Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'L. Lindoy' 'Jack K. Clegg' 'John C. McMurtrie' 'David Schilter' _publ_contact_author_name 'Prof Leonard F. Lindoy' _publ_contact_author_address ; School of Chemistry, F11 University of Sydney Sydney NSW 2006. AUSTRALIA ; _publ_contact_author_email 'LINDOY@CHEM.USYD.EDU.AU ' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Dinuclear bis-beta-diketonato ligand derivatives with of iron(III) and copper(II) and use of the latter as components for the assembly of extended metallo-supramolecular structures ; data_lj29sad _database_code_depnum_ccdc_archive 'CCDC 258475' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H26 O4' _chemical_formula_sum 'C20 H26 O4' _chemical_formula_weight 330.41 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' O O 0.0106 0.0060 '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 ' _symmetry_space_group_name_Hall '-C 2yc' 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 19.3711(10) _cell_length_b 9.5415(5) _cell_length_c 10.8882(6) _cell_angle_alpha 90.00 _cell_angle_beta 116.1840(10) _cell_angle_gamma 90.00 _cell_volume 1805.94(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5754 _cell_measurement_theta_min 2.343 _cell_measurement_theta_max 28.2585 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.550 _exptl_crystal_size_mid 0.435 _exptl_crystal_size_min 0.290 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.215 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 0.083 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.864 _exptl_absorpt_correction_T_max 0.980 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 129 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 8673 _diffrn_reflns_av_R_equivalents 0.0147 _diffrn_reflns_av_sigmaI/netI 0.0122 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 28.27 _reflns_number_total 2176 _reflns_number_gt 1972 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker,1995)' _computing_cell_refinement 'SAINT (Bruker,1995)' _computing_data_reduction 'SAINT and XPREP (Bruker, 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEPIII (Farrugia, 1997) WINGX-32 (Farrugia, 1999) ; _computing_publication_material 'enCIFer 1.0 (CCDC, 2003)' _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^)+(0.0658P)^2^+1.0128P] 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 2176 _refine_ls_number_parameters 116 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0436 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.1170 _refine_ls_wR_factor_gt 0.1136 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 C1 C 0.74086(7) 0.59587(13) -0.13843(13) 0.0336(3) Uani 1 1 d . . . H1A H 0.7101 0.5197 -0.1977 0.050 Uiso 1 1 calc R . . H1B H 0.7080 0.6778 -0.1505 0.050 Uiso 1 1 calc R . . H1C H 0.7630 0.5654 -0.0427 0.050 Uiso 1 1 calc R . . C2 C 0.85373(7) 0.75356(12) -0.08276(13) 0.0352(3) Uani 1 1 d . . . H2A H 0.8772 0.7211 0.0124 0.053 Uiso 1 1 calc R . . H2B H 0.8203 0.8340 -0.0920 0.053 Uiso 1 1 calc R . . H2C H 0.8942 0.7815 -0.1087 0.053 Uiso 1 1 calc R . . C3 C 0.77186(8) 0.68188(14) -0.32577(12) 0.0373(3) Uani 1 1 d . . . H3A H 0.8135 0.7065 -0.3497 0.056 Uiso 1 1 calc R . . H3B H 0.7389 0.7638 -0.3384 0.056 Uiso 1 1 calc R . . H3C H 0.7413 0.6055 -0.3850 0.056 Uiso 1 1 calc R . . C4 C 0.80594(6) 0.63478(11) -0.17669(10) 0.0248(2) Uani 1 1 d . . . C5 C 0.85625(6) 0.50523(11) -0.15643(10) 0.0229(2) Uani 1 1 d . . . C6 C 0.89508(6) 0.44321(11) -0.02244(10) 0.0240(2) Uani 1 1 d . . . H6 H 0.8944 0.4893 0.0543 0.029 Uiso 1 1 calc R . . C7 C 0.93291(6) 0.31851(11) -0.00504(10) 0.0234(2) Uani 1 1 d . . . C8 C 0.96802(6) 0.24251(11) 0.12631(10) 0.0241(2) Uani 1 1 d . . . C9 C 0.96910(7) 0.09591(12) 0.12709(12) 0.0313(3) Uani 1 1 d . . . H9 H 0.9486 0.0458 0.0431 0.038 Uiso 1 1 calc R . . C10 C 1.0000 0.02348(18) 0.2500 0.0358(4) Uani 1 2 d S . . H10 H 1.0000 -0.0761 0.2500 0.043 Uiso 1 2 calc SR . . C11 C 1.0000 0.31517(15) 0.2500 0.0233(3) Uani 1 2 d S . . H11 H 1.0000 0.4147 0.2500 0.028 Uiso 1 2 calc SR . . O1 O 0.86035(5) 0.44939(9) -0.25704(7) 0.0292(2) Uani 1 1 d . . . O2 O 0.93812(5) 0.25243(9) -0.10825(8) 0.0320(2) Uani 1 1 d D . . H2O H 0.9128(9) 0.3136(15) -0.1835(15) 0.038 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 C1 0.0301(6) 0.0368(6) 0.0387(6) 0.0047(5) 0.0196(5) 0.0055(5) C2 0.0364(6) 0.0292(6) 0.0403(6) -0.0053(5) 0.0173(5) 0.0006(5) C3 0.0475(7) 0.0404(7) 0.0253(5) 0.0093(5) 0.0171(5) 0.0172(5) C4 0.0276(5) 0.0273(5) 0.0212(5) 0.0017(4) 0.0122(4) 0.0045(4) C5 0.0229(5) 0.0264(5) 0.0205(5) -0.0007(4) 0.0105(4) -0.0002(4) C6 0.0263(5) 0.0277(5) 0.0185(4) -0.0020(4) 0.0102(4) 0.0009(4) C7 0.0221(5) 0.0270(5) 0.0205(5) -0.0037(4) 0.0089(4) -0.0020(4) C8 0.0221(5) 0.0259(5) 0.0235(5) -0.0006(4) 0.0094(4) 0.0010(4) C9 0.0353(6) 0.0269(6) 0.0312(6) -0.0052(4) 0.0142(5) -0.0010(4) C10 0.0459(10) 0.0228(7) 0.0390(9) 0.000 0.0191(8) 0.000 C11 0.0227(6) 0.0228(7) 0.0231(7) 0.000 0.0090(5) 0.000 O1 0.0367(4) 0.0324(4) 0.0204(4) -0.0003(3) 0.0144(3) 0.0058(3) O2 0.0380(5) 0.0340(4) 0.0227(4) -0.0034(3) 0.0122(3) 0.0089(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C4 1.5374(15) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C4 1.5336(16) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.5255(15) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.5287(14) . ? C5 O1 1.2518(12) . ? C5 C6 1.4408(14) . ? C6 C7 1.3660(15) . ? C6 H6 0.9500 . ? C7 O2 1.3308(12) . ? C7 C8 1.4749(14) . ? C8 C11 1.3936(12) . ? C8 C9 1.3988(16) . ? C9 C10 1.3856(14) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? O2 H2O 0.948(13) . ? 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 C4 C1 H1A 109.5 . . ? C4 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C2 H2A 109.5 . . ? C4 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C3 C4 C5 109.92(9) . . ? C3 C4 C2 110.02(10) . . ? C5 C4 C2 110.03(9) . . ? C3 C4 C1 109.75(10) . . ? C5 C4 C1 108.20(9) . . ? C2 C4 C1 108.88(9) . . ? O1 C5 C6 120.33(9) . . ? O1 C5 C4 120.03(9) . . ? C6 C5 C4 119.54(9) . . ? C7 C6 C5 120.44(9) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? O2 C7 C6 122.11(9) . . ? O2 C7 C8 114.30(9) . . ? C6 C7 C8 123.53(9) . . ? C11 C8 C9 119.51(10) . . ? C11 C8 C7 120.70(10) . . ? C9 C8 C7 119.79(10) . . ? C10 C9 C8 120.23(11) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C9 120.16(15) 2_755 . ? C9 C10 H10 119.9 2_755 . ? C9 C10 H10 119.9 . . ? C8 C11 C8 120.33(14) . 2_755 ? C8 C11 H11 119.8 . . ? C8 C11 H11 119.8 2_755 . ? C7 O2 H2O 103.6(10) . . ? 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 C3 C4 C5 O1 -4.33(15) . . . . ? C2 C4 C5 O1 -125.64(11) . . . . ? C1 C4 C5 O1 115.51(11) . . . . ? C3 C4 C5 C6 179.38(10) . . . . ? C2 C4 C5 C6 58.06(12) . . . . ? C1 C4 C5 C6 -60.78(12) . . . . ? O1 C5 C6 C7 -3.95(16) . . . . ? C4 C5 C6 C7 172.34(10) . . . . ? C5 C6 C7 O2 2.64(16) . . . . ? C5 C6 C7 C8 -174.39(9) . . . . ? O2 C7 C8 C11 149.43(9) . . . . ? C6 C7 C8 C11 -33.33(15) . . . . ? O2 C7 C8 C9 -30.77(14) . . . . ? C6 C7 C8 C9 146.47(11) . . . . ? C11 C8 C9 C10 1.62(15) . . . . ? C7 C8 C9 C10 -178.18(8) . . . . ? C8 C9 C10 C9 -0.81(17) . . . 2_755 ? C9 C8 C11 C8 -0.80(8) . . . 2_755 ? C7 C8 C11 C8 179.00(11) . . . 2_755 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2O O1 0.948(13) 1.623(14) 2.5044(11) 152.9(15) . _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.350 _refine_diff_density_min -0.228 _refine_diff_density_rms 0.043 data_lj45sad _database_code_depnum_ccdc_archive 'CCDC 258476' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H64 Cu2 N4 O8, 2(C10 H8 N2)' _chemical_formula_sum 'C80 H80 Cu2 N8 O8' _chemical_formula_weight 1408.60 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 _symmetry_space_group_name_Hall '-P 2ybc' 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 11.8449(7) _cell_length_b 11.7625(7) _cell_length_c 25.3454(15) _cell_angle_alpha 90.00 _cell_angle_beta 94.3280(10) _cell_angle_gamma 90.00 _cell_volume 3521.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 16612 _cell_measurement_theta_min 2.366 _cell_measurement_theta_max 28.227 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.54 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.329 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1476 _exptl_absorpt_coefficient_mu 0.667 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.760 _exptl_absorpt_correction_T_max 0.846 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 381 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.04 _diffrn_reflns_number 33963 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_av_sigmaI/netI 0.0190 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 28.33 _reflns_number_total 8407 _reflns_number_gt 7108 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1995)' _computing_cell_refinement 'SAINT (Bruker, 1995)' _computing_data_reduction 'SAINT and XPREP (Bruker, 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEPIII (Farrugia, 1997) WINGX-32 (Farrugia, 1999) ; _computing_publication_material 'enCIFer 1.0 (CCDC, 2003)' _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^)+(0.0705P)^2^+2.2948P] 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 8407 _refine_ls_number_parameters 448 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0516 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.1247 _refine_ls_wR_factor_gt 0.1172 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.003 _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 0.152303(18) 0.190690(19) 0.412913(9) 0.02418(8) Uani 1 1 d . . . O1 O 0.12240(12) 0.26387(12) 0.34522(5) 0.0306(3) Uani 1 1 d . . . O2 O -0.00008(11) 0.13398(12) 0.41252(5) 0.0286(3) Uani 1 1 d . . . O3 O -0.17165(11) -0.14830(12) 0.51327(5) 0.0285(3) Uani 1 1 d . . . O4 O -0.30005(11) -0.26088(12) 0.58449(5) 0.0292(3) Uani 1 1 d . . . C1 C 0.1644(3) 0.2707(3) 0.23680(12) 0.0620(8) Uani 1 1 d . . . H1A H 0.1733 0.3121 0.2038 0.093 Uiso 1 1 calc R . . H1B H 0.1675 0.1887 0.2301 0.093 Uiso 1 1 calc R . . H1C H 0.2255 0.2919 0.2632 0.093 Uiso 1 1 calc R . . C2 C -0.0424(3) 0.2638(3) 0.21656(10) 0.0558(7) Uani 1 1 d . . . H2A H -0.1174 0.2805 0.2285 0.084 Uiso 1 1 calc R . . H2B H -0.0354 0.1818 0.2107 0.084 Uiso 1 1 calc R . . H2C H -0.0327 0.3044 0.1835 0.084 Uiso 1 1 calc R . . C3 C 0.0449(3) 0.4277(2) 0.26735(12) 0.0605(8) Uani 1 1 d . . . H3A H 0.0592 0.4675 0.2346 0.091 Uiso 1 1 calc R . . H3B H 0.1034 0.4481 0.2951 0.091 Uiso 1 1 calc R . . H3C H -0.0296 0.4497 0.2784 0.091 Uiso 1 1 calc R . . C4 C 0.0473(2) 0.3015(2) 0.25811(9) 0.0408(5) Uani 1 1 d . . . C5 C 0.04018(17) 0.24186(17) 0.31188(8) 0.0292(4) Uani 1 1 d . . . C6 C -0.05006(18) 0.16994(17) 0.32184(8) 0.0318(4) Uani 1 1 d . . . H6 H -0.1038 0.1529 0.2932 0.038 Uiso 1 1 calc R . . C7 C -0.06649(15) 0.12149(15) 0.37098(7) 0.0243(4) Uani 1 1 d . . . C8 C -0.16870(15) 0.04913(16) 0.37825(7) 0.0248(4) Uani 1 1 d . . . C9 C -0.25843(17) 0.03720(18) 0.33965(8) 0.0293(4) Uani 1 1 d . . . H9 H -0.2570 0.0772 0.3071 0.035 Uiso 1 1 calc R . . C10 C -0.34945(17) -0.03231(19) 0.34833(8) 0.0332(4) Uani 1 1 d . . . H10 H -0.4094 -0.0407 0.3215 0.040 Uiso 1 1 calc R . . C11 C -0.35385(17) -0.08981(18) 0.39581(8) 0.0313(4) Uani 1 1 d . . . H11 H -0.4165 -0.1376 0.4014 0.038 Uiso 1 1 calc R . . C12 C -0.26611(16) -0.07760(16) 0.43561(7) 0.0264(4) Uani 1 1 d . . . C13 C -0.17378(16) -0.00916(16) 0.42600(7) 0.0260(4) Uani 1 1 d . . . H13 H -0.1131 -0.0020 0.4525 0.031 Uiso 1 1 calc R . . C14 C -0.26792(16) -0.13454(16) 0.48822(7) 0.0268(4) Uani 1 1 d . . . C15 C -0.37219(17) -0.16710(19) 0.50661(8) 0.0324(4) Uani 1 1 d . . . H15 H -0.4395 -0.1447 0.4865 0.039 Uiso 1 1 calc R . . C16 C -0.38295(16) -0.23055(17) 0.55276(8) 0.0285(4) Uani 1 1 d . . . C17 C -0.49886(17) -0.2728(2) 0.56767(9) 0.0357(5) Uani 1 1 d . . . C18 C -0.5981(2) -0.2203(3) 0.53438(13) 0.0628(8) Uani 1 1 d . . . H18A H -0.5903 -0.1373 0.5345 0.094 Uiso 1 1 calc R . . H18B H -0.6692 -0.2414 0.5493 0.094 Uiso 1 1 calc R . . H18C H -0.5985 -0.2484 0.4980 0.094 Uiso 1 1 calc R . . C19 C -0.4975(2) -0.4023(2) 0.56214(13) 0.0544(7) Uani 1 1 d . . . H19A H -0.5672 -0.4339 0.5746 0.082 Uiso 1 1 calc R . . H19B H -0.4320 -0.4332 0.5833 0.082 Uiso 1 1 calc R . . H19C H -0.4923 -0.4226 0.5249 0.082 Uiso 1 1 calc R . . C20 C -0.5102(2) -0.2429(3) 0.62599(11) 0.0485(6) Uani 1 1 d . . . H20A H -0.5051 -0.1603 0.6306 0.073 Uiso 1 1 calc R . . H20B H -0.4491 -0.2796 0.6480 0.073 Uiso 1 1 calc R . . H20C H -0.5835 -0.2697 0.6366 0.073 Uiso 1 1 calc R . . N3 N -0.2611(3) 0.5226(3) 0.32441(12) 0.0738(8) Uani 1 1 d . . . N4 N -0.0835(3) 0.4027(3) 0.59276(11) 0.0708(8) Uani 1 1 d . . . C31 C -0.2229(3) 0.4213(3) 0.33984(13) 0.0644(8) Uani 1 1 d . . . H31 H -0.2213 0.3632 0.3139 0.077 Uiso 1 1 calc R . . C32 C -0.1851(2) 0.3944(3) 0.39112(12) 0.0562(7) Uani 1 1 d . . . H32 H -0.1589 0.3197 0.3994 0.067 Uiso 1 1 calc R . . C33 C -0.1852(2) 0.4767(2) 0.43122(12) 0.0508(6) Uani 1 1 d . . . C34 C -0.2246(3) 0.5810(3) 0.41427(14) 0.0653(8) Uani 1 1 d . . . H34 H -0.2262 0.6412 0.4392 0.078 Uiso 1 1 calc R . . C35 C -0.2618(3) 0.6012(3) 0.36266(15) 0.0782(10) Uani 1 1 d . . . H35 H -0.2896 0.6750 0.3535 0.094 Uiso 1 1 calc R . . C36 C -0.1495(2) 0.4503(2) 0.48585(12) 0.0522(7) Uani 1 1 d . . . C37 C -0.0843(2) 0.3520(2) 0.50083(12) 0.0508(6) Uani 1 1 d . . . H37 H -0.0614 0.2998 0.4751 0.061 Uiso 1 1 calc R . . C38 C -0.0559(3) 0.3356(3) 0.55308(14) 0.0674(9) Uani 1 1 d . . . H38 H -0.0121 0.2700 0.5625 0.081 Uiso 1 1 calc R . . C39 C -0.1454(3) 0.4944(3) 0.57703(15) 0.0681(9) Uani 1 1 d . . . H39 H -0.1667 0.5453 0.6036 0.082 Uiso 1 1 calc R . . C40 C -0.1791(2) 0.5193(3) 0.52650(14) 0.0603(8) Uani 1 1 d . . . H40 H -0.2238 0.5851 0.5188 0.072 Uiso 1 1 calc R . . N1 N 0.22504(14) 0.02534(14) 0.38004(7) 0.0297(3) Uani 1 1 d . . . N2 N 0.46391(18) -0.46971(17) 0.27284(8) 0.0413(4) Uani 1 1 d . . . C21 C 0.27126(18) 0.02847(17) 0.33353(8) 0.0323(4) Uani 1 1 d . . . H21 H 0.2697 0.0984 0.3148 0.039 Uiso 1 1 calc R . . C22 C 0.32110(17) -0.06417(17) 0.31124(8) 0.0309(4) Uani 1 1 d . . . H22 H 0.3532 -0.0573 0.2782 0.037 Uiso 1 1 calc R . . C23 C 0.32369(16) -0.16789(16) 0.33789(8) 0.0264(4) Uani 1 1 d . . . C24 C 0.27635(19) -0.17114(17) 0.38660(8) 0.0324(4) Uani 1 1 d . . . H24 H 0.2768 -0.2398 0.4064 0.039 Uiso 1 1 calc R . . C25 C 0.22872(19) -0.07366(18) 0.40588(8) 0.0334(4) Uani 1 1 d . . . H25 H 0.1970 -0.0773 0.4392 0.040 Uiso 1 1 calc R . . C26 C 0.37228(17) -0.27147(17) 0.31498(8) 0.0286(4) Uani 1 1 d . . . C27 C 0.45944(19) -0.2659(2) 0.28126(9) 0.0374(5) Uani 1 1 d . . . H27 H 0.4892 -0.1946 0.2715 0.045 Uiso 1 1 calc R . . C28 C 0.5021(2) -0.3660(2) 0.26216(10) 0.0441(5) Uani 1 1 d . . . H28 H 0.5629 -0.3606 0.2399 0.053 Uiso 1 1 calc R . . C29 C 0.3788(2) -0.47389(19) 0.30400(9) 0.0409(5) Uani 1 1 d . . . H29 H 0.3490 -0.5464 0.3119 0.049 Uiso 1 1 calc R . . C30 C 0.3306(2) -0.37890(19) 0.32568(9) 0.0375(5) Uani 1 1 d . . . H30 H 0.2696 -0.3871 0.3476 0.045 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02182(13) 0.02749(13) 0.02303(13) 0.00239(8) 0.00049(8) -0.00197(8) O1 0.0307(7) 0.0319(7) 0.0286(7) 0.0066(6) -0.0019(6) -0.0044(6) O2 0.0232(6) 0.0395(8) 0.0228(6) 0.0013(6) -0.0004(5) -0.0040(5) O3 0.0228(6) 0.0374(7) 0.0250(7) 0.0029(6) -0.0007(5) -0.0037(5) O4 0.0258(6) 0.0309(7) 0.0305(7) 0.0036(6) 0.0002(5) -0.0047(5) C1 0.0620(18) 0.079(2) 0.0475(15) 0.0199(15) 0.0174(13) 0.0034(16) C2 0.0672(17) 0.0677(18) 0.0306(12) 0.0164(12) -0.0082(11) -0.0242(14) C3 0.079(2) 0.0428(14) 0.0593(17) 0.0186(13) 0.0036(15) -0.0020(14) C4 0.0486(13) 0.0406(12) 0.0319(11) 0.0134(9) -0.0060(9) -0.0118(10) C5 0.0347(10) 0.0247(9) 0.0275(9) 0.0046(7) -0.0019(8) -0.0005(8) C6 0.0358(10) 0.0303(10) 0.0281(10) 0.0040(8) -0.0061(8) -0.0045(8) C7 0.0251(8) 0.0227(8) 0.0248(9) -0.0017(7) 0.0002(7) 0.0017(7) C8 0.0250(8) 0.0249(9) 0.0243(9) -0.0027(7) 0.0010(7) 0.0006(7) C9 0.0312(9) 0.0330(10) 0.0232(9) 0.0008(7) -0.0010(7) 0.0000(8) C10 0.0294(10) 0.0408(11) 0.0278(10) 0.0000(8) -0.0081(8) -0.0040(8) C11 0.0265(9) 0.0353(10) 0.0314(10) 0.0002(8) -0.0032(8) -0.0063(8) C12 0.0252(9) 0.0281(9) 0.0256(9) -0.0008(7) -0.0004(7) -0.0008(7) C13 0.0242(8) 0.0290(9) 0.0244(9) -0.0029(7) -0.0021(7) 0.0003(7) C14 0.0272(9) 0.0273(9) 0.0256(9) -0.0012(7) -0.0007(7) -0.0032(7) C15 0.0242(9) 0.0398(11) 0.0324(10) 0.0044(8) -0.0025(8) -0.0041(8) C16 0.0252(9) 0.0282(9) 0.0320(10) -0.0001(8) 0.0018(7) -0.0042(7) C17 0.0259(9) 0.0414(11) 0.0398(11) 0.0048(9) 0.0026(8) -0.0066(8) C18 0.0255(11) 0.092(2) 0.0698(19) 0.0293(17) -0.0021(11) -0.0110(13) C19 0.0491(14) 0.0454(14) 0.0704(18) -0.0117(13) 0.0147(13) -0.0217(12) C20 0.0376(12) 0.0589(16) 0.0508(14) -0.0041(12) 0.0162(11) -0.0002(11) N3 0.0716(18) 0.084(2) 0.0651(17) -0.0154(15) 0.0030(14) 0.0175(15) N4 0.086(2) 0.0653(17) 0.0630(16) -0.0018(13) 0.0189(14) -0.0247(15) C31 0.0595(17) 0.071(2) 0.0629(19) -0.0198(16) 0.0087(14) 0.0067(15) C32 0.0533(15) 0.0581(17) 0.0591(17) -0.0152(13) 0.0160(13) -0.0008(13) C33 0.0312(11) 0.0499(15) 0.0734(18) -0.0131(13) 0.0176(11) -0.0051(10) C34 0.0687(19) 0.0632(19) 0.0641(19) -0.0131(15) 0.0054(15) 0.0016(15) C35 0.091(3) 0.074(2) 0.069(2) -0.0114(18) 0.0050(19) 0.025(2) C36 0.0383(12) 0.0542(15) 0.0661(17) -0.0158(13) 0.0173(12) -0.0180(11) C37 0.0390(12) 0.0535(15) 0.0617(17) -0.0141(13) 0.0153(11) -0.0093(11) C38 0.068(2) 0.070(2) 0.066(2) -0.0003(16) 0.0122(16) -0.0246(16) C39 0.086(2) 0.0482(17) 0.074(2) -0.0041(15) 0.0286(18) -0.0194(16) C40 0.0554(16) 0.0472(15) 0.083(2) -0.0260(15) 0.0336(15) -0.0177(12) N1 0.0308(8) 0.0264(8) 0.0324(9) -0.0004(7) 0.0061(7) -0.0027(6) N2 0.0503(11) 0.0394(10) 0.0331(10) -0.0085(8) -0.0033(8) 0.0124(9) C21 0.0374(11) 0.0270(9) 0.0333(10) 0.0036(8) 0.0081(8) -0.0027(8) C22 0.0344(10) 0.0317(10) 0.0278(9) -0.0003(8) 0.0095(8) -0.0053(8) C23 0.0250(9) 0.0271(9) 0.0269(9) -0.0014(7) 0.0010(7) -0.0026(7) C24 0.0426(11) 0.0273(10) 0.0276(10) 0.0037(7) 0.0052(8) -0.0004(8) C25 0.0422(11) 0.0314(10) 0.0279(10) 0.0005(8) 0.0107(8) -0.0002(9) C26 0.0307(9) 0.0296(9) 0.0248(9) -0.0024(7) -0.0026(7) 0.0011(8) C27 0.0382(11) 0.0374(11) 0.0373(11) -0.0076(9) 0.0074(9) -0.0041(9) C28 0.0439(12) 0.0493(14) 0.0400(12) -0.0106(10) 0.0090(10) 0.0060(10) C29 0.0524(14) 0.0299(11) 0.0396(12) -0.0004(9) -0.0008(10) 0.0034(9) C30 0.0446(12) 0.0305(10) 0.0381(11) 0.0010(9) 0.0084(9) 0.0003(9) _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 O2 1.9236(13) . ? Cu1 O1 1.9282(14) . ? Cu1 O4 1.9316(13) 3_556 ? Cu1 O3 1.9331(14) 3_556 ? Cu1 N1 2.3082(17) . ? O1 C5 1.267(2) . ? O2 C7 1.274(2) . ? O3 C14 1.273(2) . ? O3 Cu1 1.9331(13) 3_556 ? O4 C16 1.272(2) . ? O4 Cu1 1.9316(13) 3_556 ? C1 C4 1.568(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C4 1.505(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.503(4) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.541(3) . ? C5 C6 1.401(3) . ? C6 C7 1.397(3) . ? C6 H6 0.9500 . ? C7 C8 1.503(3) . ? C8 C13 1.396(3) . ? C8 C9 1.396(3) . ? C9 C10 1.384(3) . ? C9 H9 0.9500 . ? C10 C11 1.385(3) . ? C10 H10 0.9500 . ? C11 C12 1.400(3) . ? C11 H11 0.9500 . ? C12 C13 1.394(3) . ? C12 C14 1.494(3) . ? C13 H13 0.9500 . ? C14 C15 1.406(3) . ? C15 C16 1.401(3) . ? C15 H15 0.9500 . ? C16 C17 1.534(3) . ? C17 C18 1.525(3) . ? C17 C19 1.530(4) . ? C17 C20 1.535(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? N3 C31 1.323(5) . ? N3 C35 1.341(4) . ? N4 C38 1.338(4) . ? N4 C39 1.347(5) . ? C31 C32 1.379(4) . ? C31 H31 0.9500 . ? C32 C33 1.404(4) . ? C32 H32 0.9500 . ? C33 C34 1.370(4) . ? C33 C36 1.451(4) . ? C34 C35 1.369(5) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C40 1.378(4) . ? C36 C37 1.426(4) . ? C37 C38 1.355(5) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C40 1.345(5) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? N1 C25 1.335(3) . ? N1 C21 1.337(3) . ? N2 C29 1.328(3) . ? N2 C28 1.336(3) . ? C21 C22 1.380(3) . ? C21 H21 0.9500 . ? C22 C23 1.394(3) . ? C22 H22 0.9500 . ? C23 C24 1.395(3) . ? C23 C26 1.484(3) . ? C24 C25 1.383(3) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.391(3) . ? C26 C30 1.391(3) . ? C27 C28 1.383(3) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.387(3) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? 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 O2 Cu1 O1 92.34(6) . . ? O2 Cu1 O4 174.71(6) . 3_556 ? O1 Cu1 O4 86.83(6) . 3_556 ? O2 Cu1 O3 87.61(6) . 3_556 ? O1 Cu1 O3 167.60(6) . 3_556 ? O4 Cu1 O3 92.08(6) 3_556 3_556 ? O2 Cu1 N1 94.68(6) . . ? O1 Cu1 N1 95.94(6) . . ? O4 Cu1 N1 90.61(6) 3_556 . ? O3 Cu1 N1 96.42(6) 3_556 . ? C5 O1 Cu1 125.63(13) . . ? C7 O2 Cu1 124.39(12) . . ? C14 O3 Cu1 123.50(12) . 3_556 ? C16 O4 Cu1 123.76(13) . 3_556 ? C4 C1 H1A 109.5 . . ? C4 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C2 H2A 109.5 . . ? C4 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C3 C4 C2 112.3(2) . . ? C3 C4 C5 108.0(2) . . ? C2 C4 C5 113.68(19) . . ? C3 C4 C1 108.1(2) . . ? C2 C4 C1 106.7(2) . . ? C5 C4 C1 108.0(2) . . ? O1 C5 C6 124.17(18) . . ? O1 C5 C4 113.96(18) . . ? C6 C5 C4 121.87(18) . . ? C7 C6 C5 124.52(18) . . ? C7 C6 H6 117.7 . . ? C5 C6 H6 117.7 . . ? O2 C7 C6 124.81(18) . . ? O2 C7 C8 114.64(16) . . ? C6 C7 C8 120.55(17) . . ? C13 C8 C9 118.53(17) . . ? C13 C8 C7 118.18(16) . . ? C9 C8 C7 123.28(17) . . ? C10 C9 C8 120.59(18) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 120.50(18) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C10 C11 C12 120.09(18) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C13 C12 C11 118.87(18) . . ? C13 C12 C14 118.63(17) . . ? C11 C12 C14 122.50(17) . . ? C12 C13 C8 121.38(17) . . ? C12 C13 H13 119.3 . . ? C8 C13 H13 119.3 . . ? O3 C14 C15 125.19(18) . . ? O3 C14 C12 115.44(16) . . ? C15 C14 C12 119.36(17) . . ? C16 C15 C14 124.01(19) . . ? C16 C15 H15 118.0 . . ? C14 C15 H15 118.0 . . ? O4 C16 C15 124.22(18) . . ? O4 C16 C17 114.57(17) . . ? C15 C16 C17 121.18(18) . . ? C18 C17 C19 111.4(2) . . ? C18 C17 C16 113.53(19) . . ? C19 C17 C16 106.50(19) . . ? C18 C17 C20 108.7(2) . . ? C19 C17 C20 108.6(2) . . ? C16 C17 C20 107.93(18) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C31 N3 C35 115.4(3) . . ? C38 N4 C39 114.1(3) . . ? N3 C31 C32 124.4(3) . . ? N3 C31 H31 117.8 . . ? C32 C31 H31 117.8 . . ? C31 C32 C33 120.4(3) . . ? C31 C32 H32 119.8 . . ? C33 C32 H32 119.8 . . ? C34 C33 C32 114.1(3) . . ? C34 C33 C36 124.0(3) . . ? C32 C33 C36 121.8(3) . . ? C33 C34 C35 122.2(3) . . ? C33 C34 H34 118.9 . . ? C35 C34 H34 118.9 . . ? N3 C35 C34 123.5(4) . . ? N3 C35 H35 118.3 . . ? C34 C35 H35 118.3 . . ? C40 C36 C37 116.2(3) . . ? C40 C36 C33 121.0(3) . . ? C37 C36 C33 122.8(2) . . ? C38 C37 C36 117.7(3) . . ? C38 C37 H37 121.1 . . ? C36 C37 H37 121.1 . . ? N4 C38 C37 126.4(4) . . ? N4 C38 H38 116.8 . . ? C37 C38 H38 116.8 . . ? C40 C39 N4 124.9(3) . . ? C40 C39 H39 117.6 . . ? N4 C39 H39 117.6 . . ? C39 C40 C36 120.7(3) . . ? C39 C40 H40 119.7 . . ? C36 C40 H40 119.7 . . ? C25 N1 C21 117.14(18) . . ? C25 N1 Cu1 123.85(13) . . ? C21 N1 Cu1 118.93(13) . . ? C29 N2 C28 116.0(2) . . ? N1 C21 C22 123.72(19) . . ? N1 C21 H21 118.1 . . ? C22 C21 H21 118.1 . . ? C21 C22 C23 119.16(18) . . ? C21 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? C22 C23 C24 117.22(18) . . ? C22 C23 C26 121.61(17) . . ? C24 C23 C26 121.16(17) . . ? C25 C24 C23 119.47(18) . . ? C25 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? N1 C25 C24 123.28(19) . . ? N1 C25 H25 118.4 . . ? C24 C25 H25 118.4 . . ? C27 C26 C30 117.0(2) . . ? C27 C26 C23 121.98(19) . . ? C30 C26 C23 121.04(18) . . ? C28 C27 C26 118.9(2) . . ? C28 C27 H27 120.6 . . ? C26 C27 H27 120.6 . . ? N2 C28 C27 124.6(2) . . ? N2 C28 H28 117.7 . . ? C27 C28 H28 117.7 . . ? N2 C29 C30 124.0(2) . . ? N2 C29 H29 118.0 . . ? C30 C29 H29 118.0 . . ? C29 C30 C26 119.5(2) . . ? C29 C30 H30 120.3 . . ? C26 C30 H30 120.3 . . ? 