# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Prof Dr Hong Zhang' _publ_contact_author_email zhangh@nenu.edu.cn loop_ _publ_author_name 'Hong Zhang' 'Yu Pang' data_complex1 #TrackingRef '- complexes1-4.cif' _database_code_depnum_ccdc_archive 'CCDC 735307' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C54 H32 Cu2 N2 O12' _chemical_formula_sum 'C54 H32 Cu2 N2 O12' _chemical_formula_weight 1027.90 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 trigonal _symmetry_space_group_name_H-M 'P 32 2 1' _symmetry_space_group_name_Hall 'P 32 2" ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' 'x-y, -y, -z+1/3' '-x, -x+y, -z+2/3' 'y, x, -z' _cell_length_a 14.0995(10) _cell_length_b 14.0995(10) _cell_length_c 20.050(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3451.8(5) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4007 _cell_measurement_theta_min 1.67 _cell_measurement_theta_max 25.08 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.484 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1572 _exptl_absorpt_coefficient_mu 0.993 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.788 _exptl_absorpt_correction_T_max 0.862 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17706 _diffrn_reflns_av_R_equivalents 0.0705 _diffrn_reflns_av_sigmaI/netI 0.0647 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.08 _reflns_number_total 4099 _reflns_number_gt 3418 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1231P)^2^+6.2174P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 4095 _refine_ls_number_parameters 307 _refine_ls_number_restraints 632 _refine_ls_R_factor_all 0.0836 _refine_ls_R_factor_gt 0.0671 _refine_ls_wR_factor_ref 0.1931 _refine_ls_wR_factor_gt 0.1780 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5821(7) 0.1214(7) 0.7684(4) 0.0315(14) Uani 1 1 d U . . C2 C 0.6308(7) 0.2042(7) 0.8244(4) 0.0348(14) Uani 1 1 d U . . C3 C 0.5674(7) 0.2421(7) 0.8558(4) 0.0319(15) Uani 1 1 d U . . H3 H 0.4944 0.2133 0.8436 0.038 Uiso 1 1 calc RU . . C4 C 0.6114(7) 0.3212(8) 0.9044(4) 0.0357(14) Uani 1 1 d U . . C5 C 0.7187(8) 0.3561(8) 0.9274(5) 0.0500(17) Uani 1 1 d U . . C6 C 0.7649(9) 0.4224(11) 0.9900(7) 0.065(2) Uani 1 1 d U . . C7 C 0.7818(8) 0.3204(9) 0.8957(5) 0.0473(15) Uani 1 1 d U . . H7 H 0.8535 0.3461 0.9096 0.057 Uiso 1 1 calc RU . . C8 C 0.7394(7) 0.2458(8) 0.8428(5) 0.0411(16) Uani 1 1 d U . . C9 C 0.8207(8) 0.2194(8) 0.8089(5) 0.0460(17) Uani 1 1 d U . . C10 C 0.8780(8) 0.2808(9) 0.7502(5) 0.0535(18) Uani 1 1 d U . . C11 C 0.8585(9) 0.3592(10) 0.7202(6) 0.061(2) Uani 1 1 d U . . H11 H 0.8088 0.3764 0.7394 0.074 Uiso 1 1 calc RU . . C12 C 0.9110(10) 0.4096(12) 0.6641(7) 0.081(3) Uani 1 1 d U . . H12 H 0.8954 0.4598 0.6442 0.097 Uiso 1 1 calc RU . . C13 C 0.9837(12) 0.3903(12) 0.6362(7) 0.086(3) Uani 1 1 d U . . H13 H 1.0175 0.4267 0.5970 0.103 Uiso 1 1 calc RU . . C14 C 1.0105(10) 0.3201(11) 0.6624(6) 0.076(3) Uani 1 1 d U . . H14 H 1.0644 0.3096 0.6428 0.091 Uiso 1 1 calc RU . . C15 C 0.9564(9) 0.2624(11) 0.7200(6) 0.068(2) Uani 1 1 d U . . H15 H 0.9728 0.2116 0.7383 0.082 Uiso 1 1 calc RU . . C16 C 0.4491(7) -0.1771(6) 0.7322(4) 0.0270(16) Uani 1 1 d U . . C17 C 0.2409(7) 0.0197(9) 0.7222(5) 0.045(2) Uani 1 1 d U . . H17 H 0.2799 0.0321 0.7617 0.054 Uiso 1 1 calc RU . . C18 C 0.1435(7) 0.0226(9) 0.7234(5) 0.0478(19) Uani 1 1 d U . . H18 H 0.1202 0.0398 0.7627 0.057 Uiso 1 1 calc RU . . C19 C 0.0825(8) 0.0000 0.6667 0.038(2) Uani 1 2 d SU . . C20 C -0.0242(8) 0.0000 0.6667 0.040(2) Uani 1 2 d SU . . C21 C -0.0923(7) -0.0346(8) 0.7214(4) 0.0402(18) Uani 1 1 d U . . H21 H -0.0724 -0.0574 0.7598 0.048 Uiso 1 1 calc RU . . C22 C -0.1896(7) -0.0350(8) 0.7187(5) 0.0379(18) Uani 1 1 d U . . H22 H -0.2357 -0.0615 0.7556 0.045 Uiso 1 1 calc RU . . C23 C 0.8503(7) 0.5249(7) 0.9965(5) 0.080(2) Uani 1 1 d GU . . C24 C 0.8997(8) 0.5938(9) 0.9423(4) 0.097(3) Uani 1 1 d GU . . H24 H 0.8729 0.5703 0.8995 0.116 Uiso 1 1 calc RU . . C25 C 0.9893(9) 0.6978(8) 0.9521(5) 0.115(3) Uani 1 1 d GU . . H25 H 1.0224 0.7439 0.9159 0.138 Uiso 1 1 calc RU . . C26 C 1.0294(8) 0.7329(7) 1.0161(6) 0.105(3) Uani 1 1 d GU . . H26 H 1.0894 0.8025 1.0227 0.126 Uiso 1 1 calc RU . . C27 C 0.9800(9) 0.6641(9) 1.0703(4) 0.112(3) Uani 1 1 d GU . . H27 H 1.0068 0.6876 1.1131 0.134 Uiso 1 1 calc RU . . C28 C 0.8904(8) 0.5601(8) 1.0605(4) 0.102(3) Uani 1 1 d GU . . H28 H 0.8573 0.5140 1.0967 0.122 Uiso 1 1 calc RU . . N1 N 0.2804(7) 0.0000 0.6667 0.034(2) Uani 1 2 d S . . N2 N -0.2224(6) 0.0000 0.6667 0.030(2) Uani 1 2 d S . . O1 O 0.4851(4) 0.0828(4) 0.7519(2) 0.0280(12) Uani 1 1 d . . . O2 O 0.6482(4) 0.0962(5) 0.7424(3) 0.0322(13) Uani 1 1 d . . . O3 O 0.7281(11) 0.3787(13) 1.0416(4) 0.114(4) Uani 1 1 d . . . O4 O 0.8400(7) 0.1537(7) 0.8372(4) 0.072(2) Uani 1 1 d . . . O5 O 0.3892(4) -0.1394(4) 0.7141(3) 0.0314(13) Uani 1 1 d . . . O6 O 0.5513(4) -0.1316(4) 0.7261(3) 0.0299(12) Uani 1 1 d . . . Cu1 Cu 0.43371(8) 0.0000 0.6667 0.0184(3) Uani 1 2 d S . . Cu2 Cu -0.37458(8) 0.0000 0.6667 0.0177(3) Uani 1 2 d S . . 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 0.029(3) 0.040(3) 0.035(3) -0.006(2) -0.002(3) 0.025(2) C2 0.032(3) 0.044(3) 0.039(3) -0.016(3) -0.005(3) 0.027(2) C3 0.030(3) 0.043(3) 0.033(3) -0.011(3) -0.008(3) 0.026(3) C4 0.034(3) 0.048(3) 0.039(3) -0.016(3) -0.007(3) 0.031(2) C5 0.039(3) 0.063(3) 0.056(3) -0.022(3) -0.008(3) 0.032(3) C6 0.052(3) 0.075(3) 0.076(4) -0.025(3) -0.002(3) 0.038(3) C7 0.038(3) 0.058(3) 0.055(3) -0.021(3) -0.007(3) 0.031(2) C8 0.035(3) 0.051(3) 0.046(3) -0.017(3) -0.006(3) 0.029(2) C9 0.036(3) 0.055(3) 0.053(3) -0.024(3) -0.011(3) 0.027(3) C10 0.036(3) 0.059(3) 0.057(3) -0.025(3) -0.002(3) 0.018(3) C11 0.043(3) 0.064(3) 0.062(3) -0.012(3) -0.004(3) 0.016(3) C12 0.055(4) 0.078(4) 0.071(4) -0.012(4) -0.004(4) 0.003(4) C13 0.059(4) 0.082(5) 0.072(5) -0.015(4) -0.001(4) 0.001(4) C14 0.049(4) 0.078(4) 0.071(4) -0.019(4) 0.003(4) 0.009(4) C15 0.047(4) 0.070(4) 0.070(4) -0.026(4) 0.002(3) 0.015(4) C16 0.028(4) 0.024(3) 0.026(4) 0.000(3) -0.002(3) 0.010(3) C17 0.024(3) 0.073(5) 0.043(4) -0.014(4) -0.005(3) 0.028(3) C18 0.030(3) 0.072(5) 0.049(4) -0.009(4) 0.000(3) 0.031(3) C19 0.024(3) 0.063(4) 0.041(4) 0.001(4) 0.0005(18) 0.031(2) C20 0.029(3) 0.061(5) 0.042(4) -0.003(4) -0.0016(18) 0.030(2) C21 0.028(3) 0.062(4) 0.039(4) 0.009(3) -0.001(3) 0.029(3) C22 0.027(3) 0.054(4) 0.042(4) 0.003(3) 0.001(3) 0.027(3) C23 0.064(3) 0.083(4) 0.091(4) -0.028(3) -0.004(3) 0.036(3) C24 0.078(4) 0.091(4) 0.106(4) -0.017(4) -0.008(4) 0.032(3) C25 0.095(4) 0.106(4) 0.118(4) -0.014(4) -0.007(4) 0.031(4) C26 0.091(4) 0.097(4) 0.111(5) -0.016(4) -0.001(4) 0.036(4) C27 0.087(5) 0.104(5) 0.114(5) -0.026(4) -0.007(4) 0.025(4) C28 0.080(4) 0.100(4) 0.111(4) -0.023(4) -0.006(4) 0.033(3) N1 0.025(3) 0.051(6) 0.035(6) -0.001(5) -0.001(2) 0.026(3) N2 0.019(3) 0.036(5) 0.039(6) -0.002(4) -0.001(2) 0.018(3) O1 0.028(3) 0.034(3) 0.025(3) -0.009(2) -0.004(2) 0.017(3) O2 0.028(3) 0.038(3) 0.033(3) -0.010(3) -0.003(2) 0.019(3) O3 0.151(10) 0.211(13) 0.043(5) -0.036(7) -0.026(6) 0.138(11) O4 0.082(6) 0.090(6) 0.073(5) -0.028(5) -0.018(4) 0.066(5) O5 0.023(3) 0.030(3) 0.039(3) 0.013(2) 0.002(2) 0.011(2) O6 0.024(3) 0.029(3) 0.032(3) 0.008(2) -0.004(2) 0.009(2) Cu1 0.0158(5) 0.0214(7) 0.0198(6) -0.0006(5) -0.0003(2) 0.0107(3) Cu2 0.0148(5) 0.0183(6) 0.0211(6) -0.0014(5) -0.0007(2) 0.0091(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 O1 1.237(10) . ? C1 O2 1.265(9) . ? C1 C2 1.513(11) . ? C2 C8 1.389(12) . ? C2 C3 1.400(11) . ? C3 C4 1.374(11) . ? C3 H3 0.9300 . ? C4 C5 1.413(12) . ? C4 C16 1.508(10) 5_666 ? C5 C7 1.378(13) . ? C5 C6 1.504(15) . ? C6 O3 1.184(16) . ? C6 C23 1.348(14) . ? C7 C8 1.400(12) . ? C7 H7 0.9300 . ? C8 C9 1.529(12) . ? C9 O4 1.227(13) . ? C9 C10 1.445(15) . ? C10 C15 1.394(15) . ? C10 C11 1.401(18) . ? C11 C12 1.339(16) . ? C11 H11 0.9300 . ? C12 C13 1.31(2) . ? C12 H12 0.9300 . ? C13 C14 1.33(2) . ? C13 H13 0.9300 . ? C14 C15 1.399(17) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 O6 1.256(10) . ? C16 O5 1.256(10) . ? C16 C4 1.508(10) 5_656 ? C17 N1 1.335(11) . ? C17 C18 1.395(12) . ? C17 H17 0.9300 . ? C18 C19 1.364(11) . ? C18 H18 0.9300 . ? C19 C18 1.364(11) 4_556 ? C19 C20 1.505(14) . ? C20 C21 1.376(10) . ? C20 C21 1.376(10) 4_556 ? C21 C22 1.370(12) . ? C21 H21 0.9300 . ? C22 N2 1.332(10) . ? C22 H22 0.9300 . ? C23 C24 1.3900 . ? C23 C28 1.3900 . ? C24 C25 1.3900 . ? C24 H24 0.9300 . ? C25 C26 1.3900 . ? C25 H25 0.9300 . ? C26 C27 1.3900 . ? C26 H26 0.9300 . ? C27 C28 1.3900 . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? N1 C17 1.335(11) 4_556 ? N1 Cu1 2.162(9) . ? N2 C22 1.332(10) 4_556 ? N2 Cu2 2.146(9) . ? O1 Cu1 1.991(5) . ? O2 Cu2 1.952(5) 1_655 ? O5 Cu1 1.981(5) . ? O6 Cu2 2.005(5) 1_655 ? Cu1 O5 1.981(5) 4_556 ? Cu1 O1 1.991(5) 4_556 ? Cu1 Cu2 2.7031(16) 1_655 ? Cu2 O2 1.952(5) 1_455 ? Cu2 O2 1.952(5) 4_456 ? Cu2 O6 2.005(5) 1_455 ? Cu2 O6 2.005(5) 4_456 ? Cu2 Cu1 2.7031(16) 1_455 ? 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 C1 O2 125.0(7) . . ? O1 C1 C2 120.8(7) . . ? O2 C1 C2 114.2(7) . . ? C8 C2 C3 120.0(7) . . ? C8 C2 C1 120.1(7) . . ? C3 C2 C1 119.9(7) . . ? C4 C3 C2 120.9(7) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 119.0(7) . . ? C3 C4 C16 123.0(7) . 5_666 ? C5 C4 C16 118.0(7) . 