Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Leonard Lindoy' _publ_contact_author_address ; School of Chemistry F11 University of Sydney Sydney NSW 2006. AUSTRALIA ; _publ_contact_author_email LINDOY@CHEM.USYD.EDU.AU _publ_section_title ; Extended three-dimensional supramolecular architectures derived from trinuclear (bis-?-diketonato)copper(II) metallocycles ; loop_ _publ_author_name 'Leonard Lindoy' 'Jack K. Clegg' 'John C. McMurtrie' 'David Schilter' # Attachment '(1)Cu3L3new.CIF' data_lj48sad _database_code_depnum_ccdc_archive 'CCDC 292064' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H48 Cu3 O12, 0.5(H2 O)' _chemical_formula_sum 'C48 H49 Cu3 O12.50' _chemical_formula_weight 1016.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2001(8) _cell_length_b 14.7227(12) _cell_length_c 15.3507(13) _cell_angle_alpha 80.131(1) _cell_angle_beta 87.500(1) _cell_angle_gamma 78.150(1) _cell_volume 2222.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6628 _cell_measurement_theta_min 2.246 _cell_measurement_theta_max 27.811 _exptl_crystal_description prism _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 1.487 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.809 _exptl_absorpt_correction_T_max 0.915 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 183 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.06 _diffrn_reflns_number 22002 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0500 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 28.37 _reflns_number_total 10284 _reflns_number_gt 7708 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1995)' _computing_cell_refinement 'SAINT (Bruker, 1995)' _computing_data_reduction 'SAINT and XPREP (Bruker, 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEPIII (Farrugia, 1997) WINGX-32 (Farrugia, 1999) ; _computing_publication_material 'enCIFer 1.0 (CCDC, 2003)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0794P)^2^+0.0818P] 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 10284 _refine_ls_number_parameters 575 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0671 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.1313 _refine_ls_wR_factor_gt 0.1185 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 1.14208(4) 0.92477(2) 1.02411(2) 0.01818(10) Uani 1 1 d . . . Cu2 Cu 0.70758(4) 1.05253(3) 0.39463(2) 0.02142(11) Uani 1 1 d . . . Cu3 Cu 0.55905(4) 0.46280(3) 0.86083(2) 0.02143(11) Uani 1 1 d . . . O1 O 1.2555(2) 1.01461(15) 1.02185(13) 0.0227(5) Uani 1 1 d . . . O2 O 1.0647(2) 0.98574(14) 0.91063(13) 0.0199(4) Uani 1 1 d . . . O3 O 0.8128(2) 1.05197(15) 0.49476(13) 0.0246(5) Uani 1 1 d . . . O4 O 0.7793(2) 1.15059(16) 0.32415(14) 0.0301(5) Uani 1 1 d . . . O5 O 0.5892(2) 1.06100(16) 0.29888(14) 0.0263(5) Uani 1 1 d . . . O6 O 0.6484(2) 0.94694(15) 0.46314(13) 0.0237(5) Uani 1 1 d . . . O7 O 0.5687(2) 0.55541(15) 0.75676(14) 0.0257(5) Uani 1 1 d . . . O8 O 0.4346(2) 0.40821(16) 0.80679(14) 0.0295(5) Uani 1 1 d . . . O9 O 0.5555(2) 0.36874(15) 0.96350(14) 0.0232(5) Uani 1 1 d . . . O10 O 0.6840(2) 0.51923(15) 0.91072(14) 0.0233(5) Uani 1 1 d . . . O11 O 1.0485(2) 0.82417(14) 1.01884(13) 0.0208(4) Uani 1 1 d . . . O12 O 1.2277(2) 0.86332(15) 1.13310(13) 0.0217(5) Uani 1 1 d . . . C1 C 1.4097(4) 1.2027(3) 0.8943(2) 0.0329(8) Uani 1 1 d . . . H1A H 1.4823 1.2311 0.9101 0.049 Uiso 1 1 calc R . . H1B H 1.3259 1.2498 0.8886 0.049 Uiso 1 1 calc R . . H1C H 1.4312 1.1800 0.8379 0.049 Uiso 1 1 calc R . . C2 C 1.3937(3) 1.1214(2) 0.9653(2) 0.0261(7) Uani 1 1 d . . . H2A H 1.3753 1.1455 1.0219 0.031 Uiso 1 1 calc R . . H2B H 1.4805 1.0761 0.9715 0.031 Uiso 1 1 calc R . . C3 C 1.2862(3) 1.0680(2) 0.9526(2) 0.0201(6) Uani 1 1 d . . . C4 C 1.2288(3) 1.0784(2) 0.86940(19) 0.0227(6) Uani 1 1 d . . . H4 H 1.2659 1.1148 0.8211 0.027 Uiso 1 1 calc R . . C5 C 1.1221(3) 1.0395(2) 0.85211(19) 0.0184(6) Uani 1 1 d . . . C6 C 1.0640(3) 1.0595(2) 0.76100(19) 0.0185(6) Uani 1 1 d . . . C7 C 1.1060(3) 1.1229(2) 0.6928(2) 0.0285(7) Uani 1 1 d . . . H7 H 1.1737 1.1551 0.7040 0.034 Uiso 1 1 calc R . . C8 C 1.0515(3) 1.1401(2) 0.6089(2) 0.0286(7) Uani 1 1 d . . . H8 H 1.0812 1.1842 0.5638 0.034 Uiso 1 1 calc R . . C9 C 0.9539(3) 1.0930(2) 0.59067(19) 0.0196(6) Uani 1 1 d . . . C10 C 0.9113(3) 1.0294(2) 0.6586(2) 0.0266(7) Uani 1 1 d . . . H10 H 0.8440 0.9970 0.6474 0.032 Uiso 1 1 calc R . . C11 C 0.9662(3) 1.0130(2) 0.7428(2) 0.0259(7) Uani 1 1 d . . . H11 H 0.9361 0.9693 0.7882 0.031 Uiso 1 1 calc R . . C12 C 0.8920(3) 1.1070(2) 0.5007(2) 0.0228(6) Uani 1 1 d . . . C13 C 0.9217(4) 1.1756(2) 0.4321(2) 0.0316(8) Uani 1 1 d . . . H13 H 0.9827 1.2129 0.4434 0.038 Uiso 1 1 calc R . . C14 C 0.8661(4) 1.1921(3) 0.3476(2) 0.0345(8) Uani 1 1 d . . . C15 C 0.9093(5) 1.2634(4) 0.2742(3) 0.0724(18) Uani 1 1 d . . . H15A H 0.9325 1.2316 0.2221 0.087 Uiso 1 1 calc R . . H15B H 0.8297 1.3139 0.2580 0.087 Uiso 1 1 calc R . . C16 C 1.0201(6) 1.3090(4) 0.2873(3) 0.0757(17) Uani 1 1 d . . . H16A H 1.0354 1.3514 0.2330 0.114 Uiso 1 1 calc R . . H16B H 1.1015 1.2609 0.3020 0.114 Uiso 1 1 calc R . . H16C H 0.9977 1.3451 0.3358 0.114 Uiso 1 1 calc R . . C17 C 0.3233(3) 1.1192(3) 0.2135(2) 0.0356(8) Uani 1 1 d . . . H17A H 0.2679 1.1332 0.1604 0.053 Uiso 1 1 calc R . . H17B H 0.3705 1.1707 0.2145 0.053 Uiso 1 1 calc R . . H17C H 0.2661 1.1127 0.2663 0.053 Uiso 1 1 calc R . . C18 C 0.4249(3) 1.0280(2) 0.2124(2) 0.0282(7) Uani 1 1 d . . . H18A H 0.4821 1.0344 0.1588 0.034 Uiso 1 1 calc R . . H18B H 0.3773 0.9762 0.2101 0.034 Uiso 1 1 calc R . . C19 C 0.5122(3) 1.0041(2) 0.2943(2) 0.0233(7) Uani 1 1 d . . . C20 C 0.4993(3) 0.9273(2) 0.3576(2) 0.0261(7) Uani 1 1 d . . . H20 H 0.4419 0.8881 0.3448 0.031 Uiso 1 1 calc R . . C21 C 0.5642(3) 0.9031(2) 0.43870(19) 0.0216(6) Uani 1 1 d . . . C22 C 0.5412(3) 0.8200(2) 0.5031(2) 0.0241(7) Uani 1 1 d . . . C23 C 0.4375(3) 0.7733(2) 0.4939(2) 0.0295(7) Uani 