data_Ligand_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15H13N5S2' _chemical_formula_sum 'C30 H26 N10 S4' _chemical_formula_weight 654.85 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 6.3410(5) _cell_length_b 12.2842(11) _cell_length_c 20.2427(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.296(2) _cell_angle_gamma 90.00 _cell_volume 1576.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10096 _cell_measurement_theta_min 1.94 _cell_measurement_theta_max 27.84 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.379 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 0.341 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9571 _exptl_absorpt_correction_T_max 0.9733 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10096 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_sigmaI/netI 0.0787 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 27.84 _reflns_number_total 5209 _reflns_number_gt 3563 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0891P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.20(14) _refine_ls_number_reflns 5209 _refine_ls_number_parameters 397 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1170 _refine_ls_R_factor_gt 0.0802 _refine_ls_wR_factor_ref 0.1860 _refine_ls_wR_factor_gt 0.1663 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 S4 S 1.1538(2) 0.15321(15) 0.77501(7) 0.0455(5) Uani 1 1 d . . . S3 S 1.1577(3) 0.22476(17) 0.48103(8) 0.0516(5) Uani 1 1 d . . . N8 N 0.9680(7) 0.1863(4) 0.6262(2) 0.0341(12) Uani 1 1 d . . . C27 C 0.9796(10) 0.0781(6) 0.8229(3) 0.0337(15) Uani 1 1 d . . . N6 N 0.7777(9) 0.2725(6) 0.4304(3) 0.0504(16) Uani 1 1 d . . . C25 C 0.8588(9) 0.2135(6) 0.6800(3) 0.0343(14) Uani 1 1 d . . . C26 C 0.9833(10) 0.2541(6) 0.7380(3) 0.0441(16) Uani 1 1 d . . . H26A H 0.8862 0.2804 0.7712 0.053 Uiso 1 1 calc R . . H26B H 1.0686 0.3154 0.7239 0.053 Uiso 1 1 calc R . . C21 C 0.8645(10) 0.1513(6) 0.5732(3) 0.0385(15) Uani 1 1 d . . . C24 C 0.6410(9) 0.2049(6) 0.6826(3) 0.0397(15) Uani 1 1 d . . . H24 H 0.5689 0.2219 0.7211 0.048 Uiso 1 1 calc R . . C19 C 0.9830(11) 0.2934(6) 0.4278(3) 0.0443(18) Uani 1 1 d . . . N10 N 0.7781(8) 0.1009(5) 0.8251(2) 0.0441(15) Uani 1 1 d . . . C22 C 0.6462(10) 0.1425(6) 0.5719(3) 0.0437(17) Uani 1 1 d . . . H22 H 0.5775 0.1178 0.5341 0.052 Uiso 1 1 calc R . . N9 N 1.0773(10) -0.0011(6) 0.8567(3) 0.0555(17) Uani 1 1 d . . . N7 N 1.0794(9) 0.3657(5) 0.3896(3) 0.0515(16) Uani 1 1 d . . . C30 C 0.6575(12) 0.0389(7) 0.8631(4) 0.057(2) Uani 1 1 d . . . H30 H 0.5131 0.0519 0.8644 0.068 Uiso 1 1 calc R . . C23 C 0.5329(10) 0.1706(7) 0.6268(3) 0.0510(18) Uani 1 1 d . . . H23 H 0.3864 0.1667 0.6266 0.061 Uiso 1 1 calc R . . C16 C 0.6610(14) 0.3329(9) 0.3873(4) 0.075(3) Uani 1 1 d . . . H16 H 0.5157 0.3227 0.3866 0.090 Uiso 1 1 calc R . . C20 C 0.9944(11) 0.1166(6) 0.5151(3) 0.0475(17) Uani 1 1 d . . . H20A H 0.9007 0.0899 0.4808 0.057 Uiso 1 1 calc R . . H20B H 1.0848 0.0568 0.5285 0.057 Uiso 1 1 calc R . . C28 C 0.9519(15) -0.0609(8) 0.8960(4) 0.062(2) Uani 1 1 d . . . H28 H 1.0122 -0.1162 0.9212 0.075 Uiso 1 1 calc R . . C18 C 0.9553(16) 0.4203(7) 0.3489(4) 0.062(2) Uani 1 1 d . . . H18 H 1.0168 0.4710 0.3208 0.075 Uiso 1 1 calc R . . C29 C 0.7407(13) -0.0437(7) 0.9004(4) 0.060(2) Uani 1 1 d . . . H29 H 0.6563 -0.0862 0.9276 0.071 Uiso 1 1 calc R . . C17 C 0.7442(17) 0.4067(7) 0.3457(4) 0.068(2) Uani 1 1 d . . . H17 H 0.6607 0.4462 0.3163 0.081 Uiso 1 1 calc R . . S1 S 0.0283(2) 0.20754(16) -0.01989(7) 0.0470(5) Uani 1 1 d . . . S2 S 0.0334(3) 0.12900(17) 0.27536(8) 0.0530(5) Uani 1 1 d . . . N3 N 0.2167(7) 0.1709(4) 0.1287(2) 0.0354(12) Uani 1 1 d . . . N5 N 0.4119(10) 0.0888(6) 0.3259(3) 0.0559(18) Uani 1 1 d . . . C10 C 0.3200(9) 0.2077(5) 0.1820(3) 0.0335(14) Uani 1 1 d . . . N2 N 0.3975(8) 0.2668(5) -0.0714(2) 0.0391(14) Uani 1 1 d . . . C4 C 0.1961(9) 0.2878(6) -0.0679(3) 0.0396(16) Uani 1 1 d . . . C5 C 0.2061(10) 0.1083(6) 0.0166(3) 0.0413(15) Uani 1 1 d . . . H5A H 0.1251 0.0455 0.0306 0.050 Uiso 1 1 calc R . . H5B H 0.3048 0.0842 -0.0168 0.050 Uiso 1 1 calc R . . C9 C 0.5372(10) 0.2226(6) 0.1824(3) 0.0466(18) Uani 1 1 d . . . H9 H 0.6062 0.2460 0.2205 0.056 Uiso 1 1 calc R . . C6 C 0.3274(9) 0.1512(6) 0.0745(3) 0.0345(14) Uani 1 1 d . . . C7 C 0.5430(10) 0.1665(7) 0.0716(3) 0.0478(19) Uani 1 1 d . . . H7 H 0.6152 0.1522 0.0326 0.057 Uiso 1 1 calc R . . C12 C 0.2126(10) 0.0629(6) 0.3272(3) 0.0437(17) Uani 1 1 d . . . N1 N 0.0915(9) 0.3682(5) -0.1000(3) 0.0509(15) Uani 1 1 d . . . C8 C 0.6486(10) 0.2022(7) 0.1255(3) 0.053(2) Uani 1 1 d . . . H8 H 0.7938 0.2128 0.1242 0.064 Uiso 1 1 calc R . . C11 C 0.1893(10) 0.2366(5) 0.2413(3) 0.0456(17) Uani 1 1 d . . . H11A H 0.0957 0.2958 0.2292 0.055 Uiso 1 1 calc R . . H11B H 0.2832 0.2634 0.2756 0.055 Uiso 1 1 calc R . . C3 C 0.5105(12) 0.3312(7) -0.1113(4) 0.054(2) Uani 1 1 d . . . H3 H 0.6554 0.3204 -0.1141 0.064 Uiso 1 1 calc R . . C13 C 0.5388(14) 0.0349(8) 0.3678(4) 0.068(2) Uani 1 1 d . . . H13 H 0.6820 0.0512 0.3683 0.081 Uiso 1 1 calc R . . N4 N 0.1241(10) -0.0115(5) 0.3663(3) 0.0593(18) Uani 1 1 d . . . C14 C 0.4657(16) -0.0428(8) 0.4096(4) 0.070(3) Uani 1 1 d . . . H14 H 0.5550 -0.0806 0.4380 0.084 Uiso 1 1 calc R . . C2 C 0.4180(15) 0.4134(7) -0.1486(4) 0.065(2) Uani 1 1 d . . . H2 H 0.4947 0.4557 -0.1781 0.078 Uiso 1 1 calc R . . C1 C 0.2058(14) 0.4277(7) -0.1391(4) 0.063(2) Uani 1 1 d . . . H1 H 0.1392 0.4836 -0.1621 0.076 Uiso 1 1 calc R . . C15 C 0.2521(16) -0.0624(7) 0.4075(4) 0.064(2) Uani 1 1 d . . . H15 H 0.1958 -0.1135 0.4364 0.077 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 S4 0.0360(8) 0.0717(13) 0.0288(8) 0.0000(8) -0.0038(6) -0.0013(8) S3 0.0433(9) 0.0781(15) 0.0333(8) 0.0046(9) -0.0014(7) 0.0000(10) N8 0.037(3) 0.043(3) 0.022(2) 0.006(2) 0.001(2) 0.003(3) C27 0.039(4) 0.041(4) 0.021(3) -0.011(3) -0.004(2) 0.000(3) N6 0.036(3) 0.076(5) 0.039(3) 0.007(3) 0.000(3) 0.002(3) C25 0.042(3) 0.035(4) 0.025(3) 0.006(3) -0.003(2) 0.002(3) C26 0.051(4) 0.051(4) 0.030(3) -0.002(3) -0.006(3) 0.002(3) C21 0.051(4) 0.040(4) 0.024(3) 0.007(3) -0.008(3) 0.004(3) C24 0.041(3) 0.050(4) 0.028(3) 0.010(3) 0.010(3) -0.007(3) C19 0.055(4) 0.059(5) 0.019(3) -0.009(3) 0.008(3) -0.008(4) N10 0.038(3) 0.057(4) 0.037(3) 0.008(3) -0.003(2) -0.006(3) C22 0.043(3) 0.054(5) 0.034(3) 0.005(3) -0.009(3) -0.012(4) N9 0.053(4) 0.062(4) 0.052(4) -0.010(3) -0.004(3) 0.016(3) N7 0.058(4) 0.059(4) 0.038(3) 0.002(3) -0.003(3) -0.011(3) C30 0.046(4) 0.068(6) 0.057(5) 0.001(4) 0.002(4) -0.008(4) C23 0.039(3) 0.071(5) 0.044(4) 0.015(4) -0.001(3) -0.009(4) C16 0.061(5) 0.106(8) 0.058(5) 0.002(5) -0.017(4) 0.023(5) C20 0.065(4) 0.049(4) 0.028(3) 0.004(3) -0.005(3) -0.001(4) C28 0.087(6) 0.045(5) 0.055(5) 0.006(4) -0.015(5) -0.001(5) C18 0.111(8) 0.035(5) 0.042(4) 0.000(3) -0.006(5) -0.016(5) C29 0.065(5) 0.052(5) 0.062(5) 0.002(4) 0.004(4) -0.015(4) C17 0.117(8) 0.046(5) 0.040(4) 0.005(4) -0.010(5) 0.019(6) S1 0.0335(8) 0.0768(14) 0.0308(8) -0.0074(8) -0.0005(6) -0.0034(9) S2 0.0421(9) 0.0827(16) 0.0343(9) -0.0013(9) 0.0002(7) -0.0067(10) N3 0.036(3) 0.037(3) 0.033(3) -0.005(2) 0.003(2) 0.001(2) N5 0.062(4) 0.075(5) 0.030(3) 0.009(3) -0.005(3) -0.016(4) C10 0.051(4) 0.031(3) 0.019(3) 0.004(3) 0.001(2) -0.001(3) N2 0.026(3) 0.056(4) 0.035(3) -0.002(3) 0.004(2) 0.002(3) C4 0.039(4) 0.048(4) 0.031(3) -0.012(3) -0.009(3) 0.004(3) C5 0.043(3) 0.049(4) 0.032(3) -0.001(3) 0.012(3) -0.010(3) C9 0.048(4) 0.054(5) 0.037(3) 0.003(4) -0.012(3) -0.001(4) C6 0.039(3) 0.033(4) 0.032(3) 0.005(3) 0.003(3) -0.003(3) C7 0.032(3) 0.067(5) 0.044(4) 0.004(4) 0.008(3) 0.004(3) C12 0.046(4) 0.059(5) 0.026(3) -0.006(3) 0.001(3) -0.010(4) N1 0.049(3) 0.046(4) 0.057(4) 0.002(3) -0.016(3) 0.005(3) C8 0.031(3) 0.074(6) 0.054(4) 0.020(4) 0.001(3) -0.006(4) C11 0.050(4) 0.047(4) 0.040(4) 0.000(3) -0.003(3) 0.014(4) C3 0.045(4) 0.065(5) 0.051(4) 0.004(4) 0.010(3) -0.010(4) C13 0.070(5) 0.086(7) 0.048(5) 0.005(5) -0.006(4) -0.009(5) N4 0.077(5) 0.054(4) 0.046(4) -0.008(3) 0.011(3) -0.010(4) C14 0.094(7) 0.063(6) 0.053(5) 0.002(4) -0.023(5) 0.010(6) C2 0.092(7) 0.047(5) 0.056(5) 0.014(4) -0.005(5) -0.014(5) C1 0.075(6) 0.048(5) 0.066(5) 0.011(4) -0.027(4) 0.001(5) C15 0.099(7) 0.049(5) 0.045(4) 0.000(4) 0.004(5) -0.005(5) _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 S4 C27 1.738(6) . ? S4 C26 1.805(7) . ? S3 C19 1.757(7) . ? S3 C20 1.823(7) . ? N8 C21 1.326(7) . ? N8 C25 1.336(7) . ? C27 N10 1.309(7) . ? C27 N9 1.340(9) . ? N6 C19 1.328(8) . ? N6 C16 1.360(10) . ? C25 C24 1.386(8) . ? C25 C26 1.497(8) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C21 C22 1.388(8) . ? C21 C20 1.501(9) . ? C24 C23 1.384(9) . ? C24 H24 0.9300 . ? C19 N7 1.329(8) . ? N10 C30 1.327(9) . ? C22 C23 1.370(9) . ? C22 H22 0.9300 . ? N9 C28 1.347(10) . ? N7 C18 1.319(10) . ? C30 C29 1.370(11) . ? C30 H30 0.9300 . ? C23 H23 0.9300 . ? C16 C17 1.347(12) . ? C16 H16 0.9300 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C28 C29 1.359(10) . ? C28 H28 0.9300 . ? C18 C17 1.351(11) . ? C18 H18 0.9300 . ? C29 H29 0.9300 . ? C17 H17 0.9300 . ? S1 C4 1.749(7) . ? S1 C5 1.815(7) . ? S2 C12 1.744(7) . ? S2 C11 1.790(7) . ? N3 C6 1.328(7) . ? N3 C10 1.337(7) . ? N5 C12 1.303(8) . ? N5 C13 1.341(10) . ? C10 C9 1.390(8) . ? C10 C11 1.505(8) . ? N2 C4 1.305(7) . ? N2 C3 1.340(8) . ? C4 N1 1.354(8) . ? C5 C6 1.494(8) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C9 C8 1.378(9) . ? C9 H9 0.9300 . ? C6 C7 1.382(8) . ? C7 C8 1.351(9) . ? C7 H7 0.9300 . ? C12 N4 1.335(9) . ? N1 C1 1.301(9) . ? C8 H8 0.9300 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C3 C2 1.390(11) . ? C3 H3 0.9300 . ? C13 C14 1.358(12) . ? C13 H13 0.9300 . ? N4 C15 1.318(10) . ? C14 C15 1.376(11) . ? C14 H14 0.9300 . ? C2 C1 1.372(10) . ? C2 H2 0.9300 . ? C1 H1 0.9300 . ? C15 H15 0.9300 . ? 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 C27 S4 C26 102.4(3) . . ? C19 S3 C20 103.0(3) . . ? C21 N8 C25 118.9(5) . . ? N10 C27 N9 125.9(6) . . ? N10 C27 S4 122.0(5) . . ? N9 C27 S4 112.1(5) . . ? C19 N6 C16 113.6(7) . . ? N8 C25 C24 122.2(5) . . ? N8 C25 C26 116.7(5) . . ? C24 C25 C26 121.1(5) . . ? C25 C26 S4 114.1(5) . . ? C25 C26 H26A 108.7 . . ? S4 C26 H26A 108.7 . . ? C25 C26 H26B 108.7 . . ? S4 C26 H26B 108.7 . . ? H26A C26 H26B 107.6 . . ? N8 C21 C22 122.0(5) . . ? N8 C21 C20 117.0(5) . . ? C22 C21 C20 121.0(6) . . ? C23 C24 C25 118.8(5) . . ? C23 C24 H24 120.6 . . ? C25 C24 H24 120.6 . . ? N6 C19 N7 127.3(7) . . ? N6 C19 S3 119.9(5) . . ? N7 C19 S3 112.8(5) . . ? C27 N10 C30 117.6(7) . . ? C23 C22 C21 119.5(6) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C27 N9 C28 115.2(6) . . ? C18 N7 C19 115.4(6) . . ? N10 C30 C29 121.6(7) . . ? N10 C30 H30 119.2 . . ? C29 C30 H30 119.2 . . ? C22 C23 C24 118.6(6) . . ? C22 C23 H23 120.7 . . ? C24 C23 H23 120.7 . . ? C17 C16 N6 123.6(8) . . ? C17 C16 H16 118.2 . . ? N6 C16 H16 118.2 . . ? C21 C20 S3 113.9(5) . . ? C21 C20 H20A 108.8 . . ? S3 C20 H20A 108.8 . . ? C21 C20 H20B 108.8 . . ? S3 C20 H20B 108.8 . . ? H20A C20 H20B 107.7 . . ? N9 C28 C29 122.6(8) . . ? N9 C28 H28 118.7 . . ? C29 C28 H28 118.7 . . ? N7 C18 C17 123.7(8) . . ? N7 C18 H18 118.1 . . ? C17 C18 H18 118.1 . . ? C28 C29 C30 117.1(8) . . ? C28 C29 H29 121.4 . . ? C30 C29 H29 121.4 . . ? C16 C17 C18 116.4(8) . . ? C16 C17 H17 121.8 . . ? C18 C17 H17 121.8 . . ? C4 S1 C5 103.1(3) . . ? C12 S2 C11 102.5(3) . . ? C6 N3 C10 118.0(5) . . ? C12 N5 C13 116.5(7) . . ? N3 C10 C9 122.1(5) . . ? N3 C10 C11 117.0(5) . . ? C9 C10 C11 120.9(6) . . ? C4 N2 C3 116.3(7) . . ? N2 C4 N1 126.5(6) . . ? N2 C4 S1 121.2(5) . . ? N1 C4 S1 112.3(5) . . ? C6 C5 S1 113.5(5) . . ? C6 C5 H5A 108.9 . . ? S1 C5 H5A 108.9 . . ? C6 C5 H5B 108.9 . . ? S1 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? C8 C9 C10 118.9(6) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? N3 C6 C7 122.5(6) . . ? N3 C6 C5 116.2(5) . . ? C7 C6 C5 121.3(5) . . ? C8 C7 C6 119.7(6) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? N5 C12 N4 126.1(7) . . ? N5 C12 S2 120.2(6) . . ? N4 C12 S2 113.7(5) . . ? C1 N1 C4 115.4(6) . . ? C7 C8 C9 118.7(6) . . ? C7 C8 H8 120.6 . . ? C9 C8 H8 120.6 . . ? C10 C11 S2 116.2(5) . . ? C10 C11 H11A 108.2 . . ? S2 C11 H11A 108.2 . . ? C10 C11 H11B 108.2 . . ? S2 C11 H11B 108.2 . . ? H11A C11 H11B 107.4 . . ? N2 C3 C2 122.1(7) . . ? N2 C3 H3 119.0 . . ? C2 C3 H3 119.0 . . ? N5 C13 C14 122.3(8) . . ? N5 C13 H13 118.8 . . ? C14 C13 H13 118.8 . . ? C15 N4 C12 116.2(7) . . ? C13 C14 C15 116.3(8) . . ? C13 C14 H14 121.8 . . ? C15 C14 H14 121.8 . . ? C1 C2 C3 115.4(7) . . ? C1 C2 H2 122.3 . . ? C3 C2 H2 122.3 . . ? N1 C1 C2 124.3(7) . . ? N1 C1 H1 117.9 . . ? C2 C1 H1 117.9 . . ? N4 C15 C14 122.6(8) . . ? N4 C15 H15 118.7 . . ? C14 C15 H15 118.7 . . ? 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 C26 S4 C27 N10 0.3(6) . . . . ? C26 S4 C27 N9 -178.3(5) . . . . ? C21 N8 C25 C24 0.9(10) . . . . ? C21 N8 C25 C26 -179.1(6) . . . . ? N8 C25 C26 S4 -66.2(7) . . . . ? C24 C25 C26 S4 113.8(6) . . . . ? C27 S4 C26 C25 -79.5(5) . . . . ? C25 N8 C21 C22 0.3(10) . . . . ? C25 N8 C21 C20 -177.2(5) . . . . ? N8 C25 C24 C23 -2.3(10) . . . . ? C26 C25 C24 C23 177.7(6) . . . . ? C16 N6 C19 N7 1.1(11) . . . . ? C16 N6 C19 S3 178.8(6) . . . . ? C20 S3 C19 N6 12.0(6) . . . . ? C20 S3 C19 N7 -170.0(5) . . . . ? N9 C27 N10 C30 -1.6(10) . . . . ? S4 C27 N10 C30 180.0(5) . . . . ? N8 C21 C22 C23 -0.1(10) . . . . ? C20 C21 C22 C23 177.3(6) . . . . ? N10 C27 N9 C28 0.0(10) . . . . ? S4 C27 N9 C28 178.5(6) . . . . ? N6 C19 N7 C18 -1.6(11) . . . . ? S3 C19 N7 C18 -179.5(6) . . . . ? C27 N10 C30 C29 2.2(11) . . . . ? C21 C22 C23 C24 -1.3(10) . . . . ? C25 C24 C23 C22 2.4(10) . . . . ? C19 N6 C16 C17 0.3(12) . . . . ? N8 C21 C20 S3 -61.1(7) . . . . ? C22 C21 C20 S3 121.5(6) . . . . ? C19 S3 C20 C21 -84.0(5) . . . . ? C27 N9 C28 C29 1.1(11) . . . . ? C19 N7 C18 C17 0.9(12) . . . . ? N9 C28 C29 C30 -0.6(13) . . . . ? N10 C30 C29 C28 -1.2(12) . . . . ? N6 C16 C17 C18 -0.9(13) . . . . ? N7 C18 C17 C16 0.3(13) . . . . ? C6 N3 C10 C9 -1.8(10) . . . . ? C6 N3 C10 C11 176.0(6) . . . . ? C3 N2 C4 N1 -0.6(10) . . . . ? C3 N2 C4 S1 177.8(5) . . . . ? C5 S1 C4 N2 1.2(6) . . . . ? C5 S1 C4 N1 179.9(5) . . . . ? C4 S1 C5 C6 79.4(5) . . . . ? N3 C10 C9 C8 2.2(11) . . . . ? C11 C10 C9 C8 -175.6(7) . . . . ? C10 N3 C6 C7 0.5(10) . . . . ? C10 N3 C6 C5 179.0(6) . . . . ? S1 C5 C6 N3 69.3(7) . . . . ? S1 C5 C6 C7 -112.3(7) . . . . ? N3 C6 C7 C8 0.4(12) . . . . ? C5 C6 C7 C8 -178.0(7) . . . . ? C13 N5 C12 N4 0.4(11) . . . . ? C13 N5 C12 S2 179.3(6) . . . . ? C11 S2 C12 N5 -8.7(7) . . . . ? C11 S2 C12 N4 170.3(5) . . . . ? N2 C4 N1 C1 1.8(10) . . . . ? S1 C4 N1 C1 -176.8(5) . . . . ? C6 C7 C8 C9 -0.1(12) . . . . ? C10 C9 C8 C7 -1.2(12) . . . . ? N3 C10 C11 S2 59.3(7) . . . . ? C9 C10 C11 S2 -122.9(7) . . . . ? C12 S2 C11 C10 84.5(5) . . . . ? C4 N2 C3 C2 -2.1(10) . . . . ? C12 N5 C13 C14 -0.1(12) . . . . ? N5 C12 N4 C15 0.4(11) . . . . ? S2 C12 N4 C15 -178.6(5) . . . . ? N5 C13 C14 C15 -1.0(13) . . . . ? N2 C3 C2 C1 3.4(12) . . . . ? C4 N1 C1 C2 -0.3(11) . . . . ? C3 C2 C1 N1 -2.1(13) . . . . ? C12 N4 C15 C14 -1.5(12) . . . . ? C13 C14 C15 N4 1.8(13) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.84 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.848 _refine_diff_density_min -0.294 _refine_diff_density_rms 0.109 #===END data_Ligand_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16H14N4S2' _chemical_formula_sum 'C16 H14 N4 S2' _chemical_formula_weight 326.43 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M PC loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 13.953(3) _cell_length_b 4.6420(10) _cell_length_c 12.389(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.550(4) _cell_angle_gamma 90.00 _cell_volume 780.