5_666 ? C7 C5 C4 119.8(8) . . ? C7 C5 C6 117.0(9) . . ? C4 C5 C6 123.0(8) . . ? O3 C6 C23 113.4(12) . . ? O3 C6 C5 117.7(12) . . ? C23 C6 C5 128.6(12) . . ? C5 C7 C8 120.9(9) . . ? C5 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? C2 C8 C7 119.0(8) . . ? C2 C8 C9 125.6(8) . . ? C7 C8 C9 115.4(8) . . ? O4 C9 C10 124.1(9) . . ? O4 C9 C8 117.0(10) . . ? C10 C9 C8 118.5(9) . . ? C15 C10 C11 116.6(11) . . ? C15 C10 C9 119.9(12) . . ? C11 C10 C9 123.4(10) . . ? C12 C11 C10 120.2(13) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C13 C12 C11 122.1(17) . . ? C13 C12 H12 118.9 . . ? C11 C12 H12 118.9 . . ? C12 C13 C14 121.9(15) . . ? C12 C13 H13 119.1 . . ? C14 C13 H13 119.1 . . ? C13 C14 C15 118.9(14) . . ? C13 C14 H14 120.6 . . ? C15 C14 H14 120.6 . . ? C10 C15 C14 120.1(14) . . ? C10 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? O6 C16 O5 126.8(7) . . ? O6 C16 C4 118.5(7) . 5_656 ? O5 C16 C4 114.7(7) . 5_656 ? N1 C17 C18 122.7(9) . . ? N1 C17 H17 118.6 . . ? C18 C17 H17 118.6 . . ? C19 C18 C17 119.6(9) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C18 C19 C18 118.2(11) . 4_556 ? C18 C19 C20 120.9(5) . . ? C18 C19 C20 120.9(5) 4_556 . ? C21 C20 C21 117.3(10) . 4_556 ? C21 C20 C19 121.4(5) . . ? C21 C20 C19 121.4(5) 4_556 . ? C22 C21 C20 119.4(8) . . ? C22 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? N2 C22 C21 124.1(8) . . ? N2 C22 H22 117.9 . . ? C21 C22 H22 117.9 . . ? C6 C23 C24 122.7(9) . . ? C6 C23 C28 117.2(9) . . ? C24 C23 C28 120.0 . . ? C25 C24 C23 120.0 . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C26 C25 C24 120.0 . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C27 120.0 . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C26 C27 C28 120.0 . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C27 C28 C23 120.0 . . ? C27 C28 H28 120.0 . . ? C23 C28 H28 120.0 . . ? C17 N1 C17 117.1(11) . 4_556 ? C17 N1 Cu1 121.4(5) . . ? C17 N1 Cu1 121.4(5) 4_556 . ? C22 N2 C22 115.7(10) . 4_556 ? C22 N2 Cu2 122.1(5) . . ? C22 N2 Cu2 122.1(5) 4_556 . ? C1 O1 Cu1 119.1(5) . . ? C1 O2 Cu2 128.9(5) . 1_655 ? C16 O5 Cu1 127.7(5) . . ? C16 O6 Cu2 117.6(5) . 1_655 ? O5 Cu1 O5 159.4(3) . 4_556 ? O5 Cu1 O1 90.7(2) . . ? O5 Cu1 O1 87.9(2) 4_556 . ? O5 Cu1 O1 87.9(2) . 4_556 ? O5 Cu1 O1 90.7(2) 4_556 4_556 ? O1 Cu1 O1 171.8(3) . 4_556 ? O5 Cu1 N1 100.32(15) . . ? O5 Cu1 N1 100.32(15) 4_556 . ? O1 Cu1 N1 94.08(16) . . ? O1 Cu1 N1 94.08(16) 4_556 . ? O5 Cu1 Cu2 79.68(15) . 1_655 ? O5 Cu1 Cu2 79.68(15) 4_556 1_655 ? O1 Cu1 Cu2 85.92(16) . 1_655 ? O1 Cu1 Cu2 85.92(16) 4_556 1_655 ? N1 Cu1 Cu2 180.000(1) . 1_655 ? O2 Cu2 O2 158.9(3) 1_455 4_456 ? O2 Cu2 O6 90.5(2) 1_455 1_455 ? O2 Cu2 O6 88.3(2) 4_456 1_455 ? O2 Cu2 O6 88.3(2) 1_455 4_456 ? O2 Cu2 O6 90.5(2) 4_456 4_456 ? O6 Cu2 O6 173.3(3) 1_455 4_456 ? O2 Cu2 N2 100.53(15) 1_455 . ? O2 Cu2 N2 100.53(15) 4_456 . ? O6 Cu2 N2 93.35(16) 1_455 . ? O6 Cu2 N2 93.35(16) 4_456 . ? O2 Cu2 Cu1 79.47(15) 1_455 1_455 ? O2 Cu2 Cu1 79.47(15) 4_456 1_455 ? O6 Cu2 Cu1 86.65(16) 1_455 1_455 ? O6 Cu2 Cu1 86.65(16) 4_456 1_455 ? N2 Cu2 Cu1 180.000(1) . 1_455 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.08 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.090 _refine_diff_density_min -1.166 _refine_diff_density_rms 0.140 data_complex2 #TrackingRef '- complexes1-4.cif' _database_code_depnum_ccdc_archive 'CCDC 751258' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C54 H14.33 N2 Ni2 O13' _chemical_formula_sum 'C54 H14.33 N2 Ni2 O13' _chemical_formula_weight 1016.43 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P 32 2 1 ' _symmetry_space_group_name_Hall 'P 32 2" ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' 'x-y, -y, -z+1/3' '-x, -x+y, -z+2/3' 'y, x, -z' _cell_length_a 14.096(5) _cell_length_b 14.096(5) _cell_length_c 20.062(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 120.000(5) _cell_volume 3452.2(19) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3254 _cell_measurement_theta_min 1.67 _cell_measurement_theta_max 25.01 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1566 _exptl_absorpt_coefficient_mu 0.887 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.766 _exptl_absorpt_correction_T_max 0.852 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart CCD Apex II' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17548 _diffrn_reflns_av_R_equivalents 0.0829 _diffrn_reflns_av_sigmaI/netI 0.0782 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4057 _reflns_number_gt 3254 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1287P)^2^+8.7229P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(4) _refine_ls_number_reflns 4057 _refine_ls_number_parameters 323 _refine_ls_number_restraints 631 _refine_ls_R_factor_all 0.0966 _refine_ls_R_factor_gt 0.0754 _refine_ls_wR_factor_ref 0.2128 _refine_ls_wR_factor_gt 0.1947 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.1908(8) 0.9644(9) 0.2191(5) 0.044(2) Uani 1 1 d U . . H1 H -0.2373 0.9379 0.2558 0.048(17) Uiso 1 1 calc RU . . C2 C -0.0923(8) 0.9652(9) 0.2211(5) 0.047(2) Uani 1 1 d U . . H2 H -0.0724 0.9422 0.2594 0.047(16) Uiso 1 1 calc RU . . C3 C -0.0236(9) 1.0000 0.1667 0.047(2) Uani 1 2 d SU . . C4 C 0.0813(9) 1.0000 0.1667 0.044(2) Uani 1 2 d SU . . C5 C 0.1445(8) 1.0244(10) 0.2226(6) 0.054(2) Uani 1 1 d U . . H5 H 0.1231 1.0443 0.2616 0.047(16) Uiso 1 1 calc RU . . C6 C 0.2415(8) 1.0196(10) 0.2215(6) 0.050(2) Uani 1 1 d U . . H6 H 0.2797 1.0307 0.2612 0.048(17) Uiso 1 1 calc RU . . C7 C 0.6268(8) 1.1777(7) 0.1018(4) 0.0327(18) Uani 1 1 d U . . C8 C 0.4608(8) 0.8778(8) 0.0650(5) 0.0407(16) Uani 1 1 d U . . C9 C 0.4250(9) 0.7957(8) 0.0091(5) 0.0432(16) Uani 1 1 d U . . C10 C 0.3251(8) 0.7578(8) -0.0226(5) 0.0428(17) Uani 1 1 d U . . H10 H 0.2805 0.7861 -0.0104 0.05(3) Uiso 1 1 calc R . . C11 C 0.2908(8) 0.6806(9) -0.0710(5) 0.0465(17) Uani 1 1 d U . . C12 C 0.3628(10) 0.6436(10) -0.0939(6) 0.0589(19) Uani 1 1 d U . . C13 C 0.4613(10) 0.6808(10) -0.0629(5) 0.0569(17) Uani 1 1 d U . . H13 H 0.5078 0.6563 -0.0778 0.064(14) Uiso 1 1 calc RU . . C14 C 0.4948(9) 0.7543(9) -0.0096(5) 0.0501(17) Uani 1 1 d U . . C15 C 0.6005(10) 0.7798(10) 0.0244(6) 0.0586(19) Uani 1 1 d U . . C16 C 0.5992(10) 0.7202(10) 0.0821(6) 0.0579(18) Uani 1 1 d U . . C17 C 0.5000(12) 0.6421(11) 0.1137(6) 0.066(2) Uani 1 1 d U . . H17 H 0.4334 0.6273 0.0953 0.063(14) Uiso 1 1 calc RU . . C18 C 0.5002(13) 0.5902(12) 0.1685(7) 0.079(3) Uani 1 1 d U . . H18 H 0.4342 0.5382 0.1875 0.064(14) Uiso 1 1 calc RU . . C19 C 0.5915(14) 0.6114(12) 0.1956(8) 0.085(3) Uani 1 1 d U . . H19 H 0.5880 0.5749 0.2350 0.068(15) Uiso 1 1 calc RU . . C20 C 0.6865(13) 0.6784(11) 0.1728(7) 0.071(2) Uani 1 1 d U . . H20 H 0.7495 0.6882 0.1940 0.060(15) Uiso 1 1 calc RU . . C21 C 0.6932(13) 0.7373(12) 0.1142(7) 0.070(2) Uani 1 1 d U . . H21 H 0.7614 0.7880 0.0971 0.050(17) Uiso 1 1 calc RU . . C22 C 0.3424(11) 0.5786(12) -0.1565(8) 0.071(2) Uani 1 1 d U . . C23 C 0.3263(9) 0.4768(7) -0.1652(6) 0.086(2) Uani 1 1 d GU . . C24 C 0.3322(9) 0.4415(9) -0.2290(5) 0.103(3) Uani 1 1 d GU . . H24 H 0.3466 0.4878 -0.2652 0.11(2) Uiso 1 1 calc RU . . C25 C 0.3167(10) 0.3370(9) -0.2385(5) 0.110(3) Uani 1 1 d GU . . H25 H 0.3207 0.3134 -0.2812 0.107(19) Uiso 1 1 calc RU . . C26 C 0.2953(9) 0.2678(7) -0.1843(6) 0.109(3) Uani 1 1 d GU . . H26 H 0.2850 0.1979 -0.1907 0.099(17) Uiso 1 1 calc RU . . C27 C 0.2894(10) 0.3030(9) -0.1205(5) 0.115(3) Uani 1 1 d GU . . H27 H 0.2751 0.2567 -0.0842 0.081(16) Uiso 1 1 calc RU . . C28 C 0.3049(9) 0.4075(10) -0.1110(4) 0.099(3) Uani 1 1 d GU . . H28 H 0.3009 0.4311 -0.0683 0.065(15) Uiso 1 1 calc RU . . N1 N -0.2213(7) 1.0000 0.1667 0.034(2) Uani 1 2 d S . . N2 N 0.2813(8) 1.0000 0.1667 0.040(3) Uani 1 2 d S . . Ni1 Ni -0.37469(9) 1.0000 0.1667 0.0179(3) Uani 1 2 d S . . Ni2 Ni 0.43380(9) 1.0000 0.1667 0.0186(3) Uani 1 2 d S . . O1 O -0.3174(5) 1.1313(5) 0.1074(3) 0.0357(14) Uani 1 1 d . . . O2 O 0.5289(5) 1.1391(5) 0.1197(3) 0.0380(16) Uani 1 1 d . . . O3 O 0.4020(5) 0.9168(5) 0.0817(3) 0.0325(14) Uani 1 1 d . . . O4 O 0.5527(5) 0.9044(5) 0.0911(3) 0.0378(15) Uani 1 1 d . . . O5 O 0.6859(7) 0.8470(9) -0.0041(5) 0.081(3) Uani 1 1 d . . . O6 O 0.3518(9) 0.6237(13) -0.2077(5) 0.116(4) 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 C1 0.034(4) 0.058(5) 0.049(4) 0.007(4) 0.002(4) 0.030(3) C2 0.032(4) 0.068(5) 0.052(4) 0.011(4) 0.000(3) 0.034(3) C3 0.035(4) 0.066(5) 0.051(5) -0.002(4) -0.001(2) 0.033(2) C4 0.030(3) 0.068(5) 0.047(5) 0.003(4) 0.0015(19) 0.034(2) C5 0.036(4) 0.076(5) 0.056(4) -0.004(4) 0.004(4) 0.033(4) C6 0.031(4) 0.076(5) 0.048(5) -0.010(4) -0.001(4) 0.030(4) C7 0.043(5) 0.035(4) 0.029(4) -0.001(3) 0.003(4) 0.026(4) C8 0.047(3) 0.049(3) 0.046(3) -0.008(3) -0.013(3) 0.039(3) C9 0.049(3) 0.054(3) 0.048(3) -0.017(3) -0.011(3) 0.042(3) C10 0.049(3) 0.054(3) 0.047(3) -0.017(3) -0.013(3) 0.042(3) C11 0.048(3) 0.061(3) 0.050(3) -0.019(3) -0.014(3) 0.042(3) C12 0.059(3) 0.069(3) 0.064(3) -0.023(3) -0.011(3) 0.044(3) C13 0.059(3) 0.067(3) 0.063(3) -0.023(3) -0.012(3) 0.044(3) C14 0.054(3) 0.060(3) 0.054(3) -0.021(3) -0.015(3) 0.041(3) C15 0.062(3) 0.065(3) 0.061(3) -0.023(3) -0.011(3) 0.040(3) C16 0.068(3) 0.061(3) 0.064(3) -0.019(3) -0.017(3) 0.047(3) C17 0.071(3) 0.069(3) 0.069(3) -0.012(3) -0.014(3) 0.044(3) C18 0.089(4) 0.075(4) 0.075(4) -0.009(4) -0.012(4) 0.043(4) C19 0.094(5) 0.079(5) 0.077(5) -0.014(4) -0.016(4) 0.040(4) C20 0.081(4) 0.074(4) 0.075(4) -0.012(4) -0.020(4) 0.051(4) C21 0.078(4) 0.070(4) 0.076(4) -0.017(4) -0.023(4) 0.048(4) C22 0.068(3) 0.079(3) 0.078(4) -0.023(3) -0.015(3) 0.046(3) C23 0.082(4) 0.087(4) 0.092(4) -0.025(3) -0.011(3) 0.043(3) C24 0.095(4) 0.098(4) 0.110(4) -0.024(4) -0.010(4) 0.043(4) C25 0.103(4) 0.100(4) 0.113(4) -0.024(4) -0.010(4) 0.041(4) C26 0.104(5) 0.099(5) 0.112(5) -0.019(4) -0.009(4) 0.040(4) C27 0.104(4) 0.107(4) 0.115(4) -0.018(4) -0.007(4) 0.038(4) C28 0.092(4) 0.091(4) 0.104(4) -0.022(4) -0.006(4) 0.039(3) N1 0.022(4) 0.027(5) 0.054(7) 0.003(5) 0.002(2) 0.014(3) N2 0.036(4) 0.057(7) 0.032(6) 0.002(5) 0.001(3) 