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 O2 Cu1 O1 C5 -18.12(17) . . . . ? O4 Cu1 O1 C5 167.11(17) 3_556 . . . ? O3 Cu1 O1 C5 -107.6(3) 3_556 . . . ? N1 Cu1 O1 C5 76.83(17) . . . . ? O1 Cu1 O2 C7 21.49(16) . . . . ? O3 Cu1 O2 C7 -170.92(16) 3_556 . . . ? N1 Cu1 O2 C7 -74.66(16) . . . . ? Cu1 O1 C5 C6 8.1(3) . . . . ? Cu1 O1 C5 C4 -171.71(14) . . . . ? C3 C4 C5 O1 -62.0(3) . . . . ? C2 C4 C5 O1 172.7(2) . . . . ? C1 C4 C5 O1 54.6(3) . . . . ? C3 C4 C5 C6 118.2(2) . . . . ? C2 C4 C5 C6 -7.1(3) . . . . ? C1 C4 C5 C6 -125.2(2) . . . . ? O1 C5 C6 C7 6.0(4) . . . . ? C4 C5 C6 C7 -174.1(2) . . . . ? Cu1 O2 C7 C6 -15.4(3) . . . . ? Cu1 O2 C7 C8 165.06(12) . . . . ? C5 C6 C7 O2 -2.0(3) . . . . ? C5 C6 C7 C8 177.48(19) . . . . ? O2 C7 C8 C13 -8.6(2) . . . . ? C6 C7 C8 C13 171.82(18) . . . . ? O2 C7 C8 C9 171.51(18) . . . . ? C6 C7 C8 C9 -8.0(3) . . . . ? C13 C8 C9 C10 -1.0(3) . . . . ? C7 C8 C9 C10 178.87(19) . . . . ? C8 C9 C10 C11 1.0(3) . . . . ? C9 C10 C11 C12 0.3(3) . . . . ? C10 C11 C12 C13 -1.5(3) . . . . ? C10 C11 C12 C14 178.04(19) . . . . ? C11 C12 C13 C8 1.6(3) . . . . ? C14 C12 C13 C8 -178.01(17) . . . . ? C9 C8 C13 C12 -0.3(3) . . . . ? C7 C8 C13 C12 179.81(17) . . . . ? Cu1 O3 C14 C15 -12.1(3) 3_556 . . . ? Cu1 O3 C14 C12 167.04(13) 3_556 . . . ? C13 C12 C14 O3 -22.9(3) . . . . ? C11 C12 C14 O3 157.55(19) . . . . ? C13 C12 C14 C15 156.34(19) . . . . ? C11 C12 C14 C15 -23.2(3) . . . . ? O3 C14 C15 C16 -7.3(3) . . . . ? C12 C14 C15 C16 173.58(19) . . . . ? Cu1 O4 C16 C15 18.8(3) 3_556 . . . ? Cu1 O4 C16 C17 -163.35(14) 3_556 . . . ? C14 C15 C16 O4 3.6(4) . . . . ? C14 C15 C16 C17 -174.1(2) . . . . ? O4 C16 C17 C18 170.8(2) . . . . ? C15 C16 C17 C18 -11.2(3) . . . . ? O4 C16 C17 C19 -66.2(2) . . . . ? C15 C16 C17 C19 111.8(2) . . . . ? O4 C16 C17 C20 50.3(3) . . . . ? C15 C16 C17 C20 -131.8(2) . . . . ? C35 N3 C31 C32 -0.2(5) . . . . ? N3 C31 C32 C33 -0.1(5) . . . . ? C31 C32 C33 C34 -0.2(4) . . . . ? C31 C32 C33 C36 178.0(3) . . . . ? C32 C33 C34 C35 0.8(5) . . . . ? C36 C33 C34 C35 -177.3(3) . . . . ? C31 N3 C35 C34 0.9(6) . . . . ? C33 C34 C35 N3 -1.2(6) . . . . ? C34 C33 C36 C40 16.6(4) . . . . ? C32 C33 C36 C40 -161.4(2) . . . . ? C34 C33 C36 C37 -164.5(3) . . . . ? C32 C33 C36 C37 17.5(4) . . . . ? C40 C36 C37 C38 -0.8(4) . . . . ? C33 C36 C37 C38 -179.8(2) . . . . ? C39 N4 C38 C37 -0.1(5) . . . . ? C36 C37 C38 N4 0.3(5) . . . . ? C38 N4 C39 C40 0.5(5) . . . . ? N4 C39 C40 C36 -1.1(5) . . . . ? C37 C36 C40 C39 1.2(4) . . . . ? C33 C36 C40 C39 -179.8(3) . . . . ? O2 Cu1 N1 C25 -65.03(17) . . . . ? O1 Cu1 N1 C25 -157.88(17) . . . . ? O4 Cu1 N1 C25 115.25(17) 3_556 . . . ? O3 Cu1 N1 C25 23.09(17) 3_556 . . . ? O2 Cu1 N1 C21 118.18(15) . . . . ? O1 Cu1 N1 C21 25.33(16) . . . . ? O4 Cu1 N1 C21 -61.54(16) 3_556 . . . ? O3 Cu1 N1 C21 -153.70(15) 3_556 . . . ? C25 N1 C21 C22 0.4(3) . . . . ? Cu1 N1 C21 C22 177.37(16) . . . . ? N1 C21 C22 C23 0.4(3) . . . . ? C21 C22 C23 C24 -0.9(3) . . . . ? C21 C22 C23 C26 177.70(19) . . . . ? C22 C23 C24 C25 0.6(3) . . . . ? C26 C23 C24 C25 -177.99(19) . . . . ? C21 N1 C25 C24 -0.7(3) . . . . ? Cu1 N1 C25 C24 -177.52(16) . . . . ? C23 C24 C25 N1 0.2(3) . . . . ? C22 C23 C26 C27 29.9(3) . . . . ? C24 C23 C26 C27 -151.5(2) . . . . ? C22 C23 C26 C30 -148.8(2) . . . . ? C24 C23 C26 C30 29.7(3) . . . . ? C30 C26 C27 C28 -2.4(3) . . . . ? C23 C26 C27 C28 178.8(2) . . . . ? C29 N2 C28 C27 0.2(4) . . . . ? C26 C27 C28 N2 1.5(4) . . . . ? C28 N2 C29 C30 -0.8(4) . . . . ? N2 C29 C30 C26 -0.2(4) . . . . ? C27 C26 C30 C29 1.8(3) . . . . ? C23 C26 C30 C29 -179.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.979 _refine_diff_density_min -0.467 _refine_diff_density_rms 0.070 data_lj40sad _database_code_depnum_ccdc_archive 'CCDC 258477' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ;C54 H68 Cu2 N4 O8, 3.25(C4 H8 O) ; _chemical_formula_sum 'C67 H94 Cu2 N4 O11.25' _chemical_formula_weight 1262.54 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 14.900(3) _cell_length_b 15.948(3) _cell_length_c 17.283(3) _cell_angle_alpha 94.774(3) _cell_angle_beta 107.625(3) _cell_angle_gamma 111.025(3) _cell_volume 3567.5(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9707 _cell_measurement_theta_min 2.215 _cell_measurement_theta_max 26.611 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.175 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 0.652 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.668 _exptl_absorpt_correction_T_max 0.949 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 193 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.06 _diffrn_reflns_number 33366 _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_av_sigmaI/netI 0.0750 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 28.32 _reflns_number_total 16053 _reflns_number_gt 10407 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1995)' _computing_cell_refinement 'SAINT (Bruker, 1995)' _computing_data_reduction 'SAINT and XPREP (Bruker, 1995)' _computing_structure_solution 'SIR97 (Altomare, et al. 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEP-3 (Farrugia, 1997) WINGX-32 (Farrugia, 1999) ; _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^)+(0.1392P)^2^+3.5309P] 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 16053 _refine_ls_number_parameters 759 _refine_ls_number_restraints 49 _refine_ls_R_factor_all 0.1239 _refine_ls_R_factor_gt 0.0813 _refine_ls_wR_factor_ref 0.2440 _refine_ls_wR_factor_gt 0.2154 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.054 _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 0.77436(4) 0.61585(3) 0.14579(3) 0.02980(16) Uani 1 1 d . . . N1 N 0.8794(3) 0.6211(3) 0.0766(3) 0.0366(9) Uani 1 1 d . . . N2 N 1.0846(4) 0.6130(3) -0.0431(4) 0.0671(15) Uani 1 1 d . . . O1 O 0.8561(3) 0.7392(2) 0.2112(2) 0.0424(9) Uani 1 1 d . . . O2 O 0.6784(2) 0.65438(19) 0.07000(19) 0.0312(7) Uani 1 1 d . . . O3 O 0.3245(2) 0.51106(19) -0.09929(19) 0.0307(7) Uani 1 1 d . . . O4 O 0.1486(2) 0.4192(2) -0.2403(2) 0.0394(8) Uani 1 1 d . . . C1A C 1.0302(6) 0.8970(9) 0.2800(9) 0.056(3) Uiso 0.45(3) 1 d PD A 1 H1A1 H 1.0832 0.9554 0.3163 0.084 Uiso 0.45(3) 1 calc PR A 1 H1A2 H 1.0403 0.8890 0.2269 0.084 Uiso 0.45(3) 1 calc PR A 1 H1A3 H 1.0352 0.8461 0.3068 0.084 Uiso 0.45(3) 1 calc PR A 1 C2A C 0.9238(12) 0.9849(5) 0.2320(9) 0.056(3) Uiso 0.45(3) 1 d PD A 1 H2A1 H 0.8608 0.9928 0.2294 0.084 Uiso 0.45(3) 1 calc PR A 1 H2A2 H 0.9277 0.9789 0.1763 0.084 Uiso 0.45(3) 1 calc PR A 1 H2A3 H 0.9838 1.0385 0.2696 0.084 Uiso 0.45(3) 1 calc PR A 1 C3A C 0.9049(10) 0.8984(11) 0.3460(5) 0.056(3) Uiso 0.45(3) 1 d PD A 1 H3A1 H 0.8884 0.8369 0.3582 0.084 Uiso 0.45(3) 1 calc PR A 1 H3A2 H 0.8474 0.9162 0.3421 0.084 Uiso 0.45(3) 1 calc PR A 1 H3A3 H 0.9672 0.9427 0.3905 0.084 Uiso 0.45(3) 1 calc PR A 1 C1B C 1.0271(5) 0.9103(8) 0.2619(7) 0.051(3) Uiso 0.55(3) 1 d PD A 2 H1B1 H 1.0802 0.9648 0.3037 0.077 Uiso 0.55(3) 1 calc PR A 2 H1B2 H 1.0284 0.9183 0.2066 0.077 Uiso 0.55(3) 1 calc PR A 2 H1B3 H 1.0404 0.8559 0.2737 0.077 Uiso 0.55(3) 1 calc PR A 2 C2B C 0.8990(9) 0.9816(5) 0.2539(8) 0.051(3) Uiso 0.55(3) 1 d PD A 2 H2B1 H 0.8286 0.9678 0.2518 0.077 Uiso 0.55(3) 1 calc PR A 2 H2B2 H 0.9057 0.9987 0.2020 0.077 Uiso 0.55(3) 1 calc PR A 2 H2B3 H 0.9476 1.0328 0.3009 0.077 Uiso 0.55(3) 1 calc PR A 2 C3B C 0.9181(9) 0.8782(8) 0.3506(4) 0.051(3) Uiso 0.55(3) 1 d PD A 2 H3B1 H 0.9643 0.9337 0.3940 0.077 Uiso 0.55(3) 1 calc PR A 2 H3B2 H 0.9397 0.8279 0.3624 0.077 Uiso 0.55(3) 1 calc PR A 2 H3B3 H 0.8475 0.8607 0.3495 0.077 Uiso 0.55(3) 1 calc PR A 2 C4 C 0.9225(4) 0.8975(3) 0.2645(3) 0.0490(14) Uani 1 1 d D . . C5 C 0.8405(3) 0.8105(3) 0.1986(3) 0.0345(10) Uani 1 1 d D A . C6 C 0.7590(3) 0.8126(3) 0.1354(3) 0.0347(10) Uani 1 1 d . . . H6 H 0.7547 0.8703 0.1320 0.042 Uiso 1 1 calc R A . C7 C 0.6818(3) 0.7348(3) 0.0757(2) 0.0226(8) Uani 1 1 d . A . C8 C 0.5922(3) 0.7444(3) 0.0136(2) 0.0218(8) Uani 1 1 d . . . C9 C 0.5903(3) 0.8298(3) 0.0010(3) 0.0281(9) Uani 1 1 d . A . H9 H 0.6489 0.8849 0.0307 0.034 Uiso 1 1 calc R . . C10 C 0.5038(3) 0.8339(3) -0.0543(3) 0.0298(9) Uani 1 1 d . . . H10 H 0.5028 0.8919 -0.0619 0.036 Uiso 1 1 calc R A . C11 C 0.4176(3) 0.7532(3) -0.0992(3) 0.0283(9) Uani 1 1 d . A . H11 H 0.3584 0.7565 -0.1374 0.034 Uiso 1 1 calc R . . C12 C 0.4183(3) 0.6677(3) -0.0878(2) 0.0239(8) Uani 1 1 d . . . C13 C 0.5063(3) 0.6652(3) -0.0314(2) 0.0217(8) Uani 1 1 d . A . H13 H 0.5072 0.6073 -0.0235 0.026 Uiso 1 1 calc R . . C14 C 0.3289(3) 0.5790(3) -0.1337(3) 0.0249(8) Uani 1 1 d . A . C15 C 0.2590(3) 0.5760(3) -0.2102(3) 0.0319(10) Uani 1 1 d . . . H15 H 0.2701 0.6315 -0.2297 0.038 Uiso 1 1 calc R A . C16 C 0.1741(3) 0.4971(3) -0.2597(2) 0.0334(10) Uani 1 1 d D A . C17 C 0.1035(4) 0.4967(3) -0.3461(3) 0.0487(14) Uani 1 1 d D . . C18A C 0.1248(9) 0.5912(5) -0.3644(6) 0.057(3) Uiso 0.55(2) 1 d PD A 1 H18A H 0.0681 0.5882 -0.4132 0.085 Uiso 0.55(2) 1 calc PR A 1 H18B H 0.1892 0.6139 -0.3754 0.085 Uiso 0.55(2) 1 calc PR A 1 H18C H 0.1310 0.6331 -0.3164 0.085 Uiso 0.55(2) 1 calc PR A 1 C19A C -0.0094(5) 0.4478(8) -0.3527(6) 0.057(3) Uiso 0.55(2) 1 d PD A 1 H19A H -0.0552 0.4371 -0.4103 0.085 Uiso 0.55(2) 1 calc PR A 1 H19B H -0.0248 0.4864 -0.3160 0.085 Uiso 0.55(2) 1 calc PR A 1 H19C H -0.0199 0.3887 -0.3361 0.085 Uiso 0.55(2) 1 calc PR A 1 C20A C 0.1218(9) 0.4378(9) -0.4109(5) 0.057(3) Uiso 0.55(2) 1 d PD A 1 H20A H 0.1115 0.3773 -0.3976 0.085 Uiso 0.55(2) 1 calc PR A 1 H20B H 0.1924 0.4687 -0.4095 0.085 Uiso 0.55(2) 1 calc PR A 1 H20C H 0.0731 0.4303 -0.4665 0.085 Uiso 0.55(2) 1 calc PR A 1 C18B C 0.0898(12) 0.5886(7) -0.3446(8) 0.064(3) Uiso 0.45(2) 1 d PD A 2 H18D H 0.0416 0.5863 -0.3987 0.096 Uiso 0.45(2) 1 calc PR A 2 H18E H 0.1565 0.6395 -0.3330 0.096 Uiso 0.45(2) 1 calc PR A 2 H18F H 0.0625 0.5980 -0.3012 0.096 Uiso 0.45(2) 1 calc PR A 2 C19B C -0.0013(7) 0.4191(8) -0.3721(8) 0.064(3) Uiso 0.45(2) 1 d PD A 2 H19D H -0.0352 0.4279 -0.3334 0.096 Uiso 0.45(2) 1 calc PR A 2 H19E H 0.0061 0.3605 -0.3713 0.096 Uiso 0.45(2) 1 calc PR A 2 H19F H -0.0429 0.4185 -0.4284 0.096 Uiso 0.45(2) 1 calc PR A 2 C20B C 0.1549(10) 0.4882(13) -0.4097(6) 0.064(3) Uiso 0.45(2) 1 d PD A 2 H20D H 0.1798 0.4392 -0.4023 0.096 Uiso 0.45(2) 1 calc PR A 2 H20E H 0.2130 0.5466 -0.4012 0.096 Uiso 0.45(2) 1 calc PR A 2 H20F H 0.1047 0.4735 -0.4661 0.096 Uiso 0.45(2) 1 calc PR A 2 C21 C 0.8509(4) 0.6013(3) -0.0064(3) 0.0448(12) Uani 1 1 d . . . H21 H 0.7814 0.5883 -0.0383 0.054 Uiso 1 1 calc R . . C22 C 0.9145(4) 0.5982(4) -0.0490(4) 0.0490(13) Uani 1 1 d . . . H22 H 0.8885 0.5834 -0.1081 0.059 Uiso 1 1 calc R . . C23 C 1.0175(4) 0.6172(3) -0.0049(4) 0.0496(14) Uani 1 1 d . . . C24 C 1.0493(4) 0.6394(4) 0.0830(4) 0.0463(13) Uani 1 1 d . . . H24 H 1.1187 0.6538 0.1165 0.056 Uiso 1 1 calc R . . C25 C 0.9795(4) 0.6402(3) 0.1196(3) 0.0406(11) Uani 1 1 d . . . H25 H 1.0028 0.6550 0.1786 0.049 Uiso 1 1 calc R . . C26 C 1.0493(6) 0.5910(5) -0.1339(5) 0.078(2) Uani 1 1 d . . . H26A H 0.9907 0.5311 -0.1554 0.117 Uiso 1 1 calc R . . H26B H 1.1055 0.5888 -0.1512 0.117 Uiso 1 1 calc R . . H26C H 1.0283 0.6384 -0.1559 0.117 Uiso 1 1 calc R . . C27 C 1.1926(5) 0.6363(5) 0.0047(5) 0.078(2) Uani 1 1 d . . . H27A H 1.2260 0.7012 0.0333 0.116 Uiso 1 1 calc R . . H27B H 1.2270 0.6255 -0.0329 0.116 Uiso 1 1 calc R . . H27C H 1.1975 0.5977 0.0457 0.116 Uiso 1 1 calc R . . Cu2 Cu 0.55100(4) -0.00084(4) 0.22375(3) 0.02859(16) Uani 1 1 d . . . N3 N 0.5502(3) -0.1428(3) 0.2152(2) 0.0341(8) Uani 1 1 d . . . N4 N 0.5372(4) -0.4093(3) 0.2208(3) 0.0511(11) Uani 1 1 d . . . O5 O 0.6689(2) 0.0587(2) 0.32559(18) 0.0360(7) Uani 1 1 d . . . O6 O 0.6324(2) 0.0474(2) 0.15697(18) 0.0314(7) Uani 1 1 d . . . O7 O 0.5700(2) 0.0318(2) -0.12574(18) 0.0301(7) Uani 1 1 d . . . O8 O 0.5315(2) 0.0291(2) -0.29351(19) 0.0357(7) Uani 1 1 d . . . C28 C 0.8293(4) 0.0649(4) 0.4639(3) 0.0495(13) Uani 1 1 d . . . H28A H 0.7573 0.0269 0.4549 0.074 Uiso 1 1 calc R . . H28B H 0.8689 0.0864 0.5237 0.074 Uiso 1 1 calc R . . H28C H 0.8580 0.0282 0.4388 0.074 Uiso 1 1 calc R . . C29 C 0.8000(5) 0.2081(4) 0.4692(3) 0.0521(14) Uani 1 1 d . . . H29A H 0.8054 0.2627 0.4456 0.078 Uiso 1 1 calc R . . H29B H 0.8434 0.2271 0.5283 0.078 Uiso 1 1 calc R . . H29C H 0.7282 0.1733 0.4633 0.078 Uiso 1 1 calc R . . C30 C 0.9471(4) 0.2028(4) 0.4315(3) 0.0524(14) Uani 1 1 d . . . H30A H 0.9682 0.1654 0.3987 0.079 Uiso 1 1 calc R . . H30B H 0.9920 0.2189 0.4900 0.079 Uiso 1 1 calc R . . H30C H 0.9525 0.2591 0.4108 0.079 Uiso 1 1 calc R . . C31 C 0.8353(4) 0.1480(3) 0.4234(3) 0.0357(10) Uani 1 1 d . . . C32 C 0.7595(3) 0.1122(3) 0.3334(3) 0.0299(9) Uani 1 1 d . . . C33 C 0.7913(3) 0.1359(3) 0.2671(3) 0.0316(9) Uani 1 1 d . . . H33 H 0.8597 0.1795 0.2796 0.038 Uiso 1 1 calc R . . C34 C 0.7278(3) 0.0991(3) 0.1827(2) 0.0247(8) Uani 1 1 d . . . C35 C 0.7721(3) 0.1198(3) 0.1158(3) 0.0248(8) Uani 1 1 d . . . C36 C 0.8779(3) 0.1593(3) 0.1315(3) 0.0326(10) Uani 1 1 d . . . H36 H 0.9253 0.1760 0.1870 0.039 Uiso 1 1 calc R . . C37 C 0.9140(3) 0.1742(3) 0.0666(3) 0.0368(10) Uani 1 1 d . . . H37 H 0.9860 0.2019 0.0781 0.044 Uiso 1 1 calc R . . C38 C 0.8464(3) 0.1492(3) -0.0146(3) 0.0322(10) Uani 1 1 d . . . H38 H 0.8721 0.1583 -0.0587 0.039 Uiso 1 1 calc R . . C39 C 0.7396(3) 0.1101(3) -0.0321(3) 0.0256(8) Uani 1 1 d . . . C40 C 0.7046(3) 0.0948(3) 0.0330(3) 0.0240(8) Uani 1 1 d . . . H40 H 0.6326 0.0666 0.0214 0.029 Uiso 1 1 calc R . . C41 C 0.6619(3) 0.0828(3) -0.1188(3) 0.0261(8) Uani 1 1 d . . . C42 C 0.6912(3) 0.1150(3) -0.1840(3) 0.0320(9) Uani 1 1 d . . . H42 H 0.7600 0.1581 -0.1710 0.038 Uiso 1 1 calc R . . C43 C 0.6244(4) 0.0872(3) -0.2678(3) 0.0328(10) Uani 1 1 d . . . C44 C 0.6606(4) 0.1238(4) -0.3377(3) 0.0487(13) Uani 1 1 d . . . C45 C 0.7649(5) 0.2062(5) -0.3054(4) 0.0639(18) Uani 1 1 d . . . H45A H 0.7820 0.2282 -0.3526 0.096 Uiso 1 1 calc R . . H45B H 0.8180 0.1876 -0.2727 0.096 Uiso 1 1 calc R . . H45C H 0.7615 0.2557 -0.2704 0.096 Uiso 1 1 calc R . . C46 C 0.5791(6) 0.1518(6) -0.3924(5) 0.088(3) Uani 1 1 d . . . H46A H 0.5745 0.2022 -0.3596 0.131 Uiso 1 1 calc R . . H46B H 0.5123 0.0990 -0.4134 0.131 Uiso 1 1 calc R . . H46C H 0.5983 0.1721 -0.4392 0.131 Uiso 1 1 calc R . . C47 C 0.6697(7) 0.0441(5) -0.3865(5) 0.098(3) Uani 1 1 d . . . H47A H 0.6901 0.0633 -0.4332 0.147 Uiso 1 1 calc R . . H47B H 0.6031 -0.0090 -0.4077 0.147 Uiso 1 1 calc R . . H47C H 0.7217 0.0270 -0.3497 0.147 Uiso 1 1 calc R . . C48 C 0.4829(4) -0.2154(3) 0.1544(3) 0.0343(10) Uani 1 1 d . . . H48 H 0.4377 -0.2048 0.1080 0.041 Uiso 1 1 calc R . . C49 C 0.4739(4) -0.3043(3) 0.1536(3) 0.0390(11) Uani 1 1 d . . . H49 H 0.4228 -0.3526 0.1083 0.047 Uiso 1 1 calc R . . C50 C 0.5400(4) -0.3236(3) 0.2195(3) 0.0385(11) Uani 1 1 d . . . C51 C 0.6083(4) -0.2484(4) 0.2849(3) 0.0471(13) Uani 1 1 d . . . H51 H 0.6534 -0.2567 0.3329 0.057 Uiso 1 1 calc R . . C52 C 0.6099(4) -0.1618(3) 0.2793(3) 0.0431(12) Uani 1 1 d . . . H52 H 0.6573 -0.1122 0.3248 0.052 Uiso 1 1 calc R . . C53 C 0.4711(6) -0.4840(4) 0.1499(4) 0.0680(18) Uani 1 1 d . . . H53A H 0.3998 -0.4904 0.1361 0.102 Uiso 1 1 calc R . . H53B H 0.4758 -0.5413 0.1631 0.102 Uiso 1 1 calc R . . H53C H 0.4927 -0.4713 0.1024 0.102 Uiso 1 1 calc R . . C54 C 0.6161(6) -0.4234(4) 0.2850(5) 0.0691(19) Uani 1 1 d . . . H54A H 0.6839 -0.3863 0.2835 0.104 Uiso 1 1 calc R . . H54B H 0.6041 -0.4886 0.2752 0.104 Uiso 1 1 calc R . . H54C H 0.6136 -0.4048 0.3395 0.104 Uiso 1 1 calc R . . O1T O 0.8244(6) 0.7931(6) 0.8523(6) 0.142(3) Uani 1 1 d . . . C1T C 0.8119(12) 0.8112(9) 0.9295(9) 0.170(7) Uani 1 1 d . . . H1T H 0.8677 0.8072 0.9759 0.204 Uiso 1 1 calc R . . H2T H 0.7448 0.7671 0.9287 0.204 Uiso 1 1 calc R . . C2T C 0.8166(13) 0.9031(8) 0.9374(11) 0.177(7) Uani 1 1 d . . . H3T H 0.7463 0.9015 0.9198 0.213 Uiso 1 1 calc R . . H4T H 0.8542 0.9370 0.9960 0.213 Uiso 1 1 calc R . . C3T C 0.8676(16) 0.9465(10) 0.8870(11) 0.214(10) Uani 1 1 d . . . H5T H 0.8385 0.9893 0.8627 0.257 Uiso 1 1 calc R . . H6T H 0.9420 0.9816 0.9193 0.257 Uiso 1 1 calc R . . C4T C 0.8527(12) 0.8773(10) 0.8261(8) 0.146(5) Uani 1 1 d . . . H7T H 0.9168 0.8905 0.8142 0.175 Uiso 1 1 calc R . . H8T H 0.7977 0.8731 0.7744 0.175 Uiso 1 1 calc R . . O2T O 0.6757(7) 0.6872(6) 0.4867(6) 0.156(3) Uani 1 1 d . . . C5T C 0.6349(13) 0.7365(14) 0.5265(14) 0.227(10) Uani 1 1 d . . . H9T H 0.6242 0.7121 0.5753 0.272 Uiso 1 1 calc R . . H10T H 0.5682 0.7321 0.4878 0.272 Uiso 1 1 calc R . . C6T C 0.7084(13) 0.8290(10) 0.5517(13) 0.194(8) Uani 1 1 d . . . H11T H 0.6861 0.8658 0.5126 0.233 Uiso 1 1 calc R . . H12T H 0.7155 0.8563 0.6079 0.233 Uiso 1 1 calc R . . C7T C 0.8022(11) 0.8289(9) 0.5520(12) 0.189(8) Uani 1 1 d . . . H13T H 0.8533 0.8489 0.6093 0.226 Uiso 1 1 calc R . . H14T H 0.8299 0.8707 0.5177 0.226 Uiso 1 1 calc R . . C8T C 0.7789(8) 0.7337(10) 0.5166(10) 0.168(7) Uani 1 1 d . . . H15T H 0.8064 0.7315 0.4713 0.202 Uiso 1 1 calc R . . H16T H 0.8110 0.7057 0.5599 0.202 Uiso 1 1 calc R . . O3T O 0.5393(13) 0.8124(7) 0.7328(7) 0.348(12) Uani 1 1 d D . . C9T C 0.5370(15) 0.7208(10) 0.7388(9) 0.246(13) Uani 1 1 d D . . H17T H 0.6067 0.7215 0.7511 0.296 Uiso 1 1 calc R . . H18T H 0.5117 0.6993 0.7833 0.296 Uiso 1 1 calc R . . C10T C 0.4670(11) 0.6612(7) 0.6579(11) 0.193(8) Uani 1 1 d D . . H19T H 0.4127 0.6080 0.6653 0.231 Uiso 1 1 calc R . . H20T H 0.5053 0.6377 0.6305 0.231 Uiso 1 1 calc R . . C11T C 0.4199(9) 0.7132(7) 0.6058(9) 0.185(7) Uani 1 1 d D . . H21T H 0.4376 0.7155 0.5550 0.222 Uiso 1 1 calc R . . H22T H 0.3440 0.6850 0.5893 0.222 Uiso 1 1 calc R . . C12T C 0.4630(8) 0.8044(6) 0.6579(7) 0.202(9) Uani 1 1 d D . . H23T H 0.4931 0.8507 0.6279 0.243 Uiso 1 1 calc R . . H24T H 0.4076 0.8170 0.6699 0.243 Uiso 1 1 calc R . . O4T O 0.7828(8) 0.5253(6) -0.2645(7) 0.108(5) Uiso 0.25 1 d PRD . . C13T C 0.7097(8) 0.4329(6) -0.2856(7) 0.108(5) Uiso 0.25 1 d PRD . . H13A H 0.6866 0.4191 -0.2383 0.130 Uiso 0.25 1 calc PR . . H13B H 0.7432 0.3914 -0.2949 0.130 Uiso 0.25 1 calc PR . . C14T C 0.6200(8) 0.4141(6) -0.3599(7) 0.108(5) Uiso 0.25 1 d PRD . . H14A H 0.6268 0.3856 -0.4097 0.130 Uiso 0.25 1 calc PR . . H14B H 0.5559 0.3730 -0.3535 0.130 Uiso 0.25 1 calc PR . . C15T C 0.6204(8) 0.5001(6) -0.3654(7) 0.108(5) Uiso 0.25 1 d PRD . . H15A H 0.5559 0.5035 -0.3636 0.130 Uiso 0.25 1 calc PR . . H15B H 0.6314 0.5182 -0.4163 0.130 Uiso 0.25 1 calc PR . . C16T C 0.7083(8) 0.5559(6) -0.2906(7) 0.108(5) Uiso 0.25 1 d PRD . . H16A H 0.7395 0.6183 -0.3005 0.130 Uiso 0.25 1 calc PR . . H16B H 0.6824 0.5620 -0.2449 0.130 Uiso 0.25 1 calc PR . . 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 0.0231(3) 0.0171(2) 0.0376(3) 0.0046(2) -0.0030(2) 0.0071(2) N1 0.0269(19) 0.0276(19) 0.043(2) 0.0045(16) 0.0040(17) 0.0048(15) N2 0.066(4) 0.045(3) 0.097(4) 0.007(3) 0.050(3) 0.015(3) O1 0.0346(18) 0.0214(15) 0.050(2) 0.0007(14) -0.0119(15) 0.0120(13) O2 0.0246(15) 0.0181(13) 0.0385(17) 0.0035(12) -0.0037(13) 0.0079(12) O3 0.0253(15) 0.0198(14) 0.0366(17) 0.0078(12) -0.0020(13) 0.0081(12) O4 0.0315(17) 0.0239(15) 0.0416(18) 0.0065(13) -0.0102(14) 0.0070(13) C4 0.042(3) 0.025(2) 0.058(3) -0.004(2) -0.011(2) 0.015(2) C5 0.029(2) 0.022(2) 0.041(3) 0.0031(18) -0.0014(19) 0.0090(17) C6 0.032(2) 0.0172(19) 0.043(3) 0.0040(18) -0.001(2) 0.0096(17) C7 0.0189(19) 0.0220(19) 0.028(2) 0.0081(15) 0.0071(16) 0.0096(15) C8 0.0215(19) 0.0189(18) 0.025(2) 0.0064(15) 0.0059(16) 0.0099(15) C9 0.026(2) 0.0183(18) 0.037(2) 0.0071(16) 0.0086(18) 0.0070(16) C10 0.031(2) 0.0184(19) 0.037(2) 0.0077(17) 0.0065(19) 0.0112(17) C11 0.024(2) 0.0218(19) 0.035(2) 0.0080(17) 0.0028(17) 0.0104(16) C12 0.024(2) 0.0209(18) 0.025(2) 0.0040(15) 0.0042(16) 0.0101(16) C13 0.0229(19) 0.0178(17) 0.024(2) 0.0050(15) 0.0062(16) 0.0097(15) C14 0.024(2) 0.0191(18) 0.033(2) 0.0070(16) 0.0083(17) 0.0111(16) C15 0.033(2) 0.024(2) 0.032(2) 0.0079(17) 0.0013(18) 0.0106(18) C16 0.033(2) 0.027(2) 0.033(2) 0.0047(18) -0.0008(19) 0.0154(19) C17 0.052(3) 0.036(3) 0.034(3) 0.006(2) -0.013(2) 0.014(2) C21 0.033(3) 0.034(2) 0.054(3) 0.008(2) 0.006(2) 0.007(2) C22 0.050(3) 0.038(3) 0.046(3) 0.003(2) 0.011(3) 0.010(2) C23 0.050(3) 0.023(2) 0.076(4) 0.008(2) 0.032(3) 0.008(2) C24 0.029(2) 0.038(3) 0.068(4) 0.012(2) 0.015(2) 0.011(2) C25 0.027(2) 0.032(2) 0.051(3) 0.006(2) 0.006(2) 0.0073(19) C26 0.105(6) 0.053(4) 0.088(5) 0.004(4) 0.061(5) 0.027(4) C27 0.058(4) 0.049(4) 0.142(7) 0.016(4) 0.057(5) 0.023(3) Cu2 0.0247(3) 0.0307(3) 0.0252(3) 0.0070(2) 0.0065(2) 0.0073(2) N3 0.036(2) 0.034(2) 0.031(2) 0.0056(16) 0.0116(17) 0.0141(17) N4 0.058(3) 0.035(2) 0.060(3) 0.003(2) 0.018(2) 0.024(2) O5 0.0306(17) 0.0420(18) 0.0265(16) 0.0063(13) 0.0062(13) 0.0081(14) O6 0.0231(15) 0.0375(17) 0.0251(15) 0.0081(13) 0.0061(12) 0.0047(13) O7 0.0241(15) 0.0330(16) 0.0274(15) 0.0116(12) 0.0073(12) 0.0055(12) O8 0.0346(17) 0.0383(17) 0.0287(16) 0.0036(13) 0.0131(14) 0.0079(14) C28 0.050(3) 0.046(3) 0.038(3) 0.011(2) 0.001(2) 0.017(3) C29 0.065(4) 0.045(3) 0.037(3) -0.001(2) 0.017(3) 0.015(3) C30 0.035(3) 0.062(4) 0.029(3) 0.000(2) -0.004(2) 0.001(3) C31 0.030(2) 0.033(2) 0.026(2) 0.0005(18) -0.0009(18) 0.0028(19) C32 0.030(2) 0.029(2) 0.026(2) 0.0008(17) 0.0038(18) 0.0126(18) C33 0.024(2) 0.029(2) 0.030(2) 0.0031(17) 0.0043(18) 0.0037(17) C34 0.024(2) 0.0216(18) 0.026(2) 0.0058(16) 0.0054(16) 0.0097(16) C35 0.023(2) 0.0185(18) 0.030(2) 0.0062(15) 0.0071(17) 0.0075(15) C36 0.022(2) 0.030(2) 0.036(2) 0.0096(18) 0.0013(18) 0.0066(17) C37 0.023(2) 0.040(3) 0.043(3) 0.015(2) 0.010(2) 0.0079(19) C38 0.025(2) 0.033(2) 0.042(3) 0.0138(19) 0.0153(19) 0.0105(18) C39 0.023(2) 0.0217(19) 0.032(2) 0.0075(16) 0.0079(17) 0.0098(16) C40 0.0199(19) 0.0193(18) 0.032(2) 0.0068(16) 0.0083(16) 0.0077(15) C41 0.027(2) 0.0218(19) 0.030(2) 0.0067(16) 0.0098(17) 0.0102(16) C42 0.027(2) 0.031(2) 0.037(2) 0.0070(18) 0.0150(19) 0.0078(18) C43 0.032(2) 0.035(2) 0.033(2) 0.0057(19) 0.0145(19) 0.0132(19) C44 0.044(3) 0.060(3) 0.035(3) 0.008(2) 0.018(2) 0.010(3) C45 0.055(4) 0.075(4) 0.050(3) 0.025(3) 0.031(3) 0.002(3) C46 0.062(4) 0.124(7) 0.066(5) 0.061(5) 0.016(4) 0.022(4) C47 0.121(7) 0.074(5) 0.085(5) -0.016(4) 0.078(5) -0.002(5) C48 0.035(2) 0.039(2) 0.029(2) 0.0053(19) 0.0127(19) 0.014(2) C49 0.038(3) 0.037(3) 0.036(3) -0.004(2) 0.012(2) 0.013(2) C50 0.039(3) 0.034(2) 0.045(3) 0.004(2) 0.022(2) 0.013(2) C51 0.044(3) 0.039(3) 0.049(3) 0.005(2) 0.003(2) 0.018(2) C52 0.042(3) 0.032(2) 0.043(3) 0.003(2) 0.002(2) 0.014(2) C53 0.090(5) 0.037(3) 0.077(4) 0.000(3) 0.031(4) 0.028(3) C54 0.080(5) 0.049(3) 0.095(5) 0.023(3) 0.032(4) 0.041(3) O1T 0.137(7) 0.115(6) 0.196(8) 0.014(6) 0.100(6) 0.043(5) C1T 0.251(15) 0.187(13) 0.270(16) 0.156(12) 0.237(15) 0.167(12) C2T 0.253(17) 0.089(8) 0.283(18) 0.068(10) 0.210(16) 0.070(10) C3T 0.40(3) 0.135(12) 0.262(19) 0.105(13) 0.27(2) 0.144(15) C4T 0.198(14) 0.155(12) 0.136(10) 0.065(9) 0.119(11) 0.072(11) O2T 0.110(6) 0.141(7) 0.163(8) -0.017(6) 0.032(6) 0.016(6) C5T 0.171(15) 0.194(18) 0.39(3) 0.035(18) 0.208(19) 0.070(14) C6T 0.165(14) 0.113(11) 0.34(2) 0.002(13) 0.136(16) 0.066(10) C7T 0.125(11) 0.099(9) 0.33(2) -0.022(11) 0.087(13) 0.035(8) C8T 0.064(6) 0.158(12) 0.219(15) -0.070(11) 0.016(8) 0.026(7) O3T 0.74(4) 0.268(16) 0.285(17) 0.197(15) 0.29(2) 0.36(2) C9T 0.52(4) 0.202(17) 0.27(2) 0.170(17) 0.29(3) 0.28(2) C10T 0.248(18) 0.057(6) 0.35(3) 0.069(10) 0.201(19) 0.064(9) C11T 0.102(8) 0.081(7) 0.291(19) -0.044(10) -0.022(10) 0.039(6) C12T 0.160(12) 0.083(8) 0.259(19) -0.038(10) -0.073(12) 0.072(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 O1 1.926(3) . ? Cu1 O2 1.941(3) . ? Cu1 O4 1.944(3) 2_665 ? Cu1 O3 1.946(3) 2_665 ? Cu1 N1 2.224(4) . ? N1 C21 1.341(7) . ? N1 C25 1.354(6) . ? N2 C23 1.370(7) . ? N2 C27 1.459(9) . ? N2 C26 1.462(9) . ? O1 C5 1.263(5) . ? O2 C7 1.260(5) . ? O3 C14 1.270(5) . ? O3 Cu1 1.946(3) 2_665 ? O4 C16 1.268(5) . ? O4 Cu1 1.944(3) 2_665 ? C1A C4 1.548(7) . ? C1A H1A1 0.9800 . ? C1A H1A2 0.9800 . ? C1A H1A3 0.9800 . ? C2A C4 1.541(7) . ? C2A H2A1 0.9800 . ? C2A H2A2 0.9800 . ? C2A H2A3 0.9800 . ? C3A C4 1.509(7) . ? C3A H3A1 0.9800 . ? C3A H3A2 0.9800 . ? C3A H3A3 0.9800 . ? C1B C4 1.513(7) . ? C1B H1B1 0.9800 . ? C1B H1B2 0.9800 . ? C1B H1B3 0.9800 . ? C2B C4 1.514(6) . ? C2B H2B1 0.9800 . ? C2B H2B2 0.9800 . ? C2B H2B3 0.9800 . ? C3B C4 1.561(7) . ? C3B H3B1 0.9800 . ? C3B H3B2 0.9800 . ? C3B H3B3 0.9800 . ? C4 C5 1.547(6) . ? C5 C6 1.379(6) . ? C6 C7 1.403(6) . ? C6 H6 0.9500 . ? C7 C8 1.505(5) . ? C8 C13 1.383(5) . ? C8 C9 1.405(5) . ? C9 C10 1.380(6) . ? C9 H9 0.9500 . ? C10 C11 1.397(6) . ? C10 H10 0.9500 . ? C11 C12 1.397(5) . ? C11 H11 0.9500 . ? C12 C13 1.393(5) . ? C12 C14 1.493(5) . ? C13 H13 0.9500 . ? C14 C15 1.398(6) . ? C15 C16 1.392(6) . ? C15 H15 0.9500 . ? C16 C17 1.543(5) . ? C17 C19B 1.506(7) . ? C17 C18A 1.507(6) . ? C17 C20B 1.540(7) . ? C17 C19A 1.543(7) . ? C17 C20A 1.549(7) . ? C17 C18B 1.551(7) . ? C18A H18A 0.9800 . ? C18A H18B 0.9800 . ? C18A H18C 0.9800 . ? C19A H19A 0.9800 . ? C19A H19B 0.9800 . ? C19A H19C 0.9800 . ? C20A H20A 0.9800 . ? C20A H20B 0.9800 . ? C20A H20C 0.9800 . ? C18B H18D 0.9800 . ? C18B H18E 0.9800 . ? C18B H18F 0.9800 . ? C19B H19D 0.9800 . ? C19B H19E 0.9800 . ? C19B H19F 0.9800 . ? C20B H20D 0.9800 . ? C20B H20E 0.9800 . ? C20B H20F 0.9800 . ? C21 C22 1.375(8) . ? C21 H21 0.9500 . ? C22 C23 1.395(8) . ? C22 H22 0.9500 . ? C23 C24 1.418(8) . ? C24 C25 1.375(7) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? Cu2 O6 1.929(3) . ? Cu2 O7 1.933(3) 2_655 ? Cu2 O5 1.933(3) . ? Cu2 O8 1.939(3) 2_655 ? Cu2 N3 2.252(4) . ? N3 C52 1.329(6) . ? N3 C48 1.332(6) . ? N4 C50 1.355(6) . ? N4 C53 1.440(7) . ? N4 C54 1.451(8) . ? O5 C32 1.270(5) . ? O6 C34 1.270(5) . ? O7 C41 1.279(5) . ? O7 Cu2 1.933(3) 2_655 ? O8 C43 1.269(5) . ? O8 Cu2 1.939(3) 2_655 ? C28 C31 1.536(7) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C31 1.521(7) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.534(7) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.532(6) . ? C32 C33 1.398(6) . ? C33 C34 1.411(6) . ? C33 H33 0.9500 . ? C34 C35 1.500(6) . ? C35 C36 1.398(6) . ? C35 C40 1.401(6) . ? C36 C37 1.386(7) . ? C36 H36 0.9500 . ? C37 C38 1.380(7) . ? C37 H37 0.9500 . ? C38 C39 1.407(6) . ? C38 H38 0.9500 . ? C39 C40 1.382(6) . ? C39 C41 1.501(6) . ? C40 H40 0.9500 . ? C41 C42 1.399(6) . ? C42 C43 1.410(6) . ? C42 H42 0.9500 . ? C43 C44 1.542(7) . ? C44 C46 1.526(9) . ? C44 C45 1.530(8) . ? C44 C47 1.537(9) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C49 1.373(7) . ? C48 H48 0.9500 . ? C49 C50 1.401(7) . ? C49 H49 0.9500 . ? C50 C51 1.397(7) . ? C51 C52 1.385(7) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? O1T C4T 1.414(13) . ? O1T C1T 1.422(13) . ? C1T C2T 1.435(15) . ? C1T H1T 0.9900 . ? C1T H2T 0.9900 . ? C2T C3T 1.393(15) . ? C2T H3T 0.9900 . ? C2T H4T 0.9900 . ? C3T C4T 1.366(17) . ? C3T H5T 0.9900 . ? C3T H6T 0.9900 . ? C4T H7T 0.9900 . ? C4T H8T 0.9900 . ? O2T C8T 1.349(12) . ? O2T C5T 1.402(16) . ? C5T C6T 1.418(19) . ? C5T H9T 0.9900 . ? C5T H10T 0.9900 . ? C6T C7T 1.397(17) . ? C6T H11T 0.9900 . ? C6T H12T 0.9900 . ? C7T C8T 1.463(17) . ? C7T H13T 0.9900 . ? C7T H14T 0.9900 . ? C8T H15T 0.9900 . ? C8T H16T 0.9900 . ? O3T C12T 1.401(9) . ? O3T C9T 1.461(8) . ? C9T C10T 1.460(9) . ? C9T H17T 0.9900 . ? C9T H18T 0.9900 . ? C10T C11T 1.466(9) . ? C10T H19T 0.9900 . ? C10T H20T 0.9900 . ? C11T C12T 1.450(8) . ? C11T H21T 0.9900 . ? C11T H22T 0.9900 . ? C12T H23T 0.9900 . ? C12T H24T 0.9900 . ? O4T C16T 1.3401 . ? O4T C13T 1.4174 . ? C13T C14T 1.4618 . ? C13T H13A 0.9900 . ? C13T H13B 0.9900 . ? C14T C15T 1.3807 . ? C14T H14A 0.9900 . ? C14T H14B 0.9900 . ? C15T C16T 1.4582 . ? C15T H15A 0.9900 . ? C15T H15B 0.9900 . ? C16T H16A 0.9900 . ? C16T H16B 0.9900 . ? 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 O1 Cu1 O2 92.19(12) . . ? O1 Cu1 O4 84.36(13) . 2_665 ? O2 Cu1 O4 165.20(15) . 2_665 ? O1 Cu1 O3 166.13(16) . 2_665 ? O2 Cu1 O3 88.63(12) . 2_665 ? O4 Cu1 O3 91.33(12) 2_665 2_665 ? O1 Cu1 N1 94.44(16) . . ? O2 Cu1 N1 99.99(14) . . ? O4 Cu1 N1 94.64(15) 2_665 . ? O3 Cu1 N1 99.06(14) 2_665 . ? C21 N1 C25 115.5(5) . . ? C21 N1 Cu1 125.3(3) . . ? C25 N1 Cu1 119.1(3) . . ? C23 N2 C27 121.4(6) . . ? C23 N2 C26 119.6(6) . . ? C27 N2 C26 118.8(6) . . ? C5 O1 Cu1 127.0(3) . . ? C7 O2 Cu1 125.8(3) . . ? C14 O3 Cu1 126.4(3) . 2_665 ? C16 O4 Cu1 127.4(3) . 2_665 ? C4 C1A H1A1 109.5 . . ? C4 C1A H1A2 109.5 . . ? C4 C1A H1A3 109.5 . . ? C4 C2A H2A1 109.5 . . ? C4 C2A H2A2 109.5 . . ? C4 C2A H2A3 109.5 . . ? C4 C3A H3A1 109.5 . . ? C4 C3A H3A2 109.5 . . ? C4 C3A H3A3 109.5 . . ? C4 C1B H1B1 109.5 . . ? C4 C1B H1B2 109.5 . . ? H1B1 C1B H1B2 109.5 . . ? C4 C1B H1B3 109.5 . . ? H1B1 C1B H1B3 109.5 . . ? H1B2 C1B H1B3 109.5 . . ? C4 C2B H2B1 109.5 . . ? C4 C2B H2B2 109.5 . . ? H2B1 C2B H2B2 109.5 . . ? C4 C2B H2B3 109.5 . . ? H2B1 C2B H2B3 109.5 . . ? H2B2 C2B H2B3 109.5 . . ? C4 C3B H3B1 109.5 . . ? C4 C3B H3B2 109.5 . . ? H3B1 C3B H3B2 109.5 . . ? C4 C3B H3B3 109.5 . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? C3A C4 C1B 120.2(7) . . ? C3A C4 C2B 91.0(6) . . ? C1B C4 C2B 113.1(5) . . ? C3A C4 C2A 111.7(6) . . ? C1B C4 C2A 94.0(7) . . ? C3A C4 C5 110.9(5) . . ? C1B C4 C5 108.3(5) . . ? C2B C4 C5 112.4(5) . . ? C2A C4 C5 110.4(5) . . ? C3A C4 C1A 107.8(6) . . ? C2B C4 C1A 123.9(7) . . ? C2A C4 C1A 106.9(6) . . ? C5 C4 C1A 108.9(5) . . ? C1B C4 C3B 109.4(5) . . ? C2B C4 C3B 106.9(5) . . ? C2A C4 C3B 126.7(7) . . ? C5 C4 C3B 106.4(5) . . ? C1A C4 C3B 95.6(7) . . ? O1 C5 C6 125.2(4) . . ? O1 C5 C4 112.3(3) . . ? C6 C5 C4 122.5(4) . . ? C5 C6 C7 124.1(4) . . ? C5 C6 H6 117.9 . . ? C7 C6 H6 117.9 . . ? O2 C7 C6 125.6(4) . . ? O2 C7 C8 115.1(3) . . ? C6 C7 C8 119.3(3) . . ? C13 C8 C9 118.5(4) . . ? C13 C8 C7 118.2(3) . . ? C9 C8 C7 123.3(4) . . ? C10 C9 C8 120.4(4) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 120.4(4) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C10 C11 C12 120.0(4) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C13 C12 C11 118.6(4) . . ? C13 C12 C14 118.6(3) . . ? C11 C12 C14 122.8(4) . . ? C8 C13 C12 122.1(3) . . ? C8 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? O3 C14 C15 125.4(4) . . ? O3 C14 C12 115.6(3) . . ? C15 C14 C12 118.9(3) . . ? C16 C15 C14 124.3(4) . . ? C16 C15 H15 117.8 . . ? C14 C15 H15 117.8 . . ? O4 C16 C15 124.5(4) . . ? O4 C16 C17 113.5(3) . . ? C15 C16 C17 122.0(4) . . ? C19B C17 C18A 125.5(7) . . ? C19B C17 C20B 110.3(6) . . ? C18A C17 C20B 82.5(6) . . ? C18A C17 C19A 110.9(5) . . ? C20B C17 C19A 130.1(6) . . ? C19B C17 C16 111.4(5) . . ? C18A C17 C16 113.5(5) . . ? C20B C17 C16 108.8(5) . . ? C19A C17 C16 108.4(5) . . ? C19B C17 C20A 85.3(6) . . ? C18A C17 C20A 109.2(5) . . ? C19A C17 C20A 107.8(5) . . ? C16 C17 C20A 106.7(5) . . ? C19B C17 C18B 108.3(6) . . ? C20B C17 C18B 108.0(6) . . ? C19A C17 C18B 88.8(6) . . ? C16 C17 C18B 110.0(5) . . ? C20A C17 C18B 132.0(6) . . ? C17 C18A H18A 109.5 . . ? C17 C18A H18B 109.5 . . ? C17 C18A H18C 109.5 . . ? C17 C19A H19A 109.5 . . ? C17 C19A H19B 109.5 . . ? C17 C19A H19C 109.5 . . ? C17 C20A H20A 109.5 . . ? C17 C20A H20B 109.5 . . ? C17 C20A H20C 109.5 . . ? C17 C18B H18D 109.5 . . ? C17 C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? C17 C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? C17 C19B H19D 109.5 . . ? C17 C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? C17 C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? C17 C20B H20D 109.5 . . ? C17 C20B H20E 109.5 . . ? H20D C20B H20E 109.5 . . ? C17 C20B H20F 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? N1 C21 C22 125.1(5) . . ? N1 C21 H21 117.4 . . ? C22 C21 H21 117.4 . . ? C21 C22 C23 119.6(5) . . ? C21 C22 H22 120.2 . . ? C23 C22 H22 120.2 . . ? N2 C23 C22 122.8(6) . . ? N2 C23 C24 121.1(6) . . ? C22 C23 C24 116.1(5) . . ? C25 C24 C23 119.8(5) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? N1 C25 C24 123.9(5) . . ? N1 C25 H25 118.1 . . ? C24 C25 H25 118.1 . . ? N2 C26 H26A 109.5 . . ? N2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N2 C27 H27A 109.5 . . ? N2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O6 Cu2 O7 87.63(12) . 2_655 ? O6 Cu2 O5 91.88(13) . . ? O7 Cu2 O5 165.86(14) 2_655 . ? O6 Cu2 O8 170.30(14) . 2_655 ? O7 Cu2 O8 91.50(13) 2_655 2_655 ? O5 Cu2 O8 86.61(13) . 2_655 ? O6 Cu2 N3 100.02(14) . . ? O7 Cu2 N3 96.43(14) 2_655 . ? O5 Cu2 N3 97.57(14) . . ? O8 Cu2 N3 89.67(14) 2_655 . ? C52 N3 C48 114.9(4) . . ? C52 N3 Cu2 119.7(3) . . ? C48 N3 Cu2 124.7(3) . . ? C50 N4 C53 120.7(5) . . ? C50 N4 C54 120.2(5) . . ? C53 N4 C54 117.7(5) . . ? C32 O5 Cu2 127.5(3) . . ? C34 O6 Cu2 127.1(3) . . ? C41 O7 Cu2 125.0(3) . 2_655 ? C43 O8 Cu2 123.7(3) . 2_655 ? C31 C28 H28A 109.5 . . ? C31 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C31 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C31 C29 H29A 109.5 . . ? C31 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C31 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 H30A 109.5 . . ? C31 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C31 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 C32 107.9(4) . . ? C29 C31 C30 109.6(4) . . ? C32 C31 C30 113.8(4) . . ? C29 C31 C28 108.1(4) . . ? C32 C31 C28 108.0(4) . . ? C30 C31 C28 109.2(4) . . ? O5 C32 C33 124.5(4) . . ? O5 C32 C31 114.3(4) . . ? C33 C32 C31 121.2(4) . . ? C32 C33 C34 123.9(4) . . ? C32 C33 H33 118.0 . . ? C34 C33 H33 118.0 . . ? O6 C34 C33 124.8(4) . . ? O6 C34 C35 115.1(3) . . ? C33 C34 C35 120.1(4) . . ? C36 C35 C40 118.1(4) . . ? C36 C35 C34 123.3(4) . . ? C40 C35 C34 118.6(3) . . ? C37 C36 C35 120.5(4) . . ? C37 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? C38 C37 C36 120.7(4) . . ? C38 C37 H37 119.6 . . ? C36 C37 H37 119.6 . . ? C37 C38 C39 120.0(4) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C40 C39 C38 118.6(4) . . ? C40 C39 C41 118.6(4) . . ? C38 C39 C41 122.8(4) . . ? C39 C40 C35 122.0(4) . . ? C39 C40 H40 119.0 . . ? C35 C40 H40 119.0 . . ? O7 C41 C42 124.9(4) . . ? O7 C41 C39 114.6(3) . . ? C42 C41 C39 120.5(4) . . ? C41 C42 C43 123.6(4) . . ? C41 C42 H42 118.2 . . ? C43 C42 H42 118.2 . . ? O8 C43 C42 124.5(4) . . ? O8 C43 C44 113.7(4) . . ? C42 C43 C44 121.8(4) . . ? C46 C44 C45 109.3(6) . . ? C46 C44 C47 111.2(6) . . ? C45 C44 C47 108.9(6) . . ? C46 C44 C43 107.8(5) . . ? C45 C44 C43 113.3(4) . . ? C47 C44 C43 106.4(5) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C44 C47 H47A 109.5 . . ? C44 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C44 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N3 C48 C49 125.1(5) . . ? N3 C48 H48 117.4 . . ? C49 C48 H48 117.4 . . ? C48 C49 C50 119.9(4) . . ? C48 C49 H49 120.1 . . ? C50 C49 H49 120.1 . . ? N4 C50 C51 122.1(5) . . ? N4 C50 C49 122.6(5) . . ? C51 C50 C49 115.3(5) . . ? C52 C51 C50 119.7(5) . . ? C52 C51 H51 120.2 . . ? C50 C51 H51 120.2 . . ? N3 C52 C51 125.0(5) . . ? N3 C52 H52 117.5 . . ? C51 C52 H52 117.5 . . ? N4 C53 H53A 109.5 . . ? N4 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? N4 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N4 C54 H54A 109.5 . . ? N4 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? N4 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C4T O1T C1T 106.9(9) . . ? O1T C1T C2T 104.1(9) . . ? O1T C1T H1T 110.9 . . ? C2T C1T H1T 110.9 . . ? O1T C1T H2T 110.9 . . ? C2T C1T H2T 110.9 . . ? H1T C1T H2T 109.0 . . ? C3T C2T C1T 108.1(11) . . ? C3T C2T H3T 110.1 . . ? C1T C2T H3T 110.1 . . ? C3T C2T H4T 110.1 . . ? C1T C2T H4T 110.1 . . ? H3T C2T H4T 108.4 . . ? C4T C3T C2T 105.3(12) . . ? C4T C3T H5T 110.7 . . ? C2T C3T H5T 110.7 . . ? C4T C3T H6T 110.7 . . ? C2T C3T H6T 110.7 . . ? H5T C3T H6T 108.8 . . ? C3T C4T O1T 109.5(10) . . ? C3T C4T H7T 109.8 . . ? O1T C4T H7T 109.8 . . ? C3T C4T H8T 109.8 . . ? O1T C4T H8T 109.8 . . ? H7T C4T H8T 108.2 . . ? C8T O2T C5T 107.5(11) . . ? O2T C5T C6T 106.0(11) . . ? O2T C5T H9T 110.5 . . ? C6T C5T H9T 110.5 . . ? O2T C5T H10T 110.5 . . ? C6T C5T H10T 110.5 . . ? H9T C5T H10T 108.7 . . ? C7T C6T C5T 107.8(12) . . ? C7T C6T H11T 110.2 . . ? C5T C6T H11T 110.2 . . ? C7T C6T H12T 110.2 . . ? C5T C6T H12T 110.2 . . ? H11T C6T H12T 108.5 . . ? C6T C7T C8T 105.2(11) . . ? C6T C7T H13T 110.7 . . ? C8T C7T H13T 110.7 . . ? C6T C7T H14T 110.7 . . ? C8T C7T H14T 110.7 . . ? H13T C7T H14T 108.8 . . ? O2T C8T C7T 107.8(11) . . ? O2T C8T H15T 110.1 . . ? C7T C8T H15T 110.1 . . ? O2T C8T H16T 110.1 . . ? C7T C8T H16T 110.1 . . ? H15T C8T H16T 108.5 . . ? C12T O3T C9T 108.3(9) . . ? C10T C9T O3T 105.7(9) . . ? C10T C9T H17T 110.6 . . ? O3T C9T H17T 110.6 . . ? C10T C9T H18T 110.6 . . ? O3T C9T H18T 110.6 . . ? H17T C9T H18T 108.7 . . ? C9T C10T C11T 109.7(8) . . ? C9T C10T H19T 109.7 . . ? C11T C10T H19T 109.7 . . ? C9T C10T H20T 109.7 . . ? C11T C10T H20T 109.7 . . ? H19T C10T H20T 108.2 . . ? C12T C11T C10T 104.5(8) . . ? C12T C11T H21T 110.9 . . ? C10T C11T H21T 110.9 . . ? C12T C11T H22T 110.9 . . ? C10T C11T H22T 110.9 . . ? H21T C11T H22T 108.9 . . ? O3T C12T C11T 111.0(8) . . ? O3T C12T H23T 109.4 . . ? C11T C12T H23T 109.4 . . ? O3T C12T H24T 109.4 . . ? C11T C12T H24T 109.4 . . ? H23T C12T H24T 108.0 . . ? C16T O4T C13T 91.6 . . ? O4T C13T C14T 112.8 . . ? C14T C13T C16T 76.9 . . ? O4T C13T H13A 109.0 . . ? C14T C13T H13A 109.0 . . ? C16T C13T H13A 101.5 . . ? O4T C13T H13B 109.0 . . ? C14T C13T H13B 109.0 . . ? C16T C13T H13B 145.6 . . ? H13A C13T H13B 107.8 . . ? C15T C14T C13T 103.5 . . ? C15T C14T H14A 111.1 . . ? C13T C14T H14A 111.1 . . ? C15T C14T H14B 111.1 . . ? C13T C14T H14B 111.1 . . ? H14A C14T H14B 109.0 . . ? C14T C15T C16T 100.1 . . ? C14T C15T H15A 111.8 . . ? C16T C15T H15A 111.8 . . ? C14T C15T H15B 111.8 . . ? C16T C15T H15B 111.8 . . ? H15A C15T H15B 109.5 . . ? O4T C16T C15T 116.9 . . ? O4T C16T C13T 45.8 . . ? C15T C16T C13T 79.5 . . ? O4T C16T H16A 108.1 . . ? C15T C16T H16A 108.1 . . ? C13T C16T H16A 149.2 . . ? O4T C16T H16B 108.1 . . ? C15T C16T H16B 108.1 . . ? C13T C16T H16B 98.0 . . ? H16A C16T H16B 107.3 . . ? 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 O1 Cu1 N1 C21 -127.1(4) . . . . ? O2 Cu1 N1 C21 -34.1(4) . . . . ? O4 Cu1 N1 C21 148.2(4) 2_665 . . . ? O3 Cu1 N1 C21 56.1(4) 2_665 . . . ? O1 Cu1 N1 C25 57.1(3) . . . . ? O2 Cu1 N1 C25 150.1(3) . . . . ? O4 Cu1 N1 C25 -27.6(4) 2_665 . . . ? O3 Cu1 N1 C25 -119.7(3) 2_665 . . . ? O2 Cu1 O1 C5 -0.5(4) . . . . ? O4 Cu1 O1 C5 -166.1(4) 2_665 . . . ? O3 Cu1 O1 C5 -93.7(6) 2_665 . . . ? N1 Cu1 O1 C5 99.7(4) . . . . ? O1 Cu1 O2 C7 -2.1(4) . . . . ? O4 Cu1 O2 C7 74.0(6) 2_665 . . . ? O3 Cu1 O2 C7 164.1(4) 2_665 . . . ? N1 Cu1 O2 C7 -97.0(4) . . . . ? Cu1 O1 C5 C6 1.6(8) . . . . ? Cu1 O1 C5 C4 179.9(3) . . . . ? C3A C4 C5 O1 -74.8(9) . . . . ? C1B C4 C5 O1 59.2(8) . . . . ? C2B C4 C5 O1 -175.1(8) . . . . ? C2A C4 C5 O1 160.8(9) . . . . ? C1A C4 C5 O1 43.6(9) . . . . ? C3B C4 C5 O1 -58.4(7) . . . . ? C3A C4 C5 C6 103.5(9) . . . . ? C1B C4 C5 C6 -122.5(7) . . . . ? C2B C4 C5 C6 3.2(9) . . . . ? C2A C4 C5 C6 -20.9(10) . . . . ? C1A C4 C5 C6 -138.1(8) . . . . ? C3B C4 C5 C6 119.9(7) . . . . ? O1 C5 C6 C7 -0.3(8) . . . . ? C4 C5 C6 C7 -178.4(4) . . . . ? Cu1 O2 C7 C6 3.8(6) . . . . ? Cu1 O2 C7 C8 -174.3(3) . . . . ? C5 C6 C7 O2 -2.6(8) . . . . ? C5 C6 C7 C8 175.3(4) . . . . ? O2 C7 C8 C13 13.1(5) . . . . ? C6 C7 C8 C13 -165.1(4) . . . . ? O2 C7 C8 C9 -169.0(4) . . . . ? C6 C7 C8 C9 12.8(6) . . . . ? C13 C8 C9 C10 0.9(6) . . . . ? C7 C8 C9 C10 -177.0(4) . . . . ? C8 C9 C10 C11 -0.8(7) . . . . ? C9 C10 C11 C12 0.4(7) . . . . ? C10 C11 C12 C13 -0.1(6) . . . . ? C10 C11 C12 C14 -179.9(4) . . . . ? C9 C8 C13 C12 -0.6(6) . . . . ? C7 C8 C13 C12 177.5(4) . . . . ? C11 C12 C13 C8 0.2(6) . . . . ? C14 C12 C13 C8 -180.0(4) . . . . ? Cu1 O3 C14 C15 4.1(6) 2_665 . . . ? Cu1 O3 C14 C12 -174.7(3) 2_665 . . . ? C13 C12 C14 O3 23.2(6) . . . . ? C11 C12 C14 O3 -156.9(4) . . . . ? C13 C12 C14 C15 -155.6(4) . . . . ? C11 C12 C14 C15 24.2(6) . . . . ? O3 C14 C15 C16 -0.2(8) . . . . ? C12 C14 C15 C16 178.5(4) . . . . ? Cu1 O4 C16 C15 -7.6(7) 2_665 . . . ? Cu1 O4 C16 C17 170.6(3) 2_665 . . . ? C14 C15 C16 O4 2.0(8) . . . . ? C14 C15 C16 C17 -176.0(4) . . . . ? O4 C16 C17 C19B 24.0(9) . . . . ? C15 C16 C17 C19B -157.7(8) . . . . ? O4 C16 C17 C18A 172.2(7) . . . . ? C15 C16 C17 C18A -9.6(8) . . . . ? O4 C16 C17 C20B -97.9(8) . . . . ? C15 C16 C17 C20B 80.4(9) . . . . ? O4 C16 C17 C19A 48.4(7) . . . . ? C15 C16 C17 C19A -133.3(7) . . . . ? O4 C16 C17 C20A -67.5(7) . . . . ? C15 C16 C17 C20A 110.7(7) . . . . ? O4 C16 C17 C18B 144.1(8) . . . . ? C15 C16 C17 C18B -37.7(9) . . . . ? C25 N1 C21 C22 0.8(7) . . . . ? Cu1 N1 C21 C22 -175.2(4) . . . . ? N1 C21 C22 C23 -0.3(8) . . . . ? C27 N2 C23 C22 177.9(5) . . . . ? C26 N2 C23 C22 2.2(8) . . . . ? C27 N2 C23 C24 -3.5(8) . . . . ? C26 N2 C23 C24 -179.2(5) . . . . ? C21 C22 C23 N2 178.2(5) . . . . ? C21 C22 C23 C24 -0.5(7) . . . . ? N2 C23 C24 C25 -177.9(5) . . . . ? C22 C23 C24 C25 0.8(7) . . . . ? C21 N1 C25 C24 -0.5(7) . . . . ? Cu1 N1 C25 C24 175.7(4) . . . . ? C23 C24 C25 N1 -0.3(8) . . . . ? O6 Cu2 N3 C52 103.8(4) . . . . ? O7 Cu2 N3 C52 -167.5(4) 2_655 . . . ? O5 Cu2 N3 C52 10.5(4) . . . . ? O8 Cu2 N3 C52 -76.0(4) 2_655 . . . ? O6 Cu2 N3 C48 -86.3(4) . . . . ? O7 Cu2 N3 C48 2.4(4) 2_655 . . . ? O5 Cu2 N3 C48 -179.6(4) . . . . ? O8 Cu2 N3 C48 93.9(4) 2_655 . . . ? O6 Cu2 O5 C32 3.6(4) . . . . ? O7 Cu2 O5 C32 -84.2(7) 2_655 . . . ? O8 Cu2 O5 C32 -166.9(4) 2_655 . . . ? N3 Cu2 O5 C32 103.9(4) . . . . ? O7 Cu2 O6 C34 165.4(4) 2_655 . . . ? O5 Cu2 O6 C34 -0.5(4) . . . . ? N3 Cu2 O6 C34 -98.5(4) . . . . ? Cu2 O5 C32 C33 -2.0(6) . . . . ? Cu2 O5 C32 C31 179.9(3) . . . . ? C29 C31 C32 O5 -65.2(5) . . . . ? C30 C31 C32 O5 173.0(4) . . . . ? C28 C31 C32 O5 51.5(6) . . . . ? C29 C31 C32 C33 116.7(5) . . . . ? C30 C31 C32 C33 -5.2(7) . . . . ? C28 C31 C32 C33 -126.7(5) . . . . ? O5 C32 C33 C34 -3.7(7) . . . . ? C31 C32 C33 C34 174.2(4) . . . . ? Cu2 O6 C34 C33 -4.3(6) . . . . ? Cu2 O6 C34 C35 175.4(3) . . . . ? C32 C33 C34 O6 7.1(7) . . . . ? C32 C33 C34 C35 -172.6(4) . . . . ? O6 C34 C35 C36 -166.7(4) . . . . ? C33 C34 C35 C36 13.0(6) . . . . ? O6 C34 C35 C40 10.5(5) . . . . ? C33 C34 C35 C40 -169.9(4) . . . . ? C40 C35 C36 C37 0.9(6) . . . . ? C34 C35 C36 C37 178.1(4) . . . . ? C35 C36 C37 C38 -1.0(7) . . . . ? C36 C37 C38 C39 1.6(7) . . . . ? C37 C38 C39 C40 -2.1(6) . . . . ? C37 C38 C39 C41 179.0(4) . . . . ? C38 C39 C40 C35 2.1(6) . . . . ? C41 C39 C40 C35 -178.9(4) . . . . ? C36 C35 C40 C39 -1.5(6) . . . . ? C34 C35 C40 C39 -178.8(4) . . . . ? Cu2 O7 C41 C42 -8.2(6) 2_655 . . . ? Cu2 O7 C41 C39 169.6(3) 2_655 . . . ? C40 C39 C41 O7 -12.6(5) . . . . ? C38 C39 C41 O7 166.4(4) . . . . ? C40 C39 C41 C42 165.4(4) . . . . ? C38 C39 C41 C42 -15.6(6) . . . . ? O7 C41 C42 C43 -7.0(7) . . . . ? C39 C41 C42 C43 175.3(4) . . . . ? Cu2 O8 C43 C42 23.1(6) 2_655 . . . ? Cu2 O8 C43 C44 -158.7(3) 2_655 . . . ? C41 C42 C43 O8 -1.3(7) . . . . ? C41 C42 C43 C44 -179.3(5) . . . . ? O8 C43 C44 C46 48.2(7) . . . . ? C42 C43 C44 C46 -133.6(6) . . . . ? O8 C43 C44 C45 169.2(5) . . . . ? C42 C43 C44 C45 -12.5(8) . . . . ? O8 C43 C44 C47 -71.2(6) . . . . ? C42 C43 C44 C47 107.0(6) . . . . ? C52 N3 C48 C49 -1.4(7) . . . . ? Cu2 N3 C48 C49 -171.7(4) . . . . ? N3 C48 C49 C50 -1.4(8) . . . . ? C53 N4 C50 C51 -175.5(5) . . . . ? C54 N4 C50 C51 -9.3(8) . . . . ? C53 N4 C50 C49 5.6(8) . . . . ? C54 N4 C50 C49 171.7(5) . . . . ? C48 C49 C50 N4 -177.6(5) . . . . ? C48 C49 C50 C51 3.4(7) . . . . ? N4 C50 C51 C52 178.2(5) . . . . ? C49 C50 C51 C52 -2.8(8) . . . . ? C48 N3 C52 C51 2.1(8) . . . . ? Cu2 N3 C52 C51 172.9(4) . . . . ? C50 C51 C52 N3 0.1(9) . . . . ? C4T O1T C1T C2T 9.6(16) . . . . ? O1T C1T C2T C3T -22(2) . . . . ? C1T C2T C3T C4T 26(2) . . . . ? C2T C3T C4T O1T -19(2) . . . . ? C1T O1T C4T C3T 5.9(18) . . . . ? C8T O2T C5T C6T 25(2) . . . . ? O2T C5T C6T C7T -19(3) . . . . ? C5T C6T C7T C8T 6(3) . . . . ? C5T O2T C8T C7T -21(2) . . . . ? C6T C7T C8T O2T 9(2) . . . . ? C12T O3T C9T C10T 9(2) . . . . ? O3T C9T C10T C11T -5(2) . . . . ? C9T C10T C11T C12T -0.5(18) . . . . ? C9T O3T C12T C11T -9.6(19) . . . . ? C10T C11T C12T O3T 6.2(18) . . . . ? C16T O4T C13T C14T 34.8 . . . . ? O4T C13T C14T C15T -21.5 . . . . ? C16T C13T C14T C15T 1.9 . . . . ? C13T C14T C15T C16T -2.5 . . . . ? C13T O4T C16T C15T -38.7 . . . . ? C14T C15T C16T O4T 28.9 . . . . ? C14T C15T C16T C13T 1.9 . . . . ? C14T C13T C16T O4T -147.3 . . . . ? O4T C13T C16T C15T 145.5 . . . . ? C14T C13T C16T C15T -1.8 . . . . ? _diffrn_measured_fraction_theta_max 0.903 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.960 _refine_diff_density_min -0.663 _refine_diff_density_rms 0.132 data_lj50sad _database_code_depnum_ccdc_archive 'CCDC 258478' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H58 Cu2 N2 O8, 1(C5 H5 N)' _chemical_formula_sum 'C55 H63 Cu2 N3 O8' _chemical_formula_weight 1021.16 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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.4084(16) _cell_length_b 10.0249(19) _cell_length_c 17.246(3) _cell_angle_alpha 97.396(3) _cell_angle_beta 99.356(3) _cell_angle_gamma 110.158(3) _cell_volume 1319.5(4) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5911 _cell_measurement_theta_min 2.209 _cell_measurement_theta_max 28.303 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 0.860 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.782 _exptl_absorpt_correction_T_max 0.942 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 122 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.03 _diffrn_reflns_number 12746 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_sigmaI/netI 0.0349 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 28.37 _reflns_number_total 6069 _reflns_number_gt 5038 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1995)' _computing_cell_refinement 'SAINT (Bruker, 1995)' _computing_data_reduction 'SAINT and XPREP (Bruker, 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEPIII (Farrugia, 1997) WINGX-32 (Farrugia, 1999) ; _computing_publication_material 'enCIFer 1.0 (CCDC, 2003)' _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^)+(0.0625P)^2^+0.1906P] 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 6069 _refine_ls_number_parameters 313 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0492 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.1024 _refine_ls_wR_factor_gt 0.0959 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 0.02419(3) 0.07074(2) -0.206574(13) 0.02198(9) Uani 1 1 d . . . O1 O 0.13388(17) 0.23851(14) -0.25020(8) 0.0255(3) Uani 1 1 d . . . O2 O 0.08297(19) 0.18328(14) -0.09940(8) 0.0290(3) Uani 1 1 d . . . O3 O 0.02837(18) 0.09689(14) 0.15727(8) 0.0255(3) Uani 1 1 d . . . O4 O 0.01024(17) 0.04692(14) 0.31105(8) 0.0243(3) Uani 1 1 d . . . C1 C 0.3926(3) 0.4221(2) -0.31140(13) 0.0320(4) Uani 1 1 d . . . H1A H 0.3195 0.3265 -0.3444 0.048 Uiso 1 1 calc R . . H1B H 0.4897 0.4141 -0.2749 0.048 Uiso 1 1 calc R . . H1C H 0.4378 0.4893 -0.3462 0.048 Uiso 1 1 calc R . . C2 C 0.3987(3) 0.6300(2) -0.21368(15) 0.0429(6) Uani 1 1 d . . . H2A H 0.4892 0.6227 -0.1728 0.064 Uiso 1 1 calc R . . H2B H 0.3273 0.6727 -0.1876 0.064 Uiso 1 1 calc R . . H2C H 0.4529 0.6916 -0.2493 0.064 Uiso 1 1 calc R . . C3 C 0.1314(3) 0.4877(3) -0.32056(14) 0.0380(5) Uani 1 1 d . . . H3A H 0.1754 0.5508 -0.3574 0.057 Uiso 1 1 calc R . . H3B H 0.0634 0.5274 -0.2901 0.057 Uiso 1 1 calc R . . H3C H 0.0574 0.3904 -0.3512 0.057 Uiso 1 1 calc R . . C4 C 0.2843(3) 0.4790(2) -0.26256(12) 0.0252(4) Uani 1 1 d . . . C5 C 0.2099(2) 0.36829(19) -0.21135(11) 0.0221(4) Uani 1 1 d . . . C6 C 0.2241(3) 0.4128(2) -0.12951(12) 0.0290(4) Uani 1 1 d . . . H6 H 0.2827 0.5131 -0.1068 0.035 Uiso 1 1 calc R . . C7 C 0.1579(2) 0.3200(2) -0.07885(11) 0.0237(4) Uani 1 1 d . . . C8 C 0.1716(3) 0.3811(2) 0.00743(11) 0.0245(4) Uani 1 1 d . . . C9 C 0.2124(3) 0.5281(2) 0.03541(13) 0.0380(5) Uani 1 1 d . . . H9 H 0.2386 0.5941 0.0002 0.046 Uiso 1 1 calc R . . C10 C 0.2149(3) 0.5785(2) 0.11410(13) 0.0381(5) Uani 1 1 d . . . H10 H 0.2419 0.6789 0.1326 0.046 Uiso 1 1 calc R . . C11 C 0.1782(3) 0.4837(2) 0.16627(12) 0.0271(4) Uani 1 1 d . . . H11 H 0.1801 0.5194 0.2203 0.033 Uiso 1 1 calc R . . C12 C 0.1385(2) 0.33634(19) 0.14000(11) 0.0215(4) Uani 1 1 d . . . C13 C 0.1336(2) 0.28656(19) 0.06002(11) 0.0211(4) Uani 1 1 d . . . H13 H 0.1035 0.1858 0.0411 0.025 Uiso 1 1 calc R . . C14 C 0.0984(2) 0.22846(19) 0.19343(11) 0.0196(3) Uani 1 1 d . . . C15 C 0.1394(2) 0.2750(2) 0.27703(11) 0.0233(4) Uani 1 1 d . . . H15 H 0.2026 0.3753 0.2984 0.028 Uiso 1 1 calc R . . C16 C 0.0929(2) 0.1829(2) 0.33086(11) 0.0220(4) Uani 1 1 d . . . C17 C 0.1435(3) 0.2428(2) 0.42167(12) 0.0296(4) Uani 1 1 d . . . C18 C 0.2220(3) 0.4080(2) 0.44534(12) 0.0359(5) Uani 1 1 d . . . H18A H 0.1391 0.4479 0.4212 0.054 Uiso 1 1 calc R . . H18B H 0.3294 0.4447 0.4262 0.054 Uiso 1 1 calc R . . H18C H 0.2479 0.4373 0.5039 0.054 Uiso 1 1 calc R . . C19 C 0.2750(5) 0.1812(4) 0.45698(16) 0.0697(10) Uani 1 1 d . . . H19A H 0.3055 0.2116 0.5155 0.104 Uiso 1 1 calc R . . H19B H 0.3798 0.2173 0.4357 0.104 Uiso 1 1 calc R . . H19C H 0.2243 0.0751 0.4424 0.104 Uiso 1 1 calc R . . C20 C -0.0189(4) 0.1887(3) 0.45536(16) 0.0634(9) Uani 1 1 d . . . H20A H -0.0701 0.0825 0.4417 0.095 Uiso 1 1 calc R . . H20B H -0.1034 0.2281 0.4322 0.095 Uiso 1 1 calc R . . H20C H 0.0123 0.2207 0.5138 0.095 Uiso 1 1 calc R . . N1 N -0.2496(2) 0.07000(17) -0.24026(10) 0.0267(3) Uani 1 1 d . . . C21 C -0.3755(3) 0.0170(2) -0.20196(14) 0.0342(5) Uani 1 1 d . . . H21 H -0.3501 -0.0209 -0.1558 0.041 Uiso 1 1 calc R . . C22 C -0.5413(3) 0.0146(3) -0.22614(17) 0.0436(6) Uani 1 1 d . . . H22 H -0.6278 -0.0243 -0.1972 0.052 Uiso 1 1 calc R . . C23 C -0.5794(3) 0.0694(3) -0.29293(17) 0.0459(6) Uani 1 1 d . . . H23 H -0.6925 0.0692 -0.3110 0.055 Uiso 1 1 calc R . . C24 C -0.4500(3) 0.1246(3) -0.33289(16) 0.0458(6) Uani 1 1 d . . . H24 H -0.4718 0.1640 -0.3789 0.055 Uiso 1 1 calc R . . C25 C -0.2883(3) 0.1220(2) -0.30512(13) 0.0339(5) Uani 1 1 d . . . H25 H -0.2001 0.1589 -0.3335 0.041 Uiso 1 1 calc R . . N2 N 0.6411(3) 0.1301(4) 0.02671(17) 0.0661(8) Uani 0.50 1 d P . . C26A C 0.4795(4) 0.1279(4) 0.00297(17) 0.0574(7) Uani 0.50 1 d P A 1 H26A H 0.4634 0.2174 0.0044 0.069 Uiso 0.50 1 calc PR A 1 C27A C 0.3374(3) 0.0011(4) -0.02322(16) 0.0605(8) Uani 0.50 1 d P . 