1 1 d . . . H23 H 0.3782 0.7957 0.4453 0.035 Uiso 1 1 calc R . . C24 C 0.4195(4) 0.6957(2) 0.5535(2) 0.0303(8) Uani 1 1 d . . . H24 H 0.3485 0.6653 0.5452 0.036 Uiso 1 1 calc R . . C25 C 0.5041(3) 0.6609(2) 0.6260(2) 0.0247(7) Uani 1 1 d . . . C26 C 0.6054(4) 0.7085(3) 0.6368(2) 0.0376(9) Uani 1 1 d . . . H26 H 0.6630 0.6872 0.6863 0.045 Uiso 1 1 calc R . . C27 C 0.6233(4) 0.7861(3) 0.5765(2) 0.0363(9) Uani 1 1 d . . . H27 H 0.6933 0.8172 0.5854 0.044 Uiso 1 1 calc R . . C28 C 0.4879(3) 0.5768(2) 0.6920(2) 0.0272(7) Uani 1 1 d . . . C29 C 0.3873(4) 0.5279(3) 0.6815(2) 0.0435(10) Uani 1 1 d . . . H29 H 0.3280 0.5521 0.6332 0.052 Uiso 1 1 calc R . . C30 C 0.3680(4) 0.4457(2) 0.7372(2) 0.0309(8) Uani 1 1 d . . . C31 C 0.2649(4) 0.3951(3) 0.7114(2) 0.0406(9) Uani 1 1 d . . . H31A H 0.2328 0.3576 0.7648 0.049 Uiso 1 1 calc R . . H31B H 0.1872 0.4418 0.6843 0.049 Uiso 1 1 calc R . . C32 C 0.3231(5) 0.3319(3) 0.6474(3) 0.0557(12) Uani 1 1 d . . . H32A H 0.2548 0.2997 0.6314 0.084 Uiso 1 1 calc R . . H32B H 0.3991 0.2851 0.6746 0.084 Uiso 1 1 calc R . . H32C H 0.3536 0.3692 0.5942 0.084 Uiso 1 1 calc R . . C33 C 0.6632(4) 0.1952(2) 1.0992(2) 0.0299(7) Uani 1 1 d . . . H33A H 0.6435 0.1473 1.1479 0.045 Uiso 1 1 calc R . . H33B H 0.7588 0.1967 1.0991 0.045 Uiso 1 1 calc R . . H33C H 0.6400 0.1799 1.0429 0.045 Uiso 1 1 calc R . . C34 C 0.5815(3) 0.2907(2) 1.1112(2) 0.0236(7) Uani 1 1 d . . . H34A H 0.4850 0.2885 1.1126 0.028 Uiso 1 1 calc R . . H34B H 0.6039 0.3054 1.1687 0.028 Uiso 1 1 calc R . . C35 C 0.6074(3) 0.3679(2) 1.0379(2) 0.0203(6) Uani 1 1 d . . . C36 C 0.6860(3) 0.4301(2) 1.0548(2) 0.0216(6) Uani 1 1 d . . . H36 H 0.7165 0.4241 1.1135 0.026 Uiso 1 1 calc R . . C37 C 0.7227(3) 0.5005(2) 0.9912(2) 0.0199(6) Uani 1 1 d . . . C38 C 0.8114(3) 0.5617(2) 1.01430(19) 0.0196(6) Uani 1 1 d . . . C39 C 0.8932(3) 0.5358(2) 1.0883(2) 0.0268(7) Uani 1 1 d . . . H39 H 0.8927 0.4776 1.1262 0.032 Uiso 1 1 calc R . . C40 C 0.9756(3) 0.5942(2) 1.1073(2) 0.0261(7) Uani 1 1 d . . . H40 H 1.0322 0.5746 1.1574 0.031 Uiso 1 1 calc R . . C41 C 0.9767(3) 0.6809(2) 1.05405(19) 0.0185(6) Uani 1 1 d . . . C42 C 0.8967(3) 0.7053(2) 0.9789(2) 0.0256(7) Uani 1 1 d . . . H42 H 0.8971 0.7634 0.9409 0.031 Uiso 1 1 calc R . . C43 C 0.8166(3) 0.6464(2) 0.9584(2) 0.0255(7) Uani 1 1 d . . . H43 H 0.7650 0.6637 0.9059 0.031 Uiso 1 1 calc R . . C44 C 1.0587(3) 0.7481(2) 1.07414(19) 0.0191(6) Uani 1 1 d . . . C45 C 1.1363(3) 0.7256(2) 1.1505(2) 0.0230(7) Uani 1 1 d . . . H45 H 1.1357 0.6668 1.1873 0.028 Uiso 1 1 calc R . . C46 C 1.2144(3) 0.7832(2) 1.17639(19) 0.0201(6) Uani 1 1 d . . . C47 C 1.2941(3) 0.7538(2) 1.2611(2) 0.0279(7) Uani 1 1 d . . . H47A H 1.3904 0.7406 1.2450 0.033 Uiso 1 1 calc R . . H47B H 1.2789 0.8081 1.2931 0.033 Uiso 1 1 calc R . . C48 C 1.2657(4) 0.6698(2) 1.3244(2) 0.0339(8) Uani 1 1 d . . . H48A H 1.3237 0.6579 1.3760 0.051 Uiso 1 1 calc R . . H48B H 1.2831 0.6145 1.2948 0.051 Uiso 1 1 calc R . . H48C H 1.1717 0.6823 1.3435 0.051 Uiso 1 1 calc R . . O1W O 1.0480(15) 0.5614(11) 0.4994(10) 0.077(3) Uiso 0.25 1 d P A 1 O2W O 1.0963(15) 0.4793(11) 0.4513(10) 0.077(3) Uiso 0.25 1 d P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02214(19) 0.01825(19) 0.01598(18) 0.00163(14) -0.00644(14) -0.01064(15) Cu2 0.0267(2) 0.0241(2) 0.01496(18) 0.00171(15) -0.00748(14) -0.01129(16) Cu3 0.0300(2) 0.0190(2) 0.01807(19) 0.00100(14) -0.00754(15) -0.01337(16) O1 0.0282(11) 0.0237(11) 0.0188(10) 0.0026(9) -0.0077(9) -0.0145(9) O2 0.0226(11) 0.0216(11) 0.0175(10) 0.0013(8) -0.0061(8) -0.0113(9) O3 0.0318(12) 0.0273(12) 0.0179(10) 0.0012(9) -0.0087(9) -0.0157(10) O4 0.0379(13) 0.0335(13) 0.0212(11) 0.0063(10) -0.0123(10) -0.0189(11) O5 0.0335(12) 0.0282(12) 0.0182(11) 0.0053(9) -0.0112(9) -0.0137(10) O6 0.0298(12) 0.0260(12) 0.0169(10) 0.0027(9) -0.0086(9) -0.0126(9) O7 0.0361(13) 0.0225(12) 0.0216(11) 0.0015(9) -0.0100(9) -0.0151(10) O8 0.0432(14) 0.0246(12) 0.0242(12) 0.0040(9) -0.0137(10) -0.0187(11) O9 0.0307(12) 0.0204(11) 0.0210(11) 0.0009(9) -0.0063(9) -0.0134(9) O10 0.0308(12) 0.0214(11) 0.0198(10) 0.0028(9) -0.0081(9) -0.0137(9) O11 0.0241(11) 0.0204(11) 0.0194(10) 0.0023(8) -0.0065(8) -0.0110(9) O12 0.0256(11) 0.0214(11) 0.0194(10) 0.0027(9) -0.0090(8) -0.0108(9) C1 0.043(2) 0.0315(19) 0.0295(18) 0.0029(15) -0.0075(15) -0.0255(16) C2 0.0304(17) 0.0266(17) 0.0239(16) 0.0036(13) -0.0102(13) -0.0163(14) C3 0.0224(15) 0.0180(15) 0.0215(15) 0.0007(12) -0.0043(12) -0.0102(12) C4 0.0273(16) 0.0275(17) 0.0153(14) 0.0022(12) -0.0023(12) -0.0143(13) C5 0.0221(15) 0.0156(14) 0.0173(14) -0.0015(11) -0.0028(11) -0.0034(12) C6 0.0208(14) 0.0179(15) 0.0176(14) -0.0031(11) -0.0038(11) -0.0047(12) C7 0.0316(18) 0.0374(19) 0.0218(16) 0.0029(14) -0.0090(13) -0.0240(15) C8 0.0340(18) 0.0364(19) 0.0180(15) 0.0050(14) -0.0055(13) -0.0203(15) C9 0.0212(15) 0.0220(15) 0.0161(14) -0.0014(12) -0.0061(11) -0.0058(12) C10 0.0317(17) 0.0290(18) 0.0240(16) 0.0002(13) -0.0082(13) -0.0192(14) C11 0.0331(17) 0.0278(17) 0.0205(15) 0.0029(13) -0.0056(13) -0.0190(14) C12 0.0262(16) 0.0251(16) 0.0178(15) -0.0026(12) -0.0061(12) -0.0062(13) C13 0.039(2) 0.0316(19) 0.0269(17) 0.0077(14) -0.0153(14) -0.0207(16) C14 0.042(2) 0.035(2) 0.0270(18) 0.0082(15) -0.0130(15) -0.0186(17) C15 0.092(4) 0.076(3) 0.054(3) 0.042(2) -0.050(3) -0.064(3) C16 0.077(4) 0.093(4) 0.056(3) 0.029(3) -0.019(3) -0.046(3) C17 0.0318(19) 0.044(2) 0.0286(18) 0.0084(16) -0.0099(15) -0.0126(16) C18 0.0383(19) 0.0285(18) 0.0193(15) 0.0060(13) -0.0116(14) -0.0161(15) C19 0.0273(16) 0.0262(17) 0.0174(14) -0.0024(12) -0.0082(12) -0.0066(13) C20 0.0334(17) 0.0243(17) 0.0230(16) 0.0012(13) -0.0113(13) -0.0134(14) C21 0.0246(16) 0.0231(16) 0.0173(14) -0.0026(12) -0.0030(12) -0.0057(13) C22 0.0330(17) 0.0226(16) 0.0180(15) -0.0019(12) -0.0057(13) -0.0086(13) C23 0.0309(18) 0.0337(19) 0.0240(16) 0.0026(14) -0.0103(14) -0.0112(15) C24 