0.029(4) Ni1 0.0143(5) 0.0175(7) 0.0228(7) -0.0008(5) -0.0004(3) 0.0088(3) Ni2 0.0153(5) 0.0197(7) 0.0225(7) -0.0007(5) -0.0004(3) 0.0098(4) O1 0.040(3) 0.041(4) 0.035(3) 0.007(3) 0.012(3) 0.026(3) O2 0.034(4) 0.032(3) 0.051(4) 0.013(3) 0.009(3) 0.019(3) O3 0.034(3) 0.034(3) 0.032(3) -0.011(2) -0.008(3) 0.019(3) O4 0.035(4) 0.046(4) 0.038(3) -0.011(3) -0.006(3) 0.024(3) O5 0.055(5) 0.098(7) 0.081(6) -0.029(5) -0.016(5) 0.031(5) O6 0.084(7) 0.198(14) 0.057(6) -0.037(7) -0.008(5) 0.064(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 C1 N1 1.327(11) . ? C1 C2 1.383(13) . ? C1 H1 0.9300 . ? C2 C3 1.377(12) . ? C2 H2 0.9300 . ? C3 C2 1.377(12) 4_675 ? C3 C4 1.479(17) . ? C4 C5 1.365(12) . ? C4 C5 1.365(12) 4_675 ? C5 C6 1.402(14) . ? C5 H5 0.9300 . ? C6 N2 1.326(12) . ? C6 H6 0.9300 . ? C7 O1 1.255(11) 1_655 ? C7 O2 1.256(11) . ? C7 C11 1.513(12) 6_565 ? C8 O3 1.248(11) . ? C8 O4 1.267(11) . ? C8 C9 1.506(13) . ? C9 C10 1.386(14) . ? C9 C14 1.422(13) . ? C10 C11 1.354(13) . ? C10 H10 0.9300 . ? C11 C12 1.428(14) . ? C11 C7 1.513(12) 6_455 ? C12 C13 1.364(16) . ? C12 C22 1.495(16) . ? C13 C14 1.396(14) . ? C13 H13 0.9300 . ? C14 C15 1.511(16) . ? C15 O5 1.238(15) . ? C15 C16 1.424(17) . ? C16 C21 1.381(17) . ? C16 C17 1.425(19) . ? C17 C18 1.320(18) . ? C17 H17 0.9300 . ? C18 C19 1.29(2) . ? C18 H18 0.9300 . ? C19 C20 1.28(2) . ? C19 H19 0.9300 . ? C20 C21 1.415(18) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 O6 1.181(17) . ? C22 C23 1.348(16) . ? C23 C24 1.3900 . ? C23 C28 1.3900 . ? C24 C25 1.3900 . ? C24 H24 0.9300 . ? C25 C26 1.3900 . ? C25 H25 0.9300 . ? C26 C27 1.3900 . ? C26 H26 0.9300 . ? C27 C28 1.3900 . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? N1 C1 1.327(11) 4_675 ? N1 Ni1 2.162(10) . ? N2 C6 1.326(12) 4_675 ? N2 Ni2 2.150(11) . ? Ni1 O4 1.945(6) 4_575 ? Ni1 O4 1.945(6) 1_455 ? Ni1 O1 1.999(6) 4_675 ? Ni1 O1 1.999(6) . ? Ni1 Ni2 2.700(2) 1_455 ? Ni2 O2 1.974(6) 4_675 ? Ni2 O2 1.974(6) . ? Ni2 O3 1.990(5) 4_675 ? Ni2 O3 1.990(5) . ? Ni2 Ni1 2.700(2) 1_655 ? O1 C7 1.255(11) 1_455 ? O4 Ni1 1.945(6) 1_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 122.2(10) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C3 C2 C1 120.3(10) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C2 C3 C2 116.6(12) . 4_675 ? C2 C3 C4 121.7(6) . . ? C2 C3 C4 121.7(6) 4_675 . ? C5 C4 C5 116.5(13) . 4_675 ? C5 C4 C3 121.7(6) . . ? C5 C4 C3 121.7(6) 4_675 . ? C4 C5 C6 120.3(11) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? N2 C6 C5 123.2(11) . . ? N2 C6 H6 118.4 . . ? C5 C6 H6 118.4 . . ? O1 C7 O2 125.9(8) 1_655 . ? O1 C7 C11 118.2(8) 1_655 6_565 ? O2 C7 C11 115.9(8) . 6_565 ? O3 C8 O4 124.4(8) . . ? O3 C8 C9 119.7(8) . . ? O4 C8 C9 115.8(8) . . ? C10 C9 C14 119.9(8) . . ? C10 C9 C8 121.6(8) . . ? C14 C9 C8 118.5(9) . . ? C11 C10 C9 121.6(8) . . ? C11 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? C10 C11 C12 119.4(9) . . ? C10 C11 C7 123.9(8) . 6_455 ? C12 C11 C7 116.7(8) . 6_455 ? C13 C12 C11 119.0(9) . . ? C13 C12 C22 117.7(10) . . ? C11 C12 C22 122.6(10) . . ? C12 C13 C14 122.4(10) . . ? C12 C13 H13 118.8 . . ? C14 C13 H13 118.8 . . ? C13 C14 C9 117.4(10) . . ? C13 C14 C15 116.7(9) . . ? C9 C14 C15 125.8(9) . . ? O5 C15 C16 123.2(12) . . ? O5 C15 C14 116.0(12) . . ? C16 C15 C14 120.5(12) . . ? C21 C16 C15 123.2(13) . . ? C21 C16 C17 114.3(12) . . ? C15 C16 C17 122.4(11) . . ? C18 C17 C16 121.7(14) . . ? C18 C17 H17 119.1 . . ? C16 C17 H17 119.1 . . ? C19 C18 C17 120.1(17) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C20 C19 C18 125.3(17) . . ? C20 C19 H19 117.4 . . ? C18 C19 H19 117.4 . . ? C19 C20 C21 118.0(14) . . ? C19 C20 H20 121.0 . . ? C21 C20 H20 121.0 . . ? C16 C21 C20 120.6(15) . . ? C16 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? O6 C22 C23 112.0(14) . . ? O6 C22 C12 117.8(13) . . ? C23 C22 C12 129.8(14) . . ? C22 C23 C24 119.5(11) . . ? C22 C23 C28 120.5(11) . . ? C24 C23 C28 120.0 . . ? C25 C24 C23 120.0 . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 120.0 . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C27 C26 C25 120.0 . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C28 C27 C26 120.0 . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C27 C28 C23 120.0 . . ? C27 C28 H28 120.0 . . ? C23 C28 H28 120.0 . . ? C1 N1 C1 118.2(11) . 4_675 ? C1 N1 Ni1 120.9(6) . . ? C1 N1 Ni1 120.9(6) 4_675 . ? C6 N2 C6 116.3(13) . 4_675 ? C6 N2 Ni2 121.9(6) . . ? C6 N2 Ni2 121.9(6) 4_675 . ? O4 Ni1 O4 159.2(3) 4_575 1_455 ? O4 Ni1 O1 90.4(3) 4_575 4_675 ? O4 Ni1 O1 88.4(3) 1_455 4_675 ? O4 Ni1 O1 88.4(3) 4_575 . ? O4 Ni1 O1 90.4(3) 1_455 . ? O1 Ni1 O1 173.2(4) 4_675 . ? O4 Ni1 N1 100.38(17) 4_575 . ? O4 Ni1 N1 100.38(17) 1_455 . ? O1 Ni1 N1 93.39(18) 4_675 . ? O1 Ni1 N1 93.39(18) . . ? O4 Ni1 Ni2 79.62(17) 4_575 1_455 ? O4 Ni1 Ni2 79.62(17) 1_455 1_455 ? O1 Ni1 Ni2 86.61(18) 4_675 1_455 ? O1 Ni1 Ni2 86.61(18) . 1_455 ? N1 Ni1 Ni2 180.000(1) . 1_455 ? O2 Ni2 O2 158.9(4) 4_675 . ? O2 Ni2 O3 91.0(3) 4_675 4_675 ? O2 Ni2 O3 87.5(3) . 4_675 ? O2 Ni2 O3 87.5(3) 4_675 . ? O2 Ni2 O3 91.0(3) . . ? O3 Ni2 O3 172.1(4) 4_675 . ? O2 Ni2 N2 100.53(18) 4_675 . ? O2 Ni2 N2 100.53(18) . . ? O3 Ni2 N2 93.97(18) 4_675 . ? O3 Ni2 N2 93.97(18) . . ? O2 Ni2 Ni1 79.47(18) 4_675 1_655 ? O2 Ni2 Ni1 79.47(18) . 1_655 ? O3 Ni2 Ni1 86.03(18) 4_675 1_655 ? O3 Ni2 Ni1 86.03(18) . 1_655 ? N2 Ni2 Ni1 180.000(1) . 1_655 ? C7 O1 Ni1 117.9(6) 1_455 . ? C7 O2 Ni2 128.4(6) . . ? C8 O3 Ni2 119.0(6) . . ? C8 O4 Ni1 129.3(6) . 1_655 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.916 _refine_diff_density_min -1.082 _refine_diff_density_rms 0.145 data_complex3 #TrackingRef '- complexes1-4.cif' _database_code_depnum_ccdc_archive 'CCDC 760284' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C186 H126 Cu5 N4 O58, 4(H2 O)' _chemical_formula_sum 'C186 H134 Cu10 N4 O62 ' _chemical_formula_weight 4052.23 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 14.9031(7) _cell_length_b 18.2115(6) _cell_length_c 18.3710(5) _cell_angle_alpha 94.803(2) _cell_angle_beta 101.600(3) _cell_angle_gamma 113.983(4) _cell_volume 4385.6(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.90 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.534 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064 _exptl_absorpt_coefficient_mu 1.280 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.688 _exptl_absorpt_correction_T_max 0.726 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'multiwire proportional' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26714 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_sigmaI/netI 0.1261 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 25.02 _reflns_number_total 15501 _reflns_number_gt 8500 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0475P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15417 _refine_ls_number_parameters 1180 _refine_ls_number_restraints 3601 _refine_ls_R_factor_all 0.0943 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1029 _refine_ls_wR_factor_gt 0.0955 _refine_ls_goodness_of_fit_ref 0.859 _refine_ls_restrained_S_all 0.937 _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 0.73901(4) 0.13445(4) 0.32964(3) 0.02193(15) Uani 1 1 d . . . Cu2 Cu 0.71843(5) 0.03299(4) 0.16937(3) 0.02716(16) Uani 1 1 d . . . Cu3 Cu 0.84038(4) -0.09569(4) 0.15704(3) 0.02184(15) Uani 1 1 d . . . Cu4 Cu 0.84250(5) 0.01615(4) 0.30814(3) 0.03095(17) Uani 1 1 d . . . Cu5 Cu 0.92261(5) 0.43027(4) -0.03666(3) 0.02419(15) Uani 1 1 d . . . O1 O 0.7859(2) 0.1173(2) 0.43222(15) 0.0265(7) Uani 1 1 d U . . O2 O 0.8505(3) 0.0271(2) 0.41579(16) 0.0344(8) Uani 1 1 d U . . O1W O 0.7325(4) -0.1251(3) 0.2956(3) 0.0915(16) Uani 1 1 d U . . H1C H 0.7372 -0.1557 0.2627 0.137 Uiso 1 1 d R . . H1D H 0.7221 -0.1422 0.3345 0.137 Uiso 1 1 d R . . O2W O 0.9581(3) -0.0332(3) 0.08717(19) 0.0653(14) Uani 1 1 d U . . H2C H 0.9229 -0.0608 0.0455 0.098 Uiso 1 1 d R . . H2D H 1.0197 -0.0163 0.0935 0.098 Uiso 1 1 d R . . O3W O 0.7824(3) 0.3278(2) -0.0971(2) 0.0541(11) Uani 1 1 d U . . H3C H 0.7455 0.3459 -0.1205 0.081 Uiso 1 1 d R . . H3D H 0.7544 0.2891 -0.0771 0.081 Uiso 1 1 d R . . O3 O 0.6267(2) 0.1359(2) 0.25423(16) 0.0323(8) Uani 1 1 d U . . O4 O 0.5952(3) 0.0499(2) 0.14770(16) 0.0347(8) Uani 1 1 d U . . O5 O 0.3253(3) 0.0244(2) -0.06676(15) 0.0373(9) Uani 1 1 d U . . O6 O 0.2679(2) 0.1209(2) -0.06597(15) 0.0300(8) Uani 1 1 d U . . O7 O 1.0375(2) 0.0745(2) 0.76381(16) 0.0333(8) Uani 1 1 d U . . O8 O 1.0330(3) -0.0075(2) 0.66454(17) 0.0451(9) Uani 1 1 d U . . O9 O 0.8222(2) 0.1581(2) 0.18116(16) 0.0328(8) Uani 1 1 d U . . O10 O 0.8946(3) 0.1664(2) 0.30222(16) 0.0331(8) Uani 1 1 d U . . O11 O 0.8266(3) -0.2061(2) 0.13183(17) 0.0336(8) Uani 1 1 d U . . O12 O 0.7104(3) -0.2472(2) 0.1966(2) 0.0623(11) Uani 1 1 d U . . O13 O 0.8485(3) -0.5248(2) 0.01613(17) 0.0341(8) Uani 1 1 d U . . O14 O 0.9787(3) -0.4048(2) 0.07617(18) 0.0378(9) Uani 1 1 d U . . O15 O 0.7156(2) 0.02739(19) 0.28033(14) 0.0233(7) Uani 1 1 d U . . H15A H 0.6639 -0.0121 0.2865 0.028 Uiso 1 1 d R . . O16 O 0.8334(2) 0.00446(18) 0.19846(14) 0.0209(7) Uani 1 1 d U . . H16A H 0.8855 0.0443 0.1932 0.025 Uiso 1 1 d R . . O17 O 0.6203(3) 0.1005(3) 0.52295(18) 0.0442(10) Uani 1 1 d U . . O18 O 0.8177(3) -0.0554(2) 0.76908(17) 0.0414(9) Uani 1 1 d U . . O19 O 1.0815(3) 0.5050(2) 0.11691(16) 0.0335(8) Uani 1 1 d U . . O20 O 0.9529(3) 0.3862(2) 0.05390(17) 0.0353(9) Uani 1 1 d U . . O21 O 1.2593(3) 0.5479(3) 0.2608(2) 0.0698(13) Uani 1 1 d U . . O22 O 1.0203(3) 0.3198(3) 0.43685(19) 0.0530(11) Uani 1 1 d U . . O23 O 0.5205(3) -0.4036(3) 0.1503(2) 0.0621(11) Uani 1 1 d U . . O24 O 0.8068(3) -0.5891(2) 0.1751(2) 0.0551(11) Uani 1 