1 H27A H 0.2248 0.0033 -0.0389 0.073 Uiso 0.50 1 calc PR . 1 C26B C 0.4795(4) 0.1279(4) 0.00297(17) 0.0574(7) Uani 0.50 1 d P B 2 H26B H 0.4634 0.2174 0.0044 0.069 Uiso 0.50 1 calc PR B 2 C27B C 0.3374(3) 0.0011(4) -0.02322(16) 0.0605(8) Uani 0.50 1 d P . 2 H27B H 0.2248 0.0033 -0.0389 0.073 Uiso 0.50 1 calc PR . 2 C28 C 0.6411(3) 0.1301(4) 0.02671(17) 0.0661(8) Uani 0.50 1 d P . . H28 H 0.7377 0.2192 0.0453 0.079 Uiso 0.50 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.03110(14) 0.01278(12) 0.01900(13) 0.00286(8) 0.00351(9) 0.00548(9) O1 0.0333(7) 0.0166(6) 0.0213(7) 0.0038(5) 0.0049(5) 0.0035(5) O2 0.0480(8) 0.0138(6) 0.0193(7) 0.0033(5) 0.0056(6) 0.0052(6) O3 0.0385(7) 0.0141(6) 0.0194(7) 0.0026(5) 0.0027(5) 0.0065(5) O4 0.0331(7) 0.0173(6) 0.0210(7) 0.0034(5) 0.0059(5) 0.0075(5) C1 0.0324(11) 0.0298(11) 0.0352(11) 0.0087(9) 0.0128(9) 0.0101(9) C2 0.0621(15) 0.0184(10) 0.0397(13) 0.0048(9) 0.0236(12) -0.0006(10) C3 0.0443(12) 0.0437(13) 0.0411(13) 0.0255(11) 0.0176(10) 0.0255(11) C4 0.0324(10) 0.0176(9) 0.0253(10) 0.0068(7) 0.0094(8) 0.0069(8) C5 0.0242(9) 0.0170(9) 0.0251(9) 0.0051(7) 0.0051(7) 0.0074(7) C6 0.0412(11) 0.0167(9) 0.0244(10) 0.0032(8) 0.0078(8) 0.0050(8) C7 0.0312(10) 0.0152(9) 0.0224(9) 0.0036(7) 0.0040(7) 0.0068(7) C8 0.0323(10) 0.0157(9) 0.0217(9) 0.0026(7) 0.0040(7) 0.0056(7) C9 0.0676(15) 0.0136(9) 0.0289(11) 0.0060(8) 0.0134(10) 0.0087(10) C10 0.0661(15) 0.0119(9) 0.0325(11) 0.0020(8) 0.0134(11) 0.0098(9) C11 0.0382(11) 0.0174(9) 0.0231(9) 0.0009(7) 0.0063(8) 0.0084(8) C12 0.0231(9) 0.0158(8) 0.0233(9) 0.0037(7) 0.0024(7) 0.0058(7) C13 0.0246(9) 0.0118(8) 0.0234(9) 0.0015(7) 0.0012(7) 0.0049(7) C14 0.0213(8) 0.0155(8) 0.0212(9) 0.0025(7) 0.0025(7) 0.0072(7) C15 0.0293(9) 0.0154(8) 0.0222(9) 0.0019(7) 0.0040(7) 0.0062(7) C16 0.0222(9) 0.0206(9) 0.0227(9) 0.0023(7) 0.0037(7) 0.0087(7) C17 0.0426(11) 0.0235(10) 0.0207(10) 0.0032(8) 0.0058(8) 0.0107(9) C18 0.0494(13) 0.0259(11) 0.0216(10) -0.0029(8) 0.0025(9) 0.0059(9) C19 0.113(3) 0.070(2) 0.0310(13) -0.0081(13) -0.0214(15) 0.063(2) C20 0.080(2) 0.0497(17) 0.0372(14) -0.0049(12) 0.0309(14) -0.0077(14) N1 0.0319(9) 0.0191(8) 0.0286(9) 0.0028(7) 0.0065(7) 0.0097(7) C21 0.0455(12) 0.0205(10) 0.0369(12) 0.0071(9) 0.0144(10) 0.0097(9) C22 0.0390(12) 0.0291(12) 0.0656(17) 0.0083(11) 0.0277(12) 0.0094(10) C23 0.0331(12) 0.0398(14) 0.0674(17) 0.0065(12) 0.0105(11) 0.0186(10) C24 0.0453(14) 0.0549(16) 0.0481(15) 0.0181(12) 0.0101(11) 0.0294(12) C25 0.0356(11) 0.0388(12) 0.0353(11) 0.0137(9) 0.0122(9) 0.0197(10) N2 0.0384(13) 0.082(2) 0.0524(16) 0.0109(15) -0.0019(11) -0.0030(13) C26A 0.0501(16) 0.0662(19) 0.0513(16) 0.0151(14) 0.0046(13) 0.0177(14) C27A 0.0383(14) 0.092(2) 0.0357(14) 0.0168(15) 0.0013(11) 0.0073(15) C26B 0.0501(16) 0.0662(19) 0.0513(16) 0.0151(14) 0.0046(13) 0.0177(14) C27B 0.0383(14) 0.092(2) 0.0357(14) 0.0168(15) 0.0013(11) 0.0073(15) C28 0.0384(13) 0.082(2) 0.0524(16) 0.0109(15) -0.0019(11) -0.0030(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 O2 1.9275(14) . ? Cu1 O3 1.9289(13) 2 ? Cu1 O1 1.9307(13) . ? Cu1 O4 1.9415(13) 2 ? Cu1 N1 2.2781(17) . ? O1 C5 1.270(2) . ? O2 C7 1.268(2) . ? O3 C14 1.268(2) . ? O3 Cu1 1.9289(13) 2 ? O4 C16 1.268(2) . ? O4 Cu1 1.9415(13) 2 ? C1 C4 1.532(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C4 1.527(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.530(3) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.535(2) . ? C5 C6 1.397(3) . ? C6 C7 1.396(3) . ? C6 H6 0.9500 . ? C7 C8 1.505(3) . ? C8 C13 1.389(3) . ? C8 C9 1.392(3) . ? C9 C10 1.380(3) . ? C9 H9 0.9500 . ? C10 C11 1.385(3) . ? C10 H10 0.9500 . ? C11 C12 1.392(3) . ? C11 H11 0.9500 . ? C12 C13 1.394(3) . ? C12 C14 1.496(2) . ? C13 H13 0.9500 . ? C14 C15 1.403(3) . ? C15 C16 1.399(3) . ? C15 H15 0.9500 . ? C16 C17 1.536(3) . ? C17 C19 1.524(3) . ? C17 C18 1.526(3) . ? C17 C20 1.525(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? N1 C21 1.330(3) . ? N1 C25 1.333(3) . ? C21 C22 1.379(3) . ? C21 H21 0.9500 . ? C22 C23 1.377(4) . ? C22 H22 0.9500 . ? C23 C24 1.376(3) . ? C23 H23 0.9500 . ? C24 C25 1.376(3) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? N2 C26A 1.346(4) . ? N2 C27A 1.383(5) 2_655 ? C26A C27A 1.370(4) . ? C26A H26A 0.9500 . ? C27A C28 1.383(5) 2_655 ? C27A H27A 0.9500 . ? 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 O2 Cu1 O3 86.05(6) . 2 ? O2 Cu1 O1 92.93(6) . . ? O3 Cu1 O1 165.90(6) 2 . ? O2 Cu1 O4 173.29(6) . 2 ? O3 Cu1 O4 91.82(6) 2 2 ? O1 Cu1 O4 87.58(6) . 2 ? O2 Cu1 N1 96.53(6) . . ? O3 Cu1 N1 98.46(6) 2 . ? O1 Cu1 N1 95.63(6) . . ? O4 Cu1 N1 90.08(6) 2 . ? C5 O1 Cu1 126.20(12) . . ? C7 O2 Cu1 126.06(12) . . ? C14 O3 Cu1 126.36(12) . 2 ? C16 O4 Cu1 125.18(12) . 2 ? C4 C1 H1A 109.5 . . ? C4 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C2 H2A 109.5 . . ? C4 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 C3 109.72(18) . . ? C2 C4 C1 108.72(17) . . ? C3 C4 C1 108.64(17) . . ? C2 C4 C5 113.83(16) . . ? C3 C4 C5 107.81(16) . . ? C1 C4 C5 107.99(16) . . ? O1 C5 C6 124.92(17) . . ? O1 C5 C4 114.33(16) . . ? C6 C5 C4 120.73(17) . . ? C7 C6 C5 124.52(18) . . ? C7 C6 H6 117.7 . . ? C5 C6 H6 117.7 . . ? O2 C7 C6 125.20(18) . . ? O2 C7 C8 114.87(16) . . ? C6 C7 C8 119.93(17) . . ? C13 C8 C9 118.84(18) . . ? C13 C8 C7 118.84(16) . . ? C9 C8 C7 122.24(17) . . ? C10 C9 C8 120.34(19) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 120.41(19) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C10 C11 C12 120.40(18) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C11 C12 C13 118.58(17) . . ? C11 C12 C14 122.98(17) . . ? C13 C12 C14 118.43(16) . . ? C8 C13 C12 121.41(17) . . ? C8 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? O3 C14 C15 124.61(16) . . ? O3 C14 C12 114.97(16) . . ? C15 C14 C12 120.42(16) . . ? C16 C15 C14 124.09(17) . . ? C16 C15 H15 118.0 . . ? C14 C15 H15 118.0 . . ? O4 C16 C15 124.86(17) . . ? O4 C16 C17 114.41(16) . . ? C15 C16 C17 120.72(17) . . ? C19 C17 C18 109.4(2) . . ? C19 C17 C20 109.7(2) . . ? C18 C17 C20 108.20(19) . . ? C19 C17 C16 106.58(17) . . ? C18 C17 C16 114.57(16) . . ? C20 C17 C16 108.32(18) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C21 N1 C25 117.51(18) . . ? C21 N1 Cu1 125.08(14) . . ? C25 N1 Cu1 117.36(13) . . ? N1 C21 C22 123.1(2) . . ? N1 C21 H21 118.5 . . ? C22 C21 H21 118.5 . . ? C23 C22 C21 118.9(2) . . ? C23 C22 H22 120.5 . . ? C21 C22 H22 120.5 . . ? C24 C23 C22 118.5(2) . . ? C24 C23 H23 120.8 . . ? C22 C23 H23 120.8 . . ? C23 C24 C25 119.0(2) . . ? C23 C24 H24 120.5 . . ? C25 C24 H24 120.5 . . ? N1 C25 C24 123.1(2) . . ? N1 C25 H25 118.4 . . ? C24 C25 H25 118.4 . . ? C26A N2 C27A 118.1(3) . 2_655 ? N2 C26A C27A 122.3(3) . . ? N2 C26A H26A 118.9 . . ? C27A C26A H26A 118.9 . . ? C26A C27A C28 119.6(3) . 2_655 ? C26A C27A H27A 120.2 . . ? C28 C27A H27A 120.2 2_655 . ? 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 O2 Cu1 O1 C5 -0.42(16) . . . . ? O3 Cu1 O1 C5 -85.9(3) 2 . . . ? O4 Cu1 O1 C5 -173.72(15) 2 . . . ? N1 Cu1 O1 C5 96.43(15) . . . . ? O3 Cu1 O2 C7 169.70(17) 2 . . . ? O1 Cu1 O2 C7 3.79(17) . . . . ? N1 Cu1 O2 C7 -92.22(17) . . . . ? Cu1 O1 C5 C6 -1.5(3) . . . . ? Cu1 O1 C5 C4 -179.75(12) . . . . ? C2 C4 C5 O1 -171.19(18) . . . . ? C3 C4 C5 O1 66.8(2) . . . . ? C1 C4 C5 O1 -50.4(2) . . . . ? C2 C4 C5 C6 10.5(3) . . . . ? C3 C4 C5 C6 -111.5(2) . . . . ? C1 C4 C5 C6 131.27(19) . . . . ? O1 C5 C6 C7 0.8(3) . . . . ? C4 C5 C6 C7 178.94(18) . . . . ? Cu1 O2 C7 C6 -5.5(3) . . . . ? Cu1 O2 C7 C8 174.01(12) . . . . ? C5 C6 C7 O2 3.0(3) . . . . ? C5 C6 C7 C8 -176.44(18) . . . . ? O2 C7 C8 C13 11.8(3) . . . . ? C6 C7 C8 C13 -168.74(19) . . . . ? O2 C7 C8 C9 -164.8(2) . . . . ? C6 C7 C8 C9 14.7(3) . . . . ? C13 C8 C9 C10 0.1(3) . . . . ? C7 C8 C9 C10 176.7(2) . . . . ? C8 C9 C10 C11 0.5(4) . . . . ? C9 C10 C11 C12 0.0(4) . . . . ? C10 C11 C12 C13 -1.1(3) . . . . ? C10 C11 C12 C14 179.75(19) . . . . ? C9 C8 C13 C12 -1.2(3) . . . . ? C7 C8 C13 C12 -177.88(17) . . . . ? C11 C12 C13 C8 1.7(3) . . . . ? C14 C12 C13 C8 -179.13(17) . . . . ? Cu1 O3 C14 C15 -4.6(3) 2 . . . ? Cu1 O3 C14 C12 174.81(11) 2 . . . ? C11 C12 C14 O3 165.12(17) . . . . ? C13 C12 C14 O3 -14.0(2) . . . . ? C11 C12 C14 C15 -15.4(3) . . . . ? C13 C12 C14 C15 165.43(17) . . . . ? O3 C14 C15 C16 -6.4(3) . . . . ? C12 C14 C15 C16 174.17(17) . . . . ? Cu1 O4 C16 C15 15.0(3) 2 . . . ? Cu1 O4 C16 C17 -164.15(12) 2 . . . ? C14 C15 C16 O4 0.7(3) . . . . ? C14 C15 C16 C17 179.80(17) . . . . ? O4 C16 C17 C19 66.4(2) . . . . ? C15 C16 C17 C19 -112.8(2) . . . . ? O4 C16 C17 C18 -172.48(17) . . . . ? C15 C16 C17 C18 8.3(3) . . . . ? O4 C16 C17 C20 -51.6(2) . . . . ? C15 C16 C17 C20 129.2(2) . . . . ? O2 Cu1 N1 C21 -59.33(16) . . . . ? O3 Cu1 N1 C21 27.63(17) 2 . . . ? O1 Cu1 N1 C21 -152.93(16) . . . . ? O4 Cu1 N1 C21 119.49(16) 2 . . . ? O2 Cu1 N1 C25 123.24(16) . . . . ? O3 Cu1 N1 C25 -149.81(15) 2 . . . ? O1 Cu1 N1 C25 29.63(16) . . . . ? O4 Cu1 N1 C25 -57.95(16) 2 . . . ? C25 N1 C21 C22 -0.4(3) . . . . ? Cu1 N1 C21 C22 -177.78(16) . . . . ? N1 C21 C22 C23 -0.1(3) . . . . ? C21 C22 C23 C24 0.0(4) . . . . ? C22 C23 C24 C25 0.5(4) . . . . ? C21 N1 C25 C24 0.9(3) . . . . ? Cu1 N1 C25 C24 178.51(19) . . . . ? C23 C24 C25 N1 -1.0(4) . . . . ? C27A N2 C26A C27A 0.8(5) 2_655 . . . ? N2 C26A C27A C28 -0.9(5) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.714 _refine_diff_density_min -0.618 _refine_diff_density_rms 0.072 data_lj49sad _database_code_depnum_ccdc_archive 'CCDC 258479' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H64 Cu2 O10' _chemical_formula_sum 'C48 H64 Cu2 O10' _chemical_formula_weight 928.07 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' 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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.0109(7) _cell_length_b 10.5767(11) _cell_length_c 16.5539(17) _cell_angle_alpha 95.966(2) _cell_angle_beta 95.216(2) _cell_angle_gamma 104.527(2) _cell_volume 1173.1(2) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7577 _cell_measurement_theta_min 2.219 _cell_measurement_theta_max 28.314 _exptl_crystal_description prism _exptl_crystal_colour 'intense blue' _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 490 _exptl_absorpt_coefficient_mu 0.961 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.724 _exptl_absorpt_correction_T_max 0.849 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 165 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.01 _diffrn_reflns_number 11339 _diffrn_reflns_av_R_equivalents 0.0166 _diffrn_reflns_av_sigmaI/netI 0.0231 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 28.32 _reflns_number_total 5382 _reflns_number_gt 4840 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1995)' _computing_cell_refinement 'SAINT (Bruker, 1995)' _computing_data_reduction 'SAINT and XPREP (Bruker, 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEPIII (Farrugia, 1997) WINGX-32 (Farrugia, 1999) ; _computing_publication_material 'enCIFer 1.0 (CCDC, 2003)' _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^)+(0.0439P)^2^+0.3992P] 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 5382 _refine_ls_number_parameters 277 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0335 _refine_ls_R_factor_gt 0.0286 _refine_ls_wR_factor_ref 0.0789 _refine_ls_wR_factor_gt 0.0762 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 -0.18159(3) 0.079620(16) -0.200783(10) 0.02023(7) Uani 1 1 d . . . O1 O -0.11045(17) 0.22644(10) -0.26041(7) 0.0271(2) Uani 1 1 d . . . O2 O -0.03451(16) 0.17823(10) -0.10090(6) 0.0242(2) Uani 1 1 d . . . O3 O 0.22552(16) 0.07801(10) 0.14802(6) 0.0215(2) Uani 1 1 d . . . O4 O 0.29340(17) 0.01971(10) 0.30515(6) 0.0241(2) Uani 1 1 d . . . C1 C 0.1797(3) 0.38389(19) -0.35251(12) 0.0420(5) Uani 1 1 d . . . H1A H 0.2013 0.4357 -0.3982 0.063 Uiso 1 1 calc R . . H1B H 0.1232 0.2907 -0.3739 0.063 Uiso 1 1 calc R . . H1C H 0.3065 0.3946 -0.3189 0.063 Uiso 1 1 calc R . . C2 C 0.1206(3) 0.57766(15) -0.26626(10) 0.0295(3) Uani 1 1 d . . . H2A H 0.1299 0.6308 -0.3115 0.044 Uiso 1 1 calc R . . H2B H 0.2531 0.5907 -0.2367 0.044 Uiso 1 1 calc R . . H2C H 0.0334 0.6048 -0.2288 0.044 Uiso 1 1 calc R . . C3 C -0.1626(3) 0.41455(18) -0.35356(11) 0.0387(4) Uani 1 1 d . . . H3A H -0.2554 0.4452 -0.3206 0.058 Uiso 1 1 calc R . . H3B H -0.2185 0.3212 -0.3749 0.058 Uiso 1 1 calc R . . H3C H -0.1403 0.4662 -0.3993 0.058 Uiso 1 1 calc R . . C4 C 0.0355(2) 0.43184(14) -0.30017(9) 0.0240(3) Uani 1 1 d . . . C5 C -0.0006(2) 0.34038(14) -0.23366(9) 0.0194(3) Uani 1 1 d . . . C6 C 0.0885(2) 0.38041(14) -0.15305(9) 0.0214(3) Uani 1 1 d . . . H6 H 0.1689 0.4682 -0.1392 0.026 Uiso 1 1 calc R . . C7 C 0.0662(2) 0.29848(13) -0.09133(9) 0.0184(3) Uani 1 1 d . . . C8 C 0.1673(2) 0.35034(13) -0.00615(9) 0.0181(3) Uani 1 1 d . . . C9 C 0.2505(2) 0.48446(14) 0.02081(9) 0.0210(3) Uani 1 1 d . . . H9 H 0.2433 0.5476 -0.0154 0.025 Uiso 1 1 calc R . . C10 C 0.3433(2) 0.52561(14) 0.10008(9) 0.0233(3) Uani 1 1 d . . . H10 H 0.3998 0.6168 0.1179 0.028 Uiso 1 1 calc R . . C11 C 0.3540(2) 0.43442(14) 0.15351(9) 0.0213(3) Uani 1 1 d . . . H11 H 0.4191 0.4636 0.2076 0.026 Uiso 1 1 calc R . . C12 C 0.2696(2) 0.29956(13) 0.12849(9) 0.0182(3) Uani 1 1 d . . . C13 C 0.1776(2) 0.25931(13) 0.04836(9) 0.0179(3) Uani 1 1 d . . . H13 H 0.1207 0.1681 0.0305 0.021 Uiso 1 1 calc R . . C14 C 0.2710(2) 0.19630(14) 0.18396(9) 0.0187(3) Uani 1 1 d . . . C15 C 0.3172(2) 0.23310(14) 0.26886(9) 0.0217(3) Uani 1 1 d . . . H15 H 0.3433 0.3237 0.2896 0.026 Uiso 1 1 calc R . . C16 C 0.3268(2) 0.14321(14) 0.32472(9) 0.0200(3) Uani 1 1 d . . . C17 C 0.3842(3) 0.18731(15) 0.41707(9) 0.0259(3) Uani 1 1 d . . . C18 C 0.4149(3) 0.33431(16) 0.44235(11) 0.0399(4) Uani 1 1 d . . . H18A H 0.4487 0.3547 0.5018 0.060 Uiso 1 1 calc R . . H18B H 0.2926 0.3589 0.4260 0.060 Uiso 1 1 calc R . . H18C H 0.5232 0.3839 0.4154 0.060 Uiso 1 1 calc R . . C19 C 0.5776(3) 0.1502(2) 0.44120(11) 0.0404(4) Uani 1 1 d . . . H19A H 0.6842 0.2012 0.4141 0.061 Uiso 1 1 calc R . . H19B H 0.5593 0.0560 0.4243 0.061 Uiso 1 1 calc R . . H19C H 0.6127 0.1698 0.5007 0.061 Uiso 1 1 calc R . . C20 C 0.2180(3) 0.1102(2) 0.46099(12) 0.0420(4) Uani 1 1 d . . . H20A H 0.2566 0.1294 0.5203 0.063 Uiso 1 1 calc R . . H20B H 0.1955 0.0156 0.4438 0.063 Uiso 1 1 calc R . . H20C H 0.0958 0.1362 0.4469 0.063 Uiso 1 1 calc R . . O5 O -0.47084(17) 0.13316(11) -0.16590(7) 0.0290(2) Uani 1 1 d . . . C21 C -0.5407(3) 0.0797(2) -0.09427(12) 0.0386(4) Uani 1 1 d . . . H21A H -0.5909 0.1442 -0.0604 0.046 Uiso 1 1 calc R . . H21B H -0.4318 0.0580 -0.0608 0.046 Uiso 1 1 calc R . . C22 C -0.7066(3) -0.0440(2) -0.12430(16) 0.0528(6) Uani 1 1 d . . . H22A H -0.8285 -0.0405 -0.0993 0.063 Uiso 1 1 calc R . . H22B H -0.6669 -0.1235 -0.1108 0.063 Uiso 1 1 calc R . . C23 C -0.7400(3) -0.0451(2) -0.21648(14) 0.0463(5) Uani 1 1 d . . . H23A H -0.8833 -0.0677 -0.2365 0.056 Uiso 1 1 calc R . . H23B H -0.6788 -0.1086 -0.2454 0.056 Uiso 1 1 calc R . . C24 C -0.6379(3) 0.09570(19) -0.22796(12) 0.0368(4) Uani 1 1 d . . . H24A H -0.5946 0.0996 -0.2831 0.044 Uiso 1 1 calc R . . H24B H -0.7275 0.1538 -0.2203 0.044 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02560(11) 0.01170(9) 0.01925(10) 0.00177(6) -0.00389(7) -0.00026(7) O1 0.0357(6) 0.0168(5) 0.0222(5) 0.0041(4) -0.0054(4) -0.0028(4) O2 0.0319(6) 0.0143(5) 0.0203(5) 0.0027(4) -0.0053(4) -0.0023(4) O3 0.0287(5) 0.0128(5) 0.0201(5) 0.0009(4) -0.0026(4) 0.0023(4) O4 0.0345(6) 0.0145(5) 0.0202(5) 0.0015(4) -0.0041(4) 0.0035(4) C1 0.0572(12) 0.0303(9) 0.0393(10) 0.0046(8) 0.0246(9) 0.0062(8) C2 0.0401(9) 0.0170(7) 0.0291(8) 0.0074(6) 0.0018(7) 0.0025(6) C3 0.0515(11) 0.0271(9) 0.0322(9) 0.0087(7) -0.0137(8) 0.0055(8) C4 0.0325(8) 0.0169(7) 0.0213(7) 0.0040(6) 0.0019(6) 0.0036(6) C5 0.0200(6) 0.0155(6) 0.0230(7) 0.0035(5) 0.0018(5) 0.0048(5) C6 0.0247(7) 0.0136(6) 0.0235(7) 0.0021(5) 0.0006(6) 0.0015(5) C7 0.0185(6) 0.0139(6) 0.0214(7) 0.0010(5) -0.0006(5) 0.0035(5) C8 0.0182(6) 0.0146(6) 0.0203(7) 0.0012(5) 0.0007(5) 0.0032(5) C9 0.0253(7) 0.0134(6) 0.0230(7) 0.0031(5) 0.0011(6) 0.0033(5) C10 0.0282(7) 0.0125(6) 0.0256(8) -0.0002(5) 0.0006(6) 0.0004(5) C11 0.0244(7) 0.0168(7) 0.0190(7) -0.0010(5) -0.0017(5) 0.0015(5) C12 0.0190(6) 0.0143(6) 0.0200(7) 0.0012(5) 0.0015(5) 0.0026(5) C13 0.0189(6) 0.0127(6) 0.0204(7) 0.0001(5) 0.0004(5) 0.0027(5) C14 0.0175(6) 0.0149(6) 0.0218(7) 0.0023(5) -0.0001(5) 0.0018(5) C15 0.0278(7) 0.0144(6) 0.0204(7) 0.0005(5) -0.0008(6) 0.0032(5) C16 0.0208(7) 0.0163(6) 0.0203(7) 0.0014(5) -0.0008(5) 0.0019(5) C17 0.0392(9) 0.0178(7) 0.0186(7) 0.0008(5) -0.0015(6) 0.0062(6) C18 0.0748(14) 0.0193(8) 0.0216(8) -0.0012(6) -0.0030(8) 0.0099(8) C19 0.0481(11) 0.0399(10) 0.0286(9) -0.0023(8) -0.0145(8) 0.0129(9) C20 0.0593(12) 0.0361(10) 0.0299(9) 0.0064(8) 0.0138(8) 0.0074(9) O5 0.0308(6) 0.0219(5) 0.0336(6) 0.0018(5) 0.0024(5) 0.0067(5) C21 0.0414(10) 0.0404(10) 0.0373(10) 0.0053(8) 0.0138(8) 0.0138(8) C22 0.0387(11) 0.0440(12) 0.0761(16) 0.0225(11) 0.0119(10) 0.0039(9) C23 0.0275(9) 0.0374(10) 0.0670(14) -0.0098(10) 0.0060(9) 0.0022(8) C24 0.0327(9) 0.0380(10) 0.0408(10) -0.0006(8) -0.0024(7) 0.0162(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 O1 1.9115(11) . ? Cu1 O4 1.9147(11) 2 ? Cu1 O2 1.9175(10) . ? Cu1 O3 1.9317(10) 2 ? Cu1 O5 2.3425(12) . ? O1 C5 1.2661(17) . ? O2 C7 1.2761(17) . ? O3 C14 1.2774(17) . ? O3 Cu1 1.9317(10) 2 ? O4 C16 1.2691(18) . ? O4 Cu1 1.9147(11) 2 ? C1 C4 1.534(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C4 1.532(2) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.536(2) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.537(2) . ? C5 C6 1.396(2) . ? C6 C7 1.402(2) . ? C6 H6 0.9500 . ? C7 C8 1.5014(19) . ? C8 C13 1.3964(19) . ? C8 C9 1.3992(19) . ? C9 C10 1.385(2) . ? C9 H9 0.9500 . ? C10 C11 1.386(2) . ? C10 H10 0.9500 . ? C11 C12 1.4019(19) . ? C11 H11 0.9500 . ? C12 C13 1.3950(19) . ? C12 C14 1.4994(19) . ? C13 H13 0.9500 . ? C14 C15 1.404(2) . ? C15 C16 1.403(2) . ? C15 H15 0.9500 . ? C16 C17 1.537(2) . ? C17 C18 1.523(2) . ? C17 C19 1.533(2) . ? C17 C20 1.534(2) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? O5 C24 1.431(2) . ? O5 C21 1.440(2) . ? C21 C22 1.518(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.521(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.521(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? 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 O1 Cu1 O4 85.32(5) . 2 ? O1 Cu1 O2 92.70(5) . . ? O4 Cu1 O2 172.03(5) 2 . ? O1 Cu1 O3 171.87(5) . 2 ? O4 Cu1 O3 91.78(4) 2 2 ? O2 Cu1 O3 89.14(4) . 2 ? O1 Cu1 O5 92.90(5) . . ? O4 Cu1 O5 96.90(4) 2 . ? O2 Cu1 O5 90.91(5) . . ? O3 Cu1 O5 94.99(4) 2 . ? C5 O1 Cu1 127.37(10) . . ? C7 O2 Cu1 126.22(10) . . ? C14 O3 Cu1 126.09(9) . 2 ? C16 O4 Cu1 127.14(10) . 2 ? C4 C1 H1A 109.5 . . ? C4 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C2 H2A 109.5 . . ? C4 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 C1 110.33(14) . . ? C2 C4 C3 109.13(13) . . ? C1 C4 C3 108.99(15) . . ? C2 C4 C5 113.77(12) . . ? C1 C4 C5 106.17(13) . . ? C3 C4 C5 108.32(13) . . ? O1 C5 C6 124.71(13) . . ? O1 C5 C4 113.32(12) . . ? C6 C5 C4 121.91(13) . . ? C5 C6 C7 123.76(13) . . ? C5 C6 H6 118.1 . . ? C7 C6 H6 118.1 . . ? O2 C7 C6 125.22(13) . . ? O2 C7 C8 114.75(12) . . ? C6 C7 C8 120.02(12) . . ? C13 C8 C9 118.93(13) . . ? C13 C8 C7 117.83(12) . . ? C9 C8 C7 123.24(12) . . ? C10 C9 C8 120.30(13) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 120.33(13) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C10 C11 C12 120.60(13) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C13 C12 C11 118.52(13) . . ? C13 C12 C14 118.25(12) . . ? C11 C12 C14 123.23(13) . . ? C12 C13 C8 121.32(13) . . ? C12 C13 H13 119.3 . . ? C8 C13 H13 119.3 . . ? O3 C14 C15 124.99(13) . . ? O3 C14 C12 115.07(12) . . ? C15 C14 C12 119.94(12) . . ? C16 C15 C14 123.52(13) . . ? C16 C15 H15 118.2 . . ? C14 C15 H15 118.2 . . ? O4 C16 C15 124.49(13) . . ? O4 C16 C17 113.31(12) . . ? C15 C16 C17 122.19(13) . . ? C18 C17 C19 109.13(15) . . ? C18 C17 C20 109.20(15) . . ? C19 C17 C20 109.63(15) . . ? C18 C17 C16 114.13(13) . . ? C19 C17 C16 107.14(13) . . ? C20 C17 C16 107.53(13) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C24 O5 C21 105.95(14) . . ? C24 O5 Cu1 116.18(10) . . ? C21 O5 Cu1 113.57(10) . . ? O5 C21 C22 106.73(16) . . ? O5 C21 H21A 110.4 . . ? C22 C21 H21A 110.4 . . ? O5 C21 H21B 110.4 . . ? C22 C21 H21B 110.4 . . ? H21A C21 H21B 108.6 . . ? C21 C22 C23 104.70(16) . . ? C21 C22 H22A 110.8 . . ? C23 C22 H22A 110.8 . . ? C21 C22 H22B 110.8 . . ? C23 C22 H22B 110.8 . . ? H22A C22 H22B 108.9 . . ? C22 C23 C24 103.14(16) . . ? C22 C23 H23A 111.1 . . ? C24 C23 H23A 111.1 . . ? C22 C23 H23B 111.1 . . ? C24 C23 H23B 111.1 . . ? H23A C23 H23B 109.1 . . ? O5 C24 C23 103.99(15) . . ? O5 C24 H24A 111.0 . . ? C23 C24 H24A 111.0 . . ? O5 C24 H24B 111.0 . . ? C23 C24 H24B 111.0 . . ? H24A C24 H24B 109.0 . . ? 