# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Sheng Hu' 'Ze-Min Zhang' 'Zhao-Sha Meng' 'Zhua-Jia Lin' ; Ming-Liang Tong ; _publ_contact_author_name 'Ming-Liang Tong' _publ_contact_author_email tongml@mail.sysu.edu.cn data_complex1 _database_code_depnum_ccdc_archive 'CCDC 768410' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H18 Cu2 N6' _chemical_formula_weight 565.56 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' _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 23.631(3) _cell_length_b 4.8043(7) _cell_length_c 23.560(3) _cell_angle_alpha 90.00 _cell_angle_beta 116.741(2) _cell_angle_gamma 90.00 _cell_volume 2388.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.573 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 1.810 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7717 _exptl_absorpt_correction_T_max 0.8687 _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 3709 _diffrn_reflns_av_R_equivalents 0.0237 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.99 _reflns_number_total 2224 _reflns_number_gt 1953 _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^)+(0.0759P)^2^+1.3339P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2224 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1358 _refine_ls_wR_factor_gt 0.1312 _refine_ls_goodness_of_fit_ref 1.159 _refine_ls_restrained_S_all 1.159 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.11368(2) 0.45725(10) 0.13167(2) 0.0292(2) Uani 1 1 d . . . N1 N 0.15056(16) 0.5278(7) 0.23389(16) 0.0310(8) Uani 1 1 d . . . N2 N 0.51401(16) 0.9952(7) 0.60763(18) 0.0336(8) Uani 1 1 d . . . N3 N 0.12723(16) 0.8480(8) 0.11231(15) 0.0332(8) Uani 1 1 d . . . C1 C 0.1323(2) 0.3777(9) 0.2702(2) 0.0356(10) Uani 1 1 d . . . H1 H 0.1038 0.2334 0.2511 0.043 Uiso 1 1 calc R . . C2 C 0.1531(2) 0.4223(9) 0.3346(2) 0.0359(10) Uani 1 1 d . . . H2 H 0.1383 0.3111 0.3574 0.043 Uiso 1 1 calc R . . C3 C 0.19614(16) 0.6340(9) 0.36484(18) 0.0276(9) Uani 1 1 d . . . C4 C 0.21628(17) 0.7867(9) 0.32755(18) 0.0300(9) Uani 1 1 d . . . H4 H 0.2458 0.9283 0.3457 0.036 Uiso 1 1 calc R . . C5 C 0.19248(18) 0.7292(9) 0.26319(18) 0.0326(9) Uani 1 1 d . . . H5 H 0.2065 0.8368 0.2392 0.039 Uiso 1 1 calc R . . C6 C 0.22132(17) 0.6950(9) 0.43383(17) 0.0288(9) Uani 1 1 d . . . C7 C 0.28497(17) 0.7661(9) 0.46712(18) 0.0318(9) Uani 1 1 d . . . H7 H 0.3089 0.7774 0.4449 0.038 Uiso 1 1 calc R . . C8 C 0.31489(17) 0.8215(9) 0.53241(18) 0.0292(9) Uani 1 1 d . . . C9 C 0.38401(17) 0.8842(9) 0.56099(18) 0.0273(9) Uani 1 1 d . . . C10 C 0.40602(19) 1.0829(10) 0.5334(2) 0.0351(10) Uani 1 1 d . . . H10 H 0.3776 1.1830 0.4983 0.042 Uiso 1 1 calc R . . C11 C 0.47025(19) 1.1324(10) 0.5579(2) 0.0350(10) Uani 1 1 d . . . H11 H 0.4838 1.2686 0.5387 0.042 Uiso 1 1 calc R . . C12 C 0.49227(19) 0.8045(10) 0.6342(2) 0.0397(11) Uani 1 1 d . . . H12 H 0.5216 0.7070 0.6692 0.048 Uiso 1 1 calc R . . C13 C 0.42914(18) 0.7439(10) 0.6130(2) 0.0364(10) Uani 1 1 d . . . H13 H 0.4168 0.6091 0.6335 0.044 Uiso 1 1 calc R . . C14 C 0.12498(18) 1.0771(8) 0.11517(18) 0.0241(8) 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 Cu1 0.0301(3) 0.0242(3) 0.0316(3) -0.0029(2) 0.0124(3) 0.00113(19) N1 0.0323(18) 0.038(2) 0.0180(18) -0.0037(14) 0.0068(16) 0.0009(15) N2 0.0219(17) 0.037(2) 0.035(2) 0.0048(16) 0.0072(16) -0.0019(14) N3 0.040(2) 0.036(2) 0.0242(18) -0.0057(15) 0.0142(16) -0.0007(16) C1 0.038(2) 0.035(2) 0.028(2) -0.0092(18) 0.010(2) -0.0096(18) C2 0.042(2) 0.040(3) 0.027(2) -0.0023(18) 0.015(2) -0.0090(19) C3 0.0162(18) 0.041(2) 0.021(2) -0.0047(17) 0.0036(17) 0.0015(16) C4 0.0226(18) 0.042(3) 0.019(2) -0.0056(17) 0.0044(17) -0.0063(17) C5 0.029(2) 0.046(3) 0.018(2) 0.0009(18) 0.0061(18) -0.0021(18) C6 0.0235(19) 0.044(3) 0.016(2) -0.0042(17) 0.0059(17) -0.0011(17) C7 0.0247(19) 0.051(3) 0.022(2) -0.0060(18) 0.0125(17) -0.0027(18) C8 0.0192(18) 0.044(2) 0.022(2) -0.0032(17) 0.0077(17) -0.0033(17) C9 0.0208(18) 0.040(2) 0.018(2) -0.0073(16) 0.0055(17) -0.0024(16) C10 0.024(2) 0.054(3) 0.021(2) 0.0055(18) 0.0049(18) 0.0008(18) C11 0.030(2) 0.044(3) 0.030(2) 0.0067(19) 0.0130(19) -0.0045(19) C12 0.027(2) 0.044(3) 0.036(3) 0.014(2) 0.003(2) -0.0009(19) C13 0.025(2) 0.044(3) 0.035(2) 0.006(2) 0.0092(19) -0.0056(18) C14 0.028(2) 0.022(2) 0.021(2) -0.0005(15) 0.0096(17) -0.0045(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 C14 1.911(4) 1_545 ? Cu1 N3 1.991(4) . ? Cu1 N2 2.172(3) 8_465 ? Cu1 N1 2.187(3) . ? N1 C1 1.330(5) . ? N1 C5 1.334(5) . ? N2 C12 1.336(5) . ? N2 C11 1.337(5) . ? N2 Cu1 2.172(3) 8_566 ? N3 C14 1.106(5) . ? C1 C2 1.385(6) . ? C1 H1 0.9300 . ? C2 C3 1.387(6) . ? C2 H2 0.9300 . ? C3 C4 1.383(5) . ? C3 C6 1.487(5) . ? C4 C5 1.387(5) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.390(5) . ? C6 C8 1.409(5) 7_566 ? C7 C8 1.399(5) . ? C7 H7 0.9300 . ? C8 C6 1.409(5) 7_566 ? C8 C9 1.491(5) . ? C9 C10 1.382(6) . ? C9 C13 1.384(6) . ? C10 C11 1.380(5) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C13 1.374(5) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 Cu1 1.911(4) 1_565 ? 