Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Blake, A.' 'Brooks, Neil R.' 'Champness, Neil' 'Crew, Marcello' 'Deveson, Anne' 'Gregory, Duncan H.' 'Hanton, Lyall R.' 'Hubberstey, P.' 'Schroder, M.' _publ_contact_author_name 'Prof M Schroder' _publ_contact_author_address ; Prof M Schroder Department of Chemistry University of Nottingham University Park Nottingham NG7 2RD UNITED KINGDOM ; _publ_contact_author_email 'M.SCHRODER@NOTTINGHAM.AC.UK' _publ_section_title ; Topological isomerism in co-ordination polymers ; data_cuipss _database_code_CSD 116866 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common cuipss _chemical_formula_moiety '(CuI)(NC5H4SSH4C5N).MeCN' _chemical_formula_sum 'C12 H11 Cu I N3 S2' _chemical_formula_weight 451.80 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.745(2) _cell_length_b 8.955(4) _cell_length_c 10.636(3) _cell_angle_alpha 94.48(4) _cell_angle_beta 96.63(3) _cell_angle_gamma 106.11(4) _cell_volume 789.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 220.0(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 12.75 _cell_measurement_theta_max 17.0 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.064 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.39 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.900 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 436 _exptl_absorpt_coefficient_mu 3.591 _exptl_absorpt_correction_type 'psi-scans' _exptl_absorpt_correction_T_min 0.520 _exptl_absorpt_correction_T_max 0.616 _exptl_special_details ; ? ; _diffrn_ambient_temperature 220.0(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 'STOE STADI-4 FOUR-CIRCLE DIFFRACTOMETER D092' _diffrn_measurement_method 'omega-theta' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 'variations +- 3.2%' _diffrn_reflns_number 2775 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0234 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 25.03 _reflns_number_total 2775 _reflns_number_gt 2415 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STADI-4 (stoe & cie, 1996a)' _computing_cell_refinement 'STADI-4 (stoe & cie, 1996a)' _computing_data_reduction 'X-RED (stoe & cie, 1996b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (version 5.03)(Sheldrick, 1994)' _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 w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+4.8943P] 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 2775 _refine_ls_number_parameters 173 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0479 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.0982 _refine_ls_wR_factor_gt 0.0904 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.016 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I I 0.60432(5) 0.81734(5) 0.90995(4) 0.04307(15) Uani 1 d . . . Cu Cu 0.45444(9) 1.03224(8) 0.88760(7) 0.0358(2) Uani 1 d . . . S1 S -0.25800(18) 0.72629(18) 0.53392(16) 0.0390(4) Uani 1 d . . . S2 S -0.27185(19) 0.50363(18) 0.46712(14) 0.0380(4) Uani 1 d . . . N1 N 0.2352(6) 0.9285(6) 0.7751(5) 0.0337(11) Uani 1 d . . . C11 C 0.1758(7) 0.7741(7) 0.7407(6) 0.0344(13) Uani 1 d . . . H11A H 0.2390 0.7088 0.7682 0.041 Uiso 1 calc R . . C12 C 0.0280(7) 0.7040(7) 0.6676(6) 0.0360(13) Uani 1 d . . . H12A H -0.0093 0.5936 0.6468 0.043 Uiso 1 calc R . . C13 C -0.0645(7) 0.7978(7) 0.6254(6) 0.0337(13) Uani 1 d . . . C14 C -0.0060(8) 0.9579(7) 0.6602(6) 0.0394(14) Uani 1 d . . . H14A H -0.0669 1.0255 0.6335 0.047 Uiso 1 calc R . . C15 C 0.1422(8) 1.0172(7) 0.7342(6) 0.0388(14) Uani 1 d . . . H15A H 0.1810 1.1271 0.7578 0.047 Uiso 1 calc R . . N2 N -0.4324(6) 0.1908(6) 0.7732(5) 0.0360(11) Uani 1 d . . . C21 C -0.3949(7) 0.1389(7) 0.6628(6) 0.0381(14) Uani 1 d . . . H21A H -0.4033 0.0308 0.6476 0.046 Uiso 1 calc R . . C22 C -0.3454(8) 0.2319(7) 0.5706(6) 0.0392(14) Uani 1 d . . . H22A H -0.3205 0.1888 0.4938 0.047 Uiso 1 calc R . . C23 C -0.3319(7) 0.3913(6) 0.5911(5) 0.0308(12) Uani 1 d . . . C24 C -0.3686(7) 0.4459(7) 0.7047(6) 0.0373(14) Uani 1 d . . . H24A H -0.3599 0.5538 0.7227 0.045 Uiso 1 calc R . . C25 C -0.4178(8) 0.3445(7) 0.7920(6) 0.0390(14) Uani 1 d . . . H25A H -0.4429 0.3850 0.8697 0.047 Uiso 1 calc R . . N1S N 0.9516(11) 0.6290(10) 1.2234(9) 0.089(3) Uani 1 d . . . C1S C 0.9929(10) 0.6798(9) 1.1370(8) 0.059(2) Uani 1 d . . . C2S C 1.0473(12) 0.7474(14) 1.0250(10) 0.087(3) Uani 1 d . . . H2S1 H 1.1608 0.8083 1.0452 0.130 Uiso 1 calc R . . H2S2 H 0.9831 0.8161 0.9978 0.130 Uiso 1 calc R . . H2S3 H 1.0350 0.6637 0.9562 0.130 Uiso 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 I 0.0511(3) 0.0439(3) 0.0404(3) -0.00206(18) 0.00662(19) 0.0257(2) Cu 0.0375(4) 0.0337(4) 0.0352(4) 0.0032(3) 0.0048(3) 0.0094(3) S1 0.0340(8) 0.0340(8) 0.0476(9) 0.0074(7) -0.0011(7) 0.0094(6) S2 0.0424(9) 0.0359(8) 0.0326(8) 0.0037(6) 0.0041(6) 0.0069(7) N1 0.032(3) 0.032(3) 0.036(3) 0.003(2) 