# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Mukherjee, Partha' _publ_contact_author_name 'Mukherjee, Partha' _publ_contact_author_email psm@ipc.iisc.ernet.in _publ_section_title ; CuII-azide polymers with various molar equivalents of blocking diamine ligands: synthesis, structures, magnetic properties with DFT studies ; # Attachment '- cif.cif' data_complex1 _database_code_depnum_ccdc_archive 'CCDC 842479' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H14 Cu2 N14' _chemical_formula_sum 'C6 H14 Cu2 N14' _chemical_formula_weight 409.39 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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 7.0267(15) _cell_length_b 20.857(5) _cell_length_c 9.927(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.113(12) _cell_angle_gamma 90.00 _cell_volume 1427.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4391 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 30.7 _exptl_crystal_description rectangular _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.905 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 3.002 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5007 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52990 _diffrn_reflns_av_R_equivalents 0.0784 _diffrn_reflns_av_sigmaI/netI 0.0423 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 30.72 _reflns_number_total 4391 _reflns_number_gt 2992 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1999)' _computing_publication_material WinGX _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^ > 2\s(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^)+(0.0368P)^2^+4.3747P] 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 4391 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0919 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1266 _refine_ls_wR_factor_gt 0.1078 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 0.24663(8) 0.10852(2) 0.26242(5) 0.03433(14) Uani 1 1 d . . . Cu2 Cu 0.29221(8) 0.00360(2) 0.04774(5) 0.03439(14) Uani 1 1 d . . . N1 N 0.3614(6) 0.19365(17) 0.3360(4) 0.0416(9) Uani 1 1 d . . . N2 N 0.1733(6) 0.11095(17) 0.4462(4) 0.0430(9) Uani 1 1 d . . . H2 H 0.0836 0.0799 0.4505 0.052 Uiso 1 1 calc R . . N3 N 0.3378(6) 0.09917(16) 0.0854(4) 0.0395(8) Uani 1 1 d . . . N4 N 0.3308(6) 0.13669(18) -0.0081(4) 0.0435(9) Uani 1 1 d . . . N5 N 0.3287(9) 0.1717(2) -0.0969(5) 0.0720(15) Uani 1 1 d . . . N6 N 0.2162(6) 0.01459(17) 0.2300(4) 0.0460(10) Uani 1 1 d . . . N7 N 0.1482(5) -0.02707(17) 0.2893(4) 0.0386(8) Uani 1 1 d . . . N8 N 0.0860(7) -0.0671(2) 0.3427(5) 0.0630(13) Uani 1 1 d . . . N9 N 0.3568(6) 0.01213(17) -0.1333(4) 0.0396(8) Uani 1 1 d . . . N10 N 0.2986(5) -0.02028(18) -0.2316(4) 0.0385(8) Uani 1 1 d . . . N11 N 0.2472(8) -0.0495(2) -0.3297(5) 0.0666(14) Uani 1 1 d . . . N12 N 0.2021(8) -0.0850(2) 0.0391(4) 0.0624(13) Uani 1 1 d . . . N13 N 0.1283(6) -0.11689(17) -0.0534(4) 0.0396(8) Uani 1 1 d . . . N14 N 0.0550(7) -0.1512(2) -0.1400(5) 0.0544(11) Uani 1 1 d . . . C1 C 0.5264(7) 0.1797(3) 0.4478(6) 0.0523(12) Uani 1 1 d . . . H1A H 0.6007 0.2188 0.4695 0.063 Uiso 1 1 calc R . . H1B H 0.6097 0.1489 0.4145 0.063 Uiso 1 1 calc R . . C2 C 0.4774(9) 0.1544(3) 0.5764(6) 0.0638(15) Uani 1 1 d . . . H2A H 0.5959 0.1413 0.6374 0.077 Uiso 1 1 calc R . . H2B H 0.4194 0.1884 0.6215 0.077 Uiso 1 1 calc R . . C3 C 0.3434(9) 0.0997(3) 0.5536(6) 0.0615(15) Uani 1 1 d . . . H3A H 0.4122 0.0625 0.5290 0.074 Uiso 1 1 calc R . . H3B H 0.3008 0.0900 0.6386 0.074 Uiso 1 1 calc R . . C4 C 0.0860(7) 0.1740(2) 0.4586(5) 0.0506(12) Uani 1 1 d . . . H4A H 0.0894 0.1838 0.5545 0.061 Uiso 1 1 calc R . . H4B H -0.0484 0.1738 0.4112 0.061 Uiso 1 1 calc R . . C5 C 0.2017(8) 0.2259(2) 0.3942(6) 0.0608(15) Uani 1 1 d . . . H5A H 0.1152 0.2485 0.3218 0.073 Uiso 1 1 calc R . . H5B H 0.2574 0.2567 0.4638 0.073 Uiso 1 1 calc R . . C6 C 0.4231(11) 0.2358(3) 0.2334(6) 0.078(2) Uani 1 1 d . . . H6A H 0.3142 0.2447 0.1613 0.117 Uiso 1 1 calc R . . H6B H 0.5226 0.2148 0.1956 0.117 Uiso 1 1 calc R . . H6C H 0.4727 0.2752 0.2764 0.117 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0468(3) 0.0241(2) 0.0351(3) -0.0058(2) 0.0155(2) -0.0055(2) Cu2 0.0476(3) 0.0257(2) 0.0318(3) -0.00467(19) 0.0121(2) -0.0028(2) N1 0.056(2) 0.0314(18) 0.037(2) -0.0017(15) 0.0088(17) -0.0134(17) N2 0.057(2) 0.0335(18) 0.044(2) -0.0114(16) 0.0237(18) -0.0139(17) N3 0.060(2) 0.0243(16) 