# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2049 data_CuLCl2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C17 H21 Cl2 Cu N5' _chemical_formula_weight 429.84 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 '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' 'H' 'H' 0.0000 0.0000 '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' 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 7.911(3) _cell_length_b 15.422(5) _cell_length_c 15.161(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.58(3) _cell_angle_gamma 90.00 _cell_volume 1840.8(11) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Green _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 884 _exptl_absorpt_coefficient_mu 1.487 _exptl_absorpt_correction_type 'PSI scans' _exptl_absorpt_correction_T_min 87.8 _exptl_absorpt_correction_T_max 98.9 _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 'Enraf-Nonius CAD4' _diffrn_measurement_method \w-2\q _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 1h _diffrn_standards_decay_% <1 _diffrn_reflns_number 1744 _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 24.97 _reflns_number_total 1620 _reflns_number_observed 1423 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 Software' _computing_cell_refinement 'CAD4 Software' _computing_data_reduction 'MolEN' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0644P)^2^+3.5603P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1620 _refine_ls_number_parameters 115 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_obs 0.0376 _refine_ls_wR_factor_all 0.1113 _refine_ls_wR_factor_obs 0.1041 _refine_ls_goodness_of_fit_all 1.080 _refine_ls_goodness_of_fit_obs 1.082 _refine_ls_restrained_S_all 1.080 _refine_ls_restrained_S_obs 1.082 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu Cu 0.0000 0.11500(3) 0.2500 0.0274(2) Uani 1 d S . Cl Cl 0.20679(11) 0.09648(6) 0.15108(6) 0.0411(3) Uani 1 d . . N1 N 0.0000 0.2569(2) 0.2500 0.0291(8) Uani 1 d S . N2 N 0.1813(3) 0.1101(2) 0.3501(2) 0.0329(6) Uani 1 d . . N4 N 0.2808(3) 0.1808(2) 0.3723(2) 0.0340(6) Uani 1 d . . C1 C 0.1394(4) 0.3011(2) 0.2810(2) 0.0315(7) Uani 1 d . . C2 C 0.1427(5) 0.3910(2) 0.2828(2) 0.0405(8) Uani 1 d . . H2 H 0.2398(5) 0.4203(2) 0.3059(2) 0.049 Uiso 1 calc R . C3 C 0.0000 0.4365(3) 0.2500 0.0458(12) Uani 1 d S . H3 H 0.0000 0.4968(3) 0.2500 0.055 Uiso 1 calc SR . C6 C 0.2976(4) 0.2496(2) 0.3081(2) 0.0379(8) Uani 1 d . . H6A H 0.3368(4) 0.2240(2) 0.2553(2) 0.045 Uiso 1 calc R . H6B H 0.3849(4) 0.2893(2) 0.3326(2) 0.045 Uiso 1 calc R . C7 C 0.3801(4) 0.1657(2) 0.4496(2) 0.0359(7) Uani 1 d . . C8 C 0.3394(4) 0.0845(2) 0.4774(2) 0.0408(8) Uani 1 d . . H8 H 0.3851(4) 0.0567(2) 0.5286(2) 0.049 Uiso 1 calc R . C9 C 0.2163(4) 0.0516(2) 0.4140(2) 0.0355(7) Uani 1 d . . C10 C 0.5083(5) 0.2292(3) 0.4882(3) 0.0502(10) Uani 1 d . . H10A H 0.5042(5) 0.2805(3) 0.4521(3) 0.060 Uiso 1 calc R . H10B H 0.6195(5) 0.2039(3) 0.4903(3) 0.060 Uiso 1 calc R . H10C H 0.4840(5) 0.2442(3) 0.5471(3) 0.060 Uiso 