# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_author_name 'Dan Li' _publ_contact_author_name 'Dan Li' _publ_contact_author_email dli@stu.edu.cn data_1 _database_code_depnum_ccdc_archive 'CCDC 805596' #TrackingRef '- complexes1-3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H9 Cu3 N14' _chemical_formula_sum 'C16 H9 Cu3 N14' _chemical_formula_weight 587.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7029(6) _cell_length_b 10.1842(6) _cell_length_c 11.1003(7) _cell_angle_alpha 107.2920(10) _cell_angle_beta 91.1910(10) _cell_angle_gamma 109.5120(10) _cell_volume 978.34(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas no _exptl_crystal_density_diffrn 1.996 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 580 _exptl_absorpt_coefficient_mu 3.272 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.707 _exptl_absorpt_correction_T_max 0.920 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _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 'Bruker APEX area-dectector diffractometer' _diffrn_measurement_method '\f and \w-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5707 _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_av_sigmaI/netI 0.0444 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3369 _reflns_number_gt 2459 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SMART (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material SHELXS-97 _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^)+(0.0717P)^2^+0.7339P] 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 3369 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0689 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1496 _refine_ls_wR_factor_gt 0.1135 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean <0.001 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 0.27972(9) 0.83364(8) 0.64778(8) 0.0469(3) Uani 1 1 d . . . Cu2 Cu 0.44893(10) 1.41679(9) 0.56854(9) 0.0567(3) Uani 1 1 d . . . Cu3 Cu 0.08230(10) 1.05701(11) 0.29632(9) 0.0627(3) Uani 1 1 d . . . C8 C 0.7724(8) 1.3889(9) 0.8380(8) 0.069(2) Uani 1 1 d . . . H8 H 0.8584 1.4483 0.8938 0.083 Uiso 1 1 calc R . . N6 N 0.0258(5) 0.8605(5) 0.7927(5) 0.0384(11) Uani 1 1 d . . . N9 N 0.3007(5) 0.9942(5) 0.5780(4) 0.0363(11) Uani 1 1 d . . . C11 C 0.1966(6) 0.9760(6) 0.4861(5) 0.0356(13) Uani 1 1 d . . . N10 N 0.3332(5) 1.2007(5) 0.5321(5) 0.0418(12) Uani 1 1 d . . . N5 N 0.1542(5) 0.8346(6) 0.7916(5) 0.0424(12) Uani 1 1 d . . . N11 N 0.2120(5) 1.0975(5) 0.4565(5) 0.0387(11) Uani 1 1 d . . . C5 C -0.0367(6) 0.8191(6) 0.8882(5) 0.0364(13) Uani 1 1 d . . . N2 N -0.2339(5) 0.8884(6) 0.8408(5) 0.0416(12) Uani 1 1 d . . . C10 C 0.3844(6) 1.1363(6) 0.6037(5) 0.0365(13) Uani 1 1 d . . . N8 N 0.5800(6) 1.3640(6) 0.6894(5) 0.0553(14) Uani 1 1 d . . . N4 N 0.1654(5) 0.7802(6) 0.8836(5) 0.0479(13) Uani 1 1 d . . . N3 N 0.0473(6) 0.7677(6) 0.9454(5) 0.0485(13) Uani 1 1 d . . . N7 N 0.5844(6) 1.1563(6) 0.7493(5) 0.0538(14) Uani 1 1 d . . . C4 C -0.1820(6) 0.8262(6) 0.9129(5) 0.0386(13) Uani 1 1 d . . . N1 N -0.2522(6) 0.7659(7) 0.9959(6) 0.0615(16) Uani 1 1 d . . . C3 C -0.3702(7) 0.8863(7) 0.8532(6) 0.0509(16) Uani 1 1 d . . . H3 H -0.4113 0.9267 0.8037 0.061 Uiso 1 1 calc R . . C6 C 0.5231(7) 1.2201(7) 0.6854(6) 0.0467(15) Uani 1 1 d . . . C2 C -0.4524(8) 0.8280(9) 0.9346(7) 0.064(2) Uani 1 1 d . . . H2 H -0.5474 0.8285 0.9425 0.077 Uiso 1 1 calc R . . C9 C 0.7048(9) 1.4452(9) 0.7645(8) 0.068(2) Uani 1 1 d . . . H9 H 0.7492 1.5430 0.7686 0.082 Uiso 1 1 calc R . . C1 C -0.3873(8) 0.7676(10) 1.0054(8) 0.073(2) Uani 1 1 d . . . H1 H -0.4409 0.7265 1.0620 0.088 Uiso 1 1 calc R . . N13 N 0.0090(5) 0.8417(6) 0.3117(5) 0.0422(12) Uani 1 1 d . . . N12 N 0.0626(5) 0.7203(6) 0.4498(5) 0.0428(12) Uani 1 1 d . . . C12 C 0.0819(6) 0.8380(6) 0.4135(5) 0.0365(13) Uani 1 1 d . . . C13 C -0.0410(7) 0.5946(8) 0.3763(7) 0.0529(17) Uani 1 1 d . . . H13 H -0.0579 0.5094 0.3977 0.064 Uiso 1 1 calc R . . C15 C -0.0967(7) 0.7142(8) 0.2402(6) 0.0492(16) Uani 1 1 d . . . H15 H -0.1519 0.7128 0.1700 0.059 Uiso 1 1 calc R . . C14 C -0.1237(7) 0.5873(8) 0.2696(7) 0.0563(17) Uani 1 1 d . . . H14 H -0.1951 0.4992 0.2197 0.068 Uiso 1 1 calc R . . C7 C 0.7087(7) 1.2447(9) 0.8254(7) 0.0581(19) Uani 1 1 d . . . H7 H 0.7545 1.2054 0.8725 0.070 Uiso 1 1 calc R . . N14 N 0.3622(5) 0.6845(6) 0.6178(5) 0.0464(13) Uani 1 1 d . . . C16 C 0.4006(7) 0.5871(7) 0.5966(6) 0.0450(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0500(5) 0.0426(5) 0.0650(6) 0.0315(4) 0.0115(4) 0.0251(4) Cu2 0.0666(6) 0.0376(5) 0.0832(6) 0.0328(4) 0.0227(5) 0.0277(4) Cu3 0.0616(6) 0.0849(7) 0.0741(6) 0.0567(6) 0.0131(5) 0.0393(5) C8 0.046(4) 0.063(5) 0.085(6) 0.018(4) -0.002(4) 0.010(4) N6 0.033(3) 0.043(3) 0.051(3) 0.025(2) 0.005(2) 0.019(2) N9 0.036(3) 0.034(3) 0.048(3) 0.024(2) 0.002(2) 0.014(2) C11 