Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Hanton, Lyall Robert' 'Caradoc-Davies, Paula L.' 'Gregory, Duncan H.' 'Turnbull, Julia M.' _publ_contact_author_name 'Dr Lyall Robert Hanton' _publ_contact_author_address ; Chemistry University of Otago PO Box 56 Dunedin NEW ZEALAND ; _publ_contact_author_email lhanton@alkali.otago.ac.nz _publ_section_title ; Probing copper halide supramolecular arrays of a ditopic ligand with complexes of a monotopic analogue ; _journal_name_full 'Dalton Transactions' data_CuCl2L' #Compound 1 _database_code_CSD 175744 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H14 Cl2 Cu N2 O S' _chemical_formula_weight 368.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.077(2) _cell_length_b 13.919(4) _cell_length_c 12.956(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.728(3) _cell_angle_gamma 90.00 _cell_volume 1451.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 2951 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 26.44 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.687 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 2.008 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.642 _exptl_absorpt_correction_T_max 0.786 _exptl_absorpt_process_details 'SADABS (Sheldrick 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 170(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18180 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 26.44 _reflns_number_total 2951 _reflns_number_gt 2413 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0274P)^2^+2.0419P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2951 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0509 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0789 _refine_ls_wR_factor_gt 0.0746 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.126 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.07975(4) 0.68010(3) 0.79636(3) 0.01956(11) Uani 1 1 d . . . Cl2 Cl 0.20356(9) 0.59031(5) 0.93013(6) 0.02376(17) Uani 1 1 d . . . Cl1 Cl -0.02823(10) 0.55330(6) 0.67591(7) 0.0342(2) Uani 1 1 d . . . S1 S -0.00518(10) 0.82768(6) 0.71420(6) 0.02589(19) Uani 1 1 d . . . N1 N 0.2899(3) 0.70656(18) 0.7285(2) 0.0218(6) Uani 1 1 d . . . N2 N -0.1289(3) 0.69884(17) 0.86722(19) 0.0206(6) Uani 1 1 d . . . C1 C 0.3950(4) 0.6356(2) 0.7081(3) 0.0306(8) Uani 1 1 d . . . H1 H 0.3731 0.5723 0.7308 0.037 Uiso 1 1 calc R . . C2 C 0.5338(4) 0.6515(3) 0.6551(3) 0.0343(8) Uani 1 1 d . . . H2 H 0.6056 0.5999 0.6412 0.041 Uiso 1 1 calc R . . C3 C 0.5670(4) 0.7435(3) 0.6226(3) 0.0307(8) Uani 1 1 d . . . H3 H 0.6616 0.7559 0.5856 0.037 Uiso 1 1 calc R . . C4 C 0.4608(4) 0.8175(2) 0.6445(2) 0.0274(7) Uani 1 1 d . . . H4 H 0.4820 0.8815 0.6235 0.033 Uiso 1 1 calc R . . C5 C 0.3225(4) 0.7966(2) 0.6977(2) 0.0213(6) Uani 1 1 d . . . C6 C 0.2054(4) 0.8747(2) 0.7258(3) 0.0290(7) Uani 1 1 d . . . H6A H 0.2136 0.9303 0.6789 0.035 Uiso 1 1 calc R . . H6B H 0.2351 0.8965 0.7977 0.035 Uiso 1 1 calc R . . C7 C -0.0969(4) 0.8699(2) 0.8305(3) 0.0270(7) Uani 1 1 d . . . H7A H -0.0085 0.8909 0.8831 0.032 Uiso 1 1 calc R . . H7B H -0.1714 0.9250 0.8132 0.032 Uiso 1 1 calc R . . C8 C -0.1941(4) 0.7876(2) 0.8723(2) 0.0214(6) Uani 1 1 d . . . C9 C -0.3438(4) 0.8030(2) 0.9148(2) 0.0259(7) Uani 1 1 d . . . H9 H -0.3876 0.8661 0.9188 0.031 Uiso 1 1 calc R . . C10 C -0.4287(4) 0.7254(3) 0.9513(3) 0.0296(7) Uani 1 1 d . . . H10 H -0.5325 0.7345 0.9795 0.036 Uiso 1 1 calc R . . C11 C -0.3606(4) 0.6341(2) 0.9465(3) 0.0283(7) Uani 1 1 d . . . H11 H -0.4165 0.5800 0.9717 0.034 Uiso 1 1 calc R . . C12 C -0.2107(4) 0.6233(2) 0.9044(2) 0.0257(7) Uani 1 1 d . . . H12 H -0.1633 0.5609 0.9013 0.031 Uiso 1 1 calc R . . O1 O 0.2619(4) 0.9531(3) 0.9626(3) 0.0697(11) Uani 1 1 d . . . H1A H 0.328(6) 0.947(4) 1.034(4) 0.084 Uiso 1 1 d . . . H1B H 0.338(7) 0.993(4) 0.927(4) 0.084 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01773(19) 0.01816(19) 0.0236(2) 0.00180(15) 0.00661(14) 0.00049(15) Cl2 0.0218(4) 0.0246(4) 0.0253(4) 0.0038(3) 0.0052(3) 0.0027(3) Cl1 0.0295(4) 0.0357(5) 0.0375(5) -0.0153(4) 0.0038(4) -0.0028(4) S1 0.0253(4) 0.0265(4) 0.0264(4) 0.0043(3) 0.0054(3) 0.0029(3) N1 0.0201(13) 0.0216(13) 