0.0367(19) 0.0321(19) 0.0254(17) 0.0042(14) -0.0087(14) -0.0204(15) C25 0.0318(17) 0.0249(17) 0.0193(15) 0.0000(13) -0.0069(13) -0.0112(14) C26 0.051(2) 0.037(2) 0.0260(17) 0.0130(15) -0.0214(16) -0.0247(18) C27 0.049(2) 0.034(2) 0.0300(18) 0.0054(15) -0.0193(16) -0.0249(17) C28 0.0391(19) 0.0238(17) 0.0210(15) 0.0004(13) -0.0080(14) -0.0137(14) C29 0.058(3) 0.042(2) 0.034(2) 0.0139(17) -0.0268(18) -0.028(2) C30 0.0393(19) 0.0297(18) 0.0290(17) -0.0020(14) -0.0103(15) -0.0191(16) C31 0.051(2) 0.042(2) 0.034(2) 0.0035(17) -0.0128(17) -0.0265(19) C32 0.062(3) 0.056(3) 0.060(3) -0.023(2) 0.002(2) -0.026(2) C33 0.0387(19) 0.0228(17) 0.0275(17) 0.0004(14) -0.0020(14) -0.0080(14) C34 0.0291(17) 0.0245(16) 0.0185(14) 0.0015(12) 0.0001(12) -0.0125(13) C35 0.0219(15) 0.0156(14) 0.0223(15) 0.0001(12) -0.0005(12) -0.0037(12) C36 0.0270(16) 0.0208(15) 0.0191(14) 0.0001(12) -0.0064(12) -0.0114(13) C37 0.0198(15) 0.0172(15) 0.0229(15) -0.0013(12) -0.0066(12) -0.0047(12) C38 0.0207(15) 0.0193(15) 0.0205(14) -0.0023(12) -0.0036(12) -0.0080(12) C39 0.0322(18) 0.0235(17) 0.0261(16) 0.0060(13) -0.0099(13) -0.0155(14) C40 0.0302(17) 0.0257(17) 0.0237(16) 0.0046(13) -0.0136(13) -0.0127(14) C41 0.0186(14) 0.0189(15) 0.0187(14) -0.0014(11) -0.0055(11) -0.0057(12) C42 0.0295(17) 0.0210(16) 0.0253(16) 0.0051(13) -0.0089(13) -0.0088(13) C43 0.0290(17) 0.0257(17) 0.0232(15) 0.0050(13) -0.0140(13) -0.0130(14) C44 0.0216(15) 0.0178(15) 0.0201(14) -0.0033(12) -0.0015(12) -0.0084(12) C45 0.0272(16) 0.0198(15) 0.0226(15) 0.0048(12) -0.0100(12) -0.0107(13) C46 0.0206(15) 0.0214(15) 0.0184(14) 0.0000(12) -0.0047(11) -0.0060(12) C47 0.0368(19) 0.0234(17) 0.0248(16) 0.0028(13) -0.0150(14) -0.0117(14) C48 0.047(2) 0.0293(19) 0.0260(17) 0.0072(14) -0.0156(16) -0.0165(16) _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 O12 1.914(2) . ? Cu1 O1 1.923(2) . ? Cu1 O11 1.934(2) . ? Cu1 O2 1.938(2) . ? Cu1 O2 2.513(2) 2_777 ? Cu2 O4 1.903(2) . ? Cu2 O3 1.911(2) . ? Cu2 O6 1.912(2) . ? Cu2 O5 1.914(2) . ? Cu3 O10 1.908(2) . ? Cu3 O9 1.916(2) . ? Cu3 O8 1.919(2) . ? Cu3 O7 1.928(2) . ? O1 C3 1.277(4) . ? O2 C5 1.295(3) . ? O2 Cu1 2.513(2) 2_777 ? O3 C12 1.272(4) . ? O4 C14 1.270(4) . ? O5 C19 1.272(4) . ? O6 C21 1.278(4) . ? O7 C28 1.274(4) . ? O8 C30 1.270(4) . ? O9 C35 1.277(4) . ? O10 C37 1.280(4) . ? O11 C44 1.273(4) . ? O12 C46 1.280(4) . ? C1 C2 1.505(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.511(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.400(4) . ? C4 C5 1.384(4) . ? C4 H4 0.9500 . ? C5 C6 1.501(4) . ? C6 C11 1.383(4) . ? C6 C7 1.393(4) . ? C7 C8 1.388(4) . ? C7 H7 0.9500 . ? C8 C9 1.387(4) . ? C8 H8 0.9500 . ? C9 C10 1.394(4) . ? C9 C12 1.508(4) . ? C10 C11 1.393(4) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.397(4) . ? C13 C14 1.401(4) . ? C13 H13 0.9500 . ? C14 C15 1.519(5) . ? C15 C16 1.466(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.521(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.521(4) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.383(4) . ? C20 C21 1.392(4) . ? C20 H20 0.9500 . ? C21 C22 1.488(4) . ? C22 C27 1.393(4) . ? C22 C23 1.398(4) . ? C23 C24 1.374(4) . ? C23 H23 0.9500 . ? C24 C25 1.397(4) . ? C24 H24 0.9500 . ? C25 C26 1.393(4) . ? C25 C28 1.492(4) . ? C26 C27 1.380(5) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C29 1.398(5) . ? C29 C30 1.402(5) . ? C29 H29 0.9500 . ? C30 C31 1.509(4) . ? C31 C32 1.489(6) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.517(4) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.512(4) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.396(4) . ? C36 C37 1.395(4) . ? C36 H36 0.9500 . ? C37 C38 1.494(4) . ? C38 C39 1.391(4) . ? C38 C43 1.396(4) . ? C39 C40 1.391(4) . ? C39 H39 0.9500 . ? C40 C41 1.395(4) . ? C40 H40 0.9500 . ? C41 C42 1.395(4) . ? C41 C44 1.496(4) . ? C42 C43 1.388(4) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 C45 1.396(4) . ? C45 C46 1.391(4) . ? C45 H45 0.9500 . ? C46 C47 1.515(4) . ? C47 C48 1.505(4) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O12 Cu1 O1 86.18(9) . . ? O12 Cu1 O11 93.13(9) . . ? O1 Cu1 O11 172.13(9) . . ? O12 Cu1 O2 176.93(9) . . ? O1 Cu1 O2 92.37(8) . . ? O11 Cu1 O2 87.93(8) . . ? O12 Cu1 O2 97.44(8) . 2_777 ? O1 Cu1 O2 98.54(8) . 2_777 ? O11 Cu1 O2 89.32(8) . 2_777 ? O2 Cu1 O2 85.44(8) . 2_777 ? O4 Cu2 O3 93.02(9) . . ? O4 Cu2 O6 175.29(10) . . ? O3 Cu2 O6 86.27(9) . . ? O4 Cu2 O5 87.31(9) . . ? O3 Cu2 O5 174.68(10) . . ? O6 Cu2 O5 93.82(9) . . ? O10 Cu3 O9 93.60(9) . . ? O10 Cu3 O8 178.08(9) . . ? O9 Cu3 O8 88.25(9) . . ? O10 Cu3 O7 85.73(9) . . ? O9 Cu3 O7 178.09(10) . . ? O8 Cu3 O7 92.41(9) . . ? C3 O1 Cu1 125.10(18) . . ? C5 O2 Cu1 124.01(18) . . ? C5 O2 Cu1 112.33(18) . 2_777 ? Cu1 O2 Cu1 94.56(8) . 2_777 ? C12 O3 Cu2 126.63(19) . . ? C14 O4 Cu2 126.6(2) . . ? C19 O5 Cu2 125.04(19) . . ? C21 O6 Cu2 125.96(19) . . ? C28 O7 Cu3 126.1(2) . . ? C30 O8 Cu3 125.8(2) . . ? C35 O9 Cu3 125.12(19) . . ? C37 O10 Cu3 126.02(19) . . ? C44 O11 Cu1 125.89(18) . . ? C46 O12 Cu1 126.22(19) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C1 C2 C3 117.3(3) . . ? C1 C2 H2A 108.0 . . ? C3 C2 H2A 108.0 . . ? C1 C2 H2B 108.0 . . ? C3 C2 H2B 108.0 . . ? H2A C2 H2B 107.2 . . ? O1 C3 C4 124.7(3) . . ? O1 C3 C2 115.1(2) . . ? C4 C3 C2 120.2(3) . . ? C5 C4 C3 124.9(3) . . ? C5 C4 H4 117.5 . . ? C3 C4 H4 117.5 . . ? O2 C5 C4 124.3(3) . . ? O2 C5 C6 115.4(2) . . ? C4 C5 C6 120.3(3) . . ? C11 C6 C7 118.1(3) . . ? C11 C6 C5 119.5(3) . . ? C7 C6 C5 122.4(3) . . ? C8 C7 C6 121.5(3) . . ? C8 C7 H7 119.2 . . ? C6 C7 H7 119.2 . . ? C9 C8 C7 120.3(3) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C10 118.5(3) . . ? C8 C9 C12 123.1(3) . . ? C10 C9 C12 118.4(3) . . ? C11 C10 C9 120.8(3) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C6 C11 C10 120.8(3) . . ? C6 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? O3 C12 C13 124.9(3) . . ? O3 C12 C9 114.0(3) . . ? C13 C12 C9 121.1(3) . . ? C12 C13 C14 123.4(3) . . ? C12 C13 H13 118.3 . . ? C14 C13 H13 118.3 . . ? O4 C14 C13 125.3(3) . . ? O4 C14 C15 113.8(3) . . ? C13 C14 C15 120.8(3) . . ? C16 C15 C14 120.6(4) . . ? C16 C15 H15A 107.2 . . ? C14 C15 H15A 107.2 . . ? C16 C15 H15B 107.2 . . ? C14 C15 H15B 107.2 . . ? H15A C15 H15B 106.