Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Chan, Albert S. C.' 'Chen, Zhong-Ning' 'Kang, Bei-Sheng' 'Ren, Chen' 'Yu, Kai-Bei' 'Zhang, Hua-Xin' 'Zhou, Zhong-Yuan' _publ_contact_author_name 'Prof Bei-Sheng Kang' _publ_contact_author_address ; Prof Bei-Sheng Kang School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 CHINA ; _publ_contact_author_email 'CEDC12@ZSU.EDU.CN' _publ_section_title ; Supramolecular architectures from the self-assembly of trans-oxamidato-bridged dicopper(II) complexes and benzene-dicarboxylate ; data_compound_1 _database_code_CSD 164202 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '[Cu2(trans-oxen)(tp)]n.2nH2O' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C14 H20 Cu2 N4 O8' _chemical_formula_weight 499.42 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 7.7373(10) _cell_length_b 14.014(2) _cell_length_c 9.1101(12) _cell_angle_alpha 90.00 _cell_angle_beta 110.472(2) _cell_angle_gamma 90.00 _cell_volume 925.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used CCD _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour 'black blue' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.792 _exptl_crystal_density_method ? _exptl_crystal_F_000 508 _exptl_absorpt_coefficient_mu 2.350 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'BRUKER AREA DETECTOR CCD' _diffrn_measurement_method 'PHI AND OMEGA SCAN' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5991 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_sigmaI/netI 0.0244 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 27.54 _reflns_number_total 2113 _reflns_number_observed 1832 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'BRUCKER SMART' _computing_cell_refinement 'BRUCKER SMART' _computing_data_reduction 'SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL' _computing_publication_material 'SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0654P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2112 _refine_ls_number_parameters 159 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0366 _refine_ls_R_factor_obs 0.0321 _refine_ls_wR_factor_all 0.0968 _refine_ls_wR_factor_obs 0.0917 _refine_ls_goodness_of_fit_all 1.077 _refine_ls_goodness_of_fit_obs 1.132 _refine_ls_restrained_S_all 1.106 _refine_ls_restrained_S_obs 1.132 _refine_ls_shift/esd_max 0.064 _refine_ls_shift/esd_mean 0.006 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.33270(3) 0.06292(2) 0.03275(3) 0.02462(13) Uani 1 d . . N1 N 0.0807(2) 0.10358(14) -0.0551(2) 0.0274(4) Uani 1 d . . N2 N 0.3828(3) 0.1845(2) -0.0620(3) 0.0336(5) Uani 1 d . . H1A H 0.4699(63) 0.1741(32) -0.0997(52) 0.086(14) Uiso 1 d . . H1B H 0.4325(50) 0.2259(29) 0.0167(46) 0.072(12) Uiso 1 d . . C1 C -0.0425(3) 0.04547(15) -0.0448(3) 0.0229(4) Uani 1 d . . C2 C 0.0469(4) 0.1956(2) -0.1361(4) 0.0422(7) Uani 1 d . . H2A H -0.0677(53) 0.2008(27) -0.2155(44) 0.070(11) Uiso 1 d . . H2B H 0.0355(64) 0.2579(40) -0.0565(58) 0.122(18) Uiso 1 d . . C3 C 0.2109(4) 0.2162(2) -0.1813(4) 0.0503(7) Uani 1 d . . H3A H 0.1962(4) 0.1844(2) -0.2795(4) 0.060 Uiso 1 calc R . H3B H 0.2176(4) 0.2843(2) -0.1975(4) 0.060 Uiso 1 calc R . C4 C 0.6281(3) 0.0496(2) 0.3010(3) 0.0250(5) Uani 1 d . . C5 C 0.8212(3) 0.0247(2) 0.4049(2) 0.0238(4) Uani 1 d . . C6 C 0.8531(3) -0.0162(2) 0.5515(3) 0.0261(5) Uani 1 d . . H6 H 0.7614(37) -0.0267(18) 0.5864(30) 0.025(6) Uiso 1 d . . C7 C 1.0309(3) -0.0412(2) 0.6449(3) 0.0262(5) Uani 1 d . . H7 H 1.0461(45) -0.0748(19) 0.7409(40) 0.038(8) Uiso 1 d . . O1 O 0.2180(2) -0.05350(11) 0.0946(2) 0.0292(4) Uani 1 d . . O1W O 0.4525(3) -0.1561(2) 0.3514(3) 0.0506(6) Uani 1 d . . H1WA H 0.4488(55) -0.1306(28) 0.4247(48) 0.065(12) Uiso 1 d . . H1WB H 0.3904(55) -0.1288(29) 0.2884(46) 0.061(12) Uiso 1 d . . O2 O 0.5878(2) 0.03117(13) 0.1546(2) 0.0281(3) Uani 1 d . . O3 O 0.5177(2) 0.08484(15) 0.3554(2) 0.0378(4) Uani 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 0.0134(2) 0.0307(2) 0.0262(2) 0.00274(9) 0.00246(13) -0.00014(9) N1 0.0163(9) 0.0298(10) 0.0324(10) 0.0086(8) 0.0040(8) 0.0024(8) N2 0.0277(10) 0.0326(11) 0.0396(12) -0.0012(9) 0.0106(10) -0.0065(9) C1 0.0172(10) 0.0289(11) 0.0195(10) 0.0030(8) 0.0025(8) 0.0026(8) C2 0.0301(13) 0.0353(14) 0.056(2) 0.0210(12) 0.0082(13) 0.0031(11) C3 0.042(2) 0.046(2) 0.057(2) 0.0211(13) 0.0101(14) -0.0028(13) C4 0.0167(10) 0.0311(11) 0.0242(11) -0.0002(8) 0.0035(9) -0.0008(8) C5 0.0164(9) 0.0304(11) 0.0211(10) -0.0040(8) 0.0021(8) 0.0008(8) C6 0.0173(10) 0.0359(13) 0.0242(11) -0.0009(9) 0.0062(9) -0.0017(9) C7 0.0210(11) 0.0352(12) 0.0200(10) 0.0005(8) 