0.0243(14) 0.0018(11) 0.0047(11) -0.0005(10) N2 0.0178(13) 0.0209(13) 0.0235(13) 0.0014(10) 0.0032(10) 0.0006(10) C1 0.0281(18) 0.0249(17) 0.040(2) 0.0092(15) 0.0123(15) 0.0052(14) C2 0.0281(19) 0.0347(19) 0.042(2) 0.0054(16) 0.0160(16) 0.0095(15) C3 0.0212(17) 0.046(2) 0.0263(17) 0.0074(15) 0.0086(13) 0.0001(15) C4 0.0245(17) 0.0296(17) 0.0285(17) 0.0071(15) 0.0040(13) -0.0063(14) C5 0.0177(15) 0.0249(16) 0.0208(15) 0.0025(12) -0.0008(12) -0.0028(12) C6 0.0268(18) 0.0224(16) 0.0394(19) 0.0015(15) 0.0115(15) -0.0031(14) C7 0.0291(18) 0.0232(16) 0.0297(18) -0.0014(14) 0.0089(14) 0.0019(14) C8 0.0205(15) 0.0234(16) 0.0200(15) 0.0002(12) 0.0007(12) 0.0001(13) C9 0.0246(16) 0.0250(17) 0.0285(17) -0.0009(13) 0.0054(13) 0.0052(13) C10 0.0167(16) 0.042(2) 0.0310(18) -0.0003(16) 0.0040(13) 0.0010(15) C11 0.0228(17) 0.0314(18) 0.0315(18) 0.0068(15) 0.0065(14) -0.0029(14) C12 0.0253(17) 0.0230(16) 0.0291(17) 0.0047(13) 0.0039(14) -0.0007(13) O1 0.056(2) 0.113(3) 0.0390(17) 0.0051(19) -0.0003(15) -0.041(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N2 2.002(2) . ? Cu1 N1 2.009(2) . ? Cu1 Cl2 2.2978(9) . ? Cu1 S1 2.3881(10) . ? Cu1 Cl1 2.4671(10) . ? S1 C6 1.817(3) . ? S1 C7 1.829(3) . ? N1 C1 1.343(4) . ? N1 C5 1.348(4) . ? N2 C8 1.347(4) . ? N2 C12 1.351(4) . ? C1 C2 1.379(4) . ? C2 C3 1.381(5) . ? C3 C4 1.385(5) . ? C4 C5 1.391(4) . ? C5 C6 1.505(4) . ? C7 C8 1.514(4) . ? C8 C9 1.386(4) . ? C9 C10 1.384(5) . ? C10 C11 1.389(5) . ? C11 C12 1.377(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu1 N1 161.91(10) . . ? N2 Cu1 Cl2 93.19(7) . . ? N1 Cu1 Cl2 95.69(8) . . ? N2 Cu1 S1 82.56(7) . . ? N1 Cu1 S1 82.48(7) . . ? Cl2 Cu1 S1 153.54(3) . . ? N2 Cu1 Cl1 96.67(8) . . ? N1 Cu1 Cl1 96.98(8) . . ? Cl2 Cu1 Cl1 101.37(4) . . ? S1 Cu1 Cl1 105.06(4) . . ? C6 S1 C7 104.86(16) . . ? C6 S1 Cu1 92.30(11) . . ? C7 S1 Cu1 91.72(11) . . ? C1 N1 C5 118.9(3) . . ? C1 N1 Cu1 121.5(2) . . ? C5 N1 Cu1 119.5(2) . . ? C8 N2 C12 119.5(3) . . ? C8 N2 Cu1 119.3(2) . . ? C12 N2 Cu1 121.1(2) . . ? N1 C1 C2 122.2(3) . . ? C1 C2 C3 119.2(3) . . ? C2 C3 C4 119.2(3) . . ? C3 C4 C5 118.8(3) . . ? N1 C5 C4 121.7(3) . . ? N1 C5 C6 117.2(3) . . ? C4 C5 C6 121.0(3) . . ? C5 C6 S1 108.9(2) . . ? C8 C7 S1 108.0(2) . . ? N2 C8 C9 121.2(3) . . ? N2 C8 C7 117.4(3) . . ? C9 C8 C7 121.3(3) . . ? C10 C9 C8 119.2(3) . . ? C9 C10 C11 119.3(3) . . ? C12 C11 C10 118.9(3) . . ? N2 C12 C11 121.8(3) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.44 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.517 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.082 #===END data_anti-Cu2Cl4L #Compound 2a _database_code_CSD 175745 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H24 Cl4 Cu2 N6 S2' _chemical_formula_weight 705.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.735(2) _cell_length_b 7.989(2) _cell_length_c 11.949(2) _cell_angle_alpha 86.02(3) _cell_angle_beta 77.61(3) _cell_angle_gamma 71.18(3) _cell_volume 682.6(3) _cell_formula_units_Z 1 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 1381 _cell_measurement_theta_min 2.84 _cell_measurement_theta_max 25.96 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.716 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 356 _exptl_absorpt_coefficient_mu 2.127 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.07081 _exptl_absorpt_correction_T_max 0.9184 _exptl_absorpt_process_details 'SADABS (sheldrick 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1768 _diffrn_reflns_av_R_equivalents 0.0533 _diffrn_reflns_av_sigmaI/netI 0.1115 _diffrn_reflns_limit_h_min -2 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 25.96 _reflns_number_total 1381 _reflns_number_gt 1138 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1381 _refine_ls_number_parameters 155 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1950 _refine_ls_R_factor_gt 0.1773 _refine_ls_wR_factor_ref 0.4752 _refine_ls_wR_factor_gt 0.4681 _refine_ls_goodness_of_fit_ref 1.892 _refine_ls_restrained_S_all 1.868 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.4629(5) 0.8744(4) 0.8577(3) 0.0378(16) Uani 1 1 d . . . Cl1 Cl 0.7619(10) 0.8407(10) 0.7708(7) 0.046(3) Uani 1 1 d . . . Cl2 Cl 