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3790 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 25.00 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.390 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 340 _exptl_absorpt_coefficient_mu 0.342 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9601 _exptl_absorpt_correction_T_max 0.9798 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3790 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1925 _reflns_number_gt 1787 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0855P)^2^+0.2329P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.11(17) _refine_ls_number_reflns 1925 _refine_ls_number_parameters 199 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0601 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.1497 _refine_ls_wR_factor_gt 0.1417 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.128 _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 S2 S 0.42920(10) -0.0447(3) 0.02831(10) 0.0588(4) Uani 1 1 d . . . S1 S -0.11132(11) 0.4994(3) -0.10546(11) 0.0544(4) Uani 1 1 d . . . C3 C -0.1176(9) 0.0082(14) 0.1475(8) 0.0707(18) Uani 1 1 d . . . H3 H -0.0758 -0.0546 0.2131 0.085 Uiso 1 1 calc R . . C11 C 0.1590(4) 0.2340(11) -0.0141(4) 0.0444(12) Uani 1 1 d . . . H11 H 0.1573 0.2175 0.0602 0.053 Uiso 1 1 calc R . . C4 C -0.1468(4) 0.2578(11) -0.0107(4) 0.0472(12) Uani 1 1 d . . . C10 C 0.2291(4) 0.0816(10) -0.0514(4) 0.0429(11) Uani 1 1 d . . . C13 C 0.4652(4) 0.1884(12) 0.1428(4) 0.0506(13) Uani 1 1 d . . . C7 C 0.0949(5) 0.4365(13) -0.1930(5) 0.0560(14) Uani 1 1 d . . . H7 H 0.0512 0.5574 -0.2405 0.067 Uiso 1 1 calc R . . C6 C 0.0906(4) 0.4117(11) -0.0823(4) 0.0444(12) Uani 1 1 d . . . C9 C 0.2301(4) 0.1057(14) -0.1629(5) 0.0571(14) Uani 1 1 d . . . H9 H 0.2759 0.0021 -0.1911 0.069 Uiso 1 1 calc R . . C14 C 0.4384(8) 0.4517(15) 0.2841(7) 0.0676(19) Uani 1 1 d . . . H14 H 0.3958 0.5243 0.3250 0.081 Uiso 1 1 calc R . . N1 N -0.2387(4) 0.1805(12) -0.0442(4) 0.0623(13) Uani 1 1 d . . . N2 N -0.0821(4) 0.1831(10) 0.0803(4) 0.0577(12) Uani 1 1 d . . . N4 N 0.5609(4) 0.2482(13) 0.1644(5) 0.0730(16) Uani 1 1 d . . . N3 N 0.4008(4) 0.2802(10) 0.1971(4) 0.0547(11) Uani 1 1 d . . . C8 C 0.1636(5) 0.2825(14) -0.2318(5) 0.0639(16) Uani 1 1 d . . . H8 H 0.1653 0.2979 -0.3062 0.077 Uiso 1 1 calc R . . C16 C 0.5928(6) 0.421(2) 0.2521(7) 0.089(2) Uani 1 1 d . . . H16 H 0.6590 0.4731 0.2702 0.107 Uiso 1 1 calc R . . C2 C -0.2143(7) -0.0813(19) 0.1221(7) 0.087(2) Uani 1 1 d . . . H2 H -0.2386 -0.1977 0.1707 0.104 Uiso 1 1 calc R . . C1 C -0.2727(6) 0.0051(17) 0.0245(7) 0.080(2) Uani 1 1 d . . . H1 H -0.3377 -0.0582 0.0046 0.096 Uiso 1 1 calc R . . C15 C 0.5340(7) 0.5239(17) 0.3153(8) 0.081(2) Uani 1 1 d . . . H15 H 0.5583 0.6386 0.3772 0.097 Uiso 1 1 calc R . . C12 C 0.3009(5) -0.1150(12) 0.0223(5) 0.0583(15) Uani 1 1 d . . . H12A H 0.2862 -0.3114 -0.0030 0.070 Uiso 1 1 calc R . . H12B H 0.2906 -0.1018 0.0969 0.070 Uiso 1 1 calc R . . C5 C 0.0151(5) 0.5818(13) -0.0403(5) 0.0579(14) Uani 1 1 d . . . H5A H 0.0262 0.7851 -0.0509 0.069 Uiso 1 1 calc R . . H5B H 0.0254 0.5487 0.0389 0.069 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 S2 0.0428(9) 0.0748(9) 0.0569(9) -0.0047(8) 0.0079(7) 0.0029(8) S1 0.0392(8) 0.0677(8) 0.0556(8) 0.0024(6) 0.0098(6) 0.0015(6) C3 0.068(5) 0.080(4) 0.061(4) 0.021(3) 0.009(3) 0.013(3) C11 0.046(3) 0.045(3) 0.042(3) -0.001(2) 0.009(2) -0.014(2) C4 0.036(3) 0.052(3) 0.053(3) -0.009(2) 0.010(2) 0.007(2) C10 0.038(3) 0.042(2) 0.047(3) 0.000(2) 0.008(2) -0.010(2) C13 0.043(3) 0.057(3) 0.052(3) 0.013(2) 0.011(3) -0.005(3) C7 0.046(3) 0.069(4) 0.052(3) 0.004(3) 0.009(3) 0.001(3) C6 0.039(3) 0.045(3) 0.051(3) -0.010(2) 0.013(2) -0.016(2) C9 0.044(3) 0.076(4) 0.051(3) -0.001(3) 0.011(3) 0.009(3) C14 0.078(6) 0.066(4) 0.061(4) 0.001(3) 0.024(4) 0.007(4) N1 0.040(3) 0.073(3) 0.072(3) 0.001(3) 0.009(2) -0.001(3) N2 0.051(3) 0.065(3) 0.054(3) -0.006(2) 0.006(2) 0.006(2) N4 0.038(3) 0.106(5) 0.074(4) 0.003(3) 0.010(3) -0.004(3) N3 0.042(2) 0.063(3) 0.059(3) 0.002(2) 0.011(2) -0.002(2) C8 0.064(4) 0.089(4) 0.041(3) 0.009(3) 0.017(3) 0.018(3) C16 0.049(4) 0.135(7) 0.076(5) -0.004(5) -0.002(4) -0.039(5) C2 0.085(6) 0.098(5) 0.082(6) 0.025(4) 0.028(5) -0.006(5) C1 0.050(4) 0.094(5) 0.100(6) 0.007(4) 0.027(4) -0.008(3) C15 0.070(6) 0.095(5) 0.074(5) -0.012(4) 0.009(4) -0.021(4) C12 0.060(4) 0.047(3) 0.063(4) 0.012(3) 0.004(3) -0.014(3) C5 0.051(4) 0.057(3) 0.066(4) -0.014(3) 0.017(3) -0.002(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 S2 C13 1.761(6) . ? S2 C12 1.804(7) . ? S1 C4 1.775(6) . ? S1 C5 1.801(7) . ? C3 N2 1.339(10) . ? C3 C2 1.375(14) . ? C3 H3 0.9300 . ? C11 C10 1.372(8) . ? C11 C6 1.388(8) . ? C11 H11 0.9300 . ? C4 N1 1.303(7) . ? C4 N2 1.315(7) . ? C10 C9 1.389(7) . ? C10 C12 1.498(8) . ? C13 N3 1.313(7) . ? C13 N4 1.328(8) . ? C7 C8 1.370(9) . ? C7 C6 1.391(8) . ? C7 H7 0.9300 . ? C6 C5 1.504(8) . ? C9 C8 1.375(9) . ? C9 H9 0.9300 . ? C14 C15 1.341(14) . ? C14 N3 1.344(10) . ? C14 H14 0.9300 . ? N1 C1 1.343(9) . ? N4 C16 1.340(10) . ? C8 H8 0.9300 . ? C16 C15 1.348(12) . ? C16 H16 0.9300 . ? C2 C1 1.352(12) . ? C2 H2 0.9300 . ? C1 H1 0.9300 . ? C15 H15 0.9300 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? 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 C13 S2 C12 103.7(3) . . ? C4 S1 C5 103.5(3) . . ? N2 C3 C2 121.8(9) . . ? N2 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? C10 C11 C6 122.9(4) . . ? C10 C11 H11 118.5 . . ? C6 C11 H11 118.5 . . ? N1 C4 N2 128.8(5) . . ? N1 C4 S1 111.7(4) . . ? N2 C4 S1 119.5(4) . . ? C11 C10 C9 117.9(5) . . ? C11 C10 C12 122.4(5) . . ? C9 C10 C12 119.6(5) . . ? N3 C13 N4 127.2(6) . . ? N3 C13 S2 120.8(4) . . ? N4 C13 S2 112.0(4) . . ? C8 C7 C6 119.8(6) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C11 C6 C7 117.8(5) . . ? C11 C6 C5 122.6(5) . . ? C7 C6 C5 119.5(5) . . ? C8 C9 C10 120.1(5) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C15 C14 N3 123.7(8) . . ? C15 C14 H14 118.1 . . ? N3 C14 H14 118.1 . . ? C4 N1 C1 115.7(6) . . ? C4 N2 C3 114.4(7) . . ? C13 N4 C16 114.6(6) . . ? C13 N3 C14 114.6(6) . . ? C7 C8 C9 121.3(5) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? N4 C16 C15 123.4(7) . . ? N4 C16 H16 118.3 . . ? C15 C16 H16 118.3 . . ? C1 C2 C3 118.0(7) . . ? C1 C2 H2 121.0 . . ? C3 C2 H2 121.0 . . ? N1 C1 C2 121.2(7) . . ? N1 C1 H1 119.4 . . ? C2 C1 H1 119.4 . . ? C14 C15 C16 116.3(8) . . ? C14 C15 H15 121.8 . . ? C16 C15 H15 121.8 . . ? C10 C12 S2 115.5(4) . . ? C10 C12 H12A 108.4 . . ? S2 C12 H12A 108.4 . . ? C10 C12 H12B 108.4 . . ? S2 C12 H12B 108.4 . . ? H12A C12 H12B 107.5 . . ? C6 C5 S1 115.2(4) . . ? C6 C5 H5A 108.5 . . ? S1 C5 H5A 108.5 . . ? C6 C5 H5B 108.5 . . ? S1 C5 H5B 108.5 . . ? H5A C5 H5B 107.5 . . ? 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 C5 S1 C4 N1 178.4(4) . . . . ? C5 S1 C4 N2 -1.0(5) . . . . ? C6 C11 C10 C9 -0.7(8) . . . . ? C6 C11 C10 C12 -178.5(5) . . . . ? C12 S2 C13 N3 -3.5(5) . . . . ? C12 S2 C13 N4 175.7(4) . . . . ? C10 C11 C6 C7 -0.7(8) . . . . ? C10 C11 C6 C5 -179.0(5) . . . . ? C8 C7 C6 C11 1.6(8) . . . . ? C8 C7 C6 C5 179.9(6) . . . . ? C11 C10 C9 C8 1.3(9) . . . . ? C12 C10 C9 C8 179.1(6) . . . . ? N2 C4 N1 C1 1.4(9) . . . . ? S1 C4 N1 C1 -177.8(5) . . . . ? N1 C4 N2 C3 -1.4(8) . . . . ? S1 C4 N2 C3 177.8(5) . . . . ? C2 C3 N2 C4 -0.5(10) . . . . ? N3 C13 N4 C16 0.2(10) . . . . ? S2 C13 N4 C16 -178.9(6) . . . . ? N4 C13 N3 C14 -0.4(9) . . . . ? S2 C13 N3 C14 178.6(5) . . . . ? C15 C14 N3 C13 -0.6(10) . . . . ? C6 C7 C8 C9 -1.0(10) . . . . ? C10 C9 C8 C7 -0.4(10) . . . . ? C13 N4 C16 C15 1.2(12) . . . . ? N2 C3 C2 C1 2.2(13) . . . . ? C4 N1 C1 C2 0.5(11) . . . . ? C3 C2 C1 N1 -2.1(13) . . . . ? N3 C14 C15 C16 1.9(12) . . . . ? N4 C16 C15 C14 -2.2(14) . . . . ? C11 C10 C12 S2 -125.3(5) . . . . ? C9 C10 C12 S2 57.0(7) . . . . ? C13 S2 C12 C10 92.5(5) . . . . ? C11 C6 C5 S1 -119.8(5) . . . . ? C7 C6 C5 S1 62.0(6) . . . . ? C4 S1 C5 C6 98.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.485 _refine_diff_density_min -0.182 _refine_diff_density_rms 0.068 #===END data_Ligand_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16H14N4S2' _chemical_formula_sum 'C16 H14 N4 S2' _chemical_formula_weight 326.43 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p2(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 12.0861(8) _cell_length_b 4.6576(3) _cell_length_c 27.9405(18) _cell_angle_alpha 90.00 _cell_angle_beta 102.5130(10) _cell_angle_gamma 90.00 _cell_volume 1535.47(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12987 _cell_measurement_theta_min 1.49 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.412 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 0.348 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9089 _exptl_absorpt_correction_T_max 0.9794 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12987 _diffrn_reflns_av_R_equivalents 0.0255 _diffrn_reflns_av_sigmaI/netI 0.0251 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3466 _reflns_number_gt 3122 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0836P)^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 3466 _refine_ls_number_parameters 256 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0541 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1270 _refine_ls_wR_factor_gt 0.1168 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.108 _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 S1 S 0.51658(7) 0.7094(2) 0.63713(2) 0.0439(2) Uani 1 1 d . . . S2 S 0.87709(7) 0.18189(16) 0.86397(2) 0.0462(2) Uani 1 1 d . . . N1 N 0.32630(19) 1.0259(5) 0.62053(8) 0.0436(6) Uani 1 1 d . . . N2 N 0.4524(2) 1.0417(6) 0.69941(8) 0.0500(6) Uani 1 1 d . . . N3 N 0.7070(2) 0.5127(5) 0.88030(8) 0.0407(5) Uani 1 1 d . . . N4 N 0.7427(3) 0.4898(6) 0.79997(9) 0.0572(7) Uani 1 1 d . . . C1 C 0.6104(2) 1.0421(6) 0.49554(10) 0.0364(6) Uani 1 1 d D . . C2 C 0.5877(2) 0.8610(6) 0.53136(10) 0.0373(6) Uani 1 1 d D . . C3 C 0.4768(2) 0.8148(5) 0.53636(9) 0.0320(5) Uani 1 1 d . . . C4 C 0.4517(3) 0.6122(6) 0.57446(10) 0.0407(6) Uani 1 1 d D . . C5 C 0.4197(2) 0.9525(6) 0.65317(9) 0.0375(6) Uani 1 1 d . . . C6 C 0.2577(3) 1.2104(7) 0.63754(13) 0.0505(8) Uani 1 1 d D . . C7 C 0.2827(4) 1.3101(8) 0.68419(14) 0.0623(10) Uani 1 1 d D . . C8 C 0.3814(4) 1.2226(9) 0.71423(11) 0.0594(9) Uani 1 1 d D . . C9 C 1.1130(2) 0.5550(6) 1.00303(10) 0.0373(6) Uani 1 1 d D . . C10 C 1.0557(2) 0.3660(5) 0.96807(10) 0.0364(6) Uani 1 1 d D . . C11 C 0.9407(2) 0.3092(5) 0.96461(9) 0.0330(6) Uani 1 1 d . . . C12 C 0.8789(3) 0.0994(6) 0.92731(10) 0.0396(6) Uani 1 1 d . . . C13 C 0.7632(2) 0.4214(6) 0.84747(9) 0.0386(6) Uani 1 1 d . . . C14 C 0.6216(3) 0.6926(7) 0.86291(14) 0.0535(8) Uani 1 1 d . . . C15 C 0.5916(4) 0.7754(9) 0.81535(15) 0.0627(10) Uani 1 1 d . . . C16 C 0.6550(4) 0.6665(9) 0.78464(14) 0.0693(12) Uani 1 1 d . . . H1 H 0.6857(13) 1.086(7) 0.4938(12) 0.054(9) Uiso 1 1 d D . . H2 H 0.646(2) 0.767(7) 0.5545(9) 0.044(9) Uiso 1 1 d D . . H41 H 0.482(3) 0.427(4) 0.5697(12) 0.055(9) Uiso 1 1 d D . . H42 H 0.3739(12) 0.600(8) 0.5766(13) 0.067(11) Uiso 1 1 d D . . H6 H 0.1865(16) 1.250(9) 0.6160(9) 0.061(11) Uiso 1 1 d D . . H7 H 0.242(3) 1.447(6) 0.6991(11) 0.059(10) Uiso 1 1 d D . . H8 H 0.392(3) 1.277(7) 0.7476(5) 0.052(9) Uiso 1 1 d D . . H9 H 1.1916(10) 0.586(7) 1.0069(12) 0.055(10) Uiso 1 1 d D . . H10 H 1.094(2) 0.279(6) 0.9454(8) 0.036(8) Uiso 1 1 d D . . H121 H 0.804(3) 0.085(6) 0.9292(10) 0.035(7) Uiso 1 1 d . . . H122 H 0.925(3) -0.080(7) 0.9304(11) 0.050(8) Uiso 1 1 d . . . H14 H 0.587(3) 0.775(9) 0.8807(11) 0.053(11) Uiso 1 1 d . . . H15 H 0.535(5) 0.887(10) 0.8046(15) 0.086(14) Uiso 1 1 d . . . H16 H 0.658(5) 0.727(12) 0.7532(14) 0.089(13) 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 S1 0.0394(4) 0.0570(6) 0.0350(4) 0.0078(3) 0.0076(3) 0.0086(3) S2 0.0464(5) 0.0569(6) 0.0349(4) -0.0041(3) 0.0077(4) 0.0082(3) N1 0.0365(13) 0.0501(13) 0.0423(13) 0.0076(10) 0.0043(10) 0.0008(10) N2 0.0563(15) 0.0619(16) 0.0315(12) 0.0035(10) 0.0088(11) 0.0057(13) N3 0.0396(13) 0.0450(12) 0.0370(12) -0.0022(9) 0.0073(9) -0.0032(10) N4 0.0632(18) 0.0744(18) 0.0340(13) 0.0066(12) 0.0105(12) 0.0059(15) C1 0.0264(13) 0.0423(14) 0.0415(14) -0.0009(11) 0.0095(10) -0.0040(10) C2 0.0329(13) 0.0401(13) 0.0370(14) 0.0023(11) 0.0034(10) 0.0018(10) C3 0.0360(14) 0.0323(13) 0.0288(13) -0.0056(9) 0.0094(11) -0.0041(10) C4 0.0492(17) 0.0374(13) 0.0380(15) 0.0019(10) 0.0152(12) -0.0058(12) C5 0.0377(14) 0.0417(14) 0.0341(14) 0.0100(10) 0.0096(10) -0.0047(11) C6 0.0343(17) 0.0616(18) 0.0553(19) 0.0115(15) 0.0091(17) 0.0049(14) C7 0.059(2) 0.069(2) 0.064(2) 0.0017(17) 0.026(2) 0.0146(18) C8 0.071(2) 0.071(2) 0.0374(17) -0.0015(15) 0.0141(17) 0.0058(18) C9 0.0305(13) 0.0387(13) 0.0423(15) 0.0050(10) 0.0073(11) -0.0006(10) C10 0.0343(14) 0.0384(12) 0.0371(13) 0.0013(10) 0.0093(11) 0.0031(10) C11 0.0376(14) 0.0265(12) 0.0334(13) 0.0064(9) 0.0047(12) 0.0009(10) C12 0.0422(16) 0.0338(12) 0.0400(15) 0.0022(10) 0.0028(12) -0.0030(11) C13 0.0384(14) 0.0421(14) 0.0325(13) 0.0004(10) 0.0018(10) -0.0045(11) C14 0.045(2) 0.0522(19) 0.062(2) -0.0042(15) 0.0083(19) 0.0011(13) C15 0.050(2) 0.067(2) 0.065(2) 0.0138(17) 0.000(2) 0.0083(17) C16 0.070(3) 0.087(3) 0.044(2) 0.0234(18) -0.0033(18) 0.006(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 S1 C5 1.755(3) . ? S1 C4 1.814(3) . ? S2 C13 1.754(3) . ? S2 C12 1.806(3) . ? N1 C5 1.333(4) . ? N1 C6 1.350(4) . ? N2 C8 1.331(5) . ? N2 C5 1.333(4) . ? N3 C13 1.325(4) . ? N3 C14 1.336(4) . ? N4 C13 1.335(3) . ? N4 C16 1.337(5) . ? C1 C2 1.381(4) . ? C1 C3 1.394(4) 3_676 ? C1 H1 0.945(10) . ? C2 C3 1.393(4) . ? C2 H2 0.957(10) . ? C3 C1 1.394(4) 3_676 ? C3 C4 1.502(4) . ? C4 H41 0.954(10) . ? C4 H42 0.957(10) . ? C6 C7 1.355(5) . ? C6 H6 0.955(10) . ? C7 C8 1.364(6) . ? C7 H7 0.953(10) . ? C8 H8 0.948(10) . ? C9 C11 1.376(4) 3_767 ? C9 C10 1.384(4) . ? C9 H9 0.943(10) . ? C10 C11 1.397(4) . ? C10 H10 0.953(10) . ? C11 C9 1.376(4) 3_767 ? C11 C12 1.504(4) . ? C12 H121 0.92(3) . ? C12 H122 0.99(3) . ? C14 C15 1.356(5) . ? C14 H14 0.81(4) . ? C15 C16 1.366(6) . ? C15 H15 0.86(5) . ? C16 H16 0.93(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 C5 S1 C4 103.58(14) . . ? C13 S2 C12 103.59(13) . . ? C5 N1 C6 114.6(3) . . ? C8 N2 C5 115.0(3) . . ? C13 N3 C14 114.9(3) . . ? C13 N4 C16 115.4(3) . . ? C2 C1 C3 120.9(2) . 3_676 ? C2 C1 H1 121(2) . . ? C3 C1 H1 118(2) 3_676 . ? C1 C2 C3 120.9(3) . . ? C1 C2 H2 122(2) . . ? C3 C2 H2 117(2) . . ? C2 C3 C1 118.2(2) . 3_676 ? C2 C3 C4 121.0(3) . . ? C1 C3 C4 120.8(3) 3_676 . ? C3 C4 S1 114.56(19) . . ? C3 C4 H41 109(2) . . ? S1 C4 H41 105(2) . . ? C3 C4 H42 116(2) . . ? S1 C4 H42 100(2) . . ? H41 C4 H42 111(3) . . ? N2 C5 N1 127.8(3) . . ? N2 C5 S1 112.0(2) . . ? N1 C5 S1 120.2(2) . . ? N1 C6 C7 122.1(3) . . ? N1 C6 H6 116(2) . . ? C7 C6 H6 121(2) . . ? C6 C7 C8 118.2(4) . . ? C6 C7 H7 128(2) . . ? C8 C7 H7 113(2) . . ? N2 C8 C7 122.3(3) . . ? N2 C8 H8 121(2) . . ? C7 C8 H8 116(2) . . ? C11 C9 C10 121.4(2) 3_767 . ? C11 C9 H9 117(2) 3_767 . ? C10 C9 H9 121(2) . . ? C9 C10 C11 120.5(3) . . ? C9 C10 H10 120(2) . . ? C11 C10 H10 119.5(19) . . ? C9 C11 C10 118.1(2) 3_767 . ? C9 C11 C12 121.3(3) 3_767 . ? C10 C11 C12 120.5(3) . . ? C11 C12 S2 116.06(19) . . ? C11 C12 H121 110.8(18) . . ? S2 C12 H121 105.6(17) . . ? C11 C12 H122 107.6(19) . . ? S2 C12 H122 98.8(18) . . ? H121 C12 H122 118(3) . . ? N3 C13 N4 126.8(3) . . ? N3 C13 S2 120.9(2) . . ? N4 C13 S2 112.3(2) . . ? N3 C14 C15 123.9(4) . . ? N3 C14 H14 122(2) . . ? C15 C14 H14 114(2) . . ? C14 C15 C16 116.2(4) . . ? C14 C15 H15 122(3) . . ? C16 C15 H15 121(3) . . ? N4 C16 C15 122.8(3) . . ? N4 C16 H16 107(4) . . ? C15 C16 H16 128(4) . . ? 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 C3 C1 C2 C3 0.4(5) 3_676 . . . ? C1 C2 C3 C1 -0.4(4) . . . 3_676 ? C1 C2 C3 C4 178.4(2) . . . . ? C2 C3 C4 S1 60.9(3) . . . . ? C1 C3 C4 S1 -120.3(2) 3_676 . . . ? C5 S1 C4 C3 85.2(2) . . . . ? C8 N2 C5 N1 1.0(5) . . . . ? C8 N2 C5 S1 -178.8(3) . . . . ? C6 N1 C5 N2 -0.8(4) . . . . ? C6 N1 C5 S1 178.9(2) . . . . ? C4 S1 C5 N2 178.1(2) . . . . ? C4 S1 C5 N1 -1.7(3) . . . . ? C5 N1 C6 C7 -0.3(5) . . . . ? N1 C6 C7 C8 1.0(6) . . . . ? C5 N2 C8 C7 -0.1(6) . . . . ? C6 C7 C8 N2 -0.8(7) . . . . ? C11 C9 C10 C11 0.3(4) 3_767 . . . ? C9 C10 C11 C9 -0.3(4) . . . 3_767 ? C9 C10 C11 C12 -178.8(2) . . . . ? C9 C11 C12 S2 122.3(2) 3_767 . . . ? C10 C11 C12 S2 -59.3(3) . . . . ? C13 S2 C12 C11 -84.0(2) . . . . ? C14 N3 C13 N4 -0.3(4) . . . . ? C14 N3 C13 S2 -179.5(2) . . . . ? C16 N4 C13 N3 -0.8(5) . . . . ? C16 N4 C13 S2 178.4(3) . . . . ? C12 S2 C13 N3 4.4(3) . . . . ? C12 S2 C13 N4 -174.9(2) . . . . ? C13 N3 C14 C15 1.1(5) . . . . ? N3 C14 C15 C16 -0.7(6) . . . . ? C13 N4 C16 C15 1.2(6) . . . . ? C14 C15 C16 N4 -0.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.445 _refine_diff_density_min -0.181 _refine_diff_density_rms 0.069 #===END data_Complex_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Cu4(C15H13N5S2)2I4' _chemical_formula_sum 'C30 H26 Cu4 I4 N10 S4' _chemical_formula_weight 1416.61 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 P2(1)/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 13.2104(10) _cell_length_b 9.9479(8) _cell_length_c 15.2018(11) _cell_angle_alpha 90.00 _cell_angle_beta 95.7570(10) _cell_angle_gamma 90.00 _cell_volume 1987.