0.039(3) 0.035(3) 0.043(3) 0.022(3) 0.009(3) 0.017(3) N10 0.038(3) 0.034(3) 0.063(3) 0.026(3) 0.006(2) 0.014(2) N5 0.038(3) 0.048(3) 0.055(3) 0.028(3) 0.005(2) 0.023(2) N11 0.036(3) 0.037(3) 0.050(3) 0.024(2) 0.004(2) 0.013(2) C5 0.039(3) 0.038(3) 0.034(3) 0.012(3) -0.004(3) 0.016(3) N2 0.030(3) 0.047(3) 0.052(3) 0.019(3) -0.003(2) 0.017(2) C10 0.031(3) 0.034(3) 0.052(4) 0.021(3) 0.000(3) 0.014(3) N8 0.057(4) 0.046(3) 0.061(4) 0.015(3) -0.002(3) 0.019(3) N4 0.044(3) 0.061(3) 0.057(3) 0.034(3) 0.009(3) 0.028(3) N3 0.049(3) 0.063(4) 0.047(3) 0.030(3) 0.004(3) 0.026(3) N7 0.056(4) 0.056(4) 0.053(3) 0.021(3) 0.005(3) 0.022(3) C4 0.038(3) 0.038(3) 0.037(3) 0.014(3) 0.001(3) 0.010(3) N1 0.054(4) 0.099(5) 0.057(3) 0.045(3) 0.017(3) 0.041(3) C3 0.046(4) 0.058(4) 0.056(4) 0.023(4) -0.003(3) 0.024(3) C6 0.051(4) 0.044(4) 0.055(4) 0.024(3) 0.012(3) 0.022(3) C2 0.056(4) 0.088(6) 0.065(5) 0.029(4) 0.016(4) 0.041(4) C9 0.058(5) 0.051(4) 0.078(5) 0.012(4) 0.004(4) 0.006(4) C1 0.057(5) 0.123(7) 0.074(5) 0.055(5) 0.030(4) 0.051(5) N13 0.043(3) 0.047(3) 0.047(3) 0.024(3) 0.005(2) 0.019(3) N12 0.040(3) 0.042(3) 0.054(3) 0.029(3) 0.002(2) 0.012(2) C12 0.030(3) 0.045(3) 0.043(3) 0.022(3) 0.007(3) 0.018(3) C13 0.048(4) 0.048(4) 0.070(5) 0.032(4) 0.000(3) 0.014(3) C15 0.035(4) 0.059(4) 0.050(4) 0.023(3) -0.002(3) 0.009(3) C14 0.049(4) 0.049(4) 0.060(4) 0.018(3) -0.002(3) 0.004(3) C7 0.040(4) 0.082(5) 0.058(4) 0.032(4) 0.000(3) 0.022(4) N14 0.042(3) 0.042(3) 0.069(4) 0.031(3) 0.015(3) 0.021(3) C16 0.041(3) 0.035(3) 0.063(4) 0.020(3) 0.012(3) 0.015(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N14 1.893(5) . ? Cu1 N9 1.963(4) . ? Cu1 N5 2.028(5) . ? Cu2 C16 1.885(6) 1_565 ? Cu2 N10 2.018(5) . ? Cu2 N8 2.126(5) . ? Cu2 C16 2.367(6) 2_676 ? Cu2 Cu2 2.5776(16) 2_686 ? Cu3 N6 1.955(4) 2_576 ? Cu3 N11 2.010(5) . ? Cu3 N13 2.129(5) . ? Cu3 N2 2.199(5) 2_576 ? C8 C7 1.351(10) . ? C8 C9 1.390(11) . ? C8 H8 0.9300 . ? N6 C5 1.338(7) . ? N6 N5 1.357(6) . ? N6 Cu3 1.955(4) 2_576 ? N9 C10 1.340(7) . ? N9 C11 1.347(7) . ? C11 N11 1.335(6) . ? C11 C12 1.452(8) . ? N10 N11 1.342(7) . ? N10 C10 1.348(7) . ? N5 N4 1.316(6) . ? C5 N3 1.342(7) . ? C5 C4 1.463(8) . ? N2 C3 1.326(7) . ? N2 C4 1.339(7) . ? N2 Cu3 2.199(5) 2_576 ? C10 C6 1.443(8) . ? N8 C9 1.313(9) . ? N8 C6 1.369(8) . ? N4 N3 1.337(7) . ? N7 C7 1.327(8) . ? N7 C6 1.339(8) . ? C4 N1 1.332(8) . ? N1 C1 1.322(8) . ? C3 C2 1.356(10) . ? C3 H3 0.9300 . ? C2 C1 1.386(10) . ? C2 H2 0.9300 . ? C9 H9 0.9300 . ? C1 H1 0.9300 . ? N13 C12 1.337(7) . ? N13 C15 1.354(8) . ? N12 C12 1.332(7) . ? N12 C13 1.342(8) . ? C13 C14 1.385(9) . ? C13 H13 0.9300 . ? C15 C14 1.369(9) . ? C15 H15 0.9300 . ? C14 H14 0.9300 . ? C7 H7 0.9300 . ? N14 C16 1.135(7) . ? C16 Cu2 1.885(6) 1_545 ? C16 Cu2 2.367(6) 2_676 ? 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 N14 Cu1 N9 133.8(2) . . ? N14 Cu1 N5 112.3(2) . . ? N9 Cu1 N5 113.79(19) . . ? C16 Cu2 N10 135.1(2) 1_565 . ? C16 Cu2 N8 129.9(3) 1_565 . ? N10 Cu2 N8 79.2(2) . . ? C16 Cu2 C16 106.3(2) 1_565 2_676 ? N10 Cu2 C16 101.9(2) . 2_676 ? N8 Cu2 C16 96.5(2) . 2_676 ? C16 Cu2 Cu2 61.77(19) 1_565 2_686 ? N10 Cu2 Cu2 135.10(16) . 2_686 ? N8 Cu2 Cu2 124.95(17) . 2_686 ? C16 Cu2 Cu2 44.58(15) 2_676 2_686 ? N6 Cu3 N11 144.5(2) 2_576 . ? N6 Cu3 N13 127.49(19) 2_576 . ? N11 Cu3 N13 80.79(19) . . ? N6 Cu3 N2 79.94(18) 2_576 2_576 ? N11 Cu3 N2 105.54(18) . 2_576 ? N13 Cu3 N2 120.33(19) . 2_576 ? C7 C8 C9 117.6(7) . . ? C7 C8 H8 121.2 . . ? C9 C8 H8 121.2 . . ? C5 N6 N5 105.3(4) . . ? C5 N6 Cu3 115.4(4) . 2_576 ? N5 N6 Cu3 139.2(4) . 2_576 ? C10 N9 C11 101.6(4) . . ? C10 N9 Cu1 138.7(4) . . ? C11 N9 Cu1 119.1(4) . . ? N11 C11 N9 114.1(5) . . ? N11 C11 C12 119.6(5) . . ? N9 C11 C12 126.1(5) . . ? N11 N10 C10 107.2(4) . . ? N11 N10 Cu2 137.9(3) . . ? C10 N10 Cu2 114.9(4) . . ? N4 N5 N6 108.3(4) . . ? N4 N5 Cu1 125.5(4) . . ? N6 N5 Cu1 124.7(3) . . ? C11 N11 N10 104.9(4) . . ? C11 N11 Cu3 112.8(4) . . ? N10 N11 Cu3 140.4(4) . . ? N6 C5 N3 111.0(5) . . ? N6 C5 C4 119.9(5) . . ? N3 C5 C4 129.0(5) . . ? C3 N2 C4 115.6(5) . . ? C3 N2 Cu3 133.0(4) . 2_576 ? C4 N2 Cu3 110.7(4) . 2_576 ? N9 C10 N10 112.2(5) . . ? N9 C10 C6 129.1(5) . . ? N10 C10 C6 118.4(5) . . ? C9 N8 C6 116.0(6) . . ? C9 N8 Cu2 130.9(5) . . ? C6 N8 Cu2 113.1(4) . . ? N5 N4 N3 110.4(4) . . ? N4 N3 C5 104.9(5) . . ? C7 N7 C6 115.3(6) . . ? N1 C4 N2 126.6(5) . . ? N1 C4 C5 119.4(5) . . ? N2 C4 C5 113.8(5) . . ? C1 N1 C4 115.4(6) . . ? N2 C3 C2 123.1(6) . . ? N2 C3 H3 118.5 . . ? C2 C3 H3 118.5 . . ? N7 C6 N8 125.8(6) . . ? N7 C6 C10 120.3(6) . . ? N8 C6 C10 113.9(5) . . ? C3 C2 C1 116.5(7) . . ? C3 C2 H2 121.8 . . ? C1 C2 H2 121.8 . . ? N8 C9 C8 121.8(7) . . ? N8 C9 H9 119.1 . . ? C8 C9 H9 119.1 . . ? N1 C1 C2 122.8(7) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C12 N13 C15 116.8(5) . . ? C12 N13 Cu3 111.3(4) . . ? C15 N13 Cu3 131.8(4) . . ? C12 N12 C13 115.8(5) . . ? N12 C12 N13 126.3(6) . . ? N12 C12 C11 118.5(5) . . ? N13 C12 C11 115.2(5) . . ? N12 C13 C14 122.3(6) . . ? N12 C13 H13 118.8 . . ? C14 C13 H13 118.8 . . ? N13 C15 C14 121.0(6) . . ? N13 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C14 C13 117.7(6) . . ? C15 C14 H14 121.2 . . ? C13 C14 H14 121.2 . . ? N7 C7 C8 123.5(7) . . ? N7 C7 H7 118.3 . . ? C8 C7 H7 118.3 . . ? C16 N14 Cu1 174.6(5) . . ? N14 C16 Cu2 174.5(5) . 