# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Luciano Pandolfo' 'Simone Contaldi' 'Corrado Di Nicola' 'Federica Garau' 'Yauhen Yu Karabach' 'Luisa M D R S Martins' 'Magda Monari' 'Claudio Pettinari' 'Armando J L Pombeiro' _publ_contact_author_name 'Luciano Pandolfo' _publ_contact_author_email LUCIANO.PANDOLFO@UNIPD.IT _publ_section_title ; New MOFs based on the trinuclear triangular [Cu(?3-OH)(?-pz)3]2+ unit and unsaturated carboxylates. Molecular and supramolecular structures, electrochemical behaviour and catalytic peroxidative oxidation of cycloalkanes. ; # Attachment 'cu3.cif' data_compd1 _database_code_depnum_ccdc_archive 'CCDC 715327' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H24 Cu3 N8 O7' _chemical_formula_weight 655.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 11.4780(19) _cell_length_b 11.8535(19) _cell_length_c 12.389(2) _cell_angle_alpha 117.338(2) _cell_angle_beta 92.502(3) _cell_angle_gamma 115.928(2) _cell_volume 1282.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1234 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 18.42 _exptl_crystal_description parallelepiped _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.697 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 662 _exptl_absorpt_coefficient_mu 2.519 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.46 _exptl_absorpt_correction_T_max 0.68 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker SMART Apex II CCD' _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 7874 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_sigmaI/netI 0.0867 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 23.36 _reflns_number_total 3684 _reflns_number_gt 2203 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT+' _computing_structure_solution 'SIR-97 (Giacovazzo, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL-99 (Keller 1999)' _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0495P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3684 _refine_ls_number_parameters 340 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0929 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1046 _refine_ls_wR_factor_gt 0.0895 _refine_ls_goodness_of_fit_ref 0.954 _refine_ls_restrained_S_all 0.954 _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 0.96152(8) 0.31642(8) 0.09215(7) 0.0448(3) Uani 1 1 d . . . Cu2 Cu 0.65937(7) 0.02620(8) 0.03361(7) 0.0438(3) Uani 1 1 d . . . Cu3 Cu 0.91485(8) 0.22497(9) 0.30631(7) 0.0482(3) Uani 1 1 d . . . N5 N 1.0690(5) 0.4181(6) 0.3549(5) 0.0488(14) Uani 1 1 d . . . N6 N 1.0880(5) 0.4522(6) 0.2640(5) 0.0469(14) Uani 1 1 d . . . N3 N 0.6394(5) -0.0250(6) 0.1630(5) 0.0482(14) Uani 1 1 d . . . N2 N 0.7121(5) 0.0541(6) -0.1038(5) 0.0474(14) Uani 1 1 d . . . N1 N 0.8313(5) 0.1731(6) -0.0785(5) 0.0533(15) Uani 1 1 d . . . N4 N 0.7465(6) 0.0528(6) 0.2713(5) 0.0518(15) Uani 1 1 d . . . C13 C 0.4325(8) -0.2788(8) -0.1689(7) 0.0489(18) Uani 1 1 d . . . C9 C 1.2035(7) 0.5831(8) 0.3165(7) 0.060(2) Uani 1 1 d . . . H9 H 1.2406 0.6309 0.2738 0.072 Uiso 1 1 calc R . . C3 C 0.6474(7) -0.0192(8) -0.2279(7) 0.062(2) Uani 1 1 d . . . H3 H 0.5626 -0.1059 -0.2703 0.074 Uiso 1 1 calc R . . C6 C 0.7017(8) -0.0076(9) 0.3411(7) 0.067(2) Uani 1 1 d . . . H6 H 0.7529 0.0266 0.4211 0.081 Uiso 1 1 calc R . . C1 C 0.8351(7) 0.1683(9) -0.1879(7) 0.068(2) Uani 1 1 d . . . H1 H 0.9063 0.2377 -0.1971 0.081 Uiso 1 1 calc R . . C7 C 1.1731(7) 0.5289(9) 0.4597(7) 0.064(2) Uani 1 1 d . . . H7 H 1.1852 0.5321 0.5360 0.077 Uiso 1 1 calc R . . C4 C 0.5358(7) -0.1309(8) 0.1684(7) 0.064(2) Uani 1 1 d . . . H4 H 0.4513 -0.1987 0.1061 0.077 Uiso 1 1 calc R . . C2 C 0.7209(8) 0.0483(9) -0.2838(7) 0.072(2) Uani 1 1 d . . . H2 H 0.6984 0.0193 -0.3690 0.086 Uiso 1 1 calc R . . C8 C 1.2596(8) 0.6370(8) 0.4417(8) 0.072(2) Uani 1 1 d . . . H8 H 1.3382 0.7264 0.5005 0.086 Uiso 1 1 calc R . . C5 C 0.5704(9) -0.1266(8) 0.2788(7) 0.074(2) Uani 1 1 d . . . H5 H 0.5177 -0.1890 0.3049 0.089 Uiso 1 1 calc R . . O5 O 0.3100(5) -0.3689(5) -0.2286(4) 0.0565(13) Uani 1 1 d . . . C14 C 0.5363(8) -0.3220(9) -0.1961(8) 0.073(2) Uani 1 1 d . . . H14 H 0.6239 -0.2592 -0.1390 0.087 Uiso 1 1 calc R . . C15 C 0.5080(10) -0.4437(11) -0.2962(10) 0.115(4) Uani 1 1 d . . . H15A H 0.4208 -0.5074 -0.3540 0.138 Uiso 1 1 calc R . . H15B H 0.5747 -0.4684 -0.3112 0.138 Uiso 1 1 calc R . . O3 O 1.1264(5) 0.2022(5) 0.0177(4) 0.0613(14) Uani 1 1 d . . . O2 O 1.1131(4) 0.3843(5) 0.0221(4) 0.0558(13) Uani 1 1 d . . . C10 C 1.1655(7) 0.3041(9) -0.0026(7) 0.0532(19) Uani 1 1 d . . . C11 C 1.2722(8) 0.3251(11) -0.0657(8) 0.084(3) Uani 1 1 d . . . H11 H 1.2891 0.2482 -0.1069 0.101 Uiso 1 1 calc R . . C12 C 1.3404(9) 0.4381(11) -0.0672(8) 0.108(3) Uani 1 1 d . . . H12A H 1.3259 0.5169 -0.0268 0.129 Uiso 1 1 calc R . . H12B H 1.4065 0.4447 -0.1088 0.129 Uiso 1 1 calc R . . N7 N 