0.0040(9) -0.0006(9) O1 0.0155(8) 0.0374(9) 0.0311(9) 0.0120(6) 0.0036(7) 0.0033(6) O1W 0.0600(14) 0.0511(13) 0.0328(11) 0.0059(10) 0.0063(11) 0.0261(11) O2 0.0145(7) 0.0444(9) 0.0199(8) -0.0023(7) -0.0008(6) 0.0025(7) O3 0.0235(9) 0.0581(11) 0.0294(9) -0.0024(8) 0.0064(7) 0.0119(8) _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 N1 1.917(2) . ? Cu1 O2 1.947(2) . ? Cu1 N2 2.008(2) . ? Cu1 O1 2.029(2) . ? Cu1 O2 2.401(2) 3_655 ? N1 C1 1.282(3) . ? N1 C2 1.463(3) . ? N2 C3 1.462(3) . ? C1 O1 1.277(3) 3 ? C1 C1 1.532(4) 3 ? C2 C3 1.493(4) . ? C4 O3 1.230(3) . ? C4 O2 1.286(3) . ? C4 C5 1.504(3) . ? C5 C7 1.391(3) 3_756 ? C5 C6 1.393(3) . ? C6 C7 1.386(3) . ? C7 C5 1.391(3) 3_756 ? O1 C1 1.277(3) 3 ? O2 Cu1 2.401(2) 3_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 O2 170.36(8) . . ? N1 Cu1 N2 83.65(9) . . ? O2 Cu1 N2 97.42(8) . . ? N1 Cu1 O1 82.83(7) . . ? O2 Cu1 O1 96.47(7) . . ? N2 Cu1 O1 166.08(8) . . ? N1 Cu1 O2 110.02(7) . 3_655 ? O2 Cu1 O2 79.57(6) . 3_655 ? N2 Cu1 O2 91.41(8) . 3_655 ? O1 Cu1 O2 90.09(7) . 3_655 ? C1 N1 C2 126.2(2) . . ? C1 N1 Cu1 117.02(15) . . ? C2 N1 Cu1 116.7(2) . . ? C3 N2 Cu1 108.4(2) . . ? O1 C1 N1 130.0(2) 3 . ? O1 C1 C1 117.9(2) 3 3 ? N1 C1 C1 112.1(2) . 3 ? N1 C2 C3 106.9(2) . . ? N2 C3 C2 112.1(2) . . ? O3 C4 O2 123.2(2) . . ? O3 C4 C5 121.1(2) . . ? O2 C4 C5 115.7(2) . . ? C7 C5 C6 119.4(2) 3_756 . ? C7 C5 C4 120.4(2) 3_756 . ? C6 C5 C4 120.2(2) . . ? C7 C6 C5 119.9(2) . . ? C6 C7 C5 120.7(2) . 3_756 ? C1 O1 Cu1 110.14(13) 3 . ? C4 O2 Cu1 112.03(14) . . ? C4 O2 Cu1 144.94(14) . 3_655 ? Cu1 O2 Cu1 100.43(6) . 3_655 ? _refine_diff_density_max 0.846 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.087 #===============================================END data_compound 2 _database_code_CSD 164203 [{Cu2(trans-oxpn)(H2O)2}{Cu2(trans-oxpn)}(isophth)2]n.7nH2O _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C32 H58 Cu4 N8 O21' _chemical_formula_weight 1145.02 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.3800(10) _cell_length_b 20.613(2) _cell_length_c 12.0930(10) _cell_angle_alpha 90.00 _cell_angle_beta 104.270(10) _cell_angle_gamma 90.00 _cell_volume 2266.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 290(2) _cell_measurement_reflns_used 32 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 18.09 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.678 _exptl_crystal_density_method ? _exptl_crystal_F_000 1180 _exptl_absorpt_coefficient_mu 1.938 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7142 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 290(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.63 _diffrn_reflns_number 5294 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_sigmaI/netI 0.0476 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 26.50 _reflns_number_total 4815 _reflns_number_observed 3712 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0534P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom but not for o13 to o21 _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0021(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(2) _refine_ls_number_reflns 4815 _refine_ls_number_parameters 587 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0500 _refine_ls_R_factor_obs 0.0352 _refine_ls_wR_factor_all 0.0881 _refine_ls_wR_factor_obs 0.0841 _refine_ls_goodness_of_fit_all 0.935 _refine_ls_goodness_of_fit_obs 1.037 _refine_ls_restrained_S_all 0.935 _refine_ls_restrained_S_obs 1.037 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.87609(8) 0.69510(4) 1.12843(6) 0.0242(2) Uani 1 d . . Cu2 Cu 1.37038(8) 0.75323(4) 1.01788(7) 0.0250(2) Uani 1 d . . Cu3 Cu 0.36285(7) 0.69163(4) 0.58405(7) 0.0256(2) Uani 1 d . . Cu4 Cu 0.89103(8) 0.75754(4) 0.56070(6) 0.0253(2) Uani 1 d . . O1 O 0.7868(4) 0.7451(2) 1.2351(4) 0.0295(11) Uani 1 d . . O2 O 0.5516(5) 0.7160(2) 1.1721(4) 0.0305(12) Uani 1 d . . O3 O 0.2436(5) 0.7760(3) 1.4419(5) 0.0389(13) Uani 1 d . . O4 O 0.2416(7) 0.8813(3) 1.4846(6) 0.058(2) Uani 1 d . . O5 O 0.6958(5) 0.7347(2) 0.9727(4) 0.0299(11) Uani 1 d . . O6 O 0.4613(4) 0.7036(3) 0.9108(4) 0.0292(11) Uani 1 d . . O7 O 1.0353(5) 0.5715(3) 0.6854(5) 0.0476(14) Uani 1 d . . O8 O 1.0094(5) 0.6771(2) 0.7066(4) 0.0353(13) Uani 1 d . . O9 O 1.2482(5) 0.6753(2) 1.0239(4) 0.0287(11) Uani 1 d . . O10 O 0.9970(5) 0.7734(2) 1.1210(4) 0.0314(12) Uani 1 d . . O11 O 0.7423(4) 0.6914(2) 0.4909(3) 0.0247(9) Uani 1 d . . O12 O 0.5135(4) 0.7562(3) 0.6544(3) 0.0271(9) Uani 1 d . . O13 O 0.2672(5) 0.7122(2) 0.7072(4) 0.0319(12) Uani 1 d . . O14 O 0.9864(5) 0.7373(2) 0.4367(4) 0.0303(11) Uani 1 d . . O15 O 0.8604(8) 0.5830(4) 0.3949(5) 0.077(2) Uani 1 d . . O16 O 0.4047(8) 0.8704(4) 0.7362(6) 0.083(2) Uani 1 d . . O17 O 1.4341(7) 0.5634(3) 1.0393(6) 0.070(2) Uani 1 d . . O18 O 0.9745(7) 0.4727(3) 0.5280(6) 0.074(2) Uani 1 d . . O19 O 0.6516(8) 0.9597(3) 0.8489(7) 0.086(2) Uani 1 d . . O20 O 0.7981(8) 0.8846(3) 1.0542(8) 0.096(3) Uani 1 d . . O21 O 1.2579(8) 0.4998(3) 0.8373(8) 0.099(3) Uani 1 d . . N1 N 0.7707(7) 0.6145(3) 1.1507(6) 0.0337(15) Uani 1 d . . H1A H 0.7877(7) 0.6078(3) 1.2264(6) 0.040 Uiso 1 calc R . H1B H 0.6738(7) 0.6224(3) 1.1250(6) 0.040 Uiso 1 calc R . N2 N 1.0327(6) 0.6504(3) 1.0758(5) 0.0260(12) Uani 1 d . . N3 N 1.2157(6) 0.7975(3) 1.0745(5) 0.0269(13) Uani 1 d . . N4 N 1.4691(7) 0.8344(3) 0.9908(7) 0.043(2) Uani 1 d . . H4A H 1.5668(7) 0.8280(3) 1.0146(7) 0.051 Uiso 1 calc R . H4B H 1.4484(7) 0.8410(3) 0.9149(7) 0.051 Uiso 1 calc R . N5 N 0.2108(6) 0.6260(3) 0.5185(5) 0.0324(14) Uani 1 d . . H5A H 0.1806(6) 0.6075(3) 0.5763(5) 0.039 Uiso 1 calc R . H5B H 0.1330(6) 0.6467(3) 0.4743(5) 0.039 Uiso 1 calc R . N6 N 0.5044(6) 0.6658(3) 0.5000(5) 0.0250(12) Uani 1 d . . N7 N 0.7486(5) 0.7829(3) 0.6450(5) 0.0262(12) Uani 1 d . . N8 N 1.0430(6) 0.8241(3) 0.6283(5) 0.0321(14) Uani 1 d . . H8A H 1.1224(6) 0.8028(3) 0.6692(5) 0.039 Uiso 1 calc R . H8B H 1.0702(6) 0.8438(3) 0.5703(5) 0.039 Uiso 1 calc R . C1 C 0.6497(6) 0.7494(3) 1.2315(5) 0.0225(13) Uani 1 d . . C2 C 0.6088(6) 0.8007(3) 1.3083(5) 0.0214(13) Uani 1 d . . C3 C 0.7024(7) 0.8531(3) 1.3472(6) 0.030(2) Uani 1 d . . H3 H 0.7920(7) 0.8561(3) 1.3275(6) 0.036 Uiso 1 calc R . C4 C 0.6631(8) 0.8999(3) 1.4139(6) 0.036(2) Uani 1 d . . H4 H 0.7248(8) 0.9350(3) 1.4387(6) 0.043 Uiso 1 calc R . C5 C 0.5291(8) 0.8945(3) 1.4449(7) 0.035(2) Uani 1 d . . H5 H 0.5009(8) 0.9265(3) 1.4895(7) 0.042 Uiso 1 calc R . C6 C 0.4380(7) 0.8412(3) 1.4089(5) 0.0229(14) Uani 1 d . . C7 C 0.4771(7) 0.7955(3) 1.3386(5) 0.0232(14) Uani 1 d . . H7 H 0.4144(7) 0.7610(3) 1.3115(5) 0.028 Uiso 1 calc R . C8 C 0.2958(8) 0.8328(4) 1.4464(6) 0.031(2) Uani 1 d . . C9 C 0.6005(6) 0.6991(4) 0.9138(5) 0.0254(13) Uani 1 d . . C10 C 0.6424(7) 0.6494(3) 0.8401(5) 0.0231(14) Uani 1 d . . C11 C 0.5541(7) 0.5948(4) 0.7982(6) 0.034(2) Uani 1 d . . H11 H 0.4627(7) 0.5903(4) 0.8144(6) 0.040 Uiso 1 calc R . C12 C 0.6006(8) 0.5493(4) 0.7351(7) 0.038(2) Uani 1 d . . H12 H 0.5409(8) 0.5137(4) 0.7092(7) 0.045 Uiso 1 calc R . C13 C 0.7376(7) 0.5545(4) 0.7076(6) 0.031(2) Uani 1 d . . H13 H 0.7699(7) 0.5219(4) 0.6666(6) 0.037 Uiso 1 calc R . C14 C 0.8242(7) 0.6095(3) 0.7431(6) 0.0279(15) Uani 1 d . . C15 C 0.7767(7) 0.6550(3) 0.8093(5) 0.0231(14) Uani 1 d . . H15 H 0.8359(7) 0.6908(3) 0.8347(5) 0.028 Uiso 1 calc R . C16 C 0.9682(8) 0.6194(4) 0.7083(6) 0.032(2) Uani 1 d . . C17 C 0.8015(8) 0.5536(4) 1.0993(7) 0.042(2) Uani 1 d . . H17A H 0.7614(8) 0.5557(4) 1.0174(7) 0.051 Uiso 1 calc R . H17B H 0.7530(8) 0.5183(4) 1.1286(7) 0.051 Uiso 1 calc R . C18 C 0.9609(7) 0.5402(3) 1.1236(7) 0.040(2) Uani 1 d . . H18A H 0.9748(7) 0.4946(3) 1.1093(7) 0.048 Uiso 1 calc R . H18B H 1.0042(7) 0.5482(3) 1.2039(7) 0.048 Uiso 1 calc R . C19 C 1.0434(8) 0.5804(3) 1.0535(7) 0.036(2) Uani 1 d . . H19A H 1.1460(8) 0.5676(3) 1.0724(7) 0.044 Uiso 1 calc R . H19B H 1.0027(8) 0.5719(3) 0.9730(7) 0.044 Uiso 1 calc R . C20 C 1.1351(6) 0.6893(3) 1.0588(5) 0.0224(13) Uani 1 d . . C21 C 1.1115(6) 0.7597(3) 1.0868(5) 0.0222(12) Uani 1 d . . C22 C 1.2061(8) 0.8661(3) 1.1018(7) 0.034(2) Uani 1 d . . H22A H 1.2396(8) 0.8717(3) 1.1837(7) 0.041 Uiso 1 calc R . H22B H 1.1040(8) 0.8796(3) 1.0789(7) 0.041 Uiso 1 calc R . C23 C 1.2936(13) 0.9078(4) 1.0455(11) 0.078(4) Uani 1 d . . H23A H 1.2392(13) 0.9114(4) 0.9664(11) 0.094 Uiso 1 calc R . H23B H 1.2936(13) 0.9506(4) 1.0788(11) 0.094 Uiso 1 calc R . C24 C 1.4336(13) 0.8948(5) 1.0445(12) 0.094(4) Uani 1 d . . H24A H 1.4909(13) 0.8948(5) 1.1231(12) 0.112 Uiso 1 calc R . H24B H 1.4687(13) 0.9308(5) 1.0068(12) 0.112 Uiso 1 calc R . C25 C 0.2543(9) 0.5740(5) 0.4506(8) 0.053(3) Uani 1 d . . H25A H 0.3186(9) 0.5442(5) 0.5018(8) 0.063 Uiso 1 calc R . H25B H 0.1670(9) 0.5501(5) 0.4123(8) 0.063 Uiso 1 calc R . C26 C 0.3295(9) 0.5965(5) 0.3647(8) 0.055(2) Uani 1 d . . H26A H 0.2765(9) 0.6336(5) 0.3256(8) 0.066 Uiso 1 calc R . H26B H 0.3245(9) 0.5623(5) 0.3087(8) 0.066 Uiso 1 calc R . C27 C 0.4894(8) 0.6155(4) 0.4106(7) 0.035(2) Uani 1 d . . H27A H 0.5463(8) 0.5776(4) 0.4422(7) 0.043 Uiso 1 calc R . H27B H 0.5283(8) 0.6319(4) 0.3488(7) 0.043 Uiso 1 calc R . C28 C 0.6267(6) 0.6984(3) 0.5296(5) 0.0196(12) Uani 1 d . . C29 C 0.6284(6) 0.7499(3) 0.6166(5) 0.0216(13) Uani 1 d . . C30 C 0.7648(8) 0.8326(4) 0.7351(7) 0.036(2) Uani 1 d . . H30A H 0.7206(8) 0.8169(4) 0.7946(7) 0.043 Uiso 1 calc R . H30B H 0.7131(8) 0.8717(4) 0.7032(7) 0.043 Uiso 1 calc R . C31 C 0.9255(9) 0.8485(4) 0.7865(7) 0.050(2) Uani 1 d . . H31A H 0.9752(9) 0.8096(4) 0.8209(7) 0.060 Uiso 1 calc R . H31B H 0.9314(9) 0.8802(4) 0.8468(7) 0.060 Uiso 1 calc R . C32 C 1.0060(10) 0.8750(4) 0.7016(7) 0.047(2) Uani 1 d . . H32A H 0.9449(10) 0.9074(4) 0.6542(7) 0.057 Uiso 1 calc R . H32B H 1.0958(10) 0.8961(4) 0.7429(7) 0.057 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0181(3) 0.0255(4) 0.0321(5) -0.0023(4) 0.0125(3) -0.0019(4) Cu2 0.0177(3) 0.0250(4) 0.0358(5) -0.0006(4) 0.0134(3) -0.0021(4) Cu3 0.0165(3) 0.0323(4) 0.0300(4) -0.0043(4) 0.0095(3) -0.0051(4) Cu4 0.0166(3) 0.0323(4) 0.0290(4) -0.0047(4) 0.0097(3) -0.0050(4) O1 0.020(2) 0.042(3) 0.029(3) -0.007(2) 0.012(2) -0.001(2) O2 0.025(3) 0.036(3) 0.031(3) -0.010(2) 0.009(2) -0.004(2) O3 0.017(2) 0.045(3) 0.058(4) 0.005(3) 0.017(2) -0.001(2) O4 0.052(4) 0.045(3) 0.091(5) 0.004(3) 0.046(3) 0.012(3) O5 0.020(2) 0.042(3) 0.028(3) -0.002(2) 0.007(2) -0.006(2) O6 0.015(2) 0.046(3) 0.029(2) -0.007(2) 0.010(2) -0.005(2) O7 0.037(3) 0.044(3) 0.072(4) -0.007(3) 0.034(3) 0.008(2) O8 0.018(2) 0.040(3) 0.050(3) 0.001(2) 0.013(2) -0.005(2) O9 0.023(2) 0.025(3) 0.043(3) -0.006(2) 0.016(2) -0.003(2) O10 0.022(2) 0.027(3) 0.051(3) -0.010(2) 0.020(2) -0.003(2) O11 0.019(2) 0.030(2) 0.027(2) -0.004(2) 0.009(2) -0.004(2) O12 0.019(2) 0.034(2) 0.031(2) -0.002(2) 0.012(2) -0.005(2) O13 0.024(2) 0.048(3) 0.028(3) -0.006(2) 0.014(2) -0.007(2) O14 0.020(2) 0.042(3) 0.031(3) -0.004(2) 0.011(2) -0.002(2) O15 0.088(5) 0.080(5) 0.061(4) -0.006(4) 0.014(4) 0.036(4) O16 0.065(5) 0.092(6) 0.088(6) -0.030(4) 0.010(4) 0.005(4) O17 0.056(4) 0.050(4) 0.115(6) 0.017(4) 0.040(4) 0.008(3) O18 0.083(5) 0.060(4) 0.091(5) -0.012(4) 0.047(4) -0.017(4) O19 0.098(5) 0.069(4) 0.110(6) -0.035(4) 0.062(5) -0.021(4) O20 0.065(5) 0.060(5) 0.155(8) -0.014(5) 0.014(5) 0.014(4) O21 0.085(6) 0.074(5) 0.133(7) 0.025(5) 0.016(5) 0.010(4) N1 0.029(3) 0.035(4) 0.043(4) 0.006(3) 0.020(3) -0.003(3) N2 0.021(3) 0.022(3) 0.036(3) -0.002(2) 0.009(2) -0.002(2) N3 0.018(3) 0.024(3) 0.042(3) -0.003(3) 0.012(2) -0.001(2) N4 0.032(4) 0.035(4) 0.069(5) 0.009(3) 0.024(3) -0.003(3) N5 0.025(3) 0.038(4) 0.035(4) -0.007(3) 0.007(3) -0.007(3) N6 0.025(3) 0.028(3) 0.025(3) 0.000(2) 0.011(2) -0.002(2) N7 0.017(3) 0.034(3) 0.027(3) -0.002(2) 0.005(2) -0.006(2) N8 0.021(3) 0.044(4) 0.033(3) 0.000(3) 0.012(3) -0.009(3) C1 0.017(3) 0.029(3) 0.021(3) 0.006(3) 0.005(2) 0.001(3) C2 0.019(3) 0.027(3) 0.019(3) 0.001(3) 0.005(2) 0.003(3) C3 0.021(3) 0.026(4) 0.046(4) 0.006(3) 0.014(3) -0.003(3) C4 0.037(4) 0.027(4) 0.050(5) -0.012(3) 0.022(4) -0.012(3) C5 0.041(4) 0.021(4) 0.045(5) -0.002(3) 0.017(4) 0.007(3) C6 0.018(3) 0.026(3) 0.025(4) 0.005(3) 0.009(3) 0.006(3) C7 0.021(3) 0.025(3) 0.024(3) 0.002(3) 0.006(3) -0.001(3) C8 0.032(4) 0.040(5) 0.025(4) 0.002(3) 0.014(3) 0.011(3) C9 0.020(3) 0.036(4) 0.022(3) 0.005(3) 0.009(2) 0.000(3) C10 0.020(3) 0.026(3) 0.026(4) 0.004(3) 0.011(3) 0.000(3) C11 0.021(3) 0.046(5) 0.036(4) 0.000(4) 0.011(3) -0.007(3) C12 0.030(4) 0.032(4) 0.052(5) -0.003(3) 0.011(3) -0.012(3) C13 0.025(3) 0.033(4) 0.035(4) -0.003(3) 0.011(3) -0.004(3) C14 0.021(3) 0.034(4) 0.031(4) 0.002(3) 0.010(3) 0.000(3) C15 0.015(3) 0.028(3) 0.027(4) 0.004(3) 0.006(3) -0.002(3) C16 0.026(4) 0.042(5) 0.028(4) 0.002(3) 0.008(3) 0.002(3) C17 0.039(4) 0.027(4) 0.066(5) -0.004(4) 0.023(4) -0.009(3) C18 0.033(4) 0.027(4) 0.058(5) 0.006(3) 0.010(3) -0.001(3) C19 0.039(4) 0.015(3) 0.059(5) -0.011(3) 0.020(4) 0.002(3) C20 0.017(3) 0.023(3) 0.030(3) -0.007(3) 0.010(2) 0.001(3) C21 0.017(3) 0.026(3) 0.022(3) -0.002(3) 0.004(2) -0.001(3) C22 0.028(4) 0.023(4) 0.054(5) 0.002(3) 0.014(3) -0.001(3) C23 0.100(9) 0.035(5) 0.124(10) -0.008(5) 0.076(8) -0.004(5) C24 0.096(8) 0.031(5) 0.186(14) -0.003(7) 0.096(9) -0.012(5) C25 0.036(5) 0.053(6) 0.075(7) -0.028(5) 0.024(4) -0.024(4) C26 0.048(5) 0.066(6) 0.054(5) -0.033(5) 0.019(4) -0.032(5) C27 0.028(4) 0.044(5) 0.037(5) -0.014(4) 0.015(4) -0.008(3) C28 0.020(3) 0.018(3) 0.021(3) 0.005(3) 0.007(2) 0.001(3) C29 0.016(3) 0.027(3) 0.023(3) 0.000(3) 0.007(2) -0.001(3) C30 0.040(4) 0.036(4) 0.035(5) -0.009(4) 0.014(4) -0.014(4) C31 0.045(5) 0.059(5) 0.050(5) -0.021(4) 0.018(4) -0.017(4) C32 0.051(5) 0.048(5) 0.048(5) -0.019(4) 0.022(4) -0.021(4) _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 N2 1.968(5) . ? Cu1 N1 1.985(6) . ? Cu1 O10 1.987(4) . ? Cu1 O1 1.990(4) . ? Cu1 O5 