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 C14 Cu1 N3 143.38(14) 1_545 . ? C14 Cu1 N2 106.37(14) 1_545 8_465 ? N3 Cu1 N2 96.22(14) . 8_465 ? C14 Cu1 N1 110.44(15) 1_545 . ? N3 Cu1 N1 94.62(13) . . ? N2 Cu1 N1 96.84(13) 8_465 . ? C1 N1 C5 116.1(3) . . ? C1 N1 Cu1 122.7(3) . . ? C5 N1 Cu1 121.2(3) . . ? C12 N2 C11 116.1(3) . . ? C12 N2 Cu1 123.4(3) . 8_566 ? C11 N2 Cu1 119.8(3) . 8_566 ? C14 N3 Cu1 155.2(3) . . ? N1 C1 C2 124.2(4) . . ? N1 C1 H1 117.9 . . ? C2 C1 H1 117.9 . . ? C1 C2 C3 119.5(4) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C4 C3 C2 116.4(4) . . ? C4 C3 C6 120.5(4) . . ? C2 C3 C6 123.1(4) . . ? C3 C4 C5 120.2(4) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? N1 C5 C4 123.5(4) . . ? N1 C5 H5 118.3 . . ? C4 C5 H5 118.3 . . ? C7 C6 C8 118.2(3) . 7_566 ? C7 C6 C3 117.7(3) . . ? C8 C6 C3 124.1(3) 7_566 . ? C6 C7 C8 123.4(3) . . ? C6 C7 H7 118.3 . . ? C8 C7 H7 118.3 . . ? C7 C8 C6 118.4(3) . 7_566 ? C7 C8 C9 116.4(3) . . ? C6 C8 C9 125.2(3) 7_566 . ? C10 C9 C13 116.7(3) . . ? C10 C9 C8 119.7(4) . . ? C13 C9 C8 123.5(4) . . ? C11 C10 C9 119.9(4) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? N2 C11 C10 123.6(4) . . ? N2 C11 H11 118.2 . . ? C10 C11 H11 118.2 . . ? N2 C12 C13 123.9(4) . . ? N2 C12 H12 118.0 . . ? C13 C12 H12 118.0 . . ? C12 C13 C9 119.8(4) . . ? C12 C13 H13 120.1 . . ? C9 C13 H13 120.1 . . ? N3 C14 Cu1 168.2(3) . 1_565 ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 0.966 _refine_diff_density_min -0.354 _refine_diff_density_rms 0.116 #=================================================END data_complex2 _database_code_depnum_ccdc_archive 'CCDC 768411' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H21 Cu N4 O5.50 S' _chemical_formula_weight 573.07 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' O O 0.0106 0.0060 '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 Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 18.175(3) _cell_length_b 8.7350(15) _cell_length_c 30.413(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4828.4(14) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2352 _exptl_absorpt_coefficient_mu 1.041 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9214 _exptl_absorpt_correction_T_max 0.9498 _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 13025 _diffrn_reflns_av_R_equivalents 0.0725 _diffrn_reflns_av_sigmaI/netI 0.0867 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4692 _reflns_number_gt 2903 _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^)+(0.0789P)^2^+2.4830P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4692 _refine_ls_number_parameters 348 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1122 _refine_ls_R_factor_gt 0.0640 _refine_ls_wR_factor_ref 0.1731 _refine_ls_wR_factor_gt 0.1488 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.067 _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 0.69693(3) 0.39150(8) 0.661129(19) 0.0215(2) Uani 1 1 d . . . S1 S 0.85658(8) 0.49742(18) 0.67157(5) 0.0295(4) Uani 1 1 d . . . O1 O 0.80411(19) 0.3665(4) 0.66539(12) 0.0271(9) Uani 1 1 d . . . O2 O 0.8147(2) 0.6396(5) 0.66682(15) 0.0452(12) Uani 1 1 d . . . O3 O 0.9120(2) 0.4880(6) 0.63731(18) 0.0631(15) Uani 1 1 d . . . O4 O 0.8887(3) 0.4856(6) 0.71436(17) 0.0670(16) Uani 1 1 d . . . N1 N 0.7042(2) 0.3742(5) 0.59402(14) 0.0243(11) Uani 1 1 d . . . N2 N 0.4083(2) 0.5430(6) 0.34908(14) 0.0248(11) Uani 1 1 d . . . N3 N 0.6876(2) 0.5586(5) 0.22549(14) 0.0231(10) Uani 1 1 d . . . N4 N 0.9873(3) 0.3123(8) 0.4743(2) 0.0597(18) Uani 1 1 d . . . C1 C 0.7047(3) 0.3775(6) 0.45278(16) 0.0228(12) Uani 1 1 d . . . C2 C 0.6366(3) 0.3940(7) 0.43302(17) 0.0247(13) Uani 1 1 d . . . H2A H 0.5948 0.3799 0.4502 0.030 Uiso 1 1 calc R . . C3 C 0.6273(3) 0.4306(7) 0.38898(17) 0.0230(13) Uani 1 1 d . . . C4 C 0.6908(3) 0.4487(7) 0.36299(17) 0.0264(13) Uani 1 1 d . . . C5 C 0.7592(3) 0.4238(7) 0.38253(17) 0.0280(14) Uani 1 1 d . . . H5A H 0.8009 0.4303 0.3649 0.034 Uiso 1 1 calc R . . C6 C 0.7683(3) 0.3900(6) 0.42647(17) 0.0237(12) Uani 1 1 d . . . C7 C 0.7069(3) 0.3703(6) 0.50193(17) 0.0233(12) Uani 1 1 d . . . C8 C 0.6537(3) 0.2918(7) 0.52588(17) 0.0242(13) Uani 1 1 d . . . H8A H 0.6178 0.2354 0.5113 0.029 Uiso 1 1 calc R . . C9 C 0.6543(3) 0.2975(7) 0.57105(18) 0.0269(13) Uani 1 1 d . . . H9A H 0.6178 0.2449 0.5863 0.032 Uiso 1 1 calc R . . C10 C 0.7550(3) 0.4502(7) 0.57146(18) 0.0323(14) Uani 1 1 d . . . H10A H 0.7899 0.5059 0.5871 0.039 Uiso 1 1 calc R . . C11 C 0.7588(3) 0.4513(7) 0.52666(17) 0.0293(14) Uani 1 1 d . . . H11A H 0.7959 0.5058 0.5126 0.035 Uiso 1 1 calc R . . C12 C 0.5518(3) 0.4661(7) 0.37317(16) 0.0226(13) Uani 1 1 d . . . C13 C 0.5358(3) 0.6054(7) 0.35339(18) 0.0304(14) Uani 1 1 d . . . H13A H 0.5730 0.6758 0.3479 0.037 Uiso 1 1 calc R . . C14 C 0.4643(3) 0.6385(7) 0.34192(18) 0.0296(14) Uani 1 1 d . . . H14A H 0.4546 0.7321 0.3285 0.036 Uiso 1 1 calc R . . C15 C 0.4232(3) 0.4072(7) 0.36768(18) 0.0299(14) Uani 1 1 d . . . H15A H 0.3850 0.3379 0.3721 0.036 Uiso 1 1 calc R . . C16 C 0.4938(3) 0.3670(7) 0.38047(19) 