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12262 _cell_measurement_theta_min 1.95 _cell_measurement_theta_max 27.89 _exptl_crystal_description BLOCK _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.367 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 5.466 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.5847 _exptl_absorpt_correction_T_max 0.7351 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12262 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_sigmaI/netI 0.0398 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 27.89 _reflns_number_total 4601 _reflns_number_gt 3635 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0464P)^2^+3.0631P] 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 4601 _refine_ls_number_parameters 236 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1002 _refine_ls_wR_factor_gt 0.0935 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 I1 I 0.85381(3) 0.90676(3) 0.03574(2) 0.03727(11) Uani 1 1 d . . . I2 I 1.04554(3) 1.14608(4) 0.22295(3) 0.04867(13) Uani 1 1 d . . . Cu1 Cu 0.96330(7) 0.91376(8) 0.19167(6) 0.0556(2) Uani 1 1 d . . . Cu2 Cu 0.97607(6) 1.11441(7) 0.05687(5) 0.0494(2) Uani 1 1 d . . . S2 S 0.80292(11) 0.92557(14) 0.27974(9) 0.0391(3) Uani 1 1 d . . . S1 S 1.14122(11) 0.82277(14) 0.13486(9) 0.0405(3) Uani 1 1 d . . . N3 N 0.9860(3) 0.7390(4) 0.2658(3) 0.0342(10) Uani 1 1 d . . . N4 N 0.8534(3) 0.8733(5) 0.4508(3) 0.0410(11) Uani 1 1 d . . . N2 N 1.1498(3) 0.5584(5) 0.1019(3) 0.0401(11) Uani 1 1 d . . . C4 C 1.1270(4) 0.6795(5) 0.0672(4) 0.0347(11) Uani 1 1 d . . . N5 N 0.8482(3) 1.1035(5) 0.4031(3) 0.0423(11) Uani 1 1 d . . . C6 C 1.0786(4) 0.6808(6) 0.2789(4) 0.0411(13) Uani 1 1 d . . . C11 C 0.8041(4) 0.7446(6) 0.2850(4) 0.0413(13) Uani 1 1 d . . . H11A H 0.7634 0.7165 0.3314 0.050 Uiso 1 1 calc R . . H11B H 0.7718 0.7097 0.2296 0.050 Uiso 1 1 calc R . . C12 C 0.8399(4) 0.9708(5) 0.3907(3) 0.0331(11) Uani 1 1 d . . . C10 C 0.9080(4) 0.6825(5) 0.3022(3) 0.0370(12) Uani 1 1 d . . . C15 C 0.8763(4) 1.1389(7) 0.4862(4) 0.0509(16) Uani 1 1 d . . . H15 H 0.8837 1.2300 0.4991 0.061 Uiso 1 1 calc R . . C5 C 1.1660(4) 0.7494(6) 0.2433(4) 0.0465(14) Uani 1 1 d . . . H5A H 1.2208 0.6847 0.2417 0.056 Uiso 1 1 calc R . . H5B H 1.1900 0.8198 0.2843 0.056 Uiso 1 1 calc R . . N1 N 1.0931(3) 0.7060(4) -0.0171(3) 0.0341(9) Uani 1 1 d . . . C1 C 1.0902(4) 0.6006(5) -0.0728(4) 0.0388(12) Uani 1 1 d . . . H1 H 1.0708 0.6147 -0.1326 0.047 Uiso 1 1 calc R . . C2 C 1.1150(4) 0.4731(6) -0.0439(4) 0.0397(13) Uani 1 1 d . . . H2 H 1.1131 0.4009 -0.0829 0.048 Uiso 1 1 calc R . . C3 C 1.1424(4) 0.4564(5) 0.0441(4) 0.0437(14) Uani 1 1 d . . . H3 H 1.1568 0.3700 0.0651 0.052 Uiso 1 1 calc R . . C13 C 0.8818(4) 0.9161(7) 0.5332(4) 0.0509(16) Uani 1 1 d . . . H13 H 0.8931 0.8534 0.5785 0.061 Uiso 1 1 calc R . . C14 C 0.8947(4) 1.0504(8) 0.5525(4) 0.0547(17) Uani 1 1 d . . . H14 H 0.9154 1.0790 0.6097 0.066 Uiso 1 1 calc R . . C9 C 0.9203(5) 0.5662(6) 0.3529(4) 0.0534(16) Uani 1 1 d . . . H9 H 0.8654 0.5296 0.3782 0.064 Uiso 1 1 calc R . . C7 C 1.0947(5) 0.5645(7) 0.3274(5) 0.0593(18) Uani 1 1 d . . . H7 H 1.1589 0.5254 0.3350 0.071 Uiso 1 1 calc R . . C8 C 1.0132(6) 0.5064(7) 0.3652(5) 0.068(2) Uani 1 1 d . . . H8 H 1.0223 0.4279 0.3983 0.082 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 0.0411(2) 0.03533(19) 0.0358(2) -0.00232(14) 0.00600(14) -0.00488(15) I2 0.0582(3) 0.0466(2) 0.0401(2) -0.00240(16) -0.00057(17) -0.00917(18) Cu1 0.0635(5) 0.0418(4) 0.0578(5) 0.0107(3) -0.0125(4) -0.0079(4) Cu2 0.0624(5) 0.0363(4) 0.0478(4) -0.0018(3) -0.0032(4) -0.0027(3) S2 0.0397(7) 0.0443(8) 0.0328(7) -0.0013(6) 0.0007(6) 0.0067(6) S1 0.0409(8) 0.0378(7) 0.0432(8) -0.0074(6) 0.0063(6) 0.0002(6) N3 0.038(2) 0.033(2) 0.031(2) -0.0036(18) -0.0008(19) 0.0007(19) N4 0.039(3) 0.048(3) 0.037(3) 0.000(2) 0.005(2) 0.007(2) N2 0.032(2) 0.036(2) 0.052(3) 0.001(2) 0.008(2) 0.0080(19) C4 0.024(2) 0.037(3) 0.044(3) -0.006(2) 0.012(2) 0.000(2) N5 0.038(3) 0.040(3) 0.050(3) -0.007(2) 0.010(2) 0.000(2) C6 0.048(3) 0.042(3) 0.033(3) -0.004(2) 0.001(2) 0.009(3) C11 0.038(3) 0.044(3) 0.040(3) -0.007(2) -0.003(2) -0.003(2) C12 0.021(2) 0.045(3) 0.034(3) -0.001(2) 0.006(2) 0.000(2) C10 0.046(3) 0.033(3) 0.031(3) -0.007(2) 0.000(2) -0.004(2) C15 0.041(3) 0.049(4) 0.063(4) -0.022(3) 0.011(3) -0.001(3) C5 0.043(3) 0.052(4) 0.044(3) -0.008(3) -0.001(3) 0.013(3) N1 0.031(2) 0.036(2) 0.036(2) -0.0041(19) 0.0095(19) 0.0007(18) C1 0.037(3) 0.038(3) 0.043(3) -0.008(2) 0.013(2) -0.005(2) C2 0.031(3) 0.037(3) 0.054(4) -0.011(3) 0.014(2) 0.004(2) C3 0.033(3) 0.027(3) 0.072(4) 0.000(3) 0.012(3) 0.002(2) C13 0.042(3) 0.081(5) 0.029(3) 0.001(3) 0.001(2) 0.009(3) C14 0.035(3) 0.090(5) 0.039(3) -0.027(3) 0.005(3) 0.005(3) C9 0.067(4) 0.041(3) 0.053(4) 0.006(3) 0.011(3) -0.001(3) C7 0.063(4) 0.052(4) 0.063(4) 0.008(3) 0.007(3) 0.026(3) C8 0.086(5) 0.047(4) 0.073(5) 0.024(3) 0.019(4) 0.017(4) _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 2.6220(8) . ? I1 Cu1 2.6510(9) . ? I1 Cu2 2.7770(9) 3_775 ? I2 Cu1 2.5777(9) . ? I2 Cu2 2.6174(9) . ? Cu1 N3 2.077(4) . ? Cu1 S2 2.6200(17) . ? Cu1 S1 2.7380(17) . ? Cu2 N1 2.069(4) 3_775 ? Cu2 I1 2.7770(9) 3_775 ? Cu2 Cu2 2.9649(15) 3_775 ? S2 C12 1.766(5) . ? S2 C11 1.802(6) . ? S1 C4 1.757(5) . ? S1 C5 1.803(6) . ? N3 C10 1.341(7) . ? N3 C6 1.350(7) . ? N4 C12 1.333(7) . ? N4 C13 1.341(7) . ? N2 C4 1.337(7) . ? N2 C3 1.339(7) . ? C4 N1 1.340(7) . ? N5 C15 1.327(8) . ? N5 C12 1.337(7) . ? C6 C7 1.377(8) . ? C6 C5 1.489(8) . ? C11 C10 1.504(8) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C10 C9 1.390(8) . ? C15 C14 1.343(9) . ? C15 H15 0.9300 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? N1 C1 1.345(7) . ? N1 Cu2 2.069(4) 3_775 ? C1 C2 1.372(8) . ? C1 H1 0.9300 . ? C2 C3 1.360(8) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C13 C14 1.374(10) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C9 C8 1.359(9) . ? C9 H9 0.9300 . ? C7 C8 1.396(10) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? 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 66.15(2) . . ? Cu2 I1 Cu2 66.55(3) . 3_775 ? Cu1 I1 Cu2 93.36(3) . 3_775 ? Cu1 I2 Cu2 67.27(3) . . ? N3 Cu1 I2 127.94(12) . . ? N3 Cu1 S2 80.81(13) . . ? I2 Cu1 S2 102.30(4) . . ? N3 Cu1 I1 119.97(12) . . ? I2 Cu1 I1 111.75(3) . . ? S2 Cu1 I1 93.53(4) . . ? N3 Cu1 S1 79.21(13) . . ? I2 Cu1 S1 89.73(4) . . ? S2 Cu1 S1 160.01(5) . . ? I1 Cu1 S1 96.77(4) . . ? N1 Cu2 I2 106.24(12) 3_775 . ? N1 Cu2 I1 113.33(12) 3_775 . ? I2 Cu2 I1 111.42(3) . . ? N1 Cu2 I1 105.87(12) 3_775 3_775 ? I2 Cu2 I1 105.95(3) . 3_775 ? I1 Cu2 I1 113.45(3) . 3_775 ? N1 Cu2 Cu2 127.32(13) 3_775 3_775 ? I2 Cu2 Cu2 125.47(4) . 3_775 ? I1 Cu2 Cu2 59.23(3) . 3_775 ? I1 Cu2 Cu2 54.22(3) 3_775 3_775 ? C12 S2 C11 102.2(3) . . ? C12 S2 Cu1 109.81(16) . . ? C11 S2 Cu1 88.52(19) . . ? C4 S1 C5 101.9(3) . . ? C4 S1 Cu1 114.08(17) . . ? C5 S1 Cu1 85.89(19) . . ? C10 N3 C6 118.8(5) . . ? C10 N3 Cu1 120.0(4) . . ? C6 N3 Cu1 121.2(4) . . ? C12 N4 C13 114.5(5) . . ? C4 N2 C3 115.2(5) . . ? N2 C4 N1 126.5(5) . . ? N2 C4 S1 119.6(4) . . ? N1 C4 S1 113.9(4) . . ? C15 N5 C12 114.1(5) . . ? N3 C6 C7 121.9(6) . . ? N3 C6 C5 118.3(5) . . ? C7 C6 C5 119.7(5) . . ? C10 C11 S2 115.0(4) . . ? C10 C11 H11A 108.5 . . ? S2 C11 H11A 108.5 . . ? C10 C11 H11B 108.5 . . ? S2 C11 H11B 108.5 . . ? H11A C11 H11B 107.5 . . ? N4 C12 N5 128.1(5) . . ? N4 C12 S2 118.4(4) . . ? N5 C12 S2 113.5(4) . . ? N3 C10 C9 121.7(5) . . ? N3 C10 C11 118.8(5) . . ? C9 C10 C11 119.5(5) . . ? N5 C15 C14 123.5(6) . . ? N5 C15 H15 118.2 . . ? C14 C15 H15 118.2 . . ? C6 C5 S1 116.2(4) . . ? C6 C5 H5A 108.2 . . ? S1 C5 H5A 108.2 . . ? C6 C5 H5B 108.2 . . ? S1 C5 H5B 108.2 . . ? H5A C5 H5B 107.4 . . ? C4 N1 C1 115.7(5) . . ? C4 N1 Cu2 123.0(3) . 3_775 ? C1 N1 Cu2 120.3(4) . 3_775 ? N1 C1 C2 121.9(5) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C3 C2 C1 117.3(5) . . ? C3 C2 H2 121.3 . . ? C1 C2 H2 121.3 . . ? N2 C3 C2 123.2(5) . . ? N2 C3 H3 118.4 . . ? C2 C3 H3 118.4 . . ? N4 C13 C14 121.7(6) . . ? N4 C13 H13 119.2 . . ? C14 C13 H13 119.2 . . ? C15 C14 C13 117.9(6) . . ? C15 C14 H14 121.0 . . ? C13 C14 H14 121.0 . . ? C8 C9 C10 119.7(6) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C6 C7 C8 119.0(6) . . ? C6 C7 H7 120.5 . . ? C8 C7 H7 120.5 . . ? C9 C8 C7 119.0(6) . . ? C9 C8 H8 120.5 . . ? C7 C8 H8 120.5 . . ? 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 Cu2 I2 Cu1 N3 158.78(16) . . . . ? Cu2 I2 Cu1 S2 -113.36(4) . . . . ? Cu2 I2 Cu1 I1 -14.46(3) . . . . ? Cu2 I2 Cu1 S1 82.73(4) . . . . ? Cu2 I1 Cu1 N3 -159.29(15) . . . . ? Cu2 I1 Cu1 N3 -96.80(14) 3_775 . . . ? Cu2 I1 Cu1 I2 14.56(3) . . . . ? Cu2 I1 Cu1 I2 77.05(4) 3_775 . . . ? Cu2 I1 Cu1 S2 119.29(4) . . . . ? Cu2 I1 Cu1 S2 -178.22(4) 3_775 . . . ? Cu2 I1 Cu1 S1 -77.86(4) . . . . ? Cu2 I1 Cu1 S1 -15.37(4) 3_775 . . . ? Cu1 I2 Cu2 N1 138.46(13) . . . 3_775 ? Cu1 I2 Cu2 I1 14.59(3) . . . . ? Cu1 I2 Cu2 I1 -109.24(3) . . . 3_775 ? Cu1 I2 Cu2 Cu2 -52.13(5) . . . 3_775 ? Cu1 I1 Cu2 N1 -134.06(13) . . . 3_775 ? Cu2 I1 Cu2 N1 120.77(13) 3_775 . . 3_775 ? Cu1 I1 Cu2 I2 -14.30(3) . . . . ? Cu2 I1 Cu2 I2 -119.47(5) 3_775 . . . ? Cu1 I1 Cu2 I1 105.17(4) . . . 3_775 ? Cu2 I1 Cu2 I1 0.0 3_775 . . 3_775 ? Cu1 I1 Cu2 Cu2 105.17(4) . . . 3_775 ? N3 Cu1 S2 C12 73.6(2) . . . . ? I2 Cu1 S2 C12 -53.4(2) . . . . ? I1 Cu1 S2 C12 -166.6(2) . . . . ? S1 Cu1 S2 C12 72.4(3) . . . . ? N3 Cu1 S2 C11 -28.8(2) . . . . ? I2 Cu1 S2 C11 -155.87(18) . . . . ? I1 Cu1 S2 C11 90.96(18) . . . . ? S1 Cu1 S2 C11 -30.1(2) . . . . ? N3 Cu1 S1 C4 71.6(2) . . . . ? I2 Cu1 S1 C4 -159.6(2) . . . . ? S2 Cu1 S1 C4 72.8(3) . . . . ? I1 Cu1 S1 C4 -47.7(2) . . . . ? N3 Cu1 S1 C5 -29.6(2) . . . . ? I2 Cu1 S1 C5 99.2(2) . . . . ? S2 Cu1 S1 C5 -28.4(3) . . . . ? I1 Cu1 S1 C5 -148.9(2) . . . . ? I2 Cu1 N3 C10 117.9(3) . . . . ? S2 Cu1 N3 C10 19.5(3) . . . . ? I1 Cu1 N3 C10 -69.3(4) . . . . ? S1 Cu1 N3 C10 -161.0(4) . . . . ? I2 Cu1 N3 C6 -61.7(4) . . . . ? S2 Cu1 N3 C6 -160.2(4) . . . . ? I1 Cu1 N3 C6 111.0(4) . . . . ? S1 Cu1 N3 C6 19.4(4) . . . . ? C3 N2 C4 N1 3.7(7) . . . . ? C3 N2 C4 S1 -176.1(4) . . . . ? C5 S1 C4 N2 -9.3(5) . . . . ? Cu1 S1 C4 N2 -100.1(4) . . . . ? C5 S1 C4 N1 170.8(4) . . . . ? Cu1 S1 C4 N1 80.1(4) . . . . ? C10 N3 C6 C7 0.7(8) . . . . ? Cu1 N3 C6 C7 -179.6(5) . . . . ? C10 N3 C6 C5 -176.0(5) . . . . ? Cu1 N3 C6 C5 3.7(6) . . . . ? C12 S2 C11 C10 -69.5(4) . . . . ? Cu1 S2 C11 C10 40.5(4) . . . . ? C13 N4 C12 N5 -2.1(8) . . . . ? C13 N4 C12 S2 179.7(4) . . . . ? C15 N5 C12 N4 2.0(8) . . . . ? C15 N5 C12 S2 -179.8(4) . . . . ? C11 S2 C12 N4 -3.9(5) . . . . ? Cu1 S2 C12 N4 -96.8(4) . . . . ? C11 S2 C12 N5 177.7(4) . . . . ? Cu1 S2 C12 N5 84.8(4) . . . . ? C6 N3 C10 C9 0.2(8) . . . . ? Cu1 N3 C10 C9 -179.5(4) . . . . ? C6 N3 C10 C11 -177.9(5) . . . . ? Cu1 N3 C10 C11 2.5(6) . . . . ? S2 C11 C10 N3 -36.7(6) . . . . ? S2 C11 C10 C9 145.2(5) . . . . ? C12 N5 C15 C14 -0.2(8) . . . . ? N3 C6 C5 S1 -41.0(6) . . . . ? C7 C6 C5 S1 142.2(5) . . . . ? C4 S1 C5 C6 -70.6(5) . . . . ? Cu1 S1 C5 C6 43.1(4) . . . . ? N2 C4 N1 C1 -5.8(7) . . . . ? S1 C4 N1 C1 174.0(3) . . . . ? N2 C4 N1 Cu2 163.0(4) . . . 3_775 ? S1 C4 N1 Cu2 -17.2(5) . . . 3_775 ? C4 N1 C1 C2 3.5(7) . . . . ? Cu2 N1 C1 C2 -165.6(4) 3_775 . . . ? N1 C1 C2 C3 0.3(8) . . . . ? C4 N2 C3 C2 0.8(7) . . . . ? C1 C2 C3 N2 -2.6(8) . . . . ? C12 N4 C13 C14 0.5(8) . . . . ? N5 C15 C14 C13 -1.1(9) . . . . ? N4 C13 C14 C15 1.0(9) . . . . ? N3 C10 C9 C8 -1.0(9) . . . . ? C11 C10 C9 C8 177.0(6) . . . . ? N3 C6 C7 C8 -0.8(10) . . . . ? C5 C6 C7 C8 175.8(6) . . . . ? C10 C9 C8 C7 0.9(11) . . . . ? C6 C7 C8 C9 0.0(11) . . . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 27.89 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.785 _refine_diff_density_min -0.921 _refine_diff_density_rms 0.143 #===END data_Complex_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Cu4(C15H13N5S2)2Br4' _chemical_formula_sum 'C30 H26 Br4 Cu4 N10 S4' _chemical_formula_weight 1228.65 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 13.1282(9) _cell_length_b 9.7714(7) _cell_length_c 14.8445(10) _cell_angle_alpha 90.00 _cell_angle_beta 95.5520(10) _cell_angle_gamma 90.00 _cell_volume 1895.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11721 _cell_measurement_theta_min 1.98 _cell_measurement_theta_max 27.88 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.153 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 6.691 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.5007 _exptl_absorpt_correction_T_max 0.6896 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11721 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 27.88 _reflns_number_total 4412 _reflns_number_gt 3354 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0408P)^2^+1.4268P] 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 4412 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0585 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.0956 _refine_ls_wR_factor_gt 0.0889 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 C9 C 0.9007(4) 0.9467(5) 0.6713(3) 0.0644(14) Uani 1 1 d . . . H9 H 0.8363 0.9872 0.6636 0.077 Uiso 1 1 calc R . . Br2 Br 0.86627(3) 0.40664(4) 1.03872(3) 0.03851(12) Uani 1 1 d . . . Br1 Br 1.04740(3) 0.63465(4) 1.21844(3) 0.04620(13) Uani 1 1 d . . . Cu1 Cu 0.96934(5) 0.40923(6) 1.19213(4) 0.05570(17) Uani 1 1 d . . . Cu2 Cu 0.97260(5) 0.61467(6) 1.05938(4) 0.05956(18) Uani 1 1 d . . . S1 S 1.19225(8) 0.57922(11) 0.72147(7) 0.0393(2) Uani 1 1 d . . . S2 S 0.85334(8) 0.68120(11) 0.86777(7) 0.0415(3) Uani 1 1 d . . . N2 N 1.1433(2) 0.6287(4) 0.5461(2) 0.0396(8) Uani 1 1 d . . . N5 N 0.9054(2) 0.7974(3) 1.0233(2) 0.0336(7) Uani 1 1 d . . . C12 C 0.8705(3) 0.8264(4) 0.9377(3) 0.0330(8) Uani 1 1 d . . . N1 N 1.1505(3) 0.3964(3) 0.5968(2) 0.0421(8) Uani 1 1 d . . . N4 N 0.8480(2) 0.9493(3) 0.9034(2) 0.0385(8) Uani 1 1 d . . . N3 N 1.0086(2) 0.7692(3) 0.7341(2) 0.0355(7) Uani 1 1 d . . . C15 C 0.9121(3) 0.9035(4) 1.0809(3) 0.0387(9) Uani 1 1 d . . . H15 H 0.9333 0.8879 1.1417 0.046 Uiso 1 1 calc R . . C5 C 1.1911(3) 0.7626(4) 0.7141(3) 0.0399(9) Uani 1 1 d . . . H5A H 1.2238 0.7992 0.7704 0.048 Uiso 1 1 calc R . . H5B H 1.2321 0.7897 0.6662 0.048 Uiso 1 1 calc R . . C4 C 1.1580(3) 0.5314(4) 0.6079(3) 0.0352(9) Uani 1 1 d . . . C10 C 0.9150(3) 0.8289(4) 0.7208(3) 0.0416(10) Uani 1 1 d . . . C6 C 1.0877(3) 0.8266(4) 0.6965(3) 0.0383(9) Uani 1 1 d . . . C11 C 0.8265(3) 0.7588(5) 0.7576(3) 0.0466(11) Uani 1 1 d . . . H11A H 0.8014 0.6883 0.7151 0.056 Uiso 1 1 calc R . . H11B H 0.7720 0.8250 0.7609 0.056 Uiso 1 1 calc R . . C13 C 0.8590(3) 1.0527(4) 0.9629(3) 0.0416(10) Uani 1 1 d . . . H13 H 0.8460 1.1412 0.9418 0.050 Uiso 1 1 calc R . . C1 C 1.1236(3) 0.3567(5) 0.5120(3) 0.0538(12) Uani 1 1 d . . . H1 H 1.1174 0.2636 0.4998 0.065 Uiso 1 1 calc R . . C14 C 0.8884(3) 1.0342(4) 1.0530(3) 0.0414(10) Uani 1 1 d . . . H14 H 0.8922 1.1072 1.0934 0.050 Uiso 1 1 calc R . . C8 C 0.9817(5) 1.0056(5) 0.6326(4) 0.0754(17) Uani 1 1 d . . . H8 H 0.9725 1.0856 0.5988 0.090 Uiso 1 1 calc R . . C2 C 1.1046(3) 0.4484(6) 0.4412(3) 0.0532(12) Uani 1 1 d . . . H2 H 1.0842 0.4190 0.3826 0.064 Uiso 1 1 calc R . . C3 C 1.1170(3) 0.5838(5) 0.4617(3) 0.0475(11) Uani 1 1 d . . . H3 H 1.1069 0.6476 0.4152 0.057 Uiso 1 1 calc R . . C7 C 1.0754(4) 0.9444(5) 0.6449(3) 0.0580(12) Uani 1 1 d . . . H7 H 1.1307 0.9816 0.6187 0.070 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 C9 0.074(3) 0.057(3) 0.062(3) 0.009(3) 0.006(3) 0.035(3) Br2 0.0470(2) 0.0322(2) 0.0360(2) -0.00202(16) 0.00193(17) -0.00480(17) Br1 0.0602(3) 0.0386(2) 0.0382(2) -0.00366(18) -0.00356(19) -0.0089(2) Cu1 0.0664(4) 0.0409(3) 0.0566(4) 0.0110(3) -0.0107(3) -0.0056(3) Cu2 0.0864(4) 0.0361(3) 0.0528(4) -0.0002(3) -0.0105(3) -0.0008(3) S1 0.0411(5) 0.0424(6) 0.0335(5) -0.0021(4) -0.0005(4) 0.0076(4) S2 0.0422(5) 0.0364(6) 0.0460(6) -0.0111(5) 0.0045(5) -0.0013(4) N2 0.0408(18) 0.046(2) 0.0320(18) -0.0053(15) 0.0015(14) 0.0050(15) N5 0.0338(16) 0.0311(17) 0.0364(18) -0.0011(14) 0.0060(14) -0.0007(13) C12 0.0261(17) 0.033(2) 0.041(2) -0.0064(17) 0.0067(16) -0.0006(15) N1 0.0433(19) 0.039(2) 0.045(2) -0.0061(16) 0.0083(16) 0.0007(15) N4 0.0357(17) 0.0333(18) 0.047(2) -0.0005(15) 0.0073(15) 0.0015(14) N3 0.0397(17) 0.0324(17) 0.0329(18) -0.0081(14) -0.0035(14) 0.0051(14) C15 0.036(2) 0.044(2) 0.038(2) -0.0058(18) 0.0113(17) -0.0028(17) C5 0.040(2) 0.040(2) 0.040(2) -0.0094(18) 0.0022(18) -0.0030(18) C4 0.0279(18) 0.041(2) 0.037(2) -0.0022(18) 0.0050(16) 0.0000(16) C10 0.047(2) 0.039(2) 0.038(2) -0.0070(18) 0.0010(18) 0.0104(18) C6 0.049(2) 0.032(2) 0.033(2) -0.0082(17) 0.0013(18) 0.0019(18) C11 0.039(2) 0.057(3) 0.041(2) -0.012(2) -0.0038(18) 0.011(2) C13 0.035(2) 0.032(2) 0.060(3) -0.0017(19) 0.0109(19) 0.0012(16) C1 0.048(2) 0.051(3) 0.064(3) -0.025(2) 0.014(2) -0.003(2) C14 0.036(2) 0.036(2) 0.053(3) -0.015(2) 0.0109(18) -0.0033(17) C8 0.102(4) 0.050(3) 0.075(4) 0.028(3) 0.015(3) 0.024(3) C2 0.038(2) 0.080(4) 0.041(3) -0.026(2) 0.0046(19) 0.001(2) C3 0.044(2) 0.066(3) 0.033(2) -0.003(2) 0.0049(18) 0.008(2) C7 0.070(3) 0.041(3) 0.063(3) 0.007(2) 0.007(3) 0.001(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 C9 C10 1.369(6) . ? C9 C8 1.382(7) . ? C9 H9 0.9300 . ? Br2 Cu2 2.4682(7) . ? Br2 Cu1 2.5341(7) . ? Br2 Cu2 2.6897(8) 3_767 ? Br1 Cu1 2.4448(7) . ? Br1 Cu2 2.4756(7) . ? Cu1 N3 2.065(3) 3_767 ? Cu1 S1 2.5855(12) 3_767 ? Cu1 S2 2.7187(12) 3_767 ? Cu1 Cu2 2.8162(8) . ? Cu2 N5 2.040(3) . ? Cu2 Br2 2.6897(8) 3_767 ? Cu2 Cu2 2.9820(12) 3_767 ? S1 C4 1.766(4) . ? S1 C5 1.795(4) . ? S1 Cu1 2.5855(12) 3_767 ? S2 C12 1.760(4) . ? S2 C11 1.806(4) . ? S2 Cu1 2.7187(12) 3_767 ? N2 C4 1.322(5) . ? N2 C3 1.341(5) . ? N5 C12 1.338(5) . ? N5 C15 1.342(5) . ? C12 N4 1.327(5) . ? N1 C4 1.331(5) . ? N1 C1 1.332(6) . ? N4 C13 1.339(5) . ? N3 C6 1.348(5) . ? N3 C10 1.357(5) . ? N3 Cu1 2.065(3) 3_767 ? C15 C14 1.369(6) . ? C15 H15 0.9300 . ? C5 C6 1.494(5) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C10 C11 1.496(6) . ? C6 C7 1.384(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C13 C14 1.368(6) . ? C13 H13 0.9300 . ? C1 C2 1.385(7) . ? C1 H1 0.9300 . ? C14 H14 0.9300 . ? C8 C7 1.364(7) . ? C8 H8 0.9300 . ? C2 C3 1.365(7) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C7 H7 0.9300 . ? 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 C10 C9 C8 120.2(4) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? Cu2 Br2 Cu1 68.51(2) . . ? Cu2 Br2 Cu2 70.49(2) . 3_767 ? Cu1 Br2 Cu2 96.19(2) . 3_767 ? Cu1 Br1 Cu2 69.82(2) . . ? N3 Cu1 Br1 129.87(9) 3_767 . ? N3 Cu1 Br2 120.24(9) 3_767 . ? Br1 Cu1 Br2 109.37(2) . . ? N3 Cu1 S1 81.59(9) 3_767 3_767 ? Br1 Cu1 S1 103.46(3) . 3_767 ? Br2 Cu1 S1 93.09(3) . 3_767 ? N3 Cu1 S2 79.52(9) 3_767 3_767 ? Br1 Cu1 S2 89.20(3) . 3_767 ? Br2 Cu1 S2 95.88(3) . 3_767 ? S1 Cu1 S2 161.10(4) 3_767 3_767 ? N3 Cu1 Cu2 164.21(9) 3_767 . ? Br1 Cu1 Cu2 55.603(19) . . ? Br2 Cu1 Cu2 54.637(19) . . ? S1 Cu1 Cu2 112.63(3) 3_767 . ? S2 Cu1 Cu2 86.06(3) 3_767 . ? N5 Cu2 Br2 117.59(9) . . ? N5 Cu2 Br1 107.64(9) . . ? Br2 Cu2 Br1 110.54(3) . . ? N5 Cu2 Br2 105.56(9) . 3_767 ? Br2 Cu2 Br2 109.51(2) . 3_767 ? Br1 Cu2 Br2 105.21(3) . 3_767 ? N5 Cu2 Cu1 140.55(9) . . ? Br2 Cu2 Cu1 56.85(2) . . ? Br1 Cu2 Cu1 54.57(2) . . ? Br2 Cu2 Cu1 112.93(3) 3_767 . ? N5 Cu2 Cu2 128.71(9) . 3_767 ? Br2 Cu2 Cu2 58.23(2) . 3_767 ? Br1 Cu2 Cu2 121.81(3) . 3_767 ? Br2 Cu2 Cu2 51.28(2) 3_767 3_767 ? Cu1 Cu2 Cu2 84.20(3) . 3_767 ? C4 S1 C5 101.90(19) . . ? C4 S1 Cu1 109.86(12) . 3_767 ? C5 S1 Cu1 89.08(13) . 3_767 ? C12 S2 C11 101.5(2) . . ? C12 S2 Cu1 112.98(12) . 3_767 ? C11 S2 Cu1 86.46(13) . 3_767 ? C4 N2 C3 114.8(4) . . ? C12 N5 C15 115.9(3) . . ? C12 N5 Cu2 122.3(2) . . ? C15 N5 Cu2 120.6(3) . . ? N4 C12 N5 126.8(4) . . ? N4 C12 S2 119.5(3) . . ? N5 C12 S2 113.7(3) . . ? C4 N1 C1 114.5(4) . . ? C12 N4 C13 115.1(4) . . ? C6 N3 C10 119.0(4) . . ? C6 N3 Cu1 119.8(3) . 3_767 ? C10 N3 Cu1 121.3(3) . 3_767 ? N5 C15 C14 121.9(4) . . ? N5 C15 H15 119.0 . . ? C14 C15 H15 119.0 . . ? C6 C5 S1 115.5(3) . . ? C6 C5 H5A 108.4 . . ? S1 C5 H5A 108.4 . . ? C6 C5 H5B 108.4 . . ? S1 C5 H5B 108.4 . . ? H5A C5 H5B 107.5 . . ? N2 C4 N1 128.5(4) . . ? N2 C4 S1 118.6(3) . . ? N1 C4 S1 112.9(3) . . ? N3 C10 C9 120.9(4) . . ? N3 C10 C11 118.3(4) . . ? C9 C10 C11 120.7(4) . . ? N3 C6 C7 121.5(4) . . ? N3 C6 C5 118.5(4) . . ? C7 C6 C5 120.0(4) . . ? C10 C11 S2 115.6(3) . . ? C10 C11 H11A 108.4 . . ? S2 C11 H11A 108.4 . . ? C10 C11 H11B 108.4 . . ? S2 C11 H11B 108.4 . . ? H11A C11 H11B 107.4 . . ? N4 C13 C14 123.2(4) . . ? N4 C13 H13 118.4 . . ? C14 C13 H13 118.4 . . ? N1 C1 C2 122.7(4) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C13 C14 C15 117.0(4) . . ? C13 C14 H14 121.5 . . ? C15 C14 H14 121.5 . . ? C7 C8 C9 118.8(5) . . ? C7 C8 H8 120.6 . . ? C9 C8 H8 120.6 . . ? C3 C2 C1 116.7(4) . . ? C3 C2 H2 121.6 . . ? C1 C2 H2 121.6 . . ? N2 C3 C2 122.7(4) . . ? N2 C3 H3 118.7 . . ? C2 C3 H3 118.7 . . ? C8 C7 C6 119.6(5) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? 