1 d U . . O25 O 0.1554(3) 0.1211(2) 0.05478(18) 0.0415(9) Uani 1 1 d U . . O26 O 0.4458(3) 0.1011(2) 0.31507(18) 0.0493(10) Uani 1 1 d U . . N1 N 0.7750(3) 0.2485(2) 0.36667(19) 0.0282(10) Uani 1 1 d . . . N2 N 0.8249(3) 0.3678(3) 0.4369(2) 0.0412(12) Uani 1 1 d . . . C1 C 0.8042(4) 0.2896(4) 0.4360(3) 0.0404(13) Uani 1 1 d U . . H1 H 0.8096 0.2668 0.4791 0.049 Uiso 1 1 calc R . . C2 C 0.8089(5) 0.3781(4) 0.3638(3) 0.0495(14) Uani 1 1 d U . . H2 H 0.8171 0.4267 0.3471 0.059 Uiso 1 1 calc R . . C3 C 0.7791(4) 0.3057(3) 0.3206(3) 0.0384(12) Uani 1 1 d U . . H3 H 0.7636 0.2952 0.2681 0.046 Uiso 1 1 calc R . . C4 C 0.8622(5) 0.4309(4) 0.5051(3) 0.0574(15) Uani 1 1 d U . . H4A H 0.8402 0.4052 0.5465 0.069 Uiso 1 1 calc R . . H4B H 0.8325 0.4688 0.4961 0.069 Uiso 1 1 calc R . . C5 C 0.9763(5) 0.4776(4) 0.5275(3) 0.0626(17) Uani 1 1 d U . . H5A H 0.9956 0.5163 0.5738 0.075 Uiso 1 1 calc R . . H5B H 1.0048 0.4393 0.5389 0.075 Uiso 1 1 calc R . . C6 C 0.8901(4) 0.1944(3) 0.2422(2) 0.0261(10) Uani 1 1 d U . . C7 C 0.9672(4) 0.2800(3) 0.2449(2) 0.0271(10) Uani 1 1 d U . . C8 C 0.9648(4) 0.3155(3) 0.1815(2) 0.0278(10) Uani 1 1 d U . . H8 H 0.9186 0.2838 0.1362 0.033 Uiso 1 1 calc R . . C9 C 1.0282(4) 0.3963(3) 0.1826(2) 0.0309(10) Uani 1 1 d U . . C10 C 1.0976(4) 0.4437(3) 0.2502(3) 0.0344(11) Uani 1 1 d U . . C11 C 1.1004(4) 0.4080(3) 0.3138(3) 0.0360(11) Uani 1 1 d U . . H11 H 1.1470 0.4395 0.3589 0.043 Uiso 1 1 calc R . . C12 C 1.0373(4) 0.3281(3) 0.3128(2) 0.0303(10) Uani 1 1 d U . . C13 C 1.0491(4) 0.2963(3) 0.3861(3) 0.0418(12) Uani 1 1 d U . . C14 C 1.1106(4) 0.2489(3) 0.3967(3) 0.0536(13) Uani 1 1 d DU . . C15 C 1.1781(4) 0.2554(3) 0.3543(3) 0.0694(14) Uani 1 1 d DU . . H15 H 1.1829 0.2865 0.3163 0.083 Uiso 1 1 calc R . . C16 C 1.2398(5) 0.2149(4) 0.3685(3) 0.0880(17) Uani 1 1 d DU . . H16 H 1.2868 0.2189 0.3407 0.106 Uiso 1 1 calc R . . C17 C 1.2299(5) 0.1696(4) 0.4235(4) 0.093(2) Uani 1 1 d DU . . H17 H 1.2697 0.1414 0.4317 0.111 Uiso 1 1 calc R . . C18 C 1.1653(5) 0.1633(4) 0.4670(3) 0.0875(19) Uani 1 1 d DU . . H18 H 1.1623 0.1328 0.5054 0.105 Uiso 1 1 calc R . . C19 C 1.1024(5) 0.2038(4) 0.4530(3) 0.0748(17) Uani 1 1 d DU . . H19 H 1.0561 0.2000 0.4815 0.090 Uiso 1 1 calc R . . C20 C 1.1714(5) 0.5324(4) 0.2613(3) 0.0444(12) Uani 1 1 d U . . C21 C 1.1404(5) 0.5957(3) 0.2843(3) 0.0453(13) Uani 1 1 d U . . C22 C 1.0402(5) 0.5783(4) 0.2767(3) 0.0512(13) Uani 1 1 d U . . H22 H 0.9894 0.5261 0.2551 0.061 Uiso 1 1 calc R . . C23 C 1.0163(6) 0.6404(4) 0.3021(3) 0.0713(17) Uani 1 1 d U . . H23 H 0.9486 0.6308 0.2953 0.086 Uiso 1 1 calc R . . C24 C 1.0929(6) 0.7163(4) 0.3374(3) 0.0711(17) Uani 1 1 d U . . H24 H 1.0761 0.7567 0.3562 0.085 Uiso 1 1 calc R . . C25 C 1.1889(6) 0.7328(4) 0.3449(4) 0.0745(18) Uani 1 1 d U . . H25 H 1.2391 0.7848 0.3680 0.089 Uiso 1 1 calc R . . C26 C 1.2159(6) 0.6733(4) 0.3188(3) 0.0640(16) Uani 1 1 d U . . H26 H 1.2840 0.6851 0.3242 0.077 Uiso 1 1 calc R . . C27 C 1.0204(4) 0.4319(3) 0.1121(3) 0.0282(10) Uani 1 1 d U . . C28 C 0.5753(4) 0.0964(3) 0.1884(2) 0.0253(10) Uani 1 1 d U . . C29 C 0.4846(4) 0.1122(3) 0.1574(2) 0.0240(10) Uani 1 1 d U . . C30 C 0.4389(3) 0.0895(3) 0.0803(2) 0.0252(10) Uani 1 1 d U . . H30 H 0.4606 0.0603 0.0499 0.030 Uiso 1 1 calc R . . C31 C 0.4485(4) 0.1529(3) 0.2033(2) 0.0267(10) Uani 1 1 d U . . C32 C 0.3736(4) 0.1746(3) 0.1706(2) 0.0289(10) Uani 1 1 d U . . H32 H 0.3516 0.2036 0.2011 0.035 Uiso 1 1 calc R . . C33 C 0.3297(4) 0.1539(3) 0.0927(2) 0.0272(10) Uani 1 1 d U . . C34 C 0.2413(4) 0.1751(3) 0.0672(2) 0.0308(10) Uani 1 1 d U . . C35 C 0.2644(4) 0.2616(3) 0.0691(3) 0.0370(11) Uani 1 1 d U . . C36 C 0.3557(5) 0.3175(4) 0.0620(3) 0.0513(13) Uani 1 1 d U . . H36 H 0.4042 0.2996 0.0550 0.062 Uiso 1 1 calc R . . C37 C 0.3791(5) 0.4005(4) 0.0648(3) 0.0653(16) Uani 1 1 d U . . H37 H 0.4404 0.4372 0.0577 0.078 Uiso 1 1 calc R . . C38 C 0.3074(6) 0.4254(4) 0.0783(3) 0.0679(17) Uani 1 1 d U . . H38 H 0.3219 0.4806 0.0831 0.082 Uiso 1 1 calc R . . C39 C 0.2196(6) 0.3733(4) 0.0845(3) 0.0635(15) Uani 1 1 d U . . H39 H 0.1728 0.3925 0.0930 0.076 Uiso 1 1 calc R . . C40 C 0.1927(5) 0.2892(4) 0.0789(3) 0.0548(14) Uani 1 1 d U . . H40 H 0.1286 0.2530 0.0817 0.066 Uiso 1 1 calc R . . C41 C 0.4747(4) 0.1626(4) 0.2888(3) 0.0346(11) Uani 1 1 d U . . C42 C 0.5189(4) 0.2449(4) 0.3368(3) 0.0404(11) Uani 1 1 d U . . C43 C 0.5387(5) 0.3159(4) 0.3088(3) 0.0557(14) Uani 1 1 d U . . H43 H 0.5287 0.3143 0.2570 0.067 Uiso 1 1 calc R . . C44 C 0.5733(5) 0.3902(5) 0.3570(4) 0.0744(17) Uani 1 1 d U . . H44 H 0.5839 0.4377 0.3376 0.089 Uiso 1 1 calc R . . C45 C 0.5914(6) 0.3925(5) 0.4329(4) 0.0759(18) Uani 1 1 d U . . H45 H 0.6161 0.4423 0.4656 0.091 Uiso 1 1 calc R . . C46 C 0.5742(5) 0.3243(5) 0.4609(4) 0.0729(17) Uani 1 1 d U . . H46 H 0.5871 0.3276 0.5130 0.088 Uiso 1 1 calc R . . C47 C 0.5377(5) 0.2488(4) 0.4149(3) 0.0588(15) Uani 1 1 d U . . H47 H 0.5260 0.2018 0.4355 0.071 Uiso 1 1 calc R . . C48 C 0.8191(4) 0.0678(3) 0.4531(2) 0.0274(10) Uani 1 1 d U . . C49 C 0.8220(4) 0.0547(3) 0.5336(2) 0.0240(9) Uani 1 1 d U . . C50 C 0.9057(4) 0.0501(3) 0.5778(2) 0.0258(9) Uani 1 1 d U . . H50 H 0.9600 0.0541 0.5581 0.031 Uiso 1 1 calc R . . C51 C 0.9076(4) 0.0392(3) 0.6522(2) 0.0264(10) Uani 1 1 d U . . C52 C 0.8284(4) 0.0332(3) 0.6819(2) 0.0262(10) Uani 1 1 d U . . C53 C 0.7434(4) 0.0375(3) 0.6373(2) 0.0286(10) Uani 1 1 d U . . H53 H 0.6891 0.0331 0.6572 0.034 Uiso 1 1 calc R . . C54 C 0.7403(4) 0.0483(3) 0.5625(2) 0.0257(10) Uani 1 1 d U . . C55 C 0.6470(4) 0.0477(3) 0.5112(2) 0.0297(10) Uani 1 1 d U . . C56 C 0.5916(4) -0.0211(3) 0.4445(3) 0.0349(11) Uani 1 1 d U . . C57 C 0.5926(4) -0.0962(4) 0.4451(3) 0.0479(13) Uani 1 1 d U . . H57 H 0.6296 -0.1050 0.4878 0.057 Uiso 1 1 calc R . . C58 C 0.5397(5) -0.1583(4) 0.3834(3) 0.0660(16) Uani 1 1 d U . . H58 H 0.5402 -0.2092 0.3842 0.079 Uiso 1 1 calc R . . C59 C 0.4855(5) -0.1438(4) 0.3196(3) 0.0647(17) Uani 1 1 d U . . H59 H 0.4494 -0.1854 0.2774 0.078 Uiso 1 1 calc R . . C60 C 0.4848(4) -0.0706(4) 0.3185(3) 0.0527(14) Uani 1 1 d U . . H60 H 0.4497 -0.0613 0.2751 0.063 Uiso 1 1 calc R . . C61 C 0.5350(4) -0.0096(4) 0.3804(3) 0.0400(12) Uani 1 1 d U . . H61 H 0.5313 0.0401 0.3797 0.048 Uiso 1 1 calc R . . C62 C 0.8262(4) 0.0111(3) 0.7599(2) 0.0310(10) Uani 1 1 d U . . C63 C 0.8375(4) 0.0742(3) 0.8215(2) 0.0330(11) Uani 1 1 d U . . C64 C 0.8719(5) 0.1551(4) 0.8162(3) 0.0510(13) Uani 1 1 d U . . H64 H 0.8825 0.1710 0.7707 0.061 Uiso 1 1 calc R . . C65 C 0.8909(5) 0.2128(4) 0.8772(3) 0.0679(17) Uani 1 1 d U . . H65 H 0.9154 0.2677 0.8732 0.081 Uiso 1 1 calc R . . C66 C 0.8741(5) 0.1901(4) 0.9435(3) 0.0690(17) Uani 1 1 d U . . H66 H 0.8877 0.2297 0.9848 0.083 Uiso 1 1 calc R . . C67 C 0.8380(5) 0.1108(4) 0.9499(3) 0.0638(16) Uani 1 1 d U . . H67 H 0.8252 0.0958 0.9953 0.077 Uiso 1 1 calc R . . C68 C 0.8199(5) 0.0514(4) 0.8891(3) 0.0514(14) Uani 1 1 d U . . H68 H 0.7961 -0.0033 0.8939 0.062 Uiso 1 1 calc R . . C69 C 0.7642(4) -0.2593(3) 0.1584(3) 0.0346(11) Uani 1 1 d U . . C70 C 0.7544(4) -0.3455(3) 0.1430(3) 0.0341(10) Uani 1 1 d U . . C71 C 0.8232(4) -0.3617(3) 0.1116(3) 0.0332(10) Uani 1 1 d U . . H71 H 0.8746 -0.3192 0.0986 0.040 Uiso 1 1 calc R . . C72 C 0.8167(4) -0.4396(3) 0.0992(3) 0.0312(10) Uani 1 1 d U . . C73 C 0.7418(4) -0.5040(3) 0.1215(3) 0.0330(10) Uani 1 1 d U . . C74 C 0.6736(4) -0.4873(3) 0.1526(3) 0.0392(11) Uani 1 1 d U . . H74 H 0.6234 -0.5294 0.1669 0.047 Uiso 1 1 calc R . . C75 C 0.6778(4) -0.4092(3) 0.1633(3) 0.0391(11) Uani 1 1 d U . . C76 C 0.5965(5) -0.3991(4) 0.1929(3) 0.0506(13) Uani 1 1 d U . . C77 C 0.6063(6) -0.3947(4) 0.2762(4) 0.0675(15) Uani 1 1 d U . . C78 C 0.6968(6) -0.3710(4) 0.3254(4) 0.0817(17) Uani 1 1 d U . . H78 H 0.7545 -0.3575 0.3074 0.098 Uiso 1 1 calc R . . C79 C 0.7070(8) -0.3658(5) 0.4048(5) 0.115(2) Uani 1 1 d U . . H79 H 0.7688 -0.3516 0.4395 0.138 Uiso 1 1 calc R . . C80 C 0.6180(8) -0.3834(6) 0.4256(5) 0.110(2) Uani 1 1 d U . . H80 H 0.6230 -0.3741 0.4771 0.132 Uiso 1 1 calc R . . C81 C 0.5284(8) -0.4115(5) 0.3806(5) 0.104(2) Uani 1 1 d U . . H81 H 0.4712 -0.4280 0.3994 0.125 Uiso 1 1 calc R . . C82 C 0.5189(7) -0.4167(5) 0.3011(4) 0.0884(18) Uani 1 1 d U . . H82 H 0.4557 -0.4343 0.2671 0.106 Uiso 1 1 calc R . . C83 C 0.7459(4) -0.5854(3) 0.1230(3) 0.0373(11) Uani 1 1 d U . . C84 C 0.6742(4) -0.6591(3) 0.0645(3) 0.0397(11) Uani 1 1 d U . . C85 C 0.5994(4) -0.6570(4) 0.0080(3) 0.0478(13) Uani 1 1 d U . . H85 H 0.5903 -0.6095 0.0067 0.057 Uiso 1 1 calc R . . C86 C 0.5371(5) -0.7267(4) -0.0475(3) 0.0574(15) Uani 1 1 d U . . H86 H 0.4847 -0.7268 -0.0848 0.069 Uiso 1 1 calc R . . C87 C 0.5548(5) -0.7957(4) -0.0458(4) 0.0648(17) Uani 1 1 d U . . H87 H 0.5154 -0.8416 -0.0836 0.078 Uiso 1 1 calc R . . C88 C 0.6282(5) -0.7975(4) 0.0096(4) 0.0582(15) Uani 1 1 d U . . H88 H 0.6383 -0.8447 0.0099 0.070 Uiso 1 1 calc R . . C89 C 0.6881(5) -0.7304(4) 0.0657(3) 0.0502(14) Uani 1 1 d U . . H89 H 0.7376 -0.7324 0.1043 0.060 Uiso 1 1 calc R . . C90 C 0.3139(4) 0.0827(3) -0.0356(2) 0.0267(10) Uani 1 1 d U . . C91 C 0.3618(4) 0.1094(3) 0.0479(2) 0.0253(10) Uani 1 1 d U . . C92 C 1.0010(4) 0.0355(3) 0.6984(2) 0.0256(10) Uani 1 1 d U . . C93 C 0.8870(4) -0.4575(3) 0.0611(3) 0.0304(10) Uani 1 1 d U . . O4W O 0.0227(3) 0.1219(3) 0.1860(2) 0.0732(14) Uani 1 1 d U . . H4C H 0.0695 0.1202 0.2170 0.110 Uiso 1 1 d R . . H4D H 0.0028 0.0908 0.1453 0.110 Uiso 1 1 d R . . O5W O 0.3778(4) 0.6625(3) 0.1885(3) 0.0884(16) Uani 1 1 d . . . H5C H 0.3415 0.6295 0.2101 0.133 Uiso 1 1 d R . . H5D H 0.4178 0.6460 0.1774 0.133 Uiso 1 1 d 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 0.0253(4) 0.0236(4) 0.0176(3) 0.0016(2) -0.0013(2) 0.0148(3) Cu2 0.0295(4) 