0.005(2) 0.007(2) C11 0.034(3) 0.034(3) 0.039(3) 0.007(3) 0.004(3) 0.015(3) C12 0.037(3) 0.034(3) 0.035(3) 0.006(3) 0.003(3) 0.007(3) C13 0.030(3) 0.036(3) 0.038(3) 0.009(3) 0.006(2) 0.012(2) C14 0.043(4) 0.033(3) 0.048(4) 0.008(3) 0.003(3) 0.020(3) C15 0.042(3) 0.033(3) 0.041(3) 0.003(3) 0.002(3) 0.013(3) N2 0.036(3) 0.033(3) 0.039(3) 0.007(2) 0.008(2) 0.009(2) C21 0.040(3) 0.021(3) 0.050(4) 0.000(3) 0.008(3) 0.005(2) C22 0.041(3) 0.035(3) 0.043(4) 0.003(3) 0.013(3) 0.012(3) C23 0.027(3) 0.027(3) 0.036(3) 0.002(2) 0.002(2) 0.005(2) C24 0.039(3) 0.028(3) 0.044(4) 0.001(3) 0.008(3) 0.010(3) C25 0.045(4) 0.030(3) 0.041(3) 0.000(3) 0.011(3) 0.009(3) N1S 0.117(7) 0.074(5) 0.107(7) 0.043(5) 0.058(6) 0.054(5) C1S 0.065(5) 0.049(4) 0.071(5) 0.017(4) 0.022(4) 0.025(4) C2S 0.066(6) 0.116(9) 0.080(7) 0.034(6) 0.015(5) 0.022(6) _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_noflag I Cu 2.6224(13) . ? I Cu 2.6271(13) 2_677 ? Cu N2 2.060(5) 1_665 ? Cu N1 2.069(5) . ? Cu Cu 2.5916(17) 2_677 ? Cu I 2.6271(13) 2_677 ? S1 C13 1.772(6) . ? S1 S2 2.030(2) . ? S2 C23 1.761(6) . ? N1 C11 1.339(7) . ? N1 C15 1.346(8) . ? C11 C12 1.382(8) . ? C12 C13 1.383(8) . ? C13 C14 1.386(8) . ? C14 C15 1.378(9) . ? N2 C21 1.338(8) . ? N2 C25 1.344(8) . ? N2 Cu 2.060(5) 1_445 ? C21 C22 1.368(9) . ? C22 C23 1.396(8) . ? C23 C24 1.374(8) . ? C24 C25 1.371(9) . ? N1S C1S 1.110(10) . ? C1S C2S 1.448(12) . ? 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_noflag Cu I Cu 59.17(4) . 2_677 ? N2 Cu N1 101.3(2) 1_665 . ? N2 Cu Cu 132.07(15) 1_665 2_677 ? N1 Cu Cu 126.59(15) . 2_677 ? N2 Cu I 109.06(14) 1_665 . ? N1 Cu I 107.43(14) . . ? Cu Cu I 60.51(4) 2_677 . ? N2 Cu I 109.57(15) 1_665 2_677 ? N1 Cu I 106.80(14) . 2_677 ? Cu Cu I 60.33(4) 2_677 2_677 ? I Cu I 120.83(4) . 2_677 ? C13 S1 S2 104.1(2) . . ? C23 S2 S1 105.2(2) . . ? C11 N1 C15 116.3(5) . . ? C11 N1 Cu 123.8(4) . . ? C15 N1 Cu 119.9(4) . . ? N1 C11 C12 124.0(5) . . ? C11 C12 C13 118.7(6) . . ? C12 C13 C14 118.5(6) . . ? C12 C13 S1 124.3(5) . . ? C14 C13 S1 117.2(4) . . ? C15 C14 C13 118.8(5) . . ? N1 C15 C14 123.8(6) . . ? C21 N2 C25 116.4(5) . . ? C21 N2 Cu 119.5(4) . 1_445 ? C25 N2 Cu 123.1(4) . 1_445 ? N2 C21 C22 124.0(5) . . ? C21 C22 C23 119.0(6) . . ? C24 C23 C22 117.4(5) . . ? C24 C23 S2 125.9(5) . . ? C22 C23 S2 116.7(5) . . ? C25 C24 C23 119.9(6) . . ? N2 C25 C24 123.3(6) . . ? N1S C1S C2S 179.4(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C13 S1 S2 C23 83.6(3) . . . . y C15 N1 C11 C12 -0.1(9) . . . . ? N1 C11 C12 C13 0.9(9) . . . . ? C11 C12 C13 C14 -1.1(9) . . . . ? C11 C12 C13 S1 -178.6(5) . . . . ? S2 S1 C13 C12 -16.4(6) . . . . ? S2 S1 C13 C14 166.0(4) . . . . ? C12 C13 C14 C15 0.6(9) . . . . ? S1 C13 C14 C15 178.3(5) . . . . ? C11 N1 C15 C14 -0.5(9) . . . . ? Cu N1 C15 C14 -179.3(5) . . . . ? C13 C14 C15 N1 0.2(10) . . . . ? C25 N2 C21 C22 -0.6(9) . . . . ? Cu N2 C21 C22 168.4(5) 1_445 . . . ? N2 C21 C22 C23 0.1(10) . . . . ? C21 C22 C23 C24 0.5(9) . . . . ? C21 C22 C23 S2 -178.6(5) . . . . ? S1 S2 C23 C24 3.1(6) . . . . ? S1 S2 C23 C22 -177.9(4) . . . . ? C22 C23 C24 C25 -0.6(9) . . . . ? S2 C23 C24 C25 178.4(5) . . . . ? C21 N2 C25 C24 0.4(9) . . . . ? Cu N2 C25 C24 -168.2(5) 1_445 . . . ? C23 C24 C25 N2 0.2(10) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.913 _refine_diff_density_min -1.002 _refine_diff_density_rms 0.127 #===END data_ipyscu _database_code_CSD 164101 _audit_creation_method SHELXL-97 _chemical_name_systematic ; copperiodide bipyridyldisulfide dichloromethane solvate ; _chemical_name_common '(CuI)bpds.CH2CL2' _chemical_formula_moiety '(CuI)(NC5H4C5H4N)(CH2Cl2)' _chemical_formula_sum 'C11 H10 Cl2 Cu I N2 S2' _chemical_formula_weight 495.67 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' 'Cl' 'Cl' 0.1484 0.1585 '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 8.4250(17) _cell_length_b 10.318(2) _cell_length_c 10.670(2) _cell_angle_alpha 113.92(3) _cell_angle_beta 97.23(3) _cell_angle_gamma 92.21(3) _cell_volume 837.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 100 _cell_measurement_theta_min 6.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.967 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 476 _exptl_absorpt_coefficient_mu 3.704 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 'not recorded' _exptl_absorpt_correction_T_max 'not recorded' _exptl_absorpt_process_details 'Habitus (W. Herrendorf, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 STOE_IPDS _diffrn_measurement_method 'area detector frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 5359 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0235 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 28.03 _reflns_number_total 3415 _reflns_number_gt 3255 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE_IPDS software' _computing_cell_refinement 'STOE_IPDS