0.0381(19) -0.0012(14) 0.0189(17) -0.0014(16) N4 0.062(3) 0.0328(19) 0.039(2) 0.0007(16) 0.0182(19) 0.0071(18) N5 0.124(5) 0.043(2) 0.055(3) 0.017(2) 0.031(3) 0.012(3) N6 0.075(3) 0.0245(16) 0.047(2) -0.0080(15) 0.033(2) -0.0103(17) N7 0.047(2) 0.0305(17) 0.041(2) -0.0001(15) 0.0167(17) -0.0003(16) N8 0.078(3) 0.052(3) 0.065(3) 0.015(2) 0.029(3) -0.009(2) N9 0.051(2) 0.0359(19) 0.0334(19) -0.0046(15) 0.0116(16) -0.0041(16) N10 0.043(2) 0.0367(19) 0.037(2) -0.0004(16) 0.0101(16) 0.0036(16) N11 0.082(4) 0.068(3) 0.050(3) -0.023(2) 0.012(2) -0.018(3) N12 0.105(4) 0.039(2) 0.042(2) -0.0083(18) 0.010(2) -0.025(2) N13 0.047(2) 0.0263(17) 0.045(2) -0.0025(15) 0.0081(17) 0.0001(16) N14 0.062(3) 0.038(2) 0.056(3) -0.0120(19) -0.006(2) 0.000(2) C1 0.039(3) 0.052(3) 0.063(3) -0.007(3) 0.005(2) -0.005(2) C2 0.067(4) 0.062(4) 0.057(3) 0.008(3) -0.003(3) -0.001(3) C3 0.092(4) 0.047(3) 0.045(3) 0.002(2) 0.014(3) 0.006(3) C4 0.050(3) 0.051(3) 0.055(3) -0.021(2) 0.019(2) 0.001(2) C5 0.062(3) 0.032(2) 0.078(4) -0.016(2) -0.013(3) 0.012(2) C6 0.127(6) 0.052(3) 0.053(3) 0.002(3) 0.015(4) -0.037(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 1.990(4) . ? Cu1 N6 1.990(3) . ? Cu1 N3 1.992(3) . ? Cu1 N1 2.027(4) . ? Cu1 N14 2.401(4) 3 ? Cu2 N9 1.945(4) . ? Cu2 N12 1.949(4) . ? Cu2 N6 1.996(4) . ? Cu2 N3 2.042(3) . ? Cu2 N9 2.470(4) 3_655 ? N1 C1 1.472(6) . ? N1 C6 1.472(6) . ? N1 C5 1.514(7) . ? N2 C3 1.459(7) . ? N2 C4 1.467(6) . ? N3 N4 1.208(5) . ? N4 N5 1.142(5) . ? N6 N7 1.199(5) . ? N7 N8 1.121(5) . ? N9 N10 1.192(5) . ? N9 Cu2 2.470(4) 3_655 ? N10 N11 1.147(5) . ? N12 N13 1.171(5) . ? N13 N14 1.160(5) . ? N14 Cu1 2.401(4) 3 ? C1 C2 1.481(8) . ? C2 C3 1.469(8) . ? C4 C5 1.562(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu1 N6 97.73(15) . . ? N2 Cu1 N3 174.40(16) . . ? N6 Cu1 N3 78.70(14) . . ? N2 Cu1 N1 78.61(15) . . ? N6 Cu1 N1 160.63(18) . . ? N3 Cu1 N1 103.32(15) . . ? N2 Cu1 N14 95.48(17) . 3 ? N6 Cu1 N14 103.05(17) . 3 ? N3 Cu1 N14 89.56(16) . 3 ? N1 Cu1 N14 96.25(15) . 3 ? N9 Cu2 N12 100.22(17) . . ? N9 Cu2 N6 167.99(15) . . ? N12 Cu2 N6 90.42(17) . . ? N9 Cu2 N3 91.36(14) . . ? N12 Cu2 N3 166.25(18) . . ? N6 Cu2 N3 77.40(14) . . ? N9 Cu2 N9 86.24(15) . 3_655 ? N12 Cu2 N9 100.57(18) . 3_655 ? N6 Cu2 N9 97.32(16) . 3_655 ? N3 Cu2 N9 87.46(14) . 3_655 ? C1 N1 C6 110.2(4) . . ? C1 N1 C5 109.5(4) . . ? C6 N1 C5 109.8(4) . . ? C1 N1 Cu1 107.4(3) . . ? C6 N1 Cu1 115.0(3) . . ? C5 N1 Cu1 104.7(3) . . ? C3 N2 C4 112.4(4) . . ? C3 N2 Cu1 110.2(3) . . ? C4 N2 Cu1 106.6(3) . . ? N4 N3 Cu1 129.9(3) . . ? N4 N3 Cu2 120.7(3) . . ? Cu1 N3 Cu2 101.03(15) . . ? N5 N4 N3 178.2(5) . . ? N7 N6 Cu1 132.4(3) . . ? N7 N6 Cu2 124.3(3) . . ? Cu1 N6 Cu2 102.72(16) . . ? N8 N7 N6 178.3(5) . . ? N10 N9 Cu2 126.8(3) . . ? N10 N9 Cu2 111.6(3) . 3_655 ? Cu2 N9 Cu2 93.76(15) . 3_655 ? N11 N10 N9 176.6(5) . . ? N13 N12 Cu2 131.7(4) . . ? N14 N13 N12 176.3(5) . . ? N13 N14 Cu1 111.7(3) . 3 ? N1 C1 C2 116.1(4) . . ? C3 C2 C1 113.1(5) . . ? N2 C3 C2 113.5(4) . . ? N2 C4 C5 109.1(4) . . ? N1 C5 C4 109.4(4) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 30.72 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.961 _refine_diff_density_min -0.563 _refine_diff_density_rms 0.116 #===END data_complex2 _database_code_depnum_ccdc_archive 'CCDC 842480' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C3 H10 Cu2 N14' _chemical_formula_sum 'C3 H10 Cu2 N14' _chemical_formula_weight 369.33 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.6280(3) _cell_length_b 8.2478(4) _cell_length_c 9.9050(4) _cell_angle_alpha 92.252(3) _cell_angle_beta 91.946(3) _cell_angle_gamma 98.562(3) _cell_volume 615.24(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3545 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 30.0 _exptl_crystal_description rectangular _exptl_crystal_colour black _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.994 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 368 _exptl_absorpt_coefficient_mu 3.470 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6067 _exptl_absorpt_correction_T_max 0.9338 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12310 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 30.03 _reflns_number_total 3545 _reflns_number_gt 2681 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1999)' _computing_publication_material WinGX _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^ > 2\s(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^)+(0.0807P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3545 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0588 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.1225 _refine_ls_wR_factor_gt 0.1130 _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_restrained_S_all 0.972 _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 0.21540(5) 0.21592(4) 0.68102(3) 0.02930(13) Uani 1 1 d . . . Cu2 Cu 0.18937(5) -0.07377(4) 0.46876(3) 0.02906(13) Uani 1 1 d . . . N1 N 0.2991(4) 0.2600(4) 0.8762(3) 0.0364(6) Uani 1 1 d . . . H1 H 0.4148 0.2448 0.8825 0.044 Uiso 1 1 calc R . . N2 N 0.1231(3) 0.4295(3) 0.6957(3) 0.0297(5) Uani 1 1 d . . . H2A H 0.1894 0.5046 0.6479 0.036 Uiso 1 1 calc R . . H2B H 0.0105 0.4173 0.6623 0.036 Uiso 1 1 calc R . . N3 N 0.2837(5) -0.0066(4) 0.6558(3) 0.0481(8) Uani 1 1 d . . . N4 N 0.3652(4) -0.0870(3) 0.7247(3) 0.0409(7) Uani 1 1 d . . . N5 N 0.4406(6) -0.1656(5) 0.7889(4) 0.0789(13) Uani 1 1 d . . . N6 N 0.1232(4) 0.1563(3) 0.4884(3) 0.0287(5) Uani 1 1 d . . . N7 N 0.1487(4) 0.2502(3) 0.3938(3) 0.0355(6) Uani 1 1 d . . . N8 N 0.1682(5) 0.3333(4) 0.3061(4) 0.0625(10) Uani 1 1 d . . . N9 N 0.2487(4) -0.2987(3) 0.4787(3) 0.0374(6) Uani 1 1 d . . . N10 N 0.3838(4) -0.3294(3) 0.4325(3) 0.0329(6) Uani 1 1 d . . . N11 N 0.5092(4) -0.3673(4) 0.3899(4) 0.0557(9) Uani 1 1 d . . . N12 N 0.1404(4) -0.0824(4) 0.2729(3) 0.0453(7) Uani 1 1 d . . . N13 N 0.2230(4) -0.1549(3) 0.1982(3) 0.0358(6) Uani 1 1 d . . . N14 N 0.2959(5) -0.2239(5) 0.1200(3) 0.0550(9) Uani 1 1 d . . . C1 C 0.2931(5) 0.4363(5) 0.9052(4) 0.0502(10) Uani 1 1 d . . . H1A H 0.3978 0.5013 0.8716 0.060 Uiso 1 1 calc R . . H1B H 0.2926 0.4579 1.0022 0.060 Uiso 1 1 calc R . . C2 C 0.1308(5) 0.4844(4) 0.8396(3) 0.0436(8) Uani 1 1 d . . . H2C H 0.0259 0.4335 0.8832 0.052 Uiso 1 1 calc R . . H2D H 0.1353 0.6025 0.8478 0.052 Uiso 1 1 calc R . . C3 C 0.2011(6) 0.1519(6) 0.9722(4) 0.0590(11) Uani 1 1 d . . . H3A H 0.2100 0.0396 0.9482 0.089 Uiso 1 1 calc R . . H3B H 0.0786 0.1668 0.9689 0.089 Uiso 1 1 calc R . . H3C H 0.2508 0.1790 1.0620 0.089 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0397(2) 0.0258(2) 0.0240(2) -0.00555(14) 0.00083(15) 0.01182(15) Cu2 0.0364(2) 0.0254(2) 0.0268(2) -0.00558(14) 0.00381(15) 0.01034(15) N1 0.0377(14) 0.0406(15) 0.0319(14) -0.0078(11) -0.0034(11) 0.0126(12) N2 0.0332(13) 0.0255(12) 0.0307(13) -0.0046(10) 0.0047(10) 0.0070(10) N3 0.077(2) 0.0354(16) 0.0357(15) -0.0125(12) -0.0160(15) 0.0278(15) N4 0.0481(17) 0.0321(14) 0.0424(16) -0.0038(12) -0.0066(14) 0.0089(13) N5 0.099(3) 0.064(3) 0.078(3) 0.000(2) -0.031(2) 0.038(2) N6 0.0369(14) 0.0233(12) 0.0263(12) -0.0054(9) 0.0011(10) 0.0082(10) N7 0.0445(16) 0.0317(14) 0.0328(14) -0.0022(12) 0.0022(12) 0.0143(12) N8 0.093(3) 0.052(2) 0.048(2) 0.0088(16) 0.0112(19) 0.0271(19) N9 0.0404(15) 0.0275(13) 0.0459(16) -0.0046(12) 0.0138(13) 0.0098(11) N10 0.0332(14) 0.0248(12) 0.0413(15) -0.0004(11) 0.0051(11) 0.0055(10) N11 0.0418(17) 0.0483(19) 0.082(3) 0.0114(17) 0.0246(17) 0.0164(15) N12 0.065(2) 0.0456(17) 0.0292(14) -0.0069(12) 0.0040(13) 0.0237(15) N13 0.0425(15) 0.0355(14) 0.0293(13) -0.0040(11) 0.0014(12) 0.0067(12) N14 0.061(2) 0.065(2) 0.0413(17) -0.0201(16) 0.0094(15) 0.0221(17) C1 0.057(2) 0.048(2) 0.045(2) -0.0224(17) -0.0103(18) 0.0149(18) C2 0.056(2) 0.0379(18) 0.0386(18) -0.0138(14) 0.0016(16) 0.0168(16) C3 0.071(3) 0.072(3) 0.0330(19) 0.0084(18) 0.0017(18) 0.007(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N3 1.990(3) . ? Cu1 N2 1.994(3) . ? Cu1 N1 2.017(3) . ? Cu1 N6 2.027(3) . ? Cu1 N11 2.419(3) 2_656 ? Cu2 N12 1.959(3) . ? Cu2 N9 1.979(3) . ? Cu2 N3 1.991(3) . ? Cu2 N6 2.039(3) . ? Cu2 N6 2.436(3) 2_556 ? N1 C3 1.475(5) . ? N1 C1 1.479(4) . ? N1 H1 0.9100 . ? N2 C2 1.475(4) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N3 N4 1.192(4) . ? N4 N5 1.129(4) . ? N6 N7 1.241(4) . ? N6 Cu2 2.436(3) 2_556 ? N7 N8 1.128(4) . ? N9 N10 1.198(4) . ? N10 N11 1.138(4) . ? N11 Cu1 2.419(3) 2_656 ? N12 N13 1.188(4) . ? N13 N14 1.149(4) . ? C1 C2 1.491(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2C 0.9700 . ? C2 H2D 0.9700 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 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 N3 Cu1 N2 173.97(12) . . ? N3 Cu1 N1 97.99(12) . . ? N2 Cu1 N1 86.44(11) . . ? N3 Cu1 N6 79.36(11) . . ? N2 Cu1 N6 96.01(11) . . ? N1 Cu1 N6 176.08(11) . . ? N3 Cu1 N11 96.58(14) . 