# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Zhao, Xiao-Jun' _publ_contact_author_email 'xiaojun zhao15@yahoo.com.cn' _publ_section_title ; Two unique antiferromagnetic 3D frameworks with unusual CuII4 cluster and alternate CuII4 + CuII1 structural motif tuned by aromatic polycarboxylate coligand ; loop_ _publ_author_name 'En-Cui Yang' 'You-Li Yang' 'Zhong-Yi Liu' 'Kai-Sheng Liu' ; Xiao-Yun Wu ; 'Xiao-Jun Zhao' data_81128a _database_code_depnum_ccdc_archive 'CCDC 742989' #TrackingRef '81128A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H9 Cu2.50 N4 O10' _chemical_formula_weight 528.08 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 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 26.982(8) _cell_length_b 7.503(2) _cell_length_c 15.853(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.316(7) _cell_angle_gamma 90.00 _cell_volume 3028.7(15) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6436 _cell_measurement_theta_min 2.83 _cell_measurement_theta_max 27.80 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2092 _exptl_absorpt_coefficient_mu 3.565 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5358 _exptl_absorpt_correction_T_max 0.7884 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 7445 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_sigmaI/netI 0.0215 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2658 _reflns_number_gt 2478 _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^)+(0.0342P)^2^+8.2359P] 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 2658 _refine_ls_number_parameters 258 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0246 _refine_ls_R_factor_gt 0.0227 _refine_ls_wR_factor_ref 0.0637 _refine_ls_wR_factor_gt 0.0626 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.002 _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 0.752361(12) 0.62636(4) 0.915930(19) 0.01444(10) Uani 1 1 d . . . Cu2 Cu 0.638623(12) 0.73928(4) 0.921689(19) 0.01436(10) Uani 1 1 d . . . Cu3 Cu 0.5000 0.98142(6) 0.7500 0.01530(12) Uani 1 2 d S . . O1 O 0.63634(8) 0.7469(3) 0.79597(12) 0.0249(5) Uani 1 1 d . . . O2 O 0.71180(7) 0.6329(3) 0.78715(12) 0.0217(4) Uani 1 1 d . . . O3 O 0.54357(8) 0.9763(3) 0.67504(12) 0.0225(4) Uani 1 1 d . . . O4 O 0.53015(8) 0.6810(3) 0.67329(14) 0.0285(5) Uani 1 1 d . . . O5 O 0.56381(7) 1.0048(2) 0.35662(12) 0.0192(4) Uani 1 1 d . . . O6 O 0.58037(8) 0.7298(2) 0.31604(12) 0.0223(4) Uani 1 1 d . . . O7 O 0.70273(8) 0.7820(2) 0.40375(13) 0.0223(4) Uani 1 1 d . . . O8 O 0.69865(7) 0.5019(2) 0.45135(12) 0.0164(4) Uani 1 1 d . . . O9 O 0.70464(7) 0.8653(2) 0.95943(11) 0.0153(4) Uani 1 1 d . . . H9 H 0.7039 0.9685 0.9369 0.023 Uiso 1 1 d R . . O10 O 0.57350(7) 0.5926(2) 0.88356(12) 0.0191(4) Uani 1 1 d . . . H10A H 0.5790 0.4917 0.8640 0.029 Uiso 1 1 d R . . H10B H 0.5467 0.6501 0.8519 0.029 Uiso 1 1 d R . . N1 N 0.63823(9) 0.7466(3) 1.04855(15) 0.0167(5) Uani 1 1 d . . . N2 N 0.68457(9) 0.7996(3) 1.11471(14) 0.0193(5) Uani 1 1 d . . . N3 N 0.62700(10) 0.7374(3) 