0.0335(15) Uani 1 1 d . . . H16A H 0.5021 0.2732 0.3940 0.040 Uiso 1 1 calc R . . C17 C 0.6878(3) 0.4872(7) 0.31519(17) 0.0259(13) Uani 1 1 d . . . C18 C 0.7336(3) 0.5973(8) 0.29821(18) 0.0341(15) Uani 1 1 d . . . H18A H 0.7659 0.6495 0.3166 0.041 Uiso 1 1 calc R . . C19 C 0.7317(3) 0.6305(7) 0.25384(19) 0.0331(15) Uani 1 1 d . . . H19A H 0.7626 0.7068 0.2432 0.040 Uiso 1 1 calc R . . C20 C 0.6428(3) 0.4511(7) 0.24247(18) 0.0284(13) Uani 1 1 d . . . H20A H 0.6116 0.3992 0.2234 0.034 Uiso 1 1 calc R . . C21 C 0.6404(3) 0.4135(7) 0.28606(17) 0.0255(13) Uani 1 1 d . . . H21A H 0.6075 0.3398 0.2961 0.031 Uiso 1 1 calc R . . C22 C 0.8436(3) 0.3631(7) 0.44333(18) 0.0280(14) Uani 1 1 d . . . C23 C 0.8596(3) 0.2459(8) 0.4723(2) 0.0387(16) Uani 1 1 d . . . H23A H 0.8227 0.1805 0.4821 0.046 Uiso 1 1 calc R . . C24 C 0.9313(4) 0.2272(9) 0.4864(3) 0.057(2) Uani 1 1 d . . . H24A H 0.9406 0.1480 0.5061 0.068 Uiso 1 1 calc R . . C25 C 0.9714(4) 0.4214(10) 0.4464(3) 0.061(2) Uani 1 1 d . . . H25A H 1.0101 0.4824 0.4366 0.074 Uiso 1 1 calc R . . C26 C 0.9018(3) 0.4540(9) 0.4300(2) 0.0449(18) Uani 1 1 d . . . H26A H 0.8945 0.5349 0.4106 0.054 Uiso 1 1 calc R . . O1W O 0.5000 0.2022(10) 0.2500 0.106(3) Uani 1 2 d S . . O2W O 0.5673(5) 0.0225(14) 0.3278(3) 0.071(3) Uani 0.50 1 d PU . . O3W O 0.5666(9) -0.1937(18) 0.2684(5) 0.132(5) Uani 0.50 1 d PU . . 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 0.0206(3) 0.0308(4) 0.0131(3) -0.0002(3) -0.0006(3) 0.0030(3) S1 0.0231(7) 0.0305(8) 0.0349(8) 0.0037(7) -0.0029(6) -0.0005(7) O1 0.0235(19) 0.028(2) 0.030(2) -0.0014(18) 0.0010(17) -0.0015(17) O2 0.053(3) 0.026(2) 0.056(3) 0.003(2) 0.001(2) 0.005(2) O3 0.039(3) 0.058(3) 0.092(4) -0.005(3) 0.030(3) -0.004(3) O4 0.068(3) 0.073(4) 0.060(3) 0.006(3) -0.040(3) -0.013(3) N1 0.027(2) 0.032(3) 0.014(2) 0.000(2) -0.0031(18) -0.001(2) N2 0.019(2) 0.037(3) 0.018(2) -0.002(2) 0.0011(18) 0.004(2) N3 0.025(2) 0.029(3) 0.016(2) -0.001(2) 0.0008(18) 0.000(2) N4 0.030(3) 0.077(5) 0.072(5) 0.001(4) -0.015(3) 0.007(3) C1 0.021(3) 0.032(3) 0.015(3) 0.001(2) -0.001(2) -0.001(3) C2 0.019(3) 0.034(3) 0.021(3) 0.001(3) 0.001(2) -0.002(3) C3 0.024(3) 0.029(3) 0.016(3) 0.002(2) -0.002(2) 0.005(2) C4 0.028(3) 0.030(3) 0.021(3) 0.000(3) -0.002(2) 0.000(3) C5 0.019(3) 0.044(4) 0.021(3) 0.002(3) 0.003(2) -0.002(3) C6 0.024(3) 0.027(3) 0.020(3) -0.002(3) -0.003(2) 0.003(3) C7 0.020(3) 0.030(3) 0.020(3) -0.002(3) 0.000(2) 0.006(3) C8 0.021(3) 0.032(3) 0.019(3) -0.003(3) -0.003(2) -0.004(3) C9 0.023(3) 0.035(4) 0.022(3) 0.000(3) 0.005(2) -0.002(3) C10 0.032(3) 0.043(4) 0.022(3) 0.000(3) -0.005(3) -0.011(3) C11 0.031(3) 0.038(4) 0.019(3) 0.003(3) 0.001(2) -0.008(3) C12 0.019(3) 0.033(4) 0.016(3) -0.001(3) 0.003(2) 0.005(2) C13 0.023(3) 0.036(4) 0.032(3) 0.003(3) 0.001(2) -0.001(3) C14 0.030(3) 0.030(4) 0.029(3) 0.008(3) 0.005(2) 0.003(3) C15 0.027(3) 0.034(4) 0.029(3) -0.002(3) 0.000(2) -0.002(3) C16 0.027(3) 0.035(4) 0.038(4) 0.007(3) -0.002(3) 0.008(3) C17 0.028(3) 0.034(3) 0.016(3) -0.002(3) 0.006(2) 0.003(3) C18 0.038(3) 0.047(4) 0.018(3) -0.003(3) -0.003(2) -0.019(3) C19 0.037(3) 0.039(4) 0.023(3) 0.001(3) 0.002(3) -0.014(3) C20 0.028(3) 0.032(3) 0.026(3) -0.002(3) -0.007(2) -0.006(3) C21 0.024(3) 0.035(4) 0.018(3) 0.007(3) 0.000(2) -0.005(3) C22 0.022(3) 0.041(4) 0.020(3) -0.004(3) 0.001(2) 0.000(3) C23 0.036(3) 0.037(4) 0.043(4) 0.003(3) -0.007(3) 0.000(3) C24 0.057(5) 0.053(5) 0.061(5) 0.006(4) -0.021(4) 0.019(4) C25 0.033(4) 0.084(6) 0.067(5) 0.002(5) 0.001(4) -0.019(4) C26 0.025(3) 0.071(5) 0.038(4) 0.005(4) 0.001(3) -0.002(3) O1W 0.094(7) 0.064(6) 0.160(9) 0.000 0.019(7) 0.000 O2W 0.055(5) 0.108(7) 0.051(5) 0.048(5) -0.045(4) -0.041(5) O3W 0.165(9) 0.109(8) 0.123(9) 0.036(7) 0.076(7) 0.011(8) _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 O1 1.965(3) . ? Cu1 N3 2.012(4) 7_566 ? Cu1 N2 2.020(4) 5_666 ? Cu1 N1 2.051(4) . ? Cu1 O2 2.217(4) 8_755 ? S1 O4 1.430(5) . ? S1 O3 1.452(5) . ? S1 O2 1.464(4) . ? S1 O1 1.501(4) . ? O2 Cu1 2.217(4) 8_765 ? N1 C9 1.327(7) . ? N1 C10 1.327(7) . ? N2 C14 1.335(7) . ? N2 C15 1.342(7) . ? N2 Cu1 2.020(4) 5_666 ? N3 C19 1.334(7) . ? N3 C20 1.346(7) . ? N3 Cu1 2.012(4) 7_565 ? N4 C25 1.310(9) . ? N4 C24 1.313(9) . ? C1 C2 1.382(7) . ? C1 C6 1.411(7) . ? C1 C7 1.497(7) . ? C2 C3 1.388(7) . ? C2 H2A 0.9300 . ? C3 C4 1.408(7) . ? C3 C12 1.487(7) . ? C4 C5 1.394(7) . ? C4 C17 1.493(7) . ? C5 C6 1.379(7) . ? C5 H5A 0.9300 . ? C6 C22 1.480(7) . ? C7 C8 1.391(7) . ? C7 C11 1.398(7) . ? C8 C9 1.375(7) . ? C8 H8A 0.9300 . ? C9 H9A 0.9300 . ? C10 C11 1.364(7) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C12 C16 1.383(8) . ? C12 C13 1.388(8) . ? C13 C14 1.375(8) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C15 C16 1.385(7) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? C17 C18 1.372(8) . ? C17 C21 1.394(7) . ? C18 C19 1.381(8) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C20 C21 1.367(7) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 C23 1.382(8) . ? C22 C26 1.383(8) . ? C23 C24 1.381(9) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? C25 C26 1.388(9) . ? C25 H25A 0.9300 . ? C26 H26A 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 O1 Cu1 N3 92.48(16) . 