2_656 ? N2 Cu1 N11 87.48(11) . 2_656 ? N1 Cu1 N11 90.03(12) . 2_656 ? N6 Cu1 N11 93.13(12) . 2_656 ? N12 Cu2 N9 96.44(12) . . ? N12 Cu2 N3 163.67(15) . . ? N9 Cu2 N3 93.72(12) . . ? N12 Cu2 N6 91.58(12) . . ? N9 Cu2 N6 171.56(11) . . ? N3 Cu2 N6 79.06(11) . . ? N12 Cu2 N6 91.80(12) . 2_556 ? N9 Cu2 N6 94.19(10) . 2_556 ? N3 Cu2 N6 100.18(13) . 2_556 ? N6 Cu2 N6 82.91(10) . 2_556 ? C3 N1 C1 113.4(3) . . ? C3 N1 Cu1 114.8(2) . . ? C1 N1 Cu1 105.6(2) . . ? C3 N1 H1 107.6 . . ? C1 N1 H1 107.6 . . ? Cu1 N1 H1 107.6 . . ? C2 N2 Cu1 108.4(2) . . ? C2 N2 H2A 110.0 . . ? Cu1 N2 H2A 110.0 . . ? C2 N2 H2B 110.0 . . ? Cu1 N2 H2B 110.0 . . ? H2A N2 H2B 108.4 . . ? N4 N3 Cu1 133.3(3) . . ? N4 N3 Cu2 124.4(2) . . ? Cu1 N3 Cu2 102.22(14) . . ? N5 N4 N3 178.8(4) . . ? N7 N6 Cu1 123.7(2) . . ? N7 N6 Cu2 119.3(2) . . ? Cu1 N6 Cu2 99.32(11) . . ? N7 N6 Cu2 113.6(2) . 2_556 ? Cu1 N6 Cu2 98.96(11) . 2_556 ? Cu2 N6 Cu2 97.09(10) . 2_556 ? N8 N7 N6 178.2(4) . . ? N10 N9 Cu2 119.4(2) . . ? N11 N10 N9 176.3(3) . . ? N10 N11 Cu1 133.7(3) . 2_656 ? N13 N12 Cu2 121.1(3) . . ? N14 N13 N12 176.0(4) . . ? N1 C1 C2 110.1(3) . . ? N1 C1 H1A 109.6 . . ? C2 C1 H1A 109.6 . . ? N1 C1 H1B 109.6 . . ? C2 C1 H1B 109.6 . . ? H1A C1 H1B 108.1 . . ? N2 C2 C1 108.3(3) . . ? N2 C2 H2C 110.0 . . ? C1 C2 H2C 110.0 . . ? N2 C2 H2D 110.0 . . ? C1 C2 H2D 110.0 . . ? H2C C2 H2D 108.4 . . ? N1 C3 H3A 109.5 . . ? N1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 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 N3 Cu1 N1 C3 -65.8(3) . . . . ? N2 Cu1 N1 C3 110.0(3) . . . . ? N6 Cu1 N1 C3 -18.7(17) . . . . ? N11 Cu1 N1 C3 -162.5(3) 2_656 . . . ? N3 Cu1 N1 C1 168.5(2) . . . . ? N2 Cu1 N1 C1 -15.7(2) . . . . ? N6 Cu1 N1 C1 -144.4(15) . . . . ? N11 Cu1 N1 C1 71.8(2) 2_656 . . . ? N3 Cu1 N2 C2 126.1(12) . . . . ? N1 Cu1 N2 C2 -11.3(2) . . . . ? N6 Cu1 N2 C2 165.6(2) . . . . ? N11 Cu1 N2 C2 -101.5(2) 2_656 . . . ? N2 Cu1 N3 N4 -144.3(10) . . . . ? N1 Cu1 N3 N4 -7.3(5) . . . . ? N6 Cu1 N3 N4 175.6(5) . . . . ? N11 Cu1 N3 N4 83.7(4) 2_656 . . . ? N2 Cu1 N3 Cu2 38.6(13) . . . . ? N1 Cu1 N3 Cu2 175.52(14) . . . . ? N6 Cu1 N3 Cu2 -1.57(13) . . . . ? N11 Cu1 N3 Cu2 -93.53(17) 2_656 . . . ? N12 Cu2 N3 N4 -120.0(5) . . . . ? N9 Cu2 N3 N4 8.5(4) . . . . ? N6 Cu2 N3 N4 -176.0(4) . . . . ? N6 Cu2 N3 N4 103.4(4) 2_556 . . . ? N12 Cu2 N3 Cu1 57.5(5) . . . . ? N9 Cu2 N3 Cu1 -174.03(15) . . . . ? N6 Cu2 N3 Cu1 1.56(13) . . . . ? N6 Cu2 N3 Cu1 -79.09(16) 2_556 . . . ? Cu1 N3 N4 N5 153(23) . . . . ? Cu2 N3 N4 N5 -30(23) . . . . ? N3 Cu1 N6 N7 -133.4(3) . . . . ? N2 Cu1 N6 N7 50.5(3) . . . . ? N1 Cu1 N6 N7 179(73) . . . . ? N11 Cu1 N6 N7 -37.3(3) 2_656 . . . ? N3 Cu1 N6 Cu2 1.52(12) . . . . ? N2 Cu1 N6 Cu2 -174.58(10) . . . . ? N1 Cu1 N6 Cu2 -46.1(16) . . . . ? N11 Cu1 N6 Cu2 97.62(12) 2_656 . . . ? N3 Cu1 N6 Cu2 100.29(14) . . . 2_556 ? N2 Cu1 N6 Cu2 -75.81(11) . . . 2_556 ? N1 Cu1 N6 Cu2 52.7(16) . . . 2_556 ? N11 Cu1 N6 Cu2 -163.60(11) 2_656 . . 2_556 ? N12 Cu2 N6 N7 -30.6(3) . . . . ? N9 Cu2 N6 N7 167.5(7) . . . . ? N3 Cu2 N6 N7 136.0(3) . . . . ? N6 Cu2 N6 N7 -122.2(3) 2_556 . . . ? N12 Cu2 N6 Cu1 -168.04(13) . . . . ? N9 Cu2 N6 Cu1 30.0(8) . . . . ? N3 Cu2 N6 Cu1 -1.52(12) . . . . ? N6 Cu2 N6 Cu1 100.34(13) 2_556 . . . ? N12 Cu2 N6 Cu2 91.62(12) . . . 2_556 ? N9 Cu2 N6 Cu2 -70.3(7) . . . 2_556 ? N3 Cu2 N6 Cu2 -101.85(15) . . . 2_556 ? N6 Cu2 N6 Cu2 0.0 2_556 . . 2_556 ? Cu1 N6 N7 N8 -160(12) . . . . ? Cu2 N6 N7 N8 73(12) . . . . ? Cu2 N6 N7 N8 -40(12) 2_556 . . . ? N12 Cu2 N9 N10 70.2(3) . . . . ? N3 Cu2 N9 N10 -97.0(3) . . . . ? N6 Cu2 N9 N10 -128.0(7) . . . . ? N6 Cu2 N9 N10 162.5(3) 2_556 . . . ? Cu2 N9 N10 N11 -174(6) . . . . ? N9 N10 N11 Cu1 -171(6) . . . 2_656 ? N9 Cu2 N12 N13 -35.5(3) . . . . ? N3 Cu2 N12 N13 92.7(5) . . . . ? N6 Cu2 N12 N13 147.1(3) . . . . ? N6 Cu2 N12 N13 -129.9(3) 2_556 . . . ? Cu2 N12 N13 N14 169(6) . . . . ? C3 N1 C1 C2 -86.3(4) . . . . ? Cu1 N1 C1 C2 40.2(4) . . . . ? Cu1 N2 C2 C1 36.0(3) . . . . ? N1 C1 C2 N2 -51.