# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2005 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Prof. Chun-Hua Yan' _publ_contact_author_address ; State Key Laboratory of Rare Earth Materials Chemistry and Applications & PKU-HKU Joint Laboratory in Rare Earth Materials and Bioinorganic Chemistry Peking University Beijing 100871 China ; _publ_contact_author_email yan@pku.edu.cn _publ_contact_author_phone 86-(10)-62754179 _publ_contact_author_fax 86-(10)-62754179 _publ_requested_category FO _publ_section_title ; Crystal structures and magnetic behaviours of three new azido-bridged dinuclear cobalt(II) and copper(II) complexes ; loop_ _publ_author_name _publ_author_address 'Shi-Qiang Bai' ; State Key Laboratory of Rare Earth Materials Chemistry and Applications & PKU-HKU Joint Laboratory in Rare Earth Materials and Bioinorganic Chemistry Peking University Beijing 100871 China ; 'En-Qing Gao' ; Department of Chemistry East China Normal University Shanghai 200062 China ; 'Zheng He' ; State Key Laboratory of Rare Earth Materials Chemistry and Applications & PKU-HKU Joint Laboratory in Rare Earth Materials and Bioinorganic Chemistry Peking University Beijing 100871 China ; 'Chen-Jie Fang' ; State Key Laboratory of Rare Earth Materials Chemistry and Applications & PKU-HKU Joint Laboratory in Rare Earth Materials and Bioinorganic Chemistry Peking University Beijing 100871 China ; 'Chun-Hua Yan' ; State Key Laboratory of Rare Earth Materials Chemistry and Applications & PKU-HKU Joint Laboratory in Rare Earth Materials and Bioinorganic Chemistry Peking University Beijing 100871 China ; data_1 _database_code_depnum_ccdc_archive 'CCDC 250477' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H13 Co N9' _chemical_formula_weight 330.23 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' Co Co 0.3494 0.9721 '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 24.2866(4) _cell_length_b 8.1348(2) _cell_length_c 18.8753(4) _cell_angle_alpha 90.00 _cell_angle_beta 128.8435(8) _cell_angle_gamma 90.00 _cell_volume 2904.47(11) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 21852 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.510 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 1.190 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.863 _exptl_absorpt_correction_T_max 0.924 _exptl_absorpt_process_details '(Blessing, 1995, 1997)' _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 'NONIUS KappaCCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 0.76 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 29747 _diffrn_reflns_av_R_equivalents 0.0524 _diffrn_reflns_av_sigmaI/netI 0.0332 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.61 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3337 _reflns_number_gt 