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 Cu2 Br1 Cu1 N3 161.38(12) . . . 3_767 ? Cu2 Br1 Cu1 Br2 -10.19(3) . . . . ? Cu2 Br1 Cu1 S1 -108.40(3) . . . 3_767 ? Cu2 Br1 Cu1 S2 85.77(3) . . . 3_767 ? Cu2 Br2 Cu1 N3 -162.20(11) . . . 3_767 ? Cu2 Br2 Cu1 N3 -96.01(11) 3_767 . . 3_767 ? Cu2 Br2 Cu1 Br1 10.31(3) . . . . ? Cu2 Br2 Cu1 Br1 76.50(3) 3_767 . . . ? Cu2 Br2 Cu1 S1 115.74(3) . . . 3_767 ? Cu2 Br2 Cu1 S1 -178.07(3) 3_767 . . 3_767 ? Cu2 Br2 Cu1 S2 -80.92(3) . . . 3_767 ? Cu2 Br2 Cu1 S2 -14.73(3) 3_767 . . 3_767 ? Cu2 Br2 Cu1 Cu2 66.19(3) 3_767 . . . ? Cu1 Br2 Cu2 N5 -134.37(10) . . . . ? Cu2 Br2 Cu2 N5 120.42(11) 3_767 . . . ? Cu1 Br2 Cu2 Br1 -10.25(3) . . . . ? Cu2 Br2 Cu2 Br1 -115.46(4) 3_767 . . . ? Cu1 Br2 Cu2 Br2 105.21(3) . . . 3_767 ? Cu2 Br2 Cu2 Br2 0.0 3_767 . . 3_767 ? Cu2 Br2 Cu2 Cu1 -105.21(3) 3_767 . . . ? Cu1 Br2 Cu2 Cu2 105.21(3) . . . 3_767 ? Cu1 Br1 Cu2 N5 140.19(9) . . . . ? Cu1 Br1 Cu2 Br2 10.54(3) . . . . ? Cu1 Br1 Cu2 Br2 -107.59(3) . . . 3_767 ? Cu1 Br1 Cu2 Cu2 -54.05(4) . . . 3_767 ? N3 Cu1 Cu2 N5 170.5(3) 3_767 . . . ? Br1 Cu1 Cu2 N5 -73.78(14) . . . . ? Br2 Cu1 Cu2 N5 94.41(14) . . . . ? S1 Cu1 Cu2 N5 17.38(15) 3_767 . . . ? S2 Cu1 Cu2 N5 -165.52(14) 3_767 . . . ? N3 Cu1 Cu2 Br2 76.1(3) 3_767 . . . ? Br1 Cu1 Cu2 Br2 -168.20(3) . . . . ? S1 Cu1 Cu2 Br2 -77.04(4) 3_767 . . . ? S2 Cu1 Cu2 Br2 100.07(3) 3_767 . . . ? N3 Cu1 Cu2 Br1 -115.7(3) 3_767 . . . ? Br2 Cu1 Cu2 Br1 168.20(3) . . . . ? S1 Cu1 Cu2 Br1 91.16(4) 3_767 . . . ? S2 Cu1 Cu2 Br1 -91.73(3) 3_767 . . . ? N3 Cu1 Cu2 Br2 -22.9(3) 3_767 . . 3_767 ? Br1 Cu1 Cu2 Br2 92.78(3) . . . 3_767 ? Br2 Cu1 Cu2 Br2 -99.02(3) . . . 3_767 ? S1 Cu1 Cu2 Br2 -176.06(3) 3_767 . . 3_767 ? S2 Cu1 Cu2 Br2 1.05(3) 3_767 . . 3_767 ? N3 Cu1 Cu2 Cu2 20.5(3) 3_767 . . 3_767 ? Br1 Cu1 Cu2 Cu2 136.25(4) . . . 3_767 ? Br2 Cu1 Cu2 Cu2 -55.55(2) . . . 3_767 ? S1 Cu1 Cu2 Cu2 -132.59(4) 3_767 . . 3_767 ? S2 Cu1 Cu2 Cu2 44.52(3) 3_767 . . 3_767 ? Br2 Cu2 N5 C12 -64.0(3) . . . . ? Br1 Cu2 N5 C12 170.5(3) . . . . ? Br2 Cu2 N5 C12 58.5(3) 3_767 . . . ? Cu1 Cu2 N5 C12 -134.3(2) . . . . ? Cu2 Cu2 N5 C12 6.0(3) 3_767 . . . ? Br2 Cu2 N5 C15 129.1(3) . . . . ? Br1 Cu2 N5 C15 3.5(3) . . . . ? Br2 Cu2 N5 C15 -108.4(3) 3_767 . . . ? Cu1 Cu2 N5 C15 58.7(3) . . . . ? Cu2 Cu2 N5 C15 -160.9(2) 3_767 . . . ? C15 N5 C12 N4 4.4(5) . . . . ? Cu2 N5 C12 N4 -163.1(3) . . . . ? C15 N5 C12 S2 -174.9(3) . . . . ? Cu2 N5 C12 S2 17.6(4) . . . . ? C11 S2 C12 N4 9.2(3) . . . . ? Cu1 S2 C12 N4 100.2(3) 3_767 . . . ? C11 S2 C12 N5 -171.4(3) . . . . ? Cu1 S2 C12 N5 -80.4(3) 3_767 . . . ? N5 C12 N4 C13 -2.3(5) . . . . ? S2 C12 N4 C13 177.0(3) . . . . ? C12 N5 C15 C14 -2.5(5) . . . . ? Cu2 N5 C15 C14 165.2(3) . . . . ? C4 S1 C5 C6 70.9(3) . . . . ? Cu1 S1 C5 C6 -39.2(3) 3_767 . . . ? C3 N2 C4 N1 0.4(6) . . . . ? C3 N2 C4 S1 -179.7(3) . . . . ? C1 N1 C4 N2 -0.8(6) . . . . ? C1 N1 C4 S1 179.3(3) . . . . ? C5 S1 C4 N2 2.1(3) . . . . ? Cu1 S1 C4 N2 95.5(3) 3_767 . . . ? C5 S1 C4 N1 -177.9(3) . . . . ? Cu1 S1 C4 N1 -84.6(3) 3_767 . . . ? C6 N3 C10 C9 -1.0(6) . . . . ? Cu1 N3 C10 C9 -179.5(3) 3_767 . . . ? C6 N3 C10 C11 175.8(3) . . . . ? Cu1 N3 C10 C11 -2.7(5) 3_767 . . . ? C8 C9 C10 N3 1.0(7) . . . . ? C8 C9 C10 C11 -175.7(5) . . . . ? C10 N3 C6 C7 0.0(6) . . . . ? Cu1 N3 C6 C7 178.5(3) 3_767 . . . ? C10 N3 C6 C5 178.0(3) . . . . ? Cu1 N3 C6 C5 -3.5(5) 3_767 . . . ? S1 C5 C6 N3 35.9(5) . . . . ? S1 C5 C6 C7 -146.1(4) . . . . ? N3 C10 C11 S2 39.7(5) . . . . ? C9 C10 C11 S2 -143.5(4) . . . . ? C12 S2 C11 C10 70.2(3) . . . . ? Cu1 S2 C11 C10 -42.6(3) 3_767 . . . ? C12 N4 C13 C14 -1.7(5) . . . . ? C4 N1 C1 C2 -0.3(6) . . . . ? N4 C13 C14 C15 3.3(6) . . . . ? N5 C15 C14 C13 -1.0(6) . . . . ? C10 C9 C8 C7 -0.1(8) . . . . ? N1 C1 C2 C3 1.6(6) . . . . ? C4 N2 C3 C2 1.1(6) . . . . ? C1 C2 C3 N2 -2.0(6) . . . . ? C9 C8 C7 C6 -0.9(8) . . . . ? N3 C6 C7 C8 1.0(7) . . . . ? C5 C6 C7 C8 -177.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.514 _refine_diff_density_min -1.264 _refine_diff_density_rms 0.103 #===END data_Complex_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Cu2(C16H14N4S2)2I2?¡èCH3CN]n' _chemical_formula_sum 'C34 H31 Cu2 I2 N9 S4' _chemical_formula_weight 1074.80 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 P-1 _symmetry_space_group_name_H-M triclinic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5768(6) _cell_length_b 12.7908(6) _cell_length_c 15.2079(7) _cell_angle_alpha 99.3930(10) _cell_angle_beta 101.4570(10) _cell_angle_gamma 109.8780(10) _cell_volume 2009.46(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 17397 _cell_measurement_theta_min 1.41 _cell_measurement_theta_max 27.92 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.776 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1052 _exptl_absorpt_coefficient_mu 2.840 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6289 _exptl_absorpt_correction_T_max 0.7643 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17397 _diffrn_reflns_av_R_equivalents 0.0159 _diffrn_reflns_av_sigmaI/netI 0.0249 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 27.92 _reflns_number_total 8989 _reflns_number_gt 7741 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0467P)^2^+0.5728P] 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 8989 _refine_ls_number_parameters 461 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0364 _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_ref 0.0872 _refine_ls_wR_factor_gt 0.0793 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.003 _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 1.007140(17) 0.969008(15) 0.738074(13) 0.04523(7) Uani 1 1 d . . . I2 I 0.587529(18) 0.826534(15) 0.672965(14) 0.04907(7) Uani 1 1 d . . . Cu2 Cu 0.79513(4) 1.01793(3) 0.71325(3) 0.04867(10) Uani 1 1 d . . . Cu1 Cu 0.80371(4) 0.78398(3) 0.71270(2) 0.05171(10) Uani 1 1 d . . . N5 N 0.7966(2) 1.09159(19) 0.60371(16) 0.0416(5) Uani 1 1 d . . . S2 S 0.99141(8) 0.64579(7) 0.70302(6) 0.0575(2) Uani 1 1 d . . . S1 S 0.95982(9) 0.29329(7) 0.80498(6) 0.0649(2) Uani 1 1 d . . . S3 S 0.61619(9) 1.15101(8) 0.64709(7) 0.0647(2) Uani 1 1 d . . . S4 S 0.65328(12) 1.54217(8) 0.75512(6) 0.0867(4) Uani 1 1 d . . . N4 N 0.7837(2) 0.65560(19) 0.60404(15) 0.0434(5) Uani 1 1 d . . . N7 N 0.8048(2) 1.75175(19) 0.84196(16) 0.0445(5) Uani 1 1 d . . . N2 N 0.8104(2) 0.11123(19) 0.84245(17) 0.0448(5) Uani 1 1 d . . . C29 C 0.7331(3) 1.6524(2) 0.85570(19) 0.0466(7) Uani 1 1 d . . . N8 N 0.7149(3) 1.6339(2) 0.93624(19) 0.0627(7) Uani 1 1 d . . . N3 N 0.8331(3) 0.4959(2) 0.54693(18) 0.0560(6) Uani 1 1 d . . . N1 N 0.8937(4) 0.2830(2) 0.9625(2) 0.0797(10) Uani 1 1 d . . . C4 C 0.8796(3) 0.2242(2) 0.8784(2) 0.0488(7) Uani 1 1 d . . . C13 C 0.8560(3) 0.5930(2) 0.60712(19) 0.0434(6) Uani 1 1 d . . . C16 C 0.6821(3) 0.6174(3) 0.5298(2) 0.0521(7) Uani 1 1 d . . . H16 H 0.6309 0.6596 0.5230 0.062 Uiso 1 1 calc R . . C3 C 0.7527(4) 0.0558(3) 0.8988(2) 0.0623(9) Uani 1 1 d . . . H3 H 0.7043 -0.0226 0.8772 0.075 Uiso 1 1 calc R . . C20 C 0.7292(3) 1.1568(2) 0.5855(2) 0.0453(6) Uani 1 1 d . . . C22 C 0.4559(3) 1.2647(2) 0.6502(2) 0.0437(6) Uani 1 1 d . . . C11 C 1.1556(3) 0.5544(2) 0.77457(19) 0.0456(6) Uani 1 1 d . . . C6 C 1.1411(3) 0.5133(2) 0.8527(2) 0.0466(6) Uani 1 1 d . . . C17 C 0.8795(3) 1.0910(3) 0.5538(2) 0.0509(7) Uani 1 1 d . . . H17 H 0.9271 1.0460 0.5631 0.061 Uiso 1 1 calc R . . C14 C 0.7273(3) 0.4584(3) 0.4761(2) 0.0586(8) Uani 1 1 d . . . H14 H 0.7053 0.3886 0.4340 0.070 Uiso 1 1 calc R . . C12 C 1.0447(3) 0.5269(3) 0.6916(2) 0.0576(8) Uani 1 1 d . . . H12A H 0.9758 0.4562 0.6890 0.069 Uiso 1 1 calc R . . H12B H 1.0709 0.5171 0.6351 0.069 Uiso 1 1 calc R . . N6 N 0.7416(3) 1.2212(3) 0.5257(2) 0.0678(8) Uani 1 1 d . . . C30 C 0.8638(3) 1.8386(3) 0.9172(2) 0.0583(8) Uani 1 1 d . . . H30 H 0.9154 1.9093 0.9110 0.070 Uiso 1 1 calc R . . C15 C 0.6510(3) 0.5183(3) 0.4635(2) 0.0574(8) Uani 1 1 d . . . H15 H 0.5806 0.4932 0.4120 0.069 Uiso 1 1 calc R . . C10 C 1.2773(3) 0.6239(3) 0.7738(2) 0.0594(8) Uani 1 1 d . . . H10 H 1.2875 0.6526 0.7222 0.071 Uiso 1 1 calc R . . C21 C 0.5715(3) 1.2666(3) 0.6178(3) 0.0575(8) Uani 1 1 d . . . H21A H 0.6420 1.3398 0.6472 0.069 Uiso 1 1 calc R . . H21B H 0.5523 1.2574 0.5512 0.069 Uiso 1 1 calc R . . C18 C 0.8968(4) 1.1543(4) 0.4893(3) 0.0706(10) Uani 1 1 d . . . H18 H 0.9541 1.1526 0.4546 0.085 Uiso 1 1 calc R . . C32 C 0.7742(4) 1.7228(3) 1.0092(2) 0.0724(10) Uani 1 1 d . . . H32 H 0.7628 1.7137 1.0667 0.087 Uiso 1 1 calc R . . C5 C 1.0132(4) 0.4452(3) 0.8635(3) 0.0678(10) Uani 1 1 d . . . H5A H 0.9513 0.4752 0.8377 0.081 Uiso 1 1 calc R . . H5B H 1.0185 0.4529 0.9289 0.081 Uiso 1 1 calc R . . C27 C 0.4615(3) 1.3360(2) 0.7317(2) 0.0557(8) Uani 1 1 d . . . C7 C 1.2493(4) 0.5419(3) 0.9246(2) 0.0649(9) Uani 1 1 d . . . H7 H 1.2407 0.5136 0.9765 0.078 Uiso 1 1 calc R . . C23 C 0.3388(3) 1.1895(3) 0.5934(2) 0.0585(8) Uani 1 1 d . . . H23 H 0.3351 1.1401 0.5398 0.070 Uiso 1 1 calc R . . C8 C 1.3684(4) 0.6101(3) 0.9225(3) 0.0768(11) Uani 1 1 d . . . H8 H 1.4390 0.6278 0.9723 0.092 Uiso 1 1 calc R . . C31 C 0.8518(4) 1.8282(3) 1.0029(2) 0.0737(11) Uani 1 1 d . . . H31 H 0.8942 1.8897 1.0549 0.088 Uiso 1 1 calc R . . C9 C 1.3823(3) 0.6516(3) 0.8464(3) 0.0734(10) Uani 1 1 d . . . H9 H 1.4625 0.6984 0.8441 0.088 Uiso 1 1 calc R . . C24 C 0.2285(4) 1.1851(4) 0.6133(3) 0.0821(12) Uani 1 1 d . . . H24 H 0.1506 1.1334 0.5734 0.098 Uiso 1 1 calc R . . C26 C 0.3460(5) 1.3311(3) 0.7500(3) 0.0832(13) Uani 1 1 d . . . H26 H 0.3470 1.3796 0.8031 0.100 Uiso 1 1 calc R . . C2 C 0.7614(5) 0.1092(3) 0.9864(3) 0.0929(15) Uani 1 1 d . . . H2 H 0.7204 0.0693 1.0246 0.112 Uiso 1 1 calc R . . C19 C 0.8269(4) 1.2191(4) 0.4788(3) 0.0844(13) Uani 1 1 d . . . H19 H 0.8387 1.2645 0.4368 0.101 Uiso 1 1 calc R . . C28 C 0.5856(4) 1.4166(3) 0.7991(3) 0.0903(15) Uani 1 1 d . . . H28A H 0.6446 1.3781 0.8076 0.108 Uiso 1 1 calc R . . H28B H 0.5717 1.4405 0.8587 0.108 Uiso 1 1 calc R . . C25 C 0.2313(4) 1.2551(4) 0.6901(4) 0.0927(15) Uani 1 1 d . . . H25 H 0.1552 1.2523 0.7030 0.111 Uiso 1 1 calc R . . C1 C 0.8328(6) 0.2231(4) 1.0150(3) 0.1004(17) Uani 1 1 d . . . H1 H 0.8397 0.2617 1.0744 0.121 Uiso 1 1 calc R . . C34 C 0.5976(7) 0.9294(7) 0.1471(8) 0.145(3) Uani 1 1 d . . . C33 C 0.6343(7) 1.0108(7) 0.2335(6) 0.157(3) Uani 1 1 d . . . H33A H 0.6692 1.0871 0.2253 0.235 Uiso 1 1 calc R . . H33B H 0.6975 0.9984 0.2772 0.235 Uiso 1 1 calc R . . H33C H 0.5609 1.0020 0.2565 0.235 Uiso 1 1 calc R . . N9 N 0.5750(9) 0.8683(9) 0.0798(9) 0.272(6) 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 I1 0.04355(11) 0.03910(10) 0.05168(12) 0.00919(8) 0.01529(8) 0.01402(8) I2 0.04375(11) 0.03830(11) 0.05748(12) 0.00619(8) 0.01171(9) 0.01038(8) Cu2 0.0562(2) 0.04339(19) 0.0491(2) 0.01319(16) 0.02186(17) 0.01752(17) Cu1 0.0588(2) 0.0423(2) 0.04169(19) 0.00423(15) 0.00669(16) 0.01128(17) N5 0.0446(13) 0.0364(11) 0.0438(12) 0.0084(9) 0.0136(10) 0.0153(10) S2 0.0581(5) 0.0449(4) 0.0542(4) -0.0016(3) -0.0090(4) 0.0212(4) S1 0.0797(6) 0.0369(4) 0.0643(5) -0.0033(3) 0.0404(5) 0.0017(4) S3 0.0655(5) 0.0732(6) 0.0931(7) 0.0497(5) 0.0480(5) 0.0445(5) S4 0.1173(9) 0.0468(5) 0.0412(4) 0.0110(4) 0.0013(5) -0.0232(5) N4 0.0525(14) 0.0358(11) 0.0371(11) 0.0082(9) 0.0050(10) 0.0158(10) N7 0.0482(13) 0.0372(12) 0.0377(12) 0.0077(9) 0.0039(10) 0.0089(10) N2 0.0538(14) 0.0359(12) 0.0475(13) 0.0076(10) 0.0212(11) 0.0177(10) C29 0.0463(16) 0.0424(15) 0.0388(14) 0.0111(12) 0.0008(12) 0.0077(12) N8 0.0717(19) 0.0573(16) 0.0448(14) 0.0205(12) 0.0084(13) 0.0082(14) N3 0.0585(16) 0.0522(15) 0.0484(14) -0.0029(11) 0.0021(12) 0.0246(13) N1 0.130(3) 0.0432(15) 0.0617(18) 0.0008(13) 0.0475(19) 0.0217(17) C4 0.0586(18) 0.0376(14) 0.0503(16) 0.0045(12) 0.0224(14) 0.0172(13) C13 0.0452(15) 0.0411(14) 0.0382(14) 0.0074(11) 0.0067(11) 0.0133(12) C16 0.0606(19) 0.0510(17) 0.0433(15) 0.0105(13) 0.0028(13) 0.0269(15) C3 0.088(3) 0.0400(16) 0.065(2) 0.0142(15) 0.0364(19) 0.0222(16) C20 0.0448(15) 0.0470(15) 0.0486(15) 0.0142(12) 0.0162(12) 0.0200(13) C22 0.0419(14) 0.0376(14) 0.0550(16) 0.0169(12) 0.0188(12) 0.0140(12) C11 0.0496(16) 0.0403(14) 0.0420(14) 0.0023(11) 0.0050(12) 0.0190(13) C6 0.0571(17) 0.0314(13) 0.0450(15) 0.0037(11) 0.0134(13) 0.0124(12) C17 0.0584(18) 0.0537(17) 0.0491(16) 0.0126(13) 0.0206(14) 0.0286(15) C14 0.066(2) 0.0565(19) 0.0408(15) -0.0063(14) 0.0011(14) 0.0250(16) C12 0.0617(19) 0.0510(18) 0.0538(18) 0.0019(14) 0.0012(15) 0.0272(15) N6 0.082(2) 0.087(2) 0.0733(19) 0.0491(17) 0.0432(17) 0.0541(18) C30 0.074(2) 0.0389(15) 0.0464(17) 0.0054(13) 0.0084(15) 0.0101(15) C15 0.063(2) 0.0591(19) 0.0364(15) 0.0000(13) -0.0058(14) 0.0235(16) C10 0.063(2) 0.059(2) 0.0540(18) 0.0177(15) 0.0183(16) 0.0181(16) C21 0.0521(18) 0.0566(18) 0.081(2) 0.0316(17) 0.0305(17) 0.0280(15) C18 0.090(3) 0.097(3) 0.061(2) 0.037(2) 0.047(2) 0.057(2) C32 0.098(3) 0.071(2) 0.0408(17) 0.0133(16) 0.0180(18) 0.025(2) C5 0.079(2) 0.0374(16) 0.083(2) 0.0026(16) 0.042(2) 0.0125(16) C27 0.069(2) 0.0335(14) 0.0552(18) 0.0120(13) 0.0242(16) 0.0043(14) C7 0.091(3) 0.0477(18) 0.0465(17) 0.0129(14) 0.0045(17) 0.0230(18) C23 0.0507(18) 0.0482(17) 0.066(2) 0.0073(15) 0.0151(15) 0.0105(14) C8 0.066(2) 0.064(2) 0.075(3) 0.0093(19) -0.0172(19) 0.0187(19) C31 0.106(3) 0.053(2) 0.0447(18) 0.0021(15) 0.0170(19) 0.016(2) C9 0.0464(19) 0.068(2) 0.087(3) 0.012(2) 0.0085(18) 0.0076(17) C24 0.050(2) 0.063(2) 0.121(4) 0.011(2) 0.026(2) 0.0109(18) C26 0.123(4) 0.0440(18) 0.094(3) 0.0109(19) 0.073(3) 0.025(2) C2 0.166(5) 0.055(2) 0.068(2) 0.0204(19) 0.068(3) 0.033(3) C19 0.113(3) 0.118(3) 0.084(3) 0.069(3) 0.066(3) 0.078(3) C28 0.115(3) 0.052(2) 0.055(2) 0.0230(17) -0.003(2) -0.017(2) C25 0.068(3) 0.061(2) 0.160(5) 0.023(3) 0.069(3) 0.019(2) C1 0.185(5) 0.059(2) 0.066(2) 0.0085(19) 0.067(3) 0.041(3) C34 0.097(5) 0.099(5) 0.209(10) 0.036(5) 0.018(6) 0.015(4) C33 0.121(5) 0.161(7) 0.210(9) 0.035(7) 0.089(6) 0.061(5) N9 0.175(8) 0.201(9) 0.299(13) -0.070(9) -0.013(8) 0.005(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 I1 Cu1 2.6166(4) . ? I1 Cu2 2.7040(4) . ? I2 Cu2 2.6587(4) . ? I2 Cu1 2.7125(5) . ? Cu2 N5 2.044(2) . ? Cu2 N2 2.066(2) 1_565 ? Cu2 Cu1 3.0262(6) . ? Cu1 N4 2.045(2) . ? Cu1 N7 2.072(2) 1_545 ? N5 C17 1.338(4) . ? N5 C20 1.346(4) . ? S2 C13 1.758(3) . ? S2 C12 1.822(3) . ? S1 C4 1.750(3) . ? S1 C5 1.830(3) . ? S3 C20 1.743(3) . ? S3 C21 1.815(3) . ? S4 C29 1.741(3) . ? S4 C28 1.829(3) . ? N4 C13 1.340(4) . ? N4 C16 1.341(4) . ? N7 C30 1.330(4) . ? N7 C29 1.336(4) . ? N7 Cu1 2.072(2) 1_565 ? N2 C3 1.336(4) . ? N2 C4 1.346(4) . ? N2 Cu2 2.066(2) 1_545 ? C29 N8 1.328(4) . ? N8 C32 1.324(5) . ? N3 C13 1.327(4) . ? N3 C14 1.341(4) . ? N1 C4 1.322(4) . ? N1 C1 1.334(5) . ? C16 C15 1.371(4) . ? C16 H16 0.9300 . ? C3 C2 1.361(5) . ? C3 H3 0.9300 . ? C20 N6 1.320(4) . ? C22 C23 1.374(4) . ? C22 C27 1.389(4) . ? C22 C21 1.510(4) . ? C11 C10 1.391(5) . ? C11 C6 1.392(4) . ? C11 C12 1.506(4) . ? C6 C7 1.382(4) . ? C6 C5 1.499(4) . ? C17 C18 1.372(5) . ? C17 H17 0.9300 . ? C14 C15 1.359(5) . ? C14 H14 0.9300 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? N6 C19 1.332(4) . ? C30 C31 1.361(5) . ? C30 H30 0.9300 . ? C15 H15 0.9300 . ? C10 C9 1.368(5) . ? C10 H10 0.9300 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C18 C19 1.348(5) . ? C18 H18 0.9300 . ? C32 C31 1.373(5) . ? C32 H32 0.9300 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C27 C26 1.401(5) . ? C27 C28 1.497(5) . ? C7 C8 1.368(5) . ? C7 H7 0.9300 . ? C23 C24 1.355(5) . ? C23 H23 0.9300 . ? C8 C9 1.365(6) . ? C8 H8 0.9300 . ? C31 H31 0.9300 . ? C9 H9 0.9300 . ? C24 C25 1.337(6) . ? C24 H24 0.9300 . ? C26 C25 1.376(6) . ? C26 H26 0.9300 . ? C2 C1 1.351(6) . ? C2 H2 0.9300 . ? C19 H19 0.9300 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C25 H25 0.9300 . ? C1 H1 0.9300 . ? C34 N9 1.104(12) . ? C34 C33 1.423(11) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? 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 Cu2 69.308(13) . . ? Cu2 I2 Cu1 68.576(13) . . ? N5 Cu2 N2 120.38(9) . 1_565 ? N5 Cu2 I2 110.55(7) . . ? N2 Cu2 I2 106.55(7) 1_565 . ? N5 Cu2 I1 104.42(7) . . ? N2 Cu2 I1 104.23(7) 1_565 . ? I2 Cu2 I1 110.345(14) . . ? N5 Cu2 Cu1 125.57(6) . . ? N2 Cu2 Cu1 113.65(7) 1_565 . ? I2 Cu2 Cu1 56.554(12) . . ? I1 Cu2 Cu1 53.985(11) . . ? N4 Cu1 N7 119.54(9) . 1_545 ? N4 Cu1 I1 112.37(7) . . ? N7 Cu1 I1 106.30(6) 1_545 . ? N4 Cu1 I2 106.05(7) . . ? N7 Cu1 I2 100.59(7) 1_545 . ? I1 Cu1 I2 111.380(15) . . ? N4 Cu1 Cu2 129.62(6) . . ? N7 Cu1 Cu2 110.20(7) 1_545 . ? I1 Cu1 Cu2 56.707(11) . . ? I2 Cu1 Cu2 54.871(11) . . ? C17 N5 C20 115.7(2) . . ? C17 N5 Cu2 120.8(2) . . ? C20 N5 Cu2 122.83(19) . . ? C13 S2 C12 101.04(14) . . ? C4 S1 C5 102.51(15) . . ? C20 S3 C21 99.88(14) . . ? C29 S4 C28 103.11(16) . . ? C13 N4 C16 115.4(2) . . ? C13 N4 Cu1 123.70(18) . . ? C16 N4 Cu1 120.1(2) . . ? C30 N7 C29 115.7(3) . . ? C30 N7 Cu1 119.1(2) . 1_565 ? C29 N7 Cu1 124.26(18) . 1_565 ? C3 N2 C4 115.5(3) . . ? C3 N2 Cu2 118.7(2) . 1_545 ? C4 N2 Cu2 125.8(2) . 