0.5298(10) 0.7443(9) 1.0246(7) 0.044(3) Uani 1 1 d . . . S1 S 0.3665(10) 0.6300(9) 0.7826(6) 0.038(3) Uani 1 1 d . . . N1 N 0.380(3) 1.002(3) 0.724(2) 0.045(8) Uani 1 1 d . . . N2 N 0.183(3) 0.953(3) 0.939(2) 0.037(8) Uani 1 1 d . . . C1 C 0.407(4) 1.164(3) 0.693(2) 0.036(6) Uani 1 1 d U . . H1 H 0.4679 1.2107 0.7363 0.043 Uiso 1 1 calc R . . C2 C 0.344(4) 1.259(4) 0.598(3) 0.042(7) Uani 1 1 d U . . H2 H 0.3576 1.3701 0.5834 0.051 Uiso 1 1 calc R . . C3 C 0.267(4) 1.198(4) 0.528(3) 0.045(10) Uani 1 1 d . . . H3 H 0.2318 1.2628 0.4638 0.054 Uiso 1 1 calc R . . C4 C 0.239(4) 1.034(4) 0.553(3) 0.046(11) Uani 1 1 d . . . H4 H 0.1853 0.9864 0.5065 0.056 Uiso 1 1 calc R . . C5 C 0.295(4) 0.944(4) 0.650(3) 0.036(6) Uani 1 1 d U . . C6 C 0.264(4) 0.769(4) 0.673(3) 0.043(7) Uani 1 1 d U . . H6A H 0.3101 0.7025 0.6024 0.051 Uiso 1 1 calc R . . H6B H 0.1307 0.7899 0.6936 0.051 Uiso 1 1 calc R . . C7 C 0.182(5) 0.652(4) 0.900(2) 0.066(14) Uani 1 1 d . . . H7A H 0.0875 0.6138 0.8766 0.079 Uiso 1 1 calc R . . H7B H 0.2272 0.5721 0.9596 0.079 Uiso 1 1 calc R . . C8 C 0.088(3) 0.838(3) 0.951(2) 0.017(5) Uani 1 1 d U . . C9 C 0.104(2) 1.108(2) 0.9960(18) 0.036(9) Uani 1 1 d . . . H9 H 0.1760 1.1800 1.0004 0.043 Uiso 1 1 calc R . . N3 N 0.245(2) 0.608(2) 0.4165(18) 0.086(17) Uani 1 1 d R . . C11 C 0.200(2) 0.637(2) 0.3389(18) 0.08(2) Uani 1 1 d R . . C10 C 0.143(2) 0.662(2) 0.2295(18) 0.072(11) Uani 1 1 d RU . . H10A H 0.1997 0.5545 0.1861 0.108 Uiso 1 1 calc R . . H10B H 0.1824 0.7554 0.1880 0.108 Uiso 1 1 calc R . . H10C H 0.0100 0.6930 0.2418 0.108 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.039(2) 0.024(2) 0.041(3) 0.0053(18) -0.001(2) -0.0019(15) Cl1 0.040(4) 0.055(5) 0.036(6) 0.009(4) -0.008(4) -0.005(3) Cl2 0.047(4) 0.037(4) 0.042(5) 0.011(4) -0.007(4) -0.009(3) S1 0.044(4) 0.029(4) 0.032(5) -0.004(4) -0.003(4) -0.002(3) N1 0.054(14) 0.027(13) 0.036(18) 0.013(13) -0.001(15) 0.003(11) N2 0.022(11) 0.031(13) 0.048(17) 0.007(13) 0.002(13) -0.004(10) C1 0.037(7) 0.034(7) 0.034(8) 0.001(5) -0.008(5) -0.009(5) C2 0.043(8) 0.042(8) 0.043(9) 0.000(5) -0.011(5) -0.012(5) C3 0.043(16) 0.041(19) 0.04(2) 0.015(16) -0.009(18) -0.001(14) C4 0.06(2) 0.038(17) 0.04(2) -0.007(17) 0.000(19) -0.017(16) C5 0.038(7) 0.035(7) 0.035(8) 0.001(5) -0.008(5) -0.010(5) C6 0.044(8) 0.043(8) 0.043(8) 0.001(5) -0.009(5) -0.014(5) C7 0.09(2) 0.06(2) 0.05(2) -0.028(18) 0.05(2) -0.047(19) C8 0.017(6) 0.014(6) 0.018(7) 0.000(4) -0.005(4) -0.002(5) C9 0.049(16) 0.035(17) 0.025(18) -0.005(15) -0.007(16) -0.015(14) N3 0.09(3) 0.06(2) 0.11(4) -0.01(2) -0.02(3) -0.03(2) C11 0.06(2) 0.04(2) 0.13(5) -0.02(3) 0.04(3) -0.015(18) C10 0.071(13) 0.073(13) 0.067(14) 0.011(9) -0.009(9) -0.021(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.94(3) . ? Cu1 N2 2.082(17) . ? Cu1 Cl1 2.260(7) . ? Cu1 Cl2 2.266(10) . ? Cu1 S1 2.577(7) . ? S1 C7 1.75(2) . ? S1 C6 1.80(4) . ? N1 C1 1.39(3) . ? N1 C5 1.39(4) . ? N2 C8 1.34(2) . ? N2 C9 1.35(2) . ? C1 C2 1.41(4) . ? C2 C3 1.32(4) . ? C3 C4 1.40(3) . ? C4 C5 1.40(5) . ? C5 C6 1.49(3) . ? C7 C8 1.53(3) . ? C8 C9 1.42(2) 2_577 ? C9 C8 1.42(2) 2_577 ? N3 C11 1.0435 . ? C11 C10 1.4487 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N2 86.6(9) . . ? N1 Cu1 Cl1 89.7(7) . . ? N2 Cu1 Cl1 169.7(6) . . ? N1 Cu1 Cl2 173.7(6) . . ? N2 Cu1 Cl2 87.6(7) . . ? Cl1 Cu1 Cl2 95.6(3) . . ? N1 Cu1 S1 83.1(7) . . ? N2 Cu1 S1 81.3(6) . . ? Cl1 Cu1 S1 107.8(3) . . ? Cl2 Cu1 S1 98.3(3) . . ? C7 S1 C6 104.8(17) . . ? C7 S1 Cu1 92.3(9) . . ? C6 S1 Cu1 93.6(8) . . ? C1 N1 C5 114(3) . . ? C1 N1 Cu1 121(2) . . ? C5 N1 Cu1 125(2) . . ? C8 N2 C9 119.0(16) . . ? C8 N2 Cu1 119.2(15) . . ? C9 N2 Cu1 121.0(12) . . ? N1 C1 C2 121(3) . . ? C3 C2 C1 124(3) . . ? C2 C3 C4 117(3) . . ? C3 C4 C5 119(3) . . ? N1 C5 C4 125(2) . . ? N1 C5 C6 118(3) . . ? C4 C5 C6 117(2) . . ? C5 C6 S1 119(2) . . ? C8 C7 S1 115.8(15) . . ? N2 C8 C9 119.5(17) . 2_577 ? N2 C8 C7 120.6(18) . . ? C9 C8 C7 119.8(16) 2_577 . ? N2 C9 C8 120.5(14) . 