2.346(5) . ? Cu2 N3 1.973(5) . ? Cu2 N4 1.978(6) . ? Cu2 O9 1.985(4) . ? Cu2 O6 1.998(4) 1_655 ? Cu2 O2 2.323(5) 1_655 ? Cu3 N6 1.935(6) . ? Cu3 O13 1.966(4) . ? Cu3 O12 1.975(5) . ? Cu3 N5 1.984(6) . ? Cu4 N7 1.942(5) . ? Cu4 O14 1.971(4) . ? Cu4 O11 1.984(4) . ? Cu4 N8 2.001(6) . ? O1 C1 1.279(7) . ? O2 C1 1.228(8) . ? O2 Cu2 2.323(5) 1_455 ? O3 C8 1.266(9) . ? O4 C8 1.260(9) . ? O5 C9 1.237(8) . ? O6 C9 1.301(7) . ? O6 Cu2 1.998(4) 1_455 ? O7 C16 1.239(9) . ? O8 C16 1.252(9) . ? O9 C20 1.268(7) . ? O10 C21 1.274(7) . ? O11 C28 1.291(6) . ? O12 C29 1.276(6) . ? N1 C17 1.461(9) . ? N2 C20 1.305(8) . ? N2 C19 1.476(8) . ? N3 C21 1.287(8) . ? N3 C22 1.460(9) . ? N4 C24 1.480(12) . ? N5 C25 1.467(10) . ? N6 C28 1.301(8) . ? N6 C27 1.479(9) . ? N7 C29 1.289(8) . ? N7 C30 1.476(9) . ? N8 C32 1.470(10) . ? C1 C2 1.519(9) . ? C2 C7 1.376(8) . ? C2 C3 1.398(9) . ? C3 C4 1.365(10) . ? C4 C5 1.402(10) . ? C5 C6 1.394(10) . ? C6 C7 1.379(9) . ? C6 C8 1.520(9) . ? C9 C10 1.473(9) . ? C10 C15 1.403(8) . ? C10 C11 1.415(10) . ? C11 C12 1.348(10) . ? C12 C13 1.409(10) . ? C13 C14 1.400(9) . ? C14 C15 1.377(9) . ? C14 C16 1.524(9) . ? C17 C18 1.478(9) . ? C18 C19 1.525(10) . ? C20 C21 1.518(7) . ? C22 C23 1.466(11) . ? C23 C24 1.343(13) . ? C25 C26 1.467(12) . ? C26 C27 1.517(10) . ? C28 C29 1.492(7) . ? C30 C31 1.518(10) . ? C31 C32 1.518(11) . ? 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 Cu1 N1 95.1(2) . . ? N2 Cu1 O10 83.4(2) . . ? N1 Cu1 O10 174.0(3) . . ? N2 Cu1 O1 156.8(2) . . ? N1 Cu1 O1 92.4(2) . . ? O10 Cu1 O1 86.9(2) . . ? N2 Cu1 O5 110.6(2) . . ? N1 Cu1 O5 96.6(2) . . ? O10 Cu1 O5 89.3(2) . . ? O1 Cu1 O5 90.3(2) . . ? N3 Cu2 N4 94.6(2) . . ? N3 Cu2 O9 83.2(2) . . ? N4 Cu2 O9 171.3(3) . . ? N3 Cu2 O6 158.2(2) . 1_655 ? N4 Cu2 O6 91.9(2) . 1_655 ? O9 Cu2 O6 87.3(2) . 1_655 ? N3 Cu2 O2 109.2(2) . 1_655 ? N4 Cu2 O2 97.6(2) . 1_655 ? O9 Cu2 O2 91.0(2) . 1_655 ? O6 Cu2 O2 90.4(2) 1_655 1_655 ? N6 Cu3 O13 163.3(2) . . ? N6 Cu3 O12 84.3(2) . . ? O13 Cu3 O12 86.6(2) . . ? N6 Cu3 N5 97.0(2) . . ? O13 Cu3 N5 91.9(2) . . ? O12 Cu3 N5 178.1(2) . . ? N7 Cu4 O14 163.1(2) . . ? N7 Cu4 O11 84.6(2) . . ? O14 Cu4 O11 86.2(2) . . ? N7 Cu4 N8 96.5(2) . . ? O14 Cu4 N8 92.5(2) . . ? O11 Cu4 N8 178.8(2) . . ? C1 O1 Cu1 126.5(4) . . ? C1 O2 Cu2 125.4(4) . 1_455 ? C9 O5 Cu1 122.1(4) . . ? C9 O6 Cu2 127.2(4) . 1_455 ? C20 O9 Cu2 111.4(4) . . ? C21 O10 Cu1 111.8(4) . . ? C28 O11 Cu4 109.6(4) . . ? C29 O12 Cu3 110.8(4) . . ? C17 N1 Cu1 120.3(5) . . ? C20 N2 C19 119.1(6) . . ? C20 N2 Cu1 113.6(4) . . ? C19 N2 Cu1 127.3(4) . . ? C21 N3 C22 118.0(6) . . ? C21 N3 Cu2 113.9(5) . . ? C22 N3 Cu2 128.1(5) . . ? C24 N4 Cu2 118.3(5) . . ? C25 N5 Cu3 116.7(5) . . ? C28 N6 C27 118.7(6) . . ? C28 N6 Cu3 112.7(4) . . ? C27 N6 Cu3 128.5(4) . . ? C29 N7 C30 119.2(6) . . ? C29 N7 Cu4 112.8(4) . . ? C30 N7 Cu4 128.0(4) . . ? C32 N8 Cu4 119.1(5) . . ? O2 C1 O1 125.7(6) . . ? O2 C1 C2 118.8(5) . . ? O1 C1 C2 115.5(5) . . ? C7 C2 C3 120.1(6) . . ? C7 C2 C1 119.1(6) . . ? C3 C2 C1 120.8(6) . . ? C4 C3 C2 120.3(6) . . ? C3 C4 C5 119.6(7) . . ? C6 C5 C4 119.9(7) . . ? C7 C6 C5 119.7(6) . . ? C7 C6 C8 119.5(6) . . ? C5 C6 C8 120.8(6) . . ? C2 C7 C6 120.3(6) . . ? O4 C8 O3 124.3(7) . . ? O4 C8 C6 118.8(7) . . ? O3 C8 C6 116.8(6) . . ? O5 C9 O6 123.5(6) . . ? O5 C9 C10 119.9(5) . . ? O6 C9 C10 116.7(6) . . ? C15 C10 C11 117.0(6) . . ? C15 C10 C9 119.6(6) . . ? C11 C10 C9 123.4(6) . . ? C12 C11 C10 121.0(6) . . ? C11 C12 C13 121.5(7) . . ? C14 C13 C12 118.9(7) . . ? C15 C14 C13 118.9(6) . . ? C15 C14 C16 120.4(6) . . ? C13 C14 C16 120.8(6) . . ? C14 C15 C10 122.6(6) . . ? O7 C16 O8 125.3(7) . . ? O7 C16 C14 119.3(7) . . ? O8 C16 C14 115.5(6) . . ? N1 C17 C18 111.9(6) . . ? C17 C18 C19 114.5(6) . . ? N2 C19 C18 111.3(6) . . ? O9 C20 N2 128.4(6) . . ? O9 C20 C21 118.2(5) . . ? N2 C20 C21 113.5(5) . . ? O10 C21 N3 128.9(7) . . ? O10 C21 C20 117.7(5) . . ? N3 C21 C20 113.3(5) . . ? N3 C22 C23 113.0(7) . . ? C24 C23 C22 123.3(10) . . ? C23 C24 N4 119.8(10) . . ? C26 C25 N5 114.5(8) . . ? C25 C26 C27 115.3(8) . . ? N6 C27 C26 110.8(6) . . ? O11 C28 N6 127.3(6) . . ? O11 C28 C29 118.1(5) . . ? N6 C28 C29 114.6(5) . . ? O12 C29 N7 127.6(6) . . ? O12 C29 C28 117.5(5) . . ? N7 C29 C28 114.9(5) . . ? N7 C30 C31 111.3(6) . . ? C30 C31 C32 114.2(7) . . ? N8 C32 C31 112.5(7) . . ? 