1_545 ? N8 C29 N7 126.1(3) . . ? N8 C29 S4 119.5(2) . . ? N7 C29 S4 114.3(2) . . ? C32 N8 C29 116.2(3) . . ? C13 N3 C14 115.8(3) . . ? C4 N1 C1 115.8(3) . . ? N1 C4 N2 125.8(3) . . ? N1 C4 S1 119.7(2) . . ? N2 C4 S1 114.5(2) . . ? N3 C13 N4 126.5(3) . . ? N3 C13 S2 118.3(2) . . ? N4 C13 S2 115.2(2) . . ? N4 C16 C15 122.4(3) . . ? N4 C16 H16 118.8 . . ? C15 C16 H16 118.8 . . ? N2 C3 C2 122.9(3) . . ? N2 C3 H3 118.6 . . ? C2 C3 H3 118.6 . . ? N6 C20 N5 125.5(3) . . ? N6 C20 S3 119.4(2) . . ? N5 C20 S3 115.0(2) . . ? C23 C22 C27 119.0(3) . . ? C23 C22 C21 117.0(3) . . ? C27 C22 C21 124.0(3) . . ? C10 C11 C6 118.4(3) . . ? C10 C11 C12 119.0(3) . . ? C6 C11 C12 122.5(3) . . ? C7 C6 C11 118.1(3) . . ? C7 C6 C5 119.2(3) . . ? C11 C6 C5 122.6(3) . . ? N5 C17 C18 122.3(3) . . ? N5 C17 H17 118.8 . . ? C18 C17 H17 118.8 . . ? N3 C14 C15 122.6(3) . . ? N3 C14 H14 118.7 . . ? C15 C14 H14 118.7 . . ? C11 C12 S2 107.9(2) . . ? C11 C12 H12A 110.1 . . ? S2 C12 H12A 110.1 . . ? C11 C12 H12B 110.1 . . ? S2 C12 H12B 110.1 . . ? H12A C12 H12B 108.4 . . ? C20 N6 C19 116.5(3) . . ? N7 C30 C31 122.6(3) . . ? N7 C30 H30 118.7 . . ? C31 C30 H30 118.7 . . ? C14 C15 C16 117.1(3) . . ? C14 C15 H15 121.4 . . ? C16 C15 H15 121.4 . . ? C9 C10 C11 122.1(3) . . ? C9 C10 H10 118.9 . . ? C11 C10 H10 118.9 . . ? C22 C21 S3 109.5(2) . . ? C22 C21 H21A 109.8 . . ? S3 C21 H21A 109.8 . . ? C22 C21 H21B 109.8 . . ? S3 C21 H21B 109.8 . . ? H21A C21 H21B 108.2 . . ? C19 C18 C17 116.9(3) . . ? C19 C18 H18 121.6 . . ? C17 C18 H18 121.6 . . ? N8 C32 C31 122.3(3) . . ? N8 C32 H32 118.9 . . ? C31 C32 H32 118.9 . . ? C6 C5 S1 111.0(2) . . ? C6 C5 H5A 109.4 . . ? S1 C5 H5A 109.4 . . ? C6 C5 H5B 109.4 . . ? S1 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C22 C27 C26 118.0(3) . . ? C22 C27 C28 122.2(3) . . ? C26 C27 C28 119.8(4) . . ? C8 C7 C6 122.7(3) . . ? C8 C7 H7 118.6 . . ? C6 C7 H7 118.6 . . ? C24 C23 C22 121.9(3) . . ? C24 C23 H23 119.1 . . ? C22 C23 H23 119.1 . . ? C9 C8 C7 119.2(3) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C30 C31 C32 117.0(3) . . ? C30 C31 H31 121.5 . . ? C32 C31 H31 121.5 . . ? C8 C9 C10 119.5(4) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C25 C24 C23 120.2(4) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C25 C26 C27 120.5(3) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C1 C2 C3 116.6(4) . . ? C1 C2 H2 121.7 . . ? C3 C2 H2 121.7 . . ? N6 C19 C18 123.1(3) . . ? N6 C19 H19 118.5 . . ? C18 C19 H19 118.5 . . ? C27 C28 S4 109.4(2) . . ? C27 C28 H28A 109.8 . . ? S4 C28 H28A 109.8 . . ? C27 C28 H28B 109.8 . . ? S4 C28 H28B 109.8 . . ? H28A C28 H28B 108.2 . . ? C24 C25 C26 120.4(4) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? N1 C1 C2 123.4(4) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? N9 C34 C33 176.7(11) . . ? C34 C33 H33A 109.5 . . ? C34 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C34 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? 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 I2 Cu2 N5 119.79(7) . . . . ? Cu1 I2 Cu2 N2 -107.77(7) . . . 1_565 ? Cu1 I2 Cu2 I1 4.786(12) . . . . ? Cu1 I1 Cu2 N5 -123.75(7) . . . . ? Cu1 I1 Cu2 N2 109.10(7) . . . 1_565 ? Cu1 I1 Cu2 I2 -4.938(12) . . . . ? Cu2 I1 Cu1 N4 123.69(7) . . . . ? Cu2 I1 Cu1 N7 -103.80(7) . . . 1_545 ? Cu2 I1 Cu1 I2 4.873(12) . . . . ? Cu2 I2 Cu1 N4 -127.51(7) . . . . ? Cu2 I2 Cu1 N7 107.34(7) . . . 1_545 ? Cu2 I2 Cu1 I1 -4.981(13) . . . . ? N5 Cu2 Cu1 N4 -10.84(12) . . . . ? N2 Cu2 Cu1 N4 176.52(11) 1_565 . . . ? I2 Cu2 Cu1 N4 81.74(9) . . . . ? I1 Cu2 Cu1 N4 -92.71(9) . . . . ? N5 Cu2 Cu1 N7 178.54(10) . . . 1_545 ? N2 Cu2 Cu1 N7 5.90(11) 1_565 . . 1_545 ? I2 Cu2 Cu1 N7 -88.89(7) . . . 1_545 ? I1 Cu2 Cu1 N7 96.66(7) . . . 1_545 ? N5 Cu2 Cu1 I1 81.88(8) . . . . ? N2 Cu2 Cu1 I1 -90.77(8) 1_565 . . . ? I2 Cu2 Cu1 I1 174.450(14) . . . . ? N5 Cu2 Cu1 I2 -92.57(8) . . . . ? N2 Cu2 Cu1 I2 94.78(8) 1_565 . . . ? I1 Cu2 Cu1 I2 -174.450(14) . . . . ? N2 Cu2 N5 C17 125.9(2) 1_565 . . . ? I2 Cu2 N5 C17 -109.2(2) . . . . ? I1 Cu2 N5 C17 9.5(2) . . . . ? Cu1 Cu2 N5 C17 -46.3(2) . . . . ? N2 Cu2 N5 C20 -44.4(3) 1_565 . . . ? I2 Cu2 N5 C20 80.5(2) . . . . ? I1 Cu2 N5 C20 -160.8(2) . . . . ? Cu1 Cu2 N5 C20 143.44(19) . . . . ? N7 Cu1 N4 C13 -51.7(3) 1_545 . . . ? I1 Cu1 N4 C13 73.9(2) . . . . ? I2 Cu1 N4 C13 -164.2(2) . . . . ? Cu2 Cu1 N4 C13 138.4(2) . . . . ? N7 Cu1 N4 C16 117.5(2) 1_545 . . . ? I1 Cu1 N4 C16 -116.9(2) . . . . ? I2 Cu1 N4 C16 5.0(2) . . . . ? Cu2 Cu1 N4 C16 -52.3(3) . . . . ? C30 N7 C29 N8 0.9(5) . . . . ? Cu1 N7 C29 N8 -168.3(3) 1_565 . . . ? C30 N7 C29 S4 178.0(3) . . . . ? Cu1 N7 C29 S4 8.8(3) 1_565 . . . ? C28 S4 C29 N8 -10.7(4) . . . . ? C28 S4 C29 N7 172.0(3) . . . . ? N7 C29 N8 C32 -0.1(5) . . . . ? S4 C29 N8 C32 -177.1(3) . . . . ? C1 N1 C4 N2 -0.2(6) . . . . ? C1 N1 C4 S1 -177.8(4) . . . . ? C3 N2 C4 N1 -0.4(5) . . . . ? Cu2 N2 C4 N1 -177.0(3) 1_545 . . . ? C3 N2 C4 S1 177.3(3) . . . . ? Cu2 N2 C4 S1 0.7(4) 1_545 . . . ? C5 S1 C4 N1 -13.7(4) . . . . ? C5 S1 C4 N2 168.4(3) . . . . ? C14 N3 C13 N4 0.5(5) . . . . ? C14 N3 C13 S2 178.8(3) . . . . ? C16 N4 C13 N3 -3.4(4) . . . . ? Cu1 N4 C13 N3 166.3(2) . . . . ? C16 N4 C13 S2 178.3(2) . . . . ? Cu1 N4 C13 S2 -12.0(3) . . . . ? C12 S2 C13 N3 -7.7(3) . . . . ? C12 S2 C13 N4 170.7(2) . . . . ? C13 N4 C16 C15 2.7(5) . . . . ? Cu1 N4 C16 C15 -167.4(3) . . . . ? C4 N2 C3 C2 0.5(6) . . . . ? Cu2 N2 C3 C2 177.4(4) 1_545 . . . ? C17 N5 C20 N6 -2.3(5) . . . . ? Cu2 N5 C20 N6 168.5(3) . . . . ? C17 N5 C20 S3 177.0(2) . . . . ? Cu2 N5 C20 S3 -12.2(3) . . . . ? C21 S3 C20 N6 -10.3(3) . . . . ? C21 S3 C20 N5 170.4(2) . . . . ? C10 C11 C6 C7 -1.4(4) . . . . ? C12 C11 C6 C7 178.9(3) . . . . ? C10 C11 C6 C5 175.3(3) . . . . ? C12 C11 C6 C5 -4.3(4) . . . . ? C20 N5 C17 C18 1.2(5) . . . . ? Cu2 N5 C17 C18 -169.7(3) . . . . ? C13 N3 C14 C15 3.2(5) . . . . ? C10 C11 C12 S2 -83.3(3) . . . . ? C6 C11 C12 S2 96.3(3) . . . . ? C13 S2 C12 C11 -175.2(2) . . . . ? N5 C20 N6 C19 1.2(6) . . . . ? S3 C20 N6 C19 -178.0(3) . . . . ? C29 N7 C30 C31 -0.6(5) . . . . ? Cu1 N7 C30 C31 169.2(3) 1_565 . . . ? N3 C14 C15 C16 -3.7(6) . . . . ? N4 C16 C15 C14 0.6(5) . . . . ? C6 C11 C10 C9 0.9(5) . . . . ? C12 C11 C10 C9 -179.5(3) . . . . ? C23 C22 C21 S3 -82.6(3) . . . . ? C27 C22 C21 S3 99.4(3) . . . . ? C20 S3 C21 C22 170.0(2) . . . . ? N5 C17 C18 C19 0.7(6) . . . . ? C29 N8 C32 C31 -1.0(6) . . . . ? C7 C6 C5 S1 -99.9(3) . . . . ? C11 C6 C5 S1 83.4(4) . . . . ? C4 S1 C5 C6 144.5(3) . . . . ? C23 C22 C27 C26 -2.7(5) . . . . ? C21 C22 C27 C26 175.3(3) . . . . ? C23 C22 C27 C28 177.3(3) . . . . ? C21 C22 C27 C28 -4.7(5) . . . . ? C11 C6 C7 C8 1.2(5) . . . . ? C5 C6 C7 C8 -175.6(3) . . . . ? C27 C22 C23 C24 1.8(5) . . . . ? C21 C22 C23 C24 -176.3(3) . . . . ? C6 C7 C8 C9 -0.3(6) . . . . ? N7 C30 C31 C32 -0.4(6) . . . . ? N8 C32 C31 C30 1.2(7) . . . . ? C7 C8 C9 C10 -0.3(6) . . . . ? C11 C10 C9 C8 0.1(6) . . . . ? C22 C23 C24 C25 -0.1(7) . . . . ? C22 C27 C26 C25 2.0(6) . . . . ? C28 C27 C26 C25 -178.1(4) . . . . ? N2 C3 C2 C1 -0.1(8) . . . . ? C20 N6 C19 C18 1.0(7) . . . . ? C17 C18 C19 N6 -1.8(7) . . . . ? C22 C27 C28 S4 77.2(4) . . . . ? C26 C27 C28 S4 -102.8(4) . . . . ? C29 S4 C28 C27 147.7(3) . . . . ? C23 C24 C25 C26 -0.7(7) . . . . ? C27 C26 C25 C24 -0.2(7) . . . . ? C4 N1 C1 C2 0.7(8) . . . . ? C3 C2 C1 N1 -0.5(9) . . . . ? _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 27.92 _diffrn_measured_fraction_theta_full 0.934 _refine_diff_density_max 0.855 _refine_diff_density_min -0.814 _refine_diff_density_rms 0.105 #===END data_Complex_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Cu(C16H14N4S2)I]n' _chemical_formula_sum 'C16 H14 Cu I N4 S2' _chemical_formula_weight 516.87 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.755(2) _cell_length_b 13.4624(9) _cell_length_c 8.9729(6) _cell_angle_alpha 90.00 _cell_angle_beta 99.333(2) _cell_angle_gamma 90.00 _cell_volume 3546.7(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15057 _cell_measurement_theta_min 1.39 _cell_measurement_theta_max 27.95 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.936 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 3.213 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6991 _exptl_absorpt_correction_T_max 0.8063 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15057 _diffrn_reflns_av_R_equivalents 0.0243 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 27.95 _reflns_number_total 4135 _reflns_number_gt 3524 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0529P)^2^+0.6323P] 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 4135 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0962 _refine_ls_wR_factor_gt 0.0816 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _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 I1 I 0.999927(7) 0.722054(19) 1.01157(2) 0.04505(10) Uani 1 1 d . . . Cu1 Cu 0.941253(18) 0.74395(3) 1.22983(6) 0.05201(15) Uani 1 1 d . . . S1 S 0.85337(3) 0.71212(7) 0.98498(11) 0.0465(2) Uani 1 1 d . . . S2 S 0.85561(4) 0.84330(7) 0.36726(12) 0.0557(3) Uani 1 1 d . . . C6 C 0.78681(12) 0.7561(3) 0.7529(4) 0.0442(8) Uani 1 1 d . . . N1 N 0.91081(9) 0.6119(2) 1.1795(3) 0.0395(6) Uani 1 1 d . . . C1 C 0.93017(13) 0.5283(3) 1.2398(4) 0.0479(9) Uani 1 1 d . . . H1 H 0.9535 0.5328 1.3221 0.057 Uiso 1 1 calc R . . N2 N 0.86117(12) 0.5147(2) 1.0023(4) 0.0521(8) Uani 1 1 d . . . C11 C 0.80976(12) 0.7977(3) 0.6453(4) 0.0469(8) Uani 1 1 d . . . H11 H 0.8378 0.7715 0.6323 0.056 Uiso 1 1 calc R . . C10 C 0.79221(11) 0.8764(3) 0.5577(4) 0.0461(8) Uani 1 1 d . . . C4 C 0.87671(11) 0.6002(2) 1.0627(4) 0.0391(7) Uani 1 1 d . . . C13 C 0.89117(11) 0.9289(3) 0.2968(4) 0.0423(8) Uani 1 1 d . . . C7 C 0.74586(13) 0.7975(3) 0.7748(4) 0.0525(9) Uani 1 1 d . . . H7 H 0.7303 0.7720 0.8482 0.063 Uiso 1 1 calc R . . C2 C 0.91671(14) 0.4358(3) 1.1840(5) 0.0550(9) Uani 1 1 d . . . H2 H 0.9305 0.3781 1.2262 0.066 Uiso 1 1 calc R . . C9 C 0.75061(12) 0.9154(3) 0.5792(4) 0.0531(9) Uani 1 1 d . . . H9 H 0.7379 0.9682 0.5199 0.064 Uiso 1 1 calc R . . C14 C 0.91335(15) 1.0859(3) 0.2612(5) 0.0629(11) Uani 1 1 d . . . H14 H 0.9115 1.1536 0.2793 0.075 Uiso 1 1 calc R . . C5 C 0.80679(12) 0.6682(3) 0.8442(4) 0.0498(9) Uani 1 1 d . . . H5A H 0.8179 0.6198 0.7789 0.060 Uiso 1 1 calc R . . H5B H 0.7837 0.6368 0.8932 0.060 Uiso 1 1 calc R . . N3 N 0.88586(11) 1.0248(2) 0.3206(4) 0.0549(8) Uani 1 1 d . . . C8 C 0.72820(13) 0.8765(3) 0.6874(4) 0.0612(11) Uani 1 1 d . . . H8 H 0.7006 0.9039 0.7021 0.073 Uiso 1 1 calc R . . C16 C 0.94795(13) 0.9531(3) 0.1599(4) 0.0520(9) Uani 1 1 d . . . H16 H 0.9692 0.9291 0.1035 0.062 Uiso 1 1 calc R . . C15 C 0.94392(14) 1.0536(3) 0.1754(5) 0.0609(11) Uani 1 1 d . . . H15 H 0.9614 1.0977 0.1291 0.073 Uiso 1 1 calc R . . C3 C 0.88213(14) 0.4331(3) 1.0636(4) 0.0596(10) Uani 1 1 d . . . H3 H 0.8727 0.3717 1.0224 0.071 Uiso 1 1 calc R . . N4 N 0.92269(9) 0.8879(2) 0.2222(3) 0.0416(6) Uani 1 1 d . . . C12 C 0.81813(14) 0.9273(3) 0.4466(5) 0.0627(11) Uani 1 1 d . . . H12A H 0.8360 0.9812 0.4976 0.075 Uiso 1 1 calc R . . H12B H 0.7965 0.9558 0.3653 0.075 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 0.04706(16) 0.04916(17) 0.03865(15) 0.00037(9) 0.00617(10) -0.00192(9) Cu1 0.0619(3) 0.0348(3) 0.0568(3) -0.00025(19) 0.0020(2) -0.0034(2) S1 0.0476(5) 0.0378(5) 0.0511(5) 0.0021(4) -0.0013(4) -0.0017(4) S2 0.0659(6) 0.0414(5) 0.0646(6) -0.0027(4) 0.0252(5) -0.0050(4) C6 0.0360(18) 0.050(2) 0.0438(19) -0.0040(15) -0.0011(15) -0.0029(15) N1 0.0402(15) 0.0342(14) 0.0443(15) 0.0023(12) 0.0073(12) -0.0027(12) C1 0.050(2) 0.043(2) 0.051(2) 0.0066(16) 0.0086(17) 0.0030(16) N2 0.061(2) 0.0384(17) 0.0549(19) -0.0007(13) 0.0036(16) -0.0096(14) C11 0.0376(18) 0.051(2) 0.052(2) 0.0010(16) 0.0093(15) 0.0052(16) C10 0.0446(19) 0.049(2) 0.0434(18) -0.0030(15) 0.0037(15) 0.0057(16) C4 0.0396(17) 0.0354(17) 0.0439(17) 0.0027(13) 0.0113(14) -0.0042(13) C13 0.0459(19) 0.0356(18) 0.0440(18) 0.0018(14) 0.0026(15) -0.0017(15) C7 0.042(2) 0.067(2) 0.049(2) -0.0052(18) 0.0103(16) -0.0004(18) C2 0.068(2) 0.0345(19) 0.064(2) 0.0088(17) 0.014(2) 0.0048(18) C9 0.053(2) 0.054(2) 0.050(2) -0.0019(17) -0.0002(17) 0.0165(18) C14 0.065(3) 0.034(2) 0.085(3) 0.005(2) 0.002(2) -0.0012(19) C5 0.0437(19) 0.051(2) 0.052(2) 0.0022(17) 0.0004(16) -0.0091(16) N3 0.058(2) 0.0355(16) 0.070(2) 0.0005(15) 0.0085(17) 0.0033(15) C8 0.042(2) 0.085(3) 0.057(2) -0.007(2) 0.0074(17) 0.017(2) C16 0.048(2) 0.047(2) 0.060(2) 0.0051(18) 0.0089(17) -0.0037(18) C15 0.059(2) 0.045(2) 0.078(3) 0.016(2) 0.011(2) -0.0065(19) C3 0.079(3) 0.036(2) 0.064(2) -0.0019(18) 0.011(2) -0.0103(19) N4 0.0436(15) 0.0355(15) 0.0444(15) 0.0040(12) 0.0033(12) -0.0032(12) C12 0.068(3) 0.058(2) 0.065(2) 0.014(2) 0.022(2) 0.018(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 I1 Cu1 2.6865(6) 2_757 ? I1 Cu1 2.8424(6) . ? Cu1 N1 2.013(3) . ? Cu1 N4 2.013(3) 1_556 ? Cu1 I1 2.6865(6) 2_757 ? S1 C4 1.755(3) . ? S1 C5 1.816(3) . ? S2 C13 1.750(3) . ? S2 C12 1.813(4) . ? C6 C7 1.383(5) . ? C6 C11 1.388(5) . ? C6 C5 1.504(5) . ? N1 C1 1.337(4) . ? N1 C4 1.345(4) . ? C1 C2 1.377(6) . ? C1 H1 0.9300 . ? N2 C4 1.324(4) . ? N2 C3 1.336(5) . ? C11 C10 1.372(5) . ? C11 H11 0.9300 . ? C10 C9 1.386(5) . ? C10 C12 1.519(5) . ? C13 N3 1.322(5) . ? C13 N4 1.355(4) . ? C7 C8 1.374(5) . ? C7 H7 0.9300 . ? C2 C3 1.367(6) . ? C2 H2 0.9300 . ? C9 C8 1.368(5) . ? C9 H9 0.9300 . ? C14 N3 1.331(5) . ? C14 C15 1.355(6) . ? C14 H14 0.9300 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C8 H8 0.9300 . ? C16 N4 1.336(5) . ? C16 C15 1.366(7) . ? C16 H16 0.9300 . ? C15 H15 0.9300 . ? C3 H3 0.9300 . ? N4 Cu1 2.013(3) 1_554 ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? 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 77.316(19) 2_757 . ? N1 Cu1 N4 137.02(11) . 1_556 ? N1 Cu1 I1 107.65(8) . 2_757 ? N4 Cu1 I1 105.76(8) 1_556 2_757 ? N1 Cu1 I1 93.34(8) . . ? N4 Cu1 I1 105.79(8) 1_556 . ? I1 Cu1 I1 101.351(19) 2_757 . ? C4 S1 C5 101.85(17) . . ? C13 S2 C12 100.21(19) . . ? C7 C6 C11 118.7(4) . . ? C7 C6 C5 121.3(3) . . ? C11 C6 C5 120.0(3) . . ? C1 N1 C4 116.0(3) . . ? C1 N1 Cu1 120.2(2) . . ? C4 N1 Cu1 122.2(2) . . ? N1 C1 C2 122.2(3) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C4 N2 C3 116.0(3) . . ? C10 C11 C6 121.8(3) . . ? C10 C11 H11 119.1 . . ? C6 C11 H11 119.1 . . ? C11 C10 C9 118.6(3) . . ? C11 C10 C12 122.5(3) . . ? C9 C10 C12 118.7(3) . . ? N2 C4 N1 126.1(3) . . ? N2 C4 S1 119.7(3) . . ? N1 C4 S1 114.2(2) . . ? N3 C13 N4 126.0(3) . . ? N3 C13 S2 119.3(3) . . ? N4 C13 S2 114.7(2) . . ? C8 C7 C6 119.7(4) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C3 C2 C1 116.7(4) . . ? C3 C2 H2 121.7 . . ? C1 C2 H2 121.7 . . ? C8 C9 C10 120.2(4) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? N3 C14 C15 122.8(4) . . ? N3 C14 H14 118.6 . . ? C15 C14 H14 118.6 . . ? C6 C5 S1 108.2(2) . . ? C6 C5 H5A 110.1 . . ? S1 C5 H5A 110.1 . . ? C6 C5 H5B 110.1 . . ? S1 C5 H5B 110.1 . . ? H5A C5 H5B 108.4 . . ? C13 N3 C14 116.2(3) . . ? C9 C8 C7 121.1(4) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? N4 C16 C15 122.9(4) . . ? N4 C16 H16 118.6 . . ? C15 C16 H16 118.6 . . ? C14 C15 C16 117.0(4) . . ? C14 C15 H15 121.5 . . ? C16 C15 H15 121.5 . . ? N2 C3 C2 123.0(4) . . ? N2 C3 H3 118.5 . . ? C2 C3 H3 118.5 . . ? C16 N4 C13 114.9(3) . . ? C16 N4 Cu1 118.5(2) . 1_554 ? C13 N4 Cu1 125.7(2) . 1_554 ? C10 C12 S2 112.7(3) . . ? C10 C12 H12A 109.0 . . ? S2 C12 H12A 109.0 . . ? C10 C12 H12B 109.0 . . ? S2 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? 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 -121.56(8) 2_757 . . . ? Cu1 I1 Cu1 N4 97.35(8) 2_757 . . 1_556 ? Cu1 I1 Cu1 I1 -12.81(2) 2_757 . . 2_757 ? N4 Cu1 N1 C1 -159.8(2) 1_556 . . . ? I1 Cu1 N1 C1 -20.4(3) 2_757 . . . ? I1 Cu1 N1 C1 82.6(3) . . . . ? N4 Cu1 N1 C4 35.1(3) 1_556 . . . ? I1 Cu1 N1 C4 174.5(2) 2_757 . . . ? I1 Cu1 N1 C4 -82.5(2) . . . . ? C4 N1 C1 C2 1.2(5) . . . . ? Cu1 N1 C1 C2 -164.8(3) . . . . ? C7 C6 C11 C10 -2.0(5) . . . . ? C5 C6 C11 C10 178.6(3) . . . . ? C6 C11 C10 C9 0.6(5) . . . . ? C6 C11 C10 C12 175.9(4) . . . . ? C3 N2 C4 N1 -0.9(6) . . . . ? C3 N2 C4 S1 177.0(3) . . . . ? C1 N1 C4 N2 -0.6(5) . . . . ? Cu1 N1 C4 N2 165.1(3) . . . . ? C1 N1 C4 S1 -178.6(2) . . . . ? Cu1 N1 C4 S1 -12.9(3) . . . . ? C5 S1 C4 N2 6.1(3) . . . . ? C5 S1 C4 N1 -175.8(2) . . . . ? C12 S2 C13 N3 3.5(3) . . . . ? C12 S2 C13 N4 -177.1(3) . . . . ? C11 C6 C7 C8 1.8(5) . . . . ? C5 C6 C7 C8 -178.8(4) . . . . ? N1 C1 C2 C3 -0.4(6) . . . . ? C11 C10 C9 C8 0.9(6) . . . . ? C12 C10 C9 C8 -174.6(4) . . . . ? C7 C6 C5 S1 -104.2(3) . . . . ? C11 C6 C5 S1 75.2(4) . . . . ? C4 S1 C5 C6 -172.8(2) . . . . ? N4 C13 N3 C14 2.1(6) . . . . ? S2 C13 N3 C14 -178.6(3) . . . . ? C15 C14 N3 C13 2.8(6) . . . . ? C10 C9 C8 C7 -1.1(6) . . . . ? C6 C7 C8 C9 -0.3(6) . . . . ? N3 C14 C15 C16 -4.5(6) . . . . ? N4 C16 C15 C14 1.5(6) . . . . ? C4 N2 C3 C2 1.8(6) . . . . ? C1 C2 C3 N2 -1.2(6) . . . . ? C15 C16 N4 C13 2.8(5) . . . . ? C15 C16 N4 Cu1 -166.7(3) . . . 1_554 ? N3 C13 N4 C16 -4.8(5) . . . . ? S2 C13 N4 C16 175.9(2) . . . . ? N3 C13 N4 Cu1 163.8(3) . . . 1_554 ? S2 C13 N4 Cu1 -15.5(4) . . . 1_554 ? C11 C10 C12 S2 31.0(5) . . . . ? C9 C10 C12 S2 -153.7(3) . . . . ? C13 S2 C12 C10 -162.