software' _computing_data_reduction 'STOE_IPDS software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (version 5.03)(Sheldrick, 1994)' _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 w=1/[\s^2^(Fo^2^)+(0.0876P)^2^+2.4288P] 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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3415 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0555 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.1496 _refine_ls_wR_factor_gt 0.1483 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.30807(4) 1.65061(3) 0.57235(4) 0.04196(18) Uani 1 d . . . Cu1 Cu 0.38866(7) 1.38992(6) 0.44700(7) 0.03669(19) Uani 1 d . . . S1 S 0.07133(15) 0.96267(12) 0.69510(13) 0.0357(3) Uani 1 d . . . S2 S -0.07213(14) 1.07677(13) 0.83118(13) 0.0365(3) Uani 1 d . . . N1 N 0.2989(5) 1.2652(4) 0.5376(5) 0.0357(8) Uani 1 d . . . C1 C 0.3296(6) 1.1274(5) 0.4962(5) 0.0364(10) Uani 1 d . . . H1A H 0.4016 1.0920 0.4310 0.044 Uiso 1 calc R . . C2 C 0.2611(6) 1.0352(5) 0.5441(5) 0.0366(10) Uani 1 d . . . H2A H 0.2861 0.9392 0.5127 0.044 Uiso 1 calc R . . C3 C 0.1561(5) 1.0861(5) 0.6384(5) 0.0326(9) Uani 1 d . . . C4 C 0.1211(7) 1.2272(5) 0.6815(6) 0.0402(11) Uani 1 d . . . H4A H 0.0479 1.2644 0.7452 0.048 Uiso 1 calc R . . C5 C 0.1963(7) 1.3118(5) 0.6287(6) 0.0420(11) Uani 1 d . . . H5A H 0.1735 1.4084 0.6590 0.050 Uiso 1 calc R . . N2 N 0.2518(5) 1.2988(4) 0.2509(4) 0.0367(8) Uani 1 d . . . C6 C 0.0918(6) 1.3068(6) 0.2351(6) 0.0393(10) Uani 1 d . . . H6A H 0.0451 1.3614 0.3144 0.047 Uiso 1 calc R . . C7 C -0.0066(6) 1.2398(5) 0.1098(6) 0.0389(10) Uani 1 d . . . H7A H -0.1191 1.2473 0.1030 0.047 Uiso 1 calc R . . C8 C 0.0613(6) 1.1602(5) -0.0076(5) 0.0342(9) Uani 1 d . . . C9 C 0.2240(6) 1.1494(6) 0.0064(5) 0.0389(10) Uani 1 d . . . H9A H 0.2736 1.0953 -0.0713 0.047 Uiso 1 calc R . . C10 C 0.3139(6) 1.2201(6) 0.1382(6) 0.0417(11) Uani 1 d . . . H10A H 0.4262 1.2118 0.1484 0.050 Uiso 1 calc R . . C1S C 0.3674(15) 0.6176(16) 0.1773(13) 0.109(4) Uani 1 d . . . H1SA H 0.3410 0.6616 0.2726 0.131 Uiso 1 calc R . . H1SB H 0.4436 0.5461 0.1747 0.131 Uiso 1 calc R . . Cl1 Cl 0.1956(5) 0.5326(3) 0.0647(5) 0.1279(13) Uani 1 d . . . Cl2 Cl 0.4573(5) 0.7428(6) 0.1428(7) 0.1617(19) Uani 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 I1 0.0381(2) 0.0299(2) 0.0601(3) 0.01750(16) 0.01889(15) 0.00458(13) Cu1 0.0391(3) 0.0313(3) 0.0414(4) 0.0156(2) 0.0116(2) -0.0020(2) S1 0.0414(6) 0.0286(5) 0.0397(6) 0.0166(4) 0.0083(4) -0.0024(4) S2 0.0333(5) 0.0385(6) 0.0422(6) 0.0213(5) 0.0078(4) -0.0021(4) N1 0.0376(19) 0.0298(18) 0.044(2) 0.0183(16) 0.0127(16) -0.0008(15) C1 0.036(2) 0.031(2) 0.044(3) 0.0167(19) 0.0122(18) 0.0025(17) C2 0.036(2) 0.031(2) 0.044(3) 0.0165(19) 0.0089(18) 0.0011(17) C3 0.034(2) 0.031(2) 0.035(2) 0.0164(17) 0.0048(16) -0.0048(16) C4 0.049(3) 0.030(2) 0.046(3) 0.0162(19) 0.021(2) 0.0026(18) C5 0.052(3) 0.029(2) 0.050(3) 0.019(2) 0.021(2) 0.0009(19) N2 0.038(2) 0.0347(19) 0.037(2) 0.0131(16) 0.0105(15) -0.0017(15) C6 0.042(2) 0.039(2) 0.040(2) 0.018(2) 0.0131(19) 0.0039(19) C7 0.037(2) 0.039(2) 0.046(3) 0.020(2) 0.0139(19) 0.0034(18) C8 0.036(2) 0.0293(19) 0.041(2) 0.0179(18) 0.0086(17) -0.0024(16) C9 0.036(2) 0.041(2) 0.039(2) 0.015(2) 0.0116(18) 0.0013(18) C10 0.031(2) 0.049(3) 0.043(3) 0.017(2) 0.0083(19) -0.0016(19) C1S 0.094(7) 0.142(11) 0.095(7) 0.067(8) -0.019(6) -0.035(7) Cl1 0.133(3) 0.0839(18) 0.159(3) 0.057(2) -0.021(2) -0.0219(18) Cl2 0.102(2) 0.178(4) 0.209(5) 0.102(4) -0.019(3) -0.049(3) _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 2.6251(9) 2_686 y I1 Cu1 2.6338(11) . y Cu1 N1 2.069(4) . y Cu1 N2 2.075(4) . y Cu1 I1 2.6251(9) 2_686 ? Cu1 Cu1 2.6482(16) 2_686 y S1 C3 1.778(5) . ? S1 S2 2.0299(19) . ? S2 C8 1.789(5) 1_556 ? N1 C5 1.337(7) . ? N1 C1 1.353(6) . ? C1 C2 1.388(7) . ? C2 C3 1.379(7) . ? C3 C4 1.394(7) . ? C4 C5 1.388(7) . ? N2 C10 1.334(7) . ? N2 C6 1.347(7) . ? C6 C7 1.371(8) . ? C7 C8 1.398(7) . ? C8 C9 1.374(7) . ? C8 S2 1.789(5) 1_554 ? C9 C10 1.393(7) . ? C1S Cl2 1.660(13) . ? C1S Cl1 1.709(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 Cu1 I1 Cu1 60.47(4) 2_686 . y N1 Cu1 N2 100.85(17) . . y N1 Cu1 I1 108.85(12) . 2_686 y N2 Cu1 I1 109.71(12) . 2_686 y N1 Cu1 I1 108.80(12) . . y N2 Cu1 I1 107.48(13) . . y I1 Cu1 I1 119.53(4) 2_686 . y N1 Cu1 Cu1 129.85(13) . 2_686 ? N2 Cu1 Cu1 129.28(13) . 2_686 ? I1 Cu1 Cu1 59.93(3) 2_686 2_686 ? I1 Cu1 Cu1 59.60(3) . 2_686 ? C3 S1 S2 104.42(17) . . ? C8 S2 S1 103.85(17) 1_556 . ? C5 N1 C1 117.0(4) . . ? C5 N1 Cu1 121.9(3) . . ? C1 N1 Cu1 120.7(3) . . ? N1 C1 C2 123.3(5) . . ? C3 C2 C1 118.5(4) . . ? C2 C3 C4 119.3(4) . . ? C2 C3 S1 116.4(4) . . ? C4 C3 S1 124.3(4) . . ? C5 C4 C3 118.1(5) . . ? N1 C5 C4 123.7(5) . . ? C10 N2 C6 117.2(4) . . ? C10 N2 Cu1 122.2(4) . . ? C6 N2 Cu1 120.3(3) . . ? N2 C6 C7 123.0(5) . . ? C6 C7 C8 118.9(5) . . ? C9 C8 C7 119.1(5) . . ? C9 C8 S2 123.8(4) . 