2_577 ? N3 C11 C10 175.0 . . ? _diffrn_measured_fraction_theta_max 0.515 _diffrn_reflns_theta_full 25.96 _diffrn_measured_fraction_theta_full 0.515 _refine_diff_density_max 2.162 _refine_diff_density_min -1.109 _refine_diff_density_rms 0.290 #===END data_syn-Cu2Cl4L #Compound 2b _database_code_CSD 175746 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H21 Cl4 Cu2 N5 S2' _chemical_formula_weight 664.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.363(5) _cell_length_b 11.881(3) _cell_length_c 15.710(5) _cell_angle_alpha 90.00 _cell_angle_beta 107.664(5) _cell_angle_gamma 90.00 _cell_volume 2554.4(14) _cell_formula_units_Z 4 _cell_measurement_temperature 158(2) _cell_measurement_reflns_used 3305 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 26.36 _exptl_crystal_description 'thin plate' _exptl_crystal_colour green _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.728 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 2.267 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.379 _exptl_absorpt_correction_T_max 0.956 _exptl_absorpt_process_details 'SADABS (sheldrick 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 158(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4243 _diffrn_reflns_av_R_equivalents 0.0958 _diffrn_reflns_av_sigmaI/netI 0.1598 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -2 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 26.36 _reflns_number_total 3305 _reflns_number_gt 1676 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3305 _refine_ls_number_parameters 299 _refine_ls_number_restraints 63 _refine_ls_R_factor_all 0.1540 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.1382 _refine_ls_wR_factor_gt 0.1073 _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_restrained_S_all 0.974 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.41807(10) 0.28110(8) 0.16092(9) 0.0218(4) Uani 1 1 d . . . Cu2 Cu 0.83926(11) 0.41065(10) 0.53986(10) 0.0369(5) Uani 1 1 d . . . Cl1 Cl 0.3844(2) 0.13065(18) 0.23892(18) 0.0307(8) Uani 1 1 d . . . Cl2 Cl 0.4884(2) 0.17712(19) 0.07846(18) 0.0335(8) Uani 1 1 d . . . Cl4 Cl 0.7690(2) 0.3828(2) 0.6487(2) 0.0456(9) Uani 1 1 d . . . Cl3 Cl 0.9078(3) 0.2379(2) 0.5521(3) 0.0665(12) Uani 1 1 d . . . S1 S 0.3389(2) 0.38870(18) 0.24259(18) 0.0224(7) Uani 1 1 d . . . S2 S 0.9086(2) 0.4392(2) 0.4240(2) 0.0392(10) Uani 1 1 d . . . N1 N 0.3926(6) 0.4195(5) 0.0785(6) 0.020(2) Uani 1 1 d U . . N2 N 0.5495(6) 0.3388(6) 0.2722(6) 0.018(2) Uani 1 1 d U . . N3 N 0.7041(7) 0.3930(6) 0.4192(6) 0.023(2) Uani 1 1 d U . . N4 N 0.8322(6) 0.5832(7) 0.5392(6) 0.028(3) Uani 1 1 d . . . C1 C 0.3956(8) 0.4162(8) -0.0062(8) 0.027(3) Uani 1 1 d U . . H1 H 0.4201 0.3518 -0.0253 0.032 Uiso 1 1 calc R . . C2 C 0.3647(8) 0.5021(7) -0.0656(7) 0.033(3) Uani 1 1 d . . . H2 H 0.3687 0.4962 -0.1234 0.039 Uiso 1 1 calc R . . C3 C 0.3270(8) 0.5989(8) -0.0381(9) 0.038(3) Uani 1 1 d U . . H3 H 0.3034 0.6581 -0.0775 0.045 Uiso 1 1 calc R . . C4 C 0.3258(9) 0.6044(8) 0.0489(8) 0.037(3) Uani 1 1 d . . . H4 H 0.3025 0.6690 0.0691 0.044 Uiso 1 1 calc R . . C5 C 0.3586(8) 0.5160(7) 0.1065(7) 0.020(3) Uani 1 1 d . . . C6 C 0.3635(8) 0.5251(7) 0.2023(7) 0.026(3) Uani 1 1 d U . . H6A H 0.3158 0.5794 0.2090 0.031 Uiso 1 1 calc R . . H6B H 0.4279 0.5508 0.2372 0.031 Uiso 1 1 calc R . . C7 C 0.4299(8) 0.3847(8) 0.3499(7) 0.033(3) Uani 1 1 d U . . H7A H 0.4246 0.4527 0.3822 0.040 Uiso 1 1 calc R . . H7B H 0.4163 0.3214 0.3832 0.040 Uiso 1 1 calc R . . C8 C 0.5341(8) 0.3745(7) 0.3463(7) 0.019(3) Uani 1 1 d . . . C9 C 0.6116(8) 0.4014(7) 0.4198(7) 0.020(3) Uani 1 1 d . . . H9 H 0.5992 0.4262 0.4714 0.024 Uiso 1 1 calc R . . C10 C 0.6403(8) 0.3302(7) 0.2684(7) 0.016(2) Uani 1 1 d U . . H10 H 0.6516 0.3041 0.2166 0.020 Uiso 1 1 calc R . . C11 C 0.7192(9) 0.3604(7) 0.3422(8) 0.026(3) Uani 1 1 d . . . C12 C 0.8221(8) 0.3529(9) 0.3383(7) 0.037(3) Uani 1 1 d . . . H12A H 0.8235 0.3771 0.2797 0.044 Uiso 1 1 calc R . . H12B H 0.8431 0.2750 0.3459 0.044 Uiso 1 1 calc R . . C13 C 0.8608(8) 0.5784(8) 0.3952(7) 0.034(3) Uani 1 1 d U . . H13A H 0.9054 0.6201 0.3715 0.041 Uiso 1 1 calc R . . H13B H 0.7988 0.5728 0.3483 0.041 Uiso 1 1 calc R . . C14 C 0.8457(8) 0.6426(8) 0.4715(8) 0.032(3) Uani 1 1 d U . . C15 C 0.8456(8) 0.7605(9) 0.4700(8) 0.037(3) Uani 1 1 d . . . H15 H 0.8571 0.7999 0.4230 0.044 Uiso 1 1 calc R . . C16 C 0.8279(9) 0.8158(9) 0.5401(10) 