1.0135(6) 0.2222(6) 0.4432(5) 0.0549(15) Uani 1 1 d . . . C18 C 1.1479(9) 0.1697(10) 0.5142(9) 0.095(3) Uani 1 1 d . . . H18 H 1.2061 0.1349 0.5161 0.114 Uiso 1 1 calc R . . N8 N 1.0902(7) 0.1627(6) 0.4132(6) 0.0666(17) Uani 1 1 d . . . H8A H 1.1015 0.1248 0.3394 0.080 Uiso 1 1 calc R . . C16 C 1.0232(8) 0.2676(9) 0.5637(7) 0.070(2) Uani 1 1 d . . . H16 H 0.9798 0.3147 0.6101 0.084 Uiso 1 1 calc R . . C17 C 1.1073(9) 0.2352(9) 0.6117(8) 0.083(3) Uani 1 1 d . . . H17 H 1.1305 0.2548 0.6939 0.100 Uiso 1 1 calc R . . O1 O 0.8235(4) 0.2180(4) 0.1608(4) 0.0406(11) Uani 1 1 d D . . H111 H 0.790(6) 0.275(5) 0.196(5) 0.049 Uiso 1 1 d D . . O4 O 0.4763(4) -0.1426(5) -0.0793(4) 0.0471(11) Uani 1 1 d . . . O6W O 1.0143(6) 0.0956(5) 0.1684(5) 0.0665(14) Uani 1 1 d D . . H6W H 0.961(6) 0.000(3) 0.118(5) 0.080 Uiso 1 1 d D . . H61W H 1.066(6) 0.142(7) 0.134(6) 0.080 Uiso 1 1 d D . . O7W O 0.9001(7) 0.4903(7) 0.1220(6) 0.0956(19) Uani 1 1 d D . . H7W H 0.877(9) 0.499(10) 0.055(5) 0.115 Uiso 1 1 d D . . H71W H 0.835(6) 0.467(9) 0.160(7) 0.115 Uiso 1 1 d 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 0.0391(5) 0.0462(5) 0.0479(5) 0.0304(5) 0.0075(4) 0.0159(4) Cu2 0.0398(5) 0.0434(5) 0.0400(5) 0.0262(4) 0.0028(4) 0.0121(4) Cu3 0.0491(5) 0.0496(5) 0.0420(5) 0.0287(4) 0.0020(4) 0.0191(4) N5 0.049(4) 0.044(3) 0.034(3) 0.015(3) -0.005(3) 0.017(3) N6 0.038(3) 0.042(3) 0.051(4) 0.025(3) 0.003(3) 0.014(3) N3 0.053(4) 0.046(4) 0.045(4) 0.030(3) 0.010(3) 0.019(3) N2 0.043(3) 0.051(4) 0.035(3) 0.022(3) 0.006(3) 0.016(3) N1 0.044(4) 0.064(4) 0.040(3) 0.033(3) 0.005(3) 0.014(3) N4 0.061(4) 0.050(4) 0.039(3) 0.030(3) 0.005(3) 0.020(3) C13 0.056(5) 0.055(5) 0.045(5) 0.035(4) 0.013(4) 0.026(5) C9 0.040(5) 0.058(5) 0.077(6) 0.040(5) 0.008(4) 0.018(4) C3 0.062(5) 0.060(5) 0.044(5) 0.028(4) 0.008(4) 0.019(4) C6 0.077(6) 0.074(6) 0.062(5) 0.055(5) 0.012(5) 0.028(5) C1 0.045(5) 0.088(6) 0.056(5) 0.048(5) 0.013(4) 0.013(5) C7 0.061(5) 0.068(6) 0.043(5) 0.021(4) -0.004(4) 0.029(5) C4 0.054(5) 0.065(5) 0.072(5) 0.050(5) 0.006(4) 0.016(4) C2 0.060(5) 0.095(6) 0.046(5) 0.043(5) 0.016(4) 0.023(5) C8 0.056(5) 0.042(5) 0.075(6) 0.020(5) -0.010(5) 0.008(4) C5 0.085(6) 0.062(6) 0.079(6) 0.055(5) 0.026(5) 0.023(5) O5 0.047(3) 0.047(3) 0.054(3) 0.019(3) 0.001(2) 0.017(3) C14 0.068(6) 0.054(5) 0.096(7) 0.036(5) 0.027(5) 0.034(5) C15 0.094(8) 0.096(8) 0.140(9) 0.041(8) 0.043(7) 0.060(7) O3 0.081(4) 0.050(3) 0.061(3) 0.037(3) 0.025(3) 0.032(3) O2 0.049(3) 0.066(3) 0.065(3) 0.047(3) 0.018(3) 0.026(3) C10 0.036(4) 0.062(5) 0.060(5) 0.037(4) 0.012(4) 0.019(4) C11 0.063(6) 0.114(8) 0.104(7) 0.085(7) 0.029(5) 0.038(6) C12 0.084(7) 0.133(9) 0.110(8) 0.085(8) 0.034(6) 0.037(7) N7 0.067(4) 0.057(4) 0.047(4) 0.029(3) 0.010(3) 0.036(3) C18 0.114(8) 0.110(8) 0.074(7) 0.043(6) -0.001(6) 0.077(7) N8 0.086(5) 0.072(4) 0.053(4) 0.031(4) 0.018(4) 0.051(4) C16 0.078(6) 0.091(6) 0.041(5) 0.036(5) 0.013(4) 0.042(5) C17 0.116(8) 0.083(6) 0.046(5) 0.037(5) -0.001(5) 0.047(6) O1 0.040(3) 0.038(3) 0.039(3) 0.023(2) 0.007(2) 0.015(2) O4 0.038(3) 0.044(3) 0.044(3) 0.021(3) 0.002(2) 0.014(2) O6W 0.089(4) 0.057(3) 0.055(3) 0.034(3) 0.032(3) 0.033(3) O7W 0.113(5) 0.119(5) 0.117(6) 0.091(5) 0.055(4) 0.073(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N6 1.942(5) . ? Cu1 N1 1.948(5) . ? Cu1 O2 1.995(4) . ? Cu1 O1 2.002(4) . ? Cu1 O7W 2.340(6) . ? Cu2 N3 1.948(5) . ? Cu2 N2 1.951(5) . ? Cu2 O4 1.968(4) . ? Cu2 O1 1.977(4) . ? Cu2 O4 2.426(4) 2_655 ? Cu3 N4 1.937(5) . ? Cu3 N5 1.957(5) . ? Cu3 O1 1.994(4) . ? Cu3 N7 2.019(5) . ? Cu3 O6W 2.422(5) . ? N5 C7 1.328(8) . ? N5 N6 1.357(6) . ? N6 C9 1.337(8) . ? N3 C4 1.331(8) . ? N3 N4 1.375(6) . ? N2 C3 1.334(8) . ? N2 N1 1.353(6) . ? N1 C1 1.333(7) . ? N4 C6 1.345(7) . ? C13 O5 1.239(7) . ? C13 O4 1.299(7) . ? C13 C14 1.486(10) . ? C9 C8 1.368(9) . ? C9 H9 0.9300 . ? C3 C2 1.342(9) . ? C3 H3 0.9300 . ? C6 C5 1.377(9) . ? C6 H6 0.9300 . ? C1 C2 1.355(9) . ? C1 H1 0.9300 . ? C7 C8 1.360(9) . ? C7 H7 0.9300 . ? C4 C5 1.379(9) . ? C4 H4 0.9300 . ? C2 H2 0.9300 . ? C8 H8 0.9300 . ? C5 H5 0.9300 . ? C14 C15 1.279(10) . ? C14 H14 0.9300 . ? C15 H15A 0.9300 . ? C15 H15B 0.9300 . ? O3 C10 1.239(8) . ? O2 C10 1.268(8) . ? C10 C11 1.473(10) . ? C11 C12 1.231(10) . ? C11 H11 0.9300 . ? C12 H12A 0.9300 . ? C12 H12B 0.9300 . ? N7 C16 1.313(8) . ? N7 N8 1.320(7) . ? C18 C17 1.336(10) . ? C18 N8 1.340(9) . ? C18 H18 0.9300 . ? N8 H8A 0.8600 . ? C16 C17 1.384(10) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? O1 H111 0.87(2) . ? O4 Cu2 2.426(4) 2_655 ? O6W H6W 0.87(2) . ? O6W H61W 0.89(2) . ? O7W H7W 0.92(2) . ? O7W H71W 0.91(2) . ? 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 N1 177.4(2) . . ? N6 Cu1 O2 90.2(2) . . ? N1 Cu1 O2 91.6(2) . . ? N6 Cu1 O1 88.60(19) . . ? N1 Cu1 O1 89.2(2) . . ? O2 Cu1 O1 167.17(19) . . ? N6 Cu1 O7W 89.7(2) . . ? N1 Cu1 O7W 92.0(2) . . ? O2 Cu1 O7W 97.1(2) . . ? O1 Cu1 O7W 95.66(18) . . ? N3 Cu2 N2 164.0(2) . . ? N3 Cu2 O4 91.3(2) . . ? N2 Cu2 O4 92.83(19) . . ? N3 Cu2 O1 88.62(19) . . ? N2 Cu2 O1 90.43(19) . . ? O4 Cu2 O1 168.21(18) . . ? N3 Cu2 O4 97.19(19) . 