7_566 ? O1 Cu1 N2 168.61(18) . 5_666 ? N3 Cu1 N2 90.48(17) 7_566 5_666 ? O1 Cu1 N1 89.61(16) . . ? N3 Cu1 N1 171.6(2) 7_566 . ? N2 Cu1 N1 85.95(17) 5_666 . ? O1 Cu1 O2 88.79(16) . 8_755 ? N3 Cu1 O2 97.54(18) 7_566 8_755 ? N2 Cu1 O2 101.73(19) 5_666 8_755 ? N1 Cu1 O2 90.61(18) . 8_755 ? O4 S1 O3 111.4(3) . . ? O4 S1 O2 111.3(3) . . ? O3 S1 O2 109.8(3) . . ? O4 S1 O1 108.6(3) . . ? O3 S1 O1 107.9(3) . . ? O2 S1 O1 107.7(2) . . ? S1 O1 Cu1 123.6(2) . . ? S1 O2 Cu1 154.0(3) . 8_765 ? C9 N1 C10 117.1(5) . . ? C9 N1 Cu1 121.1(4) . . ? C10 N1 Cu1 121.5(4) . . ? C14 N2 C15 117.9(5) . . ? C14 N2 Cu1 121.3(4) . 5_666 ? C15 N2 Cu1 120.4(4) . 5_666 ? C19 N3 C20 116.3(5) . . ? C19 N3 Cu1 118.4(4) . 7_565 ? C20 N3 Cu1 125.1(4) . 7_565 ? C25 N4 C24 115.0(6) . . ? C2 C1 C6 118.6(5) . . ? C2 C1 C7 117.6(5) . . ? C6 C1 C7 123.2(5) . . ? C1 C2 C3 123.6(5) . . ? C1 C2 H2A 118.2 . . ? C3 C2 H2A 118.2 . . ? C2 C3 C4 117.9(5) . . ? C2 C3 C12 118.2(5) . . ? C4 C3 C12 123.5(5) . . ? C5 C4 C3 118.3(5) . . ? C5 C4 C17 118.8(5) . . ? C3 C4 C17 122.8(5) . . ? C6 C5 C4 123.6(5) . . ? C6 C5 H5A 118.2 . . ? C4 C5 H5A 118.2 . . ? C5 C6 C1 117.9(5) . . ? C5 C6 C22 118.8(5) . . ? C1 C6 C22 123.3(5) . . ? C8 C7 C11 115.9(5) . . ? C8 C7 C1 121.6(5) . . ? C11 C7 C1 122.3(5) . . ? C9 C8 C7 120.0(5) . . ? C9 C8 H8A 120.0 . . ? C7 C8 H8A 120.0 . . ? N1 C9 C8 123.3(5) . . ? N1 C9 H9A 118.3 . . ? C8 C9 H9A 118.3 . . ? N1 C10 C11 123.7(5) . . ? N1 C10 H10A 118.1 . . ? C11 C10 H10A 118.1 . . ? C10 C11 C7 120.0(5) . . ? C10 C11 H11A 120.0 . . ? C7 C11 H11A 120.0 . . ? C16 C12 C13 117.2(5) . . ? C16 C12 C3 121.4(5) . . ? C13 C12 C3 121.1(5) . . ? C14 C13 C12 119.6(5) . . ? C14 C13 H13A 120.2 . . ? C12 C13 H13A 120.2 . . ? N2 C14 C13 123.2(5) . . ? N2 C14 H14A 118.4 . . ? C13 C14 H14A 118.4 . . ? N2 C15 C16 121.9(6) . . ? N2 C15 H15A 119.0 . . ? C16 C15 H15A 119.0 . . ? C12 C16 C15 120.2(5) . . ? C12 C16 H16A 119.9 . . ? C15 C16 H16A 119.9 . . ? C18 C17 C21 117.4(5) . . ? C18 C17 C4 120.2(5) . . ? C21 C17 C4 122.5(5) . . ? C17 C18 C19 120.0(5) . . ? C17 C18 H18A 120.0 . . ? C19 C18 H18A 120.0 . . ? N3 C19 C18 123.2(5) . . ? N3 C19 H19A 118.4 . . ? C18 C19 H19A 118.4 . . ? N3 C20 C21 124.1(5) . . ? N3 C20 H20A 118.0 . . ? C21 C20 H20A 118.0 . . ? C20 C21 C17 119.0(5) . . ? C20 C21 H21A 120.5 . . ? C17 C21 H21A 120.5 . . ? C23 C22 C26 116.8(6) . . ? C23 C22 C6 122.2(5) . . ? C26 C22 C6 121.0(5) . . ? C24 C23 C22 119.0(6) . . ? C24 C23 H23A 120.5 . . ? C22 C23 H23A 120.5 . . ? N4 C24 C23 125.2(7) . . ? N4 C24 H24A 117.4 . . ? C23 C24 H24A 117.4 . . ? N4 C25 C26 125.6(7) . . ? N4 C25 H25A 117.2 . . ? C26 C25 H25A 117.2 . . ? C22 C26 C25 118.4(7) . . ? C22 C26 H26A 120.8 . . ? C25 C26 H26A 120.8 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.305 _refine_diff_density_min -0.393 _refine_diff_density_rms 0.109 #=================================================END data_complex3 _database_code_depnum_ccdc_archive 'CCDC 768412' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H21 Br2 Cu2 N5' _chemical_formula_weight 714.40 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' _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 13.1150(19) _cell_length_b 22.273(3) _cell_length_c 10.6802(15) _cell_angle_alpha 90.00 _cell_angle_beta 118.973(2) _cell_angle_gamma 90.00 _cell_volume 2729.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.739 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 4.513 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2530 _exptl_absorpt_correction_T_max 0.3352 _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 4976 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_sigmaI/netI 0.0496 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 3 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2537 _reflns_number_gt 2040 _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^)+(0.0578P)^2^+5.5660P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2537 _refine_ls_number_parameters 169 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0700 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1309 _refine_ls_wR_factor_gt 0.1242 _refine_ls_goodness_of_fit_ref 1.136 _refine_ls_restrained_S_all 1.137 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.91871(6) 0.33624(3) 0.79580(8) 0.0389(2) Uani 1 1 d . . . Br1 Br 0.87224(6) 0.37504(3) 0.55449(7) 0.0441(2) Uani 1 1 d . . . N1 N 0.9294(4) 0.24655(19) 0.8397(5) 0.0297(10) Uani 1 1 d . . . N2 N 1.3137(4) -0.1197(2) 0.8544(6) 0.0372(12) Uani 1 1 d . . . C1 C 1.0340(5) 0.2233(3) 0.9284(6) 0.0337(13) Uani 1 1 d . . . H1A H 1.0979 0.2489 0.9651 0.040 Uiso 1 1 calc R . . C2 C 1.0535(5) 0.1641(2) 0.9691(6) 0.0316(13) Uani 1 1 d . . . H2A H 1.1284 0.1502 1.0301 0.038 Uiso 1 1 calc R . . C3 C 0.9589(5) 0.1256(2) 0.9170(6) 0.0279(12) Uani 1 1 d . . . C4 C 0.8514(5) 0.1480(2) 0.8215(6) 0.0299(12) Uani 1 1 d . . . H4A H 0.7864 0.1231 0.7808 0.036 Uiso 1 1 calc R . . C5 C 0.8417(5) 0.2080(2) 0.7870(6) 0.0324(13) Uani 1 1 d . . . H5A H 0.7683 0.2225 0.7220 0.039 Uiso 1 1 calc R . . C6 C 0.9786(5) 0.0609(2) 0.9635(6) 0.0279(12) Uani 1 1 d . . . C7 C 1.0585(5) 0.0282(2) 0.9414(5) 0.0275(12) Uani 1 1 d . . . H7A H 1.0989 0.0479 0.9022 0.033 Uiso 1 1 calc R . . C8 C 1.0815(5) -0.0319(2) 0.9743(6) 0.0273(12) Uani 1 1 d . . . C9 C 1.1629(5) -0.0627(2) 0.9357(6) 0.0284(12) Uani 1 1 d . . . C10 C 1.2583(5) -0.0338(3) 0.9440(7) 0.0439(16) Uani 1 1 d . . . H10A H 1.2752 0.0055 0.9778 0.053 Uiso 1 1 calc R . . C11 C 1.3295(6) -0.0635(3) 0.9016(8) 0.0473(17) Uani 1 1 d . . . H11A H 1.3927 -0.0426 0.9066 0.057 Uiso 1 1 calc R . . C12 C 1.2208(5) -0.1476(3) 0.8476(6) 0.0363(14) Uani 1 1 d . . . H12A H 1.2069 -0.1871 0.8149 0.044 Uiso 1 1 calc R . . C13 C 1.1445(5) -0.1219(2) 0.8858(6) 0.0327(13) Uani 1 1 d . . . H13A H 1.0813 -0.1436 0.8785 0.039 Uiso 1 1 calc R . . C14 C 1.0000 0.3687(7) 0.2500 0.121(6) Uani 1 2 d SU . . C15 C 1.0000 0.3039(7) 0.2500 0.090(4) Uani 1 2 d S . . N3 N 1.0000 0.2553(9) 0.2500 0.163(7) Uani 1 2 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 Cu1 0.0423(5) 0.0284(4) 0.0623(5) 0.0060(3) 0.0384(4) 0.0092(3) Br1 0.0416(4) 0.0404(4) 0.0495(4) 0.0084(3) 0.0215(3) 0.0088(3) N1 0.035(3) 0.021(2) 0.042(3) 0.004(2) 0.026(2) 0.003(2) N2 0.041(3) 0.028(3) 0.059(3) 0.003(2) 0.037(3) 0.007(2) C1 0.034(3) 0.028(3) 0.044(3) 0.001(3) 0.023(3) -0.006(3) C2 0.028(3) 0.025(3) 0.046(3) 0.008(3) 0.021(3) 0.005(3) C3 0.038(3) 0.022(3) 0.036(3) 0.002(2) 0.028(3) 0.009(2) C4 0.028(3) 0.024(3) 0.038(3) 0.000(2) 0.016(3) -0.002(2) C5 0.030(3) 0.028(3) 0.042(3) 0.008(3) 0.019(3) 0.007(3) C6 0.031(3) 0.018(3) 0.038(3) 0.001(2) 0.019(3) 0.001(2) C7 0.030(3) 0.025(3) 0.039(3) 0.002(2) 0.026(2) 0.003(2) C8 0.029(3) 0.022(3) 0.037(3) 0.002(2) 0.021(2) 0.004(2) C9 0.031(3) 0.022(3) 0.041(3) 0.007(2) 0.024(3) 0.009(2) C10 0.049(4) 0.025(3) 0.080(5) -0.010(3) 0.049(4) -0.003(3) C11 0.045(4) 0.028(3) 0.092(5) -0.001(3) 0.052(4) -0.002(3) C12 0.043(3) 0.025(3) 0.050(4) -0.004(3) 0.030(3) 0.006(3) C13 0.034(3) 0.031(3) 0.046(3) -0.002(3) 0.029(3) 0.001(3) C14 0.130(10) 0.090(8) 0.118(9) 0.000 0.042(7) 0.000 C15 0.097(11) 0.066(9) 0.116(11) 0.000 0.059(9) 0.000 N3 0.164(10) 0.151(10) 0.180(10) 0.000 0.087(8) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N2 2.021(4) 3_455 ? Cu1 N1 2.041(4) . ? Cu1 Br1 2.4977(10) . ? Cu1 Br1 2.5638(10) 2_756 ? Cu1 Cu1 2.7430(13) 2_756 ? Br1 Cu1 2.5638(10) 2_756 ? N1 C5 1.323(7) . ? N1 C1 1.337(7) . ? N2 C11 1.327(7) . ? N2 C12 1.339(7) . ? N2 Cu1 2.021(4) 3_545 ? C1 C2 1.372(7) . ? C1 H1A 0.9300 . ? C2 C3 1.384(8) . ? C2 H2A 0.9300 . ? C3 C4 1.372(8) . ? C3 C6 1.505(7) . ? C4 C5 1.376(7) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 C7 1.387(7) . ? C6 C8 1.411(7) 5_757 ? C7 C8 1.379(7) . ? C7 H7A 0.9300 . ? C8 C6 1.411(7) 5_757 ? C8 C9 1.486(7) . ? C9 C10 1.372(8) . ? C9 C13 1.397(7) . ? C10 C11 1.387(8) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C12 C13 1.375(7) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C15 1.44(2) . ? C15 N3 1.084(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu1 N1 112.66(18) 3_455 . ? N2 Cu1 Br1 106.81(14) 3_455 . ? N1 Cu1 Br1 122.08(13) . . ? N2 Cu1 Br1 109.03(15) 3_455 2_756 ? N1 Cu1 Br1 104.65(14) . 2_756 ? Br1 Cu1 Br1 100.35(3) . 2_756 ? N2 Cu1 Cu1 150.94(13) 3_455 2_756 ? N1 Cu1 Cu1 95.93(12) . 2_756 ? Br1 Cu1 Cu1 58.35(3) . 2_756 ? Br1 Cu1 Cu1 56.03(3) 2_756 2_756 ? Cu1 Br1 Cu1 65.62(3) . 2_756 ? C5 N1 C1 115.6(5) . . ? C5 N1 Cu1 126.1(4) . . ? C1 N1 Cu1 118.4(4) . . ? C11 N2 C12 115.4(5) . . ? C11 N2 Cu1 124.9(4) . 3_545 ? C12 N2 Cu1 119.7(4) . 3_545 ? N1 C1 C2 124.5(5) . . ? N1 C1 H1A 117.7 . . ? C2 C1 H1A 117.7 . . ? C1 C2 C3 118.3(5) . . ? C1 C2 H2A 120.8 . . ? C3 C2 H2A 120.8 . . ? C4 C3 C2 118.1(5) . . ? C4 C3 C6 122.9(5) . . ? C2 C3 C6 118.9(5) . . ? C3 C4 C5 118.7(5) . . ? C3 C4 H4A 120.6 . . ? C5 C4 H4A 120.6 . . ? N1 C5 C4 124.6(5) . . ? N1 C5 H5A 117.7 . . ? C4 C5 H5A 117.7 . . ? C7 C6 C8 118.7(5) . 5_757 ? C7 C6 C3 118.0(4) . . ? C8 C6 C3 123.2(4) 5_757 . ? C8 C7 C6 123.8(5) . . ? C8 C7 H7A 118.1 . . ? C6 C7 H7A 118.1 . . ? C7 C8 C6 117.4(5) . 5_757 ? C7 C8 C9 118.5(4) . . ? C6 C8 C9 124.0(5) 5_757 . ? C10 C9 C13 116.9(5) . . ? C10 C9 C8 121.3(5) . . ? C13 C9 C8 121.8(5) . . ? C9 C10 C11 119.4(5) . . ? C9 C10 H10A 120.3 . . ? C11 C10 H10A 120.3 . . ? N2 C11 C10 124.7(5) . . ? N2 C11 H11A 117.7 . . ? C10 C11 H11A 117.7 . . ? N2 C12 C13 124.3(5) . . ? N2 C12 H12A 117.8 . . ? C13 C12 H12A 117.8 . . ? C12 C13 C9 119.4(5) . . ? C12 C13 H13A 120.3 . . ? C9 C13 H13A 120.3 . . ? N3 C15 C14 180.000(3) . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 1.306 _refine_diff_density_min -0.456 _refine_diff_density_rms 0.122 #=================================================END data_complex4 _database_code_depnum_ccdc_archive 'CCDC 768413' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H40 Cu10 I10 N8 O2' _chemical_formula_weight 2713.32 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1652(8) _cell_length_b 14.6342(12) _cell_length_c 15.2829(12) _cell_angle_alpha 117.5380(10) _cell_angle_beta 96.1410(10) _cell_angle_gamma 104.3380(10) _cell_volume 1887.1(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.388 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1244 _exptl_absorpt_coefficient_mu 6.886 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5889 _exptl_absorpt_correction_T_max 0.7290 _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 13440 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_sigmaI/netI 0.0475 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 25.99 _reflns_number_total 7168 _reflns_number_gt 5557 _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^)+(0.0552P)^2^+1.3222P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7168 _refine_ls_number_parameters 379 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0627 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1111 _refine_ls_wR_factor_gt 0.1025 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.038 _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 1.06010(11) 0.42453(9) 0.46631(8) 0.0480(3) Uani 1 1 d . . . Cu2 Cu 1.05841(12) 0.38349(9) 0.25476(8) 0.0533(3) Uani 1 1 d . . . Cu3 Cu 1.26431(13) 0.27354(11) 0.21815(10) 0.0665(4) Uani 1 1 d . . . Cu4 Cu 1.32794(11) 0.48919(9) 0.24570(9) 0.0543(3) Uani 1 1 d . . . Cu5 Cu 1.15207(12) 0.31448(8) 0.08543(7) 0.0469(3) Uani 1 1 d . . . I1 I 1.29036(5) 0.46144(4) 0.40899(4) 0.03950(14) Uani 1 1 d . . . I2 I 0.84529(5) 0.41237(4) 0.33542(4) 0.04237(15) Uani 1 1 d . . . I3 I 0.99483(6) 0.16719(4) 0.12842(4) 0.04404(15) Uani 1 1 d . . . I4 I 1.10266(6) 0.50209(4) 0.15727(4) 0.04451(15) Uani 1 1 d . . . I5 I 1.43175(6) 0.33781(5) 0.12593(5) 0.05655(18) Uani 1 1 d . . . N1 N 0.9577(6) 0.2905(5) 0.4735(5) 0.0393(16) Uani 1 1 d . . . N2 N 0.3434(8) 0.1892(6) 0.2730(6) 0.053(2) Uani 1 1 d . . . N3 N 1.1033(7) 0.2337(5) -0.0683(4) 0.0384(16) Uani 1 1 d . . . N4 N 1.4991(7) 0.3728(5) -0.3118(5) 0.0426(16) Uani 1 1 d . . . C1 C 0.8711(8) 0.1996(6) 0.3894(6) 0.0371(18) Uani 1 1 d . . . H1A H 0.8876 0.1863 0.3266 0.044 Uiso 1 1 calc R . . C2 C 0.7602(8) 0.1254(6) 0.3902(6) 0.0385(18) Uani 1 1 d . . . H2A H 0.7026 0.0641 0.3293 0.046 Uiso 1 1 calc R . . C3 C 0.7339(7) 0.1429(6) 0.4843(6) 0.0301(16) Uani 1 1 d . . . C4 C 0.8253(8) 0.2340(6) 0.5703(6) 0.0355(17) Uani 1 1 d . . . H4A H 0.8128 0.2481 0.6342 0.043 Uiso 1 1 calc R . . C5 C 0.9356(8) 0.3052(7) 0.5635(6) 0.0421(19) Uani 1 1 d . . . H5A H 0.9969 0.3656 0.6234 0.050 Uiso 1 1 calc R . . C6 C 0.6105(8) 0.0711(6) 0.4911(6) 0.0342(17) Uani 1 1 d . . . C7 C 0.6343(8) 0.0334(6) 0.5576(6) 0.0328(17) Uani 1 1 d . . . H7A H 0.7246 0.0577 0.5979 0.039 Uiso 1 1 calc R . . C8 C 0.4750(7) 0.0403(6) 0.4350(6) 0.0319(16) Uani 1 1 d . . . C9 C 0.4360(7) 0.0896(6) 0.3730(6) 0.0319(16) Uani 1 1 d . . . C10 C 0.4951(8) 0.2000(7) 0.4099(6) 0.0409(19) Uani 1 1 d . . . H10A H 0.5675 0.2431 0.4695 0.049 Uiso 1 1 calc R . . C11 C 0.4470(9) 0.2474(7) 0.3585(7) 0.048(2) Uani 1 1 d . . . H11A H 0.4883 0.3221 0.3845 0.058 Uiso 1 1 calc R . . C12 C 0.2910(9) 0.0826(7) 0.2351(7) 0.052(2) Uani 1 1 d . . . H12A H 0.2219 0.0407 0.1736 0.062 Uiso 1 1 calc R . . C13 C 0.3335(8) 0.0308(7) 0.2819(6) 0.045(2) Uani 1 1 d . . . H13A H 0.2930 -0.0446 0.2520 0.054 Uiso 1 1 calc R . . C14 C 1.0890(9) 0.1290(7) -0.1204(6) 0.044(2) Uani 1 1 d . . . H14A H 1.0909 0.0927 -0.0841 0.053 Uiso 1 1 calc R . . C15 C 1.0715(9) 0.0698(6) -0.2234(5) 0.0387(19) Uani 1 1 d . . . H15A H 1.0624 -0.0040 -0.2553 0.046 Uiso 1 1 calc R . . C16 C 1.0677(7) 0.1216(6) -0.2792(5) 0.0293(16) Uani 1 1 d . . . C17 C 1.0844(8) 0.2317(6) -0.2268(5) 0.0390(19) Uani 1 1 d . . . H17A H 1.0848 0.2702 -0.2611 0.047 Uiso 1 1 calc R . . C18 C 1.1004(9) 0.2834(7) -0.1224(6) 0.047(2) Uani 1 1 d . . . H18A H 1.1096 0.3572 -0.0879 0.056 Uiso 1 1 calc R . . C19 C 1.0404(7) 0.0585(6) -0.3939(5) 0.0295(16) Uani 1 1 d . . . C20 C 0.9291(7) -0.0385(6) -0.4466(5) 0.0305(16) Uani 1 1 d . . . H20A H 0.8821 -0.0655 -0.4099 0.037 Uiso 1 1 calc R . . C21 C 1.1155(7) 0.0972(6) -0.4479(5) 0.0304(16) Uani 1 1 d . . . C22 C 1.2475(7) 0.1960(6) -0.3970(5) 0.0289(16) Uani 1 1 d . . . C23 C 1.2669(8) 0.2758(6) -0.4237(6) 0.0367(18) Uani 1 1 d . . . H23A H 1.1965 0.2715 -0.4712 0.044 Uiso 1 1 calc R . . C24 C 1.3921(8) 0.3619(6) -0.3790(6) 0.043(2) Uani 1 1 d . . . H24A H 1.4028 0.4157 -0.3967 0.051 Uiso 1 1 calc R . . C25 C 1.4792(8) 0.2950(7) -0.2895(6) 0.046(2) Uani 1 1 d . . . H25A H 1.5529 0.2993 -0.2444 0.055 Uiso 1 1 calc R . . C26 C 1.3581(8) 0.2080(6) -0.3275(6) 0.0386(19) Uani 1 1 d . . . H26A H 1.3501 0.1570 -0.3065 0.046 Uiso 1 1 calc R . . O1W O 1.481(2) 0.0967(16) 0.0360(17) 0.132(7) Uani 0.50 1 d PU . . O1W' O 1.621(3) 0.050(3) 0.045(3) 0.205(12) Uani 0.50 1 d PU . . 