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.95 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.780 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.187 #===END data_Complex_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Cu(C16H14N4S2)Br]n' _chemical_formula_sum 'C16 H14 Br Cu N4 S2' _chemical_formula_weight 469.88 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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.830(3) _cell_length_b 13.1418(11) _cell_length_c 8.7840(7) _cell_angle_alpha 90.00 _cell_angle_beta 98.868(2) _cell_angle_gamma 90.00 _cell_volume 3402.4(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10473 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 27.88 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.835 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 3.883 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.5754 _exptl_absorpt_correction_T_max 0.7213 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10473 _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 27.88 _reflns_number_total 3870 _reflns_number_gt 3322 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0362P)^2^+1.4613P] 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 3870 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0351 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0699 _refine_ls_wR_factor_gt 0.0671 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.004 _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 N1 N 0.91509(6) 0.10890(13) 1.1843(2) 0.0330(4) Uani 1 1 d . . . N4 N 0.92405(6) 0.39266(13) 0.22291(19) 0.0332(4) Uani 1 1 d . . . Cu1 Cu 0.941859(11) 0.24667(2) 0.23220(4) 0.04122(9) Uani 1 1 d . . . Br1 Br 0.999802(8) 0.228221(18) 0.02594(2) 0.03763(8) Uani 1 1 d . . . S1 S 0.85547(2) 0.20721(4) 0.99061(7) 0.03871(14) Uani 1 1 d . . . S2 S 0.85608(2) 0.34749(4) 0.36673(7) 0.04328(15) Uani 1 1 d . . . N2 N 0.86688(7) 0.00500(14) 1.0078(2) 0.0440(5) Uani 1 1 d . . . C13 C 0.89263(7) 0.43487(16) 0.2992(2) 0.0331(5) Uani 1 1 d . . . N3 N 0.88772(7) 0.53319(15) 0.3249(2) 0.0439(5) Uani 1 1 d . . . C6 C 0.78818(8) 0.24973(17) 0.7583(3) 0.0380(5) Uani 1 1 d . . . C10 C 0.79300(7) 0.37687(17) 0.5623(2) 0.0368(5) Uani 1 1 d . . . C11 C 0.81116(8) 0.29636(17) 0.6521(3) 0.0380(5) Uani 1 1 d . . . H11 H 0.8398 0.2726 0.6409 0.046 Uiso 1 1 calc R . . C4 C 0.88103(7) 0.09434(16) 1.0678(2) 0.0322(4) Uani 1 1 d . . . C12 C 0.81900(9) 0.43239(19) 0.4532(3) 0.0483(6) Uani 1 1 d . . . H12A H 0.8370 0.4859 0.5088 0.058 Uiso 1 1 calc R . . H12B H 0.7977 0.4640 0.3724 0.058 Uiso 1 1 calc R . . C9 C 0.75000(8) 0.41111(19) 0.5801(3) 0.0435(6) Uani 1 1 d . . . H9 H 0.7367 0.4642 0.5192 0.052 Uiso 1 1 calc R . . C16 C 0.94954(8) 0.45884(18) 0.1582(3) 0.0411(5) Uani 1 1 d . . . H16 H 0.9706 0.4338 0.0997 0.049 Uiso 1 1 calc R . . C14 C 0.91526(8) 0.59602(18) 0.2646(3) 0.0480(6) Uani 1 1 d . . . H14 H 0.9136 0.6653 0.2842 0.058 Uiso 1 1 calc R . . C5 C 0.80915(8) 0.16018(18) 0.8499(3) 0.0429(5) Uani 1 1 d . . . H5A H 0.8204 0.1113 0.7822 0.052 Uiso 1 1 calc R . . H5B H 0.7867 0.1267 0.9016 0.052 Uiso 1 1 calc R . . C1 C 0.93656(8) 0.02536(18) 1.2450(3) 0.0415(5) Uani 1 1 d . . . H1 H 0.9601 0.0322 1.3271 0.050 Uiso 1 1 calc R . . C7 C 0.74589(8) 0.2864(2) 0.7768(3) 0.0454(6) Uani 1 1 d . . . H7 H 0.7301 0.2571 0.8492 0.055 Uiso 1 1 calc R . . C3 C 0.89006(9) -0.07598(18) 1.0692(3) 0.0513(6) Uani 1 1 d . . . H3 H 0.8820 -0.1397 1.0278 0.062 Uiso 1 1 calc R . . C15 C 0.94587(8) 0.56276(18) 0.1749(3) 0.0469(6) Uani 1 1 d . . . H15 H 0.9634 0.6079 0.1275 0.056 Uiso 1 1 calc R . . C2 C 0.92479(9) -0.07001(18) 1.1891(3) 0.0484(6) Uani 1 1 d . . . H2 H 0.9398 -0.1279 1.2312 0.058 Uiso 1 1 calc R . . C8 C 0.72705(8) 0.3671(2) 0.6869(3) 0.0514(6) Uani 1 1 d . . . H8 H 0.6986 0.3915 0.6992 0.062 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 N1 0.0328(9) 0.0274(9) 0.0399(10) 0.0012(7) 0.0092(8) -0.0015(7) N4 0.0355(10) 0.0261(9) 0.0371(10) 0.0039(7) 0.0028(8) -0.0016(7) Cu1 0.04533(19) 0.02572(15) 0.05189(19) -0.00086(11) 0.00524(14) -0.00158(11) Br1 0.03920(14) 0.03957(14) 0.03483(13) 0.00043(9) 0.00788(9) -0.00236(9) S1 0.0409(3) 0.0301(3) 0.0434(3) 0.0006(2) 0.0009(2) -0.0016(2) S2 0.0517(4) 0.0304(3) 0.0521(4) -0.0022(2) 0.0217(3) -0.0040(2) N2 0.0539(13) 0.0294(10) 0.0493(12) -0.0018(8) 0.0096(10) -0.0103(9) C13 0.0345(11) 0.0282(11) 0.0350(11) 0.0037(8) 0.0002(9) -0.0002(9) N3 0.0491(12) 0.0265(10) 0.0566(12) 0.0006(9) 0.0097(10) 0.0024(8) C6 0.0354(13) 0.0428(13) 0.0350(12) -0.0057(9) 0.0025(10) -0.0049(9) C10 0.0378(12) 0.0380(12) 0.0349(11) -0.0037(9) 0.0062(9) 0.0024(9) C11 0.0333(12) 0.0374(12) 0.0444(13) -0.0014(10) 0.0092(10) 0.0034(9) C4 0.0351(11) 0.0290(11) 0.0352(11) -0.0003(8) 0.0143(9) -0.0057(8) C12 0.0548(15) 0.0402(14) 0.0533(15) 0.0075(11) 0.0196(12) 0.0132(11) C9 0.0407(13) 0.0442(14) 0.0437(13) -0.0051(10) 0.0004(10) 0.0106(11) C16 0.0382(13) 0.0368(12) 0.0483(14) 0.0057(10) 0.0065(10) -0.0028(10) C14 0.0503(15) 0.0240(11) 0.0671(17) 0.0054(11) 0.0012(12) 0.0011(10) C5 0.0414(13) 0.0421(13) 0.0444(13) 0.0025(10) 0.0040(10) -0.0126(10) C1 0.0459(14) 0.0325(12) 0.0480(14) 0.0073(10) 0.0130(11) 0.0030(10) C7 0.0361(13) 0.0615(15) 0.0396(13) -0.0062(11) 0.0086(10) -0.0043(11) C3 0.0721(18) 0.0276(12) 0.0564(15) -0.0021(11) 0.0169(14) -0.0102(12) C15 0.0439(14) 0.0325(12) 0.0633(16) 0.0135(11) 0.0051(12) -0.0070(10) C2 0.0630(17) 0.0260(12) 0.0592(15) 0.0069(11) 0.0185(13) 0.0056(11) C8 0.0319(12) 0.0698(18) 0.0524(15) -0.0076(13) 0.0064(11) 0.0065(12) _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 N1 C1 1.339(3) . ? N1 C4 1.340(3) . ? N1 Cu1 1.9972(17) 1_556 ? N4 C16 1.338(3) . ? N4 C13 1.352(3) . ? N4 Cu1 1.9891(18) . ? Cu1 N1 1.9972(17) 1_554 ? Cu1 Br1 2.5418(4) 2_755 ? Cu1 Br1 2.7008(4) . ? Br1 Cu1 2.5418(4) 2_755 ? S1 C4 1.755(2) . ? S1 C5 1.814(2) . ? S2 C13 1.749(2) . ? S2 C12 1.818(2) . ? N2 C4 1.329(3) . ? N2 C3 1.336(3) . ? C13 N3 1.324(3) . ? N3 C14 1.331(3) . ? C6 C7 1.383(3) . ? C6 C11 1.383(3) . ? C6 C5 1.506(3) . ? C10 C11 1.380(3) . ? C10 C9 1.391(3) . ? C10 C12 1.511(3) . ? C11 H11 0.9300 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C9 C8 1.372(4) . ? C9 H9 0.9300 . ? C16 C15 1.380(3) . ? C16 H16 0.9300 . ? C14 C15 1.366(4) . ? C14 H14 0.9300 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C1 C2 1.372(3) . ? C1 H1 0.9300 . ? C7 C8 1.388(4) . ? C7 H7 0.9300 . ? C3 C2 1.361(4) . ? C3 H3 0.9300 . ? C15 H15 0.9300 . ? C2 H2 0.9300 . ? C8 H8 0.9300 . ? 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 C1 N1 C4 116.5(2) . . ? C1 N1 Cu1 120.54(16) . 1_556 ? C4 N1 Cu1 121.45(14) . 1_556 ? C16 N4 C13 115.24(19) . . ? C16 N4 Cu1 118.60(16) . . ? C13 N4 Cu1 125.20(14) . . ? N4 Cu1 N1 140.37(7) . 1_554 ? N4 Cu1 Br1 105.69(5) . 2_755 ? N1 Cu1 Br1 106.83(5) 1_554 2_755 ? N4 Cu1 Br1 104.69(5) . . ? N1 Cu1 Br1 93.08(5) 1_554 . ? Br1 Cu1 Br1 97.216(14) 2_755 . ? Cu1 Br1 Cu1 81.794(14) 2_755 . ? C4 S1 C5 102.41(10) . . ? C13 S2 C12 100.95(11) . . ? C4 N2 C3 115.5(2) . . ? N3 C13 N4 126.1(2) . . ? N3 C13 S2 119.45(18) . . ? N4 C13 S2 114.50(15) . . ? C13 N3 C14 116.5(2) . . ? C7 C6 C11 118.7(2) . . ? C7 C6 C5 121.4(2) . . ? C11 C6 C5 119.9(2) . . ? C11 C10 C9 118.1(2) . . ? C11 C10 C12 122.6(2) . . ? C9 C10 C12 119.2(2) . . ? C10 C11 C6 122.2(2) . . ? C10 C11 H11 118.9 . . ? C6 C11 H11 118.9 . . ? N2 C4 N1 125.9(2) . . ? N2 C4 S1 120.08(17) . . ? N1 C4 S1 114.03(15) . . ? C10 C12 S2 111.94(17) . . ? C10 C12 H12A 109.2 . . ? S2 C12 H12A 109.2 . . ? C10 C12 H12B 109.2 . . ? S2 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C8 C9 C10 120.5(2) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? N4 C16 C15 122.6(2) . . ? N4 C16 H16 118.7 . . ? C15 C16 H16 118.7 . . ? N3 C14 C15 122.6(2) . . ? N3 C14 H14 118.7 . . ? C15 C14 H14 118.7 . . ? C6 C5 S1 107.92(16) . . ? C6 C5 H5A 110.1 . . ? S1 C5 H5A 110.1 . . ? C6 C5 H5B 110.1 . . ? S1 C5 H5B 110.1 . . ? H5A C5 H5B 108.4 . . ? N1 C1 C2 121.8(2) . . ? N1 C1 H1 119.1 . . ? C2 C1 H1 119.1 . . ? C6 C7 C8 119.8(2) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? N2 C3 C2 123.4(2) . . ? N2 C3 H3 118.3 . . ? C2 C3 H3 118.3 . . ? C14 C15 C16 116.7(2) . . ? C14 C15 H15 121.7 . . ? C16 C15 H15 121.7 . . ? C3 C2 C1 116.9(2) . . ? C3 C2 H2 121.6 . . ? C1 C2 H2 121.6 . . ? C9 C8 C7 120.7(2) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? 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 C16 N4 Cu1 N1 -130.80(16) . . . 1_554 ? C13 N4 Cu1 N1 61.0(2) . . . 1_554 ? C16 N4 Cu1 Br1 85.04(16) . . . 2_755 ? C13 N4 Cu1 Br1 -83.19(16) . . . 2_755 ? C16 N4 Cu1 Br1 -17.00(16) . . . . ? C13 N4 Cu1 Br1 174.78(15) . . . . ? N4 Cu1 Br1 Cu1 97.36(5) . . . 2_755 ? N1 Cu1 Br1 Cu1 -118.40(5) 1_554 . . 2_755 ? Br1 Cu1 Br1 Cu1 -11.002(15) 2_755 . . 2_755 ? C16 N4 C13 N3 -5.8(3) . . . . ? Cu1 N4 C13 N3 162.81(17) . . . . ? C16 N4 C13 S2 174.08(15) . . . . ? Cu1 N4 C13 S2 -17.3(2) . . . . ? C12 S2 C13 N3 1.8(2) . . . . ? C12 S2 C13 N4 -178.04(16) . . . . ? N4 C13 N3 C14 2.8(3) . . . . ? S2 C13 N3 C14 -177.06(17) . . . . ? C9 C10 C11 C6 -0.3(3) . . . . ? C12 C10 C11 C6 176.1(2) . . . . ? C7 C6 C11 C10 -1.2(3) . . . . ? C5 C6 C11 C10 178.2(2) . . . . ? C3 N2 C4 N1 -1.7(4) . . . . ? C3 N2 C4 S1 176.56(17) . . . . ? C1 N1 C4 N2 0.0(3) . . . . ? Cu1 N1 C4 N2 166.10(17) 1_556 . . . ? C1 N1 C4 S1 -178.37(16) . . . . ? Cu1 N1 C4 S1 -12.2(2) 1_556 . . . ? C5 S1 C4 N2 5.9(2) . . . . ? C5 S1 C4 N1 -175.67(16) . . . . ? C11 C10 C12 S2 34.6(3) . . . . ? C9 C10 C12 S2 -149.07(19) . . . . ? C13 S2 C12 C10 -162.65(17) . . . . ? C11 C10 C9 C8 1.5(3) . . . . ? C12 C10 C9 C8 -175.0(2) . . . . ? C13 N4 C16 C15 3.4(3) . . . . ? Cu1 N4 C16 C15 -165.95(17) . . . . ? C13 N3 C14 C15 2.7(3) . . . . ? C7 C6 C5 S1 -108.2(2) . . . . ? C11 C6 C5 S1 72.4(2) . . . . ? C4 S1 C5 C6 -172.03(16) . . . . ? C4 N1 C1 C2 1.0(3) . . . . ? Cu1 N1 C1 C2 -165.24(18) 1_556 . . . ? C11 C6 C7 C8 1.4(4) . . . . ? C5 C6 C7 C8 -178.0(2) . . . . ? C4 N2 C3 C2 2.5(4) . . . . ? N3 C14 C15 C16 -4.7(4) . . . . ? N4 C16 C15 C14 1.4(3) . . . . ? N2 C3 C2 C1 -1.7(4) . . . . ? N1 C1 C2 C3 -0.2(4) . . . . ? C10 C9 C8 C7 -1.3(4) . . . . ? C6 C7 C8 C9 -0.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 0.560 _refine_diff_density_min -0.366 _refine_diff_density_rms 0.068 #===END data_Complex_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Cu(C16H14N4S2)CN]n' _chemical_formula_sum 'C17 H14 Cu N5 S2' _chemical_formula_weight 415.99 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnc2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y+1/2, z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 14.0560(12) _cell_length_b 4.8159(4) _cell_length_c 12.5757(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 851.28(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4773 _cell_measurement_theta_min 1.45 _cell_measurement_theta_max 27.50 _exptl_crystal_description plate _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.623 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 424 _exptl_absorpt_coefficient_mu 1.538 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7484 _exptl_absorpt_correction_T_max 0.8370 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4773 _diffrn_reflns_av_R_equivalents 0.0191 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 27.50 _reflns_number_total 1809 _reflns_number_gt 1723 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0840P)^2^+2.4616P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(5) _refine_ls_number_reflns 1809 _refine_ls_number_parameters 115 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0629 _refine_ls_R_factor_gt 0.0592 _refine_ls_wR_factor_ref 0.1999 _refine_ls_wR_factor_gt 0.1883 _refine_ls_goodness_of_fit_ref 1.217 _refine_ls_restrained_S_all 1.212 _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 0.5000 0.0000 0.5000(2) 0.0661(5) Uani 1 2 d S . . S1 S 0.74161(10) 0.2778(4) 0.4678(2) 0.0445(4) Uani 1 1 d . . . N1 N 0.6232(4) -0.0475(10) 0.3656(5) 0.0409(13) Uani 1 1 d D . . N2 N 0.7824(4) -0.0493(10) 0.2998(5) 0.0409(14) Uani 1 1 d D . . C1 C 0.6002(5) -0.2230(15) 0.2894(7) 0.0512(19) Uani 1 1 d D . . H1 H 0.5371 -0.2803 0.2843 0.061 Uiso 1 1 calc R . . C2 C 0.6640(4) -0.3246(16) 0.2178(7) 0.057(2) Uani 1 1 d D . . H2 H 0.6468 -0.4537 0.1663 0.069 Uiso 1 1 calc R . . C3 C 0.7545(5) -0.226(2) 0.2262(8) 0.062(2) Uani 1 1 d D . . H3 H 0.7993 -0.2872 0.1771 0.075 Uiso 1 1 calc R . . C4 C 0.7144(3) 0.0389(14) 0.3674(6) 0.0389(15) Uani 1 1 d D . . C5 C 0.8667(5) 0.3551(11) 0.4449(7) 0.0434(16) Uani 1 1 d . . . H5A H 0.8790 0.3440 0.3691 0.052 Uiso 1 1 calc R . . H5B H 0.8787 0.5450 0.4668 0.052 Uiso 1 1 calc R . . C6 C 0.9356(4) 0.1694(12) 0.5012(4) 0.0378(13) Uani 1 1 d D . . C7 C 0.9360(5) 0.1678(15) 0.6120(4) 0.0460(17) Uani 1 1 d D . . H7 H 0.8935 0.2792 0.6493 0.055 Uiso 1 1 calc R . . C8 C 1.0000 0.0000 0.6673(9) 0.061(3) Uani 1 2 d SD . . H8 H 1.0000 0.0000 0.7413 0.073 Uiso 1 2 calc SR . . C9 C 1.0000 0.0000 0.4471(7) 0.038(2) Uani 1 2 d SD . . H9 H 1.0000 0.0000 0.3731 0.046 Uiso 1 2 calc SR . . C17 C 0.5008(5) 0.3823(15) 0.5322(6) 0.0462(15) Uani 0.50 1 d P . . N5 N 0.5008(5) 0.3823(15) 0.5322(6) 0.0462(15) Uani 0.50 1 d P . . 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 0.0900(11) 0.0393(7) 0.0689(10) 0.000 0.000 0.0105(7) S1 0.0332(6) 0.0445(9) 0.0557(9) -0.0018(9) -0.0003(9) 0.0018(6) N1 0.042(3) 0.021(2) 0.060(4) -0.001(2) 0.004(3) 0.002(2) N2 0.045(3) 0.013(2) 0.064(4) 0.003(2) 0.007(3) 0.005(2) C1 0.048(4) 0.032(4) 0.074(5) -0.009(4) 0.000(4) 0.000(3) C2 0.068(5) 0.045(4) 0.059(5) -0.008(4) -0.006(5) 0.011(3) C3 0.062(4) 0.073(6) 0.052(5) -0.005(4) 0.011(4) 0.028(4) C4 0.033(3) 0.036(3) 0.047(4) 0.009(3) 0.001(3) 0.006(3) C5 0.049(4) 0.009(2) 0.071(5) 0.003(3) -0.001(3) -0.007(2) C6 0.029(3) 0.034(3) 0.051(3) 0.003(3) -0.001(3) -0.008(2) C7 0.039(3) 0.048(4) 0.051(4) -0.006(3) 0.006(3) 0.006(3) C8 0.042(5) 0.096(10) 0.044(6) 0.000 0.000 0.004(6) C9 0.035(4) 0.044(5) 0.035(5) 0.000 0.000 -0.010(4) C17 0.045(3) 0.041(3) 0.053(4) 0.000(3) 0.001(3) 0.002(3) N5 0.045(3) 0.041(3) 0.053(4) 0.000(3) 0.001(3) 0.002(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 Cu1 C17 1.885(7) . ? Cu1 N5 1.885(7) 2_655 ? Cu1 C17 1.885(7) 2_655 ? Cu1 N1 2.431(6) 2_655 ? Cu1 N1 2.431(6) . ? S1 C4 1.750(8) . ? S1 C5 1.820(7) . ? N1 C1 1.318(8) . ? N1 C4 1.348(6) . ? N2 C3 1.317(8) . ? N2 C4 1.347(6) . ? C1 C2 1.362(8) . ? C1 H1 0.9300 . ? C2 C3 1.362(8) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C5 C6 1.496(9) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.394(5) . ? C6 C9 1.396(5) . ? C7 C8 1.395(5) . ? C7 H7 0.9300 . ? C8 C7 1.395(5) 2_755 ? C8 H8 0.9300 . ? C9 C6 1.396(5) 2_755 ? C9 H9 0.9300 . ? C17 N5 1.134(14) 2_665 ? C17 C17 1.134(14) 2_665 ? 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 C17 Cu1 N5 155.2(4) . 2_655 ? C17 Cu1 C17 155.2(4) . 2_655 ? N5 Cu1 C17 0.00(9) 2_655 2_655 ? C17 Cu1 N1 93.5(2) . 2_655 ? N5 Cu1 N1 103.7(3) 2_655 2_655 ? C17 Cu1 N1 103.7(3) 2_655 2_655 ? C17 Cu1 N1 103.7(3) . . ? N5 Cu1 N1 93.5(2) 2_655 . ? C17 Cu1 N1 93.5(2) 2_655 . ? N1 Cu1 N1 91.9(3) 2_655 . ? C4 S1 C5 103.4(3) . . ? C1 N1 C4 116.3(6) . . ? C1 N1 Cu1 113.0(5) . . ? C4 N1 Cu1 129.6(5) . . ? C3 N2 C4 115.8(6) . . ? N1 C1 C2 123.3(7) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C1 C2 C3 116.0(8) . . ? C1 C2 H2 122.0 . . ? C3 C2 H2 122.0 . . ? N2 C3 C2 123.9(7) . . ? N2 C3 H3 118.0 . . ? C2 C3 H3 118.0 . . ? N2 C4 N1 124.5(7) . . ? N2 C4 S1 120.5(4) . . ? N1 C4 S1 115.0(4) . . ? C6 C5 S1 115.4(4) . . ? C6 C5 H5A 108.4 . . ? S1 C5 H5A 108.4 . . ? C6 C5 H5B 108.4 . . ? S1 C5 H5B 108.4 . . ? H5A C5 H5B 107.5 . . ? C7 C6 C9 118.8(6) . . ? C7 C6 C5 118.6(5) . . ? C9 C6 C5 122.6(5) . . ? C6 C7 C8 120.3(7) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C7 C8 C7 120.2(9) 2_755 . ? C7 C8 H8 119.9 2_755 . ? C7 C8 H8 119.9 . . ? C6 C9 C6 121.6(8) . 2_755 ? C6 C9 H9 119.2 . . ? C6 C9 H9 119.2 2_755 . ? N5 C17 C17 0.0(8) 2_665 2_665 ? N5 C17 Cu1 167.5(2) 2_665 . ? C17 C17 Cu1 167.5(2) 2_665 . ? 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 C17 Cu1 N1 C1 -140.6(6) . . . . ? N5 Cu1 N1 C1 57.3(6) 2_655 . . . ? C17 Cu1 N1 C1 57.3(6) 2_655 . . . ? N1 Cu1 N1 C1 -46.5(5) 2_655 . . . ? C17 Cu1 N1 C4 52.0(6) . . . . ? N5 Cu1 N1 C4 -110.1(6) 2_655 . . . ? C17 Cu1 N1 C4 -110.1(6) 2_655 . . . ? N1 Cu1 N1 C4 146.1(6) 2_655 . . . ? C4 N1 C1 C2 2.7(12) . . . . ? Cu1 N1 C1 C2 -166.6(7) . . . . ? N1 C1 C2 C3 -2.4(14) . . . . ? C4 N2 C3 C2 -1.7(14) . . . . ? C1 C2 C3 N2 1.9(15) . . . . ? C3 N2 C4 N1 2.0(10) . . . . ? C3 N2 C4 S1 -179.1(7) . . . . ? C1 N1 C4 N2 -2.4(10) . . . . ? Cu1 N1 C4 N2 164.7(5) . . . . ? C1 N1 C4 S1 178.6(6) . . . . ? Cu1 N1 C4 S1 -14.3(7) . . . . ? C5 S1 C4 N2 2.5(6) . . . . ? C5 S1 C4 N1 -178.5(5) . . . . ? C4 S1 C5 C6 -89.4(5) . . . . ? S1 C5 C6 C7 -63.0(7) . . . . ? S1 C5 C6 C9 117.7(5) . . . . ? C9 C6 C7 C8 0.1(9) . . . . ? C5 C6 C7 C8 -179.2(5) . . . . ? C6 C7 C8 C7 -0.1(5) . . . 2_755 ? C7 C6 C9 C6 -0.1(5) . . . 2_755 ? C5 C6 C9 C6 179.3(6) . . . 2_755 ? N5 Cu1 C17 N5 -173(4) 2_655 . . 2_665 ? C17 Cu1 C17 N5 -173(4) 2_655 . . 2_665 ? N1 Cu1 C17 N5 -39(4) 2_655 . . 2_665 ? N1 Cu1 C17 N5 54(4) . . . 2_665 ? N5 Cu1 C17 C17 -173(4) 2_655 . . 2_665 ? C17 Cu1 C17 C17 -173(4) 2_655 . . 2_665 ? N1 Cu1 C17 C17 -39(4) 2_655 . . 2_665 ? N1 Cu1 C17 C17 54(4) . . . 2_665 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.421 _refine_diff_density_min -0.469 _refine_diff_density_rms 0.120 #===END data_Complex_7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Cu(C16H14N4S2]CN]n' _chemical_formula_sum 'C17 H14 Cu N5 S2' _chemical_formula_weight 415.99 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 12.3143(11) _cell_length_b 4.8205(4) _cell_length_c 28.265(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1677.