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.132 _refine_diff_density_min -0.695 _refine_diff_density_rms 0.134 #===END data_complex3 _database_code_depnum_ccdc_archive 'CCDC 842481' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H24 Cu5 N34' _chemical_formula_sum 'C8 H24 Cu5 N34' _chemical_formula_weight 914.31 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.6737(3) _cell_length_b 9.4801(4) _cell_length_c 11.3796(5) _cell_angle_alpha 113.678(2) _cell_angle_beta 92.067(2) _cell_angle_gamma 93.776(2) _cell_volume 754.73(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4513 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 30.5 _exptl_crystal_description rectangular _exptl_crystal_colour black _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.012 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 455 _exptl_absorpt_coefficient_mu 3.534 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5790 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_process_details SADABS _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 11543 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 30.50 _reflns_number_total 4513 _reflns_number_gt 3660 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1999)' _computing_publication_material WinGX _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^ > 2\s(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^)+(0.0370P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4513 _refine_ls_number_parameters 214 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_gt 0.0279 _refine_ls_wR_factor_ref 0.0714 _refine_ls_wR_factor_gt 0.0677 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 0.18929(3) 0.36741(3) 0.32068(2) 0.02734(7) Uani 1 1 d . . . Cu2 Cu 0.14263(3) 0.09736(3) 0.44589(2) 0.02466(7) Uani 1 1 d . . . Cu3 Cu 0.5000 0.0000 0.5000 0.02559(8) Uani 1 2 d S . . N1 N 0.1918(2) 0.3395(2) 0.13285(16) 0.0328(4) Uani 1 1 d . . . N2 N 0.4412(2) 0.3248(2) 0.30563(17) 0.0346(4) Uani 1 1 d . . . H2A H 0.5072 0.4009 0.3696 0.042 Uiso 1 1 calc R . . H2B H 0.4557 0.2352 0.3131 0.042 Uiso 1 1 calc R . . N3 N 0.2261(2) 0.4166(2) 0.50974(16) 0.0314(4) Uani 1 1 d . . . N4 N 0.13256(19) 0.48673(18) 0.58731(15) 0.0247(3) Uani 1 1 d . . . N5 N 0.0476(2) 0.5545(2) 0.67111(17) 0.0347(4) Uani 1 1 d . . . N6 N 0.0465(2) 0.1202(2) 0.29388(17) 0.0324(4) Uani 1 1 d . . . N7 N -0.1069(2) 0.0910(2) 0.25843(16) 0.0316(4) Uani 1 1 d . . . N8 N -0.2513(3) 0.0646(3) 0.2198(2) 0.0538(6) Uani 1 1 d . . . N9 N -0.0456(2) 0.1675(2) 0.56393(17) 0.0324(4) Uani 1 1 d . . . N10 N -0.1731(2) 0.22855(19) 0.55194(17) 0.0288(3) Uani 1 1 d . . . N11 N -0.2989(3) 0.2846(3) 0.5464(2) 0.0511(5) Uani 1 1 d . . . N12 N 0.3567(2) 0.0079(2) 0.35385(15) 0.0292(4) Uani 1 1 d . . . N13 N 0.3488(2) -0.0756(2) 0.24009(17) 0.0332(4) Uani 1 1 d . . . N14 N 0.3392(3) -0.1493(3) 0.1335(2) 0.0651(7) Uani 1 1 d . . . N15 N 0.3121(2) 0.1192(2) 0.59305(16) 0.0294(4) Uani 1 1 d . . . N16 N 0.3108(2) 0.2225(2) 0.69711(18) 0.0345(4) Uani 1 1 d . . . N17 N 0.3048(4) 0.3213(3) 0.7950(2) 0.0692(7) Uani 1 1 d . . . C1 C 0.3485(3) 0.2546(4) 0.0849(2) 0.0571(7) Uani 1 1 d . . . H1A H 0.3210 0.1457 0.0647 0.069 Uiso 1 1 calc R . . H1B H 0.3795 0.2645 0.0065 0.069 Uiso 1 1 calc R . . C2 C 0.4984(3) 0.3150(4) 0.1811(2) 0.0524(7) Uani 1 1 d . . . H2C H 0.5918 0.2469 0.1549 0.063 Uiso 1 1 calc R . . H2D H 0.5426 0.4165 0.1883 0.063 Uiso 1 1 calc R . . C3 C 0.2071(4) 0.4926(3) 0.1283(3) 0.0579(7) Uani 1 1 d . . . H3A H 0.3076 0.5532 0.1818 0.087 Uiso 1 1 calc R . . H3B H 0.1037 0.5438 0.1588 0.087 Uiso 1 1 calc R . . H3C H 0.2200 0.4808 0.0413 0.087 Uiso 1 1 calc R . . C4 C 0.0376(3) 0.2482(4) 0.0513(2) 0.0581(7) Uani 1 1 d . . . H4A H 0.0269 0.1479 0.0537 0.087 Uiso 1 1 calc R . . H4B H 0.0502 0.2370 -0.0355 0.087 Uiso 1 1 calc R . . H4C H -0.0654 0.2999 0.0825 0.087 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02219(12) 0.03623(15) 0.02546(13) 0.01348(10) 0.00353(9) 0.00773(9) Cu2 0.01647(11) 0.03265(14) 0.02758(13) 0.01415(10) 0.00192(8) 0.00771(9) Cu3 0.01617(14) 0.0387(2) 0.02427(16) 0.01418(14) 0.00120(11) 0.00935(13) N1 0.0288(8) 0.0439(11) 0.0280(9) 0.0158(8) 0.0047(7) 0.0091(7) N2 0.0233(8) 0.0451(11) 0.0355(10) 0.0157(8) 0.0028(7) 0.0060(7) N3 0.0265(8) 0.0402(10) 0.0288(9) 0.0142(8) 0.0033(7) 0.0094(7) N4 0.0197(7) 0.0281(8) 0.0278(8) 0.0133(7) -0.0045(6) 0.0020(6) N5 0.0307(9) 0.0428(11) 0.0293(9) 0.0116(8) 0.0025(7) 0.0133(8) N6 0.0236(8) 0.0433(11) 0.0375(10) 0.0236(8) -0.0033(7) 0.0074(7) N7 0.0314(9) 0.0345(10) 0.0327(9) 0.0177(8) -0.0036(7) 0.0040(7) N8 0.0343(11) 0.0690(15) 0.0650(15) 0.0376(12) -0.0156(10) -0.0078(10) N9 0.0203(8) 0.0398(10) 0.0406(10) 0.0188(8) 0.0074(7) 0.0089(7) N10 0.0216(7) 0.0276(9) 0.0370(9) 0.0127(7) 0.0044(7) 