 0.0221(6) 0.0379(2) 0.7963(2) 0.037(2) 1.000 Uij ? ? S S6 -0.0145(6) 0.1976(2) 0.8181(2) 0.040(2) 1.000 Uij ? ? S S7 0.6835(6) 0.0635(2) 0.9347(2) 0.048(2) 1.000 Uij ? ? S S8 0.5164(7) 0.1435(2) 0.9838(2) 0.061(2) 1.000 Uij ? ? S S9 -0.4371(6) 0.3712(2) 0.6176(2) 0.054(2) 1.000 Uij ? ? S S10 0.9845(5) 0.3742(2) 0.8976(2) 0.045(2) 1.000 Uij ? ? S N1 -0.063(2) 0.3733(6) 0.7212(5) 0.049(3) 1.000 Uiso ? ? N N2 0.510(2) 0.3699(6) 0.8298(5) 0.059(3) 1.000 Uiso ? ? N C1 -0.846(2) 0.0453(7) 0.5906(6) 0.043(3) 1.000 Uiso ? ? C C2 -0.887(2) 0.2262(6) 0.6147(6) 0.038(3) 1.000 Uiso ? ? C C3 -0.693(2) 0.0953(6) 0.6388(6) 0.033(3) 1.000 Uiso ? ? C C4 -0.711(2) 0.1686(6) 0.6500(6) 0.032(3) 1.000 Uiso ? ? C C5 -0.342(2) 0.1235(7) 0.7303(5) 0.035(3) 1.000 Uiso ? ? C C6 -0.130(2) 0.1196(6) 0.7757(5) 0.030(3) 1.000 Uiso ? ? C C7 0.231(2) 0.0765(6) 0.8571(6) 0.036(3) 1.000 Uiso ? ? C C8 0.221(2) 0.1497(6) 0.8666(6) 0.034(3) 1.000 Uiso ? ? C C9 0.411(2) 0.0214(7) 0.8945(6) 0.046(3) 1.000 Uiso ? ? C C10 0.371(2) 0.1975(7) 0.9160(7) 0.054(4) 1.000 Uiso ? ? C C11 -0.221(2) 0.3718(7) 0.6781(5) 0.037(3) 1.000 Uiso ? ? C C12 0.709(2) 0.3715(7) 0.8598(5) 0.035(3) 1.000 Uiso ? ? C H1 0.3283 -0.0063 0.9258 0.0553 1.000 Uiso calc C9 H H2 0.4591 -0.0169 0.8639 0.0553 1.000 Uiso calc C9 H H3 0.4990 0.2246 0.8955 0.0645 1.000 Uiso calc C10 H H4 0.2699 0.2371 0.9318 0.0645 1.000 Uiso calc C10 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 CU1 0.0423(8) 0.064(1) 0.087(1) -0.002(1) -0.0034(8) -0.004(1) Cu S1a 0.032(2) 0.043(2) 0.042(2) 0.000(2) 0.015(2) -0.003(2) S S1b 0.06(1) 0.10(2) 0.12(2) 0.02(1) -0.03(1) -0.01(1) S S2a 0.063(3) 0.055(2) 0.028(2) 0.016(2) 0.002(2) -0.015(2) S S2b 0.18(2) 0.08(1) 0.11(1) -0.02(1) -0.10(1) 0.06(1) S S3 0.056(2) 0.028(2) 0.042(2) 0.003(2) -0.004(2) -0.001(2) S S4 0.051(2) 0.029(2) 0.033(2) -0.001(1) 0.003(1) -0.002(1) S S5 0.054(2) 0.029(2) 0.032(2) -0.002(2) 0.003(1) -0.003(1) S S6 0.054(2) 0.028(1) 0.044(2) -0.002(2) -0.005(2) 0.004(2) S S7 0.044(2) 0.053(2) 0.048(2) 0.004(2) 0.003(2) -0.001(2) S S8 0.085(2) 0.064(2) 0.041(2) 0.019(2) -0.008(2) -0.015(2) S S9 0.063(2) 0.046(2) 0.054(2) -0.000(2) -0.002(2) -0.000(2) S S10 0.037(2) 0.053(2) 0.048(2) -0.003(2) 0.009(1) 0.003(2) S # 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 CU1 S10 2.576(4) . ._455 ? CU1 N1 1.858(9) . . ? CU1 N2 1.839(9) . . ? S1a S1b 1.84(2) . . ? S1a S2a 2.044(6) . . ? S1a C2 1.81(1) . . ? S1b S2a 1.28(2) . . ? S1b S2b 1.92(3) . . ? S1b C1 1.75(2) . . ? S2a S2b 1.55(2) . . ? S2a C1 1.84(1) . . ? S2b C2 1.78(2) . . ? S3 C3 1.75(1) . . ? S3 C5 1.70(1) . . ? S4 C4 1.73(1) . . ? S4 C5 1.71(1) . . ? S5 C6 1.70(1) . . ? S5 C7 1.73(1) . . ? S6 C6 1.72(1) . . ? S6 C8 1.74(1) . . ? S7 S8 2.023(5) . . ? S7 C9 1.77(1) . . ? S8 C10 1.80(1) . . ? S9 C11 1.61(1) . . ? S10 C12 1.60(1) . . ? N1 C11 1.16(1) . . ? N2 C12 1.18(1) . . ? C1 C3 1.51(2) . . ? C1 C4 2.57(2) . . ? C2 C3 2.57(2) . . ? C2 C4 1.52(2) . . ? C3 C4 1.33(2) . . ? C3 C5 2.56(1) . . ? C4 C5 2.57(1) . . ? C5 C6 1.40(1) . . ? C6 C7 2.54(1) . . ? C6 C8 2.56(1) . . ? C7 C8 1.32(1) . . ? C7 