1_554 ? C7 C8 S2 117.1(4) . 1_554 ? C8 C9 C10 117.8(5) . . ? N2 C10 C9 124.0(5) . . ? Cl2 C1S Cl1 113.7(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cu1 I1 Cu1 N1 125.81(14) 2_686 . . . ? Cu1 I1 Cu1 N2 -125.79(13) 2_686 . . . ? Cu1 I1 Cu1 I1 0.0 2_686 . . 2_686 ? C3 S1 S2 C8 -85.7(2) . . . 1_556 y N2 Cu1 N1 C5 -103.3(4) . . . . ? I1 Cu1 N1 C5 141.4(4) 2_686 . . . ? I1 Cu1 N1 C5 9.6(5) . . . . ? Cu1 Cu1 N1 C5 75.2(5) 2_686 . . . ? N2 Cu1 N1 C1 70.1(4) . . . . ? I1 Cu1 N1 C1 -45.3(4) 2_686 . . . ? I1 Cu1 N1 C1 -177.1(4) . . . . ? Cu1 Cu1 N1 C1 -111.4(4) 2_686 . . . ? C5 N1 C1 C2 -0.4(8) . . . . ? Cu1 N1 C1 C2 -174.1(4) . . . . ? N1 C1 C2 C3 0.2(8) . . . . ? C1 C2 C3 C4 0.5(7) . . . . ? C1 C2 C3 S1 179.6(4) . . . . ? S2 S1 C3 C2 179.6(3) . . . . ? S2 S1 C3 C4 -1.4(5) . . . . ? C2 C3 C4 C5 -1.0(8) . . . . ? S1 C3 C4 C5 180.0(4) . . . . ? C1 N1 C5 C4 -0.1(9) . . . . ? Cu1 N1 C5 C4 173.5(5) . . . . ? C3 C4 C5 N1 0.8(9) . . . . ? N1 Cu1 N2 C10 -108.3(4) . . . . ? I1 Cu1 N2 C10 6.4(4) 2_686 . . . ? I1 Cu1 N2 C10 137.8(4) . . . . ? Cu1 Cu1 N2 C10 73.1(5) 2_686 . . . ? N1 Cu1 N2 C6 65.5(4) . . . . ? I1 Cu1 N2 C6 -179.7(4) 2_686 . . . ? I1 Cu1 N2 C6 -48.3(4) . . . . ? Cu1 Cu1 N2 C6 -113.0(4) 2_686 . . . ? C10 N2 C6 C7 -0.8(8) . . . . ? Cu1 N2 C6 C7 -174.9(4) . . . . ? N2 C6 C7 C8 -0.6(8) . . . . ? C6 C7 C8 C9 1.2(8) . . . . ? C6 C7 C8 S2 -179.2(4) . . . 1_554 ? C7 C8 C9 C10 -0.6(8) . . . . ? S2 C8 C9 C10 179.9(4) 1_554 . . . ? C6 N2 C10 C9 1.5(8) . . . . ? Cu1 N2 C10 C9 175.5(4) . . . . ? C8 C9 C10 N2 -0.8(9) . . . . ? _diffrn_measured_fraction_theta_max 0.844 _diffrn_reflns_theta_full 28.03 _diffrn_measured_fraction_theta_full 0.844 _refine_diff_density_max 1.387 _refine_diff_density_min -1.124 _refine_diff_density_rms 0.125 #===END data_cupysi _database_code_CSD 164102 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(CUI)4(bpds)' _chemical_formula_moiety ' Cu4I4(NC5H4SSC5H4N).0.5EtCN' _chemical_formula_sum 'C11.50 H10.50 Cu2 I2 N2.50 S2' _chemical_formula_weight 628.72 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 Orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 19.493(4) _cell_length_b 10.760(2) _cell_length_c 17.334(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3635.7(13) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.297 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2344 _exptl_absorpt_coefficient_mu 5.957 _exptl_absorpt_correction_type HABITUS _exptl_absorpt_correction_T_min 0.5873 _exptl_absorpt_correction_T_max 0.5873 _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 STOE_IPDS _diffrn_measurement_method 'area detector frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 9227 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 28.12 _reflns_number_total 3999 _reflns_number_gt 3475 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE_IPDS software' _computing_cell_refinement 'STOE_IPDS software' _computing_data_reduction 'STOE_IPDS software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (version 5.03)(Sheldrick, 1994)' _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 w=1/[\s^2^(Fo^2^)+(0.0563P)^2^+3.1045P] 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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3999 _refine_ls_number_parameters 180 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0390 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0949 _refine_ls_wR_factor_gt 0.0916 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.062 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.641927(13) 0.79967(3) 0.106818(18) 0.05205(11) Uani 1 d . . . I2 I 0.715492(13) 0.54920(3) -0.076903(16) 0.04609(10) Uani 1 d . . . Cu1 Cu 0.68526(2) 0.78258(5) -0.03973(3) 0.04869(14) Uani 1 d . . . Cu2 Cu 0.73473(3) 0.62286(5) 0.06639(3) 0.05079(14) Uani 1 d . . . S1 S 0.38703(6) 0.79535(9) -0.30351(6) 0.0484(2) Uani 1 d . . . S2 S 0.41546(6) 0.94656(9) -0.24188(8) 0.0540(3) Uani 1 d . . . N1 N 0.60566(16) 0.8345(3) -0.1069(2) 0.0431(7) Uani 1 d . . . C1 C 0.5705(2) 0.9374(4) -0.0911(3) 0.0518(10) Uani 1 d . . . H1A H 0.5849 0.9876 -0.0491 0.062 Uiso 1 calc R . . C2 C 0.5135(2) 0.9745(4) -0.1333(3) 0.0516(10) Uani 1 d . . . H2A H 0.4903 1.0498 -0.1214 0.062 Uiso 1 calc R . . C3 C 0.49130(18) 0.8998(3) -0.1930(2) 0.0417(8) Uani 1 d . . . C4 C 0.5282(2) 0.7956(4) -0.2108(3) 0.0546(11) Uani 1 d . . . H4A H 0.5151 0.7441 -0.2527 0.066 Uiso 1 calc R . . C5 C 0.5850(2) 0.7666(5) -0.1664(3) 0.0560(11) Uani 1 d . . . H5A H 0.6106 0.6944 -0.1793 0.067 Uiso 1 calc R . . C6 C 0.34878(19) 0.6958(4) -0.2345(3) 0.0423(8) Uani 1 d . . . C7 C 0.3207(2) 0.5873(4) -0.2631(3) 0.0517(10) Uani 1 d . . . H7A H 0.3201 0.5712 -0.3170 0.062 Uiso 1 calc R . . C8 C 0.2937(3) 0.5033(5) -0.2119(3) 0.0597(11) Uani 1 d . . . H8A H 0.2746 0.4288 -0.2319 0.072 Uiso 1 calc R . . C9 C 0.3184(3) 