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 N2 Cu1 O1 C1 -161.1(6) . . . . ? N1 Cu1 O1 C1 -52.2(6) . . . . ? O10 Cu1 O1 C1 133.7(5) . . . . ? O5 Cu1 O1 C1 44.4(5) . . . . ? N2 Cu1 O5 C9 78.4(5) . . . . ? N1 Cu1 O5 C9 -19.6(5) . . . . ? O10 Cu1 O5 C9 161.1(5) . . . . ? O1 Cu1 O5 C9 -112.0(5) . . . . ? N3 Cu2 O9 C20 0.1(4) . . . . ? N4 Cu2 O9 C20 -75.6(16) . . . . ? O6 Cu2 O9 C20 -160.3(5) 1_655 . . . ? O2 Cu2 O9 C20 109.4(4) 1_655 . . . ? N2 Cu1 O10 C21 0.6(4) . . . . ? N1 Cu1 O10 C21 76.6(22) . . . . ? O1 Cu1 O10 C21 159.5(4) . . . . ? O5 Cu1 O10 C21 -110.2(4) . . . . ? N7 Cu4 O11 C28 2.4(4) . . . . ? O14 Cu4 O11 C28 -163.3(4) . . . . ? N8 Cu4 O11 C28 -156.4(111) . . . . ? N6 Cu3 O12 C29 -1.8(4) . . . . ? O13 Cu3 O12 C29 164.2(4) . . . . ? N5 Cu3 O12 C29 129.6(68) . . . . ? N2 Cu1 N1 C17 -16.2(6) . . . . ? O10 Cu1 N1 C17 -91.5(22) . . . . ? O1 Cu1 N1 C17 -174.2(6) . . . . ? O5 Cu1 N1 C17 95.2(6) . . . . ? N1 Cu1 N2 C20 -175.5(5) . . . . ? O10 Cu1 N2 C20 -1.3(5) . . . . ? O1 Cu1 N2 C20 -67.1(8) . . . . ? O5 Cu1 N2 C20 85.5(5) . . . . ? N1 Cu1 N2 C19 5.3(6) . . . . ? O10 Cu1 N2 C19 179.5(6) . . . . ? O1 Cu1 N2 C19 113.6(7) . . . . ? O5 Cu1 N2 C19 -93.8(6) . . . . ? N4 Cu2 N3 C21 170.3(5) . . . . ? O9 Cu2 N3 C21 -1.3(5) . . . . ? O6 Cu2 N3 C21 63.2(8) 1_655 . . . ? O2 Cu2 N3 C21 -90.0(5) 1_655 . . . ? N4 Cu2 N3 C22 -9.1(7) . . . . ? O9 Cu2 N3 C22 179.4(6) . . . . ? O6 Cu2 N3 C22 -116.1(7) 1_655 . . . ? O2 Cu2 N3 C22 90.6(6) 1_655 . . . ? N3 Cu2 N4 C24 16.0(8) . . . . ? O9 Cu2 N4 C24 90.9(18) . . . . ? O6 Cu2 N4 C24 175.3(8) 1_655 . . . ? O2 Cu2 N4 C24 -94.1(8) 1_655 . . . ? N6 Cu3 N5 C25 10.8(6) . . . . ? O13 Cu3 N5 C25 -155.0(6) . . . . ? O12 Cu3 N5 C25 -120.5(68) . . . . ? O13 Cu3 N6 C28 -54.5(10) . . . . ? O12 Cu3 N6 C28 2.6(4) . . . . ? N5 Cu3 N6 C28 -176.0(5) . . . . ? O13 Cu3 N6 C27 125.3(8) . . . . ? O12 Cu3 N6 C27 -177.6(6) . . . . ? N5 Cu3 N6 C27 3.8(6) . . . . ? O14 Cu4 N7 C29 55.0(10) . . . . ? O11 Cu4 N7 C29 -2.6(5) . . . . ? N8 Cu4 N7 C29 177.0(5) . . . . ? O14 Cu4 N7 C30 -126.3(8) . . . . ? O11 Cu4 N7 C30 176.1(6) . . . . ? N8 Cu4 N7 C30 -4.3(6) . . . . ? N7 Cu4 N8 C32 -8.1(6) . . . . ? O14 Cu4 N8 C32 157.6(6) . . . . ? O11 Cu4 N8 C32 150.7(110) . . . . ? Cu2 O2 C1 O1 -111.6(6) 1_455 . . . ? Cu2 O2 C1 C2 68.4(7) 1_455 . . . ? Cu1 O1 C1 O2 11.4(9) . . . . ? Cu1 O1 C1 C2 -168.6(4) . . . . ? O2 C1 C2 C7 20.9(9) . . . . ? O1 C1 C2 C7 -159.1(6) . . . . ? O2 C1 C2 C3 -158.5(6) . . . . ? O1 C1 C2 C3 21.5(9) . . . . ? C7 C2 C3 C4 -1.0(10) . . . . ? C1 C2 C3 C4 178.4(6) . . . . ? C2 C3 C4 C5 1.1(11) . . . . ? C3 C4 C5 C6 0.9(11) . . . . ? C4 C5 C6 C7 -3.0(11) . . . . ? C4 C5 C6 C8 177.0(7) . . . . ? C3 C2 C7 C6 -1.1(9) . . . . ? C1 C2 C7 C6 179.5(6) . . . . ? C5 C6 C7 C2 3.1(10) . . . . ? C8 C6 C7 C2 -176.9(6) . . . . ? C7 C6 C8 O4 -161.8(7) . . . . ? C5 C6 C8 O4 18.3(10) . . . . ? C7 C6 C8 O3 21.5(10) . . . . ? C5 C6 C8 O3 -158.4(7) . . . . ? Cu1 O5 C9 O6 112.9(6) . . . . ? Cu1 O5 C9 C10 -68.6(7) . . . . ? Cu2 O6 C9 O5 -13.4(10) 1_455 . . . ? Cu2 O6 C9 C10 168.0(4) 1_455 . . . ? O5 C9 C10 C15 -19.6(9) . . . . ? O6 C9 C10 C15 159.0(6) . . . . ? O5 C9 C10 C11 159.9(7) . . . . ? O6 C9 C10 C11 -21.5(10) . . . . ? C15 C10 C11 C12 2.4(10) . . . . ? C9 C10 C11 C12 -177.0(7) . . . . ? C10 C11 C12 C13 -0.6(12) . . . . ? C11 C12 C13 C14 -2.5(11) . . . . ? C12 C13 C14 C15 3.7(10) . . . . ? C12 C13 C14 C16 -175.8(7) . . . . ? C13 C14 C15 C10 -1.9(10) . . . . ? C16 C14 C15 C10 177.6(6) . . . . ? C11 C10 C15 C14 -1.1(10) . . . . ? C9 C10 C15 C14 178.4(6) . . . . ? C15 C14 C16 O7 154.9(7) . . . . ? C13 C14 C16 O7 -25.6(10) . . . . ? C15 C14 C16 O8 -24.6(10) . . . . ? C13 C14 C16 O8 154.9(7) . . . . ? Cu1 N1 C17 C18 49.7(8) . . . . ? N1 C17 C18 C19 -75.9(9) . . . . ? C20 N2 C19 C18 155.0(6) . . . . ? Cu1 N2 C19 C18 -25.8(9) . . . . ? C17 C18 C19 N2 61.2(9) . . . . ? Cu2 O9 C20 N2 -178.3(6) . . . . ? Cu2 O9 C20 C21 0.9(6) . . . . ? C19 N2 C20 O9 0.2(11) . . . . ? Cu1 N2 C20 O9 -179.1(5) . . . . ? C19 N2 C20 C21 -179.1(5) . . . . ? Cu1 N2 C20 C21 1.6(6) . . . . ? Cu1 O10 C21 N3 -178.2(6) . . . . ? Cu1 O10 C21 C20 0.1(6) . . . . ? C22 N3 C21 O10 -0.3(11) . . . . ? Cu2 N3 C21 O10 -179.7(5) . . . . ? C22 N3 C21 C20 -178.6(6) . . . . ? Cu2 N3 C21 C20 2.0(6) . . . . ? O9 C20 C21 O10 179.5(6) . . . . ? N2 C20 C21 O10 -1.2(7) . . . . ? O9 C20 C21 N3 -2.0(7) . . . . ? N2 C20 C21 N3 177.3(7) . . . . ? C21 N3 C22 C23 -157.9(8) . . . . ? Cu2 N3 C22 C23 21.4(11) . . . . ? N3 C22 C23 C24 -47.2(15) . . . . ? C22 C23 C24 N4 61.1(18) . . . . ? Cu2 N4 C24 C23 -41.9(15) . . . . ? Cu3 N5 C25 C26 -48.1(10) . . . . ? N5 C25 C26 C27 77.0(11) . . . . ? C28 N6 C27 C26 -164.2(7) . . . . ? Cu3 N6 C27 C26 16.0(10) . . . . ? C25 C26 C27 N6 -56.0(11) . . . . ? Cu4 O11 C28 N6 176.9(5) . . . . ? Cu4 O11 C28 C29 -1.9(6) . . . . ? C27 N6 C28 O11 -1.4(10) . . . . ? Cu3 N6 C28 O11 178.4(5) . . . . ? C27 