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 0.0454(6) 0.0462(6) 0.0585(7) 0.0334(6) 0.0197(5) 0.0083(5) Cu2 0.0541(7) 0.0546(7) 0.0475(6) 0.0227(6) 0.0198(5) 0.0164(5) Cu3 0.0631(8) 0.0780(9) 0.0814(9) 0.0632(8) 0.0059(7) 0.0190(7) Cu4 0.0418(6) 0.0420(6) 0.0564(7) 0.0211(5) -0.0024(5) -0.0076(5) Cu5 0.0701(7) 0.0402(6) 0.0205(5) 0.0112(4) 0.0047(5) 0.0146(5) I1 0.0341(3) 0.0484(3) 0.0312(3) 0.0208(2) 0.0088(2) 0.0050(2) I2 0.0396(3) 0.0432(3) 0.0408(3) 0.0204(3) 0.0107(2) 0.0099(2) I3 0.0515(3) 0.0349(3) 0.0380(3) 0.0174(2) 0.0116(2) 0.0045(2) I4 0.0563(3) 0.0404(3) 0.0392(3) 0.0208(3) 0.0112(3) 0.0192(3) I5 0.0505(3) 0.0654(4) 0.0579(4) 0.0318(3) 0.0223(3) 0.0214(3) N1 0.038(4) 0.039(4) 0.048(4) 0.030(3) 0.015(3) 0.006(3) N2 0.058(5) 0.060(5) 0.064(5) 0.050(4) 0.012(4) 0.016(4) N3 0.061(4) 0.030(4) 0.016(3) 0.009(3) 0.005(3) 0.010(3) N4 0.042(4) 0.036(4) 0.039(4) 0.018(3) 0.007(3) -0.001(3) C1 0.044(4) 0.041(5) 0.039(4) 0.027(4) 0.020(4) 0.018(4) C2 0.047(5) 0.031(4) 0.038(4) 0.019(4) 0.012(4) 0.008(4) C3 0.034(4) 0.027(4) 0.041(4) 0.023(3) 0.017(3) 0.015(3) C4 0.039(4) 0.033(4) 0.037(4) 0.022(4) 0.013(3) 0.006(3) C5 0.042(5) 0.042(5) 0.040(5) 0.025(4) 0.004(4) 0.004(4) C6 0.035(4) 0.038(4) 0.040(4) 0.025(4) 0.017(3) 0.014(3) C7 0.032(4) 0.033(4) 0.038(4) 0.022(4) 0.012(3) 0.010(3) C8 0.034(4) 0.032(4) 0.039(4) 0.025(4) 0.014(3) 0.010(3) C9 0.035(4) 0.028(4) 0.039(4) 0.020(3) 0.012(3) 0.012(3) C10 0.035(4) 0.042(5) 0.044(5) 0.025(4) 0.002(4) 0.008(4) C11 0.044(5) 0.041(5) 0.059(6) 0.030(5) 0.002(4) 0.010(4) C12 0.049(5) 0.054(6) 0.050(5) 0.035(5) -0.002(4) 0.002(4) C13 0.046(5) 0.038(5) 0.043(5) 0.023(4) 0.002(4) 0.001(4) C14 0.072(6) 0.043(5) 0.025(4) 0.020(4) 0.013(4) 0.026(4) C15 0.060(5) 0.025(4) 0.024(4) 0.010(3) 0.011(4) 0.010(4) C16 0.024(4) 0.038(4) 0.018(3) 0.011(3) 0.004(3) 0.006(3) C17 0.059(5) 0.036(4) 0.023(4) 0.017(4) 0.010(4) 0.013(4) C18 0.069(6) 0.039(5) 0.027(4) 0.016(4) 0.008(4) 0.014(4) C19 0.030(4) 0.029(4) 0.023(4) 0.012(3) 0.004(3) 0.006(3) C20 0.032(4) 0.034(4) 0.016(3) 0.009(3) 0.005(3) 0.004(3) C21 0.033(4) 0.026(4) 0.027(4) 0.012(3) 0.005(3) 0.005(3) C22 0.028(4) 0.027(4) 0.016(3) 0.005(3) 0.002(3) 0.000(3) C23 0.034(4) 0.042(5) 0.038(4) 0.025(4) 0.003(3) 0.009(3) C24 0.037(4) 0.036(5) 0.050(5) 0.028(4) 0.003(4) -0.001(4) C25 0.038(4) 0.045(5) 0.037(4) 0.021(4) -0.013(4) -0.005(4) C26 0.042(4) 0.030(4) 0.041(4) 0.023(4) 0.003(4) 0.001(3) O1W 0.143(10) 0.099(10) 0.155(11) 0.051(7) 0.089(9) 0.050(8) O1W' 0.199(15) 0.203(15) 0.205(15) 0.100(10) 0.045(10) 0.068(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.039(6) . ? Cu1 I1 2.6053(11) . ? Cu1 Cu1 2.633(2) 2_766 ? Cu1 I2 2.7101(12) . ? Cu1 I2 2.7120(12) 2_766 ? Cu1 Cu2 3.0002(16) . ? Cu2 I2 2.6333(12) . ? Cu2 Cu5 2.6853(14) . ? Cu2 I3 2.6896(13) . ? Cu2 I1 2.7220(13) . ? Cu2 I4 2.7537(13) . ? Cu2 Cu4 2.8458(15) . ? Cu2 Cu3 2.8929(18) . ? Cu3 N2 2.044(7) 1_655 ? Cu3 I5 2.5912(14) . ? Cu3 Cu5 2.5966(15) . ? Cu3 I3 2.6301(14) . ? Cu3 I1 2.8629(16) . ? Cu3 Cu4 2.8734(17) . ? Cu4 N4 2.041(6) 2_865 ? Cu4 Cu5 2.5964(14) . ? Cu4 I4 2.6257(13) . ? Cu4 I5 2.6820(14) . ? Cu4 I1 2.7573(13) . ? Cu5 N3 2.013(6) . ? Cu5 I4 2.6475(12) . ? Cu5 I3 2.7314(12) . ? Cu5 I5 2.7441(13) . ? I2 Cu1 2.7120(12) 2_766 ? N1 C1 1.339(10) . ? N1 C5 1.344(10) . ? N2 C12 1.318(11) . ? N2 C11 1.332(11) . ? N2 Cu3 2.044(7) 1_455 ? N3 C14 1.319(10) . ? N3 C18 1.332(10) . ? N4 C25 1.310(10) . ? N4 C24 1.337(10) . ? N4 Cu4 2.041(6) 2_865 ? C1 C2 1.364(10) . ? C1 H1A 0.9300 . ? C2 C3 1.409(10) . ? C2 H2A 0.9300 . ? C3 C4 1.369(10) . ? C3 C6 1.471(9) . ? C4 C5 1.378(10) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 C8 1.384(10) . ? C6 C7 1.388(10) . ? C7 C8 1.400(9) 2_656 ? C7 H7A 0.9300 . ? C8 C7 1.400(9) 2_656 ? C8 C9 1.506(10) . ? C9 C10 1.377(10) . ? C9 C13 1.380(10) . ? C10 C11 1.388(11) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C12 C13 1.368(11) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C15 1.365(10) . ? C14 H14A 0.9300 . ? C15 C16 1.383(10) . ? C15 H15A 0.9300 . ? C16 C17 1.381(10) . ? C16 C19 1.508(9) . ? C17 C18 1.384(10) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 C20 1.377(9) . ? C19 C21 1.392(9) . ? C20 C21 1.384(9) 2_754 ? C20 H20A 0.9300 . ? C21 C20 1.384(9) 2_754 ? C21 C22 1.507(9) . ? C22 C26 1.378(10) . ? C22 C23 1.384(10) . ? C23 C24 1.377(10) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? C25 C26 1.364(10) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? O1W O1W' 1.75(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 I1 127.89(19) . . ? N1 Cu1 Cu1 112.13(19) . 2_766 ? I1 Cu1 Cu1 119.91(6) . 2_766 ? N1 Cu1 I2 97.36(19) . . ? I1 Cu1 I2 109.32(4) . . ? Cu1 Cu1 I2 60.98(4) 2_766 . ? N1 Cu1 I2 103.75(19) . 2_766 ? I1 Cu1 I2 98.83(4) . 2_766 ? Cu1 Cu1 I2 60.91(4) 2_766 2_766 ? I2 Cu1 I2 121.89(4) . 