1 calc R . C11 C 0.1348(5) -0.0355(2) 0.4101(2) 0.0463(9) Uani 1 d . . H11A H 0.0547(5) -0.0390(2) 0.3585(2) 0.056 Uiso 1 calc R . H11B H 0.0770(5) -0.0442(2) 0.4622(2) 0.056 Uiso 1 calc R . H11C H 0.2203(5) -0.0793(2) 0.4072(2) 0.056 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0314(3) 0.0274(3) 0.0225(3) 0.000 -0.0029(2) 0.000 Cl 0.0445(5) 0.0439(5) 0.0358(5) 0.0014(3) 0.0079(4) 0.0094(4) N1 0.033(2) 0.026(2) 0.028(2) 0.000 0.0030(15) 0.000 N2 0.0369(15) 0.0330(15) 0.0275(14) 0.0046(11) -0.0036(11) -0.0038(11) N4 0.0304(13) 0.0367(15) 0.0337(15) 0.0013(12) -0.0038(11) -0.0006(11) C1 0.039(2) 0.030(2) 0.025(2) 0.0012(12) 0.0031(13) -0.0044(13) C2 0.051(2) 0.033(2) 0.037(2) -0.0026(14) 0.000(2) -0.0109(14) C3 0.061(3) 0.026(2) 0.048(3) 0.000 -0.004(2) 0.000 C6 0.032(2) 0.037(2) 0.044(2) 0.0039(15) 0.0000(14) -0.0075(14) C7 0.029(2) 0.047(2) 0.031(2) -0.0069(14) -0.0057(13) 0.0077(14) C8 0.044(2) 0.048(2) 0.028(2) 0.0000(15) -0.0073(14) 0.013(2) C9 0.041(2) 0.038(2) 0.027(2) 0.0016(14) 0.0015(13) 0.0065(14) C10 0.036(2) 0.066(3) 0.045(2) -0.015(2) -0.010(2) -0.001(2) C11 0.065(2) 0.034(2) 0.039(2) 0.008(2) 0.001(2) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu N1 2.189(4) . yes Cu N2 1.985(3) . yes Cu N2 1.985(3) 2 yes Cu Cl 2.3418(11) . yes Cu Cl 2.3418(11) 2 yes N1 C1 1.342(4) . ? N1 C1 1.342(4) 2 ? N2 C9 1.333(4) . ? N2 N4 1.368(4) . ? N4 C7 1.365(4) . ? N4 C6 1.455(4) . ? C1 C2 1.386(5) . ? C1 C6 1.505(4) . ? C2 C3 1.380(5) . ? C3 C2 1.380(5) 2 ? C7 C8 1.369(5) . ? C7 C10 1.488(5) . ? C8 C9 1.396(5) . ? C9 C11 1.488(5) . ? 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 Cu N2 92.18(7) . . yes N1 Cu N2 92.18(7) . 2 yes N1 Cu Cl 97.01(3) . . yes N1 Cu Cl 97.01(3) . 2 yes N2 Cu N2 175.65(15) 2 . yes N2 Cu Cl 90.21(9) 2 . yes N2 Cu Cl 89.26(9) . . yes N2 Cu Cl 89.26(9) 2 2 yes N2 Cu Cl 90.21(9) . 2 yes Cl Cu Cl 165.99(5) . 2 yes C1 N1 C1 119.0(4) . 2 ? C1 N1 Cu 120.5(2) . . ? C1 N1 Cu 120.5(2) 2 . ? C9 N2 N4 106.6(3) . . ? C9 N2 Cu 131.7(2) . . ? N4 N2 Cu 121.0(2) . . ? C7 N4 N2 110.2(3) . . ? C7 N4 C6 128.0(3) . . ? N2 N4 C6 120.2(3) . . ? N1 C1 C2 121.9(3) . . ? N1 C1 C6 117.4(3) . . ? C2 C1 C6 120.6(3) . . ? C3 C2 C1 119.2(3) . . ? C2 C3 C2 118.9(4) 2 . ? N4 C6 C1 116.2(3) . . ? N4 C7 C8 106.6(3) . . ? N4 C7 C10 122.6(3) . . ? C8 C7 C10 130.7(3) . . ? C7 C8 C9 106.9(3) . . ? N2 C9 C8 109.7(3) . . ? N2 C9 C11 121.5(3) . . ? C8 C9 C11 128.8(3) . . ? _refine_diff_density_max 0.555 _refine_diff_density_min -0.637 _refine_diff_density_rms 0.087 #===END data_CuLBr2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C17 H21 Br2 Cu N5' _chemical_formula_weight 518.74 _chemical_melting_point ? _chemical_compound_source ? 