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 O4 Cu1 O1 C5 -171.22(13) 2 . . . ? O2 Cu1 O1 C5 1.05(13) . . . . ? O5 Cu1 O1 C5 92.09(13) . . . . ? O1 Cu1 O2 C7 -0.34(13) . . . . ? O3 Cu1 O2 C7 171.73(12) 2 . . . ? O5 Cu1 O2 C7 -93.29(12) . . . . ? Cu1 O1 C5 C6 -0.9(2) . . . . ? Cu1 O1 C5 C4 176.34(10) . . . . ? C2 C4 C5 O1 164.96(14) . . . . ? C1 C4 C5 O1 -73.50(17) . . . . ? C3 C4 C5 O1 43.43(18) . . . . ? C2 C4 C5 C6 -17.7(2) . . . . ? C1 C4 C5 C6 103.83(17) . . . . ? C3 C4 C5 C6 -139.25(15) . . . . ? O1 C5 C6 C7 -0.2(2) . . . . ? C4 C5 C6 C7 -177.26(13) . . . . ? Cu1 O2 C7 C6 -0.5(2) . . . . ? Cu1 O2 C7 C8 -179.74(9) . . . . ? C5 C6 C7 O2 1.0(2) . . . . ? C5 C6 C7 C8 -179.82(13) . . . . ? O2 C7 C8 C13 13.04(19) . . . . ? C6 C7 C8 C13 -166.22(13) . . . . ? O2 C7 C8 C9 -166.78(13) . . . . ? C6 C7 C8 C9 14.0(2) . . . . ? C13 C8 C9 C10 0.7(2) . . . . ? C7 C8 C9 C10 -179.46(13) . . . . ? C8 C9 C10 C11 -0.2(2) . . . . ? C9 C10 C11 C12 -0.6(2) . . . . ? C10 C11 C12 C13 1.0(2) . . . . ? C10 C11 C12 C14 -178.19(13) . . . . ? C11 C12 C13 C8 -0.5(2) . . . . ? C14 C12 C13 C8 178.74(13) . . . . ? C9 C8 C13 C12 -0.4(2) . . . . ? C7 C8 C13 C12 179.80(12) . . . . ? Cu1 O3 C14 C15 6.9(2) 2 . . . ? Cu1 O3 C14 C12 -172.09(9) 2 . . . ? C13 C12 C14 O3 14.56(19) . . . . ? C11 C12 C14 O3 -166.27(13) . . . . ? C13 C12 C14 C15 -164.51(13) . . . . ? C11 C12 C14 C15 14.7(2) . . . . ? O3 C14 C15 C16 2.7(2) . . . . ? C12 C14 C15 C16 -178.28(13) . . . . ? Cu1 O4 C16 C15 -11.0(2) 2 . . . ? Cu1 O4 C16 C17 170.19(10) 2 . . . ? C14 C15 C16 O4 -0.7(2) . . . . ? C14 C15 C16 C17 178.03(14) . . . . ? O4 C16 C17 C18 -177.11(15) . . . . ? C15 C16 C17 C18 4.0(2) . . . . ? O4 C16 C17 C19 61.96(18) . . . . ? C15 C16 C17 C19 -116.90(16) . . . . ? O4 C16 C17 C20 -55.82(18) . . . . ? C15 C16 C17 C20 125.32(16) . . . . ? O1 Cu1 O5 C24 79.47(11) . . . . ? O4 Cu1 O5 C24 -6.16(12) 2 . . . ? O2 Cu1 O5 C24 172.22(11) . . . . ? O3 Cu1 O5 C24 -98.57(11) 2 . . . ? O1 Cu1 O5 C21 -157.26(11) . . . . ? O4 Cu1 O5 C21 117.10(11) 2 . . . ? O2 Cu1 O5 C21 -64.52(11) . . . . ? O3 Cu1 O5 C21 24.70(11) 2 . . . ? C24 O5 C21 C22 29.52(19) . . . . ? Cu1 O5 C21 C22 -99.18(15) . . . . ? O5 C21 C22 C23 -6.8(2) . . . . ? C21 C22 C23 C24 -16.6(2) . . . . ? C21 O5 C24 C23 -40.24(17) . . . . ? Cu1 O5 C24 C23 86.91(15) . . . . ? C22 C23 C24 O5 34.71(19) . . . . ? _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.529 _refine_diff_density_min -0.563 _refine_diff_density_rms 0.057 data_lj46sad _database_code_depnum_ccdc_archive 'CCDC 258480' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C88 H104 Cu4 N4 O16, 4(C4 H8 O)' _chemical_formula_sum 'C104 H136 Cu4 N4 O20' _chemical_formula_weight 2016.33 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 37.359(3) _cell_length_b 14.9784(10) _cell_length_c 20.4038(14) _cell_angle_alpha 90.00 _cell_angle_beta 116.9050(10) _cell_angle_gamma 90.00 _cell_volume 10181.7(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 12709 _cell_measurement_theta_min 2.145 _cell_measurement_theta_max 27.625 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.59 _exptl_crystal_size_mid 0.53 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.315 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4256 _exptl_absorpt_coefficient_mu 0.893 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.625 _exptl_absorpt_correction_T_max 0.814 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 282 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.34 _diffrn_reflns_number 48373 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_sigmaI/netI 0.0450 _diffrn_reflns_limit_h_min -49 _diffrn_reflns_limit_h_max 49 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 28.32 _reflns_number_total 12117 _reflns_number_gt 8629 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1995)' _computing_cell_refinement 'SAINT (Bruker, 1995)' _computing_data_reduction 'SAINT and XPREP (Bruker, 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEPIII (Farrugia, 1997) WINGX-32 (Farrugia, 1999) ; _computing_publication_material 'enCIFer 1.0 (CCDC, 2003)' _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^)+(0.0562P)^2^+13.3390P] 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 12117 _refine_ls_number_parameters 607 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0729 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.1160 _refine_ls_wR_factor_gt 0.1002 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _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 0.143660(8) 0.408674(18) 0.587296(15) 0.02186(8) Uani 1 1 d . . . Cu2 Cu 0.357708(8) 0.448318(19) 0.668942(15) 0.02296(8) Uani 1 1 d . . . O1 O 0.11237(5) 0.33513(11) 0.61940(9) 0.0288(4) Uani 1 1 d . . . O2 O 0.19374(5) 0.36478(11) 0.66271(9) 0.0243(3) Uani 1 1 d . . . O3 O 0.32757(5) 0.38627(11) 0.70970(9) 0.0276(4) Uani 1 1 d . . . O4 O 0.40849(5) 0.41391(11) 0.74882(9) 0.0275(4) Uani 1 1 d . . . O5 O 0.09394(5) 0.46452(11) 0.52194(9) 0.0275(4) Uani 1 1 d . . . O6 O 0.17423(4) 0.48938(10) 0.55796(8) 0.0218(3) Uani 1 1 d . . . O7 O 0.30790(5) 0.50287(11) 0.60103(9) 0.0293(4) Uani 1 1 d . . . O8 O 0.38797(5) 0.51670(11) 0.63142(9) 0.0257(4) Uani 1 1 d . . . C1 C 0.06220(10) 0.1885(3) 0.59699(18) 0.0695(12) Uani 1 1 d . . . H1A H 0.0749 0.1473 0.5765 0.104 Uiso 1 1 calc R . . H1B H 0.0523 0.2409 0.5651 0.104 Uiso 1 1 calc R . . H1C H 0.0397 0.1584 0.6001 0.104 Uiso 1 1 calc R . . C2 C 0.07286(10) 0.2814(2) 0.7063(2) 0.0594(10) Uani 1 1 d . . . H2A H 0.0627 0.3340 0.6746 0.089 Uiso 1 1 calc R . . H2B H 0.0926 0.3001 0.7555 0.089 Uiso 1 1 calc R . . H2C H 0.0505 0.2507 0.7094 0.089 Uiso 1 1 calc R . . C3 C 0.10873(8) 0.1363(2) 0.72331(17) 0.0429(7) Uani 1 1 d . . . H3A H 0.0862 0.1040 0.7245 0.064 Uiso 1 1 calc R . . H3B H 0.1274 0.1556 0.7731 0.064 Uiso 1 1 calc R . . H3C H 0.1228 0.0970 0.7042 0.064 Uiso 1 1 calc R . . C4 C 0.09292(7) 0.21770(18) 0.67371(14) 0.0339(6) Uani 1 1 d . . . C5 C 0.12579(7) 0.27088(16) 0.66504(12) 0.0239(5) Uani 1 1 d . . . C6 C 0.16623(7) 0.24932(16) 0.70556(13) 0.0249(5) Uani 1 1 d . . . H6 H 0.1729 0.1990 0.7373 0.030 Uiso 1 1 calc R . . C7 C 0.19782(7) 0.29693(15) 0.70263(12) 0.0207(5) Uani 1 1 d . . . C8 C 0.24025(7) 0.26773(15) 0.74904(12) 0.0209(5) Uani 1 1 d . . . C9 C 0.25073(7) 0.19788(16) 0.79956(13) 0.0249(5) Uani 1 1 d . . . H9 H 0.2305 0.1682 0.8073 0.030 Uiso 1 1 calc R . . C10 C 0.29039(7) 0.17140(17) 0.83849(13) 0.0281(5) Uani 1 1 d . . . H10 H 0.2971 0.1232 0.8722 0.034 Uiso 1 1 calc R . . C11 C 0.32021(7) 0.21473(16) 0.82857(13) 0.0254(5) Uani 1 1 d . . . H11 H 0.3473 0.1961 0.8556 0.031 Uiso 1 1 calc R . . C12 C 0.31082(7) 0.28548(15) 0.77923(12) 0.0216(5) Uani 1 1 d . . . C13 C 0.27071(7) 0.31089(15) 0.73957(12) 0.0216(5) Uani 1 1 d . . . H13 H 0.2640 0.3586 0.7054 0.026 Uiso 1 1 calc R . . C14 C 0.34176(7) 0.33416(15) 0.76459(12) 0.0220(5) Uani 1 1 d . . . C15 C 0.38258(7) 0.31986(16) 0.81029(13) 0.0258(5) Uani 1 1 d . . . H15 H 0.3897 0.2801 0.8505 0.031 Uiso 1 1 calc R . . C16 C 0.41359(7) 0.36051(16) 0.80045(12) 0.0233(5) Uani 1 1 d . . . C17 C 0.45791(7) 0.34211(19) 0.85412(14) 0.0303(6) Uani 1 1 d . . . C18 C 0.47590(10) 0.4322(2) 0.89141(19) 0.0584(10) Uani 1 1 d . . . H18A H 0.4608 0.4547 0.9167 0.088 Uiso 1 1 calc R . . H18B H 0.4743 0.4754 0.8541 0.088 Uiso 1 1 calc R . . H18C H 0.5041 0.4236 0.9271 0.088 Uiso 1 1 calc R . . C19 C 0.47865(10) 0.3101(3) 0.80886(18) 0.0664(12) Uani 1 1 d . . . H19A H 0.5075 0.3035 0.8409 0.100 Uiso 1 1 calc R . . H19B H 0.4744 0.3539 0.7703 0.100 Uiso 1 1 calc R . . H19C H 0.4674 0.2524 0.7863 0.100 Uiso 1 1 calc R . . C20 C 0.46421(8) 0.2737(2) 0.91291(14) 0.0365(6) Uani 1 1 d . . . H20A H 0.4525 0.2166 0.8897 0.055 Uiso 1 1 calc R . . H20B H 0.4512 0.2942 0.9425 0.055 Uiso 1 1 calc R . . H20C H 0.4930 0.2660 0.9446 0.055 Uiso 1 1 calc R . . C21 C 0.02305(9) 0.4359(2) 0.3900(2) 0.0529(9) Uani 1 1 d . . . H21A H 0.0345 0.4034 0.3622 0.079 Uiso 1 1 calc R . . H21B H -0.0058 0.4446 0.3591 0.079 Uiso 1 1 calc R . . H21C H 0.0273 0.4015 0.4338 0.079 Uiso 1 1 calc R . . C22 C 0.02614(8) 0.5779(2) 0.45821(16) 0.0410(7) Uani 1 1 d . . . H22A H 0.0315 0.5441 0.5028 0.062 Uiso 1 1 calc R . . H22B H -0.0029 0.5848 0.4284 0.062 Uiso 1 1 calc R . . H22C H 0.0387 0.6369 0.4718 0.062 Uiso 1 1 calc R . . C23 C 0.03668(8) 0.5825(2) 0.34618(15) 0.0425(7) Uani 1 1 d . . . H23A H 0.0510 0.6395 0.3619 0.064 Uiso 1 1 calc R . . H23B H 0.0079 0.5938 0.3171 0.064 Uiso 1 1 calc R . . H23C H 0.0467 0.5499 0.3162 0.064 Uiso 1 1 calc R . . C24 C 0.04371(7) 0.52719(17) 0.41348(13) 0.0292(5) Uani 1 1 d . . . C25 C 0.08821(7) 0.50909(15) 0.46504(13) 0.0236(5) Uani 1 1 d . . . C26 C 0.11884(7) 0.54043(16) 0.44939(13) 0.0253(5) Uani 1 1 d . . . H26 H 0.1114 0.5690 0.4035 0.030 Uiso 1 1 calc R . . C27 C 0.15973(7) 0.53211(14) 0.49749(12) 0.0195(4) Uani 1 1 d . . . C28 C 0.19046(7) 0.57648(14) 0.47970(12) 0.0207(5) Uani 1 1 d . . . C29 C 0.18026(7) 0.63836(16) 0.42273(13) 0.0263(5) Uani 1 1 d . . . H29 H 0.1529 0.6536 0.3931 0.032 Uiso 1 1 calc R . . C30 C 0.20996(7) 0.67739(18) 0.40947(14) 0.0316(6) Uani 1 1 d . . . H30 H 0.2028 0.7196 0.3708 0.038 Uiso 1 1 calc R . . C31 C 0.24993(7) 0.65556(17) 0.45183(13) 0.0283(5) Uani 1 1 d . . . H31 H 0.2700 0.6826 0.4419 0.034 Uiso 1 1 calc R . . C32 C 0.26096(7) 0.59399(15) 0.50916(12) 0.0214(5) Uani 1 1 d . . . C33 C 0.23081(7) 0.55495(15) 0.52241(12) 0.0206(4) Uani 1 1 d . . . H33 H 0.2380 0.5130 0.5612 0.025 Uiso 1 1 calc R . . C34 C 0.30353(7) 0.56596(15) 0.55661(12) 0.0218(5) Uani 1 1 d . . . C35 C 0.33506(7) 0.60722(16) 0.54870(13) 0.0257(5) Uani 1 1 d . . . H35 H 0.3288 0.6574 0.5169 0.031 Uiso 1 1 calc R . . C36 C 0.37502(7) 0.57923(15) 0.58465(13) 0.0227(5) Uani 1 1 d . . . C37 C 0.40731(7) 0.62183(17) 0.56736(14) 0.0287(5) Uani 1 1 d . . . C38 C 0.39280(9) 0.70508(19) 0.51938(18) 0.0421(7) Uani 1 1 d . . . H38A H 0.3828 0.7486 0.5429 0.063 Uiso 1 1 calc R . . H38B H 0.3712 0.6888 0.4712 0.063 Uiso 1 1 calc R . . H38C H 0.4151 0.7313 0.5132 0.063 Uiso 1 1 calc R . . C39 C 0.41914(11) 0.5514(2) 0.5261(2) 0.0536(9) Uani 1 1 d . . . H39A H 0.3964 0.5400 0.4780 0.080 Uiso 1 1 calc R . . H39B H 0.4267 0.4959 0.5546 0.080 Uiso 1 1 calc R . . H39C H 0.4420 0.5732 0.5193 0.080 Uiso 1 1 calc R . . C40 C 0.44364(9) 0.6437(3) 0.63948(17) 0.0595(10) Uani 1 1 d . . . H40A H 0.4655 0.6651 0.6296 0.089 Uiso 1 1 calc R . . H40B H 0.4523 0.5900 0.6701 0.089 Uiso 1 1 calc R . . H40C H 0.4365 0.6902 0.6653 0.089 Uiso 1 1 calc R . . N1 N 0.14165(6) 0.30613(14) 0.49745(12) 0.0316(5) Uani 1 1 d . . . N2 N 0.14264(7) 0.17519(14) 0.40183(12) 0.0318(5) Uani 1 1 d . . . C41 C 0.10988(8) 0.25552(17) 0.45900(15) 0.0331(6) Uani 1 1 d . . . H41 H 0.0862 0.2642 0.4645 0.040 Uiso 1 1 calc R . . C42 C 0.11016(8) 0.19046(18) 0.41117(14) 0.0336(6) Uani 1 1 d . . . H42 H 0.0867 0.1559 0.3844 0.040 Uiso 1 1 calc R . . C43 C 0.17435(8) 0.22611(19) 0.44006(16) 0.0387(6) Uani 1 1 d . . . H43 H 0.1980 0.2175 0.4346 0.046 Uiso 1 1 calc R . . C44 C 0.17396(9) 0.29147(19) 0.48781(16) 0.0401(7) Uani 1 1 d . . . H44 H 0.1973 0.3265 0.5142 0.048 Uiso 1 1 calc R . . O1T O 0.07975(9) 0.4399(3) 0.23045(18) 0.0999(11) Uani 1 1 d . . . C1T C 0.09973(10) 0.4646(2) 0.1886(2) 0.0560(9) Uani 1 1 d . . . H1T H 0.0876 0.5190 0.1594 0.067 Uiso 1 1 calc R . . H2T H 0.0985 0.4159 0.1549 0.067 Uiso 1 1 calc R . . C2T C 0.14251(11) 0.4818(3) 0.2453(2) 0.0612(9) Uani 1 1 d . . . H3T H 0.1617 0.4700 0.2251 0.073 Uiso 1 1 calc R . . H4T H 0.1460 0.5439 0.2637 0.073 Uiso 1 1 calc R . . C3T C 0.14769(11) 0.4157(2) 0.30477(18) 0.0543(9) Uani 1 1 d . . . H5T H 0.1625 0.3623 0.3017 0.065 Uiso 1 1 calc R . . H6T H 0.1627 0.4431 0.3540 0.065 Uiso 1 1 calc R . . C4T C 0.10575(12) 0.3910(3) 0.2912(2) 0.0641(10) Uani 1 1 d . . . H7T H 0.1011 0.3263 0.2815 0.077 Uiso 1 1 calc R . . H8T H 0.1016 0.4061 0.3346 0.077 Uiso 1 1 calc R . . O2T O 0.20796(10) 0.1416(2) 0.60390(17) 0.0887(9) Uani 1 1 d . . . C5T C 0.17828(12) 0.0793(2) 0.58721(19) 0.0598(10) Uani 1 1 d . . . H9T H 0.1712 0.0523 0.5386 0.072 Uiso 1 1 calc R . . H10T H 0.1539 0.1074 0.5858 0.072 Uiso 1 1 calc R . . C6T C 0.19444(14) 0.0094(3) 0.6465(2) 0.0823(13) Uani 1 1 d . . . H11T H 0.1876 0.0238 0.6868 0.099 Uiso 1 1 calc R . . H12T H 0.1834 -0.0502 0.6264 0.099 Uiso 1 1 calc R . . C7T C 0.23853(13) 0.0115(3) 0.6728(2) 0.0766(13) Uani 1 1 d . . . H13T H 0.2481 -0.0449 0.6609 0.092 Uiso 1 1 calc R . . H14T H 0.2528 0.0213 0.7266 0.092 Uiso 1 1 calc R . . C8T C 0.24450(14) 0.0878(3) 0.6324(3) 0.0863(15) Uani 1 1 d . . . H15T H 0.2678 0.1240 0.6658 0.104 Uiso 1 1 calc R . . H16T H 0.2495 0.0660 0.5915 0.104 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01749(14) 0.02153(15) 0.02302(14) 0.00633(11) 0.00606(11) -0.00100(11) Cu2 0.01874(15) 0.02402(15) 0.02548(15) 0.00566(12) 0.00943(12) 0.00085(11) O1 0.0192(8) 0.0310(9) 0.0328(9) 0.0122(8) 0.0089(7) -0.0001(7) O2 0.0182(8) 0.0249(8) 0.0276(8) 0.0093(7) 0.0084(7) -0.0002(7) O3 0.0180(8) 0.0325(9) 0.0308(9) 0.0128(7) 0.0096(7) 0.0023(7) O4 0.0206(8) 0.0327(9) 0.0271(9) 0.0069(7) 0.0091(7) 0.0001(7) O5 0.0184(8) 0.0300(9) 0.0310(9) 0.0110(7) 0.0085(7) 0.0011(7) O6 0.0187(8) 0.0217(8) 0.0211(8) 0.0043(6) 0.0055(6) -0.0015(6) O7 0.0195(9) 0.0327(10) 0.0349(9) 0.0145(8) 0.0116(7) 0.0023(7) O8 0.0221(8) 0.0262(8) 0.0303(9) 0.0046(7) 0.0130(7) 0.0014(7) C1 0.050(2) 0.087(3) 0.0448(18) 0.0181(19) -0.0021(16) -0.043(2) C2 0.047(2) 0.059(2) 0.093(3) 0.031(2) 0.050(2) 0.0139(17) C3 0.0303(15) 0.0429(16) 0.0539(18) 0.0221(14) 0.0176(13) -0.0042(13) C4 0.0231(13) 0.0383(15) 0.0352(14) 0.0153(12) 0.0086(11) -0.0066(11) C5 0.0234(12) 0.0242(12) 0.0228(11) 0.0011(9) 0.0092(9) -0.0035(10) C6 0.0244(12) 0.0240(12) 0.0260(12) 0.0060(10) 0.0112(10) -0.0002(10) C7 0.0208(11) 0.0222(11) 0.0188(10) 0.0000(9) 0.0087(9) -0.0004(9) C8 0.0217(11) 0.0207(11) 0.0205(10) 0.0014(9) 0.0098(9) 0.0006(9) C9 0.0243(12) 0.0268(12) 0.0269(12) 0.0058(10) 0.0145(10) 0.0016(10) C10 0.0275(13) 0.0293(13) 0.0272(12) 0.0107(10) 0.0121(10) 0.0048(10) C11 0.0202(12) 0.0286(12) 0.0250(11) 0.0049(10) 0.0080(10) 0.0046(10) C12 0.0198(11) 0.0232(11) 0.0207(10) 0.0002(9) 0.0082(9) 0.0009(9) C13 0.0221(11) 0.0208(11) 0.0201(10) 0.0041(9) 0.0081(9) 0.0010(9) C14 0.0209(11) 0.0218(11) 0.0231(11) 0.0010(9) 0.0098(9) 0.0021(9) C15 0.0216(12) 0.0273(12) 0.0258(12) 0.0073(10) 0.0082(10) 0.0040(10) C16 0.0208(12) 0.0248(12) 0.0227(11) -0.0017(9) 0.0085(9) 0.0036(9) C17 0.0164(12) 0.0433(15) 0.0289(12) 0.0084(11) 0.0083(10) 0.0026(11) C18 0.0370(18) 0.058(2) 0.0534(19) 0.0091(17) -0.0035(15) -0.0170(16) C19 0.0381(18) 0.125(3) 0.0445(18) 0.024(2) 0.0259(15) 0.037(2) C20 0.0215(13) 0.0490(17) 0.0341(14) 0.0119(13) 0.0082(11) 0.0055(12) C21 0.0236(15) 0.0434(17) 0.070(2) -0.0048(16) 0.0019(14) -0.0087(13) C22 0.0301(15) 0.0518(18) 0.0416(16) 0.0138(14) 0.0166(13) 0.0132(13) C23 0.0246(14) 0.063(2) 0.0311(14) 0.0148(14) 0.0045(11) 0.0073(13) C24 0.0176(12) 0.0320(13) 0.0294(12) 0.0059(11) 0.0032(10) 0.0002(10) C25 0.0202(12) 0.0202(11) 0.0244(11) 0.0012(9) 0.0048(10) -0.0002(9) C26 0.0221(12) 0.0277(13) 0.0215(11) 0.0048(10) 0.0058(9) -0.0008(10) C27 0.0222(11) 0.0143(10) 0.0203(10) -0.0005(8) 0.0081(9) 0.0006(9) C28 0.0217(11) 0.0180(11) 0.0201(10) -0.0004(9) 0.0076(9) -0.0008(9) C29 0.0216(12) 0.0289(13) 0.0246(11) 0.0064(10) 0.0071(10) 0.0022(10) C30 0.0291(13) 0.0349(14) 0.0294(13) 0.0140(11) 0.0121(11) 0.0025(11) C31 0.0265(13) 0.0318(13) 0.0307(13) 0.0076(11) 0.0165(11) -0.0015(10) C32 0.0224(11) 0.0192(11) 0.0232(11) 0.0001(9) 0.0110(9) -0.0002(9) C33 0.0239(12) 0.0182(11) 0.0195(10) 0.0011(9) 0.0096(9) 0.0001(9) C34 0.0222(12) 0.0215(11) 0.0226(11) 0.0014(9) 0.0110(9) 0.0012(9) C35 0.0257(12) 0.0228(12) 0.0300(12) 0.0062(10) 0.0139(10) 0.0008(10) C36 0.0243(12) 0.0208(11) 0.0263(11) -0.0025(9) 0.0143(10) -0.0020(9) C37 0.0235(12) 0.0327(13) 0.0354(13) 0.0039(11) 0.0182(11) -0.0008(10) C38 0.0373(16) 0.0376(16) 0.0626(19) 0.0166(14) 0.0325(15) 0.0018(13) C39 0.064(2) 0.0435(18) 0.084(2) 0.0065(17) 0.060(2) 0.0070(16) C40 0.0388(18) 0.085(3) 0.0473(18) 0.0106(18) 0.0126(15) -0.0292(18) N1 0.0310(12) 0.0265(11) 0.0338(11) -0.0023(9) 0.0115(10) -0.0009(9) N2 0.0345(12) 0.0266(11) 0.0332(11) -0.0013(9) 0.0144(10) -0.0007(9) C41 0.0315(14) 0.0267(13) 0.0416(15) -0.0031(11) 0.0169(12) -0.0015(11) C42 0.0310(14) 0.0308(14) 0.0362(14) -0.0037(11) 0.0127(12) -0.0033(11) C43 0.0332(15) 0.0369(15) 0.0490(16) -0.0061(13) 0.0212(13) -0.0044(12) C44 0.0330(15) 0.0358(15) 0.0500(17) -0.0129(13) 0.0175(13) -0.0091(12) O1T 0.0576(18) 0.149(3) 0.089(2) 0.051(2) 0.0292(17) 0.0054(19) C1T 0.050(2) 0.055(2) 0.058(2) 0.0077(17) 0.0195(17) -0.0019(16) C2T 0.061(2) 0.053(2) 0.064(2) 0.0001(18) 0.0240(19) 0.0004(18) C3T 0.058(2) 0.051(2) 0.0470(18) -0.0078(16) 0.0182(16) 0.0047(17) C4T 0.078(3) 0.059(2) 0.057(2) -0.0004(18) 0.032(2) 0.000(2) O2T 0.109(2) 0.0656(18) 0.081(2) 0.0069(16) 0.0340(19) -0.0065(18) C5T 0.070(2) 0.0384(18) 0.051(2) -0.0062(15) 0.0101(18) -0.0018(17) C6T 0.100(4) 0.064(3) 0.069(3) 0.011(2) 0.026(3) -0.014(2) C7T 0.090(3) 0.052(2) 0.064(2) -0.010(2) 0.014(2) 0.019(2) C8T 0.081(3) 0.074(3) 0.121(4) -0.036(3) 0.061(3) -0.013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O5 1.9200(16) . ? Cu1 O2 1.9222(15) . ? Cu1 O1 1.9240(16) . ? Cu1 O6 1.9346(15) . ? Cu1 N1 2.366(2) . ? Cu2 O3 1.9160(16) . ? Cu2 O8 1.9227(16) . ? Cu2 O7 1.9278(16) . ? Cu2 O4 1.9295(16) . ? Cu2 N2 2.343(2) 7_556 ? O1 C5 1.274(3) . ? O2 C7 1.268(3) . ? O3 C14 1.268(3) . ? O4 C16 1.267(3) . ? O5 C25 1.271(3) . ? O6 C27 1.273(3) . ? O7 C34 1.268(3) . ? O8 C36 1.266(3) . ? C1 C4 1.528(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C4 1.537(4) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.522(4) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.539(3) . ? C5 C6 1.393(3) . ? C6 C7 1.403(3) . ? C6 H6 0.9500 . ? C7 C8 1.498(3) . ? C8 C9 1.395(3) . ? C8 C13 1.396(3) . ? C9 C10 1.385(3) . ? C9 H9 0.9500 . ? C10 C11 1.381(3) . ? C10 H10 0.9500 . ? C11 C12 1.393(3) . ? C11 H11 0.9500 . ? C12 C13 1.396(3) . ? C12 C14 1.506(3) . ? C13 H13 0.9500 . ? C14 C15 1.398(3) . ? C15 C16 1.401(3) . ? C15 H15 0.9500 . ? C16 C17 1.541(3) . ? C17 C20 1.513(4) . ? C17 C19 1.527(4) . ? C17 C18 1.545(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C24 1.536(4) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.543(4) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.522(4) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.537(3) . ? C25 C26 1.401(3) . ? C26 C27 1.398(3) . ? C26 H26 0.9500 . ? C27 C28 1.506(3) . ? C28 C33 1.395(3) . ? C28 C29 1.398(3) . ? C29 C30 1.385(3) . ? C29 H29 0.9500 . ? C30 C31 1.384(3) . ? C30 H30 0.9500 . ? C31 C32 1.397(3) . ? C31 H31 0.9500 . ? C32 C33 1.400(3) . ? C32 C34 1.500(3) . ? C33 H33 0.9500 . ? C34 C35 1.403(3) . ? C35 C36 1.397(3) . ? C35 H35 0.9500 . ? C36 C37 1.540(3) . ? C37 C40 1.519(4) . ? C37 C38 1.525(4) . ? C37 C39 1.534(4) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? N1 C41 1.325(3) . ? N1 C44 1.327(3) . ? N2 C43 1.326(3) . ? N2 C42 1.331(3) . ? N2 Cu2 2.343(2) 7_556 ? C41 C42 1.383(4) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.386(4) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? O1T C4T 1.388(4) . ? O1T C1T 1.414(4) . ? C1T C2T 1.512(5) . ? C1T H1T 0.9900 . ? C1T H2T 0.9900 . ? C2T C3T 1.509(5) . ? C2T H3T 0.9900 . ? C2T H4T 0.9900 . ? C3T C4T 1.509(5) . ? C3T H5T 0.9900 . ? C3T H6T 0.9900 . ? C4T H7T 0.9900 . ? C4T H8T 0.9900 . ? O2T C5T 1.369(4) . ? O2T C8T 1.460(5) . ? C5T C6T 1.504(5) . ? C5T H9T 0.9900 . ? C5T H10T 0.9900 . ? C6T C7T 1.484(6) . ? C6T H11T 0.9900 . ? C6T H12T 0.9900 . ? C7T C8T 1.485(6) . ? C7T H13T 0.9900 . ? C7T H14T 0.9900 . ? C8T H15T 0.9900 . ? C8T H16T 0.9900 . ? 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 O5 Cu1 O2 172.00(7) . . ? O5 Cu1 O1 86.57(7) . . ? O2 Cu1 O1 93.03(7) . . ? O5 Cu1 O6 91.94(7) . . ? O2 Cu1 O6 87.96(6) . . ? O1 Cu1 O6 176.16(7) . . ? O5 Cu1 N1 93.62(8) . . ? O2 Cu1 N1 94.38(7) . . ? O1 Cu1 N1 94.64(8) . . ? O6 Cu1 N1 88.98(7) . . ? O3 Cu2 O8 176.58(7) . . ? O3 Cu2 O7 87.24(7) . . ? O8 Cu2 O7 92.19(7) . . ? O3 Cu2 O4 92.88(7) . . ? O8 Cu2 O4 87.02(7) . . ? O7 Cu2 O4 168.71(8) . . ? O3 Cu2 N2 92.53(8) . 7_556 ? O8 Cu2 N2 90.88(7) . 7_556 ? O7 Cu2 N2 99.05(8) . 7_556 ? O4 Cu2 N2 92.22(8) . 7_556 ? C5 O1 Cu1 125.65(15) . . ? C7 O2 Cu1 125.38(15) . . ? C14 O3 Cu2 126.08(15) . . ? C16 O4 Cu2 126.26(15) . . ? C25 O5 Cu1 125.01(15) . . ? C27 O6 Cu1 124.20(14) . . ? C34 O7 Cu2 126.87(15) . . ? C36 O8 Cu2 126.95(15) . . ? C4 C1 H1A 109.5 . . ? C4 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C2 H2A 109.5 . . ? C4 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C3 C4 C1 109.7(3) . . ? C3 C4 C2 109.2(2) . . ? C1 C4 C2 109.5(3) . . ? C3 C4 C5 113.6(2) . . ? C1 C4 C5 107.4(2) . . ? C2 C4 C5 107.4(2) . . ? O1 C5 C6 124.9(2) . . ? O1 C5 C4 113.9(2) . . ? C6 C5 C4 121.3(2) . . ? C5 C6 C7 124.3(2) . . ? C5 C6 H6 117.8 . . ? C7 C6 H6 117.8 . . ? O2 C7 C6 125.2(2) . . ? O2 C7 C8 115.18(19) . . ? C6 C7 C8 119.7(2) . . ? C9 C8 C13 118.4(2) . . ? C9 C8 C7 123.3(2) . . ? C13 C8 C7 118.2(2) . . ? C10 C9 C8 120.6(2) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C11 C10 C9 120.4(2) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 C12 120.5(2) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C11 C12 C13 118.7(2) . . ? C11 C12 C14 123.1(2) . . ? C13 C12 C14 118.2(2) . . ? C12 C13 C8 121.5(2) . . ? C12 C13 H13 119.3 . . ? C8 C13 H13 119.3 . . ? O3 C14 C15 125.3(2) . . ? O3 C14 C12 114.92(19) . . ? C15 C14 C12 119.8(2) . . ? C14 C15 C16 124.1(2) . . ? C14 C15 H15 117.9 . . ? C16 C15 H15 117.9 . . ? O4 C16 C15 124.8(2) . . ? O4 C16 C17 114.4(2) . . ? C15 C16 C17 120.8(2) . . ? C20 C17 C19 109.1(2) . . ? C20 C17 C16 114.6(2) . . ? C19 C17 C16 107.6(2) . . ? C20 C17 C18 108.9(2) . . ? C19 C17 C18 110.2(3) . . ? C16 C17 C18 106.4(2) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C24 C21 H21A 109.5 . . ? C24 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C24 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C24 C22 H22A 109.5 . . ? C24 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C24 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C23 C24 C21 110.3(2) . . ? C23 C24 C25 113.9(2) . . ? C21 C24 C25 107.0(2) . . ? C23 C24 C22 108.7(2) . . ? C21 C24 C22 109.5(2) . . ? C25 C24 C22 107.4(2) . . ? O5 C25 C26 124.5(2) . . ? O5 C25 C24 113.6(2) . . ? C26 C25 C24 121.8(2) . . ? C27 C26 C25 123.8(2) . . ? C27 C26 H26 118.1 . . ? C25 C26 H26 118.1 . . ? O6 C27 C26 125.1(2) . . ? O6 C27 C28 114.77(19) . . ? C26 C27 C28 120.09(19) . . ? C33 C28 C29 118.9(2) . . ? C33 C28 C27 118.25(19) . . ? C29 C28 C27 122.8(2) . . ? C30 C29 C28 120.1(2) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C31 C30 C29 120.8(2) . . ? C31 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C30 C31 C32 120.3(2) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C31 C32 C33 118.6(2) . . ? C31 C32 C34 123.4(2) . . ? C33 C32 C34 118.0(2) . . ? C28 C33 C32 121.3(2) . . ? C28 C33 H33 119.4 . . ? C32 C33 H33 119.4 . . ? O7 C34 C35 124.6(2) . . ? O7 C34 C32 115.2(2) . . ? C35 C34 C32 120.2(2) . . ? C36 C35 C34 124.1(2) . . ? C36 C35 H35 117.9 . . ? C34 C35 H35 117.9 . . ? O8 C36 C35 124.8(2) . . ? O8 C36 C37 114.0(2) . . ? C35 C36 C37 121.1(2) . . ? C40 C37 C38 110.3(2) . . ? C40 C37 C39 109.1(3) . . ? C38 C37 C39 108.5(2) . . ? C40 C37 C36 108.5(2) . . ? C38 C37 C36 113.4(2) . . ? C39 C37 C36 106.9(2) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C41 N1 C44 116.7(2) . . ? C41 N1 Cu1 122.40(18) . . ? C44 N1 Cu1 120.69(18) . . ? C43 N2 C42 116.5(2) . . ? C43 N2 Cu2 124.83(18) . 7_556 ? C42 N2 Cu2 118.23(17) . 7_556 ? N1 C41 C42 122.0(2) . . ? N1 C41 H41 119.0 . . ? C42 C41 H41 119.0 . . ? N2 C42 C41 121.4(2) . . ? N2 C42 H42 119.3 . . ? C41 C42 H42 119.3 . . ? N2 C43 C44 122.0(3) . . ? N2 C43 H43 119.0 . . ? C44 C43 H43 119.0 . . ? N1 C44 C43 121.4(3) . . ? N1 C44 H44 119.3 . . ? C43 C44 H44 119.3 . . ? C4T O1T C1T 109.3(3) . . ? O1T C1T C2T 104.3(3) . . ? O1T C1T H1T 110.9 . . ? C2T C1T H1T 110.9 . . ? O1T C1T H2T 110.9 . . ? C2T C1T H2T 110.9 . . ? H1T C1T H2T 108.9 . . ? C3T C2T C1T 102.1(3) . . ? C3T C2T H3T 111.3 . . ? C1T C2T H3T 111.3 . . ? C3T C2T H4T 111.3 . . ? C1T C2T H4T 111.3 . . ? H3T C2T H4T 109.2 . . ? C4T C3T C2T 105.6(3) . . ? C4T C3T H5T 110.6 . . ? C2T C3T H5T 110.6 . . ? C4T C3T H6T 110.6 . . ? C2T C3T H6T 110.6 . . ? H5T C3T H6T 108.8 . . ? O1T C4T C3T 106.5(3) . . ? O1T C4T H7T 110.4 . . ? C3T C4T H7T 110.4 . . ? O1T C4T H8T 110.4 . . ? C3T C4T H8T 110.4 . . ? H7T C4T H8T 108.6 . . ? C5T O2T C8T 103.2(3) . . ? O2T C5T C6T 106.8(3) . . ? O2T C5T H9T 110.4 . . ? C6T C5T H9T 110.4 . . ? O2T C5T H10T 110.4 . . ? C6T C5T H10T 110.4 . . ? H9T C5T H10T 108.6 . . ? C7T C6T C5T 104.6(4) . . ? C7T C6T H11T 110.8 . . ? C5T C6T H11T 110.8 . . ? C7T C6T H12T 110.8 . . ? C5T C6T H12T 110.8 . . ? H11T C6T H12T 108.9 . . ? C6T C7T C8T 103.6(3) . . ? C6T C7T H13T 111.0 . . ? C8T C7T H13T 111.0 . . ? C6T C7T H14T 111.0 . . ? C8T C7T H14T 111.0 . . ? H13T C7T H14T 109.0 . . ? O2T C8T C7T 107.4(3) . . ? O2T C8T H15T 110.2 . . ? C7T C8T H15T 110.2 . . ? O2T C8T H16T 110.2 . . ? C7T C8T H16T 110.2 . . ? H15T C8T H16T 108.5 . . ? 