2_766 ? N1 Cu1 Cu2 114.99(19) . . ? I1 Cu1 Cu2 57.59(3) . . ? Cu1 Cu1 Cu2 101.98(6) 2_766 . ? I2 Cu1 Cu2 54.64(3) . . ? I2 Cu1 Cu2 141.25(4) 2_766 . ? I2 Cu2 Cu5 147.52(5) . . ? I2 Cu2 I3 107.50(4) . . ? Cu5 Cu2 I3 61.09(3) . . ? I2 Cu2 I1 108.13(4) . . ? Cu5 Cu2 I1 104.32(4) . . ? I3 Cu2 I1 110.27(5) . . ? I2 Cu2 I4 108.46(5) . . ? Cu5 Cu2 I4 58.24(3) . . ? I3 Cu2 I4 113.21(4) . . ? I1 Cu2 I4 109.12(4) . . ? I2 Cu2 Cu4 145.25(5) . . ? Cu5 Cu2 Cu4 55.90(4) . . ? I3 Cu2 Cu4 107.25(4) . . ? I1 Cu2 Cu4 59.32(3) . . ? I4 Cu2 Cu4 55.90(3) . . ? I2 Cu2 Cu3 146.68(5) . . ? Cu5 Cu2 Cu3 55.33(4) . . ? I3 Cu2 Cu3 56.07(4) . . ? I1 Cu2 Cu3 61.22(4) . . ? I4 Cu2 Cu3 104.81(4) . . ? Cu4 Cu2 Cu3 60.09(4) . . ? I2 Cu2 Cu1 57.07(3) . . ? Cu5 Cu2 Cu1 153.20(6) . . ? I3 Cu2 Cu1 108.43(4) . . ? I1 Cu2 Cu1 53.90(3) . . ? I4 Cu2 Cu1 138.37(5) . . ? Cu4 Cu2 Cu1 111.34(5) . . ? Cu3 Cu2 Cu1 97.99(5) . . ? N2 Cu3 I5 110.3(2) 1_655 . ? N2 Cu3 Cu5 158.5(2) 1_655 . ? I5 Cu3 Cu5 63.87(4) . . ? N2 Cu3 I3 109.3(2) 1_655 . ? I5 Cu3 I3 120.71(5) . . ? Cu5 Cu3 I3 63.01(4) . . ? N2 Cu3 I1 98.7(2) 1_655 . ? I5 Cu3 I1 107.75(5) . . ? Cu5 Cu3 I1 102.82(5) . . ? I3 Cu3 I1 107.80(5) . . ? N2 Cu3 Cu4 140.5(2) 1_655 . ? I5 Cu3 Cu4 58.51(4) . . ? Cu5 Cu3 Cu4 56.40(4) . . ? I3 Cu3 Cu4 108.11(5) . . ? I1 Cu3 Cu4 57.46(4) . . ? N2 Cu3 Cu2 137.0(2) 1_655 . ? I5 Cu3 Cu2 110.63(5) . . ? Cu5 Cu3 Cu2 58.27(4) . . ? I3 Cu3 Cu2 58.05(4) . . ? I1 Cu3 Cu2 56.44(4) . . ? Cu4 Cu3 Cu2 59.14(4) . . ? N4 Cu4 Cu5 151.10(19) 2_865 . ? N4 Cu4 I4 115.1(2) 2_865 . ? Cu5 Cu4 I4 60.92(4) . . ? N4 Cu4 I5 101.1(2) 2_865 . ? Cu5 Cu4 I5 62.62(4) . . ? I4 Cu4 I5 116.91(5) . . ? N4 Cu4 I1 102.01(19) 2_865 . ? Cu5 Cu4 I1 105.77(4) . . ? I4 Cu4 I1 111.92(4) . . ? I5 Cu4 I1 108.28(4) . . ? N4 Cu4 Cu2 147.42(19) 2_865 . ? Cu5 Cu4 Cu2 58.92(4) . . ? I4 Cu4 Cu2 60.27(4) . . ? I5 Cu4 Cu2 109.41(4) . . ? I1 Cu4 Cu2 58.10(3) . . ? N4 Cu4 Cu3 136.0(2) 2_865 . ? Cu5 Cu4 Cu3 56.41(4) . . ? I4 Cu4 Cu3 108.84(4) . . ? I5 Cu4 Cu3 55.48(4) . . ? I1 Cu4 Cu3 61.08(4) . . ? Cu2 Cu4 Cu3 60.77(4) . . ? N3 Cu5 Cu4 142.21(19) . . ? N3 Cu5 Cu3 132.2(2) . . ? Cu4 Cu5 Cu3 67.19(5) . . ? N3 Cu5 I4 110.56(19) . . ? Cu4 Cu5 I4 60.09(4) . . ? Cu3 Cu5 I4 117.15(5) . . ? N3 Cu5 Cu2 147.2(2) . . ? Cu4 Cu5 Cu2 65.18(4) . . ? Cu3 Cu5 Cu2 66.39(5) . . ? I4 Cu5 Cu2 62.17(4) . . ? N3 Cu5 I3 103.50(18) . . ? Cu4 Cu5 I3 113.56(4) . . ? Cu3 Cu5 I3 59.10(4) . . ? I4 Cu5 I3 115.31(4) . . ? Cu2 Cu5 I3 59.54(3) . . ? N3 Cu5 I5 99.8(2) . . ? Cu4 Cu5 I5 60.22(4) . . ? Cu3 Cu5 I5 57.97(4) . . ? I4 Cu5 I5 114.05(4) . . ? Cu2 Cu5 I5 112.44(4) . . ? I3 Cu5 I5 111.95(4) . . ? Cu1 I1 Cu2 68.51(4) . . ? Cu1 I1 Cu4 128.39(4) . . ? Cu2 I1 Cu4 62.58(3) . . ? Cu1 I1 Cu3 108.77(4) . . ? Cu2 I1 Cu3 62.33(4) . . ? Cu4 I1 Cu3 61.46(3) . . ? Cu2 I2 Cu1 68.30(4) . . ? Cu2 I2 Cu1 110.18(4) . 2_766 ? Cu1 I2 Cu1 58.11(4) . 2_766 ? Cu3 I3 Cu2 65.87(4) . . ? Cu3 I3 Cu5 57.90(3) . . ? Cu2 I3 Cu5 59.38(3) . . ? Cu4 I4 Cu5 58.99(3) . . ? Cu4 I4 Cu2 63.83(4) . . ? Cu5 I4 Cu2 59.59(3) . . ? Cu3 I5 Cu4 66.01(4) . . ? Cu3 I5 Cu5 58.16(4) . . ? Cu4 I5 Cu5 57.16(3) . . ? C1 N1 C5 116.8(6) . . ? C1 N1 Cu1 120.4(5) . . ? C5 N1 Cu1 118.4(5) . . ? C12 N2 C11 117.7(7) . . ? C12 N2 Cu3 124.6(6) . 1_455 ? C11 N2 Cu3 117.3(6) . 1_455 ? C14 N3 C18 116.0(6) . . ? C14 N3 Cu5 120.4(5) . . ? C18 N3 Cu5 123.1(5) . . ? C25 N4 C24 115.8(7) . . ? C25 N4 Cu4 125.2(6) . 2_865 ? C24 N4 Cu4 118.8(5) . 2_865 ? N1 C1 C2 124.0(7) . . ? N1 C1 H1A 118.0 . . ? C2 C1 H1A 118.0 . . ? C1 C2 C3 119.1(7) . . ? C1 C2 H2A 120.4 . . ? C3 C2 H2A 120.4 . . ? C4 C3 C2 116.7(6) . . ? C4 C3 C6 120.9(6) . . ? C2 C3 C6 122.3(7) . . ? C3 C4 C5 120.9(7) . . ? C3 C4 H4A 119.6 . . ? C5 C4 H4A 119.6 . . ? N1 C5 C4 122.4(7) . . ? N1 C5 H5A 118.8 . . ? C4 C5 H5A 118.8 . . ? C8 C6 C7 119.7(6) . . ? C8 C6 C3 123.4(7) . . ? C7 C6 C3 116.9(7) . . ? C6 C7 C8 121.3(7) . 2_656 ? C6 C7 H7A 119.4 . . ? C8 C7 H7A 119.4 2_656 . ? C6 C8 C7 118.9(7) . 2_656 ? C6 C8 C9 123.4(6) . . ? C7 C8 C9 117.4(6) 2_656 . ? C10 C9 C13 116.2(7) . . ? C10 C9 C8 120.4(7) . . ? C13 C9 C8 123.2(7) . . ? C9 C10 C11 120.3(8) . . ? C9 C10 H10A 119.9 . . ? C11 C10 H10A 119.9 . . ? N2 C11 C10 122.0(8) . . ? N2 C11 H11A 119.0 . . ? C10 C11 H11A 119.0 . . ? N2 C12 C13 123.1(8) . . ? N2 C12 H12A 118.4 . . ? C13 C12 H12A 118.4 . . ? C12 C13 C9 120.5(8) . . ? C12 C13 H13A 119.8 . . ? C9 C13 H13A 119.8 . . ? N3 C14 C15 125.1(7) . . ? N3 C14 H14A 117.5 . . ? C15 C14 H14A 117.5 . . ? C14 C15 C16 118.7(7) . . ? C14 C15 H15A 120.7 . . ? C16 C15 H15A 120.7 . . ? C17 C16 C15 117.7(6) . . ? C17 C16 C19 121.4(6) . . ? C15 C16 C19 120.8(7) . . ? C16 C17 C18 118.6(7) . . ? C16 C17 H17A 120.7 . . ? C18 C17 H17A 120.7 . . ? N3 C18 C17 123.8(8) . . ? N3 C18 H18A 118.1 . . ? C17 C18 H18A 118.1 . . ? C20 C19 C21 119.4(6) . . ? C20 C19 C16 117.2(6) . . ? C21 C19 C16 123.2(6) . . ? C19 C20 C21 122.3(6) . 2_754 ? C19 C20 H20A 118.8 . . ? C21 C20 H20A 118.8 2_754 . ? C20 C21 C19 118.2(6) 2_754 . ? C20 C21 C22 118.6(6) 2_754 . ? C19 C21 C22 123.1(6) . . ? C26 C22 C23 116.6(6) . . ? C26 C22 C21 122.3(7) . . ? C23 C22 C21 121.0(6) . . ? C24 C23 C22 119.0(7) . . ? C24 C23 H23A 120.5 . . ? C22 C23 H23A 120.5 . . ? N4 C24 C23 124.0(7) . . ? N4 C24 H24A 118.0 . . ? C23 C24 H24A 118.0 . . ? N4 C25 C26 124.7(8) . . ? N4 C25 H25A 117.7 . . ? C26 C25 H25A 117.7 . . ? C25 C26 C22 119.9(7) . . ? C25 C26 H26A 120.1 . . ? C22 C26 H26A 120.1 . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.608 _refine_diff_density_min -1.176 _refine_diff_density_rms 0.164 #_eof #End of Crystallographic Information File