2514 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD (Nonius B. V., 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0480P)^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 SHELXL _refine_ls_extinction_coef 0.0022(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3337 _refine_ls_number_parameters 193 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0507 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0802 _refine_ls_wR_factor_gt 0.0740 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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 Co1 Co 0.067117(11) 0.87835(3) 0.072506(16) 0.03513(11) Uani 1 1 d . . . N1 N 0.07757(7) 0.66953(18) 0.15027(10) 0.0358(3) Uani 1 1 d . . . N2 N 0.14510(8) 0.98133(19) 0.19561(11) 0.0427(4) Uani 1 1 d . . . N3 N 0.14740(8) 0.9533(2) 0.26901(11) 0.0434(4) Uani 1 1 d . . . N4 N 0.09503(9) 0.7518(2) 0.01066(12) 0.0538(4) Uani 1 1 d . . . N5 N 0.08358(9) 0.8020(2) -0.05729(14) 0.0551(5) Uani 1 1 d . . . N6 N 0.07119(15) 0.8468(3) -0.12389(17) 0.0861(7) Uani 1 1 d . . . N7 N -0.03707(8) 0.90123(19) 0.01195(11) 0.0412(4) Uani 1 1 d . . . N8 N -0.06794(8) 0.8180(2) 0.02964(11) 0.0464(4) Uani 1 1 d . . . N9 N -0.09747(10) 0.7401(3) 0.04674(15) 0.0782(7) Uani 1 1 d . . . C1 C 0.07430(10) 0.5155(2) 0.12325(14) 0.0443(4) Uani 1 1 d . . . H1 H 0.0707 0.4995 0.0717 0.053 Uiso 1 1 calc R . . C2 C 0.07599(12) 0.3805(3) 0.16748(17) 0.0574(6) Uani 1 1 d . . . H2 H 0.0736 0.2753 0.1464 0.069 Uiso 1 1 calc R . . C3 C 0.08134(13) 0.4025(3) 0.24373(18) 0.0634(6) Uani 1 1 d . . . H3 H 0.0815 0.3127 0.2743 0.076 Uiso 1 1 calc R . . C4 C 0.08649(11) 0.5602(3) 0.27409(15) 0.0544(5) Uani 1 1 d . . . H4 H 0.0915 0.5777 0.3266 0.065 Uiso 1 1 calc R . . C5 C 0.08413(9) 0.6919(2) 0.22624(12) 0.0382(4) Uani 1 1 d . . . C6 C 0.08864(10) 0.8668(2) 0.25516(14) 0.0452(5) Uani 1 1 d . . . H6A H 0.0448 0.9232 0.2089 0.054 Uiso 1 1 calc R . . H6B H 0.0949 0.8681 0.3112 0.054 Uiso 1 1 calc R . . C7 C 0.20923(11) 1.0070(3) 0.34677(14) 0.0574(6) Uani 1 1 d . . . C8 C 0.24712(11) 1.0720(3) 0.32294(17) 0.0644(7) Uani 1 1 d . . . H8 H 0.2917 1.1195 0.3621 0.077 Uiso 1 1 calc R . . C9 C 0.20678(10) 1.0543(3) 0.22911(16) 0.0534(5) Uani 1 1 d . . . C10 C 0.22442(13) 1.0979(4) 0.16907(19) 0.0808(9) Uani 1 1 d . . . H10A H 0.2005 1.0243 0.1181 0.121 Uiso 1 1 calc R . . H10B H 0.2745 1.0889 0.2026 0.121 Uiso 1 1 calc R . . H10C H 0.2097 1.2087 0.1478 0.121 Uiso 1 1 calc R . . C11 C 0.22785(15) 0.9871(4) 0.43822(16) 0.0886(10) Uani 1 1 d . . . H11A H 0.1955 1.0496 0.4406 0.133 Uiso 1 1 calc R . . H11B H 0.2751 1.0259 0.4842 0.133 Uiso 1 1 calc R . . H11C H 0.2249 0.8731 0.4486 0.133 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 Co1 0.03193(15) 0.03766(16) 0.03453(16) 0.00310(10) 0.02022(12) 0.00328(10) N1 