2_655 ? N2 Cu2 O4 98.83(18) . 2_655 ? O4 Cu2 O4 78.03(19) . 2_655 ? O1 Cu2 O4 90.28(15) . 2_655 ? N4 Cu3 N5 170.0(2) . . ? N4 Cu3 O1 88.62(19) . . ? N5 Cu3 O1 89.01(19) . . ? N4 Cu3 N7 91.8(2) . . ? N5 Cu3 N7 91.3(2) . . ? O1 Cu3 N7 175.1(2) . . ? N4 Cu3 O6W 97.9(2) . . ? N5 Cu3 O6W 91.9(2) . . ? O1 Cu3 O6W 89.71(17) . . ? N7 Cu3 O6W 85.4(2) . . ? C7 N5 N6 106.8(5) . . ? C7 N5 Cu3 134.8(5) . . ? N6 N5 Cu3 118.2(4) . . ? C9 N6 N5 107.4(5) . . ? C9 N6 Cu1 131.7(5) . . ? N5 N6 Cu1 120.9(4) . . ? C4 N3 N4 108.0(5) . . ? C4 N3 Cu2 131.7(5) . . ? N4 N3 Cu2 120.3(4) . . ? C3 N2 N1 106.8(5) . . ? C3 N2 Cu2 132.5(5) . . ? N1 N2 Cu2 120.5(4) . . ? C1 N1 N2 107.0(5) . . ? C1 N1 Cu1 130.7(5) . . ? N2 N1 Cu1 122.2(4) . . ? C6 N4 N3 106.3(5) . . ? C6 N4 Cu3 132.1(5) . . ? N3 N4 Cu3 121.4(4) . . ? O5 C13 O4 121.8(7) . . ? O5 C13 C14 121.4(7) . . ? O4 C13 C14 116.8(7) . . ? N6 C9 C8 110.6(7) . . ? N6 C9 H9 124.7 . . ? C8 C9 H9 124.7 . . ? N2 C3 C2 111.2(7) . . ? N2 C3 H3 124.4 . . ? C2 C3 H3 124.4 . . ? N4 C6 C5 111.3(6) . . ? N4 C6 H6 124.3 . . ? C5 C6 H6 124.3 . . ? N1 C1 C2 110.7(6) . . ? N1 C1 H1 124.7 . . ? C2 C1 H1 124.7 . . ? N5 C7 C8 111.6(7) . . ? N5 C7 H7 124.2 . . ? C8 C7 H7 124.2 . . ? N3 C4 C5 110.9(7) . . ? N3 C4 H4 124.5 . . ? C5 C4 H4 124.5 . . ? C3 C2 C1 104.3(7) . . ? C3 C2 H2 127.8 . . ? C1 C2 H2 127.8 . . ? C7 C8 C9 103.5(7) . . ? C7 C8 H8 128.2 . . ? C9 C8 H8 128.2 . . ? C6 C5 C4 103.4(6) . . ? C6 C5 H5 128.3 . . ? C4 C5 H5 128.3 . . ? C15 C14 C13 121.5(9) . . ? C15 C14 H14 119.2 . . ? C13 C14 H14 119.2 . . ? C14 C15 H15A 120.0 . . ? C14 C15 H15B 120.0 . . ? H15A C15 H15B 120.0 . . ? C10 O2 Cu1 109.3(4) . . ? O3 C10 O2 123.2(7) . . ? O3 C10 C11 117.5(8) . . ? O2 C10 C11 119.2(7) . . ? C12 C11 C10 124.1(10) . . ? C12 C11 H11 118.0 . . ? C10 C11 H11 118.0 . . ? C11 C12 H12A 120.0 . . ? C11 C12 H12B 120.0 . . ? H12A C12 H12B 120.0 . . ? C16 N7 N8 106.4(6) . . ? C16 N7 Cu3 135.7(6) . . ? N8 N7 Cu3 117.9(5) . . ? C17 C18 N8 108.1(8) . . ? C17 C18 H18 125.9 . . ? N8 C18 H18 125.9 . . ? N7 N8 C18 110.3(7) . . ? N7 N8 H8A 124.8 . . ? C18 N8 H8A 124.8 . . ? N7 C16 C17 110.3(8) . . ? N7 C16 H16 124.8 . . ? C17 C16 H16 124.8 . . ? C18 C17 C16 104.8(7) . . ? C18 C17 H17 127.6 . . ? C16 C17 H17 127.6 . . ? Cu2 O1 Cu3 116.07(19) . . ? Cu2 O1 Cu1 116.49(19) . . ? Cu3 O1 Cu1 110.35(19) . . ? Cu2 O1 H111 102(4) . . ? Cu3 O1 H111 104(4) . . ? Cu1 O1 H111 106(4) . . ? C13 O4 Cu2 132.5(4) . . ? C13 O4 Cu2 125.0(4) . 2_655 ? Cu2 O4 Cu2 101.97(19) . 2_655 ? Cu3 O6W H6W 116(5) . . ? Cu3 O6W H61W 115(5) . . ? H6W O6W H61W 116(7) . . ? Cu1 O7W H7W 120(6) . . ? Cu1 O7W H71W 99(6) . . ? H7W O7W H71W 117(8) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 23.36 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.419 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.083 #===END data_compd2 _database_code_depnum_ccdc_archive 'CCDC 715328' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H20 Cu3 N6 O6' _chemical_formula_weight 583.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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)/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 10.982(2) _cell_length_b 20.322(4) _cell_length_c 10.4061(19) _cell_angle_alpha 90.00 _cell_angle_beta 113.891(3) _cell_angle_gamma 90.00 _cell_volume 2123.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2313 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 22.35 _exptl_crystal_description parallelepiped _exptl_crystal_colour blue _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.824 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1172 _exptl_absorpt_coefficient_mu 3.023 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.47 _exptl_absorpt_correction_T_max 0.63 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 SMART Apex II CCD' _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 16594 _diffrn_reflns_av_R_equivalents 0.0772 _diffrn_reflns_av_sigmaI/netI 0.0773 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 26.45 _reflns_number_total 4369 _reflns_number_gt 2829 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT+' _computing_structure_solution 'SIR-97 (Giacovazzo, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL-99 (Keller 1999)' _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0601P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4369 _refine_ls_number_parameters 305 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0856 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1157 _refine_ls_wR_factor_gt 0.0972 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.935 _refine_ls_shift/su_max 