0.0341(4) 0.0203(3) -0.0036(2) -0.0052(2) 0.0231(3) Cu3 0.0248(4) 0.0217(4) 0.0201(3) 0.0028(2) -0.0013(2) 0.0147(3) Cu4 0.0353(4) 0.0528(5) 0.0177(3) 0.0047(3) 0.0021(2) 0.0342(4) Cu5 0.0284(4) 0.0173(4) 0.0309(3) 0.0075(2) 0.0123(2) 0.0111(3) O1 0.0324(16) 0.0316(16) 0.0208(13) 0.0077(12) 0.0043(12) 0.0195(14) O2 0.0430(17) 0.0499(19) 0.0229(14) 0.0092(13) 0.0050(13) 0.0335(15) O1W 0.126(4) 0.054(3) 0.097(3) 0.007(2) 0.057(3) 0.029(3) O2W 0.036(2) 0.082(3) 0.051(2) 0.002(2) 0.0070(18) 0.002(2) O3W 0.043(3) 0.032(3) 0.074(3) 0.0047(19) 0.010(2) 0.007(2) O3 0.0355(16) 0.0352(16) 0.0260(14) -0.0031(12) -0.0076(12) 0.0239(13) O4 0.0346(18) 0.045(2) 0.0289(16) -0.0081(14) -0.0065(13) 0.0309(16) O5 0.043(2) 0.051(2) 0.0212(16) -0.0077(14) -0.0091(14) 0.0343(17) O6 0.0359(18) 0.0326(18) 0.0245(14) 0.0015(13) -0.0055(13) 0.0246(15) O7 0.0389(18) 0.0429(19) 0.0247(15) 0.0010(13) -0.0011(13) 0.0293(15) O8 0.044(2) 0.076(2) 0.0254(16) -0.0042(16) -0.0023(14) 0.0441(19) O9 0.0351(17) 0.0259(17) 0.0338(15) 0.0075(13) 0.0001(13) 0.0133(14) O10 0.0405(16) 0.0296(16) 0.0271(14) 0.0095(12) 0.0073(12) 0.0130(13) O11 0.044(2) 0.028(2) 0.0371(17) 0.0056(14) 0.0080(15) 0.0254(17) O12 0.082(3) 0.042(2) 0.084(3) 0.0046(19) 0.050(2) 0.035(2) O13 0.0384(18) 0.0299(18) 0.0420(16) 0.0039(14) 0.0189(14) 0.0191(15) O14 0.040(2) 0.0269(19) 0.0515(18) 0.0034(15) 0.0211(15) 0.0155(17) O15 0.0267(15) 0.0277(16) 0.0201(13) 0.0055(12) 0.0039(11) 0.0169(13) O16 0.0205(17) 0.0209(17) 0.0229(14) 0.0041(12) 0.0013(12) 0.0125(14) O17 0.038(2) 0.062(3) 0.046(2) 0.0114(18) 0.0078(16) 0.035(2) O18 0.068(3) 0.035(2) 0.0346(18) 0.0144(16) 0.0193(16) 0.032(2) O19 0.0426(19) 0.0257(18) 0.0365(16) 0.0123(14) 0.0157(14) 0.0153(15) O20 0.043(2) 0.0261(19) 0.0349(17) 0.0104(14) 0.0068(15) 0.0143(16) O21 0.046(3) 0.052(3) 0.098(3) 0.021(2) 0.014(2) 0.010(2) O22 0.057(2) 0.059(3) 0.0375(19) 0.0055(17) 0.0156(17) 0.019(2) O23 0.054(3) 0.061(3) 0.087(3) 0.013(2) 0.027(2) 0.037(2) O24 0.067(3) 0.039(2) 0.063(2) 0.0134(18) 0.009(2) 0.030(2) O25 0.028(2) 0.050(2) 0.047(2) 0.0126(17) 0.0048(16) 0.0197(19) O26 0.060(2) 0.050(2) 0.0379(19) 0.0165(18) 0.0070(17) 0.026(2) N1 0.034(3) 0.021(2) 0.025(2) -0.0017(17) -0.0025(17) 0.014(2) N2 0.047(3) 0.024(3) 0.046(3) -0.007(2) 0.008(2) 0.013(2) C1 0.048(3) 0.037(3) 0.036(2) 0.003(2) 0.004(2) 0.022(2) C2 0.059(3) 0.035(3) 0.050(3) 0.004(2) 0.006(2) 0.021(2) C3 0.048(2) 0.035(2) 0.031(2) 0.0037(18) 0.0005(18) 0.0220(19) C4 0.064(3) 0.044(3) 0.052(3) -0.015(2) 0.011(2) 0.018(3) C5 0.070(4) 0.045(3) 0.050(3) -0.012(2) 0.009(3) 0.009(3) C6 0.0316(19) 0.0252(19) 0.0282(18) 0.0044(16) 0.0114(16) 0.0171(16) C7 0.0323(19) 0.0256(19) 0.0304(18) 0.0087(16) 0.0100(15) 0.0178(16) C8 0.031(2) 0.027(2) 0.0305(18) 0.0082(16) 0.0087(16) 0.0164(17) C9 0.037(2) 0.027(2) 0.0353(19) 0.0101(16) 0.0143(16) 0.0175(17) C10 0.041(2) 0.026(2) 0.0400(19) 0.0106(16) 0.0141(17) 0.0156(17) C11 0.041(2) 0.030(2) 0.0343(18) 0.0053(17) 0.0068(17) 0.0143(18) C12 0.036(2) 0.0280(19) 0.0329(18) 0.0080(16) 0.0095(16) 0.0189(17) C13 0.043(2) 0.033(2) 0.042(2) 0.0081(18) -0.0002(19) 0.0138(19) C14 0.055(2) 0.041(2) 0.052(2) 0.008(2) -0.009(2) 0.019(2) C15 0.068(3) 0.055(2) 0.070(2) -0.001(2) -0.013(2) 0.029(2) C16 0.080(3) 0.072(3) 0.099(3) -0.010(3) -0.017(3) 0.043(2) C17 0.091(3) 0.064(3) 0.103(3) 0.000(3) -0.025(3) 0.040(3) C18 0.087(3) 0.058(3) 0.090(3) 0.015(3) -0.022(3) 0.025(3) C19 0.072(3) 0.054(3) 0.074(3) 0.014(2) -0.018(2) 0.021(2) C20 0.050(2) 0.035(2) 0.044(2) 0.0137(18) 0.0115(19) 0.013(2) C21 0.060(2) 0.030(2) 0.042(2) 0.0113(18) 0.0139(19) 0.015(2) C22 0.066(2) 0.035(2) 0.053(2) 0.0052(19) 0.016(2) 0.022(2) C23 0.083(3) 0.055(3) 0.073(3) 0.008(3) 0.018(3) 0.028(3) C24 0.098(4) 0.043(3) 0.069(3) 0.003(3) 0.019(3) 0.030(3) C25 0.093(3) 0.042(3) 0.068(3) 0.005(2) 0.013(3) 0.015(3) C26 0.078(3) 0.040(3) 0.059(3) 0.008(2) 0.014(2) 0.013(3) C27 0.036(2) 0.024(2) 0.036(2) 0.0109(17) 0.0159(17) 0.0204(18) C28 0.028(2) 0.031(2) 0.0207(18) 0.0016(16) -0.0007(16) 0.0204(17) C29 0.028(2) 0.030(2) 0.0205(17) 0.0029(16) 0.0009(15) 0.0218(17) C30 0.028(2) 0.033(2) 0.0197(17) 0.0003(16) 0.0016(15) 0.0222(17) C31 0.031(2) 0.034(2) 0.0222(17) 0.0030(16) 0.0021(15) 0.0232(17) C32 0.0342(19) 0.0346(19) 0.0261(17) 0.0009(16) 0.0034(16) 0.0258(17) C33 0.0293(19) 0.034(2) 0.0255(17) 0.0067(16) 0.0019(15) 0.0231(17) C34 0.037(2) 0.040(2) 0.0270(18) 0.0060(17) 0.0059(17) 0.0287(18) C35 0.042(2) 0.042(2) 0.039(2) 0.0075(18) 0.0051(18) 0.0311(19) C36 0.049(2) 0.043(2) 0.064(2) 0.005(2) 0.001(2) 0.028(2) C37 0.061(3) 0.050(3) 0.080(3) 0.005(3) 0.003(3) 0.027(3) C38 0.071(3) 0.049(3) 0.079(3) -0.003(3) 0.002(3) 0.034(3) C39 0.066(3) 0.057(3) 0.079(3) 0.004(3) 0.013(3) 0.043(3) C40 0.056(3) 0.051(3) 0.067(3) 0.010(2) 0.014(2) 0.034(2) C41 0.039(2) 0.043(2) 0.0284(19) 0.0005(18) 0.0037(17) 0.0276(19) C42 0.045(2) 0.047(2) 0.0308(19) -0.0053(18) 0.0030(17) 0.0279(19) C43 0.060(2) 0.049(2) 0.047(2) -0.010(2) 0.000(2) 0.023(2) C44 0.077(3) 0.059(3) 0.071(3) -0.013(2) 0.000(3) 0.027(3) C45 0.075(3) 0.064(3) 0.067(3) -0.029(3) 0.001(3) 0.024(3) C46 0.074(3) 0.072(3) 0.054(3) -0.021(2) 0.004(2) 0.026(3) C47 0.064(3) 0.062(3) 0.041(2) -0.013(2) 0.004(2) 0.028(2) C48 0.0260(19) 0.039(2) 0.0228(17) 0.0080(16) 0.0035(15) 0.0201(17) C49 0.0247(19) 0.034(2) 0.0227(17) 0.0109(15) 0.0083(15) 0.0197(17) C50 0.0264(19) 0.040(2) 0.0217(17) 0.0088(16) 0.0057(15) 0.0246(16) C51 0.032(2) 0.036(2) 0.0233(17) 0.0082(16) 0.0061(15) 0.0260(17) C52 0.033(2) 0.035(2) 0.0207(17) 0.0103(16) 0.0092(16) 0.0221(17) C53 0.0292(19) 0.038(2) 0.0281(17) 0.0128(16) 0.0109(15) 0.0217(17) C54 0.0254(19) 0.035(2) 0.0254(17) 0.0115(16) 0.0056(15) 0.0211(17) C55 0.027(2) 0.041(2) 0.0306(19) 0.0176(17) 0.0111(16) 0.0198(18) C56 0.028(2) 0.043(2) 0.0351(19) 0.0131(18) 0.0074(16) 0.0164(18) C57 0.037(2) 0.051(2) 0.047(2) 0.0105(19) 0.0007(18) 0.015(2) C58 0.055(3) 0.053(3) 0.072(3) 0.004(3) 0.006(2) 0.012(3) C59 0.043(3) 0.065(3) 0.060(3) -0.005(3) 0.007(2) 0.004(3) C60 0.037(2) 0.062(3) 0.046(2) 0.009(2) 0.005(2) 0.012(2) C61 0.029(2) 0.050(2) 0.038(2) 0.0125(18) 0.0028(17) 0.0158(19) C62 0.039(2) 0.036(2) 0.0284(19) 0.0106(17) 0.0128(16) 0.0236(18) C63 0.046(2) 0.033(2) 0.0298(19) 0.0088(17) 0.0148(17) 0.0241(19) C64 0.069(2) 0.043(2) 0.042(2) 0.0083(19) 0.023(2) 0.021(2) C65 0.087(3) 0.042(3) 0.064(3) -0.001(2) 0.023(3) 0.018(3) C66 0.088(3) 0.051(3) 0.058(3) -0.012(3) 0.020(3) 0.025(3) C67 0.089(3) 0.052(3) 0.046(3) 0.001(2) 0.030(2) 0.023(3) C68 0.076(3) 0.039(3) 0.039(2) 0.005(2) 0.025(2) 0.021(2) C69 0.046(2) 0.031(2) 0.039(2) 0.0043(19) 0.0141(19) 0.027(2) C70 0.047(2) 0.030(2) 0.0378(19) 0.0076(17) 0.0177(17) 0.0255(18) C71 0.043(2) 0.028(2) 0.0393(19) 0.0112(17) 0.0174(17) 0.0215(18) C72 0.040(2) 0.028(2) 0.0377(19) 0.0088(17) 0.0178(17) 0.0213(18) C73 0.042(2) 0.027(2) 0.0419(19) 0.0090(17) 0.0194(17) 0.0227(18) C74 0.047(2) 0.034(2) 0.0481(19) 0.0113(17) 0.0252(17) 0.0213(18) C75 0.050(2) 0.035(2) 0.0462(19) 0.0081(18) 0.0245(17) 0.0267(18) C76 0.063(2) 0.039(2) 0.060(2) 0.006(2) 0.029(2) 0.027(2) C77 0.078(3) 0.056(3) 0.076(3) 0.008(2) 0.041(2) 0.028(2) C78 0.093(3) 0.064(3) 0.075(3) 0.002(2) 0.035(2) 0.017(3) C79 0.123(4) 0.087(4) 0.102(4) 0.000(3) 0.029(3) 0.015(4) C80 0.125(4) 0.087(4) 0.097(4) -0.010(3) 0.047(3) 0.023(4) C81 0.113(4) 0.090(4) 0.104(3) 0.005(3) 0.056(3) 0.028(3) C82 0.099(3) 0.079(3) 0.092(3) 0.012(3) 0.047(3) 0.034(3) C83 0.042(2) 0.032(2) 0.050(2) 0.0130(18) 0.0244(18) 0.0209(18) C84 0.043(2) 0.029(2) 0.055(2) 0.0127(18) 0.0241(18) 0.0172(19) C85 0.046(2) 0.037(2) 0.064(2) 0.011(2) 0.023(2) 0.017(2) C86 0.048(3) 0.049(3) 0.068(3) 0.010(2) 0.022(2) 0.010(3) C87 0.057(3) 0.043(3) 0.077(3) -0.005(3) 0.030(3) 0.002(3) C88 0.056(3) 0.036(3) 0.081(3) 0.008(2) 0.028(2) 0.015(2) C89 0.049(3) 0.035(3) 0.070(3) 0.010(2) 0.026(2) 0.017(2) C90 0.026(2) 0.033(2) 0.0227(19) 0.0014(18) 0.0012(17) 0.0175(19) C91 0.030(2) 0.031(2) 0.0203(17) 0.0021(16) 0.0018(16) 0.0217(17) C92 0.029(2) 0.040(2) 0.0197(19) 0.0107(17) 0.0079(16) 0.0256(19) C93 0.041(2) 0.025(2) 0.040(2) 0.0153(18) 0.0185(18) 0.0234(19) O4W 0.063(3) 0.064(3) 0.094(3) 0.016(3) 0.022(2) 0.028(3) O5W 0.069(3) 0.093(4) 0.119(4) 0.040(3) 0.037(3) 0.041(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 O15 1.941(3) . ? Cu1 N1 1.942(4) . ? Cu1 O3 1.958(3) . ? Cu1 O1 1.970(3) . ? Cu1 O10 2.322(4) . ? Cu2 O5 1.922(3) 2_655 ? Cu2 O4 1.954(3) . ? Cu2 O16 1.973(3) . ? Cu2 O15 2.057(3) . ? Cu2 O9 2.132(3) . ? Cu2 Cu4 2.9509(7) . ? Cu3 O11 1.942(3) . ? Cu3 O6 1.948(3) 2_655 ? Cu3 O7 1.962(3) 2_756 ? Cu3 O16 1.967(3) . ? Cu3 O2W 2.355(4) . ? Cu4 O8 1.897(4) 2_756 ? Cu4 O2 1.946(3) . ? Cu4 O15 1.955(3) . ? Cu4 O16 1.980(3) . ? Cu4 O1W 2.383(5) . ? Cu5 O20 1.957(3) . ? Cu5 O14 1.957(4) 2_755 ? Cu5 O13 1.966(3) 1_565 ? Cu5 O19 1.970(3) 2_765 ? Cu5 O3W 2.152(3) . ? Cu5 Cu5 2.6460(12) 2_765 ? O1 C48 1.246(6) . ? O2 C48 1.250(6) . ? O1W H1C 0.8199 . ? O1W H1D 0.8200 . ? O2W H2C 0.8200 . ? O2W H2D 0.8200 . ? O3W H3C 0.8203 . ? O3W H3D 0.8200 . ? O3 C28 1.265(5) . ? O4 C28 1.245(6) . ? O5 C90 1.252(6) . ? O5 Cu2 1.922(3) 2_655 ? O6 C90 1.251(6) . ? O6 Cu3 1.948(3) 2_655 ? O7 C92 1.234(5) . ? O7 Cu3 1.962(3) 2_756 ? O8 C92 1.252(6) . ? O8 Cu4 1.897(4) 2_756 ? O9 C6 1.262(5) . ? O10 C6 1.254(5) . ? O11 C69 1.253(6) . ? O12 C69 1.236(6) . ? O13 C93 1.257(6) . ? O13 Cu5 1.966(3) 1_545 ? O14 C93 1.266(6) . ? O14 Cu5 1.957(4) 2_755 ? O15 H15A 0.8499 . ? O16 H16A 0.8499 . ? O17 C55 1.199(6) . ? O18 C62 1.197(6) . ? O19 C27 1.253(6) . ? O19 Cu5 1.970(3) 2_765 ? O20 C27 1.259(5) . ? O21 C20 1.225(7) . ? O22 C13 1.217(6) . ? O23 C76 1.208(7) . ? O24 C83 1.206(6) . ? O25 C34 1.217(6) . ? O26 