0.0344(7) 0.0341(8) 0.0333(8) 0.0011(6) 0.0186(6) 0.0018(6) N2 0.0367(8) 0.0386(9) 0.0422(9) 0.0010(7) 0.0196(7) -0.0022(6) N3 0.0395(8) 0.0417(9) 0.0387(9) -0.0063(7) 0.0195(7) 0.0003(7) N4 0.0589(10) 0.0612(11) 0.0484(10) 0.0083(9) 0.0371(9) 0.0167(9) N5 0.0605(11) 0.0591(11) 0.0595(12) -0.0109(10) 0.0443(10) -0.0044(9) N6 0.130(2) 0.0919(17) 0.0735(15) -0.0117(13) 0.0818(16) -0.0186(15) N7 0.0359(8) 0.0432(9) 0.0459(9) 0.0130(7) 0.0264(7) 0.0051(6) N8 0.0400(8) 0.0501(10) 0.0478(10) 0.0100(8) 0.0269(8) 0.0021(7) N9 0.0628(12) 0.0938(17) 0.0840(15) 0.0273(13) 0.0489(12) -0.0063(11) C1 0.0440(10) 0.0381(11) 0.0436(11) -0.0021(9) 0.0239(9) 0.0002(8) C2 0.0628(14) 0.0352(11) 0.0667(15) 0.0020(10) 0.0371(12) -0.0002(9) C3 0.0750(16) 0.0465(13) 0.0715(16) 0.0151(11) 0.0472(14) 0.0002(11) C4 0.0599(13) 0.0625(14) 0.0487(12) 0.0099(11) 0.0378(11) 0.0025(11) C5 0.0350(9) 0.0426(10) 0.0367(10) 0.0036(8) 0.0222(8) 0.0029(7) C6 0.0454(10) 0.0521(12) 0.0398(10) -0.0025(9) 0.0276(9) 0.0029(9) C7 0.0440(11) 0.0557(13) 0.0443(12) -0.0134(10) 0.0140(10) 0.0045(9) C8 0.0367(11) 0.0605(14) 0.0616(15) -0.0112(12) 0.0142(11) -0.0078(10) C9 0.0353(10) 0.0469(11) 0.0587(13) 0.0038(10) 0.0201(10) -0.0032(9) C10 0.0475(13) 0.095(2) 0.0795(18) 0.0173(15) 0.0300(13) -0.0185(13) C11 0.0708(16) 0.120(3) 0.0463(14) -0.0199(16) 0.0230(13) 0.0083(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N4 1.9686(17) . ? Co1 N7 2.0288(14) . ? Co1 N2 2.0415(15) . ? Co1 N1 2.1534(15) . ? Co1 N7 2.1977(15) 5_575 ? N1 C1 1.337(2) . ? N1 C5 1.352(2) . ? N2 C9 1.345(2) . ? N2 N3 1.370(2) . ? N3 C7 1.355(2) . ? N3 C6 1.460(2) . ? N4 N5 1.201(3) . ? N5 N6 1.153(3) . ? N7 N8 1.203(2) . ? N7 Co1 2.1977(15) 5_575 ? N8 N9 1.145(2) . ? C1 C2 1.364(3) . ? C2 C3 1.373(4) . ? C3 C4 1.378(3) . ? C4 C5 1.379(3) . ? C5 C6 1.503(3) . ? C7 C8 1.359(3) . ? C7 C11 1.494(3) . ? C8 C9 1.393(3) . ? C9 C10 1.484(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 N4 Co1 N7 119.05(7) . . ? N4 Co1 N2 118.09(7) . . ? N7 Co1 N2 122.86(7) . . ? N4 Co1 N1 93.11(7) . . ? N7 Co1 N1 91.64(6) . . ? N2 Co1 N1 85.37(6) . . ? N4 Co1 N7 94.47(7) . 5_575 ? N7 Co1 N7 77.71(6) . 5_575 ? N2 Co1 N7 98.03(6) . 5_575 ? N1 Co1 N7 169.00(5) . 5_575 ? C1 N1 C5 118.06(16) . . ? C1 N1 Co1 121.75(13) . . ? C5 N1 Co1 120.12(12) . . ? C9 N2 N3 105.73(16) . . ? C9 N2 Co1 132.93(15) . . ? N3 N2 Co1 120.19(11) . . ? C7 N3 N2 110.87(17) . . ? C7 N3 C6 130.10(19) . . ? N2 N3 C6 118.93(15) . . ? N5 N4 Co1 121.35(15) . . ? N6 N5 N4 178.1(3) . . ? N8 N7 Co1 124.50(13) . . ? N8 N7 Co1 132.81(12) . 5_575 ? Co1 N7 Co1 102.29(6) . 