1_545 ? N14 C16 Cu2 111.4(5) . 2_676 ? Cu2 C16 Cu2 73.7(2) 1_545 2_676 ? 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 N14 Cu1 N9 C10 -91.3(6) . . . . ? N5 Cu1 N9 C10 83.6(6) . . . . ? N14 Cu1 N9 C11 99.4(5) . . . . ? N5 Cu1 N9 C11 -85.7(4) . . . . ? C10 N9 C11 N11 -0.6(6) . . . . ? Cu1 N9 C11 N11 172.2(4) . . . . ? C10 N9 C11 C12 174.3(5) . . . . ? Cu1 N9 C11 C12 -12.9(7) . . . . ? C16 Cu2 N10 N11 45.1(7) 1_565 . . . ? N8 Cu2 N10 N11 -177.7(6) . . . . ? C16 Cu2 N10 N11 -83.2(6) 2_676 . . . ? Cu2 Cu2 N10 N11 -48.2(6) 2_686 . . . ? C16 Cu2 N10 C10 -132.5(4) 1_565 . . . ? N8 Cu2 N10 C10 4.7(4) . . . . ? C16 Cu2 N10 C10 99.2(4) 2_676 . . . ? Cu2 Cu2 N10 C10 134.2(4) 2_686 . . . ? C5 N6 N5 N4 -0.1(6) . . . . ? Cu3 N6 N5 N4 177.0(5) 2_576 . . . ? C5 N6 N5 Cu1 166.6(4) . . . . ? Cu3 N6 N5 Cu1 -16.3(8) 2_576 . . . ? N14 Cu1 N5 N4 22.9(6) . . . . ? N9 Cu1 N5 N4 -153.1(5) . . . . ? N14 Cu1 N5 N6 -141.5(4) . . . . ? N9 Cu1 N5 N6 42.5(5) . . . . ? N9 C11 N11 N10 0.5(6) . . . . ? C12 C11 N11 N10 -174.7(5) . . . . ? N9 C11 N11 Cu3 168.0(4) . . . . ? C12 C11 N11 Cu3 -7.2(6) . . . . ? C10 N10 N11 C11 -0.2(6) . . . . ? Cu2 N10 N11 C11 -177.9(5) . . . . ? C10 N10 N11 Cu3 -161.9(5) . . . . ? Cu2 N10 N11 Cu3 20.4(10) . . . . ? N6 Cu3 N11 C11 150.7(4) 2_576 . . . ? N13 Cu3 N11 C11 4.2(4) . . . . ? N2 Cu3 N11 C11 -114.8(4) 2_576 . . . ? N6 Cu3 N11 N10 -48.5(7) 2_576 . . . ? N13 Cu3 N11 N10 165.0(6) . . . . ? N2 Cu3 N11 N10 46.0(6) 2_576 . . . ? N5 N6 C5 N3 -0.4(7) . . . . ? Cu3 N6 C5 N3 -178.3(4) 2_576 . . . ? N5 N6 C5 C4 -177.2(5) . . . . ? Cu3 N6 C5 C4 4.9(7) 2_576 . . . ? C11 N9 C10 N10 0.4(6) . . . . ? Cu1 N9 C10 N10 -170.0(4) . . . . ? C11 N9 C10 C6 -173.2(6) . . . . ? Cu1 N9 C10 C6 16.4(10) . . . . ? N11 N10 C10 N9 -0.2(6) . . . . ? Cu2 N10 C10 N9 178.1(4) . . . . ? N11 N10 C10 C6 174.2(5) . . . . ? Cu2 N10 C10 C6 -7.5(7) . . . . ? C16 Cu2 N8 C9 -40.8(8) 1_565 . . . ? N10 Cu2 N8 C9 177.8(7) . . . . ? C16 Cu2 N8 C9 76.8(7) 2_676 . . . ? Cu2 Cu2 N8 C9 39.5(7) 2_686 . . . ? C16 Cu2 N8 C6 140.0(4) 1_565 . . . ? N10 Cu2 N8 C6 -1.4(4) . . . . ? C16 Cu2 N8 C6 -102.4(5) 2_676 . . . ? Cu2 Cu2 N8 C6 -139.7(4) 2_686 . . . ? N6 N5 N4 N3 0.6(7) . . . . ? Cu1 N5 N4 N3 -166.0(4) . . . . ? N5 N4 N3 C5 -0.9(7) . . . . ? N6 C5 N3 N4 0.8(7) . . . . ? C4 C5 N3 N4 177.2(6) . . . . ? C3 N2 C4 N1 -1.3(10) . . . . ? Cu3 N2 C4 N1 -172.5(6) 2_576 . . . ? C3 N2 C4 C5 174.9(5) . . . . ? Cu3 N2 C4 C5 3.6(6) 2_576 . . . ? N6 C5 C4 N1 170.7(6) . . . . ? N3 C5 C4 N1 -5.5(10) . . . . ? N6 C5 C4 N2 -5.8(8) . . . . ? N3 C5 C4 N2 178.1(6) . . . . ? N2 C4 N1 C1 0.8(11) . . . . ? C5 C4 N1 C1 -175.2(7) . . . . ? C4 N2 C3 C2 1.2(10) . . . . ? Cu3 N2 C3 C2 170.0(6) 2_576 . . . ? C7 N7 C6 N8 2.2(10) . . . . ? C7 N7 C6 C10 -177.5(6) . . . . ? C9 N8 C6 N7 -1.0(10) . . . . ? Cu2 N8 C6 N7 178.4(5) . . . . ? C9 N8 C6 C10 178.8(6) . . . . ? Cu2 N8 C6 C10 -1.9(7) . . . . ? N9 C10 C6 N7 -0.8(10) . . . . ? N10 C10 C6 N7 -174.0(5) . . . . ? N9 C10 C6 N8 179.5(6) . . . . ? N10 C10 C6 N8 6.2(8) . . . . ? N2 C3 C2 C1 -0.7(12) . . . . ? C6 N8 C9 C8 -1.7(11) . . . . ? Cu2 N8 C9 C8 179.1(6) . . . . ? C7 C8 C9 N8 3.0(12) . . . . ? C4 N1 C1 C2 -0.2(13) . . . . ? C3 C2 C1 N1 0.1(14) . . . . ? N6 Cu3 N13 C12 -156.9(4) 2_576 . . . ? N11 Cu3 N13 C12 -0.8(4) . . . . ? N2 Cu3 N13 C12 101.9(4) 2_576 . . . ? N6 Cu3 N13 C15 21.5(6) 2_576 . . . ? N11 Cu3 N13 C15 177.7(6) . . . . ? N2 Cu3 N13 C15 -79.6(6) 2_576 . . . ? C13 N12 C12 N13 -0.4(9) . . . . ? C13 N12 C12 C11 -177.5(5) . . . . ? C15 N13 C12 N12 1.5(9) . . . . ? Cu3 N13 C12 N12 -179.8(5) . . . . ? C15 N13 C12 C11 178.7(5) . . . . ? Cu3 N13 C12 C11 -2.6(6) . . . . ? N11 C11 C12 N12 -175.8(5) . . . . ? N9 C11 C12 N12 9.6(8) . . . . ? N11 C11 C12 N13 6.7(7) . . . . ? N9 C11 C12 N13 -167.8(5) . . . . ? C12 N12 C13 C14 -0.4(10) . . . . ? C12 N13 C15 C14 -1.8(9) . . . . ? Cu3 N13 C15 C14 179.8(5) . . . . ? N13 C15 C14 C13 1.2(10) . . . . ? N12 C13 C14 C15 0.0(10) . . . . ? C6 N7 C7 C8 -0.8(10) . . . . ? C9 C8 C7 N7 -1.6(12) . . . . ? N9 Cu1 N14 C16 -117(6) . . . . ? N5 Cu1 N14 C16 68(6) . . . . ? Cu1 N14 C16 Cu2 -43(11) . . . 1_545 ? Cu1 N14 C16 Cu2 115(6) . . . 