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' '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' 'N' 'N' 0.0061 0.0033 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/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 7.8585(11) _cell_length_b 15.843(8) _cell_length_c 15.4787(13) _cell_angle_alpha 90.00 _cell_angle_beta 97.401(9) _cell_angle_gamma 90.00 _cell_volume 1911.1(10) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Green _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.803 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1028 _exptl_absorpt_coefficient_mu 5.334 _exptl_absorpt_correction_type 'PSI Scans' _exptl_absorpt_correction_T_min 47.90 _exptl_absorpt_correction_T_max 99.92 _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 'Enraf-Nonius CAD4' _diffrn_measurement_method \w-2\q _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 1h _diffrn_standards_decay_% <1 _diffrn_reflns_number 1825 _diffrn_reflns_av_R_equivalents 0.0134 _diffrn_reflns_av_sigmaI/netI 0.0169 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 24.97 _reflns_number_total 1693 _reflns_number_observed 1430 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 Software' _computing_cell_refinement 'CAD4 Software' _computing_data_reduction 'MolEN' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0444P)^2^+4.4150P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1693 _refine_ls_number_parameters 115 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0417 _refine_ls_R_factor_obs 0.0304 _refine_ls_wR_factor_all 0.0873 _refine_ls_wR_factor_obs 0.0768 _refine_ls_goodness_of_fit_all 1.158 _refine_ls_goodness_of_fit_obs 1.115 _refine_ls_restrained_S_all 1.158 _refine_ls_restrained_S_obs 1.115 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu Cu 0.0000 0.11696(4) 0.7500 0.0291(2) Uani 1 d S . Br Br 0.22292(5) 0.09814(3) 0.64878(3) 0.0437(2) Uani 1 d . . N1 N 0.0000 0.2546(3) 0.7500 0.0319(9) Uani 1 d S . N2 N 0.1825(4) 0.1110(2) 0.8496(2) 0.0348(7) Uani 1 d . . N4 N 0.2810(4) 0.1799(2) 0.8752(2) 0.0352(7) Uani 1 d . . C1 C 0.1402(5) 0.2973(2) 0.7831(2) 0.0349(8) Uani 1 d . . C2 C 0.1430(6) 0.3845(3) 0.7854(3) 0.0468(10) Uani 1 d . . H2 H 0.2404(6) 0.4131(3) 0.8104(3) 0.056 Uiso 1 calc R . C3 C 0.0000 0.4284(4) 0.7500 0.055(2) Uani 1 d S . H3 H 0.0000 0.4871(4) 0.7500 0.067 Uiso 1 calc SR . C6 C 0.3002(5) 0.2479(3) 0.8142(3) 0.0415(9) Uani 1 d . . H6A H 0.3441(5) 0.2242(3) 0.7637(3) 0.050 Uiso 1 calc R . H6B H 0.3860(5) 0.2869(3) 0.8415(3) 0.050 Uiso 1 calc R . C7 C 0.3802(5) 0.1646(3) 0.9523(2) 0.0390(9) Uani 1 d . . C8 C 0.3399(5) 0.0848(3) 0.9775(3) 0.0447(10) Uani 1 d . . H8 H 0.3848(5) 0.0571(3) 1.0284(3) 0.054 Uiso 1 calc R . C9 C 0.2183(5) 0.0532(2) 0.9118(2) 0.0380(9) Uani 1 d . . C10 C 0.5064(5) 0.2265(3) 0.9947(3) 0.0530(11) Uani 1 d . . H10A H 0.5030(5) 0.2769(3) 0.9601(3) 0.064 Uiso 1 calc R . H10B H 0.6194(5) 0.2026(3) 0.9999(3) 0.064 Uiso 1 calc R . H10C H 0.4782(5) 0.2401(3) 1.0516(3) 0.064 Uiso 1 calc R . C11 C 0.1379(6) -0.0321(3) 0.9051(3) 0.0515(11) Uani 1 d . . H11A H 0.0587(6) -0.0356(3) 0.8526(3) 0.062 Uiso 1 calc R . H11B H 0.0779(6) -0.0415(3) 0.9545(3) 0.062 Uiso 1 calc R . H11C H 0.2255(6) -0.0742(3) 0.9040(3) 0.062 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0323(3) 0.0290(3) 0.0248(3) 0.000 -0.0010(2) 