5_575 ? N9 N8 N7 179.4(2) . . ? N1 C1 C2 123.3(2) . . ? C1 C2 C3 118.9(2) . . ? C2 C3 C4 118.8(2) . . ? C3 C4 C5 119.7(2) . . ? N1 C5 C4 121.24(19) . . ? N1 C5 C6 116.48(16) . . ? C4 C5 C6 122.28(19) . . ? N3 C6 C5 111.20(16) . . ? N3 C7 C8 106.7(2) . . ? N3 C7 C11 122.9(2) . . ? C8 C7 C11 130.4(2) . . ? C7 C8 C9 107.36(19) . . ? N2 C9 C8 109.3(2) . . ? N2 C9 C10 121.1(2) . . ? C8 C9 C10 129.5(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.354 _refine_diff_density_min -0.308 _refine_diff_density_rms 0.074 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 250478' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H13 Cu N9' _chemical_formula_weight 334.84 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 24.3949(3) _cell_length_b 8.04680(10) _cell_length_c 18.7195(3) _cell_angle_alpha 90.00 _cell_angle_beta 128.6544(7) _cell_angle_gamma 90.00 _cell_volume 2869.64(7) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12162 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.550 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 1.531 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.709 _exptl_absorpt_correction_T_max 0.806 _exptl_absorpt_process_details '(Blessing, 1995, 1997)' _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 'NONIUS KappaCCD Diffractometer' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 0.76 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 24923 _diffrn_reflns_av_R_equivalents 0.0672 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3300 _reflns_number_gt 2248 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD (Nonius B. V., 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0424P)^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 SHELXL _refine_ls_extinction_coef 0.0017(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3300 _refine_ls_number_parameters 193 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0775 _refine_ls_wR_factor_gt 0.0718 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.974 _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 0.072944(13) 0.89258(3) 0.074903(16) 0.03339(12) Uani 1 1 d . . . N1 N 0.07823(8) 0.6931(2) 0.14612(10) 0.0298(4) Uani 1 1 d . . . N2 N 0.14593(9) 1.0050(2) 0.19745(12) 0.0385(4) Uani 1 1 d . . . N3 N 0.14582(9) 0.9765(2) 0.26961(11) 0.0385(4) Uani 1 1 d . . . N4 N 0.09198(11) 0.7544(3) 0.00503(13) 0.0529(5) Uani 1 1 d . . . N5 N 0.07824(10) 0.7989(2) -0.06499(14) 0.0452(5) Uani 1 1 d . . . N6 N 0.06390(14) 0.8376(3) -0.13401(16) 0.0719(7) Uani 1 1 d . . . N7 N -0.04267(9) 0.9055(2) 0.00347(12) 0.0392(4) Uani 1 1 d . . . N8 N -0.07173(9) 0.8277(2) 0.02539(12) 0.0407(4) Uani 1 1 d . . . N9 N -0.09725(12) 0.7494(3) 0.04856(16) 0.0738(7) Uani 1 1 d . . . C1 C 0.07457(11) 0.5378(3) 0.11774(14) 0.0373(5) Uani 1 1 d . . . H1 H 0.0723 0.5230 0.0667 0.045 Uiso 1 1 calc R . . C2 C 0.07403(12) 0.4005(3) 0.15984(16) 0.0463(6) Uani 1 1 d . . . H2 H 0.0710 0.2947 0.1376 0.056 Uiso 1 1 calc R . . C3 C 0.07811(14) 0.4216(3) 