0.052(4) Uani 1 1 d . . . H16 H 0.8242 0.8940 0.5397 0.063 Uiso 1 1 calc R . . C17 C 0.8157(9) 0.7566(9) 0.6107(10) 0.051(4) Uani 1 1 d . . . H17 H 0.8060 0.7936 0.6595 0.062 Uiso 1 1 calc R . . C18 C 0.8182(8) 0.6394(10) 0.6078(9) 0.042(4) Uani 1 1 d . . . H18 H 0.8097 0.5988 0.6555 0.051 Uiso 1 1 calc R . . C19 C 1.0070(15) 0.9794(17) 0.6785(16) 0.40(4) Uani 1 1 d D . . C20 C 1.075(2) 0.975(3) 0.620(2) 0.213(17) Uani 1 1 d D . . H201 H 1.1087 0.9043 0.6276 0.319 Uiso 1 1 calc R . . H202 H 1.1224 1.0351 0.6367 0.319 Uiso 1 1 calc R . . H203 H 1.0377 0.9842 0.5581 0.319 Uiso 1 1 calc R . . N5 N 0.952(3) 0.989(3) 0.719(2) 0.246(14) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0272(9) 0.0171(5) 0.0209(9) 0.0000(5) 0.0072(7) 0.0011(6) Cu2 0.0318(11) 0.0352(7) 0.0426(12) -0.0060(6) 0.0097(9) -0.0019(6) Cl1 0.036(2) 0.0215(11) 0.036(2) 0.0047(11) 0.0128(16) -0.0033(11) Cl2 0.048(2) 0.0285(12) 0.025(2) 0.0015(11) 0.0129(17) 0.0137(12) Cl4 0.052(2) 0.0478(16) 0.039(2) -0.0060(14) 0.0158(19) -0.0087(15) Cl3 0.055(3) 0.0456(18) 0.104(3) 0.0103(17) 0.033(2) 0.0139(16) S1 0.026(2) 0.0242(12) 0.0179(19) 0.0008(11) 0.0074(15) -0.0008(11) S2 0.028(2) 0.0421(16) 0.044(2) -0.0115(14) 0.0050(19) -0.0054(13) N1 0.022(4) 0.014(3) 0.021(4) -0.003(3) 0.003(3) 0.006(3) N2 0.017(4) 0.018(3) 0.021(4) -0.001(3) 0.008(4) -0.003(3) N3 0.019(4) 0.028(3) 0.019(4) -0.003(3) 0.001(4) -0.001(3) N4 0.022(7) 0.047(5) 0.015(7) -0.004(5) 0.007(5) -0.005(4) C1 0.030(5) 0.030(4) 0.027(5) -0.003(4) 0.017(4) 0.005(3) C2 0.053(9) 0.033(6) 0.015(8) 0.003(5) 0.014(7) 0.007(5) C3 0.045(5) 0.036(4) 0.035(5) 0.006(4) 0.016(4) 0.003(4) C4 0.064(10) 0.025(5) 0.030(9) -0.002(5) 0.026(7) 0.001(6) C5 0.024(8) 0.021(5) 0.017(8) -0.002(4) 0.011(6) 0.000(4) C6 0.029(5) 0.028(4) 0.022(5) 0.003(3) 0.008(4) 0.001(3) C7 0.035(5) 0.038(4) 0.032(5) -0.001(4) 0.018(4) 0.001(4) C8 0.022(8) 0.017(4) 0.017(8) 0.001(4) 0.006(6) 0.001(4) C9 0.020(8) 0.025(5) 0.015(8) 0.000(4) 0.003(6) 0.000(5) C10 0.019(5) 0.018(3) 0.015(5) 0.001(3) 0.008(4) 0.003(3) C11 0.022(9) 0.023(5) 0.037(9) 0.004(5) 0.015(7) -0.001(4) C12 0.034(10) 0.054(7) 0.024(9) -0.018(5) 0.010(7) -0.007(6) C13 0.027(5) 0.039(4) 0.038(5) -0.004(4) 0.010(4) -0.006(4) C14 0.027(5) 0.036(4) 0.031(5) -0.003(4) 0.006(4) 0.001(4) C15 0.025(9) 0.047(7) 0.038(10) 0.000(6) 0.010(7) -0.001(5) C16 0.051(11) 0.032(6) 0.065(12) 0.008(7) 0.006(9) 0.006(6) C17 0.055(11) 0.033(6) 0.061(11) -0.017(6) 0.011(9) -0.001(6) C18 0.028(9) 0.061(8) 0.031(10) -0.003(6) -0.001(8) -0.015(6) C19 0.55(9) 0.028(11) 0.29(6) 0.01(2) -0.34(5) -0.02(3) C20 0.17(3) 0.14(2) 0.23(4) 0.05(2) -0.08(2) -0.028(19) N5 0.38(4) 0.19(3) 0.14(2) -0.072(17) 0.05(3) -0.08(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.056(8) . ? Cu1 Cl2 2.240(3) . ? Cu1 N2 2.255(8) . ? Cu1 Cl1 2.300(3) . ? Cu1 S1 2.336(3) . ? Cu2 N4 2.052(8) . ? Cu2 Cl4 2.258(4) . ? Cu2 Cl3 2.260(3) . ? Cu2 N3 2.274(9) . ? Cu2 S2 2.349(4) . ? S1 C7 1.793(11) . ? S1 C6 1.813(9) . ? S2 C13 1.795(10) . ? S2 C12 1.842(10) . ? N1 C1 1.345(12) . ? N1 C5 1.370(11) . ? N2 C8 1.319(11) . ? N2 C10 1.328(11) . ? N3 C9 1.335(12) . ? N3 C11 1.349(12) . ? N4 C18 1.334(13) . ? N4 C14 1.339(13) . ? C1 C2 1.363(13) . ? C2 C3 1.395(14) . ? C3 C4 1.374(14) . ? C4 C5 1.374(13) . ? C5 C6 1.489(14) . ? C7 C8 1.520(14) . ? C8 C9 1.377(13) . ? C10 C11 1.399(13) . ? C11 C12 1.500(15) . ? C13 C14 1.491(14) . ? C14 C15 1.400(14) . ? C15 C16 1.371(15) . ? C16 C17 1.369(16) . ? C17 C18 1.393(14) . ? C19 N5 1.1604(11) . ? C19 C20 1.5405(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 Cl2 95.9(2) . . ? N1 Cu1 N2 101.1(3) . . ? Cl2 Cu1 N2 101.4(2) . . ? N1 Cu1 Cl1 158.6(2) . . ? Cl2 Cu1 Cl1 94.82(10) . . ? N2 Cu1 Cl1 94.9(2) . . ? N1 Cu1 S1 83.4(2) . . ? Cl2 Cu1 S1 177.76(12) . . ? N2 Cu1 S1 80.8(2) . . ? Cl1 Cu1 S1 85.22(10) . . ? N4 Cu2 Cl4 96.8(3) . . ? N4 Cu2 Cl3 158.0(3) . . ? Cl4 Cu2 Cl3 94.93(13) . . ? N4 Cu2 N3 93.4(3) . . ? Cl4 Cu2 N3 98.8(3) . . ? Cl3 Cu2 N3 103.1(2) . . ? N4 Cu2 S2 83.3(3) . . ? Cl4 Cu2 S2 178.59(13) . . ? Cl3 Cu2 S2 85.44(13) . . ? N3 Cu2 S2 79.8(3) . . ? C7 S1 C6 100.8(5) . . ? C7 S1 Cu1 99.5(4) . . ? C6 S1 Cu1 96.8(4) . . ? C13 S2 C12 