0.002 _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 Cu3 Cu 0.37578(5) 1.07825(3) 0.35097(6) 0.03063(17) Uani 1 1 d . . . Cu1 Cu 0.44448(5) 0.92650(3) 0.27145(6) 0.02961(17) Uani 1 1 d . . . Cu2 Cu 0.12450(5) 0.97708(3) 0.15923(6) 0.03263(17) Uani 1 1 d . . . N5 N 0.5577(4) 1.0513(2) 0.3984(4) 0.0340(9) Uani 1 1 d . . . N6 N 0.5864(4) 0.98818(19) 0.3740(4) 0.0334(9) Uani 1 1 d . . . N1 N 0.2960(4) 0.8669(2) 0.1792(4) 0.0362(10) Uani 1 1 d . . . N4 N 0.1909(4) 1.1021(2) 0.3026(4) 0.0383(10) Uani 1 1 d . . . N2 N 0.1672(4) 0.8887(2) 0.1191(4) 0.0366(10) Uani 1 1 d . . . N3 N 0.0950(4) 1.0553(2) 0.2495(4) 0.0359(10) Uani 1 1 d . . . O1 O 0.3155(3) 1.00188(15) 0.2230(3) 0.0283(7) Uani 1 1 d D . . H111 H 0.334(4) 1.014(2) 0.152(3) 0.034 Uiso 1 1 d D . . C9 C 0.7173(4) 0.9849(2) 0.4119(5) 0.0372(12) Uani 1 1 d . . . H9 H 0.7631 0.9474 0.4056 0.045 Uiso 1 1 calc R . . C8 C 0.7751(5) 1.0447(3) 0.4617(6) 0.0470(14) Uani 1 1 d . . . H8 H 0.8649 1.0555 0.4948 0.056 Uiso 1 1 calc R . . C7 C 0.6721(5) 1.0849(3) 0.4520(5) 0.0411(13) Uani 1 1 d . . . H7 H 0.6802 1.1289 0.4787 0.049 Uiso 1 1 calc R . . C1 C 0.2962(5) 0.8049(3) 0.1366(6) 0.0478(14) Uani 1 1 d . . . H1 H 0.3713 0.7784 0.1614 0.057 Uiso 1 1 calc R . . C2 C 0.1675(6) 0.7860(3) 0.0499(6) 0.0549(15) Uani 1 1 d . . . H2 H 0.1392 0.7454 0.0069 0.066 Uiso 1 1 calc R . . C3 C 0.0913(6) 0.8409(3) 0.0419(6) 0.0506(15) Uani 1 1 d . . . H3 H -0.0001 0.8438 -0.0103 0.061 Uiso 1 1 calc R . . C6 C 0.1368(6) 1.1532(3) 0.3421(6) 0.0502(15) Uani 1 1 d . . . H6 H 0.1814 1.1919 0.3818 0.060 Uiso 1 1 calc R . . C5 C 0.0063(6) 1.1400(3) 0.3154(6) 0.0592(17) Uani 1 1 d . . . H5 H -0.0540 1.1671 0.3321 0.071 Uiso 1 1 calc R . . C4 C -0.0153(5) 1.0785(3) 0.2589(6) 0.0513(15) Uani 1 1 d . . . H4 H -0.0954 1.0557 0.2308 0.062 Uiso 1 1 calc R . . O2 O 0.5640(3) 0.84824(16) 0.3440(3) 0.0393(8) Uani 1 1 d . . . O4 O -0.0707(3) 0.96321(17) 0.0621(3) 0.0389(8) Uani 1 1 d . . . O3 O 0.5619(3) 0.83711(17) 0.5567(4) 0.0445(9) Uani 1 1 d . . . O6 O 0.4900(3) 0.9253(2) 0.0700(4) 0.0527(11) Uani 1 1 d D . . H61 H 0.570(3) 0.931(3) 0.069(6) 0.063 Uiso 1 1 d D . . C10 C 0.5694(5) 0.8150(2) 0.4472(5) 0.0389(12) Uani 1 1 d . . . C11 C 0.5913(6) 0.7428(3) 0.4466(6) 0.0542(16) Uani 1 1 d D . . H11 H 0.568(5) 0.720(3) 0.517(4) 0.065 Uiso 1 1 d D . . C16 C 0.3944(5) 0.9129(3) -0.0686(5) 0.0537(16) Uani 1 1 d . . . H16A H 0.3065 0.9152 -0.0701 0.081 Uiso 1 1 calc R . . H16B H 0.4089 0.8699 -0.0977 0.081 Uiso 1 1 calc R . . H16C H 0.4031 0.9453 -0.1315 0.081 Uiso 1 1 calc R . . C13 C -0.1539(5) 0.9311(2) 0.0944(5) 0.0327(11) Uani 1 1 d . . . C14 C -0.0985(6) 0.8874(3) 0.2181(6) 0.0492(14) Uani 1 1 d D . . H14 H -0.0024(14) 0.885(3) 0.274(5) 0.059 Uiso 1 1 d D . . O5 O -0.2748(3) 0.93541(17) 0.0249(4) 0.0408(9) Uani 1 1 d . . . C15 C -0.1663(7) 0.8499(4) 0.2607(7) 0.0665(18) Uani 1 1 d D . . H15A H -0.2636(14) 0.851(3) 0.212(6) 0.080 Uiso 1 1 d D . . H15B H -0.110(5) 0.827(3) 0.348(4) 0.080 Uiso 1 1 d D . . C12 C 0.6315(8) 0.7142(3) 0.3628(7) 0.071(2) Uani 1 1 d D . . H12A H 0.639(6) 0.6664(7) 0.375(7) 0.086 Uiso 1 1 d D . . H12B H 0.653(6) 0.739(3) 0.294(5) 0.086 Uiso 1 1 d 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 Cu3 0.0285(3) 0.0321(3) 0.0304(3) -0.0030(3) 0.0111(2) 0.0006(2) Cu1 0.0250(3) 0.0304(3) 0.0307(3) 0.0002(2) 0.0085(2) 0.0004(2) Cu2 0.0215(3) 0.0418(4) 0.0332(3) -0.0031(3) 0.0096(2) -0.0020(2) N5 0.027(2) 0.035(2) 0.036(2) -0.0045(19) 0.0089(18) -0.0031(17) N6 0.027(2) 0.036(2) 0.035(2) -0.0011(18) 0.0103(18) 0.0011(17) N1 0.031(2) 0.038(2) 0.037(2) -0.0010(19) 0.0108(18) -0.0027(18) N4 0.030(2) 0.042(2) 0.039(2) -0.005(2) 0.0091(19) 0.0035(19) N2 0.028(2) 0.043(3) 0.035(2) -0.007(2) 0.0092(18) -0.0083(18) N3 0.026(2) 0.052(3) 0.030(2) 0.0022(19) 0.0112(18) 0.0065(18) O1 0.0237(16) 0.0354(18) 0.0272(17) -0.0036(15) 0.0117(14) -0.0014(13) C9 0.025(2) 0.045(3) 0.037(3) 0.000(2) 0.008(2) 0.004(2) C8 0.024(3) 0.065(4) 0.046(3) 0.000(3) 0.009(2) -0.004(2) C7 0.037(3) 0.048(3) 0.038(3) -0.006(2) 0.015(2) -0.011(2) C1 0.049(3) 0.033(3) 0.057(4) -0.008(3) 0.017(3) -0.007(2) C2 0.053(4) 0.047(4) 0.058(4) -0.011(3) 0.016(3) -0.008(3) C3 0.037(3) 0.057(4) 0.052(3) -0.013(3) 0.012(3) -0.015(3) C6 0.046(3) 0.049(3) 0.045(3) -0.015(3) 0.008(3) 0.010(3) C5 0.041(3) 0.075(4) 0.058(4) -0.020(3) 0.017(3) 0.017(3) C4 0.029(3) 0.080(4) 0.047(3) -0.011(3) 0.018(3) 0.002(3) O2 0.038(2) 0.0342(19) 0.040(2) 0.0064(16) 0.0109(16) 0.0089(15) O4 0.0235(17) 0.053(2) 0.0376(19) 0.0043(16) 0.0102(15) -0.0047(15) O3 0.049(2) 0.039(2) 0.047(2) -0.0098(17) 0.0200(18) -0.0011(17) O6 0.033(2) 0.093(3) 0.035(2) 0.006(2) 0.0176(17) -0.007(2) C10 0.033(3) 0.036(3) 0.040(3) 0.000(3) 0.007(2) 0.002(2) C11 0.086(5) 0.034(3) 0.034(3) -0.003(3) 0.016(3) 0.004(3) C16 0.047(3) 0.072(4) 0.037(3) 0.000(3) 0.012(3) -0.001(3) C13 0.028(3) 0.040(3) 