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C18 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C17 C18 C19 110.8(3) . . ? C17 C18 H18A 109.5 . . ? C19 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? O5 C19 C20 125.8(3) . . ? O5 C19 C18 114.8(3) . . ? C20 C19 C18 119.4(3) . . ? C19 C20 C21 124.9(3) . . ? C19 C20 H20 117.5 . . ? C21 C20 H20 117.5 . . ? O6 C21 C20 124.3(3) . . ? O6 C21 C22 115.0(3) . . ? C20 C21 C22 120.7(3) . . ? C27 C22 C23 117.2(3) . . ? C27 C22 C21 120.3(3) . . ? C23 C22 C21 122.5(3) . . ? C24 C23 C22 121.4(3) . . ? C24 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C23 C24 C25 121.1(3) . . ? C23 C24 H24 119.5 . . ? C25 C24 H24 119.5 . . ? C26 C25 C24 117.8(3) . . ? C26 C25 C28 119.6(3) . . ? C24 C25 C28 122.7(3) . . ? C27 C26 C25 120.9(3) . . ? C27 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C26 C27 C22 121.6(3) . . ? C26 C27 H27 119.2 . . ? C22 C27 H27 119.2 . . ? O7 C28 C29 124.1(3) . . ? O7 C28 C25 115.8(3) . . ? C29 C28 C25 120.1(3) . . ? C28 C29 C30 124.5(3) . . ? C28 C29 H29 117.8 . . ? C30 C29 H29 117.8 . . ? O8 C30 C29 124.8(3) . . ? O8 C30 C31 117.1(3) . . ? C29 C30 C31 118.1(3) . . ? C32 C31 C30 110.6(3) . . ? C32 C31 H31A 109.5 . . ? C30 C31 H31A 109.5 . . ? C32 C31 H31B 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 108.1 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 H33A 109.5 . . ? C34 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C34 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 C33 112.0(3) . . ? C35 C34 H34A 109.2 . . ? C33 C34 H34A 109.2 . . ? C35 C34 H34B 109.2 . . ? C33 C34 H34B 109.2 . . ? H34A C34 H34B 107.9 . . ? O9 C35 C36 125.3(3) . . ? O9 C35 C34 115.3(3) . . ? C36 C35 C34 119.4(3) . . ? C37 C36 C35 124.4(3) . . ? C37 C36 H36 117.8 . . ? C35 C36 H36 117.8 . . ? O10 C37 C36 124.5(3) . . ? O10 C37 C38 114.6(3) . . ? C36 C37 C38 120.8(3) . . ? C39 C38 C43 118.5(3) . . ? C39 C38 C37 122.2(3) . . ? C43 C38 C37 119.2(3) . . ? C38 C39 C40 120.6(3) . . ? C38 C39 H39 119.7 . . ? C40 C39 H39 119.7 . . ? C39 C40 C41 121.2(3) . . ? C39 C40 H40 119.4 . . ? C41 C40 H40 119.4 . . ? C42 C41 C40 117.7(3) . . ? C42 C41 C44 119.2(3) . . ? C40 C41 C44 123.1(3) . . ? C43 C42 C41 121.4(3) . . ? C43 C42 H42 119.3 . . ? C41 C42 H42 119.3 . . ? C42 C43 C38 120.5(3) . . ? C42 C43 H43 119.8 . . ? C38 C43 H43 119.8 . . ? O11 C44 C45 125.0(3) . . ? O11 C44 C41 115.3(3) . . ? C45 C44 C41 119.7(3) . . ? C46 C45 C44 124.6(3) . . ? C46 C45 H45 117.7 . . ? C44 C45 H45 117.7 . . ? O12 C46 C45 125.1(3) . . ? O12 C46 C47 113.8(3) . . ? C45 C46 C47 121.1(3) . . ? C48 C47 C46 117.5(3) . . ? C48 C47 H47A 107.9 . . ? C46 C47 H47A 107.9 . . ? C48 C47 H47B 107.9 . . ? C46 C47 H47B 107.9 . . ? H47A C47 H47B 107.2 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O12 Cu1 O1 C3 158.2(3) . . . . ? O2 Cu1 O1 C3 -19.1(3) . . . . ? O2 Cu1 O1 C3 -104.8(2) 2_777 . . . ? O1 Cu1 O2 C5 22.5(2) . . . . ? O11 Cu1 O2 C5 -149.6(2) . . . . ? O2 Cu1 O2 C5 120.9(2) 2_777 . . . ? O1 Cu1 O2 Cu1 -98.39(8) . . . 2_777 ? O11 Cu1 O2 Cu1 89.49(8) . . . 2_777 ? O2 Cu1 O2 Cu1 0.000(1) 2_777 . . 2_777 ? O4 Cu2 O3 C12 3.2(3) . . . . ? O6 Cu2 O3 C12 178.5(3) . . . . ? O3 Cu2 O4 C14 0.0(3) . . . . ? O5 Cu2 O4 C14 174.7(3) . . . . ? O4 Cu2 O5 C19 171.7(3) . . . . ? O6 Cu2 O5 C19 -3.7(3) . . . . ? O3 Cu2 O6 C21 178.7(3) . . . . ? O5 Cu2 O6 C21 4.0(3) . . . . ? O10 Cu3 O7 C28 -165.6(3) . . . . ? O8 Cu3 O7 C28 14.9(3) . . . . ? O9 Cu3 O8 C30 166.5(3) . . . . ? O7 Cu3 O8 C30 -15.3(3) . . . . ? O10 Cu3 O9 C35 10.2(3) . . . . ? O8 Cu3 O9 C35 -170.3(3) . . . . ? O9 Cu3 O10 C37 -9.5(3) . . . . ? O7 Cu3 O10 C37 172.3(3) . . . . ? O12 Cu1 O11 C44 -2.1(2) . . . . ? O2 Cu1 O11 C44 175.0(2) . . . . ? O2 Cu1 O11 C44 -99.5(2) 2_777 . . . ? O1 Cu1 O12 C46 -171.8(3) . . . . ? O11 Cu1 O12 C46 0.3(3) . . . . ? O2 Cu1 O12 C46 90.0(2) 2_777 . . . ? Cu1 O1 C3 C4 8.6(5) . . . . ? Cu1 O1 C3 C2 -170.8(2) . . . . ? C1 C2 C3 O1 -164.8(3) . . . . ? C1 C2 C3 C4 15.8(5) . . . . ? O1 C3 C4 C5 6.5(5) . . . . ? C2 C3 C4 C5 -174.1(3) . . . . ? Cu1 O2 C5 C4 -15.9(4) . . . . ? Cu1 O2 C5 C4 96.5(3) 2_777 . . . ? Cu1 O2 C5 C6 164.97(19) . . . . ? Cu1 O2 C5 C6 -82.6(3) 2_777 . . . ? C3 C4 C5 O2 -2.4(5) . . . . ? C3 C4 C5 C6 176.7(3) . . . . ? O2 C5 C6 C11 -7.0(4) . . . . ? C4 C5 C6 C11 173.8(3) . . . . ? O2 C5 C6 C7 173.9(3) . . . . ? C4 C5 C6 C7 -5.3(5) . . . . ? C11 C6 C7 C8 0.5(5) . . . . ? C5 C6 C7 C8 179.6(3) . . . . ? C6 C7 C8 C9 -0.8(6) . . . . ? C7 C8 C9 C10 0.8(5) . . . . ? C7 C8 C9 C12 -179.0(3) . . . . ? C8 C9 C10 C11 -0.5(5) . . . . ? C12 C9 C10 C11 179.3(3) . . . . ? C7 C6 C11 C10 -0.2(5) . . . . ? C5 C6 C11 C10 -179.3(3) . . . . ? C9 C10 C11 C6 0.2(5) . . . . ? Cu2 O3 C12 C13 -3.7(5) . . . . ? Cu2 O3 C12 C9 176.17(19) . . . . ? C8 C9 C12 O3 174.3(3) . . . . ? C10 C9 C12 O3 -5.6(4) . . . . ? C8 C9 C12 C13 -5.8(5) . . . . ? C10 C9 C12 C13 174.3(3) . . . . ? O3 C12 C13 C14 0.4(6) . . . . ? C9 C12 C13 C14 -179.5(3) . . . . ? Cu2 O4 C14 C13 -2.8(6) . . . . ? Cu2 O4 C14 C15 176.4(3) . . . . ? C12 C13 C14 O4 3.1(7) . . . . ? C12 C13 C14 C15 -176.1(4) . . . . ? O4 C14 C15 C16 -172.6(5) . . . . ? C13 C14 C15 C16 6.6(8) . . . . ? Cu2 O5 C19 C20 0.8(5) . . . . ? Cu2 O5 C19 C18 178.3(2) . . . . ? C17 C18 C19 O5 -66.5(4) . . . . ? C17 C18 C19 C20 111.2(3) . . . . ? O5 C19 C20 C21 3.5(6) . . . . ? C18 C19 C20 C21 -173.9(3) . . . . ? Cu2 O6 C21 C20 -1.5(5) . . . . ? Cu2 O6 C21 C22 176.9(2) . . . . ? C19 C20 C21 O6 -3.1(5) . . . . ? C19 C20 C21 C22 