102.0(5) . . ? C13 S2 Cu2 96.2(4) . . ? C12 S2 Cu2 97.8(4) . . ? C1 N1 C5 117.7(8) . . ? C1 N1 Cu1 123.2(6) . . ? C5 N1 Cu1 118.6(7) . . ? C8 N2 C10 119.6(9) . . ? C8 N2 Cu1 117.2(7) . . ? C10 N2 Cu1 123.0(7) . . ? C9 N3 C11 117.3(9) . . ? C9 N3 Cu2 125.9(8) . . ? C11 N3 Cu2 116.4(8) . . ? C18 N4 C14 118.1(10) . . ? C18 N4 Cu2 121.0(8) . . ? C14 N4 Cu2 120.8(7) . . ? N1 C1 C2 123.7(9) . . ? C1 C2 C3 118.8(11) . . ? C4 C3 C2 118.1(10) . . ? C5 C4 C3 120.9(10) . . ? N1 C5 C4 120.8(10) . . ? N1 C5 C6 118.3(8) . . ? C4 C5 C6 120.8(9) . . ? C5 C6 S1 109.5(6) . . ? C8 C7 S1 114.3(8) . . ? N2 C8 C9 120.4(10) . . ? N2 C8 C7 119.3(10) . . ? C9 C8 C7 120.4(10) . . ? N3 C9 C8 122.0(10) . . ? N2 C10 C11 120.3(10) . . ? N3 C11 C10 120.4(11) . . ? N3 C11 C12 118.8(10) . . ? C10 C11 C12 120.8(10) . . ? C11 C12 S2 113.0(8) . . ? C14 C13 S2 114.0(8) . . ? N4 C14 C15 122.7(11) . . ? N4 C14 C13 117.4(9) . . ? C15 C14 C13 119.9(11) . . ? C16 C15 C14 117.8(12) . . ? C17 C16 C15 120.3(11) . . ? C16 C17 C18 118.4(13) . . ? N4 C18 C17 122.6(13) . . ? N5 C19 C20 175(2) . . ? _diffrn_measured_fraction_theta_max 0.634 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 0.634 _refine_diff_density_max 0.535 _refine_diff_density_min -0.627 _refine_diff_density_rms 0.119 #===END data_Cu2I2L'2 #Compound 3 _database_code_CSD 175747 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H24 Cu2 I2 N4 S2' _chemical_formula_weight 813.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.0239(5) _cell_length_b 18.7101(11) _cell_length_c 9.5160(6) _cell_angle_alpha 90.00 _cell_angle_beta 110.1120(10) _cell_angle_gamma 90.00 _cell_volume 1341.50(14) _cell_formula_units_Z 2 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used 2747 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 26.42 _exptl_crystal_description hexagonal _exptl_crystal_colour red _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.62 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.014 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 4.063 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3062 _exptl_absorpt_correction_T_max 0.6661 _exptl_absorpt_process_details 'SADABS (sheldrick 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17040 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 26.42 _reflns_number_total 2747 _reflns_number_gt 2514 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+1.1676P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0050(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2747 _refine_ls_number_parameters 155 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0313 _refine_ls_R_factor_gt 0.0276 _refine_ls_wR_factor_ref 0.0715 _refine_ls_wR_factor_gt 0.0698 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2103(4) 0.87490(18) 0.9903(4) 0.0298(7) Uani 1 1 d . . . H1 H 0.2003 0.9147 0.9294 0.036 Uiso 1 1 calc R . . C2 C 0.0615(5) 0.8345(2) 0.9710(4) 0.0355(8) Uani 1 1 d . . . H2 H -0.0462 0.8465 0.8982 0.043 Uiso 1 1 calc R . . C3 C 0.0752(5) 0.7758(2) 1.0619(5) 0.0442(10) Uani 1 1 d . . . H3 H -0.0238 0.7477 1.0523 0.053 Uiso 1 1 calc R . . C4 C 0.2375(5) 0.75931(19) 1.1671(5) 0.0388(9) Uani 1 1 d . . . H4 H 0.2485 0.7201 1.2296 0.047 Uiso 1 1 calc R . . C5 C 0.3849(4) 0.80132(17) 1.1798(4) 0.0251(6) Uani 1 1 d . . . C6 C 0.5645(4) 0.78286(17) 1.2915(4) 0.0280(7) Uani 1 1 d . . . H6A H 0.6554 0.8016 1.2558 0.034 Uiso 1 1 calc R . . H6B H 0.5769 0.7313 1.2972 0.034 Uiso 1 1 calc R . . C7 C 0.6609(4) 0.90951(17) 1.4586(4) 0.0262(7) Uani 1 1 d . . . H7A H 0.5637 0.9324 1.3809 0.031 Uiso 1 1 calc R . . H7B H 0.6776 0.9346 1.5516 0.031 Uiso 1 1 calc R . . C8 C 0.8264(4) 0.91612(16) 1.4204(3) 0.0209(6) Uani 1 1 d . . . C9 C 0.9938(5) 0.90717(18) 1.5284(3) 0.0281(7) Uani 1 1 d . . . H9 H 1.0043 0.8980 1.6272 0.034 Uiso 1 1 calc R . . C10 C 1.1444(5) 0.91184(19) 1.4895(4) 0.0318(7) Uani 1 1 d . . . H10 H 1.2566 0.9058 1.5610 0.038 Uiso 1 1 calc R . . C11 C 1.1246(4) 0.92564(18) 1.3423(4) 0.0302(7) Uani 1 1 d . . . H11 H 1.2233 0.9288 1.3126 0.036 Uiso 1 1 calc R . . C12 C 0.9555(4) 0.93468(16) 1.2396(4) 0.0251(7) Uani 1 1 d . . . H12 H 0.9431 0.9450 1.1410 0.030 Uiso 1 1 calc R . . N1 N 0.3710(3) 