0.6272(5) -0.1099(3) 0.0558(11) Uani 1 d . . . H9A H 0.3171 0.6419 -0.0559 0.067 Uiso 1 calc R . . C10 C 0.3465(2) 0.7177(4) -0.1564(3) 0.0531(10) Uani 1 d . . . H10A H 0.3638 0.7929 -0.1352 0.064 Uiso 1 calc R . . N2 N 0.29277(18) 0.5200(4) -0.1361(2) 0.0485(8) Uani 1 d . . . N10 N 0.4528(6) 0.7619(11) 0.0094(8) 0.088(3) Uiso 0.50 d PD A -1 C20 C 0.4719(6) 0.6769(11) 0.0062(9) 0.074(3) Uiso 0.50 d PD A -1 C30 C 0.5033(12) 0.5595(15) 0.0042(13) 0.123(6) Uiso 0.50 d PD A -1 H30A H 0.5535 0.5692 0.0107 0.147 Uiso 0.50 calc PR A -1 H30B H 0.4860 0.5084 0.0475 0.147 Uiso 0.50 calc PR A -1 C40 C 0.4899(14) 0.499(3) -0.0652(14) 0.150(8) Uiso 0.50 d PD A -1 H40A H 0.4414 0.5092 -0.0785 0.225 Uiso 0.50 calc PR A -1 H40B H 0.5006 0.4106 -0.0599 0.225 Uiso 0.50 calc PR A -1 H40C H 0.5184 0.5353 -0.1060 0.225 Uiso 0.50 calc PR A -1 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 0.03953(15) 0.0694(2) 0.04721(18) -0.00987(12) 0.00885(10) 0.00791(11) I2 0.04793(16) 0.04895(16) 0.04140(16) -0.00921(10) 0.00153(9) 0.00460(10) Cu1 0.0385(2) 0.0597(3) 0.0479(3) -0.0097(2) -0.00887(19) 0.01072(19) Cu2 0.0523(3) 0.0566(3) 0.0435(3) 0.0023(2) 0.0046(2) -0.0040(2) S1 0.0565(5) 0.0483(5) 0.0404(5) 0.0062(4) -0.0129(4) -0.0050(4) S2 0.0571(6) 0.0382(4) 0.0668(7) 0.0049(5) -0.0241(5) 0.0032(4) N1 0.0363(14) 0.0478(16) 0.0452(19) -0.0076(14) -0.0073(12) 0.0064(13) C1 0.053(2) 0.049(2) 0.054(2) -0.0111(19) -0.0125(19) 0.0103(17) C2 0.051(2) 0.044(2) 0.059(3) -0.0090(19) -0.0146(19) 0.0122(17) C3 0.0410(16) 0.0391(17) 0.045(2) 0.0058(16) -0.0087(15) 0.0012(14) C4 0.051(2) 0.061(2) 0.052(3) -0.018(2) -0.0143(19) 0.0098(18) C5 0.051(2) 0.060(2) 0.057(3) -0.020(2) -0.0139(19) 0.0197(19) C6 0.0395(16) 0.0448(18) 0.043(2) 0.0017(16) -0.0076(15) 0.0015(14) C7 0.064(2) 0.054(2) 0.037(2) -0.0031(18) -0.0068(17) -0.015(2) C8 0.074(3) 0.063(3) 0.043(2) -0.007(2) -0.006(2) -0.018(2) C9 0.069(3) 0.055(2) 0.043(2) -0.0053(19) 0.0061(19) -0.009(2) C10 0.063(2) 0.049(2) 0.047(2) -0.0107(19) 0.001(2) -0.0066(18) N2 0.0500(17) 0.0532(19) 0.0423(19) 0.0024(16) -0.0001(14) -0.0076(15) _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 Cu2 2.6394(8) 2_665 y I1 Cu1 2.6833(8) . y I1 Cu2 2.7171(7) . y I2 Cu2 2.6341(8) . y I2 Cu1 2.6587(8) . y I2 Cu1 2.7266(7) 2_665 y Cu1 N1 2.019(3) . y Cu1 Cu2 2.6175(8) 2_665 y Cu1 Cu1 2.6195(10) 2_665 y Cu1 Cu2 2.6957(9) . y Cu1 I2 2.7266(7) 2_665 y Cu2 N2 2.027(4) 5_665 y Cu2 Cu1 2.6175(8) 2_665 y Cu2 I1 2.6394(7) 2_665 y Cu2 Cu2 2.8000(13) 2_665 y S1 C6 1.771(4) . ? S1 S2 2.0238(16) . ? S2 C3 1.777(4) . ? N1 C5 1.327(6) . ? N1 C1 1.331(5) . ? C1 C2 1.389(6) . ? C2 C3 1.379(6) . ? C3 C4 1.367(6) . ? C4 C5 1.384(6) . ? C6 C10 1.374(7) . ? C6 C7 1.382(6) . ? C7 C8 1.371(7) . ? C8 N2 1.328(6) . ? C9 N2 1.335(6) . ? C9 C10 1.379(7) . ? N2 Cu2 2.027(4) 5_665 ? N10 C20 0.989(12) . ? C20 C30 1.404(15) . ? C30 C40 1.390(17) . ? 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 Cu2 I1 Cu1 58.905(17) 2_665 . y Cu2 I1 Cu2 63.01(2) 2_665 . y Cu1 I1 Cu2 59.886(17) . . y Cu2 I2 Cu1 61.235(18) . . y Cu2 I2 Cu1 58.423(17) . 2_665 y Cu1 I2 Cu1 58.19(2) . 2_665 y N1 Cu1 Cu2 139.09(10) . 2_665 ? N1 Cu1 Cu1 144.55(10) . 2_665 ? Cu2 Cu1 Cu1 61.96(2) 2_665 2_665 ? N1 Cu1 I2 106.97(10) . . y Cu2 Cu1 I2 113.92(2) 2_665 . ? Cu1 Cu1 I2 62.20(2) 2_665 . ? N1 Cu1 I1 106.56(10) . . y Cu2 Cu1 I1 59.71(2) 2_665 . ? Cu1 Cu1 I1 108.762(12) 2_665 . ? I2 Cu1 I1 111.34(2) . . y N1 Cu1 Cu2 147.66(11) . . ? Cu2 Cu1 Cu2 63.58(3) 2_665 . ? Cu1 Cu1 Cu2 58.982(18) 2_665 . ? I2 Cu1 Cu2 58.93(2) . . ? I1 Cu1 Cu2 60.68(2) . . ? N1 Cu1 I2 103.03(11) . 2_665 y Cu2 Cu1 I2 59.02(2) 2_665 2_665 ? Cu1 Cu1 I2 59.60(2) 2_665 2_665 ? I2 Cu1 I2 114.36(2) . 2_665 y I1 Cu1 I2 113.68(2) . 2_665 y Cu2 Cu1 I2 109.31(2) . 2_665 ? N2 Cu2 Cu1 150.57(11) 5_665 2_665 ? N2 Cu2 I2 107.21(11) 5_665 . y Cu1 Cu2 I2 62.56(2) 2_665 . ? N2 Cu2 I1 108.80(11) 5_665 2_665 y Cu1 Cu2 I1 61.38(2) 2_665 2_665 ? I2 Cu2 I1 118.37(2) . 2_665 y N2 Cu2 Cu1 142.69(11) 5_665 . ? Cu1 Cu2 Cu1 59.06(3) 2_665 . ? I2 Cu2 Cu1 59.83(2) . . ? I1 Cu2 Cu1 107.80(2) 2_665 . ? N2 Cu2 I1 101.62(11) 5_665 . y Cu1 Cu2 I1 107.81(3) 2_665 . ? I2 Cu2 I1 111.05(2) . . y I1 Cu2 I1 108.47(3) 2_665 . y Cu1 Cu2 I1 59.43(2) . . ? N2 Cu2 Cu2 142.88(11) 5_665 2_665 ? Cu1 Cu2 Cu2 59.57(2) 2_665 2_665 ? I2 Cu2 Cu2 108.924(15) . 2_665 ? I1 Cu2 Cu2 59.851(19) 2_665 2_665 ? Cu1 Cu2 Cu2 56.85(2) . 2_665 ? I1 Cu2 Cu2 57.14(2) . 2_665 ? C6 S1 S2 104.18(15) . . ? C3 S2 S1 104.60(14) . . ? C5 N1 C1 117.5(3) . . ? C5 N1 Cu1 122.0(3) . . ? C1 N1 Cu1 120.5(3) . . ? N1 C1 C2 122.9(4) . . ? C3 C2 C1 118.5(4) . . ? C4 C3 C2 118.8(3) . . ? C4 C3 S2 124.2(3) . . ? C2 C3 S2 117.0(3) . . ? C3 C4 C5 118.8(4) . . ? N1 C5 C4 123.4(4) . . ? C10 C6 C7 119.1(4) . . ? C10 C6 S1 125.1(3) . . ? C7 C6 S1 115.8(3) . . ? C8 C7 C6 118.4(4) . . ? N2 C8 C7 123.9(4) . . ? N2 C9 C10 124.1(5) . . ? C6 C10 C9 117.8(4) . . ? C8 N2 C9 116.6(4) . . ? C8 N2 Cu2 119.4(3) . 