178.6(3) . . . . ? O6 C21 C22 C27 -10.0(5) . . . . ? C20 C21 C22 C27 168.4(3) . . . . ? O6 C21 C22 C23 169.4(3) . . . . ? C20 C21 C22 C23 -12.2(5) . . . . ? C27 C22 C23 C24 -1.7(5) . . . . ? C21 C22 C23 C24 178.9(3) . . . . ? C22 C23 C24 C25 0.4(6) . . . . ? C23 C24 C25 C26 1.2(5) . . . . ? C23 C24 C25 C28 -179.9(3) . . . . ? C24 C25 C26 C27 -1.5(6) . . . . ? C28 C25 C26 C27 179.6(3) . . . . ? C25 C26 C27 C22 0.2(6) . . . . ? C23 C22 C27 C26 1.4(6) . . . . ? C21 C22 C27 C26 -179.2(3) . . . . ? Cu3 O7 C28 C29 -7.9(5) . . . . ? Cu3 O7 C28 C25 170.8(2) . . . . ? C26 C25 C28 O7 1.7(5) . . . . ? C24 C25 C28 O7 -177.1(3) . . . . ? C26 C25 C28 C29 -179.4(4) . . . . ? C24 C25 C28 C29 1.7(5) . . . . ? O7 C28 C29 C30 -4.5(7) . . . . ? C25 C28 C29 C30 176.8(4) . . . . ? Cu3 O8 C30 C29 9.0(5) . . . . ? Cu3 O8 C30 C31 -173.8(2) . . . . ? C28 C29 C30 O8 4.0(7) . . . . ? C28 C29 C30 C31 -173.3(4) . . . . ? O8 C30 C31 C32 -93.8(4) . . . . ? C29 C30 C31 C32 83.7(5) . . . . ? Cu3 O9 C35 C36 -6.3(4) . . . . ? Cu3 O9 C35 C34 175.08(19) . . . . ? C33 C34 C35 O9 73.7(3) . . . . ? C33 C34 C35 C36 -105.0(3) . . . . ? O9 C35 C36 C37 -2.3(5) . . . . ? C34 C35 C36 C37 176.3(3) . . . . ? Cu3 O10 C37 C36 4.6(4) . . . . ? Cu3 O10 C37 C38 -174.46(19) . . . . ? C35 C36 C37 O10 3.2(5) . . . . ? C35 C36 C37 C38 -177.7(3) . . . . ? O10 C37 C38 C39 -160.8(3) . . . . ? C36 C37 C38 C39 20.0(5) . . . . ? O10 C37 C38 C43 16.7(4) . . . . ? C36 C37 C38 C43 -162.4(3) . . . . ? C43 C38 C39 C40 1.7(5) . . . . ? C37 C38 C39 C40 179.3(3) . . . . ? C38 C39 C40 C41 1.3(5) . . . . ? C39 C40 C41 C42 -2.8(5) . . . . ? C39 C40 C41 C44 177.0(3) . . . . ? C40 C41 C42 C43 1.3(5) . . . . ? C44 C41 C42 C43 -178.6(3) . . . . ? C41 C42 C43 C38 1.8(5) . . . . ? C39 C38 C43 C42 -3.3(5) . . . . ? C37 C38 C43 C42 179.1(3) . . . . ? Cu1 O11 C44 C45 2.5(4) . . . . ? Cu1 O11 C44 C41 -179.12(19) . . . . ? C42 C41 C44 O11 -0.2(4) . . . . ? C40 C41 C44 O11 179.9(3) . . . . ? C42 C41 C44 C45 178.3(3) . . . . ? C40 C41 C44 C45 -1.6(5) . . . . ? O11 C44 C45 C46 -0.5(5) . . . . ? C41 C44 C45 C46 -178.9(3) . . . . ? Cu1 O12 C46 C45 1.3(4) . . . . ? Cu1 O12 C46 C47 -179.3(2) . . . . ? C44 C45 C46 O12 -1.5(5) . . . . ? C44 C45 C46 C47 179.1(3) . . . . ? O12 C46 C47 C48 169.1(3) . . . . ? C45 C46 C47 C48 -11.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.044 _refine_diff_density_min -0.500 _refine_diff_density_rms 0.113 # Attachment '(2)Cu3L3Bipy.CIF' data_lj41sad _database_code_depnum_ccdc_archive 'CCDC 292065' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H64 Cu3 N2 O13, 2.75(C4 H8 O)' _chemical_formula_sum 'C73 H86 Cu3 N2 O15.75' _chemical_formula_weight 1434.06 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 15.0084(18) _cell_length_b 15.8591(18) _cell_length_c 17.910(2) _cell_angle_alpha 112.600(2) _cell_angle_beta 103.553(2) _cell_angle_gamma 101.522(2) _cell_volume 3621.1(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 15099 _cell_measurement_theta_min 2.252 _cell_measurement_theta_max 28.279 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.599 _exptl_crystal_size_mid 0.350 _exptl_crystal_size_min 0.183 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.315 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1502 _exptl_absorpt_coefficient_mu 0.938 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.703 _exptl_absorpt_correction_T_max 0.841 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 376 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.19 _diffrn_reflns_number 35294 _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 28.32 _reflns_number_total 16536 _reflns_number_gt 13036 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT and XPREP (Siemens, 1995)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997), WINGX-32 (Farrugia, 1999)' _computing_publication_material 'enCIFer (CCDC, 2003)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1326P)^2^+8.3004P] 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 16536 _refine_ls_number_parameters 799 _refine_ls_number_restraints 62 _refine_ls_R_factor_all 0.0819 _refine_ls_R_factor_gt 0.0653 _refine_ls_wR_factor_ref 0.2119 _refine_ls_wR_factor_gt 0.1961 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 1.511 _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 0.84217(5) 0.58824(5) 0.08339(4) 0.02181(18) Uani 1 1 d . . . Cu2 Cu 1.24098(5) 0.51083(5) 0.61236(4) 0.0299(2) Uani 1 1 d . A . Cu3 Cu 1.12797(5) 0.01738(5) -0.02328(4) 0.02582(19) Uani 1 1 d . . . N1 N 0.7023(3) 0.4779(4) 0.0653(3) 0.0274(10) Uani 1 1 d . . . N2 N 0.2761(4) 0.1322(4) 0.0062(3) 0.0295(10) Uani 1 1 d . . . O1 O 0.8042(3) 0.7010(3) 0.1353(3) 0.0290(8) Uani 1 1 d . . . O2 O 0.9088(3) 0.5972(3) 0.1941(2) 0.0252(8) Uani 1 1 d . . . O3 O 1.1685(3) 0.5500(3) 0.5356(3) 0.0347(10) Uani 1 1 d . A . O4 O 1.2184(4) 0.5966(4) 0.7104(3) 0.0441(12) Uani 1 1 d . . . O5 O 1.3068(4) 0.4642(4) 0.6868(3) 0.0423(11) Uani 1 1 d . . . O6 O 1.2418(3) 0.4087(3) 0.5106(3) 0.0334(9) Uani 1 1 d . . . O7 O 1.1463(3) 0.0769(3) 0.0987(3) 0.0281(8) Uani 1 1 d . . . O8 O 1.1851(3) -0.0796(3) -0.0153(3) 0.0317(9) Uani 1 1 d . . . O9 O 1.0961(3) -0.0527(3) -0.1468(3) 0.0334(9) Uani 1 1 d . . . O10 O 1.0565(3) 0.1032(3) -0.0351(2) 0.0265(8) Uani 1 1 d . . . O11 O 0.8942(3) 0.4865(3) 0.0349(2) 0.0257(8) Uani 1 1 d . . . O12 O 0.7943(3) 0.5914(3) -0.0253(3) 0.0288(8) Uani 1 1 d . B . C1 C 0.7884(6) 0.8884(6) 0.3299(6) 0.0517(18) Uani 1 1 d . . . H1A H 0.7599 0.9400 0.3356 0.078 Uiso 1 1 calc R . . H1B H 0.8570 0.9164 0.3662 0.078 Uiso 1 1 calc R . . H1C H 0.7542 0.8447 0.3481 0.078 Uiso 1 1 calc R . . C2 C 0.7793(5) 0.8325(5) 0.2365(4) 0.0382(14) Uani 1 1 d . . . H2A H 0.7097 0.8068 0.2010 0.046 Uiso 1 1 calc R . . H2B H 0.8119 0.8785 0.2189 0.046 Uiso 1 1 calc R . . C3 C 0.8197(4) 0.7496(4) 0.2150(4) 0.0269(11) Uani 1 1 d . . . C4 C 0.8691(4) 0.7308(4) 0.2804(4) 