1.17937(16) 0.0245(5) Uani 1 1 d . . . H3 H 0.6128 0.7229 1.2201 0.029 Uiso 1 1 calc R . . N4 N 0.55458(11) 0.6502(4) 1.05456(19) 0.0379(7) Uani 1 1 d . . . H4A H 0.5414 0.6333 0.9978 0.045 Uiso 1 1 calc R . . H4B H 0.5360 0.6296 1.0883 0.045 Uiso 1 1 calc R . . C1 C 0.67630(12) 0.7932(4) 1.19175(18) 0.0246(6) Uani 1 1 d . . . H1 H 0.7009 0.8228 1.2467 0.030 Uiso 1 1 calc R . . C2 C 0.60394(11) 0.7083(4) 1.09033(18) 0.0201(6) Uani 1 1 d . . . C3 C 0.64462(10) 0.7235(3) 0.65350(16) 0.0144(5) Uani 1 1 d . . . C4 C 0.59403(10) 0.7952(3) 0.61362(17) 0.0148(5) Uani 1 1 d . . . C5 C 0.57712(10) 0.8423(3) 0.52410(17) 0.0162(5) Uani 1 1 d . . . H5 H 0.5447 0.8977 0.4992 0.019 Uiso 1 1 calc R . . C6 C 0.60826(10) 0.8074(3) 0.47069(16) 0.0138(5) Uani 1 1 d . . . C7 C 0.65671(10) 0.7226(3) 0.50773(16) 0.0125(5) Uani 1 1 d . . . C8 C 0.67528(10) 0.6854(3) 0.59921(16) 0.0144(5) Uani 1 1 d . . . H8 H 0.7084 0.6348 0.6245 0.017 Uiso 1 1 calc R . . C9 C 0.66607(10) 0.6970(3) 0.75375(17) 0.0167(5) Uani 1 1 d . . . C10 C 0.55374(10) 0.8161(4) 0.65997(16) 0.0173(5) Uani 1 1 d . . . C11 C 0.58367(10) 0.8498(3) 0.37323(16) 0.0148(5) Uani 1 1 d . . . C12 C 0.68902(9) 0.6695(3) 0.44878(16) 0.0131(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 Cu1 0.01278(18) 0.02086(18) 0.01044(16) 0.00123(12) 0.00488(12) -0.00216(12) Cu2 0.01463(19) 0.01862(18) 0.01092(17) -0.00094(11) 0.00569(13) -0.00153(12) Cu3 0.0165(2) 0.0184(2) 0.0128(2) 0.000 0.00727(18) 0.000 O1 0.0188(11) 0.0453(13) 0.0125(9) 0.0023(8) 0.0078(8) 0.0077(9) O2 0.0137(10) 0.0386(11) 0.0122(9) 0.0029(8) 0.0036(7) 0.0055(8) O3 0.0246(11) 0.0286(11) 0.0200(10) -0.0018(8) 0.0150(8) 0.0025(8) O4 0.0218(11) 0.0318(11) 0.0367(12) 0.0042(9) 0.0161(9) -0.0023(9) O5 0.0214(10) 0.0207(10) 0.0141(9) 0.0026(7) 0.0040(8) 0.0061(8) O6 0.0347(12) 0.0194(10) 0.0126(9) -0.0002(7) 0.0076(8) -0.0003(8) O7 0.0290(11) 0.0187(9) 0.0262(10) -0.0002(8) 0.0187(9) -0.0010(8) O8 0.0173(9) 0.0140(9) 0.0211(9) -0.0008(7) 0.0107(7) 0.0027(7) O9 0.0165(9) 0.0153(9) 0.0135(9) 0.0033(7) 0.0040(7) -0.0023(7) O10 0.0178(10) 0.0166(9) 0.0212(9) -0.0017(7) 0.0041(8) 0.0014(7) N1 0.0137(11) 0.0202(11) 0.0172(11) -0.0014(8) 0.0065(9) -0.0014(8) N2 0.0166(12) 0.0285(12) 0.0137(11) -0.0016(9) 0.0063(9) -0.0036(10) N3 0.0265(14) 0.0338(14) 0.0205(12) -0.0013(10) 0.0177(11) -0.0026(11) N4 0.0256(15) 0.0610(19) 0.0308(14) -0.0088(13) 0.0144(12) -0.0132(13) C1 0.0238(15) 0.0373(16) 0.0144(13) -0.0023(12) 0.0085(11) -0.0054(13) C2 0.0181(14) 0.0222(13) 0.0236(14) -0.0007(11) 0.0117(11) 0.0008(11) C3 0.0152(14) 0.0173(12) 0.0116(12) 0.0001(9) 0.0055(10) -0.0018(10) C4 0.0150(13) 0.0166(12) 0.0146(12) -0.0022(10) 0.0073(10) -0.0009(10) C5 0.0126(13) 0.0213(13) 0.0155(13) 0.0010(10) 0.0058(10) 0.0037(10) C6 0.0166(13) 0.0131(12) 0.0132(12) -0.0003(9) 0.0071(10) 0.0005(10) C7 0.0136(13) 0.0115(11) 0.0140(12) -0.0018(9) 0.0069(10) -0.0006(9) C8 0.0125(13) 0.0166(12) 0.0152(12) 0.0006(10) 0.0061(10) 0.0024(10) C9 0.0175(14) 0.0197(13) 0.0143(12) -0.0003(10) 