0.86001(14) 1.0932(3) 0.0250(6) Uani 1 1 d . . . N2 N 0.8070(3) 0.92925(13) 1.2762(3) 0.0212(5) Uani 1 1 d . . . S1 S 0.60152(11) 0.81763(5) 1.47782(9) 0.0301(2) Uani 1 1 d . . . Cu1 Cu 0.56510(5) 0.93529(2) 1.11316(4) 0.02746(13) Uani 1 1 d . . . I1 I 0.59662(3) 0.940236(10) 0.84663(2) 0.02321(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0249(17) 0.0335(17) 0.0295(17) -0.0023(14) 0.0075(14) -0.0011(13) C2 0.0222(17) 0.038(2) 0.041(2) -0.0110(15) 0.0039(15) 0.0005(14) C3 0.030(2) 0.035(2) 0.066(3) -0.0092(19) 0.0151(19) -0.0122(15) C4 0.034(2) 0.0270(18) 0.055(2) 0.0001(16) 0.0162(18) -0.0095(15) C5 0.0275(16) 0.0208(15) 0.0315(16) -0.0026(12) 0.0160(14) -0.0023(12) C6 0.0280(17) 0.0223(15) 0.0356(18) 0.0010(13) 0.0134(14) 0.0016(12) C7 0.0298(17) 0.0279(16) 0.0224(15) 0.0013(13) 0.0108(13) 0.0031(13) C8 0.0243(15) 0.0185(13) 0.0197(14) -0.0006(11) 0.0072(12) 0.0010(11) C9 0.0321(18) 0.0289(17) 0.0183(15) -0.0002(13) 0.0023(13) -0.0019(14) C10 0.0213(16) 0.0291(17) 0.0363(19) -0.0004(14) -0.0013(14) -0.0010(13) C11 0.0202(16) 0.0315(17) 0.039(2) -0.0039(14) 0.0108(15) -0.0005(13) C12 0.0226(16) 0.0301(17) 0.0245(16) -0.0020(12) 0.0106(13) -0.0002(12) N1 0.0225(13) 0.0267(14) 0.0266(13) -0.0022(11) 0.0095(11) -0.0017(10) N2 0.0175(12) 0.0259(13) 0.0188(12) -0.0014(10) 0.0047(10) 0.0000(10) S1 0.0320(4) 0.0331(4) 0.0272(4) 0.0078(3) 0.0126(4) -0.0016(3) Cu1 0.0208(2) 0.0385(3) 0.0218(2) 0.00086(16) 0.00569(17) -0.00376(16) I1 0.02612(15) 0.02651(14) 0.01745(13) 0.00135(7) 0.00808(9) 0.00499(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.353(4) . ? C1 C2 1.370(5) . ? C2 C3 1.380(6) . ? C3 C4 1.377(6) . ? C4 C5 1.391(5) . ? C5 N1 1.354(4) . ? C5 C6 1.507(5) . ? C6 S1 1.815(3) . ? C7 C8 1.498(4) . ? C7 S1 1.810(3) . ? C8 N2 1.349(4) . ? C8 C9 1.393(4) . ? C9 C10 1.383(5) . ? C10 C11 1.379(5) . ? C11 C12 1.383(5) . ? C12 N2 1.355(4) . ? N1 Cu1 2.060(3) . ? N2 Cu1 2.029(3) . ? Cu1 I1 2.6357(5) . ? Cu1 I1 2.7560(5) 3_677 ? I1 Cu1 2.7560(5) 3_677 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 123.6(3) . . ? C1 C2 C3 118.5(3) . . ? C4 C3 C2 119.1(3) . . ? C3 C4 C5 120.0(4) . . ? N1 C5 C4 121.0(3) . . ? N1 C5 C6 118.3(3) . . ? C4 C5 C6 120.7(3) . . ? C5 C6 S1 113.7(2) . . ? C8 C7 S1 112.9(2) . . ? N2 C8 C9 121.2(3) . . ? N2 C8 C7 117.4(3) . . ? C9 C8 C7 121.4(3) . . ? C10 C9 C8 120.3(3) . . ? C11 C10 C9 118.5(3) . . ? C10 C11 C12 118.9(3) . . ? N2 C12 C11 123.0(3) . . ? C1 N1 C5 117.8(3) . . ? C1 N1 Cu1 115.4(2) . . ? C5 N1 Cu1 126.6(2) . . ? C8 N2 C12 118.1(3) . . ? C8 N2 Cu1 122.2(2) . . ? C12 N2 Cu1 119.6(2) . . ? C7 S1 C6 101.65(15) . . ? N2 Cu1 N1 121.79(11) . . ? N2 Cu1 I1 110.78(8) . . ? N1 Cu1 I1 104.76(7) . . ? N2 Cu1 I1 108.25(7) . 3_677 ? N1 Cu1 I1 102.33(7) . 3_677 ? I1 Cu1 I1 108.028(14) . 3_677 ? Cu1 I1 Cu1 71.972(14) . 3_677 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.197 _refine_diff_density_min -0.803 _refine_diff_density_rms 0.140 #===END data_[Cu2I2L]#Compound 4 _database_code_CSD 175748 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H9 Cu I N2 S' _chemical_formula_weight 367.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.0330(10) _cell_length_b 8.7293(8) _cell_length_c 12.3735(11) _cell_angle_alpha 90.00 _cell_angle_beta 91.4210(10) _cell_angle_gamma 90.00 _cell_volume 1083.35(18) _cell_formula_units_Z 4 _cell_measurement_temperature 158(2) _cell_measurement_reflns_used 2085 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 26.38 _exptl_crystal_description triangular _exptl_crystal_colour red _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.254 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 700 _exptl_absorpt_coefficient_mu 5.018 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3689 _exptl_absorpt_correction_T_max 0.4711 _exptl_absorpt_process_details 'SADABS (Sheldrick 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 158(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemans SMART CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 7329 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0176 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 26.38 _reflns_number_total 2085 _reflns_number_gt 