0.032(3) -0.007(2) 0.015(2) 0.000(2) C14 0.042(3) 0.066(4) 0.041(3) 0.005(3) 0.018(3) -0.005(3) O5 0.0283(19) 0.051(2) 0.044(2) 0.0024(17) 0.0168(16) -0.0054(16) C15 0.063(4) 0.078(5) 0.058(4) 0.010(4) 0.023(4) 0.003(4) C12 0.124(6) 0.035(4) 0.053(4) 0.002(3) 0.034(4) 0.016(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu3 N5 1.933(4) . ? Cu3 N4 1.944(4) . ? Cu3 O3 1.954(3) 3_676 ? Cu3 O1 1.976(3) . ? Cu3 Cu2 3.3710(9) . ? Cu1 N1 1.944(4) . ? Cu1 N6 1.947(4) . ? Cu1 O2 2.005(3) . ? Cu1 O1 2.007(3) . ? Cu1 O6 2.344(4) . ? Cu1 Cu2 3.3832(10) . ? Cu2 N3 1.938(4) . ? Cu2 N2 1.943(4) . ? Cu2 O4 1.985(3) . ? Cu2 O1 1.991(3) . ? Cu2 O4 2.455(3) 3_575 ? Cu2 N1 2.879(4) . ? Cu2 N4 2.885(4) . ? Cu2 C3 2.988(6) . ? Cu2 C4 2.995(5) . ? Cu2 C13 3.001(5) . ? Cu2 Cu2 3.4622(12) 3_575 ? N5 C7 1.338(6) . ? N5 N6 1.369(5) . ? N6 C9 1.329(6) . ? N1 C1 1.335(6) . ? N1 N2 1.369(5) . ? N4 C6 1.341(6) . ? N4 N3 1.359(6) . ? N2 C3 1.321(6) . ? N3 C4 1.340(6) . ? C9 C8 1.372(7) . ? C8 C7 1.366(7) . ? C1 C2 1.388(7) . ? C2 C3 1.377(8) . ? C6 C5 1.372(8) . ? C5 C4 1.361(8) . ? O2 C10 1.251(6) . ? O4 C13 1.274(5) . ? O4 Cu2 2.455(3) 3_575 ? O3 C10 1.258(6) . ? O3 Cu3 1.954(3) 3_676 ? O6 C16 1.421(6) . ? C10 C11 1.487(7) . ? C11 C12 1.267(9) . ? C13 O5 1.231(5) . ? C13 C14 1.477(7) . ? C14 C15 1.264(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 N5 Cu3 N4 177.94(17) . . ? N5 Cu3 O3 90.24(16) . 3_676 ? N4 Cu3 O3 91.67(16) . 3_676 ? N5 Cu3 O1 88.81(14) . . ? N4 Cu3 O1 89.48(15) . . ? O3 Cu3 O1 167.89(14) 3_676 . ? N5 Cu3 Cu2 119.47(12) . . ? N4 Cu3 Cu2 58.66(12) . . ? O3 Cu3 Cu2 150.18(11) 3_676 . ? O1 Cu3 Cu2 31.96(8) . . ? N1 Cu1 N6 175.39(17) . . ? N1 Cu1 O2 88.96(15) . . ? N6 Cu1 O2 92.72(15) . . ? N1 Cu1 O1 89.21(15) . . ? N6 Cu1 O1 88.48(14) . . ? O2 Cu1 O1 171.04(14) . . ? N1 Cu1 O6 89.55(15) . . ? N6 Cu1 O6 94.77(15) . . ? O2 Cu1 O6 89.09(15) . . ? O1 Cu1 O6 99.67(13) . . ? N1 Cu1 Cu2 58.18(12) . . ? N6 Cu1 Cu2 118.86(11) . . ? O2 Cu1 Cu2 143.25(10) . . ? O1 Cu1 Cu2 32.07(9) . . ? O6 Cu1 Cu2 105.21(9) . . ? N3 Cu2 N2 164.46(17) . . ? N3 Cu2 O4 90.31(16) . . ? N2 Cu2 O4 93.69(15) . . ? N3 Cu2 O1 89.48(14) . . ? N2 Cu2 O1 89.55(15) . . ? O4 Cu2 O1 168.51(13) . . ? N3 Cu2 O4 91.47(15) . 3_575 ? N2 Cu2 O4 104.04(15) . 3_575 ? O4 Cu2 O4 78.02(13) . 3_575 ? O1 Cu2 O4 90.50(11) . 3_575 ? N3 Cu2 N1 146.64(14) . . ? N2 Cu2 N1 24.37(13) . . ? O4 Cu2 N1 117.79(13) . . ? O1 Cu2 N1 66.60(12) . . ? O4 Cu2 N1 110.75(11) 3_575 . ? N3 Cu2 N4 23.79(14) . . ? N2 Cu2 N4 153.09(14) . . ? O4 Cu2 N4 112.52(13) . . ? O1 Cu2 N4 66.00(12) . . ? O4 Cu2 N4 87.96(12) 3_575 . ? N1 Cu2 N4 128.77(11) . . ? N3 Cu2 C3 160.18(17) . . ? N2 Cu2 C3 19.32(15) . . ? O4 Cu2 C3 74.49(15) . . ? O1 Cu2 C3 107.96(14) . . ? O4 Cu2 C3 97.54(14) 3_575 . ? N1 Cu2 C3 43.68(13) . . ? N4 Cu2 C3 171.99(14) . . ? N3 Cu2 C4 19.71(16) . . ? N2 Cu2 C4 155.82(17) . . ? O4 Cu2 C4 71.02(15) . . ? O1 Cu2 C4 109.19(14) . . ? O4 Cu2 C4 91.29(14) 3_575 . ? N1 Cu2 C4 157.27(13) . . ? N4 Cu2 C4 43.37(14) . . ? C3 Cu2 C4 141.66(16) . . ? N3 Cu2 C13 90.55(15) . . ? N2 Cu2 C13 88.64(15) . . ? O4 Cu2 C13 18.12(13) . . ? O1 Cu2 C13 173.37(13) . . ? O4 Cu2 C13 96.13(12) 3_575 . ? N1 Cu2 C13 110.54(12) . . ? N4 Cu2 C13 114.32(12) . . ? C3 Cu2 C13 71.03(14) . . ? C4 Cu2 C13 70.97(14) . . ? N3 Cu2 Cu3 58.04(12) . . ? N2 Cu2 Cu3 118.66(11) . . ? O4 Cu2 Cu3 147.59(11) . . ? O1 Cu2 Cu3 31.69(9) . . ? O4 Cu2 Cu3 94.72(8) 3_575 . ? N1 Cu2 Cu3 94.41(8) . . ? N4 Cu2 Cu3 35.14(8) . . ? C3 Cu2 Cu3 137.91(11) . . ? C4 Cu2 Cu3 77.70(11) . . ? C13 Cu2 Cu3 146.97(9) . . ? N3 Cu2 Cu1 115.83(11) . . ? N2 Cu2 Cu1 59.07(11) . . ? O4 Cu2 Cu1 152.76(11) . . ? O1 Cu2 Cu1 32.36(9) . . ? O4 Cu2 Cu1 107.21(8) 3_575 . ? N1 Cu2 Cu1 35.02(8) . . ? N4 Cu2 Cu1 94.54(8) . . ? C3 Cu2 Cu1 78.30(11) . . ? C4 Cu2 Cu1 134.11(11) . . ? C13 Cu2 Cu1 143.53(10) . . ? Cu3 Cu2 Cu1 59.607(19) . . ? N3 Cu2 Cu2 91.22(11) . 3_575 ? N2 Cu2 Cu2 102.06(12) . 3_575 ? O4 Cu2 Cu2 43.91(10) . 3_575 ? O1 Cu2 Cu2 124.61(9) . 3_575 ? O4 Cu2 Cu2 34.11(7) 3_575 3_575 ? N1 Cu2 Cu2 121.23(8) . 3_575 ? N4 Cu2 Cu2 101.20(8) . 3_575 ? C3 Cu2 Cu2 86.55(11) . 3_575 ? C4 Cu2 Cu2 80.18(11) . 3_575 ? C13 Cu2 Cu2 62.02(9) . 3_575 ? Cu3 Cu2 Cu2 122.85(3) . 3_575 ? Cu1 Cu2 Cu2 136.01(3) . 3_575 ? C7 N5 N6 107.9(4) . . ? C7 N5 Cu3 131.3(4) . . ? N6 N5 Cu3 120.7(3) . . ? C9 N6 N5 107.2(4) . . ? C9 N6 Cu1 131.3(3) . . ? N5 N6 Cu1 120.7(3) . . ? C1 N1 N2 107.1(4) . . ? C1 N1 Cu1 129.7(4) . . ? N2 N1 Cu1 121.9(3) . . ? C1 N1 Cu2 143.0(3) . . ? N2 N1 Cu2 35.9(2) . . ? Cu1 N1 Cu2 86.80(14) . . ? C6 N4 N3 107.4(4) . . ? C6 N4 Cu3 131.2(4) . . ? N3 N4 Cu3 119.1(3) . . ? C6 N4 Cu2 142.1(3) . . ? N3 N4 Cu2 35.1(2) . . ? Cu3 N4 Cu2 86.20(14) . . ? C3 N2 N1 108.6(4) . . ? C3 N2 Cu2 131.6(4) . . ? N1 N2 Cu2 119.8(3) . . ? C4 N3 N4 107.4(4) . . ? C4 N3 Cu2 131.1(4) . . ? N4 N3 Cu2 121.1(3) . . ? Cu3 O1 Cu2 116.35(15) . . ? Cu3 O1 Cu1 114.85(14) . . ? Cu2 O1 Cu1 115.57(15) . . ? N6 C9 C8 110.3(4) . . ? C7 C8 C9 105.1(5) . . ? N5 C7 C8 109.6(5) . . ? N1 C1 C2 109.9(5) . . ? C3 C2 C1 104.4(5) . . ? N2 C3 C2 110.0(5) . . ? N2 C3 Cu2 29.1(2) . . ? C2 C3 Cu2 139.1(4) . . ? N4 C6 C5 110.1(5) . . ? C4 C5 C6 104.5(5) . . ? N3 C4 C5 110.5(5) . . ? N3 C4 Cu2 29.2(3) . . ? C5 C4 Cu2 139.3(4) . . ? C10 O2 Cu1 123.2(3) . . ? C13 O4 Cu2 132.9(3) . . ? C13 O4 Cu2 125.1(3) . 