0.0073(10) -0.0027(11) C10 0.0125(13) 0.0303(15) 0.0083(12) 0.0009(10) 0.0027(10) 0.0021(11) C11 0.0104(12) 0.0205(13) 0.0154(12) 0.0018(10) 0.0069(10) 0.0008(10) C12 0.0105(12) 0.0170(12) 0.0113(11) -0.0022(10) 0.0030(9) -0.0006(10) _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 O9 1.9334(18) 7_667 ? Cu1 O8 1.9697(18) 6_566 ? Cu1 O2 1.9723(19) . ? Cu1 N2 1.997(2) 7_667 ? Cu1 O9 2.4362(18) . ? Cu2 O9 1.9287(18) . ? Cu2 O1 1.9744(19) . ? Cu2 O10 1.9902(19) . ? Cu2 N1 2.015(2) . ? Cu2 O8 2.3697(19) 6_566 ? Cu3 O3 1.9288(18) 2_656 ? Cu3 O3 1.9288(18) . ? Cu3 O5 1.9766(19) 6_576 ? Cu3 O5 1.9766(19) 5_676 ? O1 C9 1.259(3) . ? O2 C9 1.266(3) . ? O3 C10 1.273(3) . ? O4 C10 1.251(4) . ? O5 C11 1.271(3) . ? O5 Cu3 1.9766(19) 5_676 ? O6 C11 1.259(3) . ? O7 C12 1.238(3) . ? O8 C12 1.282(3) . ? O8 Cu1 1.9697(18) 6_565 ? O8 Cu2 2.3697(19) 6_565 ? O9 Cu1 1.9334(18) 7_667 ? O9 H9 0.8499 . ? O10 H10A 0.8500 . ? O10 H10B 0.8500 . ? N1 C2 1.335(3) . ? N1 N2 1.398(3) . ? N2 C1 1.313(3) . ? N2 Cu1 1.997(2) 7_667 ? N3 C1 1.346(4) . ? N3 C2 1.359(4) . ? N3 H3 0.8600 . ? N4 C2 1.336(4) . ? N4 H4A 0.8600 . ? N4 H4B 0.8600 . ? C1 H1 0.9300 . ? C3 C8 1.406(3) . ? C3 C4 1.408(4) . ? C3 C9 1.514(3) . ? C4 C5 1.385(4) . ? C4 C10 1.508(3) . ? C5 C6 1.401(3) . ? C5 H5 0.9300 . ? C6 C7 1.397(4) . ? C6 C11 1.500(3) . ? C7 C8 1.397(4) . ? C7 C12 1.527(3) . ? C8 H8 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 O9 Cu1 O8 88.50(8) 7_667 6_566 ? O9 Cu1 O2 175.61(8) 7_667 . ? O8 Cu1 O2 95.66(8) 6_566 . ? O9 Cu1 N2 88.17(8) 7_667 7_667 ? O8 Cu1 N2 166.35(9) 6_566 7_667 ? O2 Cu1 N2 88.11(9) . 7_667 ? O9 Cu1 O9 83.20(7) 7_667 . ? O8 Cu1 O9 76.78(7) 6_566 . ? O2 Cu1 O9 96.34(7) . . ? N2 Cu1 O9 115.91(8) 7_667 . ? O9 Cu2 O1 90.93(8) . . ? O9 Cu2 O10 175.77(7) . . ? O1 Cu2 O10 88.84(8) . . ? O9 Cu2 N1 89.21(8) . . ? O1 Cu2 N1 176.23(9) . . ? O10 Cu2 N1 91.30(8) . . ? O9 Cu2 O8 79.18(7) . 6_566 ? O1 Cu2 O8 90.76(7) . 6_566 ? O10 Cu2 O8 96.60(7) . 6_566 ? N1 Cu2 O8 92.96(8) . 6_566 ? O3 Cu3 O3 177.74(12) 2_656 . ? O3 Cu3 O5 90.58(8) 2_656 6_576 ? O3 Cu3 O5 89.53(8) . 6_576 ? O3 Cu3 O5 89.53(8) 2_656 5_676 ? O3 Cu3 O5 90.59(8) . 5_676 ? O5 Cu3 O5 173.99(11) 6_576 5_676 ? C9 O1 Cu2 135.66(18) . . ? C9 O2 Cu1 124.94(16) . . ? C10 O3 Cu3 110.32(16) . . ? C11 O5 Cu3 114.42(16) . 5_676 ? C12 O8 Cu1 129.10(16) . 6_565 ? C12 O8 Cu2 128.66(16) . 6_565 ? Cu1 O8 Cu2 95.12(7) 6_565 6_565 ? Cu2 O9 Cu1 120.88(9) . 7_667 ? Cu2 O9 Cu1 94.11(7) . . ? Cu1 O9 Cu1 96.80(7) 7_667 . ? Cu2 O9 H9 115.1 . . ? Cu1 O9 H9 108.8 7_667 . ? Cu1 O9 H9 119.6 . . ? Cu2 O10 H10A 111.1 . . ? Cu2 O10 H10B 113.2 . . ? H10A O10 H10B 117.1 . . ? C2 N1 N2 106.5(2) . . ? C2 N1 Cu2 136.2(2) . . ? N2 N1 Cu2 117.26(16) . . ? C1 N2 N1 107.6(2) . . ? C1 N2 Cu1 131.08(19) . 7_667 ? N1 N2 Cu1 121.28(16) . 