1950 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+2.8776P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2085 _refine_ls_number_parameters 127 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0313 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0729 _refine_ls_wR_factor_gt 0.0709 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.40888(3) -0.00254(3) 0.83354(2) 0.03390(11) Uani 1 1 d . . . Cu1 Cu 0.40857(5) 0.11584(6) 1.03237(4) 0.03417(14) Uani 1 1 d . . . S1 S 0.13477(10) 0.44576(13) 1.08726(9) 0.0371(2) Uani 1 1 d . . . N1 N 0.2214(3) 0.0592(4) 1.0890(3) 0.0303(7) Uani 1 1 d . . . N2 N 0.4608(3) 0.3482(4) 1.0177(2) 0.0287(7) Uani 1 1 d . . . C1 C 0.1711(4) -0.0785(5) 1.0638(3) 0.0367(9) Uani 1 1 d . . . H1 H 0.2174 -0.1385 1.0153 0.044 Uiso 1 1 calc R . . C2 C 0.0553(4) -0.1377(5) 1.1048(3) 0.0377(9) Uani 1 1 d . . . H2 H 0.0254 -0.2348 1.0851 0.045 Uiso 1 1 calc R . . C3 C -0.0148(4) -0.0486(6) 1.1758(4) 0.0397(10) Uani 1 1 d . . . H3 H -0.0931 -0.0845 1.2055 0.048 Uiso 1 1 calc R . . C4 C 0.0333(4) 0.0941(5) 1.2017(3) 0.0359(9) Uani 1 1 d . . . H4 H -0.0129 0.1564 1.2488 0.043 Uiso 1 1 calc R . . C5 C 0.1522(4) 0.1461(5) 1.1573(3) 0.0298(8) Uani 1 1 d . . . C6 C 0.2028(4) 0.3040(5) 1.1815(3) 0.0342(8) Uani 1 1 d . . . H6A H 0.2993 0.3044 1.1780 0.041 Uiso 1 1 calc R . . H6B H 0.1792 0.3320 1.2544 0.041 Uiso 1 1 calc R . . C7 C 0.2301(4) 0.4071(5) 0.9654(3) 0.0335(8) Uani 1 1 d . . . H7A H 0.2256 0.2986 0.9487 0.040 Uiso 1 1 calc R . . H7B H 0.1909 0.4629 0.9048 0.040 Uiso 1 1 calc R . . C8 C 0.3727(4) 0.4536(5) 0.9811(3) 0.0292(8) Uani 1 1 d . . . C9 C 0.5862(4) 0.3962(4) 1.0365(3) 0.0311(8) Uani 1 1 d . . . H9 H 0.6487 0.3258 1.0626 0.037 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.03232(17) 0.03871(18) 0.03077(16) 0.00327(10) 0.00320(11) -0.00041(10) Cu1 0.0288(3) 0.0311(3) 0.0429(3) 0.0009(2) 0.0057(2) -0.0004(2) S1 0.0303(5) 0.0317(5) 0.0496(6) -0.0001(5) 0.0063(4) 0.0025(4) N1 0.0271(16) 0.0290(17) 0.0348(16) -0.0017(14) 0.0033(13) 0.0017(14) N2 0.0280(16) 0.0261(16) 0.0321(16) -0.0018(13) 0.0044(12) -0.0010(13) C1 0.034(2) 0.034(2) 0.042(2) -0.0013(18) 0.0054(17) 0.0027(18) C2 0.035(2) 0.031(2) 0.047(2) 0.0022(18) -0.0033(17) -0.0036(17) C3 0.029(2) 0.045(2) 0.045(2) 0.010(2) 0.0017(17) -0.0062(19) C4 0.030(2) 0.043(2) 0.035(2) -0.0011(18) 0.0074(16) 0.0011(18) C5 0.0279(19) 0.033(2) 0.0281(17) 0.0034(16) -0.0005(14) -0.0005(16) C6 0.032(2) 0.038(2) 0.0318(19) -0.0054(17) 0.0025(15) -0.0014(17) C7 0.029(2) 0.035(2) 0.036(2) 0.0045(17) -0.0009(15) -0.0025(17) C8 0.0279(19) 0.030(2) 0.0293(18) -0.0026(16) 0.0027(14) -0.0004(16) C9 0.0306(19) 0.0272(19) 0.0356(19) 0.0022(16) 0.0023(15) 0.0041(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Cu1 2.6334(6) 3_657 ? I1 Cu1 2.6686(6) . ? Cu1 N1 2.080(3) . ? Cu1 N2 2.104(3) . ? Cu1 I1 2.6334(6) 3_657 ? Cu1 Cu1 2.8584(10) 3_657 ? S1 C6 1.821(4) . ? S1 C7 1.837(4) . ? N1 C1 1.337(6) . ? N1 C5 1.343(5) . ? N2 C9 1.341(5) . ? N2 C8 1.347(5) . ? C1 C2 1.380(6) . ? C2 C3 1.379(7) . ? C3 C4 1.371(7) . ? C4 C5 1.400(5) . ? C5 C6 1.497(6) . ? C7 C8 1.495(5) . ? C8 C9 1.393(6) 3_667 ? C9 C8 1.393(6) 3_667 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cu1 I1 Cu1 65.244(19) 3_657 . ? N1 Cu1 N2 119.17(13) . . ? N1 Cu1 I1 108.55(9) . 3_657 ? N2 Cu1 I1 104.22(9) . 3_657 ? N1 Cu1 I1 103.89(9) . . ? N2 Cu1 I1 106.71(9) . . ? I1 Cu1 I1 114.756(19) 3_657 . ? N1 Cu1 Cu1 121.14(10) . 3_657 ? N2 Cu1 Cu1 119.66(9) . 3_657 ? I1 Cu1 Cu1 57.973(19) 3_657 3_657 ? I1 Cu1 Cu1 56.783(18) . 3_657 ? C6 S1 C7 101.88(19) . . ? C1 N1 C5 117.2(3) . . ? C1 N1 Cu1 118.3(3) . . ? C5 N1 Cu1 124.3(3) . . ? C9 N2 C8 116.7(3) . . ? C9 N2 Cu1 121.4(3) . . ? C8 N2 Cu1 121.7(3) . . ? N1 C1 C2 124.6(4) . . ? C3 C2 C1 118.1(4) . . ? C4 C3 C2 118.6(4) . . ? C3 C4 C5 120.1(4) . . ? N1 C5 C4 121.5(4) . . ? N1 C5 C6 117.9(3) . . ? C4 C5 C6 120.6(4) . . ? C5 C6 S1 112.2(3) . . ? C8 C7 S1 111.1(3) . . ? N2 C8 C9 120.1(3) . 3_667 ? N2 C8 C7 118.4(4) . . ? C9 C8 C7 121.4(4) 3_667 . ? N2 C9 C8 123.1(4) . 3_667 ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 0.930 _refine_diff_density_min -0.823 _refine_diff_density_rms 0.109 #===END