2_676 ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.764 _refine_diff_density_min -0.477 _refine_diff_density_rms 0.120 data_2 _database_code_depnum_ccdc_archive 'CCDC 805597' #TrackingRef '- complexes1-3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H6 Cu2 N13' _chemical_formula_sum 'C11 H6 Cu2 N13' _chemical_formula_weight 447.37 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 16.039(2) _cell_length_b 9.0345(12) _cell_length_c 14.6031(19) _cell_angle_alpha 90.00 _cell_angle_beta 111.974(2) _cell_angle_gamma 90.00 _cell_volume 1962.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 940 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 20.48 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 884 _exptl_absorpt_coefficient_mu 2.190 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5595 _exptl_absorpt_correction_T_max 0.6685 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 5450 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1709 _reflns_number_gt 1373 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0900P)^2^+1.7414P] 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 1709 _refine_ls_number_parameters 118 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0599 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.1622 _refine_ls_wR_factor_gt 0.1563 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_restrained_S_all 1.125 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 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 0.16161(4) 0.49192(6) 0.09620(5) 0.0720(3) Uani 1 1 d . . . N6 N 0.2306(2) 0.0359(4) 0.4522(3) 0.0558(9) Uani 1 1 d . . . N2 N 0.1947(2) 0.3189(4) 0.1929(3) 0.0648(10) Uani 1 1 d . . . C1 C 0.1931(2) 0.1957(4) 0.3147(3) 0.0501(9) Uani 1 1 d . . . C2 C 0.1709(3) 0.1347(4) 0.3951(3) 0.0507(9) Uani 1 1 d . . . N1 N 0.1451(2) 0.2929(4) 0.2474(3) 0.0614(9) Uani 1 1 d . . . N5 N 0.0977(2) 0.1853(4) 0.4074(3) 0.0648(10) Uani 1 1 d . . . N3 N 0.2691(2) 0.2403(4) 0.2258(3) 0.0622(10) Uani 1 1 d . . . C5 C 0.0856(4) 0.1328(6) 0.4863(4) 0.0766(14) Uani 1 1 d . . . H5 H 0.0364 0.1666 0.4994 0.092 Uiso 1 1 calc R . . C4 C 0.1418(4) 0.0308(7) 0.5500(5) 0.0811(16) Uani 1 1 d . . . H4 H 0.1314 -0.0046 0.6046 0.097 Uiso 1 1 calc R . . C3 C 0.2141(4) -0.0159(5) 0.5286(4) 0.0718(14) Uani 1 1 d . . . H3 H 0.2528 -0.0862 0.5693 0.086 Uiso 1 1 calc R . . N4 N 0.2693(2) 0.1615(4) 0.3029(3) 0.0554(8) Uani 1 1 d . . . C7 C 0.0385(3) 0.5004(4) 0.0205(4) 0.0652(11) Uani 0.50 1 d P . 1 N7 N 0.0385(3) 0.5004(4) 0.0205(4) 0.0652(11) Uani 0.50 1 d P . 2 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 0.0439(4) 0.0820(5) 0.0772(5) 0.0143(3) 0.0077(3) -0.0142(2) N6 0.048(2) 0.063(2) 0.055(2) -0.0049(16) 0.0176(17) 0.0046(16) N2 0.046(2) 0.070(2) 0.075(2) 0.0135(19) 0.0187(18) -0.0011(17) C1 0.0351(19) 0.051(2) 0.059(2) -0.0030(18) 0.0115(17) 0.0005(16) C2 0.0383(19) 0.054(2) 0.058(2) -0.0141(18) 0.0166(17) -0.0044(17) N1 0.0383(17) 0.066(2) 0.079(2) 0.0154(19) 0.0205(17) 0.0005(16) N5 0.056(2) 0.057(2) 0.091(3) -0.0110(19) 0.038(2) 0.0013(17) N3 0.0472(19) 0.074(2) 0.065(2) 0.0037(18) 0.0204(18) 0.0001(17) C5 0.075(3) 0.080(3) 0.097(4) -0.017(3) 0.058(3) -0.006(3) C4 0.089(4) 0.096(4) 0.073(3) -0.007(3) 0.046(3) -0.011(3) C3 0.074(3) 0.083(3) 0.058(3) -0.001(2) 0.024(3) 0.002(2) N4 0.0426(18) 0.063(2) 0.060(2) 0.0006(17) 0.0180(16) 0.0058(16) C7 0.047(2) 0.072(3) 0.069(3) 0.0044(18) 0.012(2) -0.0123(19) N7 0.047(2) 0.072(3) 0.069(3) 0.0044(18) 0.012(2) -0.0123(19) _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 C7 1.869(5) . ? Cu1 N2 2.040(4) . ? Cu1 N4 2.127(4) 4 ? Cu1 N6 2.135(3) 4 ? N6 C3 1.325(6) . ? N6 C2 1.347(5) . ? N6 Cu1 2.135(3) 4_545 ? N2 N3 1.316(5) . ? N2 N1 1.340(5) . ? C1 N1 1.328(5) . ? C1 N4 1.331(5) . ? C1 C2 1.456(6) . ? C2 N5 1.334(5) . ? N5 C5 1.326(6) . ? N3 N4 1.332(5) . ? C5 C4 1.378(8) . ? C5 H5 0.9300 . ? C4 C3 1.375(7) . ? C4 H4 0.9300 . ? C3 H3 0.9300 . ? N4 Cu1 2.127(4) 4_545 ? C7 C7 1.153(9) 5_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C7 Cu1 N2 112.60(16) . . ? C7 Cu1 N4 122.79(16) . 4 ? N2 Cu1 N4 98.02(16) . 4 ? C7 Cu1 N6 127.12(17) . 4 ? N2 Cu1 N6 109.81(14) . 4 ? N4 Cu1 N6 79.55(13) 4 4 ? C3 N6 C2 115.9(4) . . ? C3 N6 Cu1 130.9(3) . 4_545 ? C2 N6 Cu1 113.2(3) . 4_545 ? N3 N2 N1 110.4(3) . . ? N3 N2 Cu1 129.1(3) . . ? N1 N2 Cu1 119.1(3) . . ? N1 C1 N4 111.4(4) . . ? N1 C1 C2 126.6(3) . . ? N4 C1 C2 121.9(4) . . ? N5 C2 N6 127.0(4) . . ? N5 C2 C1 118.2(4) . . ? N6 C2 C1 114.8(3) . . ? C1 N1 N2 104.2(3) . . ? C5 N5 C2 114.7(4) . . ? N2 N3 N4 108.1(3) . . ? N5 C5 C4 123.6(4) . . ? N5 C5 H5 118.2 . . ? C4 C5 H5 118.2 . . ? C3 C4 C5 116.5(5) . . ? C3 C4 H4 121.8 . . ? C5 C4 H4 121.8 . . ? N6 C3 C4 122.3(5) . . ? N6 C3 H3 118.8 . . ? C4 C3 H3 118.8 . . ? N3 N4 C1 105.8(3) . . ? N3 N4 Cu1 143.7(3) . 4_545 ? C1 N4 Cu1 110.1(3) . 4_545 ? C7 C7 Cu1 174.8(6) 5_565 . ? 