3_575 ? Cu2 O4 Cu2 101.98(13) . 3_575 ? C10 O3 Cu3 128.5(3) . 3_676 ? C16 O6 Cu1 124.9(3) . . ? O2 C10 O3 125.9(5) . . ? O2 C10 C11 118.8(5) . . ? O3 C10 C11 115.3(5) . . ? C12 C11 C10 123.9(6) . . ? O5 C13 O4 121.8(5) . . ? O5 C13 C14 121.4(4) . . ? O4 C13 C14 116.8(4) . . ? O5 C13 Cu2 150.2(4) . . ? O4 C13 Cu2 29.0(2) . . ? C14 C13 Cu2 88.2(3) . . ? C15 C14 C13 125.1(6) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.45 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.843 _refine_diff_density_min -0.471 _refine_diff_density_rms 0.107 #===END data_compd3 _database_code_depnum_ccdc_archive 'CCDC 715329' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H20 Cu3 N6 O5' _chemical_formula_weight 579.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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)/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 10.0069(5) _cell_length_b 11.7324(6) _cell_length_c 17.9975(8) _cell_angle_alpha 90.00 _cell_angle_beta 95.3660(10) _cell_angle_gamma 90.00 _cell_volume 2103.74(18) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5107 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 26.31 _exptl_crystal_description platelet _exptl_crystal_colour blue _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.828 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1164 _exptl_absorpt_coefficient_mu 3.048 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.47 _exptl_absorpt_correction_T_max 0.58 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 SMART Apex II CCD' _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 17658 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4798 _reflns_number_gt 3775 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT+' _computing_structure_solution 'SIR-97 (Giacovazzo, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL-99 (Keller 1999)' _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0379P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4798 _refine_ls_number_parameters 285 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0366 _refine_ls_R_factor_gt 0.0255 _refine_ls_wR_factor_ref 0.0697 _refine_ls_wR_factor_gt 0.0669 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.004 _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 Cu2 Cu 0.64299(3) 0.86511(2) 1.029054(15) 0.03468(8) Uani 1 1 d . . . Cu3 Cu 0.89377(3) 1.02348(2) 1.110361(14) 0.03556(8) Uani 1 1 d . . . Cu1 Cu 0.79302(3) 1.06418(2) 0.927538(14) 0.03607(8) Uani 1 1 d . . . N3 N 0.69230(18) 0.85765(16) 1.13604(10) 0.0400(4) Uani 1 1 d . . . N6 N 0.95152(18) 1.14096(15) 0.97611(10) 0.0357(4) Uani 1 1 d . . . N5 N 0.98431(19) 1.13066(15) 1.05092(11) 0.0381(4) Uani 1 1 d . . . N4 N 0.79058(18) 0.92546(17) 1.16945(10) 0.0405(5) Uani 1 1 d . . . N1 N 0.64308(19) 0.97253(17) 0.88394(10) 0.0390(4) Uani 1 1 d . . . N2 N 0.58636(18) 0.89078(16) 0.92444(11) 0.0384(4) Uani 1 1 d . . . C1 C 0.5780(2) 0.9743(2) 0.81580(13) 0.0450(6) Uani 1 1 d . . . H1 H 0.5971 1.0230 0.7774 0.054 Uiso 1 1 calc R . . C4 C 0.6408(3) 0.7984(2) 1.18991(14) 0.0500(6) Uani 1 1 d . . . H4 H 0.5715 0.7457 1.1822 0.060 Uiso 1 1 calc R . . C3 C 0.4875(2) 0.8422(2) 0.87967(13) 0.0425(6) Uani 1 1 d . . . H3 H 0.4334 0.7828 0.8935 0.051 Uiso 1 1 calc R . . C9 C 1.0311(2) 1.21989(19) 0.95020(14) 0.0419(5) Uani 1 1 d . . . H9 H 1.0290 1.2429 0.9007 0.050 Uiso 1 1 calc R . . C7 C 1.0843(2) 1.2043(2) 1.07042(14) 0.0449(6) Uani 1 1 d . . . H7 H 1.1249 1.2143 1.1186 0.054 Uiso 1 1 calc R . . C2 C 0.4778(2) 0.8927(2) 0.81080(13) 0.0461(6) Uani 1 1 d . . . H2 H 0.4174 0.8759 0.7698 0.055 Uiso 1 1 calc R . . C8 C 1.1176(2) 1.2625(2) 1.00850(15) 0.0478(6) Uani 1 1 d . . . H8 H 1.1833 1.3181 1.0062 0.057 Uiso 1 1 calc R . . C5 C 0.7046(3) 0.8263(2) 1.25789(14) 0.0520(7) Uani 1 1 d . . . H5 H 0.6880 0.7974 1.3043 0.062 Uiso 1 1 calc R . . C6 C 0.7973(2) 0.9052(2) 1.24280(14) 0.0502(6) Uani 1 1 d . . . H6 H 0.8570 0.9403 1.2784 0.060 Uiso 1 1 calc R . . C14 C 0.4349(2) 0.71140(19) 1.04508(12) 0.0368(5) Uani 1 1 d . . . O3 O 0.96679(16) 0.96338(15) 0.80519(9) 0.0480(4) Uani 1 1 d . . . C10 C 0.8885(2) 1.0437(2) 0.78433(13) 0.0415(6) Uani 1 1 d . . . C11 C 0.8543(2) 1.0596(2) 0.70215(14) 0.0506(6) Uani 1 1 d . . . C12 C 0.8058(3) 1.1657(3) 0.67674(17) 0.0823(11) Uani 1 1 d . . . H12A H 0.7847 1.1780 0.6260 0.099 Uiso 1 1 calc R . . H12B H 0.7946 1.2240 0.7106 0.099 Uiso 1 