C41 1.207(6) . ? N1 C1 1.313(6) . ? N1 C3 1.387(6) . ? N2 C1 1.326(7) . ? N2 C2 1.358(6) . ? N2 C4 1.469(6) . ? C1 H1 0.9300 . ? C2 C3 1.332(7) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 C5 1.506(8) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C5 1.463(11) 2_766 ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.504(7) . ? C7 C8 1.380(6) . ? C7 C12 1.401(6) . ? C8 C9 1.384(7) . ? C8 H8 0.9300 . ? C9 C10 1.392(7) . ? C9 C27 1.501(6) . ? C10 C11 1.384(6) . ? C10 C20 1.506(7) . ? C11 C12 1.370(7) . ? C11 H11 0.9300 . ? C12 C13 1.516(7) . ? C13 C14 1.490(8) . ? C14 C19 1.367(6) . ? C14 C15 1.368(7) . ? C15 C16 1.394(7) . ? C15 H15 0.9300 . ? C16 C17 1.349(7) . ? C16 H16 0.9300 . ? C17 C18 1.347(7) . ? C17 H17 0.9300 . ? C18 C19 1.411(7) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.467(8) . ? C21 C22 1.369(8) . ? C21 C26 1.391(8) . ? C22 C23 1.390(9) . ? C22 H22 0.9300 . ? C23 C24 1.380(9) . ? C23 H23 0.9300 . ? C24 C25 1.311(10) . ? C24 H24 0.9300 . ? C25 C26 1.383(10) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C28 C29 1.507(6) . ? C29 C30 1.387(6) . ? C29 C31 1.398(6) . ? C30 C91 1.381(6) . ? C30 H30 0.9300 . ? C31 C32 1.375(6) . ? C31 C41 1.516(6) . ? C32 C33 1.396(6) . ? C32 H32 0.9300 . ? C33 C91 1.386(7) . ? C33 C34 1.517(7) . ? C34 C35 1.465(7) . ? C35 C36 1.369(8) . ? C35 C40 1.387(8) . ? C36 C37 1.400(8) . ? C36 H36 0.9300 . ? C37 C38 1.375(9) . ? C37 H37 0.9300 . ? C38 C39 1.302(9) . ? C38 H38 0.9300 . ? C39 C40 1.405(9) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C41 C42 1.484(7) . ? C42 C43 1.373(8) . ? C42 C47 1.396(7) . ? C43 C44 1.388(8) . ? C43 H43 0.9300 . ? C44 C45 1.359(8) . ? C44 H44 0.9300 . ? C45 C46 1.332(10) . ? C45 H45 0.9300 . ? C46 C47 1.383(8) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? C48 C49 1.512(6) . ? C49 C50 1.383(6) . ? C49 C54 1.390(6) . ? C50 C51 1.394(6) . ? C50 H50 0.9300 . ? C51 C52 1.366(6) . ? C51 C92 1.508(6) . ? C52 C53 1.399(6) . ? C52 C62 1.522(6) . ? C53 C54 1.399(6) . ? C53 H53 0.9300 . ? C54 C55 1.510(6) . ? C55 C56 1.500(7) . ? C56 C57 1.374(8) . ? C56 C61 1.389(6) . ? C57 C58 1.374(8) . ? C57 H57 0.9300 . ? C58 C59 1.393(8) . ? C58 H58 0.9300 . ? C59 C60 1.341(9) . ? C59 H59 0.9300 . ? C60 C61 1.362(7) . ? C60 H60 0.9300 . ? C61 H61 0.9300 . ? C62 C63 1.476(7) . ? C63 C64 1.369(7) . ? C63 C68 1.383(7) . ? C64 C65 1.369(8) . ? C64 H64 0.9300 . ? C65 C66 1.356(8) . ? C65 H65 0.9300 . ? C66 C67 1.346(9) . ? C66 H66 0.9300 . ? C67 C68 1.390(7) . ? C67 H67 0.9300 . ? C68 H68 0.9300 . ? C69 C70 1.513(7) . ? C70 C71 1.387(7) . ? C70 C75 1.398(7) . ? C71 C72 1.379(7) . ? C71 H71 0.9300 . ? C72 C73 1.410(7) . ? C72 C93 1.495(7) . ? C73 C74 1.381(7) . ? C73 C83 1.511(7) . ? C74 C75 1.392(7) . ? C74 H74 0.9300 . ? C75 C76 1.492(8) . ? C76 C77 1.501(8) . ? C77 C78 1.340(10) . ? C77 C82 1.383(10) . ? C78 C79 1.426(10) . ? C78 H78 0.9300 . ? C79 C80 1.374(12) . ? C79 H79 0.9300 . ? C80 C81 1.287(11) . ? C80 H80 0.9300 . ? C81 C82 1.431(10) . ? C81 H81 0.9300 . ? C82 H82 0.9300 . ? C83 C84 1.492(7) . ? C84 C85 1.379(8) . ? C84 C89 1.397(8) . ? C85 C86 1.399(8) . ? C85 H85 0.9300 . ? C86 C87 1.386(9) . ? C86 H86 0.9300 . ? C87 C88 1.350(9) . ? C87 H87 0.9300 . ? C88 C89 1.373(8) . ? C88 H88 0.9300 . ? C89 H89 0.9300 . ? C90 C91 1.501(6) . ? O4W H4C 0.8201 . ? O4W H4D 0.8198 . ? O5W H5C 0.8198 . ? O5W H5D 0.8200 . ? 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 O15 Cu1 N1 170.43(15) . . ? O15 Cu1 O3 92.47(13) . . ? N1 Cu1 O3 86.39(15) . . ? O15 Cu1 O1 94.35(13) . . ? N1 Cu1 O1 91.80(14) . . ? O3 Cu1 O1 146.58(14) . . ? O15 Cu1 O10 79.98(13) . . ? N1 Cu1 O10 92.32(15) . . ? O3 Cu1 O10 119.71(12) . . ? O1 Cu1 O10 93.70(12) . . ? O5 Cu2 O4 87.07(13) 2_655 . ? O5 Cu2 O16 94.64(13) 2_655 . ? O4 Cu2 O16 172.37(14) . . ? O5 Cu2 O15 147.64(14) 2_655 . ? O4 Cu2 O15 92.05(13) . . ? O16 Cu2 O15 82.53(12) . . ? O5 Cu2 O9 112.14(14) 2_655 . ? O4 Cu2 O9 96.08(14) . . ? O16 Cu2 O9 90.17(13) . . ? O15 Cu2 O9 100.13(12) . . ? O5 Cu2 Cu4 131.75(11) 2_655 . ? O4 Cu2 Cu4 133.30(9) . . ? O16 Cu2 Cu4 41.79(8) . . ? O15 Cu2 Cu4 41.32(9) . . ? O9 Cu2 Cu4 91.47(8) . . ? O11 Cu3 O6 87.65(14) . 2_655 ? O11 Cu3 O7 87.19(14) . 2_756 ? O6 Cu3 O7 169.66(14) 2_655 2_756 ? O11 Cu3 O16 166.28(14) . . ? O6 Cu3 O16 94.06(13) 2_655 . ? O7 Cu3 O16 93.08(13) 2_756 . ? O11 Cu3 O2W 97.38(16) . . ? O6 Cu3 O2W 88.10(13) 2_655 . ? O7 Cu3 O2W 83.68(13) 2_756 . ? O16 Cu3 O2W 96.29(15) . . ? O8 Cu4 O2 85.24(14) 2_756 . ? O8 Cu4 O15 178.88(16) 2_756 . ? O2 Cu4 O15 94.71(13) . . ? O8 Cu4 O16 95.02(13) 2_756 . ? O2 Cu4 O16 179.62(16) . . ? O15 Cu4 O16 85.04(12) . . ? O8 Cu4 O1W 97.12(19) 2_756 . ? O2 Cu4 O1W 87.75(15) . . ? O15 Cu4 O1W 83.99(17) . . ? O16 Cu4 O1W 91.93(14) . . ? O8 Cu4 Cu2 135.87(10) 2_756 . ? O2 Cu4 Cu2 138.16(11) . . ? O15 Cu4 Cu2 44.02(8) . . ? O16 Cu4 Cu2 41.63(9) . . ? O1W Cu4 Cu2 93.02(13) . . ? O20 Cu5 O14 90.27(15) . 2_755 ? O20 Cu5 O13 87.30(14) . 1_565 ? O14 Cu5 O13 168.18(14) 2_755 1_565 ? O20 Cu5 O19 167.98(14) . 2_765 ? O14 Cu5 O19 87.66(14) 2_755 2_765 ? O13 Cu5 O19 92.32(14) 1_565 2_765 ? O20 Cu5 O3W 98.84(14) . . ? O14 Cu5 O3W 101.15(15) 2_755 . ? O13 Cu5 O3W 90.65(15) 1_565 . ? O19 Cu5 O3W 93.17(14) 2_765 . ? O20 Cu5 Cu5 85.86(10) . 2_765 ? O14 Cu5 Cu5 86.70(10) 2_755 2_765 ? O13 Cu5 Cu5 81.60(10) 1_565 2_765 ? O19 Cu5 Cu5 82.21(10) 2_765 2_765 ? O3W Cu5 Cu5 170.77(12) . 2_765 ? C48 O1 Cu1 130.1(3) . . ? C48 O2 Cu4 127.7(3) . . ? Cu4 O1W H1C 114.9 . . ? Cu4 O1W H1D 117.3 . . ? H1C O1W H1D 117.2 . . ? Cu3 O2W H2C 97.3 . . ? Cu3 O2W H2D 135.8 . . ? H2C O2W H2D 115.9 . . ? Cu5 O3W H3C 107.6 . . ? Cu5 O3W H3D 121.4 . . ? H3C O3W H3D 115.9 . . ? C28 O3 Cu1 135.1(3) . . ? C28 O4 Cu2 126.2(3) . . ? C90 O5 Cu2 133.0(3) . 2_655 ? C90 O6 Cu3 134.6(3) . 2_655 ? C92 O7 Cu3 133.7(3) . 2_756 ? C92 O8 Cu4 129.9(3) . 2_756 ? C6 O9 Cu2 119.9(3) . . ? C6 O10 Cu1 106.2(3) . . ? C69 O11 Cu3 115.6(3) . . ? C93 O13 Cu5 125.7(3) . 1_545 ? C93 O14 Cu5 119.8(3) . 2_755 ? Cu1 O15 Cu4 108.36(14) . . ? Cu1 O15 Cu2 107.79(14) . . ? Cu4 O15 Cu2 94.66(13) . . ? Cu1 O15 H15A 114.7 . . ? Cu4 O15 H15A 114.7 . . ? Cu2 O15 H15A 114.7 . . ? Cu3 O16 Cu2 126.53(14) . . ? Cu3 O16 Cu4 112.92(14) . . ? Cu2 O16 Cu4 96.57(13) . . ? Cu3 O16 H16A 106.4 . . ? Cu2 O16 H16A 106.4 . . ? Cu4 O16 H16A 106.4 . . ? C27 O19 Cu5 124.7(3) . 2_765 ? C27 O20 Cu5 120.8(3) . . ? C1 N1 C3 105.0(4) . . ? C1 N1 Cu1 130.8(4) . . ? C3 N1 Cu1 124.2(3) . . ? C1 N2 C2 107.1(4) . . ? C1 N2 C4 125.6(5) . . ? C2 N2 C4 127.3(5) . . ? N1 C1 N2 111.7(5) . . ? N1 C1 H1 124.1 . . ? N2 C1 H1 124.1 . . ? C3 C2 N2 107.3(5) . . ? C3 C2 H2 126.4 . . ? N2 C2 H2 126.4 . . ? C2 C3 N1 108.9(5) . . ? C2 C3 H3 125.6 . . ? N1 C3 H3 125.6 . . ? N2 C4 C5 112.5(5) . . ? N2 C4 H4A 109.1 . . ? C5 C4 H4A 109.1 . . ? N2 C4 H4B 109.1 . . ? C5 C4 H4B 109.1 . . ? H4A C4 H4B 107.8 . . ? C5 C5 C4 117.1(7) 2_766 . ? C5 C5 H5A 108.0 2_766 . ? C4 C5 H5A 108.0 . . ? C5 C5 H5B 108.0 2_766 . ? C4 C5 H5B 108.0 . . ? H5A C5 H5B 107.3 . . ? O10 C6 O9 124.9(4) . . ? O10 C6 C7 117.3(4) . . ? O9 C6 C7 117.7(4) . . ? C8 C7 C12 118.2(5) . . ? C8 C7 C6 120.3(4) . . ? C12 C7 C6 121.3(4) . . ? C7 C8 C9 122.7(4) . . ? C7 C8 H8 118.7 . . ? C9 C8 H8 118.7 . . ? C8 C9 C10 118.8(4) . . ? C8 C9 C27 120.2(4) . . ? C10 C9 C27 121.0(5) . . ? C11 C10 C9 118.5(5) . . ? C11 C10 C20 115.9(4) . . ? C9 C10 C20 125.6(4) . . ? C12 C11 C10 122.7(4) . . ? C12 C11 H11 118.7 . . ? C10 C11 H11 118.7 . . ? C11 C12 C7 119.1(4) . . ? C11 C12 C13 117.3(4) . . ? C7 C12 C13 123.5(5) . . ? O22 C13 C14 122.9(5) . . ? O22 C13 C12 118.5(5) . . ? C14 C13 C12 117.8(5) . . ? C19 C14 C15 121.5(5) . . ? C19 C14 C13 118.2(5) . . ? C15 C14 C13 120.1(5) . . ? C14 C15 C16 119.3(5) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? C17 C16 C15 118.6(5) . . ? C17 C16 H16 120.7 . . ? C15 C16 H16 120.7 . . ? C18 C17 C16 123.4(5) . . ? C18 C17 H17 118.3 . . ? C16 C17 H17 118.3 . . ? C17 C18 C19 118.4(5) . . ? C17 C18 H18 120.8 . . ? C19 C18 H18 120.8 . . ? C14 C19 C18 118.8(5) . . ? C14 C19 H19 120.6 . . ? C18 C19 H19 120.6 . . ? O21 C20 C21 122.5(6) . . ? O21 C20 C10 117.6(6) . . ? C21 C20 C10 119.2(5) . . ? C22 C21 C26 120.2(6) . . ? C22 C21 C20 121.3(6) . . ? C26 C21 C20 118.3(6) . . ? C21 C22 C23 118.4(6) . . ? C21 C22 H22 120.8 . . ? C23 C22 H22 120.8 . . ? C24 C23 C22 120.0(7) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C25 C24 C23 121.5(8) . . ? C25 C24 H24 119.2 . . ? C23 C24 H24 119.2 . . ? C24 C25 C26 120.3(7) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C25 C26 C21 119.5(7) . . ? C25 C26 H26 120.3 . . ? C21 C26 H26 120.3 . . ? O19 C27 O20 126.0(4) . . ? O19 C27 C9 116.7(4) . . ? O20 C27 C9 117.3(4) . . ? O4 C28 O3 126.5(4) . . ? O4 C28 C29 118.9(4) . . ? O3 C28 C29 114.5(4) . . ? C30 C29 C31 119.0(4) . . ? C30 C29 C28 119.0(4) . . ? C31 C29 C28 121.9(4) . . ? C91 C30 C29 121.4(4) . . ? C91 C30 H30 119.3 . . ? C29 C30 H30 119.3 . . ? C32 C31 C29 119.4(4) . . ? C32 C31 C41 116.7(4) . . ? C29 C31 C41 123.2(4) . . ? C31 C32 C33 121.5(5) . . ? C31 C32 H32 119.3 . . ? C33 C32 H32 119.3 . . ? C91 C33 C32 118.9(4) . . ? C91 C33 C34 126.2(4) . . ? C32 C33 C34 114.5(4) . . ? O25 C34 C35 123.4(5) . . ? O25 C34 C33 118.3(5) . . ? C35 C34 C33 117.7(5) . . ? C36 C35 C40 118.0(6) . . ? C36 C35 C34 122.1(5) . . ? C40 C35 C34 120.0(6) . . ? C35 C36 C37 122.6(6) . . ? C35 C36 H36 118.7 . . ? C37 C36 H36 118.7 . . ? C38 C37 C36 117.2(7) . . ? C38 C37 H37 121.4 . . ? C36 C37 H37 121.4 . . ? C39 C38 C37 121.3(7) . . ? C39 C38 H38 119.3 . . ? C37 C38 H38 119.3 . . ? C38 C39 C40 122.5(7) . . ? C38 C39 H39 118.7 . . ? C40 C39 H39 118.7 . . ? C35 C40 C39 118.3(6) . . ? C35 C40 H40 120.8 . . ? C39 C40 H40 120.8 . . ? O26 C41 C42 121.7(5) . . ? O26 C41 C31 117.3(5) . . ? C42 C41 C31 120.3(5) . . ? C43 C42 C47 119.0(5) . . ? C43 C42 C41 124.0(5) . . ? C47 C42 C41 117.0(5) . . ? C42 C43 C44 120.8(6) . . ? C42 C43 H43 119.6 . . ? C44 C43 H43 119.6 . . ? C45 C44 C43 119.2(7) . . ? C45 C44 H44 120.4 . . ? C43 C44 H44 120.4 . . ? C46 C45 C44 120.6(7) . . ? C46 C45 H45 119.7 . . ? C44 C45 H45 119.7 . . ? C45 C46 C47 122.1(7) . . ? C45 C46 H46 118.9 . . ? C47 C46 H46 118.9 . . ? C46 C47 C42 118.2(7) . . ? C46 C47 H47 120.9 . . ? C42 C47 H47 120.9 . . ? O1 C48 O2 128.1(4) . . ? O1 C48 C49 116.4(4) . . ? O2 C48 C49 115.5(4) . . ? C50 C49 C54 120.8(4) . . ? C50 C49 C48 120.0(4) . . ? C54 C49 C48 119.2(4) . . ? C49 C50 C51 119.1(5) . . ? C49 C50 H50 120.4 . . ? C51 C50 H50 120.4 . . ? C52 C51 C50 121.1(4) . . ? C52 C51 C92 121.7(4) . . ? C50 C51 C92 117.2(4) . . ? C51 C52 C53 120.0(4) . . ? C51 C52 C62 120.1(4) . . ? C53 C52 C62 119.5(4) . . ? C54 C53 C52 119.6(5) . . ? C54 C53 H53 120.2 . . ? C52 C53 H53 120.2 . . ? C49 C54 C53 119.4(4) . . ? C49 C54 C55 119.5(4) . . ? C53 C54 C55 121.0(4) . . ? O17 C55 C56 122.3(5) . . ? O17 C55 C54 121.3(5) . . ? C56 C55 C54 116.3(5) . . ? C57 C56 C61 118.5(5) . . ? C57 C56 C55 122.4(4) . . ? C61 C56 C55 119.1(5) . . ? C58 C57 C56 120.9(6) . . ? C58 C57 H57 119.6 . . ? C56 C57 H57 119.6 . . ? C57 C58 C59 118.9(7) . . ? C57 C58 H58 120.6 . . ? C59 C58 H58 120.6 . . ? C60 C59 C58 120.5(6) . . ? C60 C59 H59 119.7 . . ? C58 C59 H59 119.7 . . ? C59 C60 C61 120.6(6) . . ? C59 C60 H60 119.7 . . ? C61 C60 H60 119.7 . . ? C60 C61 C56 120.5(6) . . ? C60 C61 H61 119.8 . . ? C56 C61 H61 119.8 . . ? O18 C62 C63 122.8(4) . . ? O18 C62 C52 119.1(4) . . ? C63 C62 C52 118.1(5) . . ? C64 C63 C68 118.9(5) . . ? C64 C63 C62 122.4(4) . . ? C68 C63 C62 118.5(5) . . ? C65 C64 C63 120.7(5) . . ? C65 C64 H64 119.7 . . ? C63 C64 H64 119.7 . . ? C66 C65 C64 120.1(6) . . ? C66 C65 H65 119.9 . . ? C64 C65 H65 119.9 . . ? C67 C66 C65 120.6(6) . . ? C67 C66 H66 119.7 . . ? C65 C66 H66 119.7 . . ? C66 C67 C68 120.3(6) . . ? C66 C67 H67 119.9 . . ? C68 C67 H67 119.9 . . ? C63 C68 C67 119.4(6) . . ? C63 C68 H68 120.3 . . ? C67 C68 H68 120.3 . . ? O12 C69 O11 125.5(5) . . ? O12 C69 C70 117.2(5) . . ? O11 C69 C70 117.3(5) . . ? C71 C70 C75 119.4(5) . . ? C71 C70 C69 120.7(5) . . ? C75 C70 C69 119.9(5) . . ? C72 C71 C70 121.2(5) . . ? C72 C71 H71 119.4 . . ? C70 C71 H71 119.4 . . ? C71 C72 C73 120.0(5) . . ? C71 C72 C93 120.9(5) . . ? C73 C72 C93 119.1(5) . . ? C74 C73 C72 118.2(5) . . ? C74 C73 C83 120.2(5) . . ? C72 C73 C83 120.9(5) . . ? C73 C74 C75 122.1(5) . . ? C73 C74 H74 119.0 . . ? C75 C74 H74 119.0 . . ? C74 C75 C70 119.0(5) . . ? C74 C75 C76 117.6(5) . . ? C70 C75 C76 123.4(5) . . ? O23 C76 C75 120.9(5) . . ? O23 C76 C77 121.3(6) . . ? C75 C76 C77 117.3(6) . . ? C78 C77 C82 120.6(7) . . ? C78 C77 C76 121.2(7) . . ? C82 C77 C76 118.2(7) . . ? C77 C78 C79 121.6(8) . . ? C77 C78 H78 119.2 . . ? C79 C78 H78 119.2 . . ? C80 C79 C78 114.4(9) . . ? C80 C79 H79 122.8 . . ? C78 C79 H79 122.8 . . ? C81 C80 C79 126.3(9) . . ? C81 C80 H80 116.8 . . ? C79 C80 H80 116.8 . . ? C80 C81 C82 118.5(9) . . ? C80 C81 H81 120.8 . . ? C82 C81 H81 120.8 . . ? C77 C82 C81 118.1(8) . . ? C77 C82 H82 120.9 . . ? C81 C82 H82 120.9 . . ? O24 C83 C84 121.4(5) . . ? O24 C83 C73 117.1(5) . . ? C84 C83 C73 121.4(5) . . ? C85 C84 C89 119.9(5) . . ? C85 C84 C83 121.9(5) . . ? C89 C84 C83 118.1(5) . . ? C84 C85 C86 119.7(6) . . ? C84 C85 H85 120.2 . . ? C86 C85 H85 120.2 . . ? C87 C86 C85 118.9(6) . . ? C87 C86 H86 120.5 . . ? C85 C86 H86 120.5 . . ? C88 C87 C86 121.2(6) . . ? C88 C87 H87 119.4 . . ? C86 C87 H87 119.4 . . ? C87 C88 C89 120.6(7) . . ? C87 C88 H88 119.7 . . ? C89 C88 H88 119.7 . . ? C88 C89 C84 119.6(6) . . ? C88 C89 H89 120.2 . . ? C84 C89 H89 120.2 . . ? O6 C90 O5 127.6(4) . . ? O6 C90 C91 116.8(4) . . ? O5 C90 C91 115.5(4) . . ? C30 C91 C33 119.7(4) . . ? C30 C91 C90 119.4(4) . . ? C33 C91 C90 120.9(4) . . ? O7 C92 O8 127.6(4) . . ? O7 C92 C51 117.8(4) . . ? O8 C92 C51 114.7(4) . . ? O13 C93 O14 125.9(5) . . ? O13 C93 C72 115.9(5) . . ? O14 C93 C72 118.2(5) . . ? H4C O4W H4D 116.0 . . ? H5C O5W H5D 108.3 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.649 _refine_diff_density_min -0.807 _refine_diff_density_rms 0.080 data_complex4 #TrackingRef '- complexes1-4.cif' _database_code_depnum_ccdc_archive 'CCDC 783468' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C32 H30 Cu N6 O7, H2 O' _chemical_formula_sum 'C32 H32 Cu N6 O8 ' _chemical_formula_weight 692.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.4874(12) _cell_length_b 17.602(2) _cell_length_c 21.025(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.048(2) _cell_angle_gamma 90.00 _cell_volume 3092.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4007 _cell_measurement_theta_min 1.52 _cell_measurement_theta_max 25.00 _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.487 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1436 _exptl_absorpt_coefficient_mu 0.769 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.855 _exptl_absorpt_correction_T_max 0.912 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15361 _diffrn_reflns_av_R_equivalents 0.0451 _diffrn_reflns_av_sigmaI/netI 0.0550 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5443 _reflns_number_gt 4007 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SMART (Bruker, 2002)' _computing_data_reduction 'SMART (Bruker, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0428P)^2^+1.3554P] 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 5423 _refine_ls_number_parameters 440 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0654 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.1006 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 0.0785(4) 0.27736(18) 0.73133(13) 0.0328(7) Uani 1 1 d . . . C2 C 0.0177(3) 0.30766(16) 0.66413(12) 0.0277(6) Uani 1 1 d . . . C3 C -0.0491(3) 0.25785(16) 0.61537(13) 0.0289(6) Uani 1 1 d . . . H3 H -0.0485 0.2061 0.6243 0.035 Uiso 1 1 calc R . . C4 C -0.1167(3) 0.28257(15) 0.55391(12) 0.0257(6) Uani 1 1 d . . . C5 C -0.1195(3) 0.36084(16) 0.54155(12) 0.0284(7) Uani 1 1 d . . . C6 C -0.0467(3) 0.41061(16) 0.58881(13) 0.0317(7) Uani 1 1 d . . . H6 H -0.0441 0.4622 0.5796 0.038 Uiso 1 1 calc R . . C7 C 0.0224(3) 0.38476(16) 0.64976(13) 0.0292(6) Uani 1 1 d . . . C8 C -0.1803(3) 0.22644(17) 0.50160(13) 0.0297(7) Uani 1 1 d . . . C9 C -0.2073(4) 0.39560(16) 0.47924(13) 0.0332(7) Uani 1 1 d . . . C10 C -0.3848(4) 0.39769(16) 0.47046(13) 0.0329(7) Uani 1 1 d . . . C11 C -0.4734(4) 0.4187(2) 0.41184(15) 0.0508(9) Uani 1 1 d . . . H11 H -0.4217 0.4306 0.3776 0.061 Uiso 1 1 calc R . . C12 C -0.6392(5) 0.4225(2) 0.40341(19) 0.0630(11) Uani 1 1 d . . . H12 H -0.6974 0.4368 0.3636 0.076 Uiso 1 1 calc R . . C13 C -0.7173(5) 0.4055(2) 0.45274(19) 0.0557(10) Uani 1 1 d . . . H13 H -0.8285 0.4073 0.4466 0.067 Uiso 1 1 calc R . . C14 C -0.6315(5) 0.3857(2) 0.51125(18) 0.0623(11) Uani 1 1 d . . . H14 H -0.6842 0.3747 0.5454 0.075 Uiso 1 1 calc R . . C15 C -0.4667(4) 0.3819(2) 0.52027(15) 0.0507(9) Uani 1 1 d . . . H15 H -0.4097 0.3686 0.5606 0.061 Uiso 1 1 calc R . . C16 C 0.0981(4) 0.44477(17) 0.69677(14) 0.0348(7) Uani 1 1 d . . . C17 C 0.2744(4) 0.45200(17) 0.71033(13) 0.0350(7) Uani 1 1 d . . . C18 C 0.3728(4) 0.4030(2) 0.68402(15) 0.0458(8) Uani 1 1 d . . . H18 H 0.3282 0.3632 0.6578 0.055 Uiso 1 1 calc R . . C19 C 0.5367(4) 0.4125(2) 0.69633(18) 0.0587(10) Uani 1 1 d . . . H19 H 0.6023 0.3796 0.6782 0.070 Uiso 1 1 calc R . . C20 C 0.6024(5) 0.4712(3) 0.73568(19) 0.0673(12) Uani 1 1 d . . . H20 H 0.7128 0.4775 0.7445 0.081 Uiso 1 1 calc R . . C21 C 0.5070(5) 0.5199(2) 0.76170(18) 0.0640(11) Uani 1 1 d . . . H21 H 0.5522 0.5596 0.7879 0.077 Uiso 1 1 calc R . . C22 C 0.3440(4) 0.51060(19) 0.74938(15) 0.0483(9) Uani 1 1 d . . . H22 H 0.2795 0.5441 0.7675 0.058 Uiso 1 1 calc R . . C23 C 0.5268(4) 0.3087(2) 0.82341(17) 0.0518(9) Uani 1 1 d . . . H23 H 0.5286 0.3599 0.8343 0.062 Uiso 1 1 calc R . . C24 C 0.4533(4) 0.1962(2) 0.81205(17) 0.0508(9) Uani 1 1 d . . . H24 H 0.3980 0.1507 0.8127 0.061 Uiso 1 1 calc R . . C25 C 0.6714(5) 0.1515(2) 0.75325(19) 0.0604(11) Uani 1 1 d . . . H25A H 0.6416 0.0999 0.7622 0.072 Uiso 1 1 calc R . . H25B H 0.7858 0.1567 0.7676 0.072 Uiso 1 1 calc R . . C26 C 0.6320(5) 0.1659(2) 0.68204(18) 0.0588(10) Uani 1 1 d . . . H26A H 0.7061 0.1376 0.6608 0.071 Uiso 1 1 calc R . . H26B H 0.6472 0.2194 0.6741 0.071 Uiso 1 1 calc R . . C27 C 0.4634(5) 0.1439(3) 0.65250(19) 0.0764(13) Uani 1 1 d . . . H27A H 0.4504 0.0897 0.6583 0.092 Uiso 1 1 calc R . . H27B H 0.3898 0.1698 0.6756 0.092 Uiso 1 1 calc R . . C28 C 0.4206(5) 0.1616(3) 0.5843(2) 0.0856(15) Uani 1 1 d . . . H28A H 0.5039 0.1422 0.5625 0.103 Uiso 1 1 calc R . . H28B H 0.4189 0.2164 0.5795 0.103 Uiso 1 1 calc R . . C31 C -0.0603(4) 0.3964(2) 0.87622(17) 0.0498(9) Uani 1 1 d . . . H31 H -0.0293 0.4314 0.8476 0.060 Uiso 1 1 calc R . . C32 C -0.0697(4) 0.2966(2) 0.92949(15) 0.0437(8) Uani 1 1 d . . . H32 H -0.0500 0.2484 0.9473 0.052 Uiso 1 1 calc R . . C30 C -0.2958(5) 0.3324(3) 0.98634(18) 0.0687(12) Uani 1 1 d . . . H30A H -0.3104 0.2785 0.9928 0.082 Uiso 1 1 calc R . . H30B H -0.3986 0.3537 0.9673 0.082 Uiso 1 1 calc R . . C29 C -0.2387(5) 0.3695(3) 1.05038(19) 0.0758(13) Uani 1 1 d . . . H29A H -0.3181 0.3621 1.0778 0.091 Uiso 1 1 calc R . . H29B H -0.2283 0.4238 1.0439 0.091 Uiso 1 1 calc R . . Cu1 Cu 0.20973(4) 0.29481(2) 0.861135(15) 0.02858(12) Uani 1 1 d . . . N1 N 0.4094(3) 0.26111(15) 0.83381(11) 0.0357(6) Uani 1 1 d . . . N2 N 0.6379(4) 0.27671(18) 0.79670(16) 0.0583(8) Uani 1 1 d . . . N3 N 0.5869(3) 