7_667 ? C1 N3 C2 107.0(2) . . ? C1 N3 H3 126.5 . . ? C2 N3 H3 126.5 . . ? C2 N4 H4A 120.0 . . ? C2 N4 H4B 120.0 . . ? H4A N4 H4B 120.0 . . ? N2 C1 N3 109.9(2) . . ? N2 C1 H1 125.1 . . ? N3 C1 H1 125.1 . . ? N1 C2 N4 128.1(3) . . ? N1 C2 N3 109.0(2) . . ? N4 C2 N3 122.9(2) . . ? C8 C3 C4 118.8(2) . . ? C8 C3 C9 121.2(2) . . ? C4 C3 C9 119.9(2) . . ? C5 C4 C3 120.0(2) . . ? C5 C4 C10 115.2(2) . . ? C3 C4 C10 124.7(2) . . ? C4 C5 C6 120.8(2) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C7 C6 C5 119.7(2) . . ? C7 C6 C11 124.3(2) . . ? C5 C6 C11 115.7(2) . . ? C6 C7 C8 119.5(2) . . ? C6 C7 C12 120.4(2) . . ? C8 C7 C12 120.1(2) . . ? C7 C8 C3 120.9(2) . . ? C7 C8 H8 119.6 . . ? C3 C8 H8 119.6 . . ? O1 C9 O2 126.5(2) . . ? O1 C9 C3 115.4(2) . . ? O2 C9 C3 118.0(2) . . ? O4 C10 O3 125.5(2) . . ? O4 C10 C4 119.1(2) . . ? O3 C10 C4 115.1(2) . . ? O6 C11 O5 125.5(2) . . ? O6 C11 C6 119.5(2) . . ? O5 C11 C6 114.8(2) . . ? O7 C12 O8 126.2(2) . . ? O7 C12 C7 121.0(2) . . ? O8 C12 C7 112.8(2) . . ? 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 O9 Cu2 O1 C9 56.4(3) . . . . ? O10 Cu2 O1 C9 -119.3(3) . . . . ? N1 Cu2 O1 C9 148.5(12) . . . . ? O8 Cu2 O1 C9 -22.8(3) 6_566 . . . ? O9 Cu1 O2 C9 -105.3(10) 7_667 . . . ? O8 Cu1 O2 C9 55.8(2) 6_566 . . . ? N2 Cu1 O2 C9 -137.4(2) 7_667 . . . ? O9 Cu1 O2 C9 -21.5(2) . . . . ? O3 Cu3 O3 C10 -1.02(18) 2_656 . . . ? O5 Cu3 O3 C10 91.96(18) 6_576 . . . ? O5 Cu3 O3 C10 -94.05(18) 5_676 . . . ? O1 Cu2 O9 Cu1 -165.36(11) . . . 7_667 ? O10 Cu2 O9 Cu1 -78.6(10) . . . 7_667 ? N1 Cu2 O9 Cu1 18.41(11) . . . 7_667 ? O8 Cu2 O9 Cu1 -74.76(10) 6_566 . . 7_667 ? O1 Cu2 O9 Cu1 -64.92(7) . . . . ? O10 Cu2 O9 Cu1 21.9(10) . . . . ? N1 Cu2 O9 Cu1 118.85(8) . . . . ? O8 Cu2 O9 Cu1 25.68(6) 6_566 . . . ? O9 Cu1 O9 Cu2 -121.79(9) 7_667 . . . ? O8 Cu1 O9 Cu2 -31.74(7) 6_566 . . . ? O2 Cu1 O9 Cu2 62.60(8) . . . . ? N2 Cu1 O9 Cu2 153.59(8) 7_667 . . . ? O9 Cu1 O9 Cu1 0.0 7_667 . . 7_667 ? O8 Cu1 O9 Cu1 90.05(8) 6_566 . . 7_667 ? O2 Cu1 O9 Cu1 -175.60(8) . . . 7_667 ? N2 Cu1 O9 Cu1 -84.62(9) 7_667 . . 7_667 ? O9 Cu2 N1 C2 170.6(3) . . . . ? O1 Cu2 N1 C2 78.5(14) . . . . ? O10 Cu2 N1 C2 -13.6(3) . . . . ? O8 Cu2 N1 C2 -110.3(3) 6_566 . . . ? O9 Cu2 N1 N2 -11.52(18) . . . . ? O1 Cu2 N1 N2 -103.6(13) . . . . ? O10 Cu2 N1 N2 164.28(18) . . . . ? O8 Cu2 N1 N2 67.60(18) 6_566 . . . ? C2 N1 N2 C1 -0.7(3) . . . . ? Cu2 N1 N2 C1 -179.21(19) . . . . ? C2 N1 N2 Cu1 -179.29(18) . . . 7_667 ? Cu2 N1 N2 Cu1 2.2(3) . . . 7_667 ? N1 N2 C1 N3 0.4(3) . . . . ? Cu1 N2 C1 N3 178.83(19) 7_667 . . . ? C2 N3 C1 N2 0.0(3) . . . . ? N2 N1 C2 N4 -179.2(3) . . . . ? Cu2 N1 C2 N4 -1.2(5) . . . . ? N2 N1 C2 N3 0.7(3) . . . . ? Cu2 N1 C2 N3 178.78(19) . . . . ? C1 N3 C2 N1 -0.5(3) . . . . ? C1 N3 C2 N4 179.5(3) . . . . ? C8 C3 C4 C5 -5.9(4) . . . . ? C9 C3 C4 C5 171.1(2) . . . . ? C8 C3 C4 C10 170.1(2) . . . . ? C9 C3 C4 C10 -12.8(4) . . . . ? C3 C4 C5 C6 4.7(4) . . . . ? C10 C4 C5 C6 -171.6(2) . . . . ? C4 C5 C6 C7 0.6(4) . . . . ? C4 C5 C6 C11 174.8(2) . . . . ? C5 C6 C7 C8 -4.7(4) . . . . ? C11 C6 C7 C8 -178.3(2) . . . . ? C5 C6 C7 C12 174.8(2) . . . . ? C11 C6 C7 C12 1.3(4) . . . . ? C6 C7 C8 C3 3.5(4) . . . . ? C12 C7 C8 C3 -176.1(2) . . . . ? C4 C3 C8 C7 1.9(4) . . . . ? C9 C3 C8 C7 -175.2(2) . . . . ? Cu2 O1 C9 O2 -5.8(5) . . . . ? Cu2 O1 C9 C3 176.27(18) . . . . ? Cu1 O2 C9 O1 -9.3(4) . . . . ? Cu1 O2 C9 C3 168.60(17) . . . . ? C8 C3 C9 O1 175.4(2) . . . . ? C4 C3 C9 O1 -1.6(4) . . . . ? C8 C3 C9 O2 -2.7(4) . . . . ? C4 C3 C9 O2 -179.7(2) . . . . ? Cu3 O3 C10 O4 15.2(3) . . . . ? Cu3 O3 C10 C4 -171.28(17) . . . . ? C5 C4 C10 O4 101.6(3) . . . . ? C3 C4 C10 O4 -74.6(3) . . . . ? C5 C4 C10 O3 -72.4(3) . . . . ? C3 C4 C10 O3 111.4(3) . . . . ? Cu3 O5 C11 O6 28.5(3) 5_676 . . . ? Cu3 O5 C11 C6 -145.58(17) 5_676 . . . ? C7 C6 C11 O6 49.6(4) . . . . ? C5 C6 C11 O6 -124.2(3) . . . . ? C7 C6 C11 O5 -136.0(2) . . . . ? C5 C6 C11 O5 50.2(3) . . . . ? Cu1 O8 C12 O7 18.9(4) 6_565 . . . ? Cu2 O8 C12 O7 -123.9(2) 6_565 . . . ? Cu1 O8 C12 C7 -162.05(16) 6_565 . . . ? Cu2 O8 C12 C7 55.1(3) 6_565 . . . ? C6 C7 C12 O7 57.5(3) . . . . ? C8 C7 C12 O7 -122.9(3) . . . . ? C6 C7 C12 O8 -121.6(3) . . . . ? C8 C7 C12 O8 58.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.570 _refine_diff_density_min -0.748 _refine_diff_density_rms 0.081 # Attachment 'N100628B.cif' data_n100628b _database_code_depnum_ccdc_archive 'CCDC 796827' #TrackingRef 'N100628B.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H16 Cu4 N8 O14' _chemical_formula_weight 870.59 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 P21/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 13.5623(16) _cell_length_b 7.2662(9) _cell_length_c 15.2513(13) _cell_angle_alpha 90.00 _cell_angle_beta 123.605(7) _cell_angle_gamma 90.00 _cell_volume 1251.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4126 _cell_measurement_theta_min 3.23 _cell_measurement_theta_max 30.34 _exptl_crystal_description BLOCK _exptl_crystal_colour BLUE _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 2.310 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 3.450 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7698 _exptl_absorpt_correction_T_max 0.8743 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6003 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_sigmaI/netI 0.0307 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2213 _reflns_number_gt 1996 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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^)+(0.0411P)^2^+1.4577P] 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 2213 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0301 _refine_ls_R_factor_gt 0.0259 _refine_ls_wR_factor_ref 0.0728 _refine_ls_wR_factor_gt 0.0707 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 0.99284(3) 1.10370(5) 0.58457(2) 0.01253(12) Uani 1 1 d . . . Cu2 Cu 0.74933(3) 0.97964(5) 0.39200(3) 0.01355(13) Uani 1 1 d . . . O1 O 0.73623(18) 0.9146(3) 0.51060(15) 0.0180(5) Uani 1 1 d . . . O2 O 0.89631(18) 1.0643(3) 0.64171(16) 0.0191(5) Uani 1 1 d . . . O3 O 0.86671(18) 1.2613(3) 0.96094(15) 0.0187(5) Uani 1 1 d . . . O4 O 0.8961(2) 0.9777(3) 1.02249(17) 0.0272(6) Uani 1 1 d . . . O5 O 0.41289(18) 0.9306(3) 0.68476(15) 0.0200(5) Uani 1 1 d . . . O6 