0.000 Br 0.0480(3) 0.0442(3) 0.0407(3) 0.0025(2) 0.0123(2) 0.0094(2) N1 0.034(2) 0.027(2) 0.034(2) 0.000 0.003(2) 0.000 N2 0.035(2) 0.037(2) 0.031(2) 0.0019(13) 0.0005(13) -0.0051(13) N4 0.031(2) 0.039(2) 0.035(2) 0.0004(14) -0.0018(13) -0.0010(13) C1 0.043(2) 0.030(2) 0.033(2) 0.003(2) 0.007(2) -0.002(2) C2 0.058(3) 0.033(2) 0.047(2) -0.002(2) 0.001(2) -0.011(2) C3 0.072(4) 0.025(3) 0.066(4) 0.000 -0.002(3) 0.000 C6 0.030(2) 0.041(2) 0.051(2) 0.002(2) 0.000(2) -0.006(2) C7 0.028(2) 0.054(2) 0.033(2) -0.009(2) -0.002(2) 0.008(2) C8 0.046(2) 0.057(3) 0.028(2) 0.001(2) -0.003(2) 0.014(2) C9 0.042(2) 0.042(2) 0.030(2) 0.001(2) 0.004(2) 0.009(2) C10 0.038(2) 0.068(3) 0.050(3) -0.017(2) -0.007(2) 0.003(2) C11 0.068(3) 0.040(2) 0.046(3) 0.011(2) 0.003(2) 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu N1 2.181(4) . yes Cu N2 1.968(3) . yes Cu N2 1.968(3) 2_556 yes Cu Br 2.5139(5) . yes Cu Br 2.5139(5) 2_556 yes N1 C1 1.338(4) . ? N1 C1 1.338(4) 2_556 ? N2 C9 1.332(5) . ? N2 N4 1.367(4) . ? N4 C7 1.361(5) . ? N4 C6 1.453(5) . ? C1 C2 1.382(5) . ? C1 C6 1.507(5) . ? C2 C3 1.374(5) . ? C2 H2 0.93 . ? C3 C2 1.374(5) 2_556 ? C3 H3 0.93 . ? C6 H6A 0.97 . ? C6 H6B 0.97 . ? C7 C8 1.372(6) . ? C7 C10 1.487(6) . ? C8 C9 1.395(6) . ? C8 H8 0.93 . ? C9 C11 1.491(6) . ? C10 H10A 0.96 . ? C10 H10B 0.96 . ? C10 H10C 0.96 . ? C11 H11A 0.96 . ? C11 H11B 0.96 . ? C11 H11C 0.96 . ? 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 Cu N2 92.76(9) . 2_556 yes N1 Cu N2 92.76(9) . . yes N1 Cu Br 96.81(2) . . yes N1 Cu Br 96.81(2) . 2_556 yes N2 Cu N2 174.5(2) 2_556 . yes N2 Cu Br 89.21(9) . . yes N2 Cu Br 90.14(9) 2_556 . yes N2 Cu Br 89.21(9) 2_556 2_556 yes N2 Cu Br 90.14(9) . 2_556 yes Br Cu Br 166.38(3) . 2_556 yes C1 N1 C1 119.2(4) . 2_556 ? C1 N1 Cu 120.4(2) . . ? C1 N1 Cu 120.4(2) 2_556 . ? C9 N2 N4 106.3(3) . . ? C9 N2 Cu 131.6(3) . . ? N4 N2 Cu 121.1(2) . . ? C7 N4 N2 110.5(3) . . ? C7 N4 C6 127.3(3) . . ? N2 N4 C6 120.4(3) . . ? N1 C1 C2 121.7(4) . . ? N1 C1 C6 118.2(3) . . ? C2 C1 C6 120.1(4) . . ? C3 C2 C1 119.1(4) . . ? C3 C2 H2 120.4(3) . . ? C1 C2 H2 120.4(3) . . ? C2 C3 C2 119.2(6) 2_556 . ? C2 C3 H3 120.4(3) 2_556 . ? C2 C3 H3 120.4(3) . . ? N4 C6 C1 116.1(3) . . ? N4 C6 H6A 108.3(2) . . ? C1 C6 H6A 108.3(2) . . ? N4 C6 H6B 108.3(2) . . ? C1 C6 H6B 108.3(2) . . ? H6A C6 H6B 107.4 . . ? N4 C7 C8 106.6(3) . . ? N4 C7 C10 122.9(4) . . ? C8 C7 C10 130.4(4) . . ? C7 C8 C9 106.5(4) . . ? C7 C8 H8 126.7(2) . . ? C9 C8 H8 126.7(2) . . ? N2 C9 C8 110.0(4) . . ? N2 C9 C11 121.7(4) . . ? C8 C9 C11 128.3(4) . . ? C7 C10 H10A 109.5(3) . . ? C7 C10 H10B 109.5(2) . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5(2) . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5(2) . . ? C9 C11 H11B 109.5(2) . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5(2) . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? _refine_diff_density_max 0.467 _refine_diff_density_min -0.583 _refine_diff_density_rms 0.091 #===END data_CuL(NO3)2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C17 H21 Cu N7 O6' _chemical_formula_weight 482.95 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cu' 'Cu' 0.3201 1.2651 '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' 'C' 'C' 0.0033 0.0016 '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' 'H' 'H' 0.0000 0.0000 '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/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.119(7) _cell_length_b 10.541(3) _cell_length_c 17.650(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.74(3) _cell_angle_gamma 90.00 _cell_volume 2067.7(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'Prism' _exptl_crystal_colour Blue _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 996 _exptl_absorpt_coefficient_mu 1.107 _exptl_absorpt_correction_type 'PSI Scans' _exptl_absorpt_correction_T_min 85.6 _exptl_absorpt_correction_T_max 99.7 _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 'Enraf-Nonius CAD4' _diffrn_measurement_method \w-2\q _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 1h _diffrn_standards_decay_% <1 _diffrn_reflns_number 3814 _diffrn_reflns_av_R_equivalents 0.0165 _diffrn_reflns_av_sigmaI/netI 0.0389 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 24.96 _reflns_number_total 3615 _reflns_number_observed 2512 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 Software' _computing_cell_refinement 'CAD4 Software' _computing_data_reduction 'MolEN' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0731P)^2^+2.2071P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3614 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0859 _refine_ls_R_factor_obs 0.0514 _refine_ls_wR_factor_all 0.1546 _refine_ls_wR_factor_obs 0.1226 _refine_ls_goodness_of_fit_all 1.110 _refine_ls_goodness_of_fit_obs 1.073 _refine_ls_restrained_S_all 1.111 _refine_ls_restrained_S_obs 1.073 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu Cu 0.73558(5) 0.19576(5) 0.12812(3) 0.0435(2) Uani 1 d . . O1 O 0.6957(3) 0.3798(3) 0.1235(2) 0.0520(9) Uani 1 d . . O2 O 0.9139(3) 0.2477(4) 0.0739(2) 0.0592(9) Uani 1 d . . O3 O 0.5510(4) 0.3176(5) 0.1944(3) 0.0786(12) Uani 1 d . . O4 O 1.0194(4) 0.0988(4) 0.1255(3) 0.0820(13) Uani 1 d . . O5 O 0.5775(4) 0.5174(4) 0.1713(3) 0.0854(13) Uani 1 d . . O6 O 1.1078(4) 0.2656(4) 0.0849(3) 0.0882(14) Uani 1 d . . N1 N 0.7440(3) 0.0047(4) 0.1429(2) 0.0459(10) Uani 1 d . . N2 N 0.6531(4) 0.1636(4) 0.0265(2) 0.0499(10) Uani 1 d . . N3 N 0.8038(3) 0.2216(4) 0.2336(2) 0.0497(10) Uani 1 d . . N4 N 0.6944(4) 0.0659(4) -0.0162(2) 0.0491(10) Uani 1 d . . N5 N 0.7763(4) 0.1362(4) 0.2880(2) 0.0529(10) Uani 1 d . . N6 N 0.6052(4) 0.4053(5) 0.1649(3) 0.0591(12) Uani 1 d . . N7 N 1.0142(4) 0.2042(5) 0.0957(2) 0.0568(11) Uani 1 d . . C1 C 0.7765(4) -0.0715(5) 0.0852(3) 0.0481(12) Uani 1 d . . C2 C 0.7912(5) -0.1995(5) 0.0935(3) 0.0591(14) Uani 1 d . . H2 H 0.8144(5) -0.2493(5) 0.0529(3) 0.071 Uiso 1 calc R . C3 C 0.7708(6) -0.2535(6) 0.1634(4) 0.073(2) Uani 1 d . . H3 H 0.7795(6) -0.3405(6) 0.1707(4) 0.088 Uiso 