N6 C28 C29 177.4(6) . . . . ? Cu3 N6 C28 C29 -2.7(6) . . . . ? Cu3 O12 C29 N7 -178.7(6) . . . . ? Cu3 O12 C29 C28 0.9(6) . . . . ? C30 N7 C29 O12 3.0(11) . . . . ? Cu4 N7 C29 O12 -178.2(5) . . . . ? C30 N7 C29 C28 -176.6(5) . . . . ? Cu4 N7 C29 C28 2.2(6) . . . . ? O11 C28 C29 O12 -179.8(6) . . . . ? N6 C28 C29 O12 1.2(7) . . . . ? O11 C28 C29 N7 -0.1(7) . . . . ? N6 C28 C29 N7 -179.1(7) . . . . ? C29 N7 C30 C31 159.4(7) . . . . ? Cu4 N7 C30 C31 -19.2(9) . . . . ? N7 C30 C31 C32 60.3(10) . . . . ? Cu4 N8 C32 C31 44.2(9) . . . . ? C30 C31 C32 N8 -76.2(10) . . . . ? _refine_diff_density_max 0.653 _refine_diff_density_min -0.369 _refine_diff_density_rms 0.080 #===================================================END data_Compound 3 _database_code_CSD 164204 [Cu2(trans-oxen)(phth)]n.2nH2O _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C14 H20 Cu2 N4 O8' _chemical_formula_weight 499.42 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 Orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 15.951(2) _cell_length_b 7.8879(8) _cell_length_c 14.8260(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1865.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used CCD _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description PRISM _exptl_crystal_colour 'BLACK BLUE' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.778 _exptl_crystal_density_method ? _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 2.331 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'BRUKER CCD AREA DETECTOR' _diffrn_measurement_method 'PHI AND OMEGA SCAN' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11849 _diffrn_reflns_av_R_equivalents 0.0478 _diffrn_reflns_av_sigmaI/netI 0.0500 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 27.53 _reflns_number_total 4246 _reflns_number_observed 3455 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL' _computing_publication_material 'SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0426P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.011(14) _refine_ls_number_reflns 4245 _refine_ls_number_parameters 313 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0472 _refine_ls_R_factor_obs 0.0361 _refine_ls_wR_factor_all 0.0843 _refine_ls_wR_factor_obs 0.0782 _refine_ls_goodness_of_fit_all 0.944 _refine_ls_goodness_of_fit_obs 1.002 _refine_ls_restrained_S_all 0.966 _refine_ls_restrained_S_obs 1.002 _refine_ls_shift/esd_max -0.279 _refine_ls_shift/esd_mean 0.030 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.64299(3) 0.29023(6) 0.61682(4) 0.02971(12) Uani 1 d . . Cu2 Cu 0.59980(3) -0.33893(6) 0.72953(3) 0.03149(13) Uani 1 d . . N1 N 0.5976(2) 0.0784(4) 0.5748(3) 0.0317(8) Uani 1 d . . N2 N 0.6066(3) 0.3709(5) 0.4944(3) 0.0375(9) Uani 1 d . . H2A H 0.5839(30) 0.4625(69) 0.5017(34) 0.047(16) Uiso 1 d . . H2B H 0.6579(33) 0.3643(66) 0.4479(40) 0.064(16) Uiso 1 d . . N3 N 0.6439(2) -0.1279(4) 0.7734(2) 0.0335(8) Uani 1 d . . N4 N 0.6463(2) -0.4322(5) 0.8452(3) 0.0414(9) Uani 1 d . . H4C H 0.6057(2) -0.4406(5) 0.8871(3) 0.050 Uiso 1 calc R . H4D H 0.6685(2) -0.5357(5) 0.8361(3) 0.050 Uiso 1 calc R . O1 O 0.6648(2) 0.1523(3) 0.7308(2) 0.0329(6) Uani 1 d . . O2 O 0.5740(2) -0.1998(3) 0.6187(2) 0.0333(6) Uani 1 d . . O3 O 0.8127(2) 0.3857(4) 0.5750(3) 0.0535(10) Uani 1 d . . O4 O 0.7072(2) 0.4898(4) 0.6529(2) 0.0332(7) Uani 1 d . . O5 O 0.9272(2) 0.3934(4) 0.7449(3) 0.0463(9) Uani 1 d . . O6 O 1.0356(2) 0.5358(3) 0.6924(2) 0.0346(7) Uani 1 d . . O7W O 0.7869(2) 0.2965(4) 0.8383(2) 0.0514(9) Uani 1 d . . O8W O 0.9656(3) 0.3523(5) 0.4874(3) 0.0567(10) Uani 1 d . . H8WA H 0.9991(38) 0.2888(72) 0.5302(40) 0.057(17) Uiso 1 d . . H8WB H 0.9179(37) 0.3661(68) 0.5096(39) 0.054(18) Uiso 1 d . . C1 C 0.6395(2) -0.0024(5) 0.7199(3) 0.0302(9) Uani 1 d . . C2 C 0.5997(2) -0.0483(5) 0.6296(3) 0.0285(9) Uani 1 d . . C3 C 0.5634(4) 0.0739(6) 0.4846(3) 0.0404(11) Uani 1 d . . H3A H 0.5201(31) -0.0012(79) 0.4853(37) 0.060(16) Uiso 1 d . . H3B H 0.5990(28) 0.0398(61) 0.4528(35) 0.036(14) Uiso 1 d . . C4 C 0.5381(3) 0.2536(6) 0.4626(4) 0.0434(11) Uani 1 d . . H4A H 0.5195(33) 0.2865(64) 0.4100(36) 0.049(15) Uiso 1 d . . H4B H 0.4812(26) 0.2711(50) 0.4979(28) 0.025(11) Uiso 1 d . . C5 C 0.6834(4) -0.1328(7) 0.8631(3) 0.0490(13) Uani 1 d . . H5A H 0.7280(39) -0.0685(69) 0.8607(49) 0.076(22) Uiso 1 d . . H5B H 0.6385(35) -0.0806(87) 0.9191(43) 0.091(22) Uiso 1 d . . C6 C 0.7120(4) -0.3114(7) 0.8752(4) 0.0560(15) Uani 1 d . . H6A H 0.7728(41) -0.3173(70) 0.8281(44) 0.074(19) Uiso 1 d . . H6B H 0.7255(33) -0.3291(65) 0.9296(40) 0.057(18) Uiso 1 d . . C7 C 