0.0282(11) Uani 1 1 d . . . H4 H 0.8755 0.7712 0.3380 0.034 Uiso 1 1 calc R . . C5 C 0.9098(4) 0.6561(4) 0.2665(3) 0.0235(10) Uani 1 1 d . . . C6 C 0.9608(4) 0.6429(4) 0.3418(3) 0.0237(10) Uani 1 1 d . . . C7 C 0.9396(4) 0.6736(4) 0.4176(4) 0.0293(12) Uani 1 1 d . . . H7 H 0.8915 0.7042 0.4227 0.035 Uiso 1 1 calc R . . C8 C 0.9886(5) 0.6596(4) 0.4861(4) 0.0316(12) Uani 1 1 d . . . H8 H 0.9727 0.6798 0.5372 0.038 Uiso 1 1 calc R . . C9 C 1.0600(4) 0.6165(4) 0.4802(3) 0.0281(11) Uani 1 1 d . A . C10 C 1.0806(5) 0.5845(4) 0.4038(4) 0.0323(13) Uani 1 1 d . . . H10 H 1.1285 0.5537 0.3988 0.039 Uiso 1 1 calc R . . C11 C 1.0316(4) 0.5975(4) 0.3355(4) 0.0294(12) Uani 1 1 d . . . H11 H 1.0462 0.5754 0.2838 0.035 Uiso 1 1 calc R . . C12 C 1.1160(5) 0.6027(4) 0.5537(3) 0.0313(12) Uani 1 1 d D . . C13A C 1.1250(10) 0.6632(10) 0.6359(6) 0.0360(10) Uiso 0.50 1 d PD A 1 H13A H 1.0943 0.7113 0.6436 0.043 Uiso 0.50 1 calc PR A 1 C14A C 1.1764(10) 0.6583(10) 0.7089(7) 0.0360(10) Uiso 0.50 1 d PD A 1 C15A C 1.1665(9) 0.7217(9) 0.7926(8) 0.0360(10) Uiso 0.50 1 d PD A 1 H15A H 1.2195 0.7281 0.8414 0.043 Uiso 0.50 1 calc PR A 1 H15B H 1.1731 0.7869 0.7968 0.043 Uiso 0.50 1 calc PR A 1 C16A C 1.0717(9) 0.6819(10) 0.7993(9) 0.0360(10) Uiso 0.50 1 d PD A 1 H16A H 1.0688 0.7241 0.8548 0.054 Uiso 0.50 1 calc PR A 1 H16B H 1.0648 0.6172 0.7948 0.054 Uiso 0.50 1 calc PR A 1 H16C H 1.0191 0.6781 0.7525 0.054 Uiso 0.50 1 calc PR A 1 C13B C 1.0930(10) 0.6318(10) 0.6315(7) 0.0360(10) Uiso 0.50 1 d PD A 2 H13B H 1.0410 0.6575 0.6333 0.043 Uiso 0.50 1 calc PR A 2 C14B C 1.1420(10) 0.6250(10) 0.7051(7) 0.0360(10) Uiso 0.50 1 d PD A 2 C15B C 1.1162(9) 0.6594(9) 0.7862(8) 0.0360(10) Uiso 0.50 1 d PD A 2 H15C H 1.1027 0.6050 0.8007 0.043 Uiso 0.50 1 calc PR A 2 H15D H 1.1740 0.7109 0.8337 0.043 Uiso 0.50 1 calc PR A 2 C16B C 1.0322(9) 0.6971(10) 0.7845(9) 0.0360(10) Uiso 0.50 1 d PD A 2 H16D H 1.0236 0.7174 0.8406 0.054 Uiso 0.50 1 calc PR A 2 H16E H 0.9733 0.6462 0.7398 0.054 Uiso 0.50 1 calc PR A 2 H16F H 1.0448 0.7524 0.7720 0.054 Uiso 0.50 1 calc PR A 2 C17 C 1.4842(7) 0.4397(8) 0.7820(6) 0.071(3) Uani 1 1 d . A . H17A H 1.5179 0.4263 0.8279 0.107 Uiso 1 1 calc R . . H17B H 1.4809 0.5054 0.8071 0.107 Uiso 1 1 calc R . . H17C H 1.5196 0.4338 0.7416 0.107 Uiso 1 1 calc R . . C18 C 1.3832(6) 0.3686(6) 0.7347(5) 0.0503(19) Uani 1 1 d . . . H18A H 1.3476 0.3739 0.7755 0.060 Uiso 1 1 calc R A . H18B H 1.3865 0.3021 0.7101 0.060 Uiso 1 1 calc R . . C19 C 1.3294(5) 0.3879(5) 0.6628(4) 0.0403(15) Uani 1 1 d . A . C20 C 1.3119(5) 0.3231(5) 0.5777(4) 0.0385(15) Uani 1 1 d . . . H20 H 1.3296 0.2665 0.5676 0.046 Uiso 1 1 calc R A . C21 C 1.2697(4) 0.3365(4) 0.5062(4) 0.0293(12) Uani 1 1 d . A . C22 C 1.2537(4) 0.2638(4) 0.4174(4) 0.0277(11) Uani 1 1 d . . . C23 C 1.2964(5) 0.1912(5) 0.4010(4) 0.0349(13) Uani 1 1 d . A . H23 H 1.3382 0.1873 0.4476 0.042 Uiso 1 1 calc R . . C24 C 1.2777(5) 0.1243(5) 0.3165(4) 0.0340(13) Uani 1 1 d . . . H24 H 1.3066 0.0747 0.3063 0.041 Uiso 1 1 calc R A . C25 C 1.2176(4) 0.1287(4) 0.2469(4) 0.0274(11) Uani 1 1 d . A . C26 C 1.1756(4) 0.2018(4) 0.2635(4) 0.0315(12) Uani 1 1 d . . . H26 H 1.1341 0.2058 0.2169 0.038 Uiso 1 1 calc R A . C27 C 1.1935(5) 0.2682(5) 0.3468(4) 0.0327(13) Uani 1 1 d . A . H27 H 1.1646 0.3178 0.3568 0.039 Uiso 1 1 calc R . . C28 C 1.1980(4) 0.0597(4) 0.1546(4) 0.0268(11) Uani 1 1 d . . . C29 C 1.2377(5) -0.0152(4) 0.1368(4) 0.0336(13) Uani 1 1 d . A . H29 H 1.2740 -0.0219 0.1842 0.040 Uiso 1 1 calc R . . C30 C 1.2276(4) -0.0805(4) 0.0548(4) 0.0307(12) Uani 1 1 d . . . C31 C 1.2734(5) -0.1597(5) 0.0453(5) 0.0430(16) Uani 1 1 d . A . H31A H 1.2612 -0.1868 0.0847 0.052 Uiso 1 1 calc R . . H31B H 1.2429 -0.2124 -0.0144 0.052 Uiso 1 1 calc R . . C32 C 1.3795(8) -0.1225(8) 0.0650(8) 0.075(3) Uani 1 1 d . . . H32A H 1.4069 -0.1750 0.0587 0.112 Uiso 1 1 calc R A . H32B H 1.4099 -0.0709 0.1243 0.112 Uiso 1 1 calc R . . H32C H 1.3917 -0.0970 0.0251 0.112 Uiso 1 1 calc R . . C33 C 0.9792(5) -0.0843(5) -0.3673(4) 0.0417(15) Uani 1 1 d . . . H33A H 0.9806 -0.1293 -0.4225 0.063 Uiso 1 1 calc R . . H33B H 1.0033 -0.0180 -0.3590 0.063 Uiso 1 1 calc R . . H33C H 0.9125 -0.0982 -0.3674 0.063 Uiso 1 1 calc R . . C34 C 1.0432(5) -0.0957(5) -0.2942(4) 0.0389(14) Uani 1 1 d . . . H34A H 1.0187 -0.1635 -0.3050 0.047 Uiso 1 1 calc R . . H34B H 1.1093 -0.0844 -0.2972 0.047 Uiso 1 1 calc R . . C35 C 1.0512(4) -0.0311(4) -0.2029(4) 0.0305(12) Uani 1 1 d . . . C36 C 1.0139(4) 0.0447(4) -0.1865(4) 0.0292(12) Uani 1 1 d . . . H36 H 0.9823 0.0539 -0.2340 0.035 Uiso 1 1 calc R . . C37 C 1.0198(4) 0.1088(4) -0.1039(4) 0.0248(11) Uani 1 1 d . . . C38 C 0.9829(4) 0.1923(4) -0.0929(3) 0.0237(10) Uani 1 1 d . . . C39 C 0.9542(5) 0.2188(5) -0.1582(4) 0.0319(12) Uani 1 1 d . . . H39 H 0.9571 0.1823 -0.2133 0.038 Uiso 1 1 calc R . . C40 C 0.9212(5) 0.2978(4) -0.1441(4) 0.0309(12) Uani 1 1 d . . . H40 H 0.9018 0.3144 -0.1895 0.037 Uiso 1 1 calc R . . C41 C 0.9165(4) 0.3527(4) -0.0635(3) 0.0232(10) Uani 1 1 d . . . C42 C 0.9473(4) 0.3273(4) 0.0020(4) 0.0281(11) Uani 1 1 d . . . H42 H 0.9461 0.3648 0.0576 0.034 Uiso 1 1 calc R . . C43 C 0.9797(4) 0.2483(4) -0.0120(4) 0.0281(11) Uani 1 1 d . . . H43 H 0.9998 0.2323 0.0337 0.034 Uiso 1 1 calc R . . C44 C 0.8801(4) 0.4372(4) -0.0438(3) 0.0236(10) Uani 1 1 d . . . C45 C 0.8333(5) 0.4565(5) -0.1099(4) 0.0328(13) Uani 1 1 d . B . H45 H 0.8261 0.4150 -0.1674 0.039 Uiso 1 1 calc R . . C46 C 0.7966(5) 0.5340(5) -0.0959(4) 0.0351(13) Uani 1 1 d D . . C47A C 0.7408(9) 0.5356(10) -0.1778(8) 0.0464(17) Uiso 0.55 1 d PD B 1 H47A H 0.7189 0.4709 -0.2274 0.056 Uiso 0.55 1 calc PR B 1 H47B H 0.6834 0.5553 -0.1716 0.056 Uiso 0.55 1 calc PR B 1 C48A C 0.8095(10) 0.6077(10) -0.1911(9) 0.0464(17) Uiso 0.55 1 d PD B 1 H48A H 0.7763 0.6117 -0.2432 0.070 Uiso 0.55 1 calc PR B 1 H48B H 0.8657 0.5870 -0.1977 0.070 Uiso 0.55 1 calc PR B 1 H48C H 