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 C7 Cu1 N2 N3 148.3(4) . . . . ? N4 Cu1 N2 N3 -81.1(4) 4 . . . ? N6 Cu1 N2 N3 0.6(4) 4 . . . ? C7 Cu1 N2 N1 -46.1(4) . . . . ? N4 Cu1 N2 N1 84.6(3) 4 . . . ? N6 Cu1 N2 N1 166.3(3) 4 . . . ? C3 N6 C2 N5 0.0(6) . . . . ? Cu1 N6 C2 N5 -179.1(3) 4_545 . . . ? C3 N6 C2 C1 176.9(4) . . . . ? Cu1 N6 C2 C1 -2.2(4) 4_545 . . . ? N1 C1 C2 N5 -3.8(6) . . . . ? N4 C1 C2 N5 173.7(4) . . . . ? N1 C1 C2 N6 179.0(4) . . . . ? N4 C1 C2 N6 -3.5(6) . . . . ? N4 C1 N1 N2 -0.3(5) . . . . ? C2 C1 N1 N2 177.5(4) . . . . ? N3 N2 N1 C1 0.2(5) . . . . ? Cu1 N2 N1 C1 -168.0(3) . . . . ? N6 C2 N5 C5 1.6(6) . . . . ? C1 C2 N5 C5 -175.2(4) . . . . ? N1 N2 N3 N4 -0.1(5) . . . . ? Cu1 N2 N3 N4 166.6(3) . . . . ? C2 N5 C5 C4 -1.8(7) . . . . ? N5 C5 C4 C3 0.4(8) . . . . ? C2 N6 C3 C4 -1.5(7) . . . . ? Cu1 N6 C3 C4 177.4(4) 4_545 . . . ? C5 C4 C3 N6 1.3(8) . . . . ? N2 N3 N4 C1 0.0(4) . . . . ? N2 N3 N4 Cu1 172.3(4) . . . 4_545 ? N1 C1 N4 N3 0.2(5) . . . . ? C2 C1 N4 N3 -177.6(4) . . . . ? N1 C1 N4 Cu1 -175.0(3) . . . 4_545 ? C2 C1 N4 Cu1 7.2(5) . . . 4_545 ? N2 Cu1 C7 C7 24(6) . . . 5_565 ? N4 Cu1 C7 C7 -93(6) 4 . . 5_565 ? N6 Cu1 C7 C7 164(6) 4 . . 5_565 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.468 _refine_diff_density_min -0.244 _refine_diff_density_rms 0.080 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.233 0.250 120 35 ' ' 2 0.000 -0.267 0.250 121 35 ' ' 3 0.500 -0.233 0.750 121 35 ' ' 4 0.000 0.267 0.750 121 35 ' ' _platon_squeeze_details ; ; data_3 _database_code_depnum_ccdc_archive 'CCDC 805598' #TrackingRef '- complexes1-3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H12 Cu4 N16' _chemical_formula_weight 754.64 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.3754(15) _cell_length_b 10.891(2) _cell_length_c 14.418(3) _cell_angle_alpha 96.696(3) _cell_angle_beta 101.866(3) _cell_angle_gamma 96.275(3) _cell_volume 1266.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 13481 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.93 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 1.979 _exptl_crystal_density_diffrn 1.979 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 3.363 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.4319 _exptl_absorpt_correction_T_max 0.7297 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 8878 _diffrn_reflns_av_R_equivalents 0.0206 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4375 _reflns_number_gt 3619 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0581P)^2^+1.8747P] 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 4375 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0528 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1183 _refine_ls_wR_factor_gt 0.1111 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 0.24732(7) 0.10103(5) 0.66302(4) 0.04631(18) Uani 1 1 d . . . Cu4 Cu -0.20438(7) 0.31488(5) 0.66491(5) 0.05011(19) Uani 1 1 d . . . Cu3 Cu 0.30902(9) 0.76275(6) 0.95392(5) 0.0612(2) Uani 1 1 d . . . Cu2 Cu 0.14778(9) 0.25285(5) 0.93383(6) 0.0642(2) Uani 1 1 d . . . C1 C 0.2664(5) 0.5186(3) 1.0007(3) 0.0328(9) Uani 1 1 d . . . N5 N 0.3153(4) -0.0842(3) 0.9025(2) 0.0335(7) Uani 1 1 d . . . N9 N 0.3485(4) 0.6332(3) 1.0356(2) 0.0360(8) Uani 1 1 d . . . N8 N 0.2894(5) 0.4154(3) 1.0392(3) 0.0412(9) Uani 1 1 d . . . N10 N 0.0556(4) 0.3933(3) 0.8730(2) 0.0385(8) Uani 1 1 d . . . N3 N 0.2853(5) 0.0639(3) 0.8085(2) 0.0372(8) Uani 1 1 d . . . N12 N 0.1266(4) 0.5931(3) 0.8543(3) 0.0378(8) Uani 1 1 d . . . N2 N 0.3420(4) -0.0724(3) 0.6548(2) 0.0371(8) Uani 1 1 d . . . N4 N 0.2436(4) 0.1057(3) 0.8919(2) 0.0367(8) Uani 1 1 d . . . C10 C 0.3266(5) -0.0493(4) 0.8174(3) 0.0321(9) Uani 1 1 d . . . N11 N -0.0319(4) 0.4122(3) 0.7860(3) 0.0406(8) Uani 1 1 d . . . C12 C 0.3771(5) -0.1193(4) 0.7381(3) 0.0357(9) Uani 1 1 d . . . N6 N 0.1486(5) 0.1263(3) 1.0621(3) 0.0429(9) Uani 1 1 d . . . C14 C 0.2633(5) 0.0155(3) 0.9461(3) 0.0316(9) Uani 1 1 d . . . N13 N -0.1454(5) 0.4928(4) 0.6192(3) 0.0460(9) Uani 1 1 d . . . N7 N 0.2507(5) -0.0657(4) 1.0916(3) 0.0491(10) Uani 1 1 d . . . C17 C 0.1462(5) 0.5039(4) 0.9103(3) 0.0344(9) Uani 1 1 d . . . N1 N 0.4552(5) -0.2178(3) 0.7527(3) 0.0427(9) Uani 1 1 d . . . C19 C 0.2196(5) 0.0254(4) 1.0397(3) 0.0359(9) Uani 1 1 d . . . C20 C 0.3939(6) -0.1290(4) 0.5813(3) 0.0448(11) Uani 1 1 d . . . H20 H 0.3725 -0.0989 0.5229 0.054 Uiso 1 1 calc R . . N14 N 0.0074(5) 0.6946(4) 0.6775(3) 0.0480(10) Uani 1 1 d . . . N16 N 0.4420(5) 0.2104(4) 0.6522(3) 0.0489(9) Uani 1 1 d . . . N15 N 0.0265(6) 0.1394(5) 0.6220(3) 0.0657(13) Uani 1 1 d . . . C24 C 0.0160(5) 0.5311(4) 0.7773(3) 0.0369(9) Uani 1 1 d . . . C25 C 0.5710(6) 0.2588(4) 0.6565(3) 0.0409(10) Uani 1 1 d . . . C26 C 0.4041(6) 0.4272(4) 1.1202(3) 0.0477(11) Uani 1 1 d . . . H26 H 0.4273 0.3563 1.1478 0.057 Uiso 1 1 calc R . . C27 C -0.0835(5) 0.1896(4) 0.6145(3) 0.0416(10) Uani 1 1 d . . . C28 C 0.5039(7) -0.2714(5) 0.6774(4) 0.0572(14) Uani 1 1 