1 calc R . C4 C 0.7375(5) -0.1764(6) 0.2219(4) 0.069(2) Uani 1 d . . H4 H 0.7241(5) -0.2111(6) 0.2694(4) 0.083 Uiso 1 calc R . C5 C 0.7240(4) -0.0480(5) 0.2105(3) 0.0519(13) Uani 1 d . . C6 C 0.7975(4) -0.0072(5) 0.0103(3) 0.0505(12) Uani 1 d . . H6A H 0.8667(4) 0.0485(5) 0.0157(3) 0.061 Uiso 1 calc R . H6B H 0.8157(4) -0.0710(5) -0.0273(3) 0.061 Uiso 1 calc R . C7 C 0.6316(5) 0.0553(5) -0.0826(3) 0.0534(13) Uani 1 d . . C8 C 0.5477(5) 0.1486(6) -0.0827(3) 0.0608(14) Uani 1 d . . H8 H 0.4909(5) 0.1653(6) -0.1212(3) 0.073 Uiso 1 calc R . C9 C 0.5615(5) 0.2145(5) -0.0153(3) 0.0548(13) Uani 1 d . . C10 C 0.6592(6) -0.0437(6) -0.1399(3) 0.076(2) Uani 1 d . . H10A H 0.7251(6) -0.0950(6) -0.1214(3) 0.091 Uiso 1 calc R . H10B H 0.6805(6) -0.0035(6) -0.1865(3) 0.091 Uiso 1 calc R . H10C H 0.5897(6) -0.0962(6) -0.1488(3) 0.091 Uiso 1 calc R . C11 C 0.4885(6) 0.3236(6) 0.0099(4) 0.074(2) Uani 1 d . . H11A H 0.5174(6) 0.3512(6) 0.0590(4) 0.089 Uiso 1 calc R . H11B H 0.4058(6) 0.2982(6) 0.0127(4) 0.089 Uiso 1 calc R . H11C H 0.4949(6) 0.3919(6) -0.0257(4) 0.089 Uiso 1 calc R . C12 C 0.6862(5) 0.0399(6) 0.2721(3) 0.0622(15) Uani 1 d . . H12A H 0.6109(5) 0.0805(6) 0.2569(3) 0.075 Uiso 1 calc R . H12B H 0.6728(5) -0.0086(6) 0.3178(3) 0.075 Uiso 1 calc R . C13 C 0.8326(5) 0.1638(6) 0.3543(3) 0.0604(15) Uani 1 d . . C14 C 0.8995(5) 0.2707(6) 0.3419(3) 0.065(2) Uani 1 d . . H14 H 0.9484(5) 0.3126(6) 0.3774(3) 0.078 Uiso 1 calc R . C15 C 0.8809(4) 0.3050(5) 0.2661(3) 0.0535(13) Uani 1 d . . C16 C 0.8196(7) 0.0837(7) 0.4238(3) 0.088(2) Uani 1 d . . H16A H 0.7649(7) 0.0152(7) 0.4127(3) 0.106 Uiso 1 calc R . H16B H 0.7890(7) 0.1347(7) 0.4639(3) 0.106 Uiso 1 calc R . H16C H 0.8967(7) 0.0499(7) 0.4392(3) 0.106 Uiso 1 calc R . C17 C 0.9345(5) 0.4121(6) 0.2250(3) 0.070(2) Uani 1 d . . H17A H 0.9049(5) 0.4120(6) 0.1734(3) 0.084 Uiso 1 calc R . H17B H 1.0205(5) 0.4035(6) 0.2262(3) 0.084 Uiso 1 calc R . H17C H 0.9130(5) 0.4905(6) 0.2488(3) 0.084 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0460(3) 0.0454(3) 0.0388(3) -0.0019(3) -0.0042(2) 0.0001(3) O1 0.050(2) 0.052(2) 0.054(2) -0.005(2) 0.003(2) 0.009(2) O2 0.059(2) 0.064(2) 0.054(2) 0.010(2) 0.000(2) 0.002(2) O3 0.054(2) 0.098(3) 0.084(3) 0.014(3) 0.013(2) -0.005(2) O4 0.075(3) 0.081(3) 0.090(3) 0.030(3) 0.005(2) 0.007(2) O5 0.084(3) 0.074(3) 0.098(3) -0.022(3) 0.002(3) 0.026(2) O6 0.063(3) 0.075(3) 0.127(4) -0.017(3) 0.027(3) -0.014(2) N1 0.044(2) 0.049(2) 0.044(2) 0.002(2) -0.007(2) -0.004(2) N2 0.055(2) 0.051(2) 0.043(2) -0.003(2) -0.011(2) 0.003(2) N3 0.044(2) 0.060(3) 0.045(2) -0.005(2) 0.000(2) -0.005(2) N4 0.063(3) 0.047(2) 0.036(2) -0.005(2) -0.008(2) 0.003(2) N5 0.060(3) 0.061(3) 0.037(2) -0.005(2) 0.000(2) -0.001(2) N6 0.046(3) 0.070(3) 0.061(3) -0.014(3) -0.002(2) 0.008(2) N7 0.060(3) 0.059(3) 0.052(3) -0.007(2) 0.010(2) 0.001(2) C1 0.042(3) 0.050(3) 0.051(3) -0.002(2) -0.015(2) 0.003(2) C2 0.057(3) 0.049(3) 0.071(4) 0.001(3) -0.017(3) 0.005(3) C3 0.073(4) 0.049(3) 0.096(5) 0.014(3) -0.019(4) 0.000(3) C4 