0.23626(17) 0.0529(7) Uani 1 1 d . . . H3 H 0.0780 0.3301 0.2666 0.063 Uiso 1 1 calc R . . C4 C 0.08228(12) 0.5794(3) 0.26668(15) 0.0451(6) Uani 1 1 d . . . H4 H 0.0852 0.5961 0.3181 0.054 Uiso 1 1 calc R . . C5 C 0.08215(10) 0.7133(3) 0.22091(13) 0.0329(5) Uani 1 1 d . . . C6 C 0.08649(12) 0.8898(3) 0.25166(15) 0.0398(5) Uani 1 1 d . . . H6A H 0.0436 0.9483 0.2046 0.048 Uiso 1 1 calc R . . H6B H 0.0907 0.8886 0.3067 0.048 Uiso 1 1 calc R . . C7 C 0.20758(13) 1.0255(3) 0.34949(15) 0.0506(6) Uani 1 1 d . . . C8 C 0.24656(13) 1.0888(3) 0.32759(17) 0.0584(7) Uani 1 1 d . . . H8 H 0.2913 1.1340 0.3685 0.070 Uiso 1 1 calc R . . C9 C 0.20842(12) 1.0747(3) 0.23318(16) 0.0469(6) Uani 1 1 d . . . C10 C 0.22797(14) 1.1157(4) 0.1754(2) 0.0758(10) Uani 1 1 d . . . H10A H 0.2080 1.0352 0.1272 0.114 Uiso 1 1 calc R . . H10B H 0.2782 1.1145 0.2118 0.114 Uiso 1 1 calc R . . H10C H 0.2105 1.2243 0.1494 0.114 Uiso 1 1 calc R . . C11 C 0.22355(16) 1.0027(4) 0.44009(17) 0.0796(10) Uani 1 1 d . . . H11A H 0.1917 1.0683 0.4421 0.119 Uiso 1 1 calc R . . H11B H 0.2709 1.0375 0.4880 0.119 Uiso 1 1 calc R . . H11C H 0.2184 0.8876 0.4483 0.119 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 0.03796(18) 0.03122(17) 0.03223(16) 0.00407(11) 0.02253(13) 0.00180(11) N1 0.0311(9) 0.0296(10) 0.0279(9) 0.0005(7) 0.0180(8) 0.0001(7) N2 0.0362(11) 0.0330(10) 0.0369(10) 0.0025(8) 0.0183(9) -0.0021(8) N3 0.0377(11) 0.0365(10) 0.0338(10) -0.0054(8) 0.0187(9) -0.0001(8) N4 0.0689(14) 0.0571(13) 0.0443(12) 0.0130(10) 0.0411(12) 0.0237(11) N5 0.0549(12) 0.0450(12) 0.0474(12) -0.0034(10) 0.0377(11) -0.0004(10) N6 0.110(2) 0.0735(15) 0.0571(14) -0.0045(13) 0.0644(15) -0.0088(15) N7 0.0372(10) 0.0401(11) 0.0452(11) 0.0137(8) 0.0281(9) 0.0045(8) N8 0.0364(10) 0.0443(11) 0.0378(10) 0.0077(9) 0.0214(9) 0.0012(9) N9 0.0612(15) 0.0896(17) 0.0753(16) 0.0289(14) 0.0449(14) -0.0070(13) C1 0.0414(13) 0.0340(12) 0.0351(12) -0.0031(10) 0.0232(11) -0.0003(10) C2 0.0531(15) 0.0288(12) 0.0522(14) -0.0007(11) 0.0306(13) -0.0014(11) C3 0.0646(17) 0.0412(15) 0.0569(16) 0.0143(12) 0.0400(14) 0.0006(12) C4 0.0513(15) 0.0526(16) 0.0403(13) 0.0036(11) 0.0329(12) -0.0017(11) C5 0.0282(11) 0.0384(13) 0.0307(11) 0.0021(9) 0.0178(9) 0.0020(9) C6 0.0421(13) 0.0441(13) 0.0370(12) -0.0038(10) 0.0265(11) 0.0026(11) C7 0.0415(14) 0.0501(15) 0.0394(14) -0.0126(12) 0.0151(12) 0.0021(12) C8 0.0376(14) 0.0537(16) 0.0539(16) -0.0107(13) 0.0139(13) -0.0092(12) C9 0.0330(13) 0.0406(13) 0.0482(14) 0.0027(11) 0.0161(12) -0.0066(10) C10 0.0458(16) 0.091(2) 0.0706(19) 0.0132(16) 0.0266(15) -0.0217(15) C11 0.070(2) 0.105(3) 0.0432(16) -0.0183(17) 0.0253(15) -0.0026(18) _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 N4 1.9803(19) . ? Cu1 N7 1.9960(17) 5_575 ? Cu1 N2 2.0369(17) . ? Cu1 N1 2.0385(16) . ? Cu1 