d . . . H28 H 0.5587 -0.3407 0.6844 0.069 Uiso 1 1 calc R . . C29 C 0.4569(6) 0.6434(4) 1.1189(3) 0.0443(11) Uani 1 1 d . . . H29 H 0.5124 0.7217 1.1473 0.053 Uiso 1 1 calc R . . C30 C -0.0444(5) 0.5777(4) 0.6867(3) 0.0380(9) Uani 1 1 d . . . C31 C 0.4890(6) 0.5416(4) 1.1640(3) 0.0472(11) Uani 1 1 d . . . H31 H 0.5652 0.5496 1.2219 0.057 Uiso 1 1 calc R . . C32 C -0.0477(7) 0.7291(5) 0.5914(4) 0.0544(13) Uani 1 1 d . . . H32 H -0.0156 0.8102 0.5817 0.065 Uiso 1 1 calc R . . C33 C 0.1071(6) 0.1352(5) 1.1466(4) 0.0537(12) Uani 1 1 d . . . H33 H 0.0593 0.2041 1.1662 0.064 Uiso 1 1 calc R . . C34 C 0.2056(7) -0.0532(6) 1.1763(4) 0.0620(14) Uani 1 1 d . . . H34 H 0.2249 -0.1140 1.2160 0.074 Uiso 1 1 calc R . . C35 C 0.4774(7) -0.2296(5) 0.5895(3) 0.0548(13) Uani 1 1 d . . . H35 H 0.5145 -0.2679 0.5384 0.066 Uiso 1 1 calc R . . C36 C -0.1971(6) 0.5306(5) 0.5343(4) 0.0556(13) Uani 1 1 d . . . H36 H -0.2672 0.4746 0.4854 0.067 Uiso 1 1 calc R . . C37 C 0.1326(7) 0.0460(5) 1.2059(4) 0.0602(14) Uani 1 1 d . . . H37 H 0.1011 0.0528 1.2643 0.072 Uiso 1 1 calc R . . C38 C -0.1504(7) 0.6483(5) 0.5170(4) 0.0559(13) Uani 1 1 d . . . H38 H -0.1864 0.6730 0.4574 0.067 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 0.0471(3) 0.0477(3) 0.0483(4) 0.0250(3) 0.0081(3) 0.0099(3) Cu4 0.0452(3) 0.0457(3) 0.0547(4) 0.0065(3) 0.0052(3) -0.0030(3) Cu3 0.0815(5) 0.0350(3) 0.0845(5) 0.0352(3) 0.0367(4) 0.0204(3) Cu2 0.0700(4) 0.0240(3) 0.0994(6) 0.0128(3) 0.0164(4) 0.0110(3) C1 0.043(2) 0.0226(19) 0.035(2) 0.0068(16) 0.0102(18) 0.0068(16) N5 0.0439(19) 0.0234(16) 0.0324(18) 0.0101(14) 0.0049(15) 0.0011(14) N9 0.050(2) 0.0238(17) 0.0334(19) 0.0063(14) 0.0054(16) 0.0043(15) N8 0.061(2) 0.0242(17) 0.038(2) 0.0095(15) 0.0058(18) 0.0086(16) N10 0.046(2) 0.0296(18) 0.036(2) 0.0089(15) 0.0005(16) 0.0031(15) N3 0.053(2) 0.0290(18) 0.0308(19) 0.0117(14) 0.0072(16) 0.0058(15) N12 0.045(2) 0.0282(18) 0.040(2) 0.0084(15) 0.0046(16) 0.0065(15) N2 0.043(2) 0.0365(19) 0.0306(19) 0.0108(15) 0.0018(15) 0.0066(15) N4 0.056(2) 0.0244(17) 0.0292(18) 0.0088(14) 0.0058(16) 0.0040(15) C10 0.040(2) 0.025(2) 0.031(2) 0.0098(16) 0.0044(17) 0.0035(16) N11 0.045(2) 0.0335(19) 0.040(2) 0.0081(16) 0.0010(16) 0.0025(16) C12 0.041(2) 0.032(2) 0.032(2) 0.0094(17) 0.0023(18) 0.0013(18) N6 0.051(2) 0.0320(19) 0.043(2) 0.0017(16) 0.0107(18) -0.0029(16) C14 0.039(2) 0.0203(19) 0.033(2) 0.0070(16) 0.0027(17) 0.0002(16) N13 0.047(2) 0.047(2) 0.041(2) 0.0149(18) 0.0011(18) -0.0003(18) N7 0.068(3) 0.046(2) 0.039(2) 0.0204(18) 0.0157(19) 0.0121(19) C17 0.042(2) 0.026(2) 0.035(2) 0.0056(17) 0.0071(18) 0.0057(17) N1 0.057(2) 0.039(2) 0.036(2) 0.0113(16) 0.0100(17) 0.0179(18) C19 0.044(2) 0.028(2) 0.031(2) 0.0061(17) 0.0013(18) -0.0034(18) C20 0.055(3) 0.050(3) 0.029(2) 0.011(2) 0.006(2) 0.007(2) N14 0.060(3) 0.040(2) 0.043(2) 0.0128(17) 0.0064(19) 0.0041(18) N16 0.051(2) 0.051(2) 0.046(2) 0.0163(19) 0.0103(19) 0.0030(19) N15 0.079(3) 0.071(3) 0.043(3) 0.014(2) 0.012(2) -0.013(3) C24 0.039(2) 0.031(2) 0.038(2) 0.0076(18) 0.0027(19) 0.0050(18) C25 0.043(3) 0.043(2) 0.034(2) 0.0056(19) 0.0056(19) 0.003(2) C26 0.069(3) 0.037(2) 0.039(3) 0.015(2) 0.006(2) 0.019(2) C27 0.025(2) 0.051(3) 0.051(3) 0.009(2) 0.0051(19) 0.020(2) C28 0.078(4) 0.054(3) 0.045(3) 0.009(2) 0.013(3) 0.031(3) C29 0.058(3) 0.036(2) 0.032(2) 0.0031(18) 0.002(2) -0.005(2) C30 0.040(2) 0.038(2) 0.037(2) 0.0121(19) 0.0061(19) 0.0071(18) C31 0.061(3) 0.051(3) 0.028(2) 0.009(2) 0.000(2) 0.011(2) C32 0.068(3) 0.048(3) 0.049(3) 0.022(2) 0.009(3) 0.008(2) C33 0.060(3) 0.049(3) 0.051(3) -0.004(2) 0.020(2) -0.001(2) C34 0.076(4) 0.069(4) 0.041(3) 0.026(3) 0.009(3) -0.001(3) C35 0.073(3) 0.058(3) 0.035(3) 0.006(2) 0.011(2) 0.019(3) C36 0.057(3) 0.062(3) 0.042(3) 0.015(2) -0.002(2) -0.001(2) C37 0.069(3) 0.071(4) 0.040(3) 0.001(3) 0.023(3) -0.006(3) C38 0.063(3) 0.062(3) 0.045(3) 0.027(3) 0.005(2) 0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N15 1.929(6) . ? Cu1 N16 1.956(4) . ? Cu1 N2 2.127(3) . ? Cu1 N3 2.149(3) . ? Cu4 C25 1.888(5) 1_455 ? Cu4 C27 1.947(4) . ? Cu4 N11 2.111(4) . ? Cu4 N13 2.158(4) . ? Cu3 N5 1.901(3) 1_565 ? Cu3 N9 1.953(3) . ? Cu3 N12 2.382(4) . ? Cu2 N4 1.958(3) . ? Cu2 N10 2.000(3) . ? Cu2 N8 2.241(4) . ? Cu2 N6 2.431(4) . ? C1 N8 1.326(5) . ? C1 N9 1.344(5) . ? C1 C17 1.455(6) . ? N5 C10 1.345(5) . ? N5 C14 1.349(5) . ? N5 Cu3 1.901(3) 1_545 ? N9 C29 1.334(5) . ? N8 C26 1.334(6) . ? N10 C17 1.341(5) . ? N10 N11 1.367(5) . ? N3 C10 1.330(5) . ? N3 N4 1.362(5) . ? N12 C17 1.336(5) . ? N12 C24 1.346(5) . ? N2 C20 1.337(6) . ? N2 C12 1.348(5) . ? N4 C14 1.328(5) . ? C10 C12 1.460(6) . ? N11 C24 1.341(5) . ? C12 N1 1.331(5) . ? N6 C33 1.330(6) . ? N6 C19 1.344(6) . ? C14 C19 1.464(6) . ? N13 C36 1.339(6) . ? N13 C30 1.341(6) . ? N7 C19 1.327(5) . ? N7 C34 1.348(6) . ? N1 C28 1.331(6) . ? C20 