0.8311 0.6713 -0.1413 0.070 Uiso 0.55 1 calc PR B 1 C47B C 0.7699(14) 0.5702(12) -0.1632(9) 0.0464(17) Uiso 0.45 1 d PD B 2 H47C H 0.7016 0.5683 -0.1737 0.056 Uiso 0.45 1 calc PR B 2 H47D H 0.8099 0.6388 -0.1373 0.056 Uiso 0.45 1 calc PR B 2 C48B C 0.7802(13) 0.5190(12) -0.2496(9) 0.0464(17) Uiso 0.45 1 d PD B 2 H48D H 0.7619 0.5512 -0.2849 0.070 Uiso 0.45 1 calc PR B 2 H48E H 0.7378 0.4518 -0.2786 0.070 Uiso 0.45 1 calc PR B 2 H48F H 0.8476 0.5209 -0.2413 0.070 Uiso 0.45 1 calc PR B 2 C49 C 0.7043(4) 0.4316(5) 0.1140(4) 0.0331(13) Uani 1 1 d . . . H49 H 0.7638 0.4472 0.1574 0.040 Uiso 1 1 calc R . . C50 C 0.6238(4) 0.3620(5) 0.1043(4) 0.0326(13) Uani 1 1 d . . . H50 H 0.6290 0.3308 0.1404 0.039 Uiso 1 1 calc R . . C51 C 0.5359(4) 0.3382(4) 0.0416(3) 0.0238(10) Uani 1 1 d . . . C52 C 0.5343(4) 0.3855(5) -0.0099(4) 0.0352(14) Uani 1 1 d . . . H52 H 0.4761 0.3713 -0.0542 0.042 Uiso 1 1 calc R . . C53 C 0.6184(4) 0.4536(5) 0.0040(4) 0.0358(14) Uani 1 1 d . . . H53 H 0.6160 0.4845 -0.0321 0.043 Uiso 1 1 calc R . . C54 C 0.4468(4) 0.2674(4) 0.0307(4) 0.0247(10) Uani 1 1 d . . . C55 C 0.4496(5) 0.1915(5) 0.0512(6) 0.0451(18) Uani 1 1 d . . . H55 H 0.5099 0.1841 0.0738 0.054 Uiso 1 1 calc R . . C56 C 0.3635(5) 0.1265(5) 0.0382(6) 0.0455(17) Uani 1 1 d . . . H56 H 0.3668 0.0754 0.0529 0.055 Uiso 1 1 calc R . . C57 C 0.2743(4) 0.2088(5) -0.0075(4) 0.0336(13) Uani 1 1 d . . . H57 H 0.2134 0.2175 -0.0253 0.040 Uiso 1 1 calc R . . C58 C 0.3567(4) 0.2765(5) 0.0030(4) 0.0346(13) Uani 1 1 d . . . H58 H 0.3513 0.3292 -0.0088 0.042 Uiso 1 1 calc R . . O1T O 1.4040(5) 0.6113(5) 0.6392(4) 0.0678(17) Uani 1 1 d . . . C1T C 1.4666(7) 0.6614(8) 0.7273(7) 0.074(3) Uani 1 1 d . A . H1T1 H 1.4585 0.6193 0.7558 0.089 Uiso 1 1 calc R . . H1T2 H 1.4508 0.7199 0.7583 0.089 Uiso 1 1 calc R . . C2T C 1.5647(10) 0.6878(14) 0.7289(10) 0.130(7) Uani 1 1 d . . . H2T1 H 1.6106 0.6905 0.7801 0.156 Uiso 1 1 calc R A . H2T2 H 1.5839 0.7508 0.7281 0.156 Uiso 1 1 calc R . . C3T C 1.5596(11) 0.6055(16) 0.6459(13) 0.157(9) Uani 1 1 d . A . H3T1 H 1.6000 0.6307 0.6178 0.188 Uiso 1 1 calc R . . H3T2 H 1.5837 0.5571 0.6586 0.188 Uiso 1 1 calc R . . C4T C 1.4627(9) 0.5637(10) 0.5920(9) 0.089(3) Uani 1 1 d . A . H4T1 H 1.4409 0.4937 0.5751 0.106 Uiso 1 1 calc R . . H4T2 H 1.4552 0.5721 0.5392 0.106 Uiso 1 1 calc R . . O2T O 0.7263(10) 0.0575(10) 0.4656(7) 0.0793(17) Uiso 0.60 1 d PD C 1 C6T C 0.7897(13) 0.0538(13) 0.5965(9) 0.0793(17) Uiso 0.60 1 d PD C 1 H6T1 H 0.8286 0.0114 0.6016 0.095 Uiso 0.60 1 calc PR C 1 H6T2 H 0.7641 0.0714 0.6446 0.095 Uiso 0.60 1 calc PR C 1 C5T C 0.7103(11) 0.0051(11) 0.5135(10) 0.0793(17) Uiso 0.60 1 d PD C 1 H5T1 H 0.7088 -0.0621 0.4815 0.095 Uiso 0.60 1 calc PR C 1 H5T2 H 0.6476 0.0036 0.5226 0.095 Uiso 0.60 1 calc PR C 1 C7T C 0.8489(12) 0.1407(12) 0.5981(9) 0.0793(17) Uiso 0.60 1 d PD C 1 H7T1 H 0.9187 0.1519 0.6244 0.095 Uiso 0.60 1 calc PR C 1 H7T2 H 0.8329 0.1981 0.6316 0.095 Uiso 0.60 1 calc PR C 1 C8T C 0.8249(13) 0.1218(16) 0.5069(12) 0.0793(17) Uiso 0.60 1 d PD C 1 H8T1 H 0.8301 0.1825 0.5018 0.095 Uiso 0.60 1 calc PR C 1 H8T2 H 0.8687 0.0911 0.4811 0.095 Uiso 0.60 1 calc PR C 1 O7T O 0.7169(13) 0.0817(15) 0.4844(12) 0.0793(17) Uiso 0.40 1 d PD D 2 C26T C 0.8714(12) 0.096(2) 0.5634(18) 0.0793(17) Uiso 0.40 1 d PD D 2 H26A H 0.9156 0.0668 0.5366 0.095 Uiso 0.40 1 calc PR D 2 H26B H 0.9105 0.1483 0.6217 0.095 Uiso 0.40 1 calc PR D 2 C28T C 0.7057(13) 0.030(2) 0.5329(19) 0.0793(17) Uiso 0.40 1 d PD D 2 H28A H 0.6582 -0.0352 0.4956 0.095 Uiso 0.40 1 calc PR D 2 H28B H 0.6828 0.0646 0.5799 0.095 Uiso 0.40 1 calc PR D 2 C25T C 0.8026(16) 0.024(2) 0.5687(19) 0.0793(17) Uiso 0.40 1 d PD D 2 H25A H 0.8159 0.0366 0.6294 0.095 Uiso 0.40 1 calc PR D 2 H25B H 0.8056 -0.0406 0.5352 0.095 Uiso 0.40 1 calc PR D 2 C27T C 0.8172(16) 0.133(2) 0.510(2) 0.0793(17) Uiso 0.40 1 d PD D 2 H27A H 0.8301 0.2033 0.5443 0.095 Uiso 0.40 1 calc PR D 2 H27B H 0.8369 0.1229 0.4593 0.095 Uiso 0.40 1 calc PR D 2 O3T O 0.6178(7) 0.1410(7) 0.1775(6) 0.0699(14) Uiso 0.75 1 d P . . C9T C 0.6223(10) 0.1435(11) 0.2584(9) 0.0699(14) Uiso 0.75 1 d P . . H9T1 H 0.5569 0.1155 0.2579 0.084 Uiso 0.75 1 calc PR . . H9T2 H 0.6509 0.2107 0.3049 0.084 Uiso 0.75 1 calc PR . . C10T C 0.6869(10) 0.0829(10) 0.2717(9) 0.0699(14) Uiso 0.75 1 d P . . H10A H 0.7563 0.1220 0.2970 0.084 Uiso 0.75 1 calc PR . . H10B H 0.6710 0.0546 0.3094 0.084 Uiso 0.75 1 calc PR . . C11T C 0.6634(11) 0.0091(10) 0.1854(9) 0.0699(14) Uiso 0.75 1 d P . . H11A H 0.6095 -0.0483 0.1712 0.084 Uiso 0.75 1 calc PR . . H11B H 0.7203 -0.0107 0.1770 0.084 Uiso 0.75 1 calc PR . . C12T C 0.6333(11) 0.0608(10) 0.1308(9) 0.0699(14) Uiso 0.75 1 d P . . H12A H 0.6850 0.0770 0.1081 0.084 Uiso 0.75 1 calc PR . . H12B H 0.5735 0.0171 0.0812 0.084 Uiso 0.75 1 calc PR . . O4T O 0.6160(8) 0.0806(7) 0.7045(8) 0.0588(17) Uiso 0.50 1 d PD . . C13T C 0.5157(9) 0.0693(10) 0.6802(11) 0.0588(17) Uiso 0.50 1 d PD . . H13C H 0.4816 0.0205 0.6945 0.071 Uiso 0.50 1 calc PR . . H13D H 0.4882 0.0463 0.6172 0.071 Uiso 0.50 1 calc PR . . C14T C 0.5021(10) 0.1596(12) 0.7248(12) 0.0588(17) Uiso 0.50 1 d PD . . H14A H 0.4684 0.1563 0.7655 0.071 Uiso 0.50 1 calc PR . . H14B H 0.4629 0.1767 0.6835 0.071 Uiso 0.50 1 calc PR . . C15T C 0.6013(11) 0.2330(9) 0.7725(11) 0.0588(17) Uiso 0.50 1 d PD . . H15E H 0.6042 0.2916 0.7643 0.071 Uiso 0.50 1 calc PR . . H15F H 0.6212 0.2514 0.8349 0.071 Uiso 0.50 1 calc PR . . C16T C 0.6627(9) 0.1813(9) 0.7324(11) 0.0588(17) Uiso 0.50 1 d PD . . H16G H 0.6678 0.1928 0.6827 0.071 Uiso 0.50 1 calc PR . . H16H H 0.7286 0.2035 0.7746 0.071 Uiso 0.50 1 calc PR . . O5T O 0.5047(14) 0.2267(14) 0.5571(13) 0.050(2) Uiso 0.25 1 d PD E 1 C17T C 0.552(2) 0.3215(12) 0.5682(18) 0.050(2) Uiso 0.25 1 d PD E 1 C18T C 0.6350(16) 0.3101(15) 0.5364(17) 0.050(2) Uiso 0.25 1 d PD E 1 C19T C 0.587(2) 0.2133(16) 0.4589(15) 0.050(2) Uiso 0.25 1 d PD E 