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7961 _cell_measurement_theta_min 2.88 _cell_measurement_theta_max 24.98 _exptl_crystal_description Block _exptl_crystal_colour Pale-yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.647 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 1.561 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7961 _diffrn_reflns_av_R_equivalents 0.0323 _diffrn_reflns_av_sigmaI/netI 0.0415 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 24.98 _reflns_number_total 2916 _reflns_number_gt 2453 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0623P)^2^+0.1906P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 2916 _refine_ls_number_parameters 226 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1198 _refine_ls_wR_factor_gt 0.1135 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.164 _refine_ls_shift/su_mean 0.033 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 C4 C 0.4148(6) 0.8120(16) 1.0246(3) 0.0332(16) Uani 1 1 d . . . Cu1 Cu 0.22278(5) 0.72920(15) 0.63192(10) 0.0566(2) Uani 1 1 d . . . S1 S 0.31110(14) 1.0508(3) 1.01262(5) 0.0368(4) Uani 1 1 d . . . S2 S 0.19319(15) 0.4454(3) 0.75026(5) 0.0384(5) Uani 1 1 d . . . C9 C 0.2114(6) 0.5636(11) 0.8479(3) 0.0344(17) Uani 1 1 d . . . C6 C 0.2933(5) 0.9368(11) 0.9158(3) 0.0270(15) Uani 1 1 d . . . N3 N 0.0194(6) 0.7583(10) 0.7735(3) 0.042(2) Uani 1 1 d . . . N1 N 0.4836(7) 0.7406(9) 0.9919(3) 0.039(2) Uani 1 1 d . . . C7 C 0.1838(5) 0.8887(12) 0.9108(2) 0.0343(17) Uani 1 1 d . . . H7 H 0.1354 0.9815 0.9305 0.041 Uiso 1 1 calc R . . C10 C 0.3226(5) 0.6078(13) 0.8520(3) 0.0369(17) Uani 1 1 d . . . H10 H 0.3699 0.5123 0.8322 0.044 Uiso 1 1 calc R . . N2 N 0.4178(7) 0.7159(13) 1.0671(3) 0.042(2) Uani 1 1 d . . . N4 N 0.0928(6) 0.7758(12) 0.6914(2) 0.0322(16) Uani 1 1 d . . . C11 C 0.3648(8) 0.7941(15) 0.8855(3) 0.037(2) Uani 1 1 d . . . H11 H 0.4394 0.8228 0.8877 0.045 Uiso 1 1 calc R . . C8 C 0.1444(8) 0.7088(14) 0.8779(3) 0.0297(18) Uani 1 1 d . . . H8 H 0.0698 0.6833 0.8756 0.036 Uiso 1 1 calc R . . C3 C 0.4937(7) 0.5309(16) 1.0792(3) 0.046(2) Uani 1 1 d . . . H3 H 0.4963 0.4642 1.1100 0.055 Uiso 1 1 calc R . . C1 C 0.5589(6) 0.5550(15) 1.0027(3) 0.046(2) Uani 1 1 d . . . H1 H 0.6079 0.5017 0.9794 0.055 Uiso 1 1 calc R . . C5 C 0.3364(6) 1.1361(13) 0.9513(3) 0.0421(18) Uani 1 1 d . . . H5A H 0.3052 1.3170 0.9449 0.050 Uiso 1 1 calc R . . H5B H 0.4143 1.1515 0.9468 0.050 Uiso 1 1 calc R . . C16 C 0.0134(7) 0.9584(17) 0.6831(3) 0.052(2) Uani 1 1 d . . . H16 H 0.0084 1.0284 0.6525 0.062 Uiso 1 1 calc R . . C12 C 0.1682(6) 0.3569(12) 0.8120(2) 0.0316(15) Uani 1 1 d . . . H12A H 0.0905 0.3383 0.8166 0.038 Uiso 1 1 calc R . . H12B H 0.2008 0.1774 0.8183 0.038 Uiso 1 1 calc R . . C14 C -0.0545(6) 0.9457(14) 0.7594(3) 0.047(2) Uani 1 1 d . . . H14 H -0.1049 1.0069 0.7815 0.056 Uiso 1 1 calc R . . C15 C -0.0608(7) 1.0519(15) 0.7150(3) 0.050(2) Uani 1 1 d . . . H15 H -0.1132 1.1821 0.7068 0.060 Uiso 1 1 calc R . . C2 C 0.5678(6) 0.4383(15) 1.0465(3) 0.047(2) Uani 1 1 d . . . H2 H 0.6202 0.3059 1.0537 0.056 Uiso 1 1 calc R . . C13 C 0.0886(6) 0.6899(16) 0.7381(3) 0.0310(15) Uani 1 1 d . . . C17 C 0.2572(4) 1.1111(8) 0.6312(3) 0.0359(14) Uani 0.50 1 d P . . C18 C 0.2546(4) 0.3498(11) 0.6326(3) 0.0423(13) Uani 0.50 1 d P . . N5 N 0.2572(4) 1.1111(8) 0.6312(3) 0.0359(14) Uani 0.50 1 d P . . N6 N 0.2546(4) 0.3498(11) 0.6326(3) 0.0423(13) Uani 0.50 1 d P . . 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 C4 0.045(4) 0.035(3) 0.020(3) -0.002(4) 0.000(3) -0.013(4) Cu1 0.0597(4) 0.0315(4) 0.0786(5) -0.0085(5) -0.0018(9) 0.0019(4) S1 0.0435(11) 0.0439(9) 0.0229(9) -0.0042(9) -0.0005(9) 0.0042(7) S2 0.0430(11) 0.0434(9) 0.0289(10) -0.0015(9) -0.0007(9) 0.0057(7) C9 0.050(4) 0.030(3) 0.024(4) 0.005(3) -0.001(4) -0.008(3) C6 0.030(3) 0.026(3) 0.025(4) 0.009(3) -0.004(3) -0.005(2) N3 0.020(3) 0.067(7) 0.040(4) -0.012(3) 0.001(3) -0.002(2) N1 0.065(5) 0.028(5) 0.023(3) -0.006(2) 0.007(4) 0.002(2) C7 0.046(5) 0.035(4) 0.022(4) -0.006(3) 0.006(3) 0.011(3) C10 0.032(4) 0.044(4) 0.034(5) 0.008(3) 0.002(3) -0.001(3) N2 0.048(4) 0.044(4) 0.035(4) -0.024(3) 0.010(3) 0.008(3) N4 0.037(3) 0.037(4) 0.023(3) 0.013(2) 0.007(3) 0.003(2) C11 0.038(5) 0.043(4) 0.032(4) -0.004(4) 0.007(3) -0.017(3) C8 0.021(4) 0.041(3) 0.028(4) 0.008(3) -0.006(3) 0.005(3) C3 0.057(5) 0.043(4) 0.038(5) 0.011(3) -0.025(4) 0.013(3) C1 0.038(4) 0.053(5) 0.046(7) -0.018(4) 0.013(4) -0.002(3) C5 0.048(4) 0.028(3) 0.050(5) 0.000(4) 0.002(4) -0.001(3) C16 0.062(5) 0.055(5) 0.038(5) -0.007(4) 0.022(4) 0.006(4) C12 0.049(4) 0.035(3) 0.012(3) 0.009(3) -0.006(3) -0.007(3) C14 0.030(4) 0.059(5) 0.050(7) -0.017(4) 0.003(4) 0.002(3) C15 0.044(5) 0.051(5) 0.054(6) -0.005(4) -0.009(4) 0.017(4) C2 0.044(5) 0.049(5) 0.047(6) -0.014(4) -0.001(4) 0.009(3) C13 0.028(4) 0.033(3) 0.032(4) -0.010(4) -0.007(3) -0.004(3) C17 0.050(4) 0.014(2) 0.043(3) 0.000(3) -0.011(4) 0.0010(19) C18 0.035(3) 0.059(3) 0.034(3) -0.001(6) -0.011(4) -0.001(2) N5 0.050(4) 0.014(2) 0.043(3) 0.000(3) -0.011(4) 0.0010(19) N6 0.035(3) 0.059(3) 0.034(3) -0.001(6) -0.011(4) -0.001(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 C4 N2 1.288(12) . ? C4 N1 1.299(12) . ? C4 S1 1.752(8) . ? Cu1 C18 1.871(6) . ? Cu1 C17 1.889(4) . ? Cu1 N4 2.333(7) . ? S1 C5 1.809(8) . ? S2 C13 1.780(8) . ? S2 C12 1.822(6) . ? C9 C8 1.375(11) . ? C9 C10 1.391(9) . ? C9 C12 1.519(9) . ? C6 C7 1.375(9) . ? C6 C11 1.408(11) . ? C6 C5 1.488(10) . ? N3 C14 1.344(10) . ? N3 C13 1.354(11) . ? N1 C1 1.324(11) . ? C7 C8 1.361(10) . ? C7 H7 0.9300 . ? C10 C11 1.405(11) . ? C10 H10 0.9300 . ? N2 C3 1.337(10) . ? N4 C16 1.336(10) . ? N4 C13 1.385(11) . ? C11 H11 0.9300 . ? C8 H8 0.9300 . ? C3 C2 1.373(11) . ? C3 H3 0.9300 . ? C1 C2 1.365(12) . ? C1 H1 0.9300 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C16 C15 1.359(11) . ? C16 H16 0.9300 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C14 C15 1.357(13) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C2 H2 0.9300 . ? C17 N6 1.152(6) 1_565 ? C17 C18 1.152(6) 1_565 ? C18 N5 1.152(6) 1_545 ? C18 C17 1.152(6) 1_545 ? 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 C4 N1 123.3(8) . . ? N2 C4 S1 115.9(6) . . ? N1 C4 S1 120.9(6) . . ? C18 Cu1 C17 154.96(16) . . ? C18 Cu1 N4 103.3(3) . . ? C17 Cu1 N4 93.9(3) . . ? C4 S1 C5 102.0(4) . . ? C13 S2 C12 102.6(4) . . ? C8 C9 C10 117.5(7) . . ? C8 C9 C12 122.4(7) . . ? C10 C9 C12 120.0(6) . . ? C7 C6 C11 118.0(6) . . ? C7 C6 C5 121.8(6) . . ? C11 C6 C5 120.1(6) . . ? C14 N3 C13 111.7(9) . . ? C4 N1 C1 118.2(8) . . ? C6 C7 C8 121.7(7) . . ? C6 C7 H7 119.1 . . ? C8 C7 H7 119.2 . . ? C11 C10 C9 121.2(7) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C4 N2 C3 119.9(8) . . ? C16 N4 C13 109.7(7) . . ? C16 N4 Cu1 116.1(5) . . ? C13 N4 Cu1 133.2(5) . . ? C10 C11 C6 119.4(8) . . ? C10 C11 H11 120.3 . . ? C6 C11 H11 120.3 . . ? C7 C8 C9 122.2(8) . . ? C7 C8 H8 118.9 . . ? C9 C8 H8 118.9 . . ? N2 C3 C2 120.6(8) . . ? N2 C3 H3 119.7 . . ? C2 C3 H3 119.6 . . ? N1 C1 C2 122.9(9) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.6 . . ? C6 C5 S1 116.0(5) . . ? C6 C5 H5A 108.3 . . ? S1 C5 H5A 108.3 . . ? C6 C5 H5B 108.3 . . ? S1 C5 H5B 108.3 . . ? H5A C5 H5B 107.4 . . ? N4 C16 C15 126.4(8) . . ? N4 C16 H16 116.8 . . ? C15 C16 H16 116.8 . . ? C9 C12 S2 115.3(4) . . ? C9 C12 H12A 108.4 . . ? S2 C12 H12A 108.5 . . ? C9 C12 H12B 108.4 . . ? S2 C12 H12B 108.4 . . ? H12A C12 H12B 107.5 . . ? N3 C14 C15 124.5(9) . . ? N3 C14 H14 117.8 . . ? C15 C14 H14 117.7 . . ? C16 C15 C14 116.7(8) . . ? C16 C15 H15 121.6 . . ? C14 C15 H15 121.7 . . ? C1 C2 C3 115.0(7) . . ? C1 C2 H2 122.5 . . ? C3 C2 H2 122.5 . . ? N3 C13 N4 130.9(8) . . ? N3 C13 S2 118.3(6) . . ? N4 C13 S2 110.8(6) . . ? N6 C17 C18 0.0(10) 1_565 1_565 ? N6 C17 Cu1 165.2(6) 1_565 . ? C18 C17 Cu1 165.2(6) 1_565 . ? N5 C18 C17 0.0(10) 1_545 1_545 ? N5 C18 Cu1 169.2(6) 1_545 . ? C17 C18 Cu1 169.2(6) 1_545 . ? 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 N2 C4 S1 C5 179.1(6) . . . . ? N1 C4 S1 C5 -0.6(7) . . . . ? N2 C4 N1 C1 1.7(12) . . . . ? S1 C4 N1 C1 -178.6(6) . . . . ? C11 C6 C7 C8 0.1(9) . . . . ? C5 C6 C7 C8 179.2(7) . . . . ? C8 C9 C10 C11 0.0(9) . . . . ? C12 C9 C10 C11 -178.8(6) . . . . ? N1 C4 N2 C3 -0.8(13) . . . . ? S1 C4 N2 C3 179.5(6) . . . . ? C18 Cu1 N4 C16 -143.0(6) . . . . ? C17 Cu1 N4 C16 55.3(6) . . . . ? C18 Cu1 N4 C13 50.4(7) . . . . ? C17 Cu1 N4 C13 -111.3(8) . . . . ? C9 C10 C11 C6 0.5(11) . . . . ? C7 C6 C11 C10 -0.6(10) . . . . ? C5 C6 C11 C10 -179.6(6) . . . . ? C6 C7 C8 C9 0.4(10) . . . . ? C10 C9 C8 C7 -0.4(9) . . . . ? C12 C9 C8 C7 178.3(6) . . . . ? C4 N2 C3 C2 -1.0(12) . . . . ? C4 N1 C1 C2 -0.7(12) . . . . ? C7 C6 C5 S1 63.4(8) . . . . ? C11 C6 C5 S1 -117.5(7) . . . . ? C4 S1 C5 C6 81.8(6) . . . . ? C13 N4 C16 C15 0.6(12) . . . . ? Cu1 N4 C16 C15 -169.1(7) . . . . ? C8 C9 C12 S2 116.7(6) . . . . ? C10 C9 C12 S2 -64.5(8) . . . . ? C13 S2 C12 C9 -80.5(6) . . . . ? C13 N3 C14 C15 0.8(11) . . . . ? N4 C16 C15 C14 -1.1(13) . . . . ? N3 C14 C15 C16 0.3(13) . . . . ? N1 C1 C2 C3 -1.0(12) . . . . ? N2 C3 C2 C1 1.8(11) . . . . ? C14 N3 C13 N4 -1.5(12) . . . . ? C14 N3 C13 S2 179.6(5) . . . . ? C16 N4 C13 N3 0.9(12) . . . . ? Cu1 N4 C13 N3 168.1(6) . . . . ? C16 N4 C13 S2 179.8(5) . . . . ? Cu1 N4 C13 S2 -13.0(9) . . . . ? C12 S2 C13 N3 0.9(6) . . . . ? C12 S2 C13 N4 -178.2(5) . . . . ? C18 Cu1 C17 N6 -170(2) . . . 1_565 ? N4 Cu1 C17 N6 -36(3) . . . 1_565 ? C18 Cu1 C17 C18 -170(2) . . . 1_565 ? N4 Cu1 C17 C18 -36(3) . . . 1_565 ? C17 Cu1 C18 N5 -166(3) . . . 1_545 ? N4 Cu1 C18 N5 62(3) . . . 1_545 ? C17 Cu1 C18 C17 -166(3) . . . 1_545 ? N4 Cu1 C18 C17 62(3) . . . 1_545 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.605 _refine_diff_density_min -0.284 _refine_diff_density_rms 0.079 #===END data_Complex_8 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Cu2(C16H14N4S2)I2]n' _chemical_formula_sum 'C8 H7 Cu I N2 S' _chemical_formula_weight 353.66 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 P2(1)/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 4.3816(5) _cell_length_b 16.8590(19) _cell_length_c 13.1538(14) _cell_angle_alpha 90.00 _cell_angle_beta 93.384(2) _cell_angle_gamma 90.00 _cell_volume 969.97(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5913 _cell_measurement_theta_min 1.97 _cell_measurement_theta_max 27.89 _exptl_crystal_description plate _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 668 _exptl_absorpt_coefficient_mu 5.599 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5913 _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 27.89 _reflns_number_total 2223 _reflns_number_gt 1922 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0469P)^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 2223 _refine_ls_number_parameters 118 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0798 _refine_ls_wR_factor_gt 0.0768 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 C3 C 1.0927(12) 0.7451(3) 0.2587(3) 0.0514(12) Uani 1 1 d . . . H3 H 1.1394 0.7134 0.2039 0.062 Uiso 1 1 calc R . . C2 C 1.1965(11) 0.8217(3) 0.2620(3) 0.0508(11) Uani 1 1 d . . . H2 H 1.3211 0.8415 0.2131 0.061 Uiso 1 1 calc R . . I1 I 0.34245(5) 0.945525(15) 0.623920(18) 0.03267(11) Uani 1 1 d . . . Cu1 Cu 0.80568(13) 0.91719(4) 0.51974(5) 0.05496(19) Uani 1 1 d . . . S1 S 0.6530(3) 0.72566(6) 0.50522(8) 0.0426(3) Uani 1 1 d . . . N1 N 0.9325(7) 0.83960(18) 0.4134(2) 0.0345(7) Uani 1 1 d . . . C6 C 0.7902(9) 0.5621(2) 0.4816(3) 0.0320(8) Uani 1 1 d . . . C4 C 0.8604(8) 0.7622(2) 0.4056(3) 0.0318(8) Uani 1 1 d . . . C8 C 0.8785(9) 0.5386(2) 0.5801(3) 0.0359(9) Uani 1 1 d . . . H8 H 0.7972 0.5646 0.6347 0.043 Uiso 1 1 calc R . . N2 N 0.9285(9) 0.71429(19) 0.3303(3) 0.0438(9) Uani 1 1 d . . . C7 C 0.9136(9) 0.5229(2) 0.4011(3) 0.0359(9) Uani 1 1 d . . . H7 H 0.8577 0.5377 0.3344 0.043 Uiso 1 1 calc R . . C1 C 1.1072(9) 0.8681(3) 0.3414(3) 0.0422(9) Uani 1 1 d . . . H1 H 1.1702 0.9208 0.3452 0.051 Uiso 1 1 calc R . . C5 C 0.5548(9) 0.6258(2) 0.4616(4) 0.0421(10) Uani 1 1 d . . . H5A H 0.3701 0.6098 0.4933 0.050 Uiso 1 1 calc R . . H5B H 0.5065 0.6280 0.3887 0.050 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 C3 0.081(3) 0.034(2) 0.039(2) -0.004(2) 0.010(2) 0.017(2) C2 0.059(3) 0.043(3) 0.052(3) 0.003(2) 0.016(2) 0.011(2) I1 0.03160(16) 0.02927(16) 0.03754(16) 0.00103(10) 0.00535(10) -0.00217(9) Cu1 0.0467(3) 0.0528(4) 0.0663(4) -0.0268(3) 0.0111(3) 0.0018(3) S1 0.0474(6) 0.0262(5) 0.0549(6) -0.0007(5) 0.0100(5) 0.0003(4) N1 0.0313(17) 0.0225(16) 0.0495(18) -0.0074(14) 0.0006(14) -0.0011(13) C6 0.0291(19) 0.0177(17) 0.049(2) 0.0046(15) -0.0028(16) -0.0077(14) C4 0.0298(19) 0.0231(18) 0.0420(19) -0.0046(16) -0.0035(15) 0.0043(15) C8 0.035(2) 0.024(2) 0.049(2) -0.0034(17) 0.0066(17) -0.0045(16) N2 0.063(2) 0.0221(17) 0.0462(19) -0.0064(15) 0.0001(17) 0.0045(16) C7 0.037(2) 0.030(2) 0.039(2) 0.0017(17) -0.0055(16) -0.0055(17) C1 0.041(2) 0.030(2) 0.056(2) -0.0050(19) 0.0053(19) 0.0010(17) C5 0.034(2) 0.025(2) 0.066(3) 0.0028(19) -0.0020(19) -0.0025(17) _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 C3 N2 1.325(6) . ? C3 C2 1.368(7) . ? C3 H3 0.9300 . ? C2 C1 1.380(6) . ? C2 H2 0.9300 . ? I1 Cu1 2.5602(7) . ? I1 Cu1 2.6939(7) 1_455 ? I1 Cu1 3.0338(8) 3_676 ? Cu1 N1 2.017(3) . ? Cu1 I1 2.6939(7) 1_655 ? Cu1 I1 3.0338(8) 3_676 ? S1 C4 1.750(4) . ? S1 C5 1.822(4) . ? N1 C1 1.341(5) . ? N1 C4 1.345(5) . ? C6 C7 1.385(6) . ? C6 C8 1.387(6) . ? C6 C5 1.501(5) . ? C4 N2 1.326(5) . ? C8 C7 1.393(5) 3_766 ? C8 H8 0.9300 . ? C7 C8 1.393(5) 3_766 ? C7 H7 0.9300 . ? C1 H1 0.9300 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? 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 C3 C2 122.7(4) . . ? N2 C3 H3 118.6 . . ? C2 C3 H3 118.6 . . ? C3 C2 C1 116.8(4) . . ? C3 C2 H2 121.6 . . ? C1 C2 H2 121.6 . . ? Cu1 I1 Cu1 112.99(2) . 1_455 ? Cu1 I1 Cu1 87.49(2) . 3_676 ? Cu1 I1 Cu1 70.74(2) 1_455 3_676 ? N1 Cu1 I1 138.75(9) . . ? N1 Cu1 I1 101.52(9) . 1_655 ? I1 Cu1 I1 112.99(2) . 1_655 ? N1 Cu1 I1 96.92(10) . 3_676 ? I1 Cu1 I1 92.51(2) . 3_676 ? I1 Cu1 I1 109.26(2) 1_655 3_676 ? C4 S1 C5 102.32(19) . . ? C1 N1 C4 115.8(3) . . ? C1 N1 Cu1 116.7(3) . . ? C4 N1 Cu1 127.5(3) . . ? C7 C6 C8 118.6(4) . . ? C7 C6 C5 120.1(4) . . ? C8 C6 C5 121.2(4) . . ? N2 C4 N1 125.9(4) . . ? N2 C4 S1 119.6(3) . . ? N1 C4 S1 114.5(3) . . ? C6 C8 C7 121.5(4) . 3_766 ? C6 C8 H8 119.3 . . ? C7 C8 H8 119.3 3_766 . ? C3 N2 C4 116.6(4) . . ? C6 C7 C8 120.0(4) . 3_766 ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 3_766 . ? N1 C1 C2 122.0(4) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C6 C5 S1 117.3(3) . . ? C6 C5 H5A 108.0 . . ? S1 C5 H5A 108.0 . . ? C6 C5 H5B 108.0 . . ? S1 C5 H5B 108.0 . . ? H5A C5 H5B 107.2 . . ? 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 N2 C3 C2 C1 -3.7(7) . . . . ? Cu1 I1 Cu1 N1 -35.64(16) 1_455 . . . ? Cu1 I1 Cu1 N1 -103.48(15) 3_676 . . . ? Cu1 I1 Cu1 I1 180.0 1_455 . . 1_655 ? Cu1 I1 Cu1 I1 112.16(3) 3_676 . . 1_655 ? Cu1 I1 Cu1 I1 67.84(3) 1_455 . . 3_676 ? Cu1 I1 Cu1 I1 0.0 3_676 . . 3_676 ? I1 Cu1 N1 C1 144.0(2) . . . . ? I1 Cu1 N1 C1 -69.2(3) 1_655 . . . ? I1 Cu1 N1 C1 42.2(3) 3_676 . . . ? I1 Cu1 N1 C4 -35.4(4) . . . . ? I1 Cu1 N1 C4 111.4(3) 1_655 . . . ? I1 Cu1 N1 C4 -137.3(3) 3_676 . . . ? C1 N1 C4 N2 -4.9(6) . . . . ? Cu1 N1 C4 N2 174.5(3) . . . . ? C1 N1 C4 S1 176.1(3) . . . . ? Cu1 N1 C4 S1 -4.4(4) . . . . ? C5 S1 C4 N2 -6.2(4) . . . . ? C5 S1 C4 N1 172.8(3) . . . . ? C7 C6 C8 C7 0.0(6) . . . 3_766 ? C5 C6 C8 C7 177.0(4) . . . 3_766 ? C2 C3 N2 C4 1.8(7) . . . . ? N1 C4 N2 C3 2.8(6) . . . . ? S1 C4 N2 C3 -178.3(3) . . . . ? C8 C6 C7 C8 0.0(6) . . . 3_766 ? C5 C6 C7 C8 -177.0(4) . . . 3_766 ? C4 N1 C1 C2 2.6(6) . . . . ? Cu1 N1 C1 C2 -176.9(3) . . . . ? C3 C2 C1 N1 1.4(7) . . . . ? C7 C6 C5 S1 -117.6(4) . . . . ? C8 C6 C5 S1 65.4(5) . . . . ? C4 S1 C5 C6 83.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 27.89 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 1.128 _refine_diff_density_min -0.861 _refine_diff_density_rms 0.143 #===END data_Complex_9 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Cu2(C16H14S2N4)(SCN)2]n' _chemical_formula_sum 'C18 H14 Cu2 N6 S4' _chemical_formula_weight 569.68 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M c2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.7761(14) _cell_length_b 17.229(2) _cell_length_c 10.4611(13) _cell_angle_alpha 90.00 _cell_angle_beta 97.777(2) _cell_angle_gamma 90.00 _cell_volume 2102.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6334 _cell_measurement_theta_min 2.11 _cell_measurement_theta_max 27.88 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.799 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 2.439 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6334 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_sigmaI/netI 0.0309 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.88 _reflns_number_total 2412 _reflns_number_gt 2012 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0477P)^2^+1.7432P] 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 2412 _refine_ls_number_parameters 137 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.0986 _refine_ls_wR_factor_gt 0.0892 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 C8 C 0.9011(3) 0.52048(17) 0.9224(3) 0.0436(7) Uani 1 1 d . . . H8 H 0.8342 0.5338 0.8690 0.052 Uiso 1 1 calc R . . Cu1 Cu 1.0000 0.14235(3) 1.2500 0.03655(16) Uani 1 2 d S . . Cu2 Cu 1.0000 -0.03291(4) 1.2500 0.0574(2) Uani 1 2 d S . . S2 S 1.15238(6) 0.06035(4) 1.17900(6) 0.03504(18) Uani 1 1 d . . . S1 S 1.08079(7) 0.27840(4) 1.08296(8) 0.0467(2) Uani 1 1 d . . . N3 N 0.9229(2) -0.06357(14) 1.0864(2) 0.0391(6) Uani 1 1 d . . . N1 N 0.91574(18) 0.17832(12) 1.0779(2) 0.0291(5) Uani 1 1 d . . . C9 C 1.1079(2) 0.06233(14) 1.0228(3) 0.0306(6) Uani 1 1 d . . . N2 N 0.9163(2) 0.25253(15) 0.8861(2) 0.0430(6) Uani 1 1 d . . . C4 C 0.9578(2) 0.23298(14) 1.0057(2) 0.0307(5) Uani 1 1 d . . . C1 C 0.8231(2) 0.14025(16) 1.0197(3) 0.0375(6) Uani 1 1 d . . . H1 H 0.7911 0.1014 1.0652 0.045 Uiso 1 1 calc R . . C7 C 0.9523(3) 0.44948(17) 0.9059(3) 0.0441(7) Uani 1 1 d . . . H7 H 0.9192 0.4156 0.8422 0.053 Uiso 1 1 calc R . . C5 C 1.1100(3) 0.35161(17) 0.9664(3) 0.0455(7) Uani 1 1 d . . . H5A H 1.1921 0.3597 0.9737 0.055 Uiso 1 1 calc R . . H5B H 1.0843 0.3324 0.8802 0.055 Uiso 1 1 calc R . . C6 C 1.0527(2) 0.42838(16) 0.9835(3) 0.0369(6) Uani 1 1 d . . . C2 C 0.7744(3) 0.15620(18) 0.8969(3) 0.0473(8) Uani 1 1 d . . . H2 H 0.7102 0.1295 0.8580 0.057 Uiso 1 1 calc R . . C3 C 0.8249(3) 0.2137(2) 0.8337(3) 0.0534(8) Uani 1 1 d . . . H3 H 0.7933 0.2260 0.7498 0.064 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 C8 0.0374(16) 0.0438(16) 0.0468(17) 0.0067(13) -0.0042(13) -0.0036(13) Cu1 0.0440(3) 0.0408(3) 0.0229(2) 0.000 -0.0026(2) 0.000 Cu2 0.0777(5) 0.0689(4) 0.0224(3) 0.000 -0.0053(3) 0.000 S2 0.0358(4) 0.0458(4) 0.0230(3) -0.0011(3) 0.0021(3) 0.0018(3) S1 0.0430(4) 0.0408(4) 0.0510(5) 0.0121(3) -0.0131(3) -0.0123(3) N3 0.0465(15) 0.0446(14) 0.0263(12) -0.0039(9) 0.0060(10) -0.0035(11) N1 0.0313(12) 0.0294(11) 0.0259(11) 0.0016(8) 0.0019(9) -0.0005(9) C9 0.0314(14) 0.0331(13) 0.0283(14) -0.0031(10) 0.0073(11) -0.0013(10) N2 0.0419(14) 0.0495(14) 0.0350(13) 0.0110(10) -0.0045(11) -0.0077(11) C4 0.0316(14) 0.0293(12) 0.0304(13) 0.0005(10) 0.0009(11) 0.0006(10) C1 0.0329(15) 0.0386(14) 0.0393(15) 0.0043(11) -0.0007(12) -0.0059(12) C7 0.0473(18) 0.0421(16) 0.0412(17) -0.0009(12) -0.0006(14) -0.0080(13) C5 0.0406(17) 0.0396(16) 0.059(2) 0.0080(13) 0.0156(15) -0.0072(13) C6 0.0367(16) 0.0335(13) 0.0420(16) 0.0067(11) 0.0114(13) -0.0075(11) C2 0.0409(17) 0.0545(18) 0.0420(17) 0.0007(13) -0.0108(14) -0.0103(14) C3 0.060(2) 0.064(2) 0.0317(16) 0.0115(14) -0.0133(15) -0.0072(17) _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 C8 C6 1.377(4) 5_767 ? C8 C7 1.385(4) . ? C8 H8 0.9300 . ? Cu1 N1 2.031(2) 2_757 ? Cu1 N1 2.031(2) . ? Cu1 S2 2.4756(8) 2_757 ? Cu1 S2 2.4756(8) . ? Cu1 Cu2 3.0195(9) . ? Cu2 N3 1.900(2) . ? Cu2 N3 1.900(2) 2_757 ? Cu2 S2 2.5911(8) . ? Cu2 S2 2.5911(8) 2_757 ? S2 C9 1.648(3) . ? S1 C4 1.745(3) . ? S1 C5 1.819(3) . ? N3 C9 1.151(4) 5_757 ? N1 C4 1.343(3) . ? N1 C1 1.346(3) . ? C9 N3 1.151(4) 5_757 ? N2 C3 1.323(4) . ? N2 C4 1.324(3) . ? C1 C2 1.363(4) . ? C1 H1 0.9300 . ? C7 C6 1.389(4) . ? C7 H7 0.9300 . ? C5 C6 1.506(4) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C8 1.377(4) 5_767 ? C2 C3 1.370(4) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? 