C35 1.367(7) . ? C20 H20 0.9300 . ? N14 C30 1.330(6) . ? N14 C32 1.344(6) . ? N16 C25 1.135(6) . ? N15 C27 1.114(6) . ? C24 C30 1.469(6) . ? C25 Cu4 1.888(5) 1_655 ? C26 C31 1.377(7) . ? C26 H26 0.9300 . ? C28 C35 1.380(7) . ? C28 H28 0.9300 . ? C29 C31 1.373(6) . ? C29 H29 0.9300 . ? C31 H31 0.9300 . ? C32 C38 1.378(8) . ? C32 H32 0.9300 . ? C33 C37 1.373(8) . ? C33 H33 0.9300 . ? C34 C37 1.366(8) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C38 1.366(7) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N15 Cu1 N16 122.57(18) . . ? N15 Cu1 N2 130.72(17) . . ? N16 Cu1 N2 99.11(15) . . ? N15 Cu1 N3 109.56(16) . . ? N16 Cu1 N3 107.31(15) . . ? N2 Cu1 N3 77.48(13) . . ? C25 Cu4 C27 114.47(19) 1_455 . ? C25 Cu4 N11 127.26(17) 1_455 . ? C27 Cu4 N11 103.16(17) . . ? C25 Cu4 N13 117.23(17) 1_455 . ? C27 Cu4 N13 111.43(18) . . ? N11 Cu4 N13 77.83(14) . . ? N5 Cu3 N9 164.12(15) 1_565 . ? N5 Cu3 N12 114.88(14) 1_565 . ? N9 Cu3 N12 80.99(13) . . ? N4 Cu2 N10 136.06(15) . . ? N4 Cu2 N8 123.86(15) . . ? N10 Cu2 N8 80.03(13) . . ? N4 Cu2 N6 75.85(13) . . ? N10 Cu2 N6 145.98(14) . . ? N8 Cu2 N6 90.36(12) . . ? N8 C1 N9 126.0(4) . . ? N8 C1 C17 116.2(4) . . ? N9 C1 C17 117.7(3) . . ? C10 N5 C14 102.3(3) . . ? C10 N5 Cu3 135.6(3) . 1_545 ? C14 N5 Cu3 120.3(3) . 1_545 ? C29 N9 C1 116.1(3) . . ? C29 N9 Cu3 127.2(3) . . ? C1 N9 Cu3 116.5(3) . . ? C1 N8 C26 116.6(4) . . ? C1 N8 Cu2 108.1(3) . . ? C26 N8 Cu2 134.4(3) . . ? C17 N10 N11 104.7(3) . . ? C17 N10 Cu2 112.1(3) . . ? N11 N10 Cu2 138.1(3) . . ? C10 N3 N4 106.1(3) . . ? C10 N3 Cu1 112.3(3) . . ? N4 N3 Cu1 139.2(3) . . ? C17 N12 C24 101.3(3) . . ? C17 N12 Cu3 100.3(3) . . ? C24 N12 Cu3 158.5(3) . . ? C20 N2 C12 116.6(4) . . ? C20 N2 Cu1 127.2(3) . . ? C12 N2 Cu1 115.4(3) . . ? C14 N4 N3 106.1(3) . . ? C14 N4 Cu2 120.5(3) . . ? N3 N4 Cu2 133.1(2) . . ? N3 C10 N5 112.7(4) . . ? N3 C10 C12 119.1(3) . . ? N5 C10 C12 128.2(3) . . ? C24 N11 N10 105.9(3) . . ? C24 N11 Cu4 113.5(3) . . ? N10 N11 Cu4 140.6(3) . . ? N1 C12 N2 125.9(4) . . ? N1 C12 C10 119.9(4) . . ? N2 C12 C10 114.2(4) . . ? C33 N6 C19 115.4(4) . . ? C33 N6 Cu2 137.2(3) . . ? C19 N6 Cu2 107.3(3) . . ? N4 C14 N5 112.7(3) . . ? N4 C14 C19 121.1(4) . . ? N5 C14 C19 126.1(3) . . ? C36 N13 C30 116.0(4) . . ? C36 N13 Cu4 129.4(3) . . ? C30 N13 Cu4 114.6(3) . . ? C19 N7 C34 115.1(4) . . ? N12 C17 N10 114.7(4) . . ? N12 C17 C1 124.1(4) . . ? N10 C17 C1 121.0(4) . . ? C28 N1 C12 115.4(4) . . ? N7 C19 N6 127.4(4) . . ? N7 C19 C14 117.4(4) . . ? N6 C19 C14 115.1(4) . . ? N2 C20 C35 122.0(4) . . ? N2 C20 H20 119.0 . . ? C35 C20 H20 119.0 . . ? C30 N14 C32 115.8(4) . . ? C25 N16 Cu1 166.6(4) . . ? C27 N15 Cu1 161.5(5) . . ? N11 C24 N12 113.5(4) . . ? N11 C24 C30 119.4(4) . . ? N12 C24 C30 127.0(4) . . ? N16 C25 Cu4 171.2(4) . 1_655 ? N8 C26 C31 121.7(4) . . ? N8 C26 H26 119.2 . . ? C31 C26 H26 119.2 . . ? N15 C27 Cu4 150.2(4) . . ? N1 C28 C35 123.5(5) . . ? N1 C28 H28 118.3 . . ? C35 C28 H28 118.3 . . ? N9 C29 C31 121.9(4) . . ? N9 C29 H29 119.1 . . ? C31 C29 H29 119.1 . . ? N14 C30 N13 126.4(4) . . ? N14 C30 C24 119.1(4) . . ? N13 C30 C24 114.4(4) . . ? C29 C31 C26 117.5(4) . . ? C29 C31 H31 121.2 . . ? C26 C31 H31 121.2 . . ? N14 C32 C38 122.2(5) . . ? N14 C32 H32 118.9 . . ? C38 C32 H32 118.9 . . ? N6 C33 C37 122.1(5) . . ? N6 C33 H33 119.0 . . ? C37 C33 H33 119.0 . . ? N7 C34 C37 122.1(5) . . ? N7 C34 H34 118.9 . . ? C37 C34 H34 118.9 . . ? C20 C35 C28 116.7(5) . . ? C20 C35 H35 121.7 . . ? C28 C35 H35 121.7 . . ? N13 C36 C38 122.3(5) . . ? N13 C36 H36 118.8 . . ? C38 C36 H36 118.8 . . ? C34 C37 C33 117.9(5) . . ? C34 C37 H37 121.1 . . ? C33 C37 H37 121.1 . . ? C36 C38 C32 117.3(4) . . ? C36 C38 H38 121.4 . . ? C32 C38 H38 121.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N8 C1 N9 C29 -3.4(6) . . . . ? C17 C1 N9 C29 179.6(4) . . . . ? N8 C1 N9 Cu3 171.7(3) . . . . ? C17 C1 N9 Cu3 -5.3(5) . . . . ? N5 Cu3 N9 C29 -2.4(8) 1_565 . . . ? N12 Cu3 N9 C29 176.1(4) . . . . ? N5 Cu3 N9 C1 -177.0(5) 1_565 . . . ? N12 Cu3 N9 C1 1.5(3) . . . . ? N9 C1 N8 C26 0.4(6) . . . . ? C17 C1 N8 C26 177.4(4) . . . . ? N9 C1 N8 Cu2 -170.0(3) . . . . ? C17 C1 N8 Cu2 7.0(4) . . . . ? N4 Cu2 N8 C1 128.0(3) . . . . ? N10 Cu2 N8 C1 -11.7(3) . . . . ? N6 Cu2 N8 C1 -158.8(3) . . . . ? N4 Cu2 N8 C26 -40.0(5) . . . . ? N10 Cu2 N8 C26 -179.6(5) . . . . ? N6 Cu2 N8 C26 33.2(5) . . . . ? N4 Cu2 N10 C17 -115.1(3) . . . . ? N8 Cu2 N10 C17 14.1(3) . . . . ? N6 Cu2 N10 C17 89.7(4) . . . . ? N4 Cu2 N10 N11 34.4(5) . . . . ? N8 Cu2 N10 N11 163.7(4) . . . . ? N6 Cu2 N10 N11 -120.8(4) . . . . ? N15 Cu1 N3 C10 121.6(3) . . . . ? N16 Cu1 N3 C10 -103.3(3) . . . . ? N2 Cu1 N3 C10 -7.5(3) . . . . ? N15 Cu1 N3 N4 -37.4(5) . . . . ? N16 Cu1 N3 N4 97.7(4) . . . . ? N2 Cu1 N3 N4 -166.5(4) . . . . ? N5 Cu3 N12 C17 -178.1(2) 1_565 . . . ? N9 Cu3 N12 C17 