1 calc R . . C13 C 0.8744(4) 0.9666(3) 0.65493(17) 0.0819(10) Uani 1 1 d . . . H13A H 0.8221 0.9028 0.6689 0.123 Uiso 1 1 calc R . . H13B H 0.9677 0.9462 0.6595 0.123 Uiso 1 1 calc R . . H13C H 0.8470 0.9873 0.6042 0.123 Uiso 1 1 calc R . . O4 O 0.55824(15) 0.71556(13) 1.03317(9) 0.0423(4) Uani 1 1 d . . . C15 C 0.3855(2) 0.6008(2) 1.07318(14) 0.0444(6) Uani 1 1 d . . . C17 C 0.4776(3) 0.5168(2) 1.09738(17) 0.0657(8) Uani 1 1 d . . . H17A H 0.4479 0.4487 1.1165 0.079 Uiso 1 1 calc R . . H17B H 0.5688 0.5288 1.0944 0.079 Uiso 1 1 calc R . . C16 C 0.2456(3) 0.5873(3) 1.0763(2) 0.0908(12) Uani 1 1 d . . . H16A H 0.2262 0.5089 1.0863 0.136 Uiso 1 1 calc R . . H16B H 0.1992 0.6093 1.0294 0.136 Uiso 1 1 calc R . . H16C H 0.2165 0.6344 1.1153 0.136 Uiso 1 1 calc R . . O1 O 0.74916(15) 1.00959(13) 1.02808(8) 0.0329(3) Uani 1 1 d D . . H111 H 0.703(2) 1.0639(16) 1.0342(13) 0.040 Uiso 1 1 d D . . O2 O 0.83697(17) 1.11160(15) 0.82740(9) 0.0462(4) Uani 1 1 d . . . O5 O 0.35679(17) 0.79280(15) 1.03455(11) 0.0558(5) 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 Cu2 0.03005(15) 0.03777(16) 0.03563(15) 0.00016(11) -0.00004(11) -0.00248(11) Cu3 0.03015(15) 0.04139(17) 0.03424(15) -0.00047(12) -0.00183(11) -0.00141(11) Cu1 0.03413(16) 0.03951(17) 0.03378(15) 0.00195(12) -0.00101(11) -0.00411(11) N3 0.0351(10) 0.0455(12) 0.0392(11) 0.0032(9) 0.0022(8) -0.0046(9) N6 0.0308(9) 0.0385(11) 0.0374(10) 0.0000(8) 0.0013(8) -0.0007(8) N5 0.0336(10) 0.0383(11) 0.0417(11) -0.0030(8) 0.0001(8) -0.0027(8) N4 0.0330(10) 0.0546(13) 0.0334(10) 0.0017(9) 0.0001(8) -0.0008(9) N1 0.0363(10) 0.0447(12) 0.0351(10) 0.0017(9) -0.0020(8) -0.0007(9) N2 0.0324(10) 0.0427(11) 0.0396(10) -0.0024(8) 0.0002(8) -0.0038(8) C1 0.0394(13) 0.0559(16) 0.0383(13) 0.0021(11) -0.0042(10) 0.0020(11) C4 0.0470(15) 0.0567(17) 0.0462(15) 0.0083(12) 0.0042(11) -0.0064(12) C3 0.0327(12) 0.0498(15) 0.0442(13) -0.0084(11) -0.0008(10) -0.0058(10) C9 0.0367(12) 0.0369(13) 0.0522(14) 0.0055(11) 0.0051(11) -0.0006(10) C7 0.0363(13) 0.0445(14) 0.0525(15) -0.0096(11) -0.0031(11) -0.0055(10) C2 0.0360(13) 0.0608(16) 0.0402(14) -0.0090(12) -0.0035(10) -0.0008(11) C8 0.0371(13) 0.0397(14) 0.0668(17) -0.0010(12) 0.0063(12) -0.0058(11) C5 0.0473(15) 0.0708(18) 0.0378(14) 0.0128(13) 0.0031(11) -0.0008(13) C6 0.0394(14) 0.0736(19) 0.0369(13) 0.0025(12) 0.0004(10) 0.0000(13) C14 0.0381(13) 0.0362(12) 0.0361(12) -0.0039(10) 0.0031(9) -0.0020(10) O3 0.0412(9) 0.0563(11) 0.0437(10) -0.0006(8) -0.0101(8) -0.0030(8) C10 0.0295(12) 0.0541(16) 0.0399(13) 0.0022(11) -0.0016(10) -0.0102(11) C11 0.0363(13) 0.0757(19) 0.0389(13) 0.0015(13) -0.0006(10) 0.0001(13) C12 0.098(3) 0.103(3) 0.0441(17) 0.0184(17) -0.0003(16) 0.035(2) C13 0.081(2) 0.110(3) 0.0511(19) -0.0184(18) -0.0108(16) 0.009(2) O4 0.0332(9) 0.0406(9) 0.0533(10) 0.0017(7) 0.0039(7) -0.0033(7) C15 0.0455(14) 0.0378(13) 0.0509(14) 0.0000(11) 0.0097(11) -0.0033(11) C17 0.073(2) 0.0440(16) 0.082(2) 0.0157(15) 0.0176(17) 0.0000(14) C16 0.065(2) 0.070(2) 0.139(4) 0.022(2) 0.018(2) -0.0135(17) O1 0.0296(8) 0.0339(8) 0.0346(8) -0.0003(6) -0.0008(6) 0.0020(6) O2 0.0505(10) 0.0518(11) 0.0365(9) 0.0023(8) 0.0057(8) -0.0036(8) O5 0.0508(11) 0.0444(10) 0.0747(13) 0.0110(9) 0.0196(9) 0.0135(8) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu2 N2 1.9384(19) . ? Cu2 N3 1.9444(19) . ? Cu2 O4 1.9532(16) . ? Cu2 O1 2.0016(16) . ? Cu2 C14 2.790(2) . ? Cu2 N4 2.8930(18) . ? Cu2 N1 2.9000(19) . ? Cu2 C8 2.957(2) 3_777 ? Cu2 Cu3 3.3474(4) . ? Cu2 Cu1 3.4000(4) . ? Cu3 N4 1.930(2) . ? Cu3 N5 1.9308(19) . ? Cu3 O3 1.9707(16) 3_777 ? Cu3 O1 1.9781(14) . ? Cu3 Cu1 3.3838(4) . ? Cu3 Cu1 3.4273(4) 3_777 ? Cu1 N1 1.9501(19) . ? Cu1 N6 1.9576(18) . ? Cu1 O2 1.9746(16) . ? Cu1 O1 2.0064(15) . ? Cu1 O5 2.3916(17) 3_677 ? Cu1 C10 2.841(2) . ? Cu1 N2 2.8978(19) . ? Cu1 N5 2.8997(18) . ? Cu1 Cu3 3.4273(4) 3_777 ? N3 C4 1.335(3) . ? N3 N4 1.361(3) . ? N6 C9 1.333(3) . ? N6 N5 1.361(3) . ? N5 C7 1.343(3) . ? N4 C6 1.337(3) . ? N1 C1 1.334(3) . ? N1 N2 1.360(3) . ? N2 C3 1.343(3) . ? C1 C2 1.383(3) . ? C4 C5 1.365(3) . ? C3 C2 1.369(3) . ? C9 C8 1.389(3) . ? C7 C8 1.374(4) . ? C8 Cu2 2.957(2) 3_777 ? C5 C6 1.357(4) . ? C14 O5 1.238(3) . ? C14 O4 1.273(2) . ? C14 C15 1.493(3) . ? O3 C10 1.260(3) . ? O3 Cu3 1.9707(16) 3_777 ? C10 O2 1.255(3) . ? C10 C11 1.498(3) . ? C11 C12 1.398(4) . ? C11 C13 1.409(4) . ? C15 C17 1.391(4) . ? C15 C16 1.416(4) . ? O5 Cu1 2.3916(17) 3_677 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu2 N3 173.17(8) . . ? N2 Cu2 O4 95.04(7) . . ? N3 Cu2 O4 89.59(7) . . ? N2 Cu2 O1 88.11(7) . . ? N3 Cu2 O1 87.77(7) . . ? O4 Cu2 O1 173.65(6) . . ? N2 Cu2 C14 92.73(7) . . ? N3 Cu2 C14 89.50(7) . . ? O4 Cu2 C14 23.72(6) . . ? O1 Cu2 C14 161.86(6) . . ? N2 Cu2 N4 152.79(7) . . ? N3 Cu2 N4 23.73(7) . . ? O4 Cu2 N4 112.01(6) . . ? O1 Cu2 N4 64.68(6) . . ? C14 Cu2 N4 113.13(6) . . ? N2 Cu2 N1 23.42(7) . . ? N3 Cu2 N1 152.87(7) . . ? O4 Cu2 N1 117.47(6) . . ? O1 Cu2 N1 65.11(6) . . ? C14 Cu2 N1 115.92(6) . . ? N4 Cu2 N1 129.58(6) . . ? N2 Cu2 C8 91.50(8) . 