N7 2.2455(18) . ? N1 C1 1.339(3) . ? N1 C5 1.352(2) . ? N2 C9 1.346(3) . ? N2 N3 1.372(2) . ? N3 C7 1.359(3) . ? N3 C6 1.445(3) . ? N4 N5 1.187(2) . ? N5 N6 1.151(3) . ? N7 N8 1.194(2) . ? N7 Cu1 1.9960(17) 5_575 ? N8 N9 1.145(3) . ? C1 C2 1.362(3) . ? C2 C3 1.381(3) . ? C3 C4 1.370(3) . ? C4 C5 1.375(3) . ? C5 C6 1.511(3) . ? C7 C8 1.349(4) . ? C7 C11 1.495(3) . ? C8 C9 1.396(3) . ? C9 C10 1.466(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Cu1 N7 95.92(8) . 5_575 ? N4 Cu1 N2 126.34(8) . . ? N7 Cu1 N2 97.36(7) 5_575 . ? N4 Cu1 N1 92.57(7) . . ? N7 Cu1 N1 164.76(7) 5_575 . ? N2 Cu1 N1 87.68(6) . . ? N4 Cu1 N7 110.99(8) . . ? N7 Cu1 N7 76.95(8) 5_575 . ? N2 Cu1 N7 122.63(7) . . ? N1 Cu1 N7 88.21(6) . . ? C1 N1 C5 117.83(18) . . ? C1 N1 Cu1 120.94(13) . . ? C5 N1 Cu1 121.16(13) . . ? C9 N2 N3 106.18(18) . . ? C9 N2 Cu1 131.81(17) . . ? N3 N2 Cu1 119.77(13) . . ? C7 N3 N2 110.61(19) . . ? C7 N3 C6 131.1(2) . . ? N2 N3 C6 118.01(16) . . ? N5 N4 Cu1 122.63(16) . . ? N6 N5 N4 178.0(3) . . ? N8 N7 Cu1 130.74(15) . 5_575 ? N8 N7 Cu1 124.44(14) . . ? Cu1 N7 Cu1 103.05(8) 5_575 . ? N9 N8 N7 177.3(2) . . ? N1 C1 C2 123.4(2) . . ? C1 C2 C3 118.6(2) . . ? C4 C3 C2 118.9(2) . . ? C3 C4 C5 119.8(2) . . ? N1 C5 C4 121.50(19) . . ? N1 C5 C6 116.74(18) . . ? C4 C5 C6 121.76(19) . . ? N3 C6 C5 111.36(17) . . ? C8 C7 N3 106.4(2) . . ? C8 C7 C11 131.1(2) . . ? N3 C7 C11 122.5(3) . . ? C7 C8 C9 108.4(2) . . ? N2 C9 C8 108.4(2) . . ? N2 C9 C10 121.1(2) . . ? C8 C9 C10 130.5(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.284 _refine_diff_density_min -0.337 _refine_diff_density_rms 0.066 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 250479' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H12 Cu N8' _chemical_formula_weight 343.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.0150(4) _cell_length_b 6.3940(2) _cell_length_c 19.1148(8) _cell_angle_alpha 90.00 _cell_angle_beta 102.01(3) _cell_angle_gamma 90.00 _cell_volume 1436.35(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15733 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 700 _exptl_absorpt_coefficient_mu 1.530 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.731 _exptl_absorpt_correction_T_max 0.926 _exptl_absorpt_process_details '(Blessing, 1995, 1997)' _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 'NONIUS KappaCCD Diffractometer' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 0.76 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 19983 _diffrn_reflns_av_R_equivalents 0.1247 _diffrn_reflns_av_sigmaI/netI 0.0794 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.47 _diffrn_reflns_theta_max 27.42 _reflns_number_total 3215 _reflns_number_gt 2071 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD (Nonius B. V., 