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 C6 C8 C7 121.1(3) 5_767 . ? C6 C8 H8 119.4 5_767 . ? C7 C8 H8 119.4 . . ? N1 Cu1 N1 144.47(12) 2_757 . ? N1 Cu1 S2 101.26(6) 2_757 2_757 ? N1 Cu1 S2 98.80(6) . 2_757 ? N1 Cu1 S2 98.80(6) 2_757 . ? N1 Cu1 S2 101.26(6) . . ? S2 Cu1 S2 110.40(4) 2_757 . ? N1 Cu1 Cu2 107.77(6) 2_757 . ? N1 Cu1 Cu2 107.77(6) . . ? S2 Cu1 Cu2 55.200(19) 2_757 . ? S2 Cu1 Cu2 55.200(19) . . ? N3 Cu2 N3 147.71(15) . 2_757 ? N3 Cu2 S2 100.33(8) . . ? N3 Cu2 S2 99.53(8) 2_757 . ? N3 Cu2 S2 99.53(8) . 2_757 ? N3 Cu2 S2 100.33(8) 2_757 2_757 ? S2 Cu2 S2 103.36(4) . 2_757 ? N3 Cu2 Cu1 106.15(7) . . ? N3 Cu2 Cu1 106.15(7) 2_757 . ? S2 Cu2 Cu1 51.679(19) . . ? S2 Cu2 Cu1 51.679(19) 2_757 . ? C9 S2 Cu1 98.03(9) . . ? C9 S2 Cu2 99.07(9) . . ? Cu1 S2 Cu2 73.12(3) . . ? C4 S1 C5 102.75(14) . . ? C9 N3 Cu2 159.5(2) 5_757 . ? C4 N1 C1 115.1(2) . . ? C4 N1 Cu1 122.64(17) . . ? C1 N1 Cu1 121.42(18) . . ? N3 C9 S2 179.8(3) 5_757 . ? C3 N2 C4 116.0(2) . . ? N2 C4 N1 126.4(2) . . ? N2 C4 S1 120.0(2) . . ? N1 C4 S1 113.58(19) . . ? N1 C1 C2 122.8(3) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C8 C7 C6 120.6(3) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C6 C5 S1 113.6(2) . . ? C6 C5 H5A 108.8 . . ? S1 C5 H5A 108.8 . . ? C6 C5 H5B 108.8 . . ? S1 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? C8 C6 C7 118.3(3) 5_767 . ? C8 C6 C5 120.4(3) 5_767 . ? C7 C6 C5 121.3(3) . . ? C1 C2 C3 116.5(3) . . ? C1 C2 H2 121.8 . . ? C3 C2 H2 121.8 . . ? N2 C3 C2 123.2(3) . . ? N2 C3 H3 118.4 . . ? C2 C3 H3 118.4 . . ? 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 N1 Cu1 Cu2 N3 -178.97(10) 2_757 . . . ? N1 Cu1 Cu2 N3 1.03(10) . . . . ? S2 Cu1 Cu2 N3 89.48(8) 2_757 . . . ? S2 Cu1 Cu2 N3 -90.52(8) . . . . ? N1 Cu1 Cu2 N3 1.03(10) 2_757 . . 2_757 ? N1 Cu1 Cu2 N3 -178.97(10) . . . 2_757 ? S2 Cu1 Cu2 N3 -90.52(8) 2_757 . . 2_757 ? S2 Cu1 Cu2 N3 89.48(8) . . . 2_757 ? N1 Cu1 Cu2 S2 -88.45(7) 2_757 . . . ? N1 Cu1 Cu2 S2 91.55(7) . . . . ? S2 Cu1 Cu2 S2 180.0 2_757 . . . ? N1 Cu1 Cu2 S2 91.55(7) 2_757 . . 2_757 ? N1 Cu1 Cu2 S2 -88.45(7) . . . 2_757 ? S2 Cu1 Cu2 S2 180.0 . . . 2_757 ? N1 Cu1 S2 C9 -157.33(11) 2_757 . . . ? N1 Cu1 S2 C9 -6.82(11) . . . . ? S2 Cu1 S2 C9 97.10(9) 2_757 . . . ? Cu2 Cu1 S2 C9 97.10(9) . . . . ? N1 Cu1 S2 Cu2 105.57(6) 2_757 . . . ? N1 Cu1 S2 Cu2 -103.92(6) . . . . ? S2 Cu1 S2 Cu2 0.0 2_757 . . . ? N3 Cu2 S2 C9 6.79(12) . . . . ? N3 Cu2 S2 C9 161.19(12) 2_757 . . . ? S2 Cu2 S2 C9 -95.70(9) 2_757 . . . ? Cu1 Cu2 S2 C9 -95.70(9) . . . . ? N3 Cu2 S2 Cu1 102.49(8) . . . . ? N3 Cu2 S2 Cu1 -103.10(8) 2_757 . . . ? S2 Cu2 S2 Cu1 0.0 2_757 . . . ? N3 Cu2 N3 C9 -146.0(7) 2_757 . . 5_757 ? S2 Cu2 N3 C9 -18.8(7) . . . 5_757 ? S2 Cu2 N3 C9 86.7(7) 2_757 . . 5_757 ? Cu1 Cu2 N3 C9 34.0(7) . . . 5_757 ? N1 Cu1 N1 C4 48.00(19) 2_757 . . . ? S2 Cu1 N1 C4 171.83(19) 2_757 . . . ? S2 Cu1 N1 C4 -75.2(2) . . . . ? Cu2 Cu1 N1 C4 -132.00(19) . . . . ? N1 Cu1 N1 C1 -142.7(2) 2_757 . . . ? S2 Cu1 N1 C1 -18.9(2) 2_757 . . . ? S2 Cu1 N1 C1 94.1(2) . . . . ? Cu2 Cu1 N1 C1 37.3(2) . . . . ? Cu1 S2 C9 N3 -178(100) . . . 5_757 ? Cu2 S2 C9 N3 -104(100) . . . 5_757 ? C3 N2 C4 N1 -0.3(5) . . . . ? C3 N2 C4 S1 178.1(2) . . . . ? C1 N1 C4 N2 0.7(4) . . . . ? Cu1 N1 C4 N2 170.6(2) . . . . ? C1 N1 C4 S1 -177.81(19) . . . . ? Cu1 N1 C4 S1 -7.9(3) . . . . ? C5 S1 C4 N2 4.8(3) . . . . ? C5 S1 C4 N1 -176.6(2) . . . . ? C4 N1 C1 C2 -0.6(4) . . . . ? Cu1 N1 C1 C2 -170.7(2) . . . . ? C6 C8 C7 C6 -0.6(5) 5_767 . . . ? C4 S1 C5 C6 90.2(2) . . . . ? C8 C7 C6 C8 0.6(5) . . . 5_767 ? C8 C7 C6 C5 -179.6(3) . . . . ? S1 C5 C6 C8 79.3(3) . . . 5_767 ? S1 C5 C6 C7 -100.5(3) . . . . ? N1 C1 C2 C3 0.2(5) . . . . ? C4 N2 C3 C2 -0.2(5) . . . . ? C1 C2 C3 N2 0.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.606 _refine_diff_density_min -0.326 _refine_diff_density_rms 0.080 #===END data_Complex_10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '{[Cu6(C16H14N4S2)3I5]BF4H2O}n' _chemical_formula_sum 'C48 H44 B Cu6 F4 I5 N12 O S6' _chemical_formula_weight 2099.86 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' 'B' 'B' 0.0013 0.0007 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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 Hexagonal _symmetry_space_group_name_H-M P63 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x-y, z' 'y, -x+y, z+1/2' '-x+y, -x, z' 'x-y, x, z+1/2' _cell_length_a 13.5662(7) _cell_length_b 13.5662(7) _cell_length_c 20.1867(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3217.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 17484 _cell_measurement_theta_min 1.71 _cell_measurement_theta_max 25.00 _exptl_crystal_description rhombic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.167 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 4.599 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.4311 _exptl_absorpt_correction_T_max 0.5863 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.70173 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17484 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0328 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3830 _reflns_number_gt 3581 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0607P)^2^+1.1277P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(3) _refine_ls_number_reflns 3830 _refine_ls_number_parameters 250 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.1001 _refine_ls_wR_factor_gt 0.0915 _refine_ls_goodness_of_fit_ref 1.143 _refine_ls_restrained_S_all 1.149 _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 0.0000 0.0000 0.50004(4) 0.03547(19) Uani 1 3 d S . . I2 I 0.31191(4) 0.33999(4) 0.52284(4) 0.05144(17) Uani 1 1 d . . . I3 I 0.3333 0.6667 0.53549(4) 0.0390(2) Uani 1 3 d S . . Cu1 Cu 0.17328(8) 0.14147(8) 0.57830(5) 0.0417(2) Uani 1 1 d . . . Cu2 Cu 0.27525(8) 0.48959(8) 0.45981(5) 0.0463(3) Uani 1 1 d . . . S1 S 0.40267(16) 0.55564(16) 0.36946(10) 0.0395(4) Uani 1 1 d . . . S2 S -0.09282(15) 0.08514(16) 0.16662(9) 0.0382(4) Uani 1 1 d . . . N1 N 0.5906(5) 0.7004(6) 0.4310(3) 0.0401(15) Uani 1 1 d . . . N2 N 0.5936(6) 0.5453(6) 0.3761(4) 0.0559(19) Uani 1 1 d . . . N3 N -0.2864(6) 0.0855(6) 0.1471(4) 0.0499(18) Uani 1 1 d . . . N4 N -0.2700(5) -0.0689(5) 0.1015(3) 0.0352(13) Uani 1 1 d . . . C1 C 0.7022(7) 0.7429(7) 0.4456(4) 0.0469(19) Uani 1 1 d . . . H1 H 0.7402 0.8118 0.4682 0.056 Uiso 1 1 calc R . . C2 C 0.7615(7) 0.6897(9) 0.4288(5) 0.058(3) Uani 1 1 d . . . H2 H 0.8380 0.7207 0.4396 0.070 Uiso 1 1 calc R . . C3 C 0.7012(8) 0.5850(9) 0.3942(5) 0.060(2) Uani 1 1 d . . . H3 H 0.7372 0.5438 0.3841 0.072 Uiso 1 1 calc R . . C4 C 0.5430(7) 0.6043(6) 0.3952(4) 0.0397(17) Uani 1 1 d . . . C5 C 0.3790(8) 0.4304(9) 0.3228(6) 0.071(3) Uani 1 1 d . . . H5B H 0.4326 0.4526 0.2863 0.085 Uiso 1 1 calc R . . H5A H 0.3891 0.3785 0.3512 0.085 Uiso 1 1 calc R . . C6 C 0.2556(8) 0.3723(8) 0.2961(5) 0.058(2) Uani 1 1 d . . . C7 C 0.1788(8) 0.2677(8) 0.3177(5) 0.056(2) Uani 1 1 d . . . H7 H 0.2001 0.2329 0.3499 0.067 Uiso 1 1 calc R . . C8 C 0.0696(9) 0.2111(8) 0.2932(5) 0.062(3) Uani 1 1 d . . . H8 H 0.0187 0.1382 0.3084 0.074 Uiso 1 1 calc R . . C9 C 0.0353(7) 0.2606(7) 0.2469(4) 0.050(2) Uani 1 1 d . . . C10 C 0.1152(8) 0.3703(8) 0.2244(5) 0.058(2) Uani 1 1 d . . . H10 H 0.0938 0.4057 0.1925 0.070 Uiso 1 1 calc R . . C11 C 0.2240(8) 0.4256(8) 0.2488(5) 0.062(2) Uani 1 1 d . . . H11 H 0.2762 0.4982 0.2339 0.075 Uiso 1 1 calc R . . C12 C -0.0819(7) 0.2004(8) 0.2176(5) 0.055(2) Uani 1 1 d . . . H12B H -0.0942 0.2527 0.1909 0.066 Uiso 1 1 calc R . . H12A H -0.1386 0.1705 0.2525 0.066 Uiso 1 1 calc R . . C13 C -0.2305(6) 0.0287(6) 0.1353(4) 0.0346(16) Uani 1 1 d . . . C14 C -0.3926(8) 0.0361(8) 0.1229(5) 0.059(2) Uani 1 1 d . . . H14 H -0.4345 0.0726 0.1292 0.071 Uiso 1 1 calc R . . C15 C -0.4431(7) -0.0662(8) 0.0889(6) 0.056(2) Uani 1 1 d . . . H15 H -0.5175 -0.0992 0.0733 0.067 Uiso 1 1 calc R . . C16 C -0.3780(6) -0.1166(7) 0.0792(5) 0.0475(19) Uani 1 1 d . . . H16 H -0.4093 -0.1855 0.0566 0.057 Uiso 1 1 calc R . . F1 F 0.6667 0.3333 0.5785(13) 0.175(7) Uani 1 3 d SU . . F2 F 0.6689(9) 0.2417(8) 0.4931(7) 0.159(4) Uani 1 1 d U . . B1 B 0.6667 0.3333 0.5099(16) 0.091(7) Uani 1 3 d SU . . O1 O 0.6667 0.3333 0.252(2) 0.273(11) Uani 1 3 d SU . . 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 0.0313(2) 0.0313(2) 0.0439(4) 0.000 0.000 0.01563(12) I2 0.0408(3) 0.0322(2) 0.0770(4) 0.0133(2) -0.0068(3) 0.0150(2) I3 0.0358(3) 0.0358(3) 0.0454(5) 0.000 0.000 0.01792(13) Cu1 0.0361(5) 0.0366(5) 0.0548(6) 0.0009(4) -0.0015(4) 0.0199(4) Cu2 0.0418(5) 0.0360(5) 0.0591(7) 0.0007(4) -0.0041(5) 0.0180(4) S1 0.0312(9) 0.0402(10) 0.0430(11) -0.0081(8) -0.0040(8) 0.0150(8) S2 0.0319(9) 0.0387(10) 0.0424(11) -0.0070(8) -0.0019(7) 0.0164(8) N1 0.033(3) 0.042(4) 0.041(4) -0.003(3) -0.002(3) 0.016(3) N2 0.050(4) 0.057(5) 0.066(5) -0.020(4) -0.010(4) 0.031(4) N3 0.040(4) 0.048(4) 0.065(5) -0.016(3) -0.008(3) 0.024(3) N4 0.030(3) 0.032(3) 0.045(4) 0.002(3) 0.003(2) 0.016(3) C1 0.039(4) 0.045(4) 0.054(5) -0.010(4) -0.004(4) 0.020(4) C2 0.029(4) 0.084(7) 0.064(6) 0.006(5) -0.001(4) 0.030(4) C3 0.055(6) 0.076(7) 0.068(6) -0.011(5) -0.010(5) 0.048(5) C4 0.038(4) 0.038(4) 0.038(4) -0.002(3) -0.001(3) 0.015(3) C5 0.056(6) 0.066(6) 0.080(8) -0.037(6) -0.004(5) 0.023(5) C6 0.052(5) 0.063(6) 0.057(6) -0.032(5) -0.007(4) 0.026(5) C7 0.053(5) 0.058(5) 0.055(5) -0.023(4) -0.009(4) 0.027(4) C8 0.059(6) 0.051(5) 0.064(7) -0.020(5) -0.003(5) 0.018(5) C9 0.043(4) 0.055(5) 0.048(5) -0.026(4) -0.009(4) 0.022(4) C10 0.052(5) 0.054(5) 0.064(6) -0.020(4) -0.012(4) 0.024(4) C11 0.051(5) 0.056(5) 0.062(6) -0.028(5) -0.007(4) 0.014(4) C12 0.047(5) 0.059(6) 0.059(5) -0.023(4) -0.003(4) 0.026(4) C13 0.035(4) 0.030(4) 0.042(4) -0.001(3) 0.000(3) 0.018(3) C14 0.046(5) 0.068(6) 0.079(7) 0.000(5) -0.003(4) 0.040(5) C15 0.027(4) 0.056(5) 0.085(7) -0.001(5) -0.006(4) 0.021(4) C16 0.035(4) 0.050(5) 0.060(5) -0.005(4) -0.004(4) 0.023(4) F1 0.171(7) 0.171(7) 0.183(11) 0.000 0.000 0.086(3) F2 0.172(7) 0.117(6) 0.216(8) 0.003(6) 0.010(6) 0.092(5) B1 0.081(7) 0.081(7) 0.111(11) 0.000 0.000 0.041(3) O1 0.277(10) 0.277(10) 0.264(15) 0.000 0.000 0.139(5) _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 2.6821(11) . ? I1 Cu1 2.6820(11) 5 ? I1 Cu1 2.6821(11) 3 ? I2 Cu1 2.6417(11) . ? I2 Cu2 2.6446(11) . ? I3 Cu2 2.6140(11) 5_565 ? I3 Cu2 2.6140(11) 3_665 ? I3 Cu2 2.6140(11) . ? Cu1 N4 2.049(6) 2 ? Cu1 S2 2.334(2) 4 ? Cu2 N1 2.030(7) 5_565 ? Cu2 S1 2.360(2) . ? S1 C4 1.752(8) . ? S1 C5 1.826(9) . ? S2 C13 1.745(8) . ? S2 C12 1.815(9) . ? S2 Cu1 2.334(2) 6_554 ? N1 C4 1.340(10) . ? N1 C1 1.355(9) . ? N1 Cu2 2.030(7) 3_665 ? N2 C3 1.330(11) . ? N2 C4 1.345(10) . ? N3 C14 1.341(11) . ? N3 C13 1.345(9) . ? N4 C13 1.341(9) . ? N4 C16 1.349(9) . ? N4 Cu1 2.049(6) 2_554 ? C1 C2 1.365(12) . ? C1 H1 0.9300 . ? C2 C3 1.419(14) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C5 C6 1.546(13) . ? C5 H5B 0.9700 . ? C5 H5A 0.9700 . ? C6 C7 1.345(13) . ? C6 C11 1.388(14) . ? C7 C8 1.376(13) . ? C7 H7 0.9300 . ? C8 C9 1.360(14) . ? C8 H8 0.9300 . ? C9 C10 1.409(13) . ? C9 C12 1.499(11) . ? C10 C11 1.371(13) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 H12B 0.9700 . ? C12 H12A 0.9700 . ? C14 C15 1.384(13) . ? C14 H14 0.9300 . ? C15 C16 1.375(11) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? F1 B1 1.38(4) . ? F2 B1 1.303(12) . ? B1 F2 1.303(12) 3_655 ? B1 F2 1.303(12) 5_665 ? 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 88.83(4) . 5 ? Cu1 I1 Cu1 88.83(4) . 3 ? Cu1 I1 Cu1 88.83(4) 5 3 ? Cu1 I2 Cu2 132.46(3) . . ? Cu2 I3 Cu2 89.29(4) 5_565 3_665 ? Cu2 I3 Cu2 89.29(4) 5_565 . ? Cu2 I3 Cu2 89.29(4) 3_665 . ? N4 Cu1 S2 116.53(18) 2 4 ? N4 Cu1 I2 106.61(17) 2 . ? S2 Cu1 I2 106.65(6) 4 . ? N4 Cu1 I1 109.46(16) 2 . ? S2 Cu1 I1 104.07(6) 4 . ? I2 Cu1 I1 113.73(4) . . ? N1 Cu2 S1 112.68(19) 5_565 . ? N1 Cu2 I3 113.87(18) 5_565 . ? S1 Cu2 I3 106.01(6) . . ? N1 Cu2 I2 107.97(18) 5_565 . ? S1 Cu2 I2 106.27(6) . . ? I3 Cu2 I2 109.76(4) . . ? C4 S1 C5 99.0(4) . . ? C4 S1 Cu2 111.5(3) . . ? C5 S1 Cu2 106.9(4) . . ? C13 S2 C12 101.1(4) . . ? C13 S2 Cu1 106.9(3) . 6_554 ? C12 S2 Cu1 105.4(3) . 6_554 ? C4 N1 C1 115.2(7) . . ? C4 N1 Cu2 125.0(5) . 3_665 ? C1 N1 Cu2 119.8(5) . 3_665 ? C3 N2 C4 117.7(7) . . ? C14 N3 C13 114.9(7) . . ? C13 N4 C16 116.4(6) . . ? C13 N4 Cu1 123.7(5) . 2_554 ? C16 N4 Cu1 119.8(5) . 2_554 ? N1 C1 C2 123.3(8) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C1 C2 C3 117.0(7) . . ? C1 C2 H2 121.5 . . ? C3 C2 H2 121.5 . . ? N2 C3 C2 120.5(8) . . ? N2 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? N1 C4 N2 126.2(7) . . ? N1 C4 S1 115.6(6) . . ? N2 C4 S1 118.2(6) . . ? C6 C5 S1 107.2(6) . . ? C6 C5 H5B 110.3 . . ? S1 C5 H5B 110.3 . . ? C6 C5 H5A 110.3 . . ? S1 C5 H5A 110.3 . . ? H5B C5 H5A 108.5 . . ? C7 C6 C11 119.6(9) . . ? C7 C6 C5 119.7(10) . . ? C11 C6 C5 120.8(9) . . ? C6 C7 C8 121.5(10) . . ? C6 C7 H7 119.2 . . ? C8 C7 H7 119.2 . . ? C9 C8 C7 120.6(9) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C10 118.2(8) . . ? C8 C9 C12 122.2(9) . . ? C10 C9 C12 119.5(9) . . ? C11 C10 C9 120.7(10) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C10 C11 C6 119.5(10) . . ? C10 C11 H11 120.3 . . ? C6 C11 H11 120.3 . . ? C9 C12 S2 107.5(6) . . ? C9 C12 H12B 110.2 . . ? S2 C12 H12B 110.2 . . ? C9 C12 H12A 110.2 . . ? S2 C12 H12A 110.2 . . ? H12B C12 H12A 108.5 . . ? N4 C13 N3 126.5(6) . . ? N4 C13 S2 115.4(5) . . ? N3 C13 S2 118.1(5) . . ? N3 C14 C15 123.5(7) . . ? N3 C14 H14 118.3 . . ? C15 C14 H14 118.3 . . ? C16 C15 C14 116.7(7) . . ? C16 C15 H15 121.6 . . ? C14 C15 H15 121.6 . . ? N4 C16 C15 121.9(7) . . ? N4 C16 H16 119.1 . . ? C15 C16 H16 119.1 . . ? F2 B1 F2 113.4(13) . 3_655 ? F2 B1 F2 113.4(13) . 5_665 ? F2 B1 F2 113.4(13) 3_655 5_665 ? F2 B1 F1 105.1(15) . . ? F2 B1 F1 105.1(15) 3_655 . ? F2 B1 F1 105.1(15) 5_665 . ? 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 Cu2 I2 Cu1 N4 170.11(18) . . . 2 ? Cu2 I2 Cu1 S2 -64.74(8) . . . 4 ? Cu2 I2 Cu1 I1 49.38(7) . . . . ? Cu1 I1 Cu1 N4 43.18(19) 5 . . 2 ? Cu1 I1 Cu1 N4 132.03(18) 3 . . 2 ? Cu1 I1 Cu1 S2 -82.06(5) 5 . . 4 ? Cu1 I1 Cu1 S2 6.80(6) 3 . . 4 ? Cu1 I1 Cu1 I2 162.29(4) 5 . . . ? Cu1 I1 Cu1 I2 -108.85(5) 3 . . . ? Cu2 I3 Cu2 N1 -41.5(2) 5_565 . . 5_565 ? Cu2 I3 Cu2 N1 -130.8(2) 3_665 . . 5_565 ? Cu2 I3 Cu2 S1 82.99(5) 5_565 . . . ? Cu2 I3 Cu2 S1 -6.31(6) 3_665 . . . ? Cu2 I3 Cu2 I2 -162.63(4) 5_565 . . . ? Cu2 I3 Cu2 I2 108.07(5) 3_665 . . . ? Cu1 I2 Cu2 N1 -18.4(2) . . . 5_565 ? Cu1 I2 Cu2 S1 -139.49(7) . . . . ? Cu1 I2 Cu2 I3 106.29(6) . . . . ? N1 Cu2 S1 C4 -170.8(3) 5_565 . . . ? I3 Cu2 S1 C4 64.0(3) . . . . ? I2 Cu2 S1 C4 -52.7(3) . . . . ? N1 Cu2 S1 C5 -63.6(4) 5_565 . . . ? I3 Cu2 S1 C5 171.2(4) . . . . ? I2 Cu2 S1 C5 54.4(4) . . . . ? C4 N1 C1 C2 -3.6(13) . . . . ? Cu2 N1 C1 C2 178.9(7) 3_665 . . . ? N1 C1 C2 C3 0.2(14) . . . . ? C4 N2 C3 C2 -3.8(14) . . . . ? C1 C2 C3 N2 3.7(14) . . . . ? C1 N1 C4 N2 3.6(12) . . . . ? Cu2 N1 C4 N2 -179.1(6) 3_665 . . . ? C1 N1 C4 S1 -174.4(6) . . . . ? Cu2 N1 C4 S1 2.9(9) 3_665 . . . ? C3 N2 C4 N1 0.1(14) . . . . ? C3 N2 C4 S1 178.0(7) . . . . ? C5 S1 C4 N1 178.6(7) . . . . ? Cu2 S1 C4 N1 -69.1(6) . . . . ? C5 S1 C4 N2 0.5(8) . . . . ? Cu2 S1 C4 N2 112.8(6) . . . . ? C4 S1 C5 C6 179.1(7) . . . . ? Cu2 S1 C5 C6 63.3(8) . . . . ? S1 C5 C6 C7 -115.0(9) . . . . ? S1 C5 C6 C11 66.7(11) . . . . ? C11 C6 C7 C8 1.1(13) . . . . ? C5 C6 C7 C8 -177.2(8) . . . . ? C6 C7 C8 C9 -1.2(13) . . . . ? C7 C8 C9 C10 0.9(13) . . . . ? C7 C8 C9 C12 178.2(8) . . . . ? C8 C9 C10 C11 -0.4(13) . . . . ? C12 C9 C10 C11 -177.8(8) . . . . ? C9 C10 C11 C6 0.3(14) . . . . ? C7 C6 C11 C10 -0.6(14) . . . . ? C5 C6 C11 C10 177.7(8) . . . . ? C8 C9 C12 S2 -68.5(10) . . . . ? C10 C9 C12 S2 108.8(8) . . . . ? C13 S2 C12 C9 -178.3(7) . . . . ? Cu1 S2 C12 C9 -67.2(7) 6_554 . . . ? C16 N4 C13 N3 -2.4(11) . . . . ? Cu1 N4 C13 N3 174.0(6) 2_554 . . . ? C16 N4 C13 S2 177.3(6) . . . . ? Cu1 N4 C13 S2 -6.3(8) 2_554 . . . ? C14 N3 C13 N4 1.0(12) . . . . ? C14 N3 C13 S2 -178.6(7) . . . . ? C12 S2 C13 N4 -171.9(6) . . . . ? Cu1 S2 C13 N4 78.1(6) 6_554 . . . ? C12 S2 C13 N3 7.8(7) . . . . ? Cu1 S2 C13 N3 -102.2(6) 6_554 . . . ? C13 N3 C14 C15 0.9(14) . . . . ? N3 C14 C15 C16 -1.3(16) . . . . ? C13 N4 C16 C15 1.8(12) . . . . ? Cu1 N4 C16 C15 -174.7(7) 2_554 . . . ? C14 C15 C16 N4 -0.1(15) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.283 _refine_diff_density_min -0.805 _refine_diff_density_rms 0.206 #===END