C9 1.53(2) . . ? C7 C10 2.54(2) . . ? C8 C9 2.54(2) . . ? C8 C10 1.50(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 S10 CU1 N1 108.8(3) . ._455 . ? S10 CU1 N2 96.3(3) . ._455 . ? N1 CU1 N2 154.9(5) . . . ? S1b S1a S2a 37.9(8) . . . ? S1b S1a C2 116.4(7) . . . ? S2a S1a C2 98.0(4) . . . ? S1a S1b S2a 79(1) . . . ? S1a S1b S2b 26.3(8) . . . ? S1a S1b C1 110(1) . . . ? S2a S1b S2b 53(1) . . . ? S2a S1b C1 73(1) . . . ? S2b S1b C1 99(1) . . . ? S1a S2a S1b 62(1) . . . ? S1a S2a S2b 22.9(9) . . . ? S1a S2a C1 98.6(4) . . . ? S1b S2a S2b 85(1) . . . ? S1b S2a C1 65(1) . . . ? S2b S2a C1 111.1(9) . . . ? S1b S2b S2a 41.4(9) . . . ? S1b S2b C2 113(1) . . . ? S2a S2b C2 121(1) . . . ? C3 S3 C5 95.8(5) . . . ? C4 S4 C5 96.5(5) . . . ? C6 S5 C7 95.7(5) . . . ? C6 S6 C8 95.5(5) . . . ? S8 S7 C9 97.7(4) . . . ? S7 S8 C10 99.3(5) . . . ? CU1 S10 C12 92.8(4) . ._655 . ? CU1 N1 C11 177(1) . . . ? CU1 N2 C12 173(1) . . . ? S1b C1 S2a 41.5(9) . . . ? S1b C1 C3 116(1) . . . ? S1b C1 C4 94.5(9) . . . ? S2a C1 C3 108.8(8) . . . ? S2a C1 C4 87.7(5) . . . ? C3 C1 C4 23.1(5) . . . ? S1a C2 S2b 27.7(8) . . . ? S1a C2 C3 89.3(5) . . . ? S1a C2 C4 111.3(8) . . . ? S2b C2 C3 85.7(8) . . . ? S2b C2 C4 109(1) . . . ? C3 C2 C4 23.6(5) . . . ? S3 C3 C1 113.3(8) . . . ? S3 C3 C2 143.7(6) . . . ? S3 C3 C4 116.3(8) . . . ? S3 C3 C5 41.3(4) . . . ? C1 C3 C2 102.9(7) . . . ? C1 C3 C4 130.(1) . . . ? C1 C3 C5 154.6(8) . . . ? C2 C3 C4 27.4(6) . . . ? C2 C3 C5 102.5(5) . . . ? C4 C3 C5 75.1(7) . . . ? S4 C4 C1 142.9(6) . . . ? S4 C4 C2 114.6(8) . . . ? S4 C4 C3 116.4(8) . . . ? S4 C4 C5 41.4(4) . . . ? C1 C4 C2 102.4(7) . . . ? C1 C4 C3 26.5(6) . . . ? C1 C4 C5 101.5(5) . . . ? C2 C4 C3 1281(1) . . . ? C2 C4 C5 155.9(8) . . . ? C3 C4 C5 74.9(7) . . . ? S3 C5 S4 114.8(6) . . . ? S3 C5 C3 42.9(3) . . . ? S3 C5 C4 72.9(4) . . . ? S3 C5 C6 122.0(9) . . . ? S4 C5 C3 72.0(4) . . . ? S4 C5 C4 42.0(3) . . . ? S4 C5 C6 123.1(9) . . . ? C3 C5 C4 30.0(4) . . . ? C3 C5 C6 164.5(9) . . . ? C4 C5 C6 164.7(9) . . . ? S5 C6 S6 115.2(5) . . . ? S5 C6 C5 123.2(9) . . . ? S5 C6 C7 42.7(3) . . . ? S5 C6 C8 72.6(4) . . . ? S6 C6 C5 121.5(9) . . . ? S6 C6 C7 72.6(4) . . . ? S6 C6 C8 42.7(3) . . . ? C5 C6 C7 165.2(9) . . . ? C5 C6 C8 163.8(9) . . . ? C7 C6 C8 29.9(3) . . . ? S5 C7 C6 41.7(4) . . . ? S5 C7 C8 117.7(8) . . . ? S5 C7 C9 116.0(8) . . . ? S5 C7 C10 144.8(6) . . . ? C6 C7 C8 76.1(7) . . . ? C6 C7 C9 157.6(8) . . . ? C6 C7 C10 103.1(5) . . . ? C8 C7 C9 126.(1) . . . ? C8 C7 C10 27.1(6) . . . ? C9 C7 C10 99.2(7) . . . ? S6 C8 C6 41.8(3) . . . ? S6 C8 C7 115.8(8) . . . ? S6 C8 C9 144.8(6) . . . ? S6 C8 C10 114.7(8) . . . ? C6 C8 C7 74.0(7) . . . ? C6 C8 C9 103.0(5) . . . ? C6 C8 C10 156.4(8) . . . ? C7 C8 C9 29.0(6) . . . ? C7 C8 C10 129(1) . . . ? C9 C8 C10 100.3(7) . . . ? S7 C9 C7 114.6(8) . . . ? S7 C9 C8 91.3(5) . . . ? C7 C9 C8 24.7(5) . . . ? S8 C10 C7 90.1(6) . . . ? S8 C10 C8 112.5(8) . . . ? C7 C10 C8 23.6(5) . . . ? S9 C11 N1 178(1) . . . ? S10 C12 N2 177(1) . . . ? #===END#===END#===END#===END#===END#===END#===END#===END#===END#===END#===END