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0534P)^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 SHELXL _refine_ls_extinction_coef 0.0017(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3215 _refine_ls_number_parameters 201 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0912 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1128 _refine_ls_wR_factor_gt 0.0987 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 0.05671(3) 0.22719(5) -0.00807(2) 0.03510(17) Uani 1 1 d . . . N1 N 0.1192(2) 0.2459(3) 0.09799(14) 0.0361(6) Uani 1 1 d . . . N2 N 0.2230(2) 0.2787(4) -0.00660(14) 0.0363(6) Uani 1 1 d . . . N3 N -0.0973(2) 0.1562(4) 0.00837(14) 0.0421(6) Uani 1 1 d . . . N4 N -0.1838(2) 0.1928(4) -0.03520(15) 0.0393(6) Uani 1 1 d . . . N5 N -0.2689(3) 0.2194(5) -0.07467(18) 0.0559(8) Uani 1 1 d . . . N6 N -0.0054(3) 0.2894(5) -0.10724(17) 0.0553(8) Uani 1 1 d . . . N7 N 0.0260(2) 0.2613(4) -0.16124(17) 0.0457(7) Uani 1 1 d . . . N8 N 0.0501(3) 0.2410(6) -0.2157(2) 0.0794(12) Uani 1 1 d . . . C1 C 0.0601(3) 0.2367(5) 0.14955(19) 0.0448(8) Uani 1 1 d . . . H1 H -0.0184 0.2194 0.1371 0.054 Uiso 1 1 calc R . . C2 C 0.1120(4) 0.2520(5) 0.2211(2) 0.0511(9) Uani 1 1 d . . . H2 H 0.0688 0.2471 0.2562 0.061 Uiso 1 1 calc R . . C3 C 0.2270(4) 0.2743(5) 0.2395(2) 0.0548(10) Uani 1 1 d . . . H3 H 0.2632 0.2840 0.2874 0.066 Uiso 1 1 calc R . . C4 C 0.2897(3) 0.2825(5) 0.18673(19) 0.0487(9) Uani 1 1 d . . . H4 H 0.3684 0.2963 0.1982 0.058 Uiso 1 1 calc R . . C5 C 0.2323(3) 0.2698(4) 0.11676(18) 0.0381(7) Uani 1 1 d . . . C6 C 0.2890(3) 0.2843(4) 0.05481(19) 0.0404(8) Uani 1 1 d . . . C7 C 0.4152(3) 0.3081(6) 0.0690(2) 0.0608(10) Uani 1 1 d . . . H7A H 0.4397 0.3187 0.0245 0.091 Uiso 1 1 calc R . . H7B H 0.4503 0.1886 0.0951 0.091 Uiso 1 1 calc R . . H7C H 0.4369 0.4323 0.0967 0.091 Uiso 1 1 calc R . . C8 C 0.2691(3) 0.2964(5) -0.06974(18) 0.0386(7) Uani 1 1 d . . . C9 C 0.2677(3) 0.4897(5) -0.10217(19) 0.0480(8) Uani 1 1 d . . . H9 H 0.2384 0.6058 -0.0829 0.058 Uiso 1 1 calc R . . C10 C 0.3102(3) 0.5081(6) -0.1634(2) 0.0554(9) Uani 1 1 d . . . H10 H 0.3105 0.6380 -0.1852 0.066 Uiso 1 1 calc R . . C11 C 0.3512(3) 0.3405(7) -0.1920(2) 0.0602(10) Uani 1 1 d . . . H11 H 0.3790 0.3553 -0.2337 0.072 Uiso 1 1 calc R . . C12 C 0.3526(3) 0.1464(6) -0.1603(2) 0.0640(11) Uani 1 1 d . . . H12 H 0.3812 0.0310 -0.1804 0.077 Uiso 1 1 calc R . . C13 C 0.3114(3) 0.1246(6) -0.0986(2) 0.0541(9) Uani 1 1 d . . . H13 H 0.3123 -0.0054 -0.0767 0.065 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 0.0318(2) 0.0416(2) 0.0314(2) 0.00052(17) 0.00555(16) -0.00061(16) N1 0.0359(14) 0.0374(13) 0.0342(14) -0.0029(11) 0.0056(11) 0.0009(10) N2 0.0346(14) 0.0394(13) 0.0342(15) 0.0018(11) 0.0060(12) -0.0026(10) N3 0.0342(15) 0.0588(17) 0.0334(16) -0.0009(12) 0.0074(13) 