3_777 ? N3 Cu2 C8 93.87(8) . 3_777 ? O4 Cu2 C8 85.28(6) . 3_777 ? O1 Cu2 C8 89.13(7) . 3_777 ? C14 Cu2 C8 108.96(7) . 3_777 ? N4 Cu2 C8 88.01(6) . 3_777 ? N1 Cu2 C8 86.89(7) . 3_777 ? N2 Cu2 Cu3 118.52(6) . . ? N3 Cu2 Cu3 58.78(6) . . ? O4 Cu2 Cu3 142.42(5) . . ? O1 Cu2 Cu3 32.52(4) . . ? C14 Cu2 Cu3 148.20(4) . . ? N4 Cu2 Cu3 35.08(4) . . ? N1 Cu2 Cu3 95.11(4) . . ? C8 Cu2 Cu3 77.91(5) 3_777 . ? N2 Cu2 Cu1 58.33(6) . . ? N3 Cu2 Cu1 118.63(6) . . ? O4 Cu2 Cu1 148.49(5) . . ? O1 Cu2 Cu1 32.01(4) . . ? C14 Cu2 Cu1 150.57(5) . . ? N4 Cu2 Cu1 94.95(4) . . ? N1 Cu2 Cu1 34.93(4) . . ? C8 Cu2 Cu1 79.46(5) 3_777 . ? Cu3 Cu2 Cu1 60.193(8) . . ? N4 Cu3 N5 175.08(8) . . ? N4 Cu3 O3 89.91(7) . 3_777 ? N5 Cu3 O3 92.37(8) . 3_777 ? N4 Cu3 O1 88.38(7) . . ? N5 Cu3 O1 89.27(7) . . ? O3 Cu3 O1 178.03(7) 3_777 . ? N4 Cu3 Cu2 59.49(5) . . ? N5 Cu3 Cu2 119.39(6) . . ? O3 Cu3 Cu2 145.93(5) 3_777 . ? O1 Cu3 Cu2 32.96(4) . . ? N4 Cu3 Cu1 119.59(5) . . ? N5 Cu3 Cu1 58.80(6) . . ? O3 Cu3 Cu1 149.76(5) 3_777 . ? O1 Cu3 Cu1 32.12(4) . . ? Cu2 Cu3 Cu1 60.675(8) . . ? N4 Cu3 Cu1 118.50(6) . 3_777 ? N5 Cu3 Cu1 66.42(6) . 3_777 ? O3 Cu3 Cu1 65.31(5) 3_777 3_777 ? O1 Cu3 Cu1 116.42(5) . 3_777 ? Cu2 Cu3 Cu1 114.115(10) . 3_777 ? Cu1 Cu3 Cu1 92.504(9) . 3_777 ? N1 Cu1 N6 173.82(8) . . ? N1 Cu1 O2 90.96(7) . . ? N6 Cu1 O2 92.16(7) . . ? N1 Cu1 O1 87.82(7) . . ? N6 Cu1 O1 88.88(7) . . ? O2 Cu1 O1 177.75(7) . . ? N1 Cu1 O5 91.28(8) . 3_677 ? N6 Cu1 O5 93.04(7) . 3_677 ? O2 Cu1 O5 105.18(7) . 3_677 ? O1 Cu1 O5 76.75(6) . 3_677 ? N1 Cu1 C10 84.24(7) . . ? N6 Cu1 C10 96.72(7) . . ? O2 Cu1 C10 22.10(7) . . ? O1 Cu1 C10 155.72(7) . . ? O5 Cu1 C10 126.22(7) 3_677 . ? N1 Cu1 N2 23.69(6) . . ? N6 Cu1 N2 151.48(7) . . ? O2 Cu1 N2 113.56(6) . . ? O1 Cu1 N2 65.00(6) . . ? O5 Cu1 N2 91.88(6) 3_677 . ? C10 Cu1 N2 102.88(6) . . ? N1 Cu1 N5 152.18(7) . . ? N6 Cu1 N5 23.79(6) . . ? O2 Cu1 N5 115.83(6) . . ? O1 Cu1 N5 65.14(6) . . ? O5 Cu1 N5 88.82(6) 3_677 . ? C10 Cu1 N5 117.62(6) . . ? N2 Cu1 N5 128.49(5) . . ? N1 Cu1 Cu3 117.48(6) . . ? N6 Cu1 Cu3 58.36(5) . . ? O2 Cu1 Cu3 148.83(5) . . ? O1 Cu1 Cu3 31.62(4) . . ? O5 Cu1 Cu3 87.67(5) 3_677 . ? C10 Cu1 Cu3 140.83(5) . . ? N2 Cu1 Cu3 93.83(4) . . ? N5 Cu1 Cu3 34.72(4) . . ? N1 Cu1 Cu2 58.38(6) . . ? N6 Cu1 Cu2 117.14(5) . . ? O2 Cu1 Cu2 146.22(5) . . ? O1 Cu1 Cu2 31.93(4) . . ? O5 Cu1 Cu2 90.49(4) 3_677 . ? C10 Cu1 Cu2 129.21(5) . . ? N2 Cu1 Cu2 34.70(4) . . ? N5 Cu1 Cu2 93.80(4) . . ? Cu3 Cu1 Cu2 59.132(8) . . ? N1 Cu1 Cu3 115.97(6) . 3_777 ? N6 Cu1 Cu3 60.60(5) . 3_777 ? O2 Cu1 Cu3 67.48(5) . 3_777 ? O1 Cu1 Cu3 111.40(4) . 3_777 ? O5 Cu1 Cu3 151.24(5) 3_677 3_777 ? C10 Cu1 Cu3 53.34(5) . 3_777 ? N2 Cu1 Cu3 116.73(4) . 3_777 ? N5 Cu1 Cu3 71.50(4) . 3_777 ? Cu3 Cu1 Cu3 87.496(9) . 3_777 ? Cu2 Cu1 Cu3 111.025(10) . 3_777 ? C4 N3 N4 107.18(19) . . ? C4 N3 Cu2 131.55(17) . . ? N4 N3 Cu2 121.16(14) . . ? C9 N6 N5 108.12(18) . . ? C9 N6 Cu1 130.44(16) . . ? N5 N6 Cu1 120.75(14) . . ? C7 N5 N6 107.83(18) . . ? C7 N5 Cu3 130.59(17) . . ? N6 N5 Cu3 121.58(14) . . ? C7 N5 Cu1 142.68(16) . . ? N6 N5 Cu1 35.46(9) . . ? Cu3 N5 Cu1 86.49(6) . . ? C6 N4 N3 107.5(2) . . ? C6 N4 Cu3 132.04(18) . . ? N3 N4 Cu3 120.45(14) . . ? C6 N4 Cu2 142.53(17) . . ? N3 N4 Cu2 35.11(10) . . ? Cu3 N4 Cu2 85.43(6) . . ? C1 N1 N2 108.12(19) . . ? C1 N1 Cu1 130.74(17) . . ? N2 N1 Cu1 121.13(14) . . ? C1 N1 Cu2 142.51(16) . . ? N2 N1 Cu2 34.49(9) . . ? Cu1 N1 Cu2 86.69(6) . . ? C3 N2 N1 107.39(19) . . ? C3 N2 Cu2 130.44(17) . . ? N1 N2 Cu2 122.09(14) . . ? C3 N2 Cu1 142.56(16) . . ? N1 N2 Cu1 35.17(9) . . ? Cu2 N2 Cu1 86.97(6) . . ? N1 C1 C2 109.7(2) . . ? N3 C4 C5 110.3(2) . . ? N2 C3 C2 110.2(2) . . ? N6 C9 C8 109.6(2) . . ? N5 C7 C8 109.8(2) . . ? C3 C2 C1 104.5(2) . . ? C7 C8 C9 104.6(2) . . ? C7 C8 Cu2 101.33(16) . 3_777 ? C9 C8 Cu2 96.08(15) . 3_777 ? C6 C5 C4 104.8(2) . . ? N4 C6 C5 110.3(2) . . ? O5 C14 O4 123.6(2) . . ? O5 C14 C15 119.9(2) . . ? O4 C14 C15 116.6(2) . . ? O5 C14 Cu2 87.26(13) . . ? O4 C14 Cu2 38.12(10) . . ? C15 C14 Cu2 150.52(16) . . ? C10 O3 Cu3 123.17(16) . 3_777 ? O2 C10 O3 124.8(2) . . ? O2 C10 C11 117.5(2) . . ? O3 C10 C11 117.7(2) . . ? O2 C10 Cu1 36.28(11) . . ? O3 C10 Cu1 92.60(14) . . ? C11 C10 Cu1 145.10(17) . . ? C12 C11 C13 123.9(3) . . ? C12 C11 C10 118.3(3) . . ? C13 C11 C10 117.8(3) . . ? C14 O4 Cu2 118.16(14) . . ? C17 C15 C16 122.4(3) . . ? C17 C15 C14 119.4(2) . . ? C16 C15 C14 118.1(2) . . ? Cu3 O1 Cu2 114.52(7) . . ? Cu3 O1 Cu1 116.26(7) . . ? Cu2 O1 Cu1 116.06(7) . . ? C10 O2 Cu1 121.62(16) . . ? C14 O5 Cu1 154.37(16) . 3_677 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.299 _refine_diff_density_min -0.276 _refine_diff_density_rms 0.061 #===END