O 0.41109(18) 0.7549(3) 0.56297(16) 0.0222(5) Uani 1 1 d . . . O7 O 0.90464(17) 0.8712(3) 0.46422(14) 0.0130(4) Uani 1 1 d . . . H7 H 0.8967 0.7649 0.4829 0.016 Uiso 1 1 d R . . N1 N 1.2424(2) 0.9963(3) 0.73376(19) 0.0151(5) Uani 1 1 d . . . N2 N 1.1331(2) 1.0205(4) 0.72013(19) 0.0166(6) Uani 1 1 d . . . N3 N 1.2564(2) 0.9253(4) 0.87962(19) 0.0216(6) Uani 1 1 d . . . H3 H 1.2854 0.8927 0.9437 0.026 Uiso 1 1 d R . . N4 N 1.4280(2) 0.8891(4) 0.8784(2) 0.0262(7) Uani 1 1 d . . . H4A H 1.4621 0.8985 0.8448 0.031 Uiso 1 1 d R . . H4B H 1.4674 0.8503 0.9423 0.031 Uiso 1 1 d R . . C1 C 0.7502(3) 0.9680(4) 0.6701(2) 0.0148(6) Uani 1 1 d . . . C2 C 0.8191(3) 1.0293(4) 0.7744(2) 0.0155(6) Uani 1 1 d . . . H2 H 0.8952 1.0735 0.8020 0.019 Uiso 1 1 calc R . . C3 C 0.7740(3) 1.0240(4) 0.8363(2) 0.0141(6) Uani 1 1 d . . . C4 C 0.6589(3) 0.9645(4) 0.7945(2) 0.0144(6) Uani 1 1 d . . . H4 H 0.6283 0.9634 0.8361 0.017 Uiso 1 1 calc R . . C5 C 0.5894(3) 0.9064(4) 0.6900(2) 0.0141(6) Uani 1 1 d . . . C6 C 0.6364(3) 0.9054(4) 0.6290(2) 0.0144(6) Uani 1 1 d . . . H6 H 0.5910 0.8623 0.5601 0.017 Uiso 1 1 calc R . . C7 C 0.7982(3) 0.9818(4) 0.6017(2) 0.0153(6) Uani 1 1 d . . . C8 C 0.8519(3) 1.0895(4) 0.9495(2) 0.0140(6) Uani 1 1 d . . . C9 C 0.4611(3) 0.8560(4) 0.6405(2) 0.0154(6) Uani 1 1 d . . . C10 C 1.1441(3) 0.9771(5) 0.8080(2) 0.0216(7) Uani 1 1 d . . . H10 H 1.0836 0.9812 0.8195 0.026 Uiso 1 1 calc R . . C11 C 1.3144(3) 0.9347(4) 0.8312(2) 0.0174(7) 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 0.0112(2) 0.0153(2) 0.00999(19) 0.00074(14) 0.00517(15) 0.00100(14) Cu2 0.0108(2) 0.0178(2) 0.0106(2) -0.00009(14) 0.00499(15) -0.00046(14) O1 0.0170(11) 0.0249(12) 0.0123(10) -0.0010(9) 0.0082(9) -0.0022(9) O2 0.0149(11) 0.0285(12) 0.0154(10) -0.0024(9) 0.0092(9) -0.0035(10) O3 0.0167(10) 0.0134(11) 0.0161(10) -0.0018(9) 0.0028(8) -0.0015(9) O4 0.0405(14) 0.0173(12) 0.0146(11) -0.0008(9) 0.0095(10) -0.0012(11) O5 0.0105(10) 0.0366(14) 0.0119(10) 0.0002(9) 0.0056(8) 0.0008(9) O6 0.0168(10) 0.0272(13) 0.0169(10) -0.0061(10) 0.0058(9) -0.0048(10) O7 0.0141(10) 0.0124(10) 0.0137(10) 0.0027(8) 0.0084(8) 0.0007(8) N1 0.0118(12) 0.0165(14) 0.0122(12) -0.0007(10) 0.0037(10) 0.0004(10) N2 0.0176(13) 0.0189(14) 0.0149(12) -0.0001(11) 0.0100(10) -0.0001(11) N3 0.0239(15) 0.0280(16) 0.0108(12) 0.0034(11) 0.0083(11) 0.0035(12) N4 0.0183(14) 0.0352(18) 0.0193(13) 0.0048(12) 0.0068(11) 0.0027(12) C1 0.0147(15) 0.0148(15) 0.0153(14) -0.0001(12) 0.0085(12) 0.0011(12) C2 0.0144(14) 0.0164(15) 0.0128(14) -0.0004(12) 0.0057(12) -0.0010(12) C3 0.0158(14) 0.0112(15) 0.0120(14) -0.0006(11) 0.0058(11) 0.0005(12) C4 0.0160(15) 0.0153(15) 0.0147(14) -0.0001(12) 0.0102(12) 0.0004(12) C5 0.0143(15) 0.0115(15) 0.0151(14) 0.0011(12) 0.0073(12) 0.0007(12) C6 0.0144(14) 0.0137(15) 0.0114(13) -0.0005(12) 0.0048(11) 0.0017(12) C7 0.0155(15) 0.0178(16) 0.0115(14) 0.0028(12) 0.0068(12) 0.0034(12) C8 0.0117(13) 0.0163(16) 0.0145(15) -0.0030(12) 0.0075(11) -0.0013(12) C9 0.0126(14) 0.0188(15) 0.0115(14) 