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 O5 Cu1 O1 C5 175.8(2) . . . . ? O2 Cu1 O1 C5 -12.3(2) . . . . ? N1 Cu1 O1 C5 82.4(2) . . . . ? O1 Cu1 O2 C7 12.98(19) . . . . ? O6 Cu1 O2 C7 -170.73(18) . . . . ? N1 Cu1 O2 C7 -81.91(19) . . . . ? O7 Cu2 O3 C14 -177.0(2) . . . . ? O4 Cu2 O3 C14 -8.3(2) . . . . ? N2 Cu2 O3 C14 84.0(2) 7_556 . . . ? O3 Cu2 O4 C16 6.4(2) . . . . ? O8 Cu2 O4 C16 -177.07(19) . . . . ? O7 Cu2 O4 C16 96.7(4) . . . . ? N2 Cu2 O4 C16 -86.30(19) 7_556 . . . ? O1 Cu1 O5 C25 -160.16(19) . . . . ? O6 Cu1 O5 C25 23.38(19) . . . . ? N1 Cu1 O5 C25 -65.72(19) . . . . ? O5 Cu1 O6 C27 -22.27(17) . . . . ? O2 Cu1 O6 C27 165.74(17) . . . . ? N1 Cu1 O6 C27 71.32(17) . . . . ? O3 Cu2 O7 C34 171.3(2) . . . . ? O8 Cu2 O7 C34 -5.3(2) . . . . ? O4 Cu2 O7 C34 80.4(4) . . . . ? N2 Cu2 O7 C34 -96.6(2) 7_556 . . . ? O7 Cu2 O8 C36 6.62(19) . . . . ? O4 Cu2 O8 C36 -162.11(19) . . . . ? N2 Cu2 O8 C36 105.71(19) 7_556 . . . ? Cu1 O1 C5 C6 7.5(3) . . . . ? Cu1 O1 C5 C4 -173.68(16) . . . . ? C3 C4 C5 O1 175.1(2) . . . . ? C1 C4 C5 O1 53.6(3) . . . . ? C2 C4 C5 O1 -64.1(3) . . . . ? C3 C4 C5 C6 -6.0(4) . . . . ? C1 C4 C5 C6 -127.5(3) . . . . ? C2 C4 C5 C6 114.8(3) . . . . ? O1 C5 C6 C7 1.4(4) . . . . ? C4 C5 C6 C7 -177.4(2) . . . . ? Cu1 O2 C7 C6 -9.1(3) . . . . ? Cu1 O2 C7 C8 170.69(14) . . . . ? C5 C6 C7 O2 -0.5(4) . . . . ? C5 C6 C7 C8 179.7(2) . . . . ? O2 C7 C8 C9 176.0(2) . . . . ? C6 C7 C8 C9 -4.2(3) . . . . ? O2 C7 C8 C13 -6.0(3) . . . . ? C6 C7 C8 C13 173.8(2) . . . . ? C13 C8 C9 C10 -0.9(3) . . . . ? C7 C8 C9 C10 177.1(2) . . . . ? C8 C9 C10 C11 0.9(4) . . . . ? C9 C10 C11 C12 -0.1(4) . . . . ? C10 C11 C12 C13 -0.7(3) . . . . ? C10 C11 C12 C14 -178.6(2) . . . . ? C11 C12 C13 C8 0.7(3) . . . . ? C14 C12 C13 C8 178.7(2) . . . . ? C9 C8 C13 C12 0.1(3) . . . . ? C7 C8 C13 C12 -178.0(2) . . . . ? Cu2 O3 C14 C15 7.3(3) . . . . ? Cu2 O3 C14 C12 -172.77(15) . . . . ? C11 C12 C14 O3 168.6(2) . . . . ? C13 C12 C14 O3 -9.3(3) . . . . ? C11 C12 C14 C15 -11.4(3) . . . . ? C13 C12 C14 C15 170.7(2) . . . . ? O3 C14 C15 C16 -1.3(4) . . . . ? C12 C14 C15 C16 178.7(2) . . . . ? Cu2 O4 C16 C15 -3.1(3) . . . . ? Cu2 O4 C16 C17 176.85(16) . . . . ? C14 C15 C16 O4 -0.9(4) . . . . ? C14 C15 C16 C17 179.1(2) . . . . ? O4 C16 C17 C20 -176.1(2) . . . . ? C15 C16 C17 C20 3.9(3) . . . . ? O4 C16 C17 C19 -54.6(3) . . . . ? C15 C16 C17 C19 125.4(3) . . . . ? O4 C16 C17 C18 63.5(3) . . . . ? C15 C16 C17 C18 -116.5(3) . . . . ? Cu1 O5 C25 C26 -14.1(3) . . . . ? Cu1 O5 C25 C24 166.37(16) . . . . ? C23 C24 C25 O5 178.6(2) . . . . ? C21 C24 C25 O5 -59.4(3) . . . . ? C22 C24 C25 O5 58.2(3) . . . . ? C23 C24 C25 C26 -0.9(4) . . . . ? C21 C24 C25 C26 121.1(3) . . . . ? C22 C24 C25 C26 -121.3(3) . . . . ? O5 C25 C26 C27 -5.0(4) . . . . ? C24 C25 C26 C27 174.4(2) . . . . ? Cu1 O6 C27 C26 12.1(3) . . . . ? Cu1 O6 C27 C28 -168.48(14) . . . . ? C25 C26 C27 O6 6.0(4) . . . . ? C25 C26 C27 C28 -173.4(2) . . . . ? O6 C27 C28 C33 10.9(3) . . . . ? C26 C27 C28 C33 -169.7(2) . . . . ? O6 C27 C28 C29 -168.8(2) . . . . ? C26 C27 C28 C29 10.6(3) . . . . ? C33 C28 C29 C30 -0.1(4) . . . . ? C27 C28 C29 C30 179.5(2) . . . . ? C28 C29 C30 C31 0.4(4) . . . . ? C29 C30 C31 C32 -0.4(4) . . . . ? C30 C31 C32 C33 0.3(4) . . . . ? C30 C31 C32 C34 179.0(2) . . . . ? C29 C28 C33 C32 0.0(3) . . . . ? C27 C28 C33 C32 -179.7(2) . . . . ? C31 C32 C33 C28 0.0(3) . . . . ? C34 C32 C33 C28 -178.8(2) . . . . ? Cu2 O7 C34 C35 0.7(3) . . . . ? Cu2 O7 C34 C32 178.93(15) . . . . ? C31 C32 C34 O7 -173.0(2) . . . . ? C33 C32 C34 O7 5.8(3) . . . . ? C31 C32 C34 C35 5.3(3) . . . . ? C33 C32 C34 C35 -175.9(2) . . . . ? O7 C34 C35 C36 5.4(4) . . . . ? C32 C34 C35 C36 -172.8(2) . . . . ? Cu2 O8 C36 C35 -3.3(3) . . . . ? Cu2 O8 C36 C37 178.83(15) . . . . ? C34 C35 C36 O8 -4.0(4) . . . . ? C34 C35 C36 C37 173.8(2) . . . . ? O8 C36 C37 C40 -49.0(3) . . . . ? C35 C36 C37 C40 133.0(3) . . . . ? O8 C36 C37 C38 -172.0(2) . . . . ? C35 C36 C37 C38 10.1(3) . . . . ? O8 C36 C37 C39 68.5(3) . . . . ? C35 C36 C37 C39 -109.5(3) . . . . ? O5 Cu1 N1 C41 -51.8(2) . . . . ? O2 Cu1 N1 C41 128.5(2) . . . . ? O1 Cu1 N1 C41 35.1(2) . . . . ? O6 Cu1 N1 C41 -143.6(2) . . . . ? O5 Cu1 N1 C44 134.0(2) . . . . ? O2 Cu1 N1 C44 -45.7(2) . . . . ? O1 Cu1 N1 C44 -139.2(2) . . . . ? O6 Cu1 N1 C44 42.1(2) . . . . ? C44 N1 C41 C42 0.1(4) . . . . ? Cu1 N1 C41 C42 -174.38(19) . . . . ? C43 N2 C42 C41 -0.7(4) . . . . ? Cu2 N2 C42 C41 172.35(19) 7_556 . . . ? N1 C41 C42 N2 0.4(4) . . . . ? C42 N2 C43 C44 0.5(4) . . . . ? Cu2 N2 C43 C44 -172.0(2) 7_556 . . . ? C41 N1 C44 C43 -0.3(4) . . . . ? Cu1 N1 C44 C43 174.3(2) . . . . ? N2 C43 C44 N1 0.0(5) . . . . ? C4T O1T C1T C2T -35.4(4) . . . . ? O1T C1T C2T C3T 32.6(4) . . . . ? C1T C2T C3T C4T -19.2(4) . . . . ? C1T O1T C4T C3T 22.7(4) . . . . ? C2T C3T C4T O1T -0.8(4) . . . . ? C8T O2T C5T C6T 38.1(4) . . . . ? O2T C5T C6T C7T -27.8(5) . . . . ? C5T C6T C7T C8T 5.5(4) . . . . ? C5T O2T C8T C7T -34.7(4) . . . . ? C6T C7T C8T O2T 16.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.053 _refine_diff_density_min -0.521 _refine_diff_density_rms 0.074 data_lj37sad _database_code_depnum_ccdc_archive 'CCDC 258481' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H72 Fe2 O12, C4 H10 O' _chemical_formula_sum 'C64 H82 Fe2 O13' _chemical_formula_weight 1171.00 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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 17.6982(15) _cell_length_b 19.0959(16) _cell_length_c 20.1570(17) _cell_angle_alpha 90.00 _cell_angle_beta 111.6490(10) _cell_angle_gamma 90.00 _cell_volume 6331.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 18303 _cell_measurement_theta_min 2.174 _cell_measurement_theta_max 28.117 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.175 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.228 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2488 _exptl_absorpt_coefficient_mu 0.517 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.740 _exptl_absorpt_correction_T_max 0.913 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 375 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.21 _diffrn_reflns_number 61704 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 28.35 _reflns_number_total 15183 _reflns_number_gt 11008 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT and XPREP (Siemens, 1995)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEP-3 (Farrugia, 1997) WINGX-32 (Farrugia, 1999) ; _computing_publication_material 'enCIFer (CCDC, 2003)' _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^)+(0.0732P)^2^+2.8411P] 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 15183 _refine_ls_number_parameters 730 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0720 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1334 _refine_ls_wR_factor_gt 0.1159 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 Fe1 Fe 0.803695(17) 0.288346(16) 0.218743(16) 0.02511(8) Uani 1 1 d . . . Fe2 Fe 0.379984(17) 0.190201(16) 0.082750(16) 0.02479(8) Uani 1 1 d . . . O1 O 0.86807(9) 0.34436(8) 0.30302(8) 0.0293(3) Uani 1 1 d . . . O2 O 0.72903(9) 0.27125(8) 0.26996(8) 0.0285(3) Uani 1 1 d . . . O3 O 0.45631(9) 0.21156(8) 0.18087(8) 0.0289(3) Uani 1 1 d . . . O4 O 0.32421(9) 0.12813(8) 0.12878(8) 0.0295(3) Uani 1 1 d . . . O5 O 0.87515(9) 0.32292(9) 0.16860(8) 0.0330(4) Uani 1 1 d . . . O6 O 0.72260(8) 0.35584(8) 0.15619(8) 0.0274(3) Uani 1 1 d . . . O7 O 0.43938(9) 0.26355(8) 0.04872(8) 0.0287(3) Uani 1 1 d . . . O8 O 0.30071(9) 0.26609(8) 0.07641(8) 0.0300(3) Uani 1 1 d . . . O9 O 0.88412(9) 0.21121(8) 0.25848(8) 0.0311(3) Uani 1 1 d . . . O10 O 0.74105(9) 0.21602(8) 0.14674(8) 0.0282(3) Uani 1 1 d . . . O11 O 0.46068(8) 0.12515(8) 0.06980(8) 0.0261(3) Uani 1 1 d . . . O12 O 0.30595(9) 0.15743(8) -0.01371(8) 0.0314(3) Uani 1 1 d . . . C1 C 0.97460(14) 0.43879(12) 0.39002(14) 0.0381(5) Uani 1 1 d . . . H1A H 0.9366 0.4783 0.3790 0.057 Uiso 1 1 calc R . . H1B H 0.9808 0.4226 0.3462 0.057 Uiso 1 1 calc R . . H1C H 1.0275 0.4538 0.4244 0.057 Uiso 1 1 calc R . . C2 C 0.92795(15) 0.40441(14) 0.48881(13) 0.0397(6) Uani 1 1 d . . . H2A H 0.8868 0.4415 0.4756 0.060 Uiso 1 1 calc R . . H2B H 0.9791 0.4228 0.5233 0.060 Uiso 1 1 calc R . . H2C H 0.9093 0.3653 0.5103 0.060 Uiso 1 1 calc R . . C3 C 1.00388(14) 0.31863(12) 0.44188(14) 0.0362(5) Uani 1 1 d . . . H3A H 1.0555 0.3351 0.4772 0.054 Uiso 1 1 calc R . . H3B H 1.0125 0.3028 0.3990 0.054 Uiso 1 1 calc R . . H3C H 0.9833 0.2797 0.4620 0.054 Uiso 1 1 calc R . . C4 C 0.94158(12) 0.37894(11) 0.42220(12) 0.0270(4) Uani 1 1 d . . . C5 C 0.86473(12) 0.34847(10) 0.36502(11) 0.0230(4) Uani 1 1 d . . . C6 C 0.79890(12) 0.32479(11) 0.38120(11) 0.0263(4) Uani 1 1 d . . . H6 H 0.7990 0.3333 0.4277 0.032 Uiso 1 1 calc R . . C7 C 0.73276(12) 0.28907(10) 0.33197(11) 0.0225(4) Uani 1 1 d . . . C8 C 0.66010(12) 0.26932(10) 0.34917(11) 0.0233(4) Uani 1 1 d . . . C9 C 0.65706(13) 0.27427(11) 0.41727(11) 0.0281(4) Uani 1 1 d . . . H9 H 0.7033 0.2901 0.4562 0.034 Uiso 1 1 calc R . . C10 C 0.58670(14) 0.25622(12) 0.42830(12) 0.0312(5) Uani 1 1 d . . . H10 H 0.5850 0.2601 0.4747 0.037 Uiso 1 1 calc R . . C11 C 0.51883(13) 0.23254(11) 0.37224(11) 0.0284(4) Uani 1 1 d . . . H11 H 0.4707 0.2209 0.3803 0.034 Uiso 1 1 calc R . . C12 C 0.52105(12) 0.22585(10) 0.30407(11) 0.0236(4) Uani 1 1 d . . . C13 C 0.59187(12) 0.24508(11) 0.29340(11) 0.0238(4) Uani 1 1 d . . . H13 H 0.5935 0.2415 0.2469 0.029 Uiso 1 1 calc R . . C14 C 0.45203(12) 0.19848(11) 0.24117(11) 0.0247(4) Uani 1 1 d . . . C15 C 0.38958(13) 0.15894(12) 0.25004(12) 0.0311(5) Uani 1 1 d . . . H15 H 0.3886 0.1545 0.2967 0.037 Uiso 1 1 calc R . . C16 C 0.32875(13) 0.12583(11) 0.19357(12) 0.0270(4) Uani 1 1 d . . . C17 C 0.26085(14) 0.08303(13) 0.20463(13) 0.0364(5) Uani 1 1 d . . . C18 C 0.2701(2) 0.0758(2) 0.28247(16) 0.0714(11) Uani 1 1 d . . . H18A H 0.3198 0.0497 0.3086 0.107 Uiso 1 1 calc R . . H18B H 0.2231 0.0508 0.2853 0.107 Uiso 1 1 calc R . . H18C H 0.2733 0.1225 0.3036 0.107 Uiso 1 1 calc R . . C19 C 0.18108(16) 0.12167(17) 0.16449(19) 0.0606(8) Uani 1 1 d . . . H19A H 0.1356 0.0955 0.1690 0.091 Uiso 1 1 calc R . . H19B H 0.1734 0.1257 0.1140 0.091 Uiso 1 1 calc R . . H19C H 0.1832 0.1686 0.1849 0.091 Uiso 1 1 calc R . . C20 C 0.25914(18) 0.01060(15) 0.17224(18) 0.0549(8) Uani 1 1 d . . . H20A H 0.3124 -0.0117 0.1946 0.082 Uiso 1 1 calc R . . H20B H 0.2462 0.0151 0.1208 0.082 Uiso 1 1 calc R . . H20C H 0.2176 -0.0182 0.1805 0.082 Uiso 1 1 calc R . . C21 C 0.97830(19) 0.28501(16) 0.10317(17) 0.0535(7) Uani 1 1 d . . . H21A H 1.0222 0.2867 0.0845 0.080 Uiso 1 1 calc R . . H21B H 0.9467 0.2420 0.0869 0.080 Uiso 1 1 calc R . . H21C H 1.0016 0.2857 0.1555 0.080 Uiso 1 1 calc R . . C22 C 0.89221(17) 0.35164(19) -0.00524(15) 0.0546(8) Uani 1 1 d . . . H22A H 0.8615 0.3950 -0.0219 0.082 Uiso 1 1 calc R . . H22B H 0.8569 0.3114 -0.0254 0.082 Uiso 1 1 calc R . . H22C H 0.9387 0.3505 -0.0206 0.082 Uiso 1 1 calc R . . C23 C 0.96999(18) 0.41504(16) 0.1075(2) 0.0613(9) Uani 1 1 d . . . H23A H 0.9341 0.4557 0.0914 0.092 Uiso 1 1 calc R . . H23B H 1.0158 0.4197 0.0916 0.092 Uiso 1 1 calc R . . H23C H 0.9904 0.4125 0.1597 0.092 Uiso 1 1 calc R . . C24 C 0.92271(13) 0.34852(12) 0.07605(13) 0.0331(5) Uani 1 1 d . . . C25 C 0.85386(13) 0.34453(11) 0.10482(12) 0.0277(4) Uani 1 1 d . . . C26 C 0.77415(13) 0.36464(12) 0.06350(12) 0.0317(5) Uani 1 1 d . . . H26 H 0.7612 0.3756 0.0146 0.038 Uiso 1 1 calc R . . C27 C 0.71275(12) 0.36912(11) 0.09182(12) 0.0271(4) Uani 1 1 d . . . C28 C 0.62808(12) 0.38751(11) 0.04397(12) 0.0271(4) Uani 1 1 d . . . C29 C 0.60960(14) 0.43097(12) -0.01551(13) 0.0338(5) Uani 1 1 d . . . H29 H 0.6521 0.4519 -0.0267 0.041 Uiso 1 1 calc R . . C30 C 0.52898(14) 0.44375(13) -0.05848(13) 0.0374(5) Uani 1 1 d . . . H30 H 0.5167 0.4740 -0.0985 0.045 Uiso 1 1 calc R . . C31 C 0.46661(14) 0.41266(12) -0.04339(12) 0.0323(5) Uani 1 1 d . . . H31 H 0.4116 0.4225 -0.0723 0.039 Uiso 1 1 calc R . . C32 C 0.48442(12) 0.36692(11) 0.01413(11) 0.0265(4) Uani 1 1 d . . . C33 C 0.56520(12) 0.35543(11) 0.05805(11) 0.0265(4) Uani 1 1 d . . . H33 H 0.5774 0.3253 0.0981 0.032 Uiso 1 1 calc R . . C34 C 0.42039(12) 0.32641(11) 0.02970(11) 0.0260(4) Uani 1 1 d . . . C35 C 0.34793(13) 0.35898(12) 0.02548(13) 0.0325(5) Uani 1 1 d . . . H35 H 0.3362 0.4044 0.0049 0.039 Uiso 1 1 calc R . . C36 C 0.29218(12) 0.32741(12) 0.05032(11) 0.0272(4) Uani 1 1 d . . . C37 C 0.21591(13) 0.36548(12) 0.05013(14) 0.0346(5) Uani 1 1 d . . . C38 C 0.20588(18) 0.43877(16) 0.0181(2) 0.0707(11) Uani 1 1 d . . . H38A H 0.2056 0.4361 -0.0306 0.106 Uiso 1 1 calc R . . H38B H 0.2511 0.4684 0.0473 0.106 Uiso 1 1 calc R . . H38C H 0.1545 0.4589 0.0169 0.106 Uiso 1 1 calc R . . C39 C 0.14329(14) 0.32042(16) 0.00668(16) 0.0473(7) Uani 1 1 d . . . H39A H 0.0929 0.3430 0.0051 0.071 Uiso 1 1 calc R . . H39B H 0.1480 0.2742 0.0290 0.071 Uiso 1 1 calc R . . H39C H 0.1423 0.3150 -0.0420 0.071 Uiso 1 1 calc R . . C40 C 0.22103(17) 0.36939(18) 0.12724(16) 0.0564(8) Uani 1 1 d . . . H40A H 0.2693 0.3962 0.1557 0.085 Uiso 1 1 calc R . . H40B H 0.2247 0.3219 0.1467 0.085 Uiso 1 1 calc R . . H40C H 0.1723 0.3925 0.1288 0.085 Uiso 1 1 calc R . . C41 C 0.98936(16) 0.05085(15) 0.23677(14) 0.0466(7) Uani 1 1 d . . . H41A H 0.9472 0.0163 0.2335 0.070 Uiso 1 1 calc R . . H41B H 1.0429 0.0313 0.2647 0.070 Uiso 1 1 calc R . . H41C H 0.9870 0.0625 0.1887 0.070 Uiso 1 1 calc R . . C42 C 1.04552(14) 0.16886(15) 0.28328(16) 0.0460(6) Uani 1 1 d . . . H42A H 1.0499 0.1782 0.2370 0.069 Uiso 1 1 calc R . . H42B H 1.0966 0.1486 0.3159 0.069 Uiso 1 1 calc R . . H42C H 1.0347 0.2127 0.3034 0.069 Uiso 1 1 calc R . . C43 C 0.97191(17) 0.09915(15) 0.34597(14) 0.0459(6) Uani 1 1 d . . . H43A H 0.9604 0.1417 0.3677 0.069 Uiso 1 1 calc R . . H43B H 1.0243 0.0797 0.3770 0.069 Uiso 1 1 calc R . . H43C H 0.9289 0.0646 0.3399 0.069 Uiso 1 1 calc R . . C44 C 0.97525(13) 0.11692(13) 0.27314(12) 0.0336(5) Uani 1 1 d . . . C45 C 0.89533(13) 0.15446(12) 0.23028(12) 0.0287(4) Uani 1 1 d . . . C46 C 0.83885(13) 0.12573(12) 0.16828(12) 0.0313(5) Uani 1 1 d . . . H46 H 0.8528 0.0843 0.1494 0.038 Uiso 1 1 calc R . . C47 C 0.76206(12) 0.15577(11) 0.13268(11) 0.0260(4) Uani 1 1 d . . . C48 C 0.69699(12) 0.11595(11) 0.07592(11) 0.0252(4) Uani 1 1 d . . . C49 C 0.71316(13) 0.06768(12) 0.03073(12) 0.0299(5) Uani 1 1 d . . . H49 H 0.7677 0.0573 0.0365 0.036 Uiso 1 1 calc R . . C50 C 0.64906(14) 0.03472(12) -0.02278(12) 0.0319(5) Uani 1 1 d . . . H50 H 0.6601 0.0021 -0.0537 0.038 Uiso 1 1 calc R . . C51 C 0.56912(13) 0.04931(11) -0.03119(11) 0.0289(4) Uani 1 1 d . . . H51 H 0.5257 0.0276 -0.0686 0.035 Uiso 1 1 calc R . . C52 C 0.55262(12) 0.09575(11) 0.01518(11) 0.0256(4) Uani 1 1 d . . . C53 C 0.61695(12) 0.12837(11) 0.06886(11) 0.0249(4) Uani 1 1 d . . . H53 H 0.6060 0.1595 0.1010 0.030 Uiso 1 1 calc R . . C54 C 0.46854(13) 0.11405(11) 0.00970(11) 0.0258(4) Uani 1 1 d . . . C55 C 0.40590(13) 0.11942(12) -0.05674(12) 0.0306(5) Uani 1 1 d . . . H55 H 0.4178 0.1105 -0.0982 0.037 Uiso 1 1 calc R . . C56 C 0.32573(13) 0.13745(11) -0.06519(11) 0.0285(4) Uani 1 1 d . . . C57 C 0.25725(14) 0.13660(14) -0.13891(12) 0.0372(5) Uani 1 1 d . . . C58 C 0.26613(17) 0.07531(16) -0.18467(14) 0.0507(7) Uani 1 1 d . . . H58A H 0.2188 0.0738 -0.2295 0.076 Uiso 1 1 calc R . . H58B H 0.2698 0.0313 -0.1586 0.076 Uiso 1 1 calc R . . H58C H 0.3156 0.0816 -0.1951 0.076 Uiso 1 1 calc R . . C59 C 0.2613(2) 0.20563(18) -0.17426(18) 0.0738(11) Uani 1 1 d . . . H59A H 0.2162 0.2085 -0.2205 0.111 Uiso 1 1 calc R . . H59B H 0.3130 0.2088 -0.1815 0.111 Uiso 1 1 calc R . . H59C H 0.2575 0.2443 -0.1437 0.111 Uiso 1 1 calc R . . C60 C 0.17548(17) 0.1282(3) -0.12949(17) 0.0792(12) Uani 1 1 d . . . H60A H 0.1665 0.1685 -0.1032 0.119 Uiso 1 1 calc R . . H60B H 0.1762 0.0852 -0.1028 0.119 Uiso 1 1 calc R . . H60C H 0.1316 0.1256 -0.1765 0.119 Uiso 1 1 calc R . . C61 C 0.7128(3) 0.0830(2) 0.3028(4) 0.121(2) Uani 1 1 d . . . H61A H 0.7253 0.1275 0.2850 0.182 Uiso 1 1 calc R . . H61B H 0.7490 0.0464 0.2975 0.182 Uiso 1 1 calc R . . H61C H 0.7207 0.0879 0.3533 0.182 Uiso 1 1 calc R . . C62 C 0.6279(3) 0.0637(2) 0.2618(3) 0.0952(14) Uani 1 1 d . . . H62A H 0.5916 0.1012 0.2666 0.114 Uiso 1 1 calc R . . H62B H 0.6199 0.0599 0.2106 0.114 Uiso 1 1 calc R . . C63 C 0.5260(3) -0.0221(3) 0.2462(2) 0.0895(13) Uani 1 1 d . . . H63A H 0.5172 -0.0264 0.1949 0.107 Uiso 1 1 calc R . . H63B H 0.4871 0.0130 0.2510 0.107 Uiso 1 1 calc R . . C64 C 0.5115(3) -0.0899(3) 0.2734(4) 0.144(3) Uani 1 1 d . . . H64A H 0.4557 -0.1051 0.2464 0.217 Uiso 1 1 calc R . . H64B H 0.5195 -0.0853 0.3240 0.217 Uiso 1 1 calc R . . H64C H 0.5498 -0.1245 0.2681 0.217 Uiso 1 1 calc R . . O13 O 0.60658(17) 0.00029(14) 0.28483(15) 0.0835(8) 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 Fe1 0.01600(14) 0.03426(17) 0.02663(16) -0.00510(12) 0.00969(12) -0.00294(11) Fe2 0.01717(14) 0.03225(16) 0.02596(16) -0.00266(12) 0.00914(12) -0.00333(11) O1 0.0193(7) 0.0386(8) 0.0306(8) -0.0078(6) 0.0100(6) -0.0068(6) O2 0.0194(7) 0.0396(8) 0.0279(8) -0.0084(6) 0.0105(6) -0.0083(6) O3 0.0215(7) 0.0399(8) 0.0267(8) -0.0038(6) 0.0107(6) -0.0095(6) O4 0.0224(7) 0.0369(8) 0.0299(8) -0.0040(6) 0.0103(6) -0.0086(6) O5 0.0187(7) 0.0499(10) 0.0333(9) -0.0024(7) 0.0131(6) -0.0040(6) O6 0.0193(7) 0.0342(8) 0.0312(8) -0.0023(6) 0.0122(6) -0.0024(6) O7 0.0217(7) 0.0313(8) 0.0370(8) 0.0017(6) 0.0153(6) -0.0001(6) O8 0.0207(7) 0.0360(8) 0.0373(9) -0.0005(7) 0.0153(6) -0.0014(6) O9 0.0216(7) 0.0370(8) 0.0321(8) -0.0053(6) 0.0070(6) 0.0023(6) O10 0.0203(7) 0.0330(8) 0.0300(8) -0.0068(6) 0.0077(6) -0.0004(6) O11 0.0208(7) 0.0323(8) 0.0256(7) -0.0026(6) 0.0089(6) -0.0015(6) O12 0.0195(7) 0.0456(9) 0.0284(8) -0.0052(7) 0.0082(6) -0.0024(6) C1 0.0273(12) 0.0315(12) 0.0480(14) -0.0027(10) 0.0052(10) -0.0095(9) C2 0.0288(12) 0.0484(14) 0.0359(13) -0.0183(11) 0.0048(10) -0.0069(10) C3 0.0222(11) 0.0360(12) 0.0444(14) 0.0004(10) 0.0054(10) 0.0037(9) C4 0.0182(10) 0.0274(10) 0.0315(11) -0.0025(8) 0.0048(8) -0.0020(8) C5 0.0168(9) 0.0191(9) 0.0297(11) -0.0015(8) 0.0045(8) 0.0023(7) C6 0.0217(10) 0.0319(11) 0.0249(10) -0.0044(8) 0.0082(8) -0.0038(8) C7 0.0185(9) 0.0230(9) 0.0257(10) 0.0000(8) 0.0079(8) -0.0002(7) C8 0.0208(10) 0.0240(10) 0.0250(10) -0.0006(8) 0.0082(8) -0.0023(7) C9 0.0274(11) 0.0319(11) 0.0240(10) -0.0051(8) 0.0082(9) -0.0069(8) C10 0.0373(12) 0.0338(11) 0.0279(11) -0.0061(9) 0.0185(10) -0.0096(9) C11 0.0273(11) 0.0329(11) 0.0304(11) -0.0062(9) 0.0170(9) -0.0086(9) C12 0.0206(10) 0.0255(10) 0.0267(10) -0.0031(8) 0.0111(8) -0.0040(8) C13 0.0207(10) 0.0295(10) 0.0230(10) -0.0039(8) 0.0101(8) -0.0039(8) C14 0.0181(9) 0.0289(10) 0.0285(11) -0.0040(8) 0.0102(8) -0.0022(8) C15 0.0248(11) 0.0419(12) 0.0297(11) -0.0057(9) 0.0135(9) -0.0115(9) C16 0.0222(10) 0.0296(10) 0.0330(11) -0.0024(9) 0.0145(9) -0.0036(8) C17 0.0273(12) 0.0478(14) 0.0382(13) -0.0082(10) 0.0167(10) -0.0174(10) C18 0.065(2) 0.109(3) 0.0503(17) -0.0147(18) 0.0325(16) -0.060(2) C19 0.0262(13) 0.070(2) 0.092(2) -0.0025(18) 0.0295(15) -0.0087(13) C20 0.0475(16) 0.0445(15) 0.083(2) -0.0128(15) 0.0355(16) -0.0202(13) C21 0.0526(17) 0.0576(17) 0.0672(19) 0.0126(14) 0.0418(16) 0.0182(14) C22 0.0402(15) 0.087(2) 0.0483(16) 0.0086(15) 0.0304(13) 0.0074(15) C23 0.0429(16) 0.0599(18) 0.096(3) -0.0160(17) 0.0425(17) -0.0205(14) C24 0.0256(11) 0.0385(12) 0.0439(13) -0.0027(10) 0.0229(10) -0.0017(9) C25 0.0227(10) 0.0299(11) 0.0347(12) -0.0059(9) 0.0156(9) -0.0060(8) C26 0.0247(11) 0.0415(13) 0.0328(12) 0.0017(9) 0.0153(9) -0.0013(9) C27 0.0210(10) 0.0265(10) 0.0355(12) -0.0032(9) 0.0125(9) -0.0043(8) C28 0.0205(10) 0.0313(11) 0.0322(11) -0.0003(9) 0.0128(9) -0.0015(8) C29 0.0279(11) 0.0374(12) 0.0415(13) 0.0049(10) 0.0193(10) -0.0025(9) C30 0.0325(12) 0.0442(13) 0.0378(13) 0.0127(10) 0.0156(10) 0.0026(10) C31 0.0241(11) 0.0409(12) 0.0316(12) 0.0027(9) 0.0101(9) 0.0017(9) C32 0.0207(10) 0.0328(11) 0.0284(11) -0.0003(8) 0.0118(8) -0.0011(8) C33 0.0221(10) 0.0323(11) 0.0289(11) 0.0020(8) 0.0138(9) -0.0007(8) C34 0.0188(10) 0.0365(12) 0.0225(10) -0.0012(8) 0.0075(8) -0.0023(8) C35 0.0198(10) 0.0357(12) 0.0421(13) 0.0057(10) 0.0114(9) 0.0015(9) C36 0.0161(9) 0.0360(12) 0.0283(11) -0.0042(9) 0.0068(8) -0.0018(8) C37 0.0181(10) 0.0392(13) 0.0491(14) -0.0007(10) 0.0154(10) -0.0008(9) C38 0.0399(16) 0.0497(17) 0.141(3) 0.0270(19) 0.055(2) 0.0153(13) C39 0.0176(11) 0.0667(18) 0.0535(16) -0.0024(13) 0.0083(11) -0.0033(11) C40 0.0360(15) 0.082(2) 0.0580(18) -0.0186(16) 0.0250(13) 0.0077(14) C41 0.0344(14) 0.0521(16) 0.0458(15) -0.0086(12) 0.0060(11) 0.0159(12) C42 0.0207(11) 0.0554(16) 0.0589(17) -0.0021(13) 0.0110(11) 0.0042(11) C43 0.0407(14) 0.0571(16) 0.0357(14) 0.0075(12) 0.0091(11) 0.0112(12) C44 0.0215(10) 0.0425(13) 0.0342(12) -0.0026(10) 0.0073(9) 0.0061(9) C45 0.0202(10) 0.0368(12) 0.0310(11) -0.0017(9) 0.0117(9) -0.0002(8) C46 0.0226(10) 0.0377(12) 0.0337(12) -0.0068(9) 0.0106(9) 0.0016(9) C47 0.0214(10) 0.0344(11) 0.0250(10) -0.0026(8) 0.0120(8) -0.0017(8) C48 0.0216(10) 0.0293(10) 0.0245(10) -0.0015(8) 0.0084(8) -0.0019(8) C49 0.0237(10) 0.0340(11) 0.0340(12) -0.0025(9) 0.0130(9) 0.0005(8) C50 0.0323(12) 0.0357(12) 0.0314(12) -0.0086(9) 0.0160(10) -0.0025(9) C51 0.0263(11) 0.0334(11) 0.0274(11) -0.0060(9) 0.0102(9) -0.0059(9) C52 0.0224(10) 0.0283(10) 0.0259(10) -0.0008(8) 0.0087(8) -0.0014(8) C53 0.0235(10) 0.0281(10) 0.0247(10) -0.0031(8) 0.0107(8) 0.0000(8) C54 0.0231(10) 0.0273(10) 0.0278(11) -0.0021(8) 0.0104(8) -0.0032(8) C55 0.0241(11) 0.0425(13) 0.0250(11) -0.0038(9) 0.0090(9) -0.0023(9) C56 0.0232(10) 0.0334(11) 0.0270(11) -0.0005(9) 0.0068(9) -0.0044(8) C57 0.0229(11) 0.0552(15) 0.0292(12) -0.0025(10) 0.0045(9) 0.0012(10) C58 0.0449(16) 0.0622(18) 0.0348(14) -0.0102(12) 0.0026(12) -0.0054(13) C59 0.083(3) 0.061(2) 0.0477(18) 0.0132(15) -0.0106(17) 0.0021(18) C60 0.0227(14) 0.166(4) 0.0415(17) -0.023(2) 0.0029(12) -0.0093(18) C61 0.120(4) 0.054(2) 0.202(6) 0.006(3) 0.073(4) -0.007(3) C62 0.119(4) 0.060(2) 0.120(4) 0.023(2) 0.060(3) 0.022(2) C63 0.078(3) 0.110(4) 0.072(3) -0.020(2) 0.017(2) 0.012(2) C64 0.111(4) 0.067(3) 0.229(7) -0.036(4) 0.031(4) -0.025(3) O13 0.0811(19) 0.0620(15) 0.099(2) 0.0075(14) 0.0228(16) 0.0039(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 Fe1 O1 1.9749(15) . ? Fe1 O2 1.9813(14) . ? Fe1 O6 1.9939(15) . ? Fe1 O9 1.9990(15) . ? Fe1 O5 1.9999(15) . ? Fe1 O10 2.0140(14) . ? Fe2 O4 1.9787(15) . ? Fe2 O11 1.9813(15) . ? Fe2 O3 1.9828(15) . ? Fe2 O8 1.9881(15) . ? Fe2 O12 2.0023(15) . ? Fe2 O7 2.0173(15) . ? O1 C5 1.275(3) . ? O2 C7 1.273(2) . ? O3 C14 1.270(2) . ? O4 C16 1.279(3) . ? O5 C25 1.268(3) . ? O6 C27 1.269(3) . ? O7 C34 1.267(3) . ? O8 C36 1.270(3) . ? O9 C45 1.273(3) . ? O10 C47 1.273(3) . ? O11 C54 1.287(2) . ? O12 C56 1.270(3) . ? C1 C4 1.532(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C4 1.529(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.542(3) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.536(3) . ? C5 C6 1.396(3) . ? C6 C7 1.401(3) . ? C6 H6 0.9500 . ? C7 C8 1.498(3) . ? C8 C13 1.391(3) . ? C8 C9 1.397(3) . ? C9 C10 1.387(3) . ? C9 H9 0.9500 . ? C10 C11 1.387(3) . ? C10 H10 0.9500 . ? C11 C12 1.395(3) . ? C11 H11 0.9500 . ? C12 C13 1.397(3) . ? C12 C14 1.493(3) . ? C13 H13 0.9500 . ? C14 C15 1.403(3) . ? C15 C16 1.397(3) . ? C15 H15 0.9500 . ? C16 C17 1.536(3) . ? C17 C18 1.522(4) . ? C17 C20 1.525(4) . ? C17 C19 1.533(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C24 1.530(3) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.525(4) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.525(4) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.532(3) . ? C25 C26 1.402(3) . ? C26 C27 1.404(3) . ? C26 H26 0.9500 . ? C27 C28 1.494(3) . ? C28 C33 1.388(3) . ? C28 C29 1.394(3) . ? C29 C30 1.391(3) . ? C29 H29 0.9500 . ? C30 C31 1.382(3) . ? C30 H30 0.9500 . ? C31 C32 1.392(3) . ? C31 H31 0.9500 . ? C32 C33 1.394(3) . ? C32 C34 1.498(3) . ? C33 H33 0.9500 . ? C34 C35 1.399(3) . ? C35 C36 1.397(3) . ? C35 H35 0.9500 . ? C36 C37 1.532(3) . ? C37 C38 1.524(4) . ? C37 C40 1.525(4) . ? C37 C39 1.526(3) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C44 1.525(3) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C44 1.544(3) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.529(3) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.536(3) . ? C45 C46 1.393(3) . ? C46 C47 1.404(3) . ? C46 H46 0.9500 . ? C47 C48 1.497(3) . ? C48 C53 1.391(3) . ? C48 C49 1.398(3) . ? C49 C50 1.394(3) . ? C49 H49 0.9500 . ? C50 C51 1.390(3) . ? C50 H50 0.9500 . ? C51 C52 1.395(3) . ? C51 H51 0.9500 . ? C52 C53 1.395(3) . ? C52 C54 1.492(3) . ? C53 H53 0.9500 . ? C54 C55 1.392(3) . ? C55 C56 1.408(3) . ? C55 H55 0.9500 . ? C56 C57 1.533(3) . ? C57 C59 1.513(4) . ? C57 C58 1.534(4) . ? C57 C60 1.536(4) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C62 1.469(7) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 O13 1.399(5) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 O13 1.416(5) . ? C63 C64 1.465(7) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? 