0.0000(13) N4 0.0375(17) 0.0449(15) 0.0372(16) -0.0036(12) 0.0121(14) 0.0012(12) N5 0.0415(18) 0.068(2) 0.053(2) -0.0018(15) -0.0031(15) 0.0070(14) N6 0.0447(18) 0.083(2) 0.0388(18) 0.0162(15) 0.0101(14) 0.0128(15) N7 0.0347(15) 0.0579(17) 0.0405(18) 0.0027(14) -0.0018(14) 0.0008(12) N8 0.057(2) 0.143(4) 0.038(2) -0.016(2) 0.0100(17) 0.002(2) C1 0.048(2) 0.0490(18) 0.0394(19) -0.0021(15) 0.0143(16) 0.0021(15) C2 0.066(3) 0.055(2) 0.0351(19) -0.0030(15) 0.0176(18) -0.0029(17) C3 0.073(3) 0.050(2) 0.036(2) -0.0027(16) 0.0001(19) -0.0080(18) C4 0.047(2) 0.054(2) 0.040(2) -0.0011(16) -0.0027(16) -0.0041(15) C5 0.0409(19) 0.0336(15) 0.0379(18) -0.0001(13) 0.0035(15) -0.0002(13) C6 0.0370(18) 0.0404(17) 0.0431(19) -0.0005(14) 0.0071(15) -0.0026(13) C7 0.036(2) 0.088(3) 0.055(2) 0.004(2) 0.0043(18) -0.0050(18) C8 0.0315(16) 0.0479(18) 0.0361(18) 0.0008(14) 0.0059(14) -0.0043(13) C9 0.050(2) 0.0486(19) 0.046(2) -0.0004(16) 0.0099(17) -0.0070(15) C10 0.055(2) 0.064(2) 0.048(2) 0.0077(18) 0.0145(18) -0.0088(18) C11 0.045(2) 0.091(3) 0.049(2) 0.003(2) 0.0202(19) -0.006(2) C12 0.064(3) 0.069(2) 0.066(3) -0.009(2) 0.030(2) 0.007(2) C13 0.060(2) 0.0501(19) 0.058(2) 0.0008(17) 0.0241(19) 0.0037(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N6 1.929(3) . ? Cu1 N3 1.993(3) . ? Cu1 N1 2.014(3) . ? Cu1 N2 2.019(3) . ? N1 C1 1.331(4) . ? N1 C5 1.340(4) . ? N2 C6 1.273(4) . ? N2 C8 1.434(4) . ? N3 N4 1.212(4) . ? N4 N5 1.150(4) . ? N6 N7 1.184(4) . ? N7 N8 1.144(5) . ? C1 C2 1.384(5) . ? C2 C3 1.361(6) . ? C3 C4 1.379(6) . ? C4 C5 1.374(5) . ? C5 C6 1.487(5) . ? C6 C7 1.492(5) . ? C8 C13 1.374(5) . ? C8 C9 1.381(4) . ? C9 C10 1.376(5) . ? C10 C11 1.343(5) . ? C11 C12 1.380(6) . ? C12 C13 1.376(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 N6 Cu1 N3 91.13(12) . . ? N6 Cu1 N1 164.63(11) . . ? N3 Cu1 N1 91.09(11) . . ? N6 Cu1 N2 99.18(12) . . ? N3 Cu1 N2 169.58(11) . . ? N1 Cu1 N2 79.37(11) . . ? C1 N1 C5 118.3(3) . . ? C1 N1 Cu1 126.7(2) . . ? C5 N1 Cu1 114.9(2) . . ? C6 N2 C8 119.9(3) . . ? C6 N2 Cu1 116.2(2) . . ? C8 N2 Cu1 123.8(2) . . ? N4 N3 Cu1 122.7(2) . . ? N5 N4 N3 176.2(3) . . ? N7 N6 Cu1 134.2(2) . . ? N8 N7 N6 175.5(4) . . ? N1 C1 C2 121.9(3) . . ? C3 C2 C1 119.2(4) . . ? C2 C3 C4 119.6(3) . . ? C5 C4 C3 118.0(3) . . ? N1 C5 C4 122.9(3) . . ? N1 C5 C6 113.6(3) . . ? C4 C5 C6 123.5(3) . . ? N2 C6 C5 115.6(3) . . ? N2 C6 C7 125.8(3) . . ? C5 C6 C7 118.6(3) . . ? C13 C8 C9 120.4(3) . . ? C13 C8 N2 121.0(3) . . ? C9 C8 N2 118.6(3) . . ? C10 C9 C8 119.1(3) . . ? C11 C10 C9 120.7(4) . . ? C10 C11 C12 120.7(4) . . ? C13 C12 C11 119.6(4) . . ? C8 C13 C12 119.5(4) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.42 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.548 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.104 #===END