2.4(3) . . . . ? N5 Cu3 N12 C24 1.4(9) 1_565 . . . ? N9 Cu3 N12 C24 -178.2(8) . . . . ? N15 Cu1 N2 C20 86.5(4) . . . . ? N16 Cu1 N2 C20 -62.5(4) . . . . ? N3 Cu1 N2 C20 -168.4(4) . . . . ? N15 Cu1 N2 C12 -104.9(3) . . . . ? N16 Cu1 N2 C12 106.1(3) . . . . ? N3 Cu1 N2 C12 0.2(3) . . . . ? C10 N3 N4 C14 0.4(4) . . . . ? Cu1 N3 N4 C14 160.1(3) . . . . ? C10 N3 N4 Cu2 -172.6(3) . . . . ? Cu1 N3 N4 Cu2 -12.8(6) . . . . ? N10 Cu2 N4 C14 -166.2(3) . . . . ? N8 Cu2 N4 C14 80.5(3) . . . . ? N6 Cu2 N4 C14 -0.2(3) . . . . ? N10 Cu2 N4 N3 6.0(5) . . . . ? N8 Cu2 N4 N3 -107.4(4) . . . . ? N6 Cu2 N4 N3 171.9(4) . . . . ? N4 N3 C10 N5 -0.4(5) . . . . ? Cu1 N3 C10 N5 -166.2(3) . . . . ? N4 N3 C10 C12 179.7(3) . . . . ? Cu1 N3 C10 C12 13.9(5) . . . . ? C14 N5 C10 N3 0.2(5) . . . . ? Cu3 N5 C10 N3 164.2(3) 1_545 . . . ? C14 N5 C10 C12 -179.9(4) . . . . ? Cu3 N5 C10 C12 -15.9(7) 1_545 . . . ? C17 N10 N11 C24 1.4(4) . . . . ? Cu2 N10 N11 C24 -149.5(4) . . . . ? C17 N10 N11 Cu4 178.6(4) . . . . ? Cu2 N10 N11 Cu4 27.6(7) . . . . ? C25 Cu4 N11 C24 -110.8(3) 1_455 . . . ? C27 Cu4 N11 C24 113.8(3) . . . . ? N13 Cu4 N11 C24 4.3(3) . . . . ? C25 Cu4 N11 N10 72.2(5) 1_455 . . . ? C27 Cu4 N11 N10 -63.2(5) . . . . ? N13 Cu4 N11 N10 -172.7(5) . . . . ? C20 N2 C12 N1 -1.6(6) . . . . ? Cu1 N2 C12 N1 -171.4(3) . . . . ? C20 N2 C12 C10 176.4(4) . . . . ? Cu1 N2 C12 C10 6.5(4) . . . . ? N3 C10 C12 N1 164.1(4) . . . . ? N5 C10 C12 N1 -15.8(7) . . . . ? N3 C10 C12 N2 -14.0(6) . . . . ? N5 C10 C12 N2 166.1(4) . . . . ? N4 Cu2 N6 C33 177.9(5) . . . . ? N10 Cu2 N6 C33 -19.6(6) . . . . ? N8 Cu2 N6 C33 52.9(5) . . . . ? N4 Cu2 N6 C19 2.5(3) . . . . ? N10 Cu2 N6 C19 165.0(3) . . . . ? N8 Cu2 N6 C19 -122.5(3) . . . . ? N3 N4 C14 N5 -0.3(5) . . . . ? Cu2 N4 C14 N5 173.8(3) . . . . ? N3 N4 C14 C19 -176.2(4) . . . . ? Cu2 N4 C14 C19 -2.2(5) . . . . ? C10 N5 C14 N4 0.0(5) . . . . ? Cu3 N5 C14 N4 -167.0(3) 1_545 . . . ? C10 N5 C14 C19 175.8(4) . . . . ? Cu3 N5 C14 C19 8.7(5) 1_545 . . . ? C25 Cu4 N13 C36 -57.4(5) 1_455 . . . ? C27 Cu4 N13 C36 77.2(5) . . . . ? N11 Cu4 N13 C36 176.7(5) . . . . ? C25 Cu4 N13 C30 121.4(3) 1_455 . . . ? C27 Cu4 N13 C30 -104.0(3) . . . . ? N11 Cu4 N13 C30 -4.5(3) . . . . ? C24 N12 C17 N10 -0.2(5) . . . . ? Cu3 N12 C17 N10 179.6(3) . . . . ? C24 N12 C17 C1 174.1(4) . . . . ? Cu3 N12 C17 C1 -6.1(4) . . . . ? N11 N10 C17 N12 -0.8(5) . . . . ? Cu2 N10 C17 N12 158.7(3) . . . . ? N11 N10 C17 C1 -175.3(4) . . . . ? Cu2 N10 C17 C1 -15.7(5) . . . . ? N8 C1 C17 N12 -168.8(4) . . . . ? N9 C1 C17 N12 8.5(6) . . . . ? N8 C1 C17 N10 5.1(6) . . . . ? N9 C1 C17 N10 -177.6(4) . . . . ? N2 C12 N1 C28 1.3(7) . . . . ? C10 C12 N1 C28 -176.6(4) . . . . ? C34 N7 C19 N6 -0.4(7) . . . . ? C34 N7 C19 C14 -178.9(4) . . . . ? C33 N6 C19 N7 0.8(7) . . . . ? Cu2 N6 C19 N7 177.4(4) . . . . ? C33 N6 C19 C14 179.3(4) . . . . ? Cu2 N6 C19 C14 -4.1(4) . . . . ? N4 C14 C19 N7 -176.7(4) . . . . ? N5 C14 C19 N7 7.9(6) . . . . ? N4 C14 C19 N6 4.7(6) . . . . ? N5 C14 C19 N6 -170.7(4) . . . . ? C12 N2 C20 C35 0.4(7) . . . . ? Cu1 N2 C20 C35 168.9(4) . . . . ? N15 Cu1 N16 C25 170.2(17) . . . . ? N2 Cu1 N16 C25 -37.4(18) . . . . ? N3 Cu1 N16 C25 42.3(18) . . . . ? N16 Cu1 N15 C27 -55.2(14) . . . . ? N2 Cu1 N15 C27 161.9(13) . . . . ? N3 Cu1 N15 C27 71.8(13) . . . . ? N10 N11 C24 N12 -1.7(5) . . . . ? Cu4 N11 C24 N12 -179.7(3) . . . . ? N10 N11 C24 C30 174.2(4) . . . . ? Cu4 N11 C24 C30 -3.8(5) . . . . ? C17 N12 C24 N11 1.2(5) . . . . ? Cu3 N12 C24 N11 -178.3(6) . . . . ? C17 N12 C24 C30 -174.4(4) . . . . ? Cu3 N12 C24 C30 6.1(11) . . . . ? Cu1 N16 C25 Cu4 30(4) . . . 1_655 ? C1 N8 C26 C31 2.9(7) . . . . ? Cu2 N8 C26 C31 170.1(4) . . . . ? Cu1 N15 C27 Cu4 -23(2) . . . . ? C25 Cu4 C27 N15 -132.5(8) 1_455 . . . ? N11 Cu4 C27 N15 9.7(9) . . . . ? N13 Cu4 C27 N15 91.6(9) . . . . ? C12 N1 C28 C35 0.2(8) . . . . ? C1 N9 C29 C31 3.3(7) . . . . ? Cu3 N9 C29 C31 -171.3(4) . . . . ? C32 N14 C30 N13 -0.3(7) . . . . ? C32 N14 C30 C24 177.4(4) . . . . ? C36 N13 C30 N14 0.6(7) . . . . ? Cu4 N13 C30 N14 -178.4(4) . . . . ? C36 N13 C30 C24 -177.2(4) . . . . ? Cu4 N13 C30 C24 3.9(5) . . . . ? N11 C24 C30 N14 -178.0(4) . . . . ? N12 C24 C30 N14 -2.7(7) . . . . ? N11 C24 C30 N13 -0.1(6) . . . . ? N12 C24 C30 N13 175.2(4) . . . . ? N9 C29 C31 C26 -0.3(7) . . . . ? N8 C26 C31 C29 -2.9(7) . . . . ? C30 N14 C32 C38 -0.5(7) . . . . ? C19 N6 C33 C37 -1.2(7) . . . . ? Cu2 N6 C33 C37 -176.3(4) . . . . ? C19 N7 C34 C37 0.4(8) . . . . ? N2 C20 C35 C28 0.8(8) . . . . ? N1 C28 C35 C20 -1.2(9) . . . . ? C30 N13 C36 C38 -0.1(7) . . . . ? Cu4 N13 C36 C38 178.7(4) . . . . ? N7 C34 C37 C33 -0.7(8) . . . . ? N6 C33 C37 C34 1.1(8) . . . . ? N13 C36 C38 C32 -0.7(8) . . . . ? N14 C32 C38 C36 1.0(8) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.830 _refine_diff_density_min -1.167 _refine_diff_density_rms 0.090