0.7820(2) 0.4981(4) 0.6214(3) 0.0289(8) Uani 1 d . . C8 C 0.8282(2) 0.6614(5) 0.6415(3) 0.0304(9) Uani 1 d . . C9 C 0.7900(3) 0.8105(5) 0.6120(4) 0.0406(10) Uani 1 d . . H9 H 0.7400(30) 0.8073(48) 0.5871(28) 0.025(11) Uiso 1 d . . C10 C 0.8247(3) 0.9661(6) 0.6279(4) 0.0520(15) Uani 1 d . . H10 H 0.7997(3) 1.0634(6) 0.6049(4) 0.062 Uiso 1 calc R . C11 C 0.8965(3) 0.9773(6) 0.6779(5) 0.059(2) Uani 1 d . . H11 H 0.9208(32) 1.0492(72) 0.6944(40) 0.056(18) Uiso 1 d . . C12 C 0.9365(3) 0.8311(7) 0.7033(5) 0.047(2) Uani 1 d . . H12 H 0.9647(25) 0.8301(55) 0.7279(33) 0.009(12) Uiso 1 d . . C13 C 0.9059(2) 0.6721(5) 0.6851(3) 0.0321(9) Uani 1 d . . C14 C 0.9569(2) 0.5208(5) 0.7099(3) 0.0294(9) Uani 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 0.0320(2) 0.0229(2) 0.0342(2) 0.0005(2) -0.0013(2) -0.0022(2) Cu2 0.0345(3) 0.0232(2) 0.0367(3) 0.0015(2) -0.0008(2) -0.0015(2) N1 0.036(2) 0.023(2) 0.036(2) 0.0037(15) -0.004(2) -0.0042(14) N2 0.046(2) 0.032(2) 0.034(2) 0.005(2) 0.005(2) 0.004(2) N3 0.041(2) 0.029(2) 0.031(2) 0.0012(15) -0.006(2) -0.005(2) N4 0.052(2) 0.033(2) 0.039(2) 0.007(2) 0.006(2) 0.008(2) O1 0.0374(14) 0.0261(13) 0.0352(14) 0.0018(14) -0.007(2) -0.0030(11) O2 0.0386(14) 0.0222(12) 0.0392(15) 0.0022(14) -0.010(2) -0.0028(11) O3 0.042(2) 0.039(2) 0.080(3) -0.023(2) 0.013(2) 0.001(2) O4 0.0243(15) 0.0320(15) 0.043(2) -0.0018(12) 0.0026(13) -0.0059(11) O5 0.036(2) 0.036(2) 0.067(2) 0.019(2) 0.006(2) -0.0027(13) O6 0.029(2) 0.0251(14) 0.050(2) -0.0003(13) 0.0044(13) 0.0038(12) O7W 0.045(2) 0.064(2) 0.045(2) -0.002(2) -0.006(2) -0.007(2) O8W 0.047(2) 0.066(3) 0.057(2) 0.010(2) 0.003(2) 0.005(2) C1 0.024(2) 0.028(2) 0.039(3) -0.002(2) 0.000(2) 0.0018(14) C2 0.022(2) 0.029(2) 0.035(2) -0.004(2) -0.003(2) 0.0002(15) C3 0.048(3) 0.036(3) 0.037(3) -0.001(2) -0.006(2) -0.006(2) C4 0.045(3) 0.046(3) 0.039(3) 0.007(2) -0.009(2) -0.003(2) C5 0.065(4) 0.047(3) 0.034(3) 0.005(2) -0.017(2) -0.008(3) C6 0.074(4) 0.055(3) 0.039(3) 0.010(3) -0.019(3) 0.001(3) C7 0.027(2) 0.024(2) 0.035(2) 0.007(2) -0.005(2) 0.0012(14) C8 0.028(2) 0.022(2) 0.041(2) 0.002(2) 0.011(2) 0.004(2) C9 0.031(2) 0.030(2) 0.061(3) 0.010(2) 0.010(3) 0.009(2) C10 0.036(2) 0.023(2) 0.097(4) 0.008(3) 0.028(3) 0.007(2) C11 0.038(3) 0.019(2) 0.120(5) -0.017(3) 0.029(3) -0.008(2) C12 0.026(3) 0.037(3) 0.079(5) -0.014(3) 0.010(3) -0.002(2) C13 0.023(2) 0.028(2) 0.045(2) -0.007(2) 0.014(2) -0.003(2) C14 0.027(2) 0.028(2) 0.033(3) -0.006(2) 0.001(2) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.925(3) . ? Cu1 O4 1.953(3) . ? Cu1 N2 2.009(4) . ? Cu1 O1 2.039(3) . ? Cu2 N3 1.921(3) . ? Cu2 O6 1.940(3) 3_455 ? Cu2 N4 2.008(4) . ? Cu2 O2 2.018(3) . ? N1 C2 1.289(5) . ? N1 C3 1.445(6) . ? N2 C4 1.507(6) . ? N3 C1 1.270(5) . ? N3 C5 1.472(6) . ? N4 C6 1.484(7) . ? O1 C1 1.295(4) . ? O2 C2 1.274(4) . ? O3 C7 1.224(5) . ? O4 C7 1.283(4) . ? O5 C14 1.226(5) . ? O6 C14 1.287(4) . ? O6 Cu2 1.940(3) 3 ? C1 C2 1.526(5) . ? C3 C4 1.510(7) . ? C5 C6 1.491(8) . ? C7 C8 1.514(6) . ? C8 C9 1.395(6) . ? C8 C13 1.399(6) . ? C9 C10 1.367(6) . ? C10 C11 1.367(9) . ? C11 C12 1.371(8) . ? C12 C13 1.373(7) . ? C13 C14 1.491(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 O4 170.34(13) . . ? N1 Cu1 N2 82.7(2) . . ? O4 Cu1 N2 98.25(15) . . ? N1 Cu1 O1 82.51(13) . . ? O4 Cu1 O1 96.53(12) . . ? N2 Cu1 O1 165.18(14) . . ? N3 Cu2 O6 169.50(14) . 3_455 ? N3 Cu2 N4 83.8(2) . . ? O6 Cu2 N4 98.30(14) 3_455 . ? N3 Cu2 O2 83.06(13) . . ? O6 Cu2 O2 95.53(12) 3_455 . ? N4 Cu2 O2 165.88(13) . . ? C2 N1 C3 125.1(4) . . ? C2 N1 Cu1 117.3(3) . . ? C3 N1 Cu1 117.6(3) . . ? C4 N2 Cu1 107.3(3) . . ? C1 N3 C5 127.5(4) . . ? C1 N3 Cu2 116.3(3) . . ? C5 N3 Cu2 116.1(3) . . ? C6 N4 Cu2 106.3(3) . . ? C1 O1 Cu1 110.2(3) . . ? C2 O2 Cu2 110.0(3) . . ? C7 O4 Cu1 115.4(3) . . ? C14 O6 Cu2 112.6(2) . 3 ? N3 C1 O1 129.7(4) . . ? N3 C1 C2 112.7(3) . . ? O1 C1 C2 117.6(4) . . ? O2 C2 N1 129.8(4) . . ? O2 C2 C1 117.9(4) . . ? N1 C2 C1 112.3(3) . . ? N1 C3 C4 106.1(4) . . ? N2 C4 C3 108.4(4) . . ? N3 C5 C6 105.3(4) . . ? N4 C6 C5 110.8(5) . . ? O3 C7 O4 122.7(4) . . ? O3 C7 C8 122.1(4) . . ? O4 C7 C8 115.1(4) . . ? C9 C8 C13 118.7(4) . . ? C9 C8 C7 116.3(4) . . ? C13 C8 C7 125.0(3) . . ? C10 C9 C8 121.7(5) . . ? C9 C10 C11 119.4(4) . . ? C10 C11 C12 119.0(5) . . ? C11 C12 C13 123.3(6) . . ? C12 C13 C8 117.4(4) . . ? C12 C13 C14 119.2(4) . . ? C8 C13 C14 123.3(3) . . ? O5 C14 O6 122.5(4) . . ? O5 C14 C13 123.3(4) . . ? O6 C14 C13 114.2(3) . . ? _refine_diff_density_max 0.548 _refine_diff_density_min -0.292 _refine_diff_density_rms 0.079 #======================================END