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 O1 Fe1 O2 85.70(6) . . ? O1 Fe1 O6 104.25(6) . . ? O2 Fe1 O6 88.46(6) . . ? O1 Fe1 O9 87.42(6) . . ? O2 Fe1 O9 100.54(7) . . ? O6 Fe1 O9 165.86(6) . . ? O1 Fe1 O5 89.09(6) . . ? O2 Fe1 O5 170.19(7) . . ? O6 Fe1 O5 84.77(6) . . ? O9 Fe1 O5 87.50(7) . . ? O1 Fe1 O10 168.78(7) . . ? O2 Fe1 O10 88.10(6) . . ? O6 Fe1 O10 84.90(6) . . ? O9 Fe1 O10 84.53(6) . . ? O5 Fe1 O10 98.33(6) . . ? O4 Fe2 O11 101.23(6) . . ? O4 Fe2 O3 85.97(6) . . ? O11 Fe2 O3 90.09(6) . . ? O4 Fe2 O8 90.26(6) . . ? O11 Fe2 O8 167.00(6) . . ? O3 Fe2 O8 96.84(6) . . ? O4 Fe2 O12 90.41(6) . . ? O11 Fe2 O12 85.49(6) . . ? O3 Fe2 O12 173.64(7) . . ? O8 Fe2 O12 88.39(6) . . ? O4 Fe2 O7 171.10(6) . . ? O11 Fe2 O7 84.21(6) . . ? O3 Fe2 O7 87.00(6) . . ? O8 Fe2 O7 85.18(6) . . ? O12 Fe2 O7 97.08(6) . . ? C5 O1 Fe1 130.97(13) . . ? C7 O2 Fe1 131.64(13) . . ? C14 O3 Fe2 130.91(13) . . ? C16 O4 Fe2 130.16(13) . . ? C25 O5 Fe1 127.82(13) . . ? C27 O6 Fe1 124.82(13) . . ? C34 O7 Fe2 130.34(13) . . ? C36 O8 Fe2 132.23(13) . . ? C45 O9 Fe1 130.82(14) . . ? C47 O10 Fe1 130.70(13) . . ? C54 O11 Fe2 124.11(13) . . ? C56 O12 Fe2 127.47(14) . . ? C4 C1 H1A 109.5 . . ? C4 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C2 H2A 109.5 . . ? C4 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 C1 110.05(19) . . ? C2 C4 C5 113.36(18) . . ? C1 C4 C5 109.58(18) . . ? C2 C4 C3 109.96(19) . . ? C1 C4 C3 108.54(19) . . ? C5 C4 C3 105.15(17) . . ? O1 C5 C6 123.61(18) . . ? O1 C5 C4 114.21(17) . . ? C6 C5 C4 122.12(19) . . ? C5 C6 C7 122.92(19) . . ? C5 C6 H6 118.5 . . ? C7 C6 H6 118.5 . . ? O2 C7 C6 123.54(18) . . ? O2 C7 C8 114.94(17) . . ? C6 C7 C8 121.52(18) . . ? C13 C8 C9 118.69(18) . . ? C13 C8 C7 117.40(18) . . ? C9 C8 C7 123.91(18) . . ? C10 C9 C8 120.22(19) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C11 C10 C9 120.6(2) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C10 C11 C12 120.13(19) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C13 118.72(18) . . ? C11 C12 C14 123.84(18) . . ? C13 C12 C14 117.44(18) . . ? C8 C13 C12 121.60(19) . . ? C8 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? O3 C14 C15 123.75(19) . . ? O3 C14 C12 115.13(17) . . ? C15 C14 C12 121.08(19) . . ? C16 C15 C14 123.1(2) . . ? C16 C15 H15 118.4 . . ? C14 C15 H15 118.4 . . ? O4 C16 C15 123.77(19) . . ? O4 C16 C17 114.12(18) . . ? C15 C16 C17 122.11(19) . . ? C18 C17 C20 109.7(3) . . ? C18 C17 C19 108.4(3) . . ? C20 C17 C19 110.0(2) . . ? C18 C17 C16 113.90(19) . . ? C20 C17 C16 108.27(19) . . ? C19 C17 C16 106.5(2) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C24 C21 H21A 109.5 . . ? C24 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C24 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C24 C22 H22A 109.5 . . ? C24 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C24 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C23 C24 C22 109.7(2) . . ? C23 C24 C21 109.3(2) . . ? C22 C24 C21 109.9(2) . . ? C23 C24 C25 105.97(19) . . ? C22 C24 C25 113.1(2) . . ? C21 C24 C25 108.77(19) . . ? O5 C25 C26 123.30(19) . . ? O5 C25 C24 114.81(19) . . ? C26 C25 C24 121.9(2) . . ? C25 C26 C27 122.4(2) . . ? C25 C26 H26 118.8 . . ? C27 C26 H26 118.8 . . ? O6 C27 C26 124.6(2) . . ? O6 C27 C28 115.70(18) . . ? C26 C27 C28 119.6(2) . . ? C33 C28 C29 119.2(2) . . ? C33 C28 C27 116.93(19) . . ? C29 C28 C27 123.80(19) . . ? C30 C29 C28 120.1(2) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C31 C30 C29 120.4(2) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C30 C31 C32 119.9(2) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C31 C32 C33 119.47(19) . . ? C31 C32 C34 122.85(19) . . ? C33 C32 C34 117.63(19) . . ? C28 C33 C32 120.8(2) . . ? C28 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? O7 C34 C35 125.04(19) . . ? O7 C34 C32 114.57(18) . . ? C35 C34 C32 120.33(19) . . ? C36 C35 C34 122.6(2) . . ? C36 C35 H35 118.7 . . ? C34 C35 H35 118.7 . . ? O8 C36 C35 123.69(19) . . ? O8 C36 C37 114.13(18) . . ? C35 C36 C37 122.2(2) . . ? C38 C37 C40 109.9(3) . . ? C38 C37 C39 109.4(2) . . ? C40 C37 C39 109.5(2) . . ? C38 C37 C36 113.68(19) . . ? C40 C37 C36 107.4(2) . . ? C39 C37 C36 106.8(2) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C44 C41 H41A 109.5 . . ? C44 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C44 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C44 C42 H42A 109.5 . . ? C44 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C44 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 H43A 109.5 . . ? C44 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C44 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 C43 110.4(2) . . ? C41 C44 C45 113.31(19) . . ? C43 C44 C45 106.84(19) . . ? C41 C44 C42 109.2(2) . . ? C43 C44 C42 109.3(2) . . ? C45 C44 C42 107.72(19) . . ? O9 C45 C46 123.9(2) . . ? O9 C45 C44 114.15(19) . . ? C46 C45 C44 121.9(2) . . ? C45 C46 C47 122.5(2) . . ? C45 C46 H46 118.8 . . ? C47 C46 H46 118.8 . . ? O10 C47 C46 124.24(19) . . ? O10 C47 C48 115.07(18) . . ? C46 C47 C48 120.65(19) . . ? C53 C48 C49 119.44(19) . . ? C53 C48 C47 117.31(18) . . ? C49 C48 C47 123.25(19) . . ? C50 C49 C48 119.9(2) . . ? C50 C49 H49 120.1 . . ? C48 C49 H49 120.1 . . ? C51 C50 C49 120.3(2) . . ? C51 C50 H50 119.8 . . ? C49 C50 H50 119.8 . . ? C50 C51 C52 120.1(2) . . ? C50 C51 H51 120.0 . . ? C52 C51 H51 120.0 . . ? C53 C52 C51 119.39(19) . . ? C53 C52 C54 117.33(18) . . ? C51 C52 C54 123.27(19) . . ? C48 C53 C52 120.81(19) . . ? C48 C53 H53 119.6 . . ? C52 C53 H53 119.6 . . ? O11 C54 C55 124.70(19) . . ? O11 C54 C52 114.83(18) . . ? C55 C54 C52 120.46(19) . . ? C54 C55 C56 122.9(2) . . ? C54 C55 H55 118.5 . . ? C56 C55 H55 118.5 . . ? O12 C56 C55 122.95(19) . . ? O12 C56 C57 115.95(19) . . ? C55 C56 C57 121.1(2) . . ? C59 C57 C56 106.8(2) . . ? C59 C57 C58 110.4(2) . . ? C56 C57 C58 111.8(2) . . ? C59 C57 C60 111.1(3) . . ? C56 C57 C60 109.0(2) . . ? C58 C57 C60 107.8(2) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C57 C59 H59A 109.5 . . ? C57 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C57 C60 H60A 109.5 . . ? C57 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C57 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C62 C61 H61A 109.5 . . ? C62 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C62 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? O13 C62 C61 112.0(4) . . ? O13 C62 H62A 109.2 . . ? C61 C62 H62A 109.2 . . ? O13 C62 H62B 109.2 . . ? C61 C62 H62B 109.2 . . ? H62A C62 H62B 107.9 . . ? O13 C63 C64 109.9(4) . . ? O13 C63 H63A 109.7 . . ? C64 C63 H63A 109.7 . . ? O13 C63 H63B 109.7 . . ? C64 C63 H63B 109.7 . . ? H63A C63 H63B 108.2 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C62 O13 C63 114.8(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Fe1 O1 C5 13.38(18) . . . . ? O6 Fe1 O1 C5 100.69(18) . . . . ? O9 Fe1 O1 C5 -87.40(18) . . . . ? O5 Fe1 O1 C5 -174.94(18) . . . . ? O10 Fe1 O1 C5 -43.3(4) . . . . ? O1 Fe1 O2 C7 -3.55(18) . . . . ? O6 Fe1 O2 C7 -107.97(18) . . . . ? O9 Fe1 O2 C7 83.01(19) . . . . ? O10 Fe1 O2 C7 167.09(18) . . . . ? O4 Fe2 O3 C14 -12.31(18) . . . . ? O11 Fe2 O3 C14 -113.56(19) . . . . ? O8 Fe2 O3 C14 77.46(19) . . . . ? O7 Fe2 O3 C14 162.24(19) . . . . ? O11 Fe2 O4 C16 106.31(18) . . . . ? O3 Fe2 O4 C16 17.03(18) . . . . ? O8 Fe2 O4 C16 -79.81(19) . . . . ? O12 Fe2 O4 C16 -168.20(18) . . . . ? O1 Fe1 O5 C25 -135.87(18) . . . . ? O6 Fe1 O5 C25 -31.48(18) . . . . ? O9 Fe1 O5 C25 136.68(18) . . . . ? O10 Fe1 O5 C25 52.58(19) . . . . ? O1 Fe1 O6 C27 124.31(16) . . . . ? O2 Fe1 O6 C27 -150.52(16) . . . . ? O9 Fe1 O6 C27 -20.5(3) . . . . ? O5 Fe1 O6 C27 36.59(16) . . . . ? O10 Fe1 O6 C27 -62.28(16) . . . . ? O11 Fe2 O7 C34 168.42(19) . . . . ? O3 Fe2 O7 C34 -101.19(18) . . . . ? O8 Fe2 O7 C34 -4.06(18) . . . . ? O12 Fe2 O7 C34 83.71(18) . . . . ? O4 Fe2 O8 C36 -178.06(19) . . . . ? O11 Fe2 O8 C36 -25.8(4) . . . . ? O3 Fe2 O8 C36 95.97(19) . . . . ? O12 Fe2 O8 C36 -87.66(19) . . . . ? O7 Fe2 O8 C36 9.59(19) . . . . ? O1 Fe1 O9 C45 -167.93(19) . . . . ? O2 Fe1 O9 C45 106.93(19) . . . . ? O6 Fe1 O9 C45 -21.9(4) . . . . ? O5 Fe1 O9 C45 -78.72(19) . . . . ? O10 Fe1 O9 C45 19.89(19) . . . . ? O1 Fe1 O10 C47 -56.4(4) . . . . ? O2 Fe1 O10 C47 -112.87(18) . . . . ? O6 Fe1 O10 C47 158.50(18) . . . . ? O9 Fe1 O10 C47 -12.09(18) . . . . ? O5 Fe1 O10 C47 74.56(18) . . . . ? O4 Fe2 O11 C54 126.17(15) . . . . ? O3 Fe2 O11 C54 -147.92(16) . . . . ? O8 Fe2 O11 C54 -25.5(4) . . . . ? O12 Fe2 O11 C54 36.65(16) . . . . ? O7 Fe2 O11 C54 -60.95(16) . . . . ? O4 Fe2 O12 C56 -132.32(19) . . . . ? O11 Fe2 O12 C56 -31.08(18) . . . . ? O8 Fe2 O12 C56 137.44(19) . . . . ? O7 Fe2 O12 C56 52.50(19) . . . . ? Fe1 O1 C5 C6 -16.2(3) . . . . ? Fe1 O1 C5 C4 161.15(13) . . . . ? C2 C4 C5 O1 162.21(19) . . . . ? C1 C4 C5 O1 38.8(2) . . . . ? C3 C4 C5 O1 -77.6(2) . . . . ? C2 C4 C5 C6 -20.4(3) . . . . ? C1 C4 C5 C6 -143.8(2) . . . . ? C3 C4 C5 C6 99.7(2) . . . . ? O1 C5 C6 C7 5.2(3) . . . . ? C4 C5 C6 C7 -171.90(19) . . . . ? Fe1 O2 C7 C6 -3.4(3) . . . . ? Fe1 O2 C7 C8 176.27(13) . . . . ? C5 C6 C7 O2 4.5(3) . . . . ? C5 C6 C7 C8 -175.14(19) . . . . ? O2 C7 C8 C13 -10.6(3) . . . . ? C6 C7 C8 C13 169.13(19) . . . . ? O2 C7 C8 C9 169.84(19) . . . . ? C6 C7 C8 C9 -10.5(3) . . . . ? C13 C8 C9 C10 -0.9(3) . . . . ? C7 C8 C9 C10 178.7(2) . . . . ? C8 C9 C10 C11 0.5(3) . . . . ? C9 C10 C11 C12 0.8(3) . . . . ? C10 C11 C12 C13 -1.6(3) . . . . ? C10 C11 C12 C14 177.8(2) . . . . ? C9 C8 C13 C12 0.1(3) . . . . ? C7 C8 C13 C12 -179.57(18) . . . . ? C11 C12 C13 C8 1.2(3) . . . . ? C14 C12 C13 C8 -178.23(19) . . . . ? Fe2 O3 C14 C15 4.9(3) . . . . ? Fe2 O3 C14 C12 -177.60(13) . . . . ? C11 C12 C14 O3 163.6(2) . . . . ? C13 C12 C14 O3 -17.0(3) . . . . ? C11 C12 C14 C15 -18.8(3) . . . . ? C13 C12 C14 C15 160.6(2) . . . . ? O3 C14 C15 C16 4.6(4) . . . . ? C12 C14 C15 C16 -172.7(2) . . . . ? Fe2 O4 C16 C15 -14.4(3) . . . . ? Fe2 O4 C16 C17 165.57(15) . . . . ? C14 C15 C16 O4 0.2(4) . . . . ? C14 C15 C16 C17 -179.8(2) . . . . ? O4 C16 C17 C18 175.6(3) . . . . ? C15 C16 C17 C18 -4.4(4) . . . . ? O4 C16 C17 C20 53.3(3) . . . . ? C15 C16 C17 C20 -126.7(3) . . . . ? O4 C16 C17 C19 -64.9(3) . . . . ? C15 C16 C17 C19 115.1(3) . . . . ? Fe1 O5 C25 C26 17.0(3) . . . . ? Fe1 O5 C25 C24 -164.12(14) . . . . ? C23 C24 C25 O5 -78.2(3) . . . . ? C22 C24 C25 O5 161.6(2) . . . . ? C21 C24 C25 O5 39.1(3) . . . . ? C23 C24 C25 C26 100.7(3) . . . . ? C22 C24 C25 C26 -19.5(3) . . . . ? C21 C24 C25 C26 -142.0(2) . . . . ? O5 C25 C26 C27 6.5(4) . . . . ? C24 C25 C26 C27 -172.3(2) . . . . ? Fe1 O6 C27 C26 -28.9(3) . . . . ? Fe1 O6 C27 C28 148.25(14) . . . . ? C25 C26 C27 O6 0.0(4) . . . . ? C25 C26 C27 C28 -177.0(2) . . . . ? O6 C27 C28 C33 -32.8(3) . . . . ? C26 C27 C28 C33 144.5(2) . . . . ? O6 C27 C28 C29 151.3(2) . . . . ? C26 C27 C28 C29 -31.4(3) . . . . ? C33 C28 C29 C30 2.3(3) . . . . ? C27 C28 C29 C30 178.1(2) . . . . ? C28 C29 C30 C31 -1.1(4) . . . . ? C29 C30 C31 C32 -1.6(4) . . . . ? C30 C31 C32 C33 3.0(3) . . . . ? C30 C31 C32 C34 -174.3(2) . . . . ? C29 C28 C33 C32 -0.8(3) . . . . ? C27 C28 C33 C32 -176.9(2) . . . . ? C31 C32 C33 C28 -1.8(3) . . . . ? C34 C32 C33 C28 175.63(19) . . . . ? Fe2 O7 C34 C35 -2.9(3) . . . . ? Fe2 O7 C34 C32 174.55(13) . . . . ? C31 C32 C34 O7 138.7(2) . . . . ? C33 C32 C34 O7 -38.6(3) . . . . ? C31 C32 C34 C35 -43.7(3) . . . . ? C33 C32 C34 C35 139.0(2) . . . . ? O7 C34 C35 C36 7.9(4) . . . . ? C32 C34 C35 C36 -169.4(2) . . . . ? Fe2 O8 C36 C35 -8.0(3) . . . . ? Fe2 O8 C36 C37 173.67(14) . . . . ? C34 C35 C36 O8 -2.5(4) . . . . ? C34 C35 C36 C37 175.7(2) . . . . ? O8 C36 C37 C38 -179.5(2) . . . . ? C35 C36 C37 C38 2.2(4) . . . . ? O8 C36 C37 C40 58.7(3) . . . . ? C35 C36 C37 C40 -119.7(3) . . . . ? O8 C36 C37 C39 -58.7(3) . . . . ? C35 C36 C37 C39 122.9(2) . . . . ? Fe1 O9 C45 C46 -16.3(3) . . . . ? Fe1 O9 C45 C44 167.29(15) . . . . ? C41 C44 C45 O9 -177.4(2) . . . . ? C43 C44 C45 O9 60.8(3) . . . . ? C42 C44 C45 O9 -56.5(3) . . . . ? C41 C44 C45 C46 6.2(3) . . . . ? C43 C44 C45 C46 -115.7(2) . . . . ? C42 C44 C45 C46 127.0(2) . . . . ? O9 C45 C46 C47 -2.9(4) . . . . ? C44 C45 C46 C47 173.3(2) . . . . ? Fe1 O10 C47 C46 0.9(3) . . . . ? Fe1 O10 C47 C48 178.49(13) . . . . ? C45 C46 C47 O10 10.6(4) . . . . ? C45 C46 C47 C48 -167.0(2) . . . . ? O10 C47 C48 C53 -30.1(3) . . . . ? C46 C47 C48 C53 147.6(2) . . . . ? O10 C47 C48 C49 150.0(2) . . . . ? C46 C47 C48 C49 -32.3(3) . . . . ? C53 C48 C49 C50 2.7(3) . . . . ? C47 C48 C49 C50 -177.4(2) . . . . ? C48 C49 C50 C51 -0.4(3) . . . . ? C49 C50 C51 C52 -1.7(3) . . . . ? C50 C51 C52 C53 1.4(3) . . . . ? C50 C51 C52 C54 -179.9(2) . . . . ? C49 C48 C53 C52 -3.0(3) . . . . ? C47 C48 C53 C52 177.09(19) . . . . ? C51 C52 C53 C48 1.0(3) . . . . ? C54 C52 C53 C48 -177.77(19) . . . . ? Fe2 O11 C54 C55 -29.0(3) . . . . ? Fe2 O11 C54 C52 149.74(14) . . . . ? C53 C52 C54 O11 -35.6(3) . . . . ? C51 C52 C54 O11 145.7(2) . . . . ? C53 C52 C54 C55 143.2(2) . . . . ? C51 C52 C54 C55 -35.5(3) . . . . ? O11 C54 C55 C56 -0.5(4) . . . . ? C52 C54 C55 C56 -179.1(2) . . . . ? Fe2 O12 C56 C55 15.7(3) . . . . ? Fe2 O12 C56 C57 -162.02(15) . . . . ? C54 C55 C56 O12 7.7(4) . . . . ? C54 C55 C56 C57 -174.7(2) . . . . ? O12 C56 C57 C59 94.8(3) . . . . ? C55 C56 C57 C59 -83.0(3) . . . . ? O12 C56 C57 C58 -144.4(2) . . . . ? C55 C56 C57 C58 37.9(3) . . . . ? O12 C56 C57 C60 -25.3(3) . . . . ? C55 C56 C57 C60 156.9(3) . . . . ? C61 C62 O13 C63 -178.5(4) . . . . ? C64 C63 O13 C62 178.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.726 _refine_diff_density_min -0.516 _refine_diff_density_rms 0.070 data_lj66 _database_code_depnum_ccdc_archive 'CCDC 258482' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H56 Cu2 N4 O8, 2(C4 H8 O)' _chemical_formula_sum 'C58 H72 Cu2 N4 O10' _chemical_formula_weight 1112.28 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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.426(4) _cell_length_b 16.570(7) _cell_length_c 17.638(7) _cell_angle_alpha 110.476(6) _cell_angle_beta 92.635(7) _cell_angle_gamma 100.853(6) _cell_volume 2783(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2980 _cell_measurement_theta_min 2.225 _cell_measurement_theta_max 24.45 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.368 _exptl_crystal_size_mid 0.340 _exptl_crystal_size_min 0.232 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.328 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1172 _exptl_absorpt_coefficient_mu 0.825 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 60 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.65 _diffrn_reflns_number 21930 _diffrn_reflns_av_R_equivalents 0.1249 _diffrn_reflns_av_sigmaI/netI 0.2096 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 28.33 _reflns_number_total 12117 _reflns_number_gt 4984 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT and XPREP (Siemens, 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEP-3 (Farrugia, 1997) WINGX-32 (Farrugia, 1999) ; _computing_publication_material 'enCIFer 1.0 (CCDC, 2003)' _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^)+(0.1766P)^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 12117 _refine_ls_number_parameters 655 _refine_ls_number_restraints 457 _refine_ls_R_factor_all 0.2228 _refine_ls_R_factor_gt 0.1061 _refine_ls_wR_factor_ref 0.3360 _refine_ls_wR_factor_gt 0.2716 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.981 _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 C1 C 0.6227(11) 0.8277(8) -0.2251(7) 0.067(3) Uani 1 1 d U . . H1A H 0.6991 0.8758 -0.1975 0.101 Uiso 1 1 calc R . . H1B H 0.6393 0.7724 -0.2223 0.101 Uiso 1 1 calc R . . H1C H 0.5449 0.8410 -0.1982 0.101 Uiso 1 1 calc R . . C2 C 0.5855(10) 0.9082(7) -0.3169(7) 0.062(3) Uani 1 1 d U . . H2A H 0.5246 0.9326 -0.2790 0.092 Uiso 1 1 calc R . . H2B H 0.5514 0.9001 -0.3724 0.092 Uiso 1 1 calc R . . H2C H 0.6718 0.9489 -0.3015 0.092 Uiso 1 1 calc R . . C3 C 0.7169(9) 0.7897(8) -0.3565(7) 0.061(3) Uani 1 1 d U . . H3A H 0.7985 0.8306 -0.3256 0.092 Uiso 1 1 calc R . . H3B H 0.7081 0.7905 -0.4117 0.092 Uiso 1 1 calc R . . H3C H 0.7195 0.7299 -0.3593 0.092 Uiso 1 1 calc R . . C4 C 0.5991(10) 0.8180(7) -0.3136(6) 0.052(3) Uani 1 1 d U . . C5 C 0.4621(9) 0.7548(6) -0.3503(6) 0.041(2) Uani 1 1 d U . . C6 C 0.4493(9) 0.6843(6) -0.4254(6) 0.044(2) Uani 1 1 d U . . H6 H 0.5271 0.6728 -0.4492 0.053 Uiso 1 1 calc R . . C7 C 0.3299(8) 0.6306(6) -0.4668(6) 0.036(2) Uani 1 1 d U . . C8 C 0.3232(9) 0.5616(6) -0.5499(6) 0.040(2) Uani 1 1 d U . . C9 C 0.4274(11) 0.5629(8) -0.5993(7) 0.066(3) Uani 1 1 d U . . H9 H 0.5068 0.6065 -0.5792 0.079 Uiso 1 1 calc R . . C10 C 0.4111(12) 0.4990(8) -0.6777(8) 0.074(4) Uani 1 1 d U . . H10 H 0.4807 0.5006 -0.7104 0.089 Uiso 1 1 calc R . . C11 C 0.3010(11) 0.4354(7) -0.7091(7) 0.065(3) Uani 1 1 d U . . H11 H 0.2943 0.3937 -0.7630 0.078 Uiso 1 1 calc R . . C12 C 0.1952(8) 0.4304(6) -0.6621(6) 0.036(2) Uani 1 1 d U . . C13 C 0.2108(8) 0.4974(5) -0.5827(5) 0.0299(19) Uani 1 1 d U . . H13 H 0.1395 0.4974 -0.5510 0.036 Uiso 1 1 calc R . . C14 C 0.0732(9) 0.3626(6) -0.6935(5) 0.035(2) Uani 1 1 d U . . C15 C 0.0558(10) 0.2997(6) -0.7730(6) 0.043(2) Uani 1 1 d U . . H15 H 0.1235 0.3020 -0.8069 0.051 Uiso 1 1 calc R . . C16 C -0.0617(9) 0.2319(5) -0.8040(5) 0.0309(19) Uani 1 1 d U . . C17 C -0.0658(11) 0.1623(7) -0.8933(6) 0.051(3) Uani 1 1 d U . . C18 C 0.0550(11) 0.1801(7) -0.9342(7) 0.065(3) Uani 1 1 d U . . H18A H 0.0465 0.1338 -0.9883 0.098 Uiso 1 1 calc R . . H18B H 0.1333 0.1805 -0.9010 0.098 Uiso 1 1 calc R . . H18C H 0.0635 0.2376 -0.9399 0.098 Uiso 1 1 calc R . . C19 C -0.1882(11) 0.1591(8) -0.9434(7) 0.071(3) Uani 1 1 d U . . H19A H -0.1890 0.2183 -0.9430 0.107 Uiso 1 1 calc R . . H19B H -0.2657 0.1380 -0.9205 0.107 Uiso 1 1 calc R . . H19C H -0.1898 0.1187 -0.9996 0.107 Uiso 1 1 calc R . . C20 C -0.0676(14) 0.0743(8) -0.8812(8) 0.080(4) Uani 1 1 d U . . H20A H -0.0610 0.0288 -0.9334 0.121 Uiso 1 1 calc R . . H20B H -0.1499 0.0562 -0.8610 0.121 Uiso 1 1 calc R . . H20C H 0.0071 0.0819 -0.8416 0.121 Uiso 1 1 calc R . . C21 C -0.0818(10) 0.1452(8) -1.3008(7) 0.062(3) Uani 1 1 d U . . H21A H -0.0964 0.1996 -1.3065 0.094 Uiso 1 1 calc R . . H21B H -0.1588 0.0972 -1.3275 0.094 Uiso 1 1 calc R . . H21C H -0.0039 0.1297 -1.3264 0.094 Uiso 1 1 calc R . . C22 C -0.0346(11) 0.0740(7) -1.2012(8) 0.067(3) Uani 1 1 d U . . H22A H 0.0378 0.0555 -1.2316 0.101 Uiso 1 1 calc R . . H22B H -0.1141 0.0268 -1.2218 0.101 Uiso 1 1 calc R . . H22C H -0.0108 0.0863 -1.1432 0.101 Uiso 1 1 calc R . . C23 C -0.1883(9) 0.1781(7) -1.1747(7) 0.057(3) Uani 1 1 d U . . H23A H -0.1759 0.1888 -1.1163 0.085 Uiso 1 1 calc R . . H23B H -0.2614 0.1272 -1.2016 0.085 Uiso 1 1 calc R . . H23C H -0.2084 0.2303 -1.1824 0.085 Uiso 1 1 calc R . . C24 C -0.0610(8) 0.1588(6) -1.2122(6) 0.043(2) Uani 1 1 d U . . C25 C 0.0637(8) 0.2311(6) -1.1717(5) 0.033(2) Uani 1 1 d U . . C26 C 0.0618(8) 0.2999(6) -1.0991(6) 0.039(2) Uani 1 1 d U . . H26 H -0.0202 0.3044 -1.0784 0.047 Uiso 1 1 calc R . . C27 C 0.1735(8) 0.3626(5) -1.0549(5) 0.0295(19) Uani 1 1 d U . . C28 C 0.1633(8) 0.4338(5) -0.9740(5) 0.032(2) Uani 1 1 d U . . C29 C 0.0447(10) 0.4327(7) -0.9382(7) 0.061(3) Uani 1 1 d U . . H29 H -0.0320 0.3885 -0.9653 0.074 Uiso 1 1 calc R . . C30 C 0.0420(12) 0.4976(8) -0.8621(8) 0.077(4) Uani 1 1 d U . . H30 H -0.0372 0.4971 -0.8376 0.093 Uiso 1 1 calc R . . C31 C 0.1503(9) 0.5610(7) -0.8232(7) 0.059(3) Uani 1 1 d U . . H31 H 0.1460 0.6038 -0.7714 0.071 Uiso 1 1 calc R . . C32 C 0.2701(8) 0.5651(6) -0.8577(5) 0.032(2) Uani 1 1 d U . . C33 C 0.2722(7) 0.4980(5) -0.9336(5) 0.0227(17) Uani 1 1 d U . . H33 H 0.3521 0.4976 -0.9574 0.027 Uiso 1 1 calc R . . C34 C 0.3894(8) 0.6329(5) -0.8170(5) 0.0256(18) Uani 1 1 d U . . C35 C 0.3963(8) 0.6932(6) -0.7370(5) 0.032(2) Uani 1 1 d U . . H35 H 0.3236 0.6851 -0.7079 0.039 Uiso 1 1 calc R . . C36 C 0.5039(9) 0.7655(6) -0.6961(5) 0.033(2) Uani 1 1 d U . . C37 C 0.4934(9) 0.8311(6) -0.6117(5) 0.042(2) Uani 1 1 d U . . C38 C 0.3782(9) 0.8067(7) -0.5710(5) 0.049(3) Uani 1 1 d U . . H38A H 0.2969 0.8039 -0.6029 0.074 Uiso 1 1 calc R . . H38B H 0.3849 0.8513 -0.5162 0.074 Uiso 1 1 calc R . . H38C H 0.3770 0.7490 -0.5671 0.074 Uiso 1 1 calc R . . C39 C 0.6258(10) 0.8482(7) -0.5572(6) 0.051(3) Uani 1 1 d U . . H39A H 0.6246 0.8929 -0.5034 0.077 Uiso 1 1 calc R . . H39B H 0.6994 0.8693 -0.5830 0.077 Uiso 1 1 calc R . . H39C H 0.6362 0.7932 -0.5510 0.077 Uiso 1 1 calc R . . C40 C 0.4875(10) 0.9192(6) -0.6239(6) 0.054(3) Uani 1 1 d U . . H40A H 0.4102 0.9098 -0.6623 0.082 Uiso 1 1 calc R . . H40B H 0.5673 0.9388 -0.6458 0.082 Uiso 1 1 calc R . . H40C H 0.4815 0.9644 -0.5714 0.082 Uiso 1 1 calc R . . C41A C 0.0406(11) 0.7927(7) -0.4516(7) 0.0494(17) Uiso 0.80 1 d PD A 1 H41A H 0.0013 0.7319 -0.4791 0.059 Uiso 0.80 1 calc PR A 1 C42A C 0.0103(12) 0.8530(7) -0.4833(7) 0.0494(17) Uiso 0.80 1 d PD A 1 H42A H -0.0450 0.8325 -0.5336 0.059 Uiso 0.80 1 calc PR A 1 C43A C 0.0569(9) 0.9391(6) -0.4448(5) 0.045(2) Uani 0.80 1 d PDU A 1 C44A C 0.1502(11) 0.9671(8) -0.3738(7) 0.0494(17) Uiso 0.80 1 d PD A 1 H44A H 0.1912 1.0277 -0.3466 0.059 Uiso 0.80 1 calc PR A 1 C45A C 0.1796(11) 0.9037(7) -0.3454(7) 0.0494(17) Uiso 0.80 1 d PD A 1 H45A H 0.2408 0.9213 -0.2980 0.059 Uiso 0.80 1 calc PR A 1 N1A N 0.1225(7) 0.8169(4) -0.3841(4) 0.0329(17) Uani 0.80 1 d PDU A 1 N2A N 0.0395(8) 1.0137(6) -0.4712(5) 0.058(2) Uani 0.80 1 d PU . 1 N1B N 0.1225(7) 0.8169(4) -0.3841(4) 0.0329(17) Uani 0.20 1 d PDU A 2 N2B N 0.0395(8) 1.0137(6) -0.4712(5) 0.058(2) Uani 0.20 1 d PU . 