5_665 ? C9 N2 Cu2 123.5(3) . 5_665 ? N10 C20 C30 176.0(17) . . ? C40 C30 C20 111(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 S1 S2 C3 77.4(2) . . . . y C5 N1 C1 C2 0.9(7) . . . . ? N1 C1 C2 C3 1.8(8) . . . . ? C1 C2 C3 C4 -3.3(7) . . . . ? C1 C2 C3 S2 176.6(4) . . . . ? S1 S2 C3 C4 14.1(4) . . . . ? S1 S2 C3 C2 -165.7(3) . . . . ? C2 C3 C4 C5 2.3(7) . . . . ? S2 C3 C4 C5 -177.6(4) . . . . ? C1 N1 C5 C4 -2.0(8) . . . . ? C3 C4 C5 N1 0.4(8) . . . . ? S2 S1 C6 C10 -5.3(4) . . . . ? S2 S1 C6 C7 176.1(3) . . . . ? C10 C6 C7 C8 -2.3(7) . . . . ? S1 C6 C7 C8 176.5(4) . . . . ? C6 C7 C8 N2 0.1(8) . . . . ? C7 C6 C10 C9 2.4(7) . . . . ? S1 C6 C10 C9 -176.2(4) . . . . ? N2 C9 C10 C6 -0.5(8) . . . . ? C7 C8 N2 C9 1.8(8) . . . . ? C10 C9 N2 C8 -1.6(8) . . . . ? N10 C20 C30 C40 -140(26) . . . . ? _diffrn_measured_fraction_theta_max 0.808 _diffrn_reflns_theta_full 28.12 _diffrn_measured_fraction_theta_full 0.808 _refine_diff_density_max 0.751 _refine_diff_density_min -0.916 _refine_diff_density_rms 0.095 #===END data_BPDSI1 _database_code_CSD 164103 _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(4-pyridyl)disulphide bis(copper(I) iodide) ; _chemical_name_common '[(Cu4I4)(bpds)2]' _chemical_formula_moiety 'C22 H19 Cu4 I4 N5 S4' _chemical_formula_sum 'C22 H19 Cu4 I4 N5 S4' _chemical_formula_weight 1243.43 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.878(1) _cell_length_b 10.212(1) _cell_length_c 19.307(2) _cell_angle_alpha 90.249(2) _cell_angle_beta 103.023(2) _cell_angle_gamma 92.796(2) _cell_volume 1703.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4818 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 28.45 _exptl_crystal_description column _exptl_crystal_colour ' pale yellow ' _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.419 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1150 _exptl_absorpt_coefficient_mu 6.356 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.459 _exptl_absorpt_correction_T_max 0.629 _exptl_absorpt_process_details 'SADABS (Bruker, 1999b)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 17087 _diffrn_reflns_av_R_equivalents 0.024 _diffrn_reflns_av_sigmaI/netI 0.024 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 28.62 _reflns_number_total 7690 _reflns_number_gt 6494 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART version 5.054 (Bruker, 1998)' _computing_cell_refinement 'SAINT version 6.01 (Bruker, 1999a)' _computing_data_reduction 'SAINT; SHELXTL (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC version 5.03 (Sheldrick, 1994)' _computing_publication_material 'SHELXL-97; PLATON (Spek, 2000)' _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 w=1/[\s^2^(Fo^2^)+(0.0385P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary 'difference Fourier synthesis' _atom_sites_solution_hydrogens 'placed geometrically' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7690 _refine_ls_number_parameters 337 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0335 _refine_ls_R_factor_gt 0.0255 _refine_ls_wR_factor_ref 0.0643 _refine_ls_wR_factor_gt 0.0617 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.06266(5) 0.67039(5) 0.81487(2) 0.02995(11) Uani 1 1 d . . . Cu2 Cu 0.13469(5) 0.46132(4) 0.75026(3) 0.03038(11) Uani 1 1 d . . . Cu3 Cu -0.16107(6) 0.53424(5) 0.72371(3) 0.03468(12) Uani 1 1 d . . . Cu4 Cu 0.04271(5) 0.67847(4) 0.67644(2) 0.02851(10) Uani 1 1 d . . . I1 I -0.05060(3) 0.42395(2) 0.844148(13) 0.03250(7) Uani 1 1 d . . . I2 I 0.32626(3) 0.67655(2) 0.772023(13) 0.02790(6) Uani 1 1 d . . . I3 I -0.17234(3) 0.79080(2) 0.729606(12) 0.02875(6) Uani 1 1 d . . . I4 I -0.00517(3) 0.44284(2) 0.613998(12) 0.02687(6) Uani 1 1 d . . . N1 N 0.1101(3) 0.7640(3) 0.91068(15) 0.0257(6) Uani 1 1 d . . . C2 C 0.2531(5) 0.8143(4) 0.9415(2) 0.0318(8) Uani 1 1 d . . . H2A H 0.3333 0.8078 0.9166 0.038 Uiso 1 1 calc R . . C3 C 0.2881(4) 0.8751(4) 1.0082(2) 0.0306(8) Uani 1 1 d . . . H3A H 0.3904 0.9087 1.0282 0.037 Uiso 1 1 calc R . . C4 C 0.1740(4) 0.8863(3) 1.04484(18) 0.0238(7) Uani 1 1 d . . . C5 C 0.0240(4) 0.8345(3) 1.01299(19) 0.0251(7) Uani 1 1 d . . . H5A H -0.0582 0.8398 1.0368 0.030 Uiso 1 1 calc R . . C6 C -0.0006(4) 0.7764(3) 0.94693(19) 0.0249(7) Uani 1 1 d . . . H6A H -0.1023 0.7430 0.9256 0.030 Uiso 1 1 calc R . . S7 S 0.19735(11) 0.95762(9) 1.13046(5) 0.02776(19) Uani 1 1 d . . . S8 S 0.41866(11) 1.03444(9) 1.15440(5) 0.0297(2) Uani 1 1 d . . . N11 N 0.7258(4) 0.6915(3) 1.22397(18) 0.0319(7) Uani 1 1 d . . . C12 C 0.7829(5) 0.8157(4) 1.2206(2) 0.0388(10) Uani 1 1 d . . . H12A H 0.8920 0.8317 1.2328 0.047 Uiso 1 1 calc R . . C13 C 0.6922(5) 0.9201(4) 1.2004(2) 0.0360(9) Uani 1 1 d . . . H13A H 0.7376 1.0059 1.1990 0.043 Uiso 1 1 calc R . . C14 C 0.5328(4) 0.8973(3) 1.18213(18) 0.0247(7) Uani 1 1 d . . . C15 C 0.4719(4) 0.7707(4) 1.1851(2) 0.0302(8) Uani 1 1 d . . . H15A H 0.3632 0.7521 1.1730 0.036 Uiso 1 1 calc R . . C16 C 0.5719(4) 0.6724(4) 1.2059(2) 0.0323(8) Uani 1 1 d . . . H16A H 0.5291 0.5857 1.2076 0.039 Uiso 1 1 calc R . . N21 N -0.3630(3) 0.4504(3) 0.66815(17) 0.0297(7) Uani 1 1 d . . . C22 C -0.4691(4) 0.5214(4) 0.6261(2) 0.0321(8) Uani 1 1 d . . . H22A H -0.4644 0.6135 0.6343 0.039 Uiso 1 1 calc R . . C23 C -0.5836(4) 0.4690(4) 0.5722(2) 0.0329(8) Uani 1 1 d . . . H23A H -0.6551 0.5237 0.5434 0.039 Uiso 1 1 calc R . . C24 C -0.5936(4) 0.3342(4) 0.5602(2) 0.0291(8) Uani 1 1 d . . . C25 C -0.4905(4) 0.2572(4) 0.6051(2) 0.0291(8) Uani 1 1 d . . . H25A H -0.4976 0.1644 0.6001 0.035 Uiso 1 1 calc R . . C26 C -0.3770(4) 0.3199(4) 0.6576(2) 0.0310(8) Uani 1 1 d . . . H26A H -0.3050 0.2675 0.6878 0.037 Uiso 1 1 calc R . . S27 S -0.74179(12) 0.27406(9) 0.48760(5) 0.0344(2) Uani 1 1 d . . . S28 S -0.68275(12) 0.08989(10) 0.46958(5) 0.0338(2) Uani 1 1 d . . . N31 N -0.8976(3) -0.1882(3) 0.60838(16) 0.0262(6) Uani 1 1 d . . . C32 C -0.8411(5) -0.2281(4) 0.5533(2) 0.0321(8) Uani 1 1 d . . . H32A H -0.8467 -0.3194 0.5426 0.038 Uiso 1 1 calc R . . C33 C -0.7760(5) -0.1449(4) 0.5118(2) 0.0346(9) Uani 1 1 d . . . H33A H -0.7353 -0.1780 0.4741 0.042 Uiso 1 1 calc R . . C34 C -0.7704(4) -0.0116(4) 0.52548(19) 0.0282(8) Uani 1 1 d . . . C35 C -0.8308(5) 0.0333(4) 0.5807(2) 0.0325(8) Uani 1 1 d . . . H35A H -0.8295 0.1243 0.5912 0.039 Uiso 1 1 calc R . . C36 C -0.8938(5) -0.0597(4) 0.6207(2) 0.0306(8) Uani 1 1 d . . . H36A H -0.9361 -0.0294 0.6585 0.037 Uiso 1 1 calc R . . N1S N 0.6395(5) 0.7486(5) 1.0136(2) 0.0625(12) Uiso 1 1 d . . . C1S C 0.6656(7) 0.6449(5) 1.0015(3) 0.0593(13) Uiso 1 1 d . . . C2S C 0.7027(8) 0.5090(7) 0.9885(4) 0.0791(18) 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 0.0316(3) 0.0345(2) 0.0219(2) -0.00700(18) 0.00368(19) -0.00438(19) Cu2 0.0288(2) 0.0249(2) 0.0350(3) -0.00051(19) 0.0019(2) 0.00295(18) Cu3 0.0275(2) 0.0357(3) 0.0359(3) 0.0005(2) -0.0012(2) -0.00765(19) Cu4 0.0366(3) 0.0257(2) 0.0249(2) -0.00038(18) 0.0107(2) -0.00055(18) I1 0.03728(14) 0.03089(13) 0.02888(13) 0.00460(10) 0.00827(11) -0.00685(10) I2 0.02424(12) 0.02530(12) 0.03306(13) -0.00596(9) 0.00536(10) -0.00395(9) I3 0.03055(13) 0.03124(13) 0.02478(12) -0.00466(9) 0.00611(10) 0.00578(9) I4 0.02983(13) 0.02615(12) 0.02458(12) -0.00666(9) 0.00692(10) -0.00231(9) N1 0.0270(16) 0.0283(15) 0.0198(15) -0.0006(12) 0.0018(13) -0.0009(12) C2 0.030(2) 0.036(2) 0.029(2) -0.0059(16) 0.0061(16) -0.0030(16) C3 0.0265(19) 0.033(2) 0.029(2) -0.0048(15) 0.0012(16) -0.0031(15) C4 0.0294(19) 0.0172(15) 0.0221(17) -0.0002(13) -0.0001(15) 0.0035(13) C5 0.0223(18) 0.0286(18) 0.0238(18) 0.0008(14) 0.0032(14) 0.0039(14) C6 0.0197(17) 0.0242(17) 0.0285(19) 0.0000(14) 0.0006(15) 0.0007(13) S7 0.0266(5) 0.0313(5) 0.0233(4) -0.0074(4) 0.0005(4) 0.0047(4) S8 0.0304(5) 0.0227(4) 0.0308(5) -0.0048(4) -0.0037(4) 0.0019(3) N11 0.0282(17) 0.0291(16) 0.0362(18) 0.0011(14) 0.0027(14) 0.0022(13) C12 0.026(2) 0.029(2) 0.056(3) -0.0057(18) -0.0042(19) -0.0008(15) C13 0.032(2) 0.0259(19) 0.045(2) -0.0050(17) -0.0018(18) -0.0031(15) C14 0.0278(19) 0.0253(17) 0.0202(17) -0.0017(13) 0.0028(15) 0.0051(14) C15 0.0240(19) 0.0317(19) 0.035(2) 0.0036(16) 0.0064(16) 0.0015(15) C16 0.029(2) 0.0255(18) 0.043(2) 0.0053(16) 0.0101(18) 0.0005(15) N21 0.0218(16) 0.0377(18) 0.0290(17) -0.0029(13) 0.0058(13) -0.0041(13) C22 0.0264(19) 0.032(2) 0.039(2) -0.0019(16) 0.0103(17) -0.0015(15) C23 0.0248(19) 0.035(2) 0.039(2) 0.0027(17) 0.0056(17) 0.0034(15) C24 0.0218(18) 0.038(2) 0.028(2) -0.0011(16) 0.0086(16) -0.0033(15) C25 0.0274(19) 0.0292(19) 0.031(2) -0.0010(15) 0.0072(16) -0.0019(15) C26 0.0240(19) 0.037(2) 0.030(2) 0.0023(16) 0.0036(16) -0.0016(15) S27 0.0329(5) 0.0307(5) 0.0345(5) 0.0027(4) -0.0024(4) -0.0024(4) S28 0.0413(6) 0.0318(5) 0.0290(5) -0.0001(4) 0.0108(4) -0.0061(4) N31 0.0262(16) 0.0291(16) 0.0228(15) -0.0015(12) 0.0050(13) 0.0004(12) C32 0.039(2) 0.0292(19) 0.030(2) -0.0052(15) 0.0123(17) -0.0003(16) C33 0.041(2) 0.035(2) 0.030(2) -0.0047(16) 0.0139(18) -0.0041(17) C34 0.0245(19) 0.035(2) 0.0232(18) 0.0047(15) 0.0030(15) -0.0020(15) C35 0.036(2) 0.0273(19) 0.034(2) -0.0012(16) 0.0084(17) -0.0037(15) C36 0.035(2) 0.0311(19) 0.0272(19) -0.0054(15) 0.0113(17) -0.0038(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 Cu1 N1 2.027(3) . y Cu2 N11 2.033(3) 2_667 y Cu3 N21 2.018(3) . y Cu4 N31 2.030(3) 1_665 y Cu1 I1 2.7724(6) . y Cu1 I2 2.6502(6) . y Cu1 I3 2.7008(6) . y Cu2 I1 2.7251(6) . y Cu2 I2 2.6843(5) . y Cu2 I4 2.6456(6) . y Cu3 I1 2.5962(6) . y Cu3 I3 2.6296(6) . y Cu3 I4 2.9502(6) . y Cu4 I2 2.7666(6) . y Cu4 I3 2.6648(6) . y Cu4 I4 2.6587(5) . y Cu1 Cu2 2.6443(7) . y Cu1 Cu3 2.6665(7) . y Cu1 Cu4 2.6402(7) . y Cu2 Cu3 2.7017(7) . y Cu2 Cu4 2.7009(6) . y Cu3 Cu4 2.6021(7) . y N1 C6 1.339(5) . ? N1 C2 1.350(5) . ? C2 C3 1.390(5) . ? C3 C4 1.369(5) . ? C4 C5 1.410(5) . ? C4 S7 1.768(4) . ? C5 C6 1.372(5) . ? S7 S8 2.0314(14) . ? S8 C14 1.781(3) . ? N11 C16 1.336(5) . ? N11 C12 1.350(5) . ? N11 Cu2 2.033(3) 2_667 ? C12 C13 1.372(5) . ? C13 C14 1.387(5) . ? C14 C15 1.384(5) . ? C15 C16 1.373(5) . ? N21 C22 1.341(5) . ? N21 C26 1.343(5) . ? C22 C23 1.367(5) . ? C23 C24 1.390(5) . ? C24 C25 1.388(5) . ? C24 S27 1.776(4) . ? C25 C26 1.387(5) . ? S27 S28 2.0263(15) . ? S28 C34 1.776(4) . ? N31 C36 1.330(5) . ? N31 C32 1.344(5) . ? N31 Cu4 2.030(3) 1_445 ? C32 C33 1.366(5) . ? C33 C34 1.381(5) . ? C34 C35 1.383(5) . ? C35 C36 1.399(5) . ? N1S C1S 1.129(7) . ? C1S C2S 1.476(8) . ? 