0.0025(6) N11 0.0335(10) 0.0588(14) 0.0697(15) 0.0323(12) 0.0087(10) 0.0202(10) N12 0.0213(7) 0.0444(10) 0.0242(8) 0.0146(7) 0.0027(6) 0.0134(7) N13 0.0228(8) 0.0444(11) 0.0336(10) 0.0162(8) 0.0015(7) 0.0086(7) N14 0.0532(14) 0.0874(19) 0.0349(12) 0.0030(12) -0.0006(10) 0.0158(13) N15 0.0204(7) 0.0398(10) 0.0258(8) 0.0098(7) 0.0002(6) 0.0108(7) N16 0.0316(9) 0.0406(11) 0.0331(10) 0.0164(8) 0.0002(7) 0.0084(8) N17 0.0905(19) 0.0641(17) 0.0363(13) 0.0009(12) -0.0005(12) 0.0239(14) C1 0.0534(15) 0.085(2) 0.0375(13) 0.0246(14) 0.0144(11) 0.0334(15) C2 0.0339(12) 0.087(2) 0.0549(16) 0.0443(15) 0.0174(11) 0.0243(13) C3 0.082(2) 0.0552(17) 0.0484(15) 0.0312(13) 0.0146(14) 0.0157(15) C4 0.0526(16) 0.078(2) 0.0321(13) 0.0130(13) -0.0049(11) -0.0103(14) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N5 1.9991(17) 2_566 ? Cu1 N2 2.0005(16) . ? Cu1 N3 2.0147(17) . ? Cu1 N1 2.0465(17) . ? Cu1 N6 2.4185(18) . ? Cu2 N6 1.9527(16) . ? Cu2 N9 1.9700(16) . ? Cu2 N15 2.0165(16) . ? Cu2 N12 2.0268(15) . ? Cu3 N15 1.9602(15) 2_656 ? Cu3 N15 1.9602(15) . ? Cu3 N12 1.9901(16) 2_656 ? Cu3 N12 1.9901(16) . ? N1 C4 1.467(3) . ? N1 C3 1.470(3) . ? N1 C1 1.488(3) . ? N2 C2 1.467(3) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N3 N4 1.172(2) . ? N4 N5 1.164(2) . ? N5 Cu1 1.9991(17) 2_566 ? N6 N7 1.208(2) . ? N7 N8 1.150(2) . ? N9 N10 1.200(2) . ? N10 N11 1.144(2) . ? N12 N13 1.213(2) . ? N13 N14 1.127(3) . ? N15 N16 1.197(2) . ? N16 N17 1.136(3) . ? C1 C2 1.473(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2C 0.9700 . ? C2 H2D 0.9700 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 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 N5 Cu1 N2 168.93(8) 2_566 . ? N5 Cu1 N3 96.30(7) 2_566 . ? N2 Cu1 N3 87.58(7) . . ? N5 Cu1 N1 89.42(7) 2_566 . ? N2 Cu1 N1 85.40(7) . . ? N3 Cu1 N1 170.20(7) . . ? N5 Cu1 N6 88.06(7) 2_566 . ? N2 Cu1 N6 102.49(7) . . ? N3 Cu1 N6 87.78(6) . . ? N1 Cu1 N6 100.40(7) . . ? N6 Cu2 N9 101.56(7) . . ? N6 Cu2 N15 159.79(7) . . ? N9 Cu2 N15 90.89(7) . . ? N6 Cu2 N12 91.03(7) . . ? N9 Cu2 N12 167.11(7) . . ? N15 Cu2 N12 77.81(6) . . ? N15 Cu3 N15 180.00(10) 2_656 . ? N15 Cu3 N12 80.00(6) 2_656 2_656 ? N15 Cu3 N12 100.00(6) . 2_656 ? N15 Cu3 N12 100.00(6) 2_656 . ? N15 Cu3 N12 80.00(6) . . ? N12 Cu3 N12 180.0 2_656 . ? C4 N1 C3 109.0(2) . . ? C4 N1 C1 108.3(2) . . ? C3 N1 C1 111.5(2) . . ? C4 N1 Cu1 114.35(14) . . ? C3 N1 Cu1 108.98(14) . . ? C1 N1 Cu1 104.63(14) . . ? C2 N2 Cu1 110.28(13) . . ? C2 N2 H2A 109.6 . . ? Cu1 N2 H2A 109.6 . . ? C2 N2 H2B 109.6 . . ? Cu1 N2 H2B 109.6 . . ? H2A N2 H2B 108.1 . . ? N4 N3 Cu1 124.09(14) . . ? N5 N4 N3 174.87(19) . . ? N4 N5 Cu1 133.97(15) . 2_566 ? N7 N6 Cu2 122.53(14) . . ? N7 N6 Cu1 119.03(14) . . ? Cu2 N6 Cu1 101.58(7) . . ? N8 N7 N6 176.8(2) . . ? N10 N9 Cu2 128.67(15) . . ? N11 N10 N9 175.7(2) . . ? N13 N12 Cu3 130.20(14) . . ? N13 N12 Cu2 122.23(13) . . ? Cu3 N12 Cu2 99.64(7) . . ? N14 N13 N12 177.7(2) . . ? N16 N15 Cu3 132.20(14) . . ? N16 N15 Cu2 121.99(13) . . ? Cu3 N15 Cu2 101.02(7) . . ? N17 N16 N15 178.0(2) . . ? C2 C1 N1 111.3(2) . . ? C2 C1 H1A 109.4 . . ? N1 C1 H1A 109.4 . . ? C2 C1 H1B 109.4 . . ? N1 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? N2 C2 C1 108.95(19) . . ? N2 C2 H2C 109.9 . . ? C1 C2 H2C 109.9 . . ? N2 C2 H2D 109.9 . . ? C1 C2 H2D 109.9 . . ? H2C C2 H2D 108.3 . . ? N1 C3 H3A 109.5 . . ? N1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 30.50 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.645 _refine_diff_density_min -0.389 _refine_diff_density_rms 0.076 #===END data_complex4 _database_code_depnum_ccdc_archive 'CCDC 842482' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H60 Cu5 N40' _chemical_formula_sum 'C20 H60 Cu5 N40' _chemical_formula_weight 1178.78 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 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' 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 35.781(5) _cell_length_b 9.4505(13) _cell_length_c 15.367(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.974(3) _cell_angle_gamma 90.00 _cell_volume 4883.7(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4990 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 26.4 _exptl_crystal_description rectangular _exptl_crystal_colour green _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2420 _exptl_absorpt_coefficient_mu 2.207 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5030 _exptl_absorpt_correction_T_max 0.6194 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25594 _diffrn_reflns_av_R_equivalents 0.0833 _diffrn_reflns_av_sigmaI/netI 0.0690 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 26.37 _reflns_number_total 4990 _reflns_number_gt 3137 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1999)' _computing_publication_material WinGX _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^ > 2\s(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^)+(0.0441P)^2^+1.3205P] 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 4990 _refine_ls_number_parameters 294 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1002 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1176 _refine_ls_wR_factor_gt 0.0983 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 0.705063(16) 0.71195(6) 0.51691(4) 0.03944(18) Uani 1 1 d . . . Cu2 Cu 0.588503(16) 0.82507(6) 0.20547(4) 0.04194(19) Uani 1 1 d . . . Cu3 Cu 0.5000 0.74304(9) 0.2500 0.0529(3) Uani 1 2 d S . . N1 N 0.69758(11) 0.6602(4) 0.6382(2) 0.0415(10) Uani 1 1 d . . . H1 H 0.6709 0.6533 0.6256 0.050 Uiso 1 1 calc R . . N2 N 0.71948(11) 0.5048(4) 0.5138(2) 0.0423(10) Uani 1 1 d . . . H2 H 0.7465 0.5007 0.5392 0.051 Uiso 1 1 calc R . . N3 N 0.71828(11) 0.7543(4) 0.4032(3) 0.0426(10) Uani 1 1 d . . . N4 N 0.69312(12) 0.7713(4) 0.3291(3) 0.0406(10) Uani 1 1 d . . . N5 N 0.67010(14) 0.7875(5) 0.2565(3) 0.0697(14) Uani 1 1 d . . . N6 N 0.68800(14) 0.9078(5) 0.5272(3) 0.0647(13) Uani 1 1 d . . . N7 N 0.68475(12) 0.9931(5) 0.4689(3) 0.0517(11) Uani 1 1 d . . . N8 N 0.68206(15) 1.0774(5) 0.4122(4) 0.0779(16) Uani 1 1 d . . . N9 N 0.63157(14) 0.6358(6) 0.4361(3) 0.0790(16) Uani 1 1 d . . . N10 N 0.61082(13) 0.7162(5) 0.3845(3) 0.0561(12) Uani 1 1 d . . . N11 N 0.58905(15) 0.7967(5) 0.3345(3) 0.0725(15) Uani 1 1 d . . . N12 N 0.58679(12) 0.8683(4) 0.0753(3) 0.0483(10) Uani 1 1 d . . . H12 H 0.5608 0.8643 0.0380 0.058 Uiso 1 1 calc R . . N13 N 0.60442(12) 1.0314(4) 0.2300(3) 0.0535(11) Uani 1 1 d . . . H13 H 0.6305 1.0317 0.2665 0.064 Uiso 1 1 calc R . . N14 N 0.57810(12) 0.6202(5) 0.1765(3) 0.0653(13) Uani 1 1 d . . . N15 N 0.60283(13) 0.5348(5) 0.1832(3) 0.0568(12) Uani 1 1 d . . . N16 N 0.62636(16) 0.4489(5) 0.1891(4) 0.0930(18) Uani 1 1 d . . . N17 N 0.51418(12) 0.8761(5) 0.1681(3) 0.0530(11) Uani 1 1 d . . . N18 N 0.49841(11) 0.9830(5) 0.1350(3) 0.0503(11) Uani 1 1 d . . . N19 N 0.48451(14) 1.0880(6) 0.0999(4) 0.0849(17) Uani 1 1 d . . . N20 N 0.50448(15) 0.5858(5) 0.3415(5) 0.098(2) Uani 1 1 d . . . H20 H 0.4796 0.5755 0.3442 0.117 Uiso 1 1 calc R . . C1 C 0.71374(15) 0.5181(5) 0.6650(3) 0.0531(14) Uani 1 1 d . . . H1A H 0.7020 0.4762 0.7073 0.064 Uiso 1 1 calc R . . H1B H 0.7423 0.5230 0.6959 0.064 Uiso 1 1 calc R . . C2 C 0.70419(14) 0.4301(5) 0.5791(3) 0.0490(13) Uani 1 1 d . . . H2A H 0.7166 0.3378 0.5939 0.059 Uiso 1 1 calc R . . H2B H 0.6757 0.4170 0.5516 0.059 Uiso 1 1 calc R . . C3 C 0.71232(16) 0.7618(6) 0.7153(3) 0.0637(16) Uani 1 1 d . . . H3A H 0.7008 0.8531 0.6955 0.096 Uiso 1 1 calc R . . H3B H 0.7408 0.7683 0.7339 0.096 Uiso 1 1 calc R . . H3C H 0.7050 0.7301 0.7666 0.096 Uiso 1 1 calc R . . C4 C 0.70915(19) 0.4326(6) 0.4242(4) 0.0763(19) Uani 1 1 d . . . H4A H 0.7200 0.4840 0.3846 0.114 Uiso 1 1 calc R . . H4B H 0.6807 0.4279 0.3960 0.114 Uiso 1 1 calc R . . H4C H 0.7199 0.3385 0.4334 0.114 Uiso 1 1 calc R . . C5 C 0.5997(3) 1.0126(8) 0.0740(5) 0.127(3) Uani 1 1 d . . . H5A H 0.6255 1.0099 0.0664 0.152 Uiso 1 1 calc R . . H5B H 0.5815 1.0574 0.0191 0.152 Uiso 1 1 calc R . . C6 C 0.6027(3) 1.0918(7) 0.1415(5) 0.157(5) Uani 1 1 d . . . H6A H 0.5803 1.1563 0.1223 0.189 Uiso 1 1 calc R . . H6B H 0.6265 1.1485 0.1526 0.189 Uiso 1 1 calc R . . C7 C 0.60901(19) 0.7740(8) 0.0352(4) 0.097(2) Uani 1 1 d . . . H7A H 0.5999 0.6786 0.0357 0.146 Uiso 1 1 calc R . . H7B H 0.6368 0.7793 0.0710 0.146 Uiso 1 1 calc R . . H7C H 0.6049 0.8022 -0.0274 0.146 Uiso 1 1 calc R . . C8 C 0.58388(17) 1.1201(6) 0.2764(4) 0.0802(19) Uani 1 1 d . . . H8A H 0.5861 1.0791 0.3351 0.120 Uiso 1 1 calc R . . H8B H 0.5563 1.1272 0.2388 0.120 Uiso 1 1 calc R . . H8C H 0.5956 1.2128 0.2859 0.120 Uiso 1 1 calc R . . C9 C 0.5121(4) 0.4542(7) 0.2977(9) 0.203(12) Uani 1 1 d . . . H9A H 0.5399 0.4490 0.3037 0.244 Uiso 1 1 calc R . . H9B H 0.5058 0.3724 0.3283 0.244 Uiso 1 1 calc R . . C10 C 0.5306(2) 0.6088(10) 0.4383(6) 