2 C42B C -0.036(3) 0.861(2) -0.456(3) 0.0494(17) Uiso 0.20 1 d PD A 2 H42B H -0.1196 0.8483 -0.4865 0.059 Uiso 0.20 1 calc PR A 2 C45B C 0.213(2) 0.889(2) -0.379(3) 0.0494(17) Uiso 0.20 1 d PD A 2 H45B H 0.2987 0.9001 -0.3516 0.059 Uiso 0.20 1 calc PR A 2 C43B C 0.0569(9) 0.9391(6) -0.4448(5) 0.045(2) Uani 0.20 1 d PDU A 2 C41B C -0.002(2) 0.802(2) -0.423(3) 0.0494(17) Uiso 0.20 1 d PD A 2 H41B H -0.0654 0.7504 -0.4269 0.059 Uiso 0.20 1 calc PR A 2 C44B C 0.182(2) 0.948(2) -0.413(3) 0.0494(17) Uiso 0.20 1 d PD A 2 H44B H 0.2490 0.9948 -0.4140 0.059 Uiso 0.20 1 calc PR A 2 N3 N 0.4734(12) 0.0228(8) -0.9808(7) 0.089(4) Uani 1 1 d U . . C46 C 0.4481(11) 0.0803(7) -1.0318(7) 0.060(3) Uani 1 1 d DU . . C47 C 0.4771(14) 0.0676(9) -1.1061(8) 0.094(4) Uani 1 1 d DU . . H47 H 0.5167 0.0200 -1.1338 0.113 Uiso 1 1 calc R . . C48 C 0.4490(15) 0.1251(9) -1.1447(8) 0.100(5) Uani 1 1 d DU . . H48 H 0.4718 0.1163 -1.1981 0.120 Uiso 1 1 calc R . . C49 C 0.3538(14) 0.1998(9) -1.0340(7) 0.095(5) Uani 1 1 d DU . . H49 H 0.3071 0.2442 -1.0089 0.115 Uiso 1 1 calc R . . C50 C 0.3817(15) 0.1457(10) -0.9940(9) 0.108(5) Uani 1 1 d DU . . H50 H 0.3557 0.1531 -0.9414 0.130 Uiso 1 1 calc R . . N4 N 0.3916(7) 0.1909(4) -1.1080(4) 0.0322(16) Uani 1 1 d DU . . O2T O -0.2480(15) 0.6659(10) -0.5833(9) 0.069(2) Uiso 0.55 1 d PD B 1 C5T C -0.220(2) 0.5849(14) -0.5768(14) 0.069(2) Uiso 0.55 1 d PD B 1 H5T1 H -0.2946 0.5344 -0.6042 0.083 Uiso 0.55 1 calc PR B 1 H5T2 H -0.2049 0.5918 -0.5188 0.083 Uiso 0.55 1 calc PR B 1 C6T C -0.101(2) 0.5696(15) -0.6163(15) 0.069(2) Uiso 0.55 1 d PD B 1 H6T1 H -0.1161 0.5087 -0.6571 0.083 Uiso 0.55 1 calc PR B 1 H6T2 H -0.0262 0.5780 -0.5753 0.083 Uiso 0.55 1 calc PR B 1 C7T C -0.0705(18) 0.6363(14) -0.6572(13) 0.069(2) Uiso 0.55 1 d PD B 1 H7T1 H 0.0020 0.6866 -0.6251 0.083 Uiso 0.55 1 calc PR B 1 H7T2 H -0.0479 0.6090 -0.7131 0.083 Uiso 0.55 1 calc PR B 1 C8T C -0.199(2) 0.6640(19) -0.6582(14) 0.069(2) Uiso 0.55 1 d PD B 1 H8T1 H -0.1864 0.7231 -0.6621 0.083 Uiso 0.55 1 calc PR B 1 H8T2 H -0.2618 0.6213 -0.7053 0.083 Uiso 0.55 1 calc PR B 1 O3T O -0.2215(18) 0.6381(13) -0.5744(11) 0.069(2) Uiso 0.45 1 d PD C 2 C9T C -0.133(3) 0.5764(18) -0.5898(15) 0.069(2) Uiso 0.45 1 d PD C 2 H9T1 H -0.0802 0.5855 -0.5382 0.083 Uiso 0.45 1 calc PR C 2 H9T2 H -0.1847 0.5149 -0.6120 0.083 Uiso 0.45 1 calc PR C 2 C10T C -0.045(2) 0.5914(19) -0.6483(15) 0.069(2) Uiso 0.45 1 d PD C 2 H10A H -0.0269 0.5352 -0.6855 0.083 Uiso 0.45 1 calc PR C 2 H10B H 0.0400 0.6320 -0.6200 0.083 Uiso 0.45 1 calc PR C 2 C11T C -0.121(2) 0.6320(18) -0.6936(13) 0.069(2) Uiso 0.45 1 d PD C 2 H11A H -0.0655 0.6870 -0.6948 0.083 Uiso 0.45 1 calc PR C 2 H11B H -0.1507 0.5906 -0.7503 0.083 Uiso 0.45 1 calc PR C 2 C12T C -0.230(2) 0.650(2) -0.6503(16) 0.069(2) Uiso 0.45 1 d PD C 2 H12A H -0.3113 0.6110 -0.6845 0.083 Uiso 0.45 1 calc PR C 2 H12B H -0.2358 0.7119 -0.6403 0.083 Uiso 0.45 1 calc PR C 2 O1T O 0.4939(10) 0.3646(8) -0.8583(7) 0.117(4) Uani 1 1 d U D 2 C1T C 0.6038(15) 0.3431(11) -0.8183(10) 0.098(5) Uani 1 1 d U D 2 H1T1 H 0.5988 0.3610 -0.7590 0.118 Uiso 1 1 calc R D 2 H1T2 H 0.5998 0.2788 -0.8412 0.118 Uiso 1 1 calc R D 2 C2T C 0.7180(16) 0.3884(12) -0.8326(10) 0.112(5) Uani 1 1 d U D 2 H2T1 H 0.7906 0.3578 -0.8315 0.134 Uiso 1 1 calc R D 2 H2T2 H 0.7433 0.4490 -0.7911 0.134 Uiso 1 1 calc R D 2 C3T C 0.6874(14) 0.3906(11) -0.9173(10) 0.103(5) Uani 1 1 d U D 2 H3T1 H 0.7541 0.4348 -0.9284 0.123 Uiso 1 1 calc R D 2 H3T2 H 0.6786 0.3320 -0.9608 0.123 Uiso 1 1 calc R D 2 C4T C 0.5627(16) 0.4166(11) -0.9069(11) 0.109(5) Uani 1 1 d U D 2 H4T1 H 0.5107 0.4011 -0.9604 0.131 Uiso 1 1 calc R D 2 H4T2 H 0.5759 0.4809 -0.8766 0.131 Uiso 1 1 calc R D 2 O1 O 0.3695(6) 0.7747(4) -0.3101(4) 0.0424(16) Uani 1 1 d U A . O2 O 0.2164(5) 0.6334(3) -0.4395(3) 0.0298(13) Uani 1 1 d U A . O3 O -0.0101(5) 0.3645(4) -0.6426(3) 0.0342(14) Uani 1 1 d U . . O4 O -0.1592(6) 0.2200(4) -0.7717(3) 0.0361(14) Uani 1 1 d U . . O5 O 0.1638(5) 0.2183(4) -1.2075(4) 0.0389(15) Uani 1 1 d U . . O6 O 0.2903(5) 0.3674(4) -1.0755(3) 0.0309(13) Uani 1 1 d U . . O7 O 0.4842(5) 0.6338(4) -0.8603(3) 0.0325(14) Uani 1 1 d U . . O8 O 0.6095(6) 0.7830(4) -0.7267(3) 0.0334(14) Uani 1 1 d U . . Cu1 Cu 0.18247(10) 0.71271(7) -0.33677(6) 0.0305(3) Uani 1 1 d U . . Cu2 Cu 0.34354(9) 0.28623(6) -1.17008(6) 0.0267(3) Uani 1 1 d U . . 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 C1 0.053(5) 0.073(6) 0.063(6) 0.022(5) -0.010(5) -0.006(5) C2 0.055(5) 0.051(6) 0.067(6) 0.016(5) -0.008(5) -0.003(4) C3 0.038(5) 0.068(6) 0.073(6) 0.028(5) -0.007(4) -0.001(4) C4 0.048(5) 0.051(5) 0.050(5) 0.019(4) -0.004(4) 0.001(4) C5 0.036(4) 0.045(5) 0.046(5) 0.023(4) -0.009(4) 0.009(4) C6 0.032(4) 0.042(5) 0.056(5) 0.015(4) -0.002(4) 0.010(4) C7 0.029(4) 0.028(4) 0.053(5) 0.013(4) 0.001(4) 0.013(3) C8 0.039(4) 0.027(4) 0.057(5) 0.017(4) 0.016(4) 0.012(4) C9 0.060(5) 0.053(6) 0.071(6) 0.007(5) 0.027(5) 0.006(5) C10 0.058(6) 0.070(6) 0.074(6) 0.001(5) 0.028(5) 0.010(5) C11 0.072(6) 0.053(6) 0.062(6) 0.011(5) 0.033(5) 0.009(5) C12 0.039(4) 0.030(4) 0.040(5) 0.009(4) 0.014(4) 0.015(3) C13 0.034(4) 0.024(4) 0.041(4) 0.018(3) 0.012(3) 0.015(3) C14 0.051(5) 0.023(4) 0.036(4) 0.014(3) 0.004(4) 0.014(4) C15 0.059(5) 0.045(5) 0.038(5) 0.023(4) 0.018(4) 0.028(4) C16 0.049(5) 0.018(4) 0.026(4) 0.009(3) -0.011(4) 0.012(3) C17 0.064(5) 0.043(5) 0.040(5) 0.007(4) 0.011(4) 0.015(4) C18 0.072(6) 0.061(6) 0.059(6) 0.013(5) 0.017(5) 0.020(5) C19 0.078(6) 0.076(6) 0.044(5) 0.008(5) 0.001(5) 0.008(5) C20 0.113(7) 0.054(6) 0.069(6) 0.012(5) 0.021(6) 0.026(5) C21 0.049(5) 0.068(6) 0.060(6) 0.016(5) -0.016(4) 0.009(5) C22 0.065(6) 0.048(6) 0.082(7) 0.021(5) -0.009(5) 0.005(5) C23 0.042(5) 0.058(6) 0.062(6) 0.021(5) -0.015(4) 0.000(4) C24 0.030(4) 0.041(5) 0.052(5) 0.014(4) -0.011(4) 0.002(4) C25 0.027(4) 0.028(4) 0.042(4) 0.010(3) -0.005(3) 0.009(3) C26 0.031(4) 0.030(4) 0.053(5) 0.014(4) 0.003(4) 0.006(3) C27 0.032(4) 0.021(4) 0.038(4) 0.011(3) 0.000(3) 0.012(3) C28 0.028(4) 0.024(4) 0.045(5) 0.012(3) 0.014(3) 0.007(3) C29 0.039(5) 0.049(5) 0.074(6) -0.003(4) 0.023(5) 0.003(4) C30 0.059(6) 0.065(6) 0.082(6) -0.004(5) 0.040(5) 0.006(5) C31 0.042(5) 0.054(6) 0.065(6) -0.002(4) 0.029(4) 0.012(4) C32 0.035(4) 0.030(4) 0.035(4) 0.011(3) 0.011(3) 0.016(3) C33 0.020(3) 0.021(4) 0.029(4) 0.008(3) 0.002(3) 0.012(3) C34 0.032(4) 0.026(4) 0.026(4) 0.013(3) 0.006(3) 0.014(3) C35 0.036(4) 0.038(5) 0.027(4) 0.013(3) 0.005(3) 0.013(3) C36 0.046(4) 0.033(4) 0.020(4) 0.008(3) -0.009(3) 0.018(4) C37 0.057(5) 0.046(5) 0.023(4) 0.006(4) -0.005(4) 0.029(4) C38 0.062(5) 0.061(6) 0.028(4) 0.012(4) 0.003(4) 0.032(4) C39 0.060(5) 0.061(6) 0.030(4) 0.008(4) -0.010(4) 0.028(4) C40 0.069(6) 0.041(5) 0.044(5) 0.000(4) -0.009(4) 0.025(4) C43A 0.057(4) 0.047(5) 0.039(4) 0.020(4) 0.006(4) 0.023(4) N1A 0.040(3) 0.025(3) 0.035(3) 0.014(3) -0.008(3) 0.008(3) N2A 0.055(4) 0.057(4) 0.055(4) 0.011(4) -0.005(3) 0.018(4) N1B 0.040(3) 0.025(3) 0.035(3) 0.014(3) -0.008(3) 0.008(3) N2B 0.055(4) 0.057(4) 0.055(4) 0.011(4) -0.005(3) 0.018(4) C43B 0.057(4) 0.047(5) 0.039(4) 0.020(4) 0.006(4) 0.023(4) N3 0.091(6) 0.088(7) 0.078(6) 0.021(5) 0.019(5) 0.015(5) C46 0.071(6) 0.065(6) 0.053(6) 0.035(5) -0.018(5) 0.014(5) C47 0.106(7) 0.094(7) 0.098(8) 0.033(6) 0.023(6) 0.059(6) C48 0.119(8) 0.106(8) 0.095(8) 0.047(6) 0.036(6) 0.047(6) C49 0.102(7) 0.106(8) 0.090(7) 0.046(6) 0.010(6) 0.032(6) C50 0.119(8) 0.110(8) 0.107(8) 0.052(7) 0.014(6) 0.029(6) N4 0.035(3) 0.033(4) 0.029(4) 0.010(3) 0.000(3) 0.010(3) O1T 0.090(6) 0.140(7) 0.110(6) 0.027(5) 0.016(5) 0.031(5) C1T 0.105(8) 0.099(8) 0.100(8) 0.048(6) 0.009(6) 0.022(6) C2T 0.095(8) 0.126(9) 0.119(8) 0.056(7) 0.003(6) 0.018(6) C3T 0.088(7) 0.124(8) 0.095(8) 0.050(6) 0.009(6) 0.004(6) C4T 0.124(8) 0.104(8) 0.118(8) 0.059(7) 0.000(6) 0.036(6) O1 0.045(3) 0.037(4) 0.034(3) 0.007(3) -0.009(3) -0.005(3) O2 0.023(3) 0.023(3) 0.036(3) 0.005(2) -0.006(2) 0.001(2) O3 0.031(3) 0.031(3) 0.031(3) 0.000(2) 0.007(2) 0.005(2) O4 0.046(3) 0.031(3) 0.026(3) 0.006(3) 0.002(3) 0.007(3) O5 0.032(3) 0.029(3) 0.043(3) -0.002(3) -0.009(3) 0.008(2) O6 0.019(3) 0.032(3) 0.035(3) 0.005(2) 0.005(2) 0.004(2) O7 0.034(3) 0.026(3) 0.028(3) 0.003(2) 0.000(2) 0.001(2) O8 0.037(3) 0.033(3) 0.022(3) 0.001(2) -0.002(2) 0.006(3) Cu1 0.0389(6) 0.0233(6) 0.0238(6) 0.0042(5) -0.0103(4) 0.0060(5) Cu2 0.0274(5) 0.0231(6) 0.0234(6) 0.0006(4) -0.0068(4) 0.0086(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 C1 C4 1.517(14) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C4 1.547(15) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.535(14) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.559(13) . ? C5 O1 1.250(10) . ? C5 C6 1.408(13) . ? C6 C7 1.385(12) . ? C6 H6 0.9500 . ? C7 O2 1.300(9) . ? C7 C8 1.500(12) . ? C8 C13 1.370(12) . ? C8 C9 1.425(13) . ? C9 C10 1.395(15) . ? C9 H9 0.9500 . ? C10 C11 1.346(15) . ? C10 H10 0.9500 . ? C11 C12 1.417(13) . ? C11 H11 0.9500 . ? C12 C13 1.430(11) . ? C12 C14 1.466(12) . ? C13 H13 0.9500 . ? C14 O3 1.273(10) . ? C14 C15 1.403(12) . ? C15 C16 1.432(13) . ? C15 H15 0.9500 . ? C16 O4 1.206(10) . ? C16 C17 1.586(12) . ? C17 C19 1.500(15) . ? C17 C18 1.512(14) . ? C17 C20 1.543(15) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C24 1.498(14) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.555(14) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.548(13) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.537(11) . ? C25 O5 1.258(10) . ? C25 C26 1.390(12) . ? C26 C27 1.391(11) . ? C26 H26 0.9500 . ? C27 O6 1.283(9) . ? C27 C28 1.524(11) . ? C28 C33 1.367(11) . ? C28 C29 1.414(12) . ? C29 C30 1.401(14) . ? C29 H29 0.9500 . ? C30 C31 1.352(14) . ? C30 H30 0.9500 . ? C31 C32 1.415(12) . ? C31 H31 0.9500 . ? C32 C33 1.414(10) . ? C32 C34 1.466(11) . ? C33 H33 0.9500 . ? C34 O7 1.278(9) . ? C34 C35 1.404(11) . ? C35 C36 1.425(12) . ? C35 H35 0.9500 . ? C36 O8 1.277(10) . ? C36 C37 1.528(11) . ? C37 C38 1.490(13) . ? C37 C40 1.560(13) . ? C37 C39 1.566(12) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41A N1A 1.323(11) . ? C41A C42A 1.379(12) . ? C41A H41A 0.9500 . ? C42A C43A 1.329(11) . ? C42A H42A 0.9500 . ? C43A C44A 1.429(11) . ? C43A N2A 1.501(12) . ? C44A C45A 1.387(13) . ? C44A H44A 0.9500 . ? C45A N1A 1.357(11) . ? C45A H45A 0.9500 . ? N1A Cu1 2.332(6) . ? N2A N2A 1.173(15) 2_574 ? C42B C41B 1.397(19) . ? C42B H42B 0.9500 . ? C45B C44B 1.383(19) . ? C45B H45B 0.9500 . ? C41B H41B 0.9500 . ? C44B H44B 0.9500 . ? N3 N3 1.082(19) 2_653 ? N3 C46 1.569(15) . ? C46 C47 1.311(12) . ? C46 C50 1.385(12) . ? C47 C48 1.413(13) . ? C47 H47 0.9500 . ? C48 N4 1.325(11) . ? C48 H48 0.9500 . ? C49 N4 1.346(11) . ? C49 C50 1.382(13) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? N4 Cu2 2.325(7) . ? O2T C8T 1.430(16) . ? O2T C5T 1.469(16) . ? C5T C6T 1.473(16) . ? C5T H5T1 0.9900 . ? C5T H5T2 0.9900 . ? C6T C7T 1.513(17) . ? C6T H6T1 0.9900 . ? C6T H6T2 0.9900 . ? C7T C8T 1.500(17) . ? C7T H7T1 0.9900 . ? C7T H7T2 0.9900 . ? C8T H8T1 0.9900 . ? C8T H8T2 0.9900 . ? O3T C12T 1.422(16) . ? O3T C9T 1.470(17) . ? C9T C10T 1.466(17) . ? C9T H9T1 0.9900 . ? C9T H9T2 0.9900 . ? C10T C11T 1.495(16) . ? C10T H10A 0.9900 . ? C10T H10B 0.9900 . ? C11T C12T 1.421(16) . ? C11T H11A 0.9900 . ? C11T H11B 0.9900 . ? C12T H12A 0.9900 . ? C12T H12B 0.9900 . ? O1T C1T 1.481(16) . ? O1T C4T 1.528(17) . ? C1T C2T 1.367(18) . ? C1T H1T1 0.9900 . ? C1T H1T2 0.9900 . ? C2T C3T 1.528(19) . ? C2T H2T1 0.9900 . ? C2T H2T2 0.9900 . ? C3T C4T 1.444(19) . ? C3T H3T1 0.9900 . ? C3T H3T2 0.9900 . ? C4T H4T1 0.9900 . ? C4T H4T2 0.9900 . ? O1 Cu1 1.975(6) . ? O2 Cu1 1.924(5) . ? O3 Cu1 1.936(6) 2_564 ? O4 Cu1 1.902(6) 2_564 ? O5 Cu2 1.946(6) . ? O6 Cu2 1.923(5) . ? O7 Cu2 1.946(6) 2_663 ? O8 Cu2 1.923(5) 2_663 ? Cu1 O4 1.902(6) 2_564 ? Cu1 O3 1.936(6) 2_564 ? Cu2 O8 1.923(5) 2_663 ? Cu2 O7 1.946(6) 2_663 ? 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 C4 C1 H1A 109.5 . . ? C4 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C2 H2A 109.5 . . ? C4 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 C3 108.7(9) . . ? C1 C4 C2 108.7(10) . . ? C3 C4 C2 109.9(9) . . ? C1 C4 C5 107.6(8) . . ? C3 C4 C5 116.1(9) . . ? C2 C4 C5 105.5(8) . . ? O1 C5 C6 125.0(9) . . ? O1 C5 C4 115.1(9) . . ? C6 C5 C4 119.8(9) . . ? C7 C6 C5 123.8(9) . . ? C7 C6 H6 118.1 . . ? C5 C6 H6 118.1 . . ? O2 C7 C6 125.4(8) . . ? O2 C7 C8 114.0(7) . . ? C6 C7 C8 120.6(8) . . ? C13 C8 C9 117.7(9) . . ? C13 C8 C7 119.8(8) . . ? C9 C8 C7 122.4(9) . . ? C10 C9 C8 119.0(11) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? C11 C10 C9 123.0(11) . . ? C11 C10 H10 118.5 . . ? C9 C10 H10 118.5 . . ? C10 C11 C12 120.3(10) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C11 C12 C13 116.6(9) . . ? C11 C12 C14 122.5(9) . . ? C13 C12 C14 120.9(7) . . ? C8 C13 C12 123.4(8) . . ? C8 C13 H13 118.3 . . ? C12 C13 H13 118.3 . . ? O3 C14 C15 124.4(9) . . ? O3 C14 C12 114.9(8) . . ? C15 C14 C12 120.7(8) . . ? C14 C15 C16 121.4(8) . . ? C14 C15 H15 119.3 . . ? C16 C15 H15 119.3 . . ? O4 C16 C15 129.0(8) . . ? O4 C16 C17 114.7(8) . . ? C15 C16 C17 116.3(8) . . ? C19 C17 C18 111.0(10) . . ? C19 C17 C20 112.1(10) . . ? C18 C17 C20 106.5(9) . . ? C19 C17 C16 108.4(8) . . ? C18 C17 C16 114.1(9) . . ? C20 C17 C16 104.5(8) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C24 C21 H21A 109.5 . . ? C24 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C24 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C24 C22 H22A 109.5 . . ? C24 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C24 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 C25 109.1(8) . . ? C21 C24 C23 108.2(8) . . ? C25 C24 C23 114.9(8) . . ? C21 C24 C22 110.6(9) . . ? C25 C24 C22 105.9(7) . . ? C23 C24 C22 108.1(9) . . ? O5 C25 C26 125.3(8) . . ? O5 C25 C24 114.1(7) . . ? C26 C25 C24 120.5(8) . . ? C25 C26 C27 123.6(8) . . ? C25 C26 H26 118.2 . . ? C27 C26 H26 118.2 . . ? O6 C27 C26 126.0(8) . . ? O6 C27 C28 113.9(7) . . ? C26 C27 C28 120.1(7) . . ? C33 C28 C29 119.3(8) . . ? C33 C28 C27 119.5(7) . . ? C29 C28 C27 121.2(8) . . ? C30 C29 C28 119.0(10) . . ? C30 C29 H29 120.5 . . ? C28 C29 H29 120.5 . . ? C31 C30 C29 121.0(10) . . ? C31 C30 H30 119.5 . . ? C29 C30 H30 119.5 . . ? C30 C31 C32 121.6(9) . . ? C30 C31 H31 119.2 . . ? C32 C31 H31 119.2 . . ? C33 C32 C31 116.7(8) . . ? C33 C32 C34 120.3(7) . . ? C31 C32 C34 122.9(8) . . ? C28 C33 C32 122.4(7) . . ? C28 C33 H33 118.8 . . ? C32 C33 H33 118.8 . . ? O7 C34 C35 123.1(8) . . ? O7 C34 C32 115.0(7) . . ? C35 C34 C32 121.9(7) . . ? C34 C35 C36 125.1(8) . . ? C34 C35 H35 117.4 . . ? C36 C35 H35 117.4 . . ? O8 C36 C35 124.3(7) . . ? O8 C36 C37 115.9(8) . . ? C35 C36 C37 119.7(8) . . ? C38 C37 C36 116.7(8) . . ? C38 C37 C40 108.9(7) . . ? C36 C37 C40 105.6(7) . . ? C38 C37 C39 111.1(8) . . ? C36 C37 C39 107.3(7) . . ? C40 C37 C39 106.8(8) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N1A C41A C42A 122.1(10) . . ? N1A C41A H41A 118.9 . . ? C42A C41A H41A 118.9 . . ? C43A C42A C41A 121.2(10) . . ? C43A C42A H42A 119.4 . . ? C41A C42A H42A 119.4 . . ? C42A C43A C44A 117.9(8) . . ? C42A C43A N2A 128.8(9) . . ? C44A C43A N2A 112.8(8) . . ? C45A C44A C43A 118.4(10) . . ? C45A C44A H44A 120.8 . . ? C43A C44A H44A 120.8 . . ? N1A C45A C44A 121.2(9) . . ? N1A C45A H45A 119.4 . . ? C44A C45A H45A 119.4 . . ? C41A N1A C45A 118.9(8) . . ? C41A N1A Cu1 121.3(6) . . ? C45A N1A Cu1 119.7(6) . . ? N2A N2A C43A 109.2(12) 2_574 . ? C41B C42B H42B 120.6 . . ? C44B C45B H45B 119.7 . . ? C42B C41B H41B 119.9 . . ? C45B C44B H44B 119.5 . . ? N3 N3 C46 103.3(16) 2_653 . ? C47 C46 C50 120.0(10) . . ? C47 C46 N3 125.7(10) . . ? C50 C46 N3 114.2(10) . . ? C46 C47 C48 119.6(10) . . ? C46 C47 H47 120.2 . . ? C48 C47 H47 120.2 . . ? N4 C48 C47 121.3(10) . . ? N4 C48 H48 119.3 . . ? C47 C48 H48 119.3 . . ? N4 C49 C50 121.3(11) . . ? N4 C49 H49 119.3 . . ? C50 C49 H49 119.3 . . ? C49 C50 C46 118.8(11) . . ? C49 C50 H50 120.6 . . ? C46 C50 H50 120.6 . . ? C48 N4 C49 118.7(9) . . ? C48 N4 Cu2 122.1(7) . . ? C49 N4 Cu2 119.0(7) . . ? C8T O2T C5T 101.9(14) . . ? O2T C5T C6T 107.2(12) . . ? O2T C5T H5T1 110.3 . . ? C6T C5T H5T1 110.3 . . ? O2T C5T H5T2 110.3 . . ? C6T C5T H5T2 110.3 . . ? H5T1 C5T H5T2 108.5 . . ? C5T C6T C7T 106.3(13) . . ? C5T C6T H6T1 110.5 . . ? C7T C6T H6T1 110.5 . . ? C5T C6T H6T2 110.5 . . ? C7T C6T H6T2 110.5 . . ? H6T1 C6T H6T2 108.7 . . ? C8T C7T C6T 100.9(13) . . ? C8T C7T H7T1 111.6 . . ? C6T C7T H7T1 111.6 . . ? C8T C7T H7T2 111.6 . . ? C6T C7T H7T2 111.6 . . ? H7T1 C7T H7T2 109.4 . . ? O2T C8T C7T 106.1(14) . . ? O2T C8T H8T1 110.5 . . ? C7T C8T H8T1 110.5 . . ? O2T C8T H8T2 110.5 . . ? C7T C8T H8T2 110.5 . . ? H8T1 C8T H8T2 108.7 . . ? C12T O3T C9T 100.3(12) . . ? C10T C9T O3T 109.6(13) . . ? C10T C9T H9T1 109.7 . . ? O3T C9T H9T1 109.7 . . ? C10T C9T H9T2 109.7 . . ? O3T C9T H9T2 109.8 . . ? H9T1 C9T H9T2 108.2 . . ? C9T C10T C11T 103.0(11) . . ? C9T C10T H10A 111.2 . . ? C11T C10T H10A 111.2 . . ? C9T C10T H10B 111.2 . . ? C11T C10T H10B 111.2 . . ? H10A C10T H10B 109.1 . . ? C12T C11T C10T 105.7(11) . . ? C12T C11T H11A 110.6 . . ? C10T C11T H11A 110.6 . . ? C12T C11T H11B 110.6 . . ? C10T C11T H11B 110.6 . . ? H11A C11T H11B 108.7 . . ? C11T C12T O3T 113.2(12) . . ? C11T C12T H12A 108.9 . . ? O3T C12T H12A 108.9 . . ? C11T C12T H12B 108.9 . . ? O3T C12T H12B 108.9 . . ? H12A C12T H12B 107.7 . . ? C1T O1T C4T 103.4(11) . . ? C2T C1T O1T 107.1(13) . . ? C2T C1T H1T1 110.3 . . ? O1T C1T H1T1 110.3 . . ? C2T C1T H1T2 110.3 . . ? O1T C1T H1T2 110.3 . . ? H1T1 C1T H1T2 108.5 . . ? C1T C2T C3T 104.8(14) . . ? C1T C2T H2T1 110.8 . . ? C3T C2T H2T1 110.8 . . ? C1T C2T H2T2 110.8 . . ? C3T C2T H2T2 110.8 . . ? H2T1 C2T H2T2 108.9 . . ? C4T C3T C2T 98.6(13) . . ? C4T C3T H3T1 112.1 . . ? C2T C3T H3T1 112.1 . . ? C4T C3T H3T2 112.1 . . ? C2T C3T H3T2 112.1 . . ? H3T1 C3T H3T2 109.7 . . ? C3T C4T O1T 104.4(12) . . ? C3T C4T H4T1 110.9 . . ? O1T C4T H4T1 110.9 . . ? C3T C4T H4T2 110.9 . . ? O1T C4T H4T2 110.9 . . ? H4T1 C4T H4T2 108.9 . . ? C5 O1 Cu1 127.4(6) . . ? C7 O2 Cu1 126.9(5) . . ? C14 O3 Cu1 126.3(6) . 2_564 ? C16 O4 Cu1 125.4(6) . 2_564 ? C25 O5 Cu2 127.1(6) . . ? C27 O6 Cu2 126.1(5) . . ? C34 O7 Cu2 127.8(5) . 2_663 ? C36 O8 Cu2 126.9(5) . 2_663 ? O4 Cu1 O2 171.3(2) 2_564 . ? O4 Cu1 O3 93.3(2) 2_564 2_564 ? O2 Cu1 O3 86.6(2) . 2_564 ? O4 Cu1 O1 87.4(3) 2_564 . ? O2 Cu1 O1 91.1(2) . . ? O3 Cu1 O1 169.5(3) 2_564 . ? O4 Cu1 N1A 91.3(2) 2_564 . ? O2 Cu1 N1A 97.3(2) . . ? O3 Cu1 N1A 97.4(2) 2_564 . ? O1 Cu1 N1A 93.1(3) . . ? O6 Cu2 O8 171.0(3) . 2_663 ? O6 Cu2 O5 91.9(2) . . ? O8 Cu2 O5 87.7(2) 2_663 . ? O6 Cu2 O7 86.7(2) . 2_663 ? O8 Cu2 O7 92.3(2) 2_663 2_663 ? O5 Cu2 O7 171.5(3) . 2_663 ? O6 Cu2 N4 96.0(2) . . ? O8 Cu2 N4 93.0(2) 2_663 . ? O5 Cu2 N4 92.0(3) . . ? O7 Cu2 N4 96.5(2) 2_663 . ? 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 C1 C4 C5 O1 51.4(12) . . . . ? C3 C4 C5 O1 173.6(9) . . . . ? C2 C4 C5 O1 -64.5(11) . . . . ? C1 C4 C5 C6 -131.6(10) . . . . ? C3 C4 C5 C6 -9.5(14) . . . . ? C2 C4 C5 C6 112.4(10) . . . . ? O1 C5 C6 C7 3.8(16) . . . . ? C4 C5 C6 C7 -172.9(9) . . . . ? C5 C6 C7 O2 -5.6(16) . . . . ? C5 C6 C7 C8 174.9(9) . . . . ? O2 C7 C8 C13 -13.2(12) . . . . ? C6 C7 C8 C13 166.4(9) . . . . ? O2 C7 C8 C9 162.7(9) . . . . ? C6 C7 C8 C9 -17.7(15) . . . . ? C13 C8 C9 C10 -0.6(16) . . . . ? C7 C8 C9 C10 -176.6(10) . . . . ? C8 C9 C10 C11 0(2) . . . . ? C9 C10 C11 C12 0(2) . . . . ? C10 C11 C12 C13 2.2(16) . . . . ? C10 C11 C12 C14 179.8(11) . . . . ? C9 C8 C13 C12 2.5(14) . . . . ? C7 C8 C13 C12 178.6(8) . . . . ? C11 C12 C13 C8 -3.3(13) . . . . ? C14 C12 C13 C8 179.1(8) . . . . ? C11 C12 C14 O3 176.9(9) . . . . ? C13 C12 C14 O3 -5.6(12) . . . . ? C11 C12 C14 C15 -0.7(14) . . . . ? C13 C12 C14 C15 176.8(8) . . . . ? O3 C14 C15 C16 1.3(14) . . . . ? C12 C14 C15 C16 178.7(8) . . . . ? C14 C15 C16 O4 2.9(14) . . . . ? C14 C15 C16 C17 -177.2(8) . . . . ? O4 C16 C17 C19 53.5(11) . . . . ? C15 C16 C17 C19 -126.4(9) . . . . ? O4 C16 C17 C18 177.7(9) . . . . ? C15 C16 C17 C18 -2.2(12) . . . . ? O4 C16 C17 C20 -66.3(10) . . . . ? C15 C16 C17 C20 113.8(9) . . . . ? C21 C24 C25 O5 -52.1(11) . . . . ? C23 C24 C25 O5 -173.8(8) . . . . ? C22 C24 C25 O5 67.0(10) . . . . ? C21 C24 C25 C26 131.8(9) . . . . ? C23 C24 C25 C26 10.1(12) . . . . ? C22 C24 C25 C26 -109.1(10) . . . . ? O5 C25 C26 C27 -2.2(15) . . . . ? C24 C25 C26 C27 173.5(8) . . . . ? C25 C26 C27 O6 2.0(15) . . . . ? C25 C26 C27 C28 -177.5(8) . . . . ? O6 C27 C28 C33 4.2(11) . . . . ? C26 C27 C28 C33 -176.2(8) . . . . ? O6 C27 C28 C29 -173.3(9) . . . . ? C26 C27 C28 C29 6.3(13) . . . . ? C33 C28 C29 C30 0.0(16) . . . . ? C27 C28 C29 C30 177.5(10) . . . . ? C28 C29 C30 C31 0(2) . . . . ? C29 C30 C31 C32 1(2) . . . . ? C30 C31 C32 C33 -2.1(16) . . . . ? C30 C31 C32 C34 -179.9(11) . . . . ? C29 C28 C33 C32 -1.5(13) . . . . ? C27 C28 C33 C32 -179.0(8) . . . . ? C31 C32 C33 C28 2.5(13) . . . . ? C34 C32 C33 C28 -179.7(8) . . . . ? C33 C32 C34 O7 10.3(11) . . . . ? C31 C32 C34 O7 -172.0(9) . . . . ? C33 C32 C34 C35 -171.2(8) . . . . ? C31 C32 C34 C35 6.5(13) . . . . ? O7 C34 C35 C36 4.4(13) . . . . ? C32 C34 C35 C36 -174.0(8) . . . . ? C34 C35 C36 O8 -2.1(13) . . . . ? C34 C35 C36 C37 174.4(8) . . . . ? O8 C36 C37 C38 -173.3(7) . . . . ? C35 C36 C37 C38 9.9(11) . . . . ? O8 C36 C37 C40 65.6(9) . . . . ? C35 C36 C37 C40 -111.2(9) . . . . ? O8 C36 C37 C39 -48.0(11) . . . . ? C35 C36 C37 C39 135.2(9) . . . . ? N1A C41A C42A C43A -4(2) . . . . ? C41A C42A C43A C44A 6.2(18) . . . . ? C41A C42A C43A N2A 177.3(10) . . . . ? C42A C43A C44A C45A -4.7(17) . . . . ? N2A C43A C44A C45A -177.1(10) . . . . ? C43A C44A C45A N1A 0.6(18) . . . . ? C42A C41A N1A C45A -0.7(17) . . . . ? C42A C41A N1A Cu1 -175.9(9) . . . . ? C44A C45A N1A C41A 2.1(17) . . . . ? C44A C45A N1A Cu1 177.4(9) . . . . ? C42A C43A N2A N2A 9.6(18) . . . 2_574 ? C44A C43A N2A N2A -179.0(12) . . . 2_574 ? N3 N3 C46 C47 5(2) 2_653 . . . ? N3 N3 C46 C50 -179.2(16) 2_653 . . . ? C50 C46 C47 C48 5(2) . . . . ? N3 C46 C47 C48 -179.8(13) . . . . ? C46 C47 C48 N4 -1(2) . . . . ? N4 C49 C50 C46 -1(2) . . . . ? C47 C46 C50 C49 -4(2) . . . . ? N3 C46 C50 C49 -179.7(13) . . . . ? C47 C48 N4 C49 -3(2) . . . . ? C47 C48 N4 Cu2 -179.8(11) . . . . ? C50 C49 N4 C48 4(2) . . . . ? C50 C49 N4 Cu2 -179.0(11) . . . . ? C8T O2T C5T C6T 31(2) . . . . ? O2T C5T C6T C7T -8(3) . . . . ? C5T C6T C7T C8T -17(3) . . . . ? C5T O2T C8T C7T -43(2) . . . . ? C6T C7T C8T O2T 37(3) . . . . ? C12T O3T C9T C10T 29(3) . . . . ? O3T C9T C10T C11T -25(3) . . . . ? C9T C10T C11T C12T 9(3) . . . . ? C10T C11T C12T O3T 9(4) . . . . ? C9T O3T C12T C11T -23(3) . . . . ? C4T O1T C1T C2T 8.2(18) . . . . ? O1T C1T C2T C3T -33.8(19) . . . . ? C1T C2T C3T C4T 46.7(18) . . . . ? C2T C3T C4T O1T -39.9(16) . . . . ? C1T O1T C4T C3T 21.9(16) . . . . ? C6 C5 O1 Cu1 2.3(14) . . . . ? C4 C5 O1 Cu1 179.1(6) . . . . ? C6 C7 O2 Cu1 1.1(13) . . . . ? C8 C7 O2 Cu1 -179.3(5) . . . . ? C15 C14 O3 Cu1 -4.0(12) . . . 2_564 ? C12 C14 O3 Cu1 178.5(5) . . . 2_564 ? C15 C16 O4 Cu1 -3.7(12) . . . 2_564 ? C17 C16 O4 Cu1 176.4(6) . . . 2_564 ? C26 C25 O5 Cu2 3.2(13) . . . . ? C24 C25 O5 Cu2 -172.7(6) . . . . ? C26 C27 O6 Cu2 -2.9(12) . . . . ? C28 C27 O6 Cu2 176.7(5) . . . . ? C35 C34 O7 Cu2 0.4(11) . . . 2_663 ? C32 C34 O7 Cu2 178.9(5) . . . 2_663 ? C35 C36 O8 Cu2 -4.8(11) . . . 2_663 ? C37 C36 O8 Cu2 178.6(5) . . . 2_663 ? C7 O2 Cu1 O3 -166.6(7) . . . 2_564 ? C7 O2 Cu1 O1 3.2(7) . . . . ? C7 O2 Cu1 N1A 96.4(7) . . . . ? C5 O1 Cu1 O4 166.6(8) . . . 2_564 ? C5 O1 Cu1 O2 -4.8(8) . . . . ? C5 O1 Cu1 O3 72.4(16) . . . 2_564 ? C5 O1 Cu1 N1A -102.3(8) . . . . ? C41A N1A Cu1 O4 -135.5(8) . . . 2_564 ? C45A N1A Cu1 O4 49.3(8) . . . 2_564 ? C41A N1A Cu1 O2 45.5(8) . . . . ? C45A N1A Cu1 O2 -129.6(8) . . . . ? C41A N1A Cu1 O3 -42.0(8) . . . 2_564 ? C45A N1A Cu1 O3 142.9(8) . . . 2_564 ? C41A N1A Cu1 O1 137.1(8) . . . . ? C45A N1A Cu1 O1 -38.1(8) . . . . ? C27 O6 Cu2 O5 2.8(7) . . . . ? C27 O6 Cu2 O7 174.4(7) . . . 2_663 ? C27 O6 Cu2 N4 -89.5(7) . . . . ? C25 O5 Cu2 O6 -3.0(7) . . . . ? C25 O5 Cu2 O8 -174.0(7) . . . 2_663 ? C25 O5 Cu2 N4 93.1(7) . . . . ? C48 N4 Cu2 O6 -172.1(10) . . . . ? C49 N4 Cu2 O6 11.5(9) . . . . ? C48 N4 Cu2 O8 8.0(10) . . . 2_663 ? C49 N4 Cu2 O8 -168.4(9) . . . 2_663 ? C48 N4 Cu2 O5 95.8(10) . . . . ? C49 N4 Cu2 O5 -80.6(9) . . . . ? C48 N4 Cu2 O7 -84.7(10) . . . 2_663 ? C49 N4 Cu2 O7 98.9(9) . . . 2_663 ? _diffrn_measured_fraction_theta_max 0.874 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 3.338 _refine_diff_density_min -1.233 _refine_diff_density_rms 0.160