0.072(4) 0.069(4) 0.065(4) 0.025(3) -0.010(3) -0.015(3) C5 0.043(3) 0.060(3) 0.052(3) 0.009(3) -0.009(2) -0.015(2) C6 0.054(3) 0.056(3) 0.041(3) -0.009(2) -0.001(2) 0.008(2) C7 0.057(3) 0.061(3) 0.042(3) -0.002(2) -0.009(2) -0.012(3) C8 0.064(4) 0.063(3) 0.053(3) 0.004(3) -0.024(3) -0.003(3) C9 0.056(3) 0.048(3) 0.058(3) 0.007(2) -0.017(3) -0.001(2) C10 0.088(4) 0.090(5) 0.048(3) -0.018(3) -0.014(3) -0.010(4) C11 0.074(4) 0.064(4) 0.084(4) -0.003(3) -0.030(3) 0.019(3) C12 0.057(3) 0.082(4) 0.048(3) 0.006(3) 0.006(2) -0.012(3) C13 0.076(4) 0.064(4) 0.041(3) -0.016(3) -0.007(3) 0.019(3) C14 0.070(4) 0.070(4) 0.055(3) -0.024(3) -0.018(3) 0.014(3) C15 0.047(3) 0.058(3) 0.055(3) -0.016(3) -0.005(2) 0.002(3) C16 0.135(6) 0.087(5) 0.041(3) -0.011(3) -0.014(4) 0.020(4) C17 0.064(4) 0.069(4) 0.075(4) -0.018(3) -0.005(3) -0.011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu N1 2.032(4) . yes Cu N2 2.019(4) . yes Cu N3 2.008(4) . yes Cu O1 1.991(3) . yes Cu O2 2.294(4) . yes O1 N6 1.289(5) . ? O2 N7 1.256(6) . ? O3 N6 1.228(6) . ? O4 N7 1.229(6) . ? O5 N6 1.227(6) . ? O6 N7 1.245(6) . ? N1 C5 1.342(6) . ? N1 C1 1.354(6) . ? N2 C9 1.350(6) . ? N2 N4 1.364(5) . ? N3 C15 1.344(6) . ? N3 N5 1.358(6) . ? N4 C7 1.350(6) . ? N4 C6 1.447(6) . ? N5 C13 1.342(6) . ? N5 C12 1.448(7) . ? C1 C2 1.366(7) . ? C1 C6 1.512(7) . ? C2 C3 1.384(9) . ? C3 C4 1.374(9) . ? C4 C5 1.376(8) . ? C5 C12 1.498(8) . ? C7 C8 1.356(8) . ? C7 C10 1.492(8) . ? C8 C9 1.382(7) . ? C9 C11 1.483(8) . ? C13 C14 1.371(8) . ? C13 C16 1.499(8) . ? C14 C15 1.395(8) . ? C15 C17 1.477(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu N2 88.0(2) . . yes N1 Cu N3 90.0(2) . . yes N1 Cu O1 168.51(15) . . yes N1 Cu O2 104.64(15) . . yes N2 Cu N3 174.7(2) . . yes N2 Cu O1 91.89(15) . . yes N2 Cu O2 92.5(2) . . yes N3 Cu O1 89.0(2) . . yes N3 Cu O2 92.73(15) . . yes O1 Cu O2 86.84(14) . . yes N6 O1 Cu 110.9(3) . . ? N7 O2 Cu 123.7(3) . . ? C5 N1 C1 118.6(4) . . ? C5 N1 Cu 121.1(3) . . ? C1 N1 Cu 120.3(3) . . ? C9 N2 N4 105.1(4) . . ? C9 N2 Cu 137.1(4) . . ? N4 N2 Cu 117.8(3) . . ? C15 N3 N5 106.7(4) . . ? C15 N3 Cu 134.6(4) . . ? N5 N3 Cu 118.6(3) . . ? C7 N4 N2 111.6(4) . . ? C7 N4 C6 128.3(4) . . ? N2 N4 C6 120.0(4) . . ? C13 N5 N3 111.3(4) . . ? C13 N5 C12 128.6(5) . . ? N3 N5 C12 119.8(4) . . ? O5 N6 O3 124.0(5) . . ? O5 N6 O1 117.1(5) . . ? O3 N6 O1 119.0(5) . . ? O4 N7 O6 120.5(5) . . ? O4 N7 O2 119.4(5) . . ? O6 N7 O2 120.1(5) . . ? N1 C1 C2 122.7(5) . . ? N1 C1 C6 116.3(4) . . ? C2 C1 C6 121.0(5) . . ? C1 C2 C3 118.6(6) . . ? C4 C3 C2 118.8(6) . . ? C3 C4 C5 120.2(6) . . ? N1 C5 C4 121.1(5) . . ? N1 C5 C12 116.6(5) . . ? C4 C5 C12 122.3(5) . . ? N4 C6 C1 112.3(4) . . ? N4 C7 C8 106.2(5) . . ? N4 C7 C10 122.4(5) . . ? C8 C7 C10 131.4(5) . . ? C7 C8 C9 107.7(5) . . ? N2 C9 C8 109.4(5) . . ? N2 C9 C11 123.8(5) . . ? C8 C9 C11 126.8(5) . . ? N5 C12 C5 111.5(4) . . ? N5 C13 C14 106.2(5) . . ? N5 C13 C16 122.5(6) . . ? C14 C13 C16 131.3(5) . . ? C13 C14 C15 107.6(5) . . ? N3 C15 C14 108.2(5) . . ? N3 