0.20473(16) 0.78911(13) 0.0417(6) Uani 1 1 d . . . N4 N 0.0108(3) 0.32825(15) 0.88822(11) 0.0361(6) Uani 1 1 d . . . N5 N -0.1821(3) 0.34317(17) 0.94169(13) 0.0497(8) Uani 1 1 d . . . N6 N -0.1765(4) 0.40910(17) 0.90821(15) 0.0557(8) Uani 1 1 d . . . O1 O 0.1252(2) 0.32867(11) 0.77352(8) 0.0338(5) Uani 1 1 d . . . O2 O 0.0812(3) 0.20913(13) 0.74192(11) 0.0589(7) Uani 1 1 d . . . O3 O -0.1854(3) 0.15811(12) 0.51513(10) 0.0475(6) Uani 1 1 d . . . O4 O -0.2207(2) 0.25525(11) 0.44587(8) 0.0324(5) Uani 1 1 d . . . O5 O -0.1342(3) 0.42573(13) 0.44131(10) 0.0493(6) Uani 1 1 d . . . O6 O 0.0121(3) 0.49030(14) 0.71755(12) 0.0591(7) Uani 1 1 d . . . O1W O 0.3111(4) 0.42015(19) 0.89922(15) 0.0575(8) Uani 1 1 d . . . O2W O 0.5759(4) 0.5235(2) 0.91876(19) 0.0804(10) Uani 1 1 d . . . H1WA H 0.366(5) 0.452(2) 0.9001(19) 0.062(16) Uiso 1 1 d . . . H2WA H 0.655(6) 0.502(3) 0.916(2) 0.094(19) Uiso 1 1 d . . . H1WB H 0.318(6) 0.412(3) 0.935(2) 0.095(19) Uiso 1 1 d . . . H2WB H 0.614(9) 0.558(4) 0.945(3) 0.18(3) Uiso 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 C1 0.0308(18) 0.040(2) 0.0249(15) 0.0056(13) -0.0021(13) 0.0007(14) C2 0.0246(16) 0.0363(17) 0.0207(14) 0.0019(12) -0.0007(12) 0.0023(13) C3 0.0327(18) 0.0266(15) 0.0264(15) 0.0029(12) 0.0028(13) -0.0004(13) C4 0.0250(16) 0.0306(17) 0.0202(13) 0.0016(11) 0.0004(11) -0.0015(12) C5 0.0254(17) 0.0377(17) 0.0202(14) 0.0011(12) -0.0017(12) -0.0046(13) C6 0.0326(18) 0.0294(16) 0.0302(16) 0.0045(12) -0.0030(13) -0.0014(13) C7 0.0245(16) 0.0361(17) 0.0252(14) -0.0043(12) -0.0007(12) -0.0008(13) C8 0.0254(17) 0.0382(18) 0.0249(15) -0.0024(13) 0.0026(12) -0.0037(13) C9 0.0385(19) 0.0328(17) 0.0247(15) 0.0016(13) -0.0049(13) -0.0032(14) C10 0.0356(19) 0.0302(16) 0.0289(15) 0.0023(12) -0.0050(13) -0.0014(14) C11 0.046(2) 0.066(2) 0.0358(18) 0.0161(16) -0.0055(16) -0.0079(18) C12 0.044(3) 0.080(3) 0.056(2) 0.018(2) -0.0171(19) -0.001(2) C13 0.037(2) 0.055(2) 0.073(3) 0.000(2) 0.0003(19) 0.0081(18) C14 0.047(3) 0.089(3) 0.053(2) -0.001(2) 0.0152(19) 0.015(2) C15 0.043(2) 0.075(3) 0.0317(18) 0.0001(17) 0.0006(15) 0.0123(19) C16 0.040(2) 0.0325(17) 0.0279(16) -0.0013(13) -0.0041(14) 0.0027(15) C17 0.0352(19) 0.0406(18) 0.0265(15) 0.0008(13) -0.0020(13) -0.0063(15) C18 0.036(2) 0.057(2) 0.0411(19) -0.0007(16) 0.0002(15) -0.0039(17) C19 0.038(2) 0.078(3) 0.061(2) 0.017(2) 0.0108(19) 0.004(2) C20 0.038(2) 0.096(3) 0.060(3) 0.034(2) -0.014(2) -0.027(2) C21 0.061(3) 0.076(3) 0.048(2) 0.002(2) -0.010(2) -0.035(2) C22 0.054(2) 0.049(2) 0.0389(18) -0.0039(16) -0.0017(17) -0.0162(18) C23 0.042(2) 0.054(2) 0.062(2) -0.0050(18) 0.0188(19) 0.0009(18) C24 0.047(2) 0.046(2) 0.063(2) 0.0011(18) 0.0195(19) -0.0055(17) C25 0.051(3) 0.059(2) 0.076(3) 0.002(2) 0.024(2) 0.0135(19) C26 0.051(3) 0.068(3) 0.063(3) -0.009(2) 0.025(2) 0.006(2) C27 0.067(3) 0.104(4) 0.061(3) -0.010(2) 0.022(2) 0.004(3) C28 0.063(3) 0.142(4) 0.057(3) 0.001(3) 0.026(2) -0.008(3) C31 0.046(2) 0.052(2) 0.053(2) 0.0120(17) 0.0149(18) 0.0100(18) C32 0.039(2) 0.053(2) 0.0409(18) 0.0077(16) 0.0121(15) 0.0085(17) C30 0.046(3) 0.106(3) 0.062(3) 0.011(2) 0.032(2) 0.013(2) C29 0.058(3) 0.120(4) 0.056(3) 0.009(2) 0.027(2) 0.019(3) Cu1 0.0258(2) 0.0415(2) 0.01733(17) 0.00195(15) 0.00093(13) 0.00302(17) N1 0.0322(16) 0.0471(16) 0.0277(13) 0.0015(11) 0.0050(11) 0.0010(13) N2 0.048(2) 0.058(2) 0.072(2) -0.0081(16) 0.0209(17) -0.0059(16) N3 0.0352(16) 0.0456(17) 0.0470(16) -0.0004(13) 0.0147(13) 0.0046(14) N4 0.0316(15) 0.0497(16) 0.0273(13) 0.0057(12) 0.0060(11) 0.0051(13) N5 0.0347(17) 0.072(2) 0.0456(17) 0.0085(15) 0.0150(13) 0.0125(15) N6 0.049(2) 0.0567(19) 0.065(2) 0.0086(16) 0.0188(16) 0.0170(15) O1 0.0366(13) 0.0442(12) 0.0183(10) 0.0002(9) -0.0016(9) 0.0011(10) O2 0.083(2) 0.0440(15) 0.0381(13) 0.0113(11) -0.0208(12) -0.0064(13) O3 0.0726(18) 0.0316(13) 0.0334(12) -0.0003(10) -0.0046(11) -0.0079(11) O4 0.0387(13) 0.0375(12) 0.0185(10) -0.0019(8) -0.0015(9) -0.0034(10) O5 0.0444(15) 0.0613(15) 0.0387(13) 0.0202(11) -0.0025(11) -0.0151(12) O6 0.0450(16) 0.0614(16) 0.0663(16) -0.0305(13) -0.0036(12) 0.0140(13) O1W 0.070(2) 0.0535(18) 0.0472(18) -0.0021(14) 0.0055(15) -0.0164(16) O2W 0.055(2) 0.073(2) 0.112(3) -0.034(2) 0.0099(19) 0.0040(18) _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 O2 1.221(3) . ? C1 O1 1.280(3) . ? C1 C2 1.514(4) . ? C2 C7 1.392(4) . ? C2 C3 1.393(4) . ? C3 C4 1.389(4) . ? C3 H3 0.9300 . ? C4 C5 1.401(4) . ? C4 C8 1.507(4) . ? C5 C6 1.387(4) . ? C5 C9 1.518(4) . ? C6 C7 1.389(4) . ? C6 H6 0.9300 . ? C7 C16 1.511(4) . ? C8 O3 1.238(3) . ? C8 O4 1.268(3) . ? C9 O5 1.215(3) . ? C9 C10 1.485(4) . ? C10 C11 1.378(4) . ? C10 C15 1.383(4) . ? C11 C12 1.389(5) . ? C11 H11 0.9300 . ? C12 C13 1.358(5) . ? C12 H12 0.9300 . ? C13 C14 1.361(5) . ? C13 H13 0.9300 . ? C14 C15 1.380(5) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 O6 1.215(3) . ? C16 C17 1.479(4) . ? C17 C18 1.382(4) . ? C17 C22 1.385(4) . ? C18 C19 1.380(5) . ? C18 H18 0.9300 . ? C19 C20 1.379(6) . ? C19 H19 0.9300 . ? C20 C21 1.358(6) . ? C20 H20 0.9300 . ? C21 C22 1.372(5) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 N2 1.306(4) . ? C23 N1 1.348(4) . ? C23 H23 0.9300 . ? C24 N1 1.308(4) . ? C24 N3 1.316(4) . ? C24 H24 0.9300 . ? C25 N3 1.466(4) . ? C25 C26 1.498(5) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.508(6) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.450(6) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.517(6) 4_665 ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C31 N6 1.306(4) . ? C31 N4 1.346(4) . ? C31 H31 0.9300 . ? C32 N5 1.317(4) . ? C32 N4 1.318(4) . ? C32 H32 0.9300 . ? C30 N5 1.472(4) . ? C30 C29 1.499(6) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C29 C28 1.517(6) 4_566 ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? Cu1 O1 1.9499(18) . ? Cu1 N4 1.964(2) . ? Cu1 N1 1.974(3) . ? Cu1 O4 1.9830(18) 4_666 ? N2 N3 1.339(4) . ? N5 N6 1.362(4) . ? O4 Cu1 1.9830(18) 4_565 ? O1W H1WA 0.73(4) . ? O1W H1WB 0.76(5) . ? O2W H2WA 0.79(5) . ? O2W H2WB 0.85(7) . ? 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 C1 O1 125.0(3) . . ? O2 C1 C2 120.6(3) . . ? O1 C1 C2 114.3(3) . . ? C7 C2 C3 118.5(2) . . ? C7 C2 C1 121.9(2) . . ? C3 C2 C1 119.6(3) . . ? C4 C3 C2 122.5(3) . . ? C4 C3 H3 118.8 . . ? C2 C3 H3 118.8 . . ? C3 C4 C5 118.1(2) . . ? C3 C4 C8 120.7(2) . . ? C5 C4 C8 121.1(2) . . ? C6 C5 C4 119.8(2) . . ? C6 C5 C9 117.0(3) . . ? C4 C5 C9 123.1(2) . . ? C5 C6 C7 121.2(3) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C6 C7 C2 119.7(3) . . ? C6 C7 C16 115.9(3) . . ? C2 C7 C16 124.3(2) . . ? O3 C8 O4 125.9(3) . . ? O3 C8 C4 119.5(2) . . ? O4 C8 C4 114.6(2) . . ? O5 C9 C10 122.1(3) . . ? O5 C9 C5 120.8(3) . . ? C10 C9 C5 116.9(2) . . ? C11 C10 C15 117.6(3) . . ? C11 C10 C9 120.1(3) . . ? C15 C10 C9 122.3(3) . . ? C10 C11 C12 120.6(3) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C13 C12 C11 120.7(3) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C12 C13 C14 119.4(4) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? C13 C14 C15 120.4(4) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C14 C15 C10 121.2(3) . . ? C14 C15 H15 119.4 . . ? C10 C15 H15 119.4 . . ? O6 C16 C17 121.6(3) . . ? O6 C16 C7 118.9(3) . . ? C17 C16 C7 119.1(3) . . ? C18 C17 C22 118.5(3) . . ? C18 C17 C16 122.1(3) . . ? C22 C17 C16 119.4(3) . . ? C19 C18 C17 120.6(3) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C20 C19 C18 119.5(4) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C21 C20 C19 120.5(4) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 120.1(4) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C21 C22 C17 120.8(4) . . ? C21 C22 H22 119.6 . . ? C17 C22 H22 119.6 . . ? N2 C23 N1 114.3(3) . . ? N2 C23 H23 122.8 . . ? N1 C23 H23 122.8 . . ? N1 C24 N3 110.2(3) . . ? N1 C24 H24 124.9 . . ? N3 C24 H24 124.9 . . ? N3 C25 C26 111.2(3) . . ? N3 C25 H25A 109.4 . . ? C26 C25 H25A 109.4 . . ? N3 C25 H25B 109.4 . . ? C26 C25 H25B 109.4 . . ? H25A C25 H25B 108.0 . . ? C25 C26 C27 113.5(3) . . ? C25 C26 H26A 108.9 . . ? C27 C26 H26A 108.9 . . ? C25 C26 H26B 108.9 . . ? C27 C26 H26B 108.9 . . ? H26A C26 H26B 107.7 . . ? C28 C27 C26 114.1(4) . . ? C28 C27 H27A 108.7 . . ? C26 C27 H27A 108.7 . . ? C28 C27 H27B 108.7 . . ? C26 C27 H27B 108.7 . . ? H27A C27 H27B 107.6 . . ? C27 C28 C29 115.9(4) . 4_665 ? C27 C28 H28A 108.3 . . ? C29 C28 H28A 108.3 4_665 . ? C27 C28 H28B 108.3 . . ? C29 C28 H28B 108.3 4_665 . ? H28A C28 H28B 107.4 . . ? N6 C31 N4 114.2(3) . . ? N6 C31 H31 122.9 . . ? N4 C31 H31 122.9 . . ? N5 C32 N4 109.9(3) . . ? N5 C32 H32 125.0 . . ? N4 C32 H32 125.0 . . ? N5 C30 C29 111.8(3) . . ? N5 C30 H30A 109.3 . . ? C29 C30 H30A 109.3 . . ? N5 C30 H30B 109.3 . . ? C29 C30 H30B 109.3 . . ? H30A C30 H30B 107.9 . . ? C30 C29 C28 112.8(4) . 4_566 ? C30 C29 H29A 109.0 . . ? C28 C29 H29A 109.0 4_566 . ? C30 C29 H29B 109.0 . . ? C28 C29 H29B 109.0 4_566 . ? H29A C29 H29B 107.8 . . ? O1 Cu1 N4 89.38(9) . . ? O1 Cu1 N1 90.56(9) . . ? N4 Cu1 N1 179.90(13) . . ? O1 Cu1 O4 170.90(9) . 4_666 ? N4 Cu1 O4 90.51(9) . 4_666 ? N1 Cu1 O4 89.53(9) . 4_666 ? C24 N1 C23 102.8(3) . . ? C24 N1 Cu1 132.5(2) . . ? C23 N1 Cu1 123.9(2) . . ? C23 N2 N3 102.5(3) . . ? C24 N3 N2 110.2(3) . . ? C24 N3 C25 130.2(3) . . ? N2 N3 C25 119.3(3) . . ? C32 N4 C31 103.5(3) . . ? C32 N4 Cu1 129.4(2) . . ? C31 N4 Cu1 126.3(2) . . ? C32 N5 N6 109.8(3) . . ? C32 N5 C30 128.5(3) . . ? N6 N5 C30 121.7(3) . . ? C31 N6 N5 102.6(3) . . ? C1 O1 Cu1 117.24(18) . . ? C8 O4 Cu1 129.99(18) . 4_565 ? H1WA O1W H1WB 101(5) . . ? H2WA O2W H2WB 99(6) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.542 _refine_diff_density_min -0.352 _refine_diff_density_rms 0.057