0.155(5) Uani 1 1 d . . . H10A H 0.5232 0.6951 0.4611 0.232 Uiso 1 1 calc R . . H10B H 0.5578 0.6152 0.4408 0.232 Uiso 1 1 calc R . . H10C H 0.5279 0.5311 0.4759 0.232 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0447(4) 0.0388(3) 0.0381(3) 0.0058(2) 0.0182(3) 0.0006(3) Cu2 0.0422(4) 0.0407(4) 0.0460(4) 0.0064(3) 0.0190(3) 0.0048(3) Cu3 0.0554(6) 0.0348(5) 0.0789(7) 0.000 0.0365(5) 0.000 N1 0.036(2) 0.047(2) 0.043(2) 0.0034(19) 0.0155(19) -0.0023(18) N2 0.045(2) 0.045(2) 0.039(2) -0.0003(18) 0.0164(19) -0.0072(19) N3 0.038(2) 0.051(3) 0.040(2) 0.0094(19) 0.013(2) -0.0037(19) N4 0.042(2) 0.040(2) 0.043(3) 0.004(2) 0.019(2) 0.0026(19) N5 0.067(3) 0.092(4) 0.040(3) 0.008(3) 0.004(3) 0.020(3) N6 0.085(4) 0.055(3) 0.068(3) 0.021(3) 0.044(3) 0.027(3) N7 0.046(3) 0.040(3) 0.072(3) -0.001(2) 0.024(2) 0.004(2) N8 0.102(4) 0.043(3) 0.088(4) 0.015(3) 0.032(3) -0.001(3) N9 0.055(3) 0.100(4) 0.071(4) 0.035(3) 0.006(3) 0.005(3) N10 0.045(3) 0.073(3) 0.054(3) 0.012(3) 0.021(2) 0.001(2) N11 0.073(3) 0.091(4) 0.066(3) 0.037(3) 0.039(3) 0.041(3) N12 0.047(3) 0.054(3) 0.042(2) 0.000(2) 0.014(2) 0.000(2) N13 0.058(3) 0.050(3) 0.053(3) -0.003(2) 0.019(2) 0.001(2) N14 0.039(3) 0.046(3) 0.113(4) -0.006(3) 0.029(3) 0.002(2) N15 0.045(3) 0.043(3) 0.088(4) -0.004(2) 0.031(3) -0.008(2) N16 0.074(4) 0.049(3) 0.163(6) -0.006(3) 0.050(4) 0.011(3) N17 0.044(3) 0.058(3) 0.059(3) 0.012(2) 0.021(2) 0.009(2) N18 0.033(2) 0.069(3) 0.047(3) 0.002(2) 0.011(2) 0.000(2) N19 0.061(3) 0.081(4) 0.098(4) 0.028(3) 0.009(3) 0.020(3) N20 0.053(3) 0.066(4) 0.196(7) 0.064(4) 0.071(4) 0.022(3) C1 0.059(3) 0.056(3) 0.048(3) 0.019(3) 0.024(3) 0.007(3) C2 0.046(3) 0.042(3) 0.060(3) 0.010(2) 0.018(3) -0.006(2) C3 0.082(4) 0.068(4) 0.046(3) -0.004(3) 0.029(3) -0.005(3) C4 0.121(5) 0.054(4) 0.051(4) -0.015(3) 0.026(4) -0.011(3) C5 0.217(10) 0.110(7) 0.061(5) 0.003(4) 0.057(6) -0.068(7) C6 0.358(15) 0.055(5) 0.096(6) -0.003(4) 0.126(8) -0.061(7) C7 0.088(5) 0.154(7) 0.055(4) 0.008(4) 0.031(4) 0.054(5) C8 0.077(4) 0.067(4) 0.092(5) -0.026(4) 0.023(4) 0.007(3) C9 0.187(19) 0.050(4) 0.47(4) 0.095(9) 0.24(2) 0.050(7) C10 0.052(5) 0.203(10) 0.204(10) 0.155(8) 0.035(6) 0.022(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N6 1.972(4) . ? Cu1 N3 2.000(4) . ? Cu1 N2 2.029(4) . ? Cu1 N1 2.032(4) . ? Cu2 N14 1.993(4) . ? Cu2 N11 1.994(5) . ? Cu2 N12 2.022(4) . ? Cu2 N13 2.030(4) . ? Cu3 N17 1.965(4) 2_655 ? Cu3 N17 1.965(4) . ? Cu3 N20 2.015(5) 2_655 ? Cu3 N20 2.015(5) . ? N1 C1 1.465(6) . ? N1 C3 1.475(6) . ? N2 C4 1.467(6) . ? N2 C2 1.476(5) . ? N3 N4 1.197(5) . ? N4 N5 1.147(5) . ? N6 N7 1.181(5) . ? N7 N8 1.161(5) . ? N9 N10 1.164(6) . ? N10 N11 1.169(6) . ? N12 C5 1.443(7) . ? N12 C7 1.463(6) . ? N13 C8 1.452(6) . ? N13 C6 1.457(7) . ? N14 N15 1.176(5) . ? N15 N16 1.151(6) . ? N17 N18 1.183(5) . ? N18 N19 1.158(6) . ? N20 C10 1.478(10) . ? N20 C9 1.483(11) . ? C1 C2 1.498(6) . ? C5 C6 1.254(8) . ? C9 C9 1.42(2) 2_655 ? 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 N6 Cu1 N3 93.13(17) . . ? N6 Cu1 N2 174.52(16) . . ? N3 Cu1 N2 91.98(15) . . ? N6 Cu1 N1 90.61(17) . . ? N3 Cu1 N1 173.88(15) . . ? N2 Cu1 N1 84.46(14) . . ? N14 Cu2 N11 91.7(2) . . ? N14 Cu2 N12 92.02(18) . . ? N11 Cu2 N12 175.91(18) . . ? N14 Cu2 N13 173.54(17) . . ? N11 Cu2 N13 92.13(19) . . ? N12 Cu2 N13 84.37(16) . . ? N17 Cu3 N17 100.4(3) 2_655 . ? N17 Cu3 N20 160.59(17) 2_655 2_655 ? N17 Cu3 N20 90.1(2) . 2_655 ? N17 Cu3 N20 90.1(2) 2_655 . ? N17 Cu3 N20 160.59(17) . . ? N20 Cu3 N20 84.9(4) 2_655 . ? C1 N1 C3 111.9(4) . . ? C1 N1 Cu1 108.4(3) . . ? C3 N1 Cu1 117.2(3) . . ? C4 N2 C2 112.5(4) . . ? C4 N2 Cu1 119.1(3) . . ? C2 N2 Cu1 106.8(3) . . ? N4 N3 Cu1 122.2(3) . . ? N5 N4 N3 177.5(5) . . ? N7 N6 Cu1 122.2(4) . . ? N8 N7 N6 179.1(6) . . ? N9 N10 N11 177.5(5) . . ? N10 N11 Cu2 121.2(4) . . ? C5 N12 C7 110.3(5) . . ? C5 N12 Cu2 107.6(3) . . ? C7 N12 Cu2 117.2(3) . . ? C8 N13 C6 111.4(5) . . ? C8 N13 Cu2 119.3(3) . . ? C6 N13 Cu2 106.4(4) . . ? N15 N14 Cu2 124.7(4) . . ? N16 N15 N14 178.4(6) . . ? N18 N17 Cu3 129.2(3) . . ? N19 N18 N17 176.0(5) . . ? C10 N20 C9 115.4(7) . . ? C10 N20 Cu3 117.8(5) . . ? C9 N20 Cu3 106.5(6) . . ? N1 C1 C2 108.2(4) . . ? N2 C2 C1 107.9(4) . . ? C6 C5 N12 119.3(6) . . ? C5 C6 N13 120.2(6) . . ? C9 C9 N20 109.1(9) 2_655 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.412 _refine_diff_density_min -0.383 _refine_diff_density_rms 0.082 #===END