0.0027(12) 0.0046(11) 0.0008(12) C10 0.0220(17) 0.0263(18) 0.0172(15) 0.0014(14) 0.0113(13) 0.0019(14) C11 0.0176(15) 0.0151(15) 0.0133(14) -0.0008(12) 0.0047(12) -0.0004(13) _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 O7 1.915(2) 3_776 ? Cu1 O2 1.954(2) . ? Cu1 O3 1.968(2) 4_585 ? Cu1 N2 1.976(3) . ? Cu1 O7 2.286(2) . ? Cu2 O7 1.924(2) . ? Cu2 O5 1.946(2) 3_676 ? Cu2 O1 1.970(2) . ? Cu2 N1 1.990(3) 3_776 ? Cu2 O3 2.309(2) 4_585 ? O1 C7 1.258(4) . ? O2 C7 1.267(4) . ? O3 C8 1.261(4) . ? O3 Cu1 1.968(2) 4_586 ? O3 Cu2 2.309(2) 4_586 ? O4 C8 1.233(4) . ? O5 C9 1.291(4) . ? O5 Cu2 1.946(2) 3_676 ? O6 C9 1.229(4) . ? O7 Cu1 1.915(2) 3_776 ? O7 H7 0.8499 . ? N1 C11 1.325(4) . ? N1 N2 1.389(4) . ? N1 Cu2 1.990(3) 3_776 ? N2 C10 1.303(4) . ? N3 C11 1.346(4) . ? N3 C10 1.347(4) . ? N3 H3 0.8599 . ? N4 C11 1.332(4) . ? N4 H4A 0.8600 . ? N4 H4B 0.8600 . ? C1 C6 1.383(4) . ? C1 C2 1.399(4) . ? C1 C7 1.508(4) . ? C2 C3 1.381(4) . ? C2 H2 0.9300 . ? C3 C4 1.389(4) . ? C3 C8 1.517(4) . ? C4 C5 1.395(4) . ? C4 H4 0.9300 . ? C5 C6 1.388(4) . ? C5 C9 1.509(4) . ? C6 H6 0.9300 . ? C10 H10 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 O7 Cu1 O2 175.76(9) 3_776 . ? O7 Cu1 O3 90.76(9) 3_776 4_585 ? O2 Cu1 O3 93.35(9) . 4_585 ? O7 Cu1 N2 87.13(9) 3_776 . ? O2 Cu1 N2 89.06(10) . . ? O3 Cu1 N2 167.89(10) 4_585 . ? O7 Cu1 O7 85.89(8) 3_776 . ? O2 Cu1 O7 93.89(8) . . ? O3 Cu1 O7 78.93(8) 4_585 . ? N2 Cu1 O7 112.76(9) . . ? O7 Cu2 O5 175.37(10) . 3_676 ? O7 Cu2 O1 90.14(9) . . ? O5 Cu2 O1 89.22(9) 3_676 . ? O7 Cu2 N1 87.70(9) . 3_776 ? O5 Cu2 N1 92.22(9) 3_676 3_776 ? O1 Cu2 N1 171.00(10) . 3_776 ? O7 Cu2 O3 79.22(8) . 4_585 ? O5 Cu2 O3 105.41(9) 3_676 4_585 ? O1 Cu2 O3 99.64(8) . 4_585 ? N1 Cu2 O3 88.55(9) 3_776 4_585 ? C7 O1 Cu2 125.2(2) . . ? C7 O2 Cu1 129.71(19) . . ? C8 O3 Cu1 127.85(19) . 4_586 ? C8 O3 Cu2 136.64(19) . 4_586 ? Cu1 O3 Cu2 92.55(8) 4_586 4_586 ? C9 O5 Cu2 123.89(17) . 3_676 ? Cu1 O7 Cu2 122.60(10) 3_776 . ? Cu1 O7 Cu1 94.11(8) 3_776 . ? Cu2 O7 Cu1 94.44(8) . . ? Cu1 O7 H7 118.1 3_776 . ? Cu2 O7 H7 105.2 . . ? Cu1 O7 H7 120.6 . . ? C11 N1 N2 105.9(2) . . ? C11 N1 Cu2 135.3(2) . 3_776 ? N2 N1 Cu2 117.98(18) . 3_776 ? C10 N2 N1 108.1(3) . . ? C10 N2 Cu1 130.2(2) . . ? N1 N2 Cu1 121.68(19) . . ? C11 N3 C10 106.4(3) . . ? C11 N3 H3 126.8 . . ? C10 N3 H3 126.8 . . ? C11 N4 H4A 120.0 . . ? C11 N4 H4B 120.0 . . ? H4A N4 H4B 120.0 . . ? C6 C1 C2 119.7(3) . . ? C6 C1 C7 120.6(3) . . ? C2 C1 C7 119.5(3) . . ? C3 C2 C1 120.0(3) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 120.3(3) . . ? C2 C3 C8 118.5(3) . . ? C4 C3 C8 121.2(3) . . ? C3 C4 C5 119.7(3) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C6 C5 C4 119.8(3) . . ? C6 C5 C9 119.6(3) . . ? C4 C5 C9 120.5(3) . . ? C1 C6 C5 120.4(3) . . ? C1 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? O1 C7 O2 126.7(3) . . ? O1 C7 C1 117.2(3) . . ? O2 C7 C1 116.0(3) . . ? O4 C8 O3 124.5(3) . . ? O4 C8 C3 120.3(3) . . ? O3 C8 C3 115.2(3) . . ? O6 C9 O5 125.8(3) . . ? O6 C9 C5 119.7(3) . . ? O5 C9 C5 114.5(3) . . ? N2 C10 N3 109.6(3) . . ? N2 C10 H10 125.2 . . ? N3 C10 H10 125.2 . . ? N1 C11 N4 127.1(3) . . ? N1 C11 N3 109.9(3) . . ? N4 C11 N3 122.9(3) . . ? 