C15 C17 123.6(5) . . ? C14 C15 C17 128.2(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 Cu O1 N6 -73.3(3) . . . . ? N2 Cu O1 N6 101.5(3) . . . . ? N1 Cu O1 N6 12.2(9) . . . . ? O2 Cu O1 N6 -166.1(3) . . . . ? O1 Cu O2 N7 135.6(4) . . . . ? N3 Cu O2 N7 46.7(4) . . . . ? N2 Cu O2 N7 -132.6(4) . . . . ? N1 Cu O2 N7 -44.0(4) . . . . ? O1 Cu N1 C5 -50.3(9) . . . . ? N3 Cu N1 C5 35.0(4) . . . . ? N2 Cu N1 C5 -140.0(4) . . . . ? O2 Cu N1 C5 127.9(3) . . . . ? O1 Cu N1 C1 133.2(7) . . . . ? N3 Cu N1 C1 -141.4(4) . . . . ? N2 Cu N1 C1 43.6(4) . . . . ? O2 Cu N1 C1 -48.6(4) . . . . ? O1 Cu N2 C9 -28.6(5) . . . . ? N3 Cu N2 C9 71.4(20) . . . . ? N1 Cu N2 C9 140.0(5) . . . . ? O2 Cu N2 C9 -115.5(5) . . . . ? O1 Cu N2 N4 151.4(3) . . . . ? N3 Cu N2 N4 -108.7(18) . . . . ? N1 Cu N2 N4 -40.1(4) . . . . ? O2 Cu N2 N4 64.5(4) . . . . ? O1 Cu N3 C15 -48.7(5) . . . . ? N2 Cu N3 C15 -148.8(17) . . . . ? N1 Cu N3 C15 142.8(5) . . . . ? O2 Cu N3 C15 38.1(5) . . . . ? O1 Cu N3 N5 135.7(4) . . . . ? N2 Cu N3 N5 35.6(20) . . . . ? N1 Cu N3 N5 -32.9(4) . . . . ? O2 Cu N3 N5 -137.5(3) . . . . ? C9 N2 N4 C7 0.1(6) . . . . ? Cu N2 N4 C7 -179.8(3) . . . . ? C9 N2 N4 C6 177.3(4) . . . . ? Cu N2 N4 C6 -2.7(6) . . . . ? C15 N3 N5 C13 0.7(6) . . . . ? Cu N3 N5 C13 177.5(3) . . . . ? C15 N3 N5 C12 174.5(4) . . . . ? Cu N3 N5 C12 -8.7(6) . . . . ? Cu O1 N6 O5 174.7(4) . . . . ? Cu O1 N6 O3 -6.4(6) . . . . ? Cu O2 N7 O4 28.5(6) . . . . ? Cu O2 N7 O6 -154.0(4) . . . . ? C5 N1 C1 C2 -0.9(7) . . . . ? Cu N1 C1 C2 175.6(4) . . . . ? C5 N1 C1 C6 179.8(4) . . . . ? Cu N1 C1 C6 -3.7(5) . . . . ? N1 C1 C2 C3 0.7(8) . . . . ? C6 C1 C2 C3 180.0(5) . . . . ? C1 C2 C3 C4 -0.5(8) . . . . ? C2 C3 C4 C5 0.5(9) . . . . ? C1 N1 C5 C4 0.9(7) . . . . ? Cu N1 C5 C4 -175.6(4) . . . . ? C1 N1 C5 C12 -179.0(4) . . . . ? Cu N1 C5 C12 4.5(6) . . . . ? C3 C4 C5 N1 -0.7(8) . . . . ? C3 C4 C5 C12 179.1(5) . . . . ? C7 N4 C6 C1 -123.2(5) . . . . ? N2 N4 C6 C1 60.1(6) . . . . ? N1 C1 C6 N4 -55.6(6) . . . . ? C2 C1 C6 N4 125.1(5) . . . . ? N2 N4 C7 C8 0.0(6) . . . . ? C6 N4 C7 C8 -176.9(5) . . . . ? N2 N4 C7 C10 179.7(5) . . . . ? C6 N4 C7 C10 2.8(8) . . . . ? N4 C7 C8 C9 -0.1(6) . . . . ? C10 C7 C8 C9 -179.7(6) . . . . ? N4 N2 C9 C8 -0.2(6) . . . . ? Cu N2 C9 C8 179.8(4) . . . . ? N4 N2 C9 C11 179.2(5) . . . . ? Cu N2 C9 C11 -0.8(9) . . . . ? C7 C8 C9 N2 0.2(7) . . . . ? C7 C8 C9 C11 -179.2(6) . . . . ? C13 N5 C12 C5 -123.8(6) . . . . ? N3 N5 C12 C5 63.6(6) . . . . ? N1 C5 C12 N5 -60.2(6) . . . . ? C4 C5 C12 N5 120.0(6) . . . . ? N3 N5 C13 C14 -0.4(6) . . . . ? C12 N5 C13 C14 -173.6(5) . . . . ? N3 N5 C13 C16 -179.0(5) . . . . ? C12 N5 C13 C16 7.9(9) . . . . ? N5 C13 C14 C15 0.0(6) . . . . ? C16 C13 C14 C15 178.4(6) . . . . ? N5 N3 C15 C14 -0.7(6) . . . . ? Cu N3 C15 C14 -176.7(4) . . . . ? N5 N3 C15 C17 178.7(5) . . . . ? Cu N3 C15 C17 2.7(8) . . . . ? C13 C14 C15 N3 0.5(6) . . . . ? C13 C14 C15 C17 -178.9(6) . . . . ? _refine_diff_density_max 0.435 _refine_diff_density_min -0.516 _refine_diff_density_rms 0.082