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 Cu4 149.17(8) . . ? N1 Cu1 Cu2 141.45(9) . . ? Cu4 Cu1 Cu2 61.473(17) . . ? N1 Cu1 I2 106.10(9) . . y Cu4 Cu1 I2 63.061(16) . . ? Cu2 Cu1 I2 60.927(16) . . ? N1 Cu1 Cu3 142.48(9) . . ? Cu4 Cu1 Cu3 58.724(18) . . ? Cu2 Cu1 Cu3 61.156(19) . . ? I2 Cu1 Cu3 111.26(2) . . ? N1 Cu1 I3 107.57(9) . . y Cu4 Cu1 I3 59.845(15) . . ? Cu2 Cu1 I3 110.66(2) . . ? I2 Cu1 I3 115.606(19) . . y Cu3 Cu1 I3 58.669(17) . . ? N1 Cu1 I1 103.40(8) . . y Cu4 Cu1 I1 107.249(19) . . ? Cu2 Cu1 I1 60.354(16) . . ? I2 Cu1 I1 115.678(19) . . y Cu3 Cu1 I1 56.985(15) . . ? I3 Cu1 I1 107.495(18) . . y N11 Cu2 Cu1 137.33(10) 2_667 . ? N11 Cu2 I4 109.31(10) 2_667 . y Cu1 Cu2 I4 113.34(2) . . ? N11 Cu2 I2 105.16(9) 2_667 . y Cu1 Cu2 I2 59.644(16) . . ? I4 Cu2 I2 109.169(18) . . y N11 Cu2 Cu4 153.20(10) 2_667 . ? Cu1 Cu2 Cu4 59.188(18) . . ? I4 Cu2 Cu4 59.628(15) . . ? I2 Cu2 Cu4 61.827(16) . . ? N11 Cu2 Cu3 144.67(9) 2_667 . ? Cu1 Cu2 Cu3 59.826(17) . . ? I4 Cu2 Cu3 66.961(16) . . ? I2 Cu2 Cu3 109.13(2) . . ? Cu4 Cu2 Cu3 57.584(17) . . ? N11 Cu2 I1 99.88(9) 2_667 . y Cu1 Cu2 I1 62.151(16) . . ? I4 Cu2 I1 116.03(2) . . y I2 Cu2 I1 116.141(19) . . y Cu4 Cu2 I1 106.890(19) . . ? Cu3 Cu2 I1 57.161(16) . . ? N21 Cu3 I1 114.41(9) . . y N21 Cu3 Cu4 128.23(9) . . ? I1 Cu3 Cu4 113.96(2) . . ? N21 Cu3 I3 111.28(9) . . y I1 Cu3 I3 115.26(2) . . y Cu4 Cu3 I3 61.239(16) . . ? N21 Cu3 Cu1 166.39(9) . . ? I1 Cu3 Cu1 63.563(17) . . ? Cu4 Cu3 Cu1 60.135(18) . . ? I3 Cu3 Cu1 61.319(16) . . ? N21 Cu3 Cu2 133.24(9) . . ? I1 Cu3 Cu2 61.873(16) . . ? Cu4 Cu3 Cu2 61.192(19) . . ? I3 Cu3 Cu2 111.084(19) . . ? Cu1 Cu3 Cu2 59.018(18) . . ? N21 Cu3 I4 89.69(9) . . y I1 Cu3 I4 110.27(2) . . y Cu4 Cu3 I4 56.803(16) . . ? I3 Cu3 I4 113.274(18) . . y Cu1 Cu3 I4 103.68(2) . . ? Cu2 Cu3 I4 55.611(16) . . ? N31 Cu4 Cu3 152.00(9) 1_665 . ? N31 Cu4 Cu1 135.50(9) 1_665 . ? Cu3 Cu4 Cu1 61.142(18) . . ? N31 Cu4 I4 109.66(9) 1_665 . y Cu3 Cu4 I4 68.213(17) . . ? Cu1 Cu4 I4 113.049(19) . . ? N31 Cu4 I3 104.88(9) 1_665 . y Cu3 Cu4 I3 59.891(17) . . ? Cu1 Cu4 I3 61.207(15) . . ? I4 Cu4 I3 122.341(19) . . y N31 Cu4 Cu2 143.47(9) 1_665 . ? Cu3 Cu4 Cu2 61.224(18) . . ? Cu1 Cu4 Cu2 59.338(18) . . ? I4 Cu4 Cu2 59.153(16) . . ? I3 Cu4 Cu2 110.03(2) . . ? N31 Cu4 I2 97.88(9) 1_665 . y Cu3 Cu4 I2 109.61(2) . . ? Cu1 Cu4 I2 58.646(16) . . ? I4 Cu4 I2 106.368(17) . . y I3 Cu4 I2 112.950(19) . . y Cu2 Cu4 I2 58.791(15) . . ? Cu3 I1 Cu2 60.967(17) . . y Cu3 I1 Cu1 59.452(15) . . y Cu2 I1 Cu1 57.495(14) . . y Cu1 I2 Cu2 59.429(16) . . y Cu1 I2 Cu4 58.293(16) . . y Cu2 I2 Cu4 59.382(15) . . y Cu3 I3 Cu4 58.871(15) . . y Cu3 I3 Cu1 60.012(15) . . y Cu4 I3 Cu1 58.947(16) . . y Cu2 I4 Cu4 61.220(15) . . y Cu2 I4 Cu3 57.428(16) . . y Cu4 I4 Cu3 54.984(14) . . y C6 N1 C2 117.0(3) . . ? C6 N1 Cu1 120.7(2) . . ? C2 N1 Cu1 122.3(3) . . ? N1 C2 C3 122.8(4) . . ? C4 C3 C2 119.5(4) . . ? C3 C4 C5 118.0(3) . . ? C3 C4 S7 125.9(3) . . ? C5 C4 S7 116.1(3) . . ? C6 C5 C4 118.7(3) . . ? N1 C6 C5 123.9(3) . . ? C4 S7 S8 104.59(13) . . ? C14 S8 S7 104.29(13) . . ? C16 N11 C12 116.5(3) . . ? C16 N11 Cu2 121.2(3) . 2_667 ? C12 N11 Cu2 122.2(3) . 2_667 ? N11 C12 C13 123.7(4) . . ? C12 C13 C14 118.5(4) . . ? C15 C14 C13 118.7(3) . . ? C15 C14 S8 124.0(3) . . ? C13 C14 S8 117.3(3) . . ? C16 C15 C14 118.6(3) . . ? N11 C16 C15 123.9(3) . . ? C22 N21 C26 116.8(3) . . ? C22 N21 Cu3 121.3(3) . . ? C26 N21 Cu3 119.6(3) . . ? N21 C22 C23 123.8(4) . . ? C22 C23 C24 118.9(4) . . ? C25 C24 C23 118.7(3) . . ? C25 C24 S27 125.1(3) . . ? C23 C24 S27 116.2(3) . . ? C26 C25 C24 118.0(3) . . ? N21 C26 C25 123.7(4) . . ? C24 S27 S28 104.45(14) . . ? C34 S28 S27 105.14(14) . . ? C36 N31 C32 117.1(3) . . ? C36 N31 Cu4 122.3(3) . 1_445 ? C32 N31 Cu4 120.0(2) . 1_445 ? N31 C32 C33 123.7(4) . . ? C32 C33 C34 118.9(4) . . ? C33 C34 C35 119.0(3) . . ? C33 C34 S28 116.1(3) . . ? C35 C34 S28 124.8(3) . . ? C34 C35 C36 117.9(3) . . ? N31 C36 C35 123.3(4) . . ? N1S C1S C2S 177.8(7) . . ? _diffrn_measured_fraction_theta_max 0.881 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.73 _refine_diff_density_min -0.67 _refine_diff_density_rms 0.12 #===END