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 O7 Cu2 O1 C7 66.6(2) . . . . ? O5 Cu2 O1 C7 -118.0(2) 3_676 . . . ? N1 Cu2 O1 C7 142.7(5) 3_776 . . . ? O3 Cu2 O1 C7 -12.5(3) 4_585 . . . ? O7 Cu1 O2 C7 -106.3(11) 3_776 . . . ? O3 Cu1 O2 C7 59.7(3) 4_585 . . . ? N2 Cu1 O2 C7 -132.2(3) . . . . ? O7 Cu1 O2 C7 -19.4(3) . . . . ? O5 Cu2 O7 Cu1 106.9(10) 3_676 . . 3_776 ? O1 Cu2 O7 Cu1 -171.04(13) . . . 3_776 ? N1 Cu2 O7 Cu1 17.71(13) 3_776 . . 3_776 ? O3 Cu2 O7 Cu1 -71.25(12) 4_585 . . 3_776 ? O5 Cu2 O7 Cu1 -155.3(10) 3_676 . . . ? O1 Cu2 O7 Cu1 -73.28(8) . . . . ? N1 Cu2 O7 Cu1 115.47(9) 3_776 . . . ? O3 Cu2 O7 Cu1 26.51(7) 4_585 . . . ? O7 Cu1 O7 Cu1 0.0 3_776 . . 3_776 ? O2 Cu1 O7 Cu1 -175.76(9) . . . 3_776 ? O3 Cu1 O7 Cu1 91.58(9) 4_585 . . 3_776 ? N2 Cu1 O7 Cu1 -85.15(11) . . . 3_776 ? O7 Cu1 O7 Cu2 -123.18(11) 3_776 . . . ? O2 Cu1 O7 Cu2 61.06(9) . . . . ? O3 Cu1 O7 Cu2 -31.60(9) 4_585 . . . ? N2 Cu1 O7 Cu2 151.67(10) . . . . ? C11 N1 N2 C10 1.1(3) . . . . ? Cu2 N1 N2 C10 172.3(2) 3_776 . . . ? C11 N1 N2 Cu1 -178.0(2) . . . . ? Cu2 N1 N2 Cu1 -6.8(3) 3_776 . . . ? O7 Cu1 N2 C10 176.8(3) 3_776 . . . ? O2 Cu1 N2 C10 -5.0(3) . . . . ? O3 Cu1 N2 C10 96.7(5) 4_585 . . . ? O7 Cu1 N2 C10 -98.8(3) . . . . ? O7 Cu1 N2 N1 -4.3(2) 3_776 . . . ? O2 Cu1 N2 N1 173.8(2) . . . . ? O3 Cu1 N2 N1 -84.5(5) 4_585 . . . ? O7 Cu1 N2 N1 80.0(2) . . . . ? C6 C1 C2 C3 1.1(4) . . . . ? C7 C1 C2 C3 177.4(3) . . . . ? C1 C2 C3 C4 -2.4(5) . . . . ? C1 C2 C3 C8 179.3(3) . . . . ? C2 C3 C4 C5 1.3(5) . . . . ? C8 C3 C4 C5 179.5(3) . . . . ? C3 C4 C5 C6 1.1(4) . . . . ? C3 C4 C5 C9 -175.0(3) . . . . ? C2 C1 C6 C5 1.3(5) . . . . ? C7 C1 C6 C5 -175.0(3) . . . . ? C4 C5 C6 C1 -2.4(4) . . . . ? C9 C5 C6 C1 173.7(3) . . . . ? Cu2 O1 C7 O2 -19.0(4) . . . . ? Cu2 O1 C7 C1 159.4(2) . . . . ? Cu1 O2 C7 O1 -4.7(5) . . . . ? Cu1 O2 C7 C1 176.9(2) . . . . ? C6 C1 C7 O1 -8.1(4) . . . . ? C2 C1 C7 O1 175.7(3) . . . . ? C6 C1 C7 O2 170.4(3) . . . . ? C2 C1 C7 O2 -5.8(4) . . . . ? Cu1 O3 C8 O4 19.1(5) 4_586 . . . ? Cu2 O3 C8 O4 -135.7(3) 4_586 . . . ? Cu1 O3 C8 C3 -160.5(2) 4_586 . . . ? Cu2 O3 C8 C3 44.7(4) 4_586 . . . ? C2 C3 C8 O4 -106.6(4) . . . . ? C4 C3 C8 O4 75.1(4) . . . . ? C2 C3 C8 O3 73.0(4) . . . . ? C4 C3 C8 O3 -105.3(3) . . . . ? Cu2 O5 C9 O6 -36.3(4) 3_676 . . . ? Cu2 O5 C9 C5 142.0(2) 3_676 . . . ? C6 C5 C9 O6 26.0(4) . . . . ? C4 C5 C9 O6 -157.9(3) . . . . ? C6 C5 C9 O5 -152.4(3) . . . . ? C4 C5 C9 O5 23.7(4) . . . . ? N1 N2 C10 N3 0.1(4) . . . . ? Cu1 N2 C10 N3 179.1(2) . . . . ? C11 N3 C10 N2 -1.4(4) . . . . ? N2 N1 C11 N4 178.8(3) . . . . ? Cu2 N1 C11 N4 9.8(5) 3_776 . . . ? N2 N1 C11 N3 -2.0(3) . . . . ? Cu2 N1 C11 N3 -170.9(2) 3_776 . . . ? C10 N3 C11 N1 2.1(4) . . . . ? C10 N3 C11 N4 -178.6(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.489 _refine_diff_density_min -0.437 _refine_diff_density_rms 0.095