1 C20T C 0.5266(18) 0.1589(11) 0.4910(16) 0.050(2) Uiso 0.25 1 d PD E 1 O6T O 0.5635(14) 0.3104(14) 0.5868(12) 0.050(2) Uiso 0.25 1 d PD F 2 C21T C 0.6580(15) 0.3369(17) 0.5806(14) 0.050(2) Uiso 0.25 1 d PD F 2 C22T C 0.6501(17) 0.2758(16) 0.4921(15) 0.050(2) Uiso 0.25 1 d PD F 2 C23T C 0.5627(19) 0.1913(16) 0.4609(14) 0.050(2) Uiso 0.25 1 d PD F 2 C24T C 0.519(2) 0.2109(16) 0.5299(17) 0.050(2) Uiso 0.25 1 d PD F 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0232(3) 0.0242(3) 0.0215(3) 0.0135(3) 0.0050(2) 0.0115(3) Cu2 0.0362(4) 0.0324(4) 0.0191(3) 0.0110(3) 0.0022(3) 0.0170(3) Cu3 0.0269(4) 0.0218(3) 0.0280(4) 0.0093(3) 0.0088(3) 0.0112(3) N1 0.024(2) 0.030(2) 0.029(2) 0.016(2) 0.0061(19) 0.0075(19) N2 0.026(2) 0.027(2) 0.036(3) 0.017(2) 0.007(2) 0.0083(19) O1 0.031(2) 0.032(2) 0.029(2) 0.0173(17) 0.0061(16) 0.0168(17) O2 0.0270(19) 0.0280(19) 0.0215(18) 0.0126(16) 0.0044(15) 0.0126(16) O3 0.047(3) 0.041(2) 0.0210(19) 0.0156(18) 0.0077(18) 0.026(2) O4 0.062(3) 0.050(3) 0.0187(19) 0.0119(19) 0.005(2) 0.033(3) O5 0.052(3) 0.049(3) 0.024(2) 0.016(2) 0.0016(19) 0.028(2) O6 0.037(2) 0.038(2) 0.025(2) 0.0138(18) 0.0037(17) 0.0207(19) O7 0.032(2) 0.0257(19) 0.029(2) 0.0130(17) 0.0108(17) 0.0134(16) O8 0.036(2) 0.025(2) 0.035(2) 0.0120(17) 0.0130(18) 0.0148(17) O9 0.035(2) 0.031(2) 0.030(2) 0.0082(18) 0.0095(18) 0.0177(18) O10 0.0257(19) 0.027(2) 0.0253(19) 0.0097(16) 0.0068(15) 0.0128(16) O11 0.031(2) 0.0265(19) 0.0231(18) 0.0131(16) 0.0074(15) 0.0152(16) O12 0.033(2) 0.036(2) 0.028(2) 0.0207(18) 0.0115(17) 0.0202(18) C1 0.058(5) 0.043(4) 0.061(5) 0.023(4) 0.023(4) 0.027(4) C2 0.044(4) 0.040(3) 0.042(3) 0.022(3) 0.016(3) 0.027(3) C3 0.026(3) 0.027(3) 0.031(3) 0.016(2) 0.008(2) 0.012(2) C4 0.033(3) 0.029(3) 0.024(3) 0.012(2) 0.008(2) 0.016(2) C5 0.019(2) 0.027(3) 0.022(2) 0.012(2) 0.0022(19) 0.006(2) C6 0.024(3) 0.023(2) 0.023(2) 0.011(2) 0.004(2) 0.008(2) C7 0.031(3) 0.033(3) 0.027(3) 0.015(2) 0.008(2) 0.017(2) C8 0.040(3) 0.033(3) 0.022(3) 0.013(2) 0.008(2) 0.015(3) C9 0.037(3) 0.022(3) 0.019(2) 0.008(2) 0.001(2) 0.010(2) C10 0.040(3) 0.033(3) 0.025(3) 0.013(2) 0.007(2) 0.022(3) C11 0.034(3) 0.034(3) 0.023(3) 0.014(2) 0.007(2) 0.017(2) C12 0.040(3) 0.025(3) 0.022(3) 0.009(2) 0.000(2) 0.013(2) C17 0.060(5) 0.101(8) 0.047(5) 0.033(5) -0.003(4) 0.041(5) C18 0.059(5) 0.066(5) 0.034(3) 0.029(4) 0.006(3) 0.036(4) C19 0.042(4) 0.052(4) 0.032(3) 0.025(3) 0.005(3) 0.026(3) C20 0.041(3) 0.047(4) 0.033(3) 0.020(3) 0.007(3) 0.029(3) C21 0.027(3) 0.034(3) 0.029(3) 0.016(2) 0.006(2) 0.015(2) C22 0.027(3) 0.031(3) 0.027(3) 0.014(2) 0.006(2) 0.013(2) C23 0.036(3) 0.039(3) 0.031(3) 0.017(3) 0.005(2) 0.020(3) C24 0.037(3) 0.031(3) 0.034(3) 0.014(3) 0.008(3) 0.020(3) C25 0.025(3) 0.025(3) 0.031(3) 0.012(2) 0.008(2) 0.008(2) C26 0.035(3) 0.031(3) 0.029(3) 0.015(2) 0.007(2) 0.016(2) C27 0.037(3) 0.033(3) 0.030(3) 0.014(2) 0.008(2) 0.020(3) C28 0.024(3) 0.023(3) 0.030(3) 0.012(2) 0.007(2) 0.005(2) C29 0.034(3) 0.024(3) 0.035(3) 0.009(2) 0.004(2) 0.012(2) C30 0.026(3) 0.021(3) 0.039(3) 0.011(2) 0.005(2) 0.007(2) C31 0.041(4) 0.027(3) 0.052(4) 0.013(3) 0.005(3) 0.019(3) C32 0.068(6) 0.071(6) 0.101(8) 0.040(6) 0.038(6) 0.041(5) C33 0.046(4) 0.039(4) 0.028(3) 0.006(3) 0.011(3) 0.012(3) C34 0.042(4) 0.036(3) 0.034(3) 0.007(3) 0.016(3) 0.021(3) C35 0.025(3) 0.028(3) 0.031(3) 0.006(2) 0.011(2) 0.008(2) C36 0.030(3) 0.029(3) 0.024(3) 0.008(2) 0.008(2) 0.012(2) C37 0.019(2) 0.024(3) 0.029(3) 0.009(2) 0.008(2) 0.007(2) C38 0.019(2) 0.023(3) 0.025(3) 0.009(2) 0.006(2) 0.006(2) C39 0.040(3) 0.035(3) 0.026(3) 0.013(2) 0.015(2) 0.017(3) C40 0.040(3) 0.033(3) 0.027(3) 0.017(2) 0.014(2) 0.017(3) C41 0.020(2) 0.025(3) 0.025(3) 0.013(2) 0.007(2) 0.006(2) C42 0.036(3) 0.028(3) 0.023(3) 0.011(2) 0.010(2) 0.016(2) C43 0.035(3) 0.027(3) 0.021(2) 0.010(2) 0.006(2) 0.012(2) C44 0.021(2) 0.027(3) 0.026(3) 0.014(2) 0.008(2) 0.009(2) C45 0.042(3) 0.041(3) 0.022(3) 0.016(2) 0.011(2) 0.024(3) C46 0.037(3) 0.050(4) 0.032(3) 0.027(3) 0.014(3) 0.024(3) C49 0.022(3) 0.043(3) 0.036(3) 0.025(3) 0.003(2) 0.007(2) C50 0.026(3) 0.039(3) 0.039(3) 0.028(3) 0.005(2) 0.008(2) C51 0.021(2) 0.025(3) 0.026(3) 0.013(2) 0.006(2) 0.009(2) C52 0.027(3) 0.043(4) 0.033(3) 0.024(3) 0.000(2) 0.003(3) C53 0.030(3) 0.044(4) 0.036(3) 0.029(3) 0.003(2) 0.004(3) C54 0.022(2) 0.026(3) 0.027(3) 0.013(2) 0.007(2) 0.009(2) C55 0.025(3) 0.046(4) 0.081(5) 0.045(4) 0.015(3) 0.017(3) C56 0.032(3) 0.039(4) 0.079(5) 0.040(4) 0.016(3) 0.015(3) C57 0.023(3) 0.035(3) 0.044(3) 0.024(3) 0.003(2) 0.007(2) C58 0.027(3) 0.036(3) 0.047(4) 0.029(3) 0.006(3) 0.011(2) O1T 0.061(4) 0.075(4) 0.051(3) 0.024(3) 0.013(3) 0.005(3) C1T 0.058(6) 0.067(6) 0.071(6) 0.027(5) -0.006(5) 0.008(5) C2T 0.076(9) 0.156(15) 0.094(10) 0.040(10) 0.004(7) -0.028(9) C3T 0.073(9) 0.184(19) 0.147(16) 0.023(14) 0.050(10) -0.001(11) C4T 0.072(7) 0.098(9) 0.091(8) 0.034(7) 0.028(6) 0.037(7) _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 O11 1.926(4) . ? Cu1 O12 1.934(4) . ? Cu1 O2 1.936(4) . ? Cu1 O1 1.940(4) . ? Cu1 N1 2.313(5) . ? Cu2 O4 1.917(5) . ? Cu2 O3 1.919(4) . ? Cu2 O6 1.923(4) . ? Cu2 O5 1.933(4) . ? Cu2 O1T 2.461(7) . ? Cu3 O10 1.936(4) . ? Cu3 O8 1.939(4) . ? Cu3 O9 1.940(4) . ? Cu3 O7 1.941(4) . ? Cu3 N2 2.372(5) 1_655 ? N1 C53 1.331(8) . ? N1 C49 1.337(7) . ? N2 C57 1.334(8) . ? N2 C56 1.339(8) . ? N2 Cu3 2.372(5) 1_455 ? O1 C3 1.269(7) . ? O2 C5 1.269(7) . ? O3 C12 1.264(7) . ? O4 C14A 1.271(13) . ? O4 C14B 1.310(13) . ? O5 C19 1.264(8) . ? O6 C21 1.277(7) . ? O7 C28 1.269(7) . ? O8 C30 1.274(8) . ? O9 C35 1.273(8) . ? O10 C37 1.270(7) . ? O11 C44 1.262(7) . ? O12 C46 1.256(8) . ? C1 C2 1.518(10) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.510(8) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.401(7) . ? C4 C5 1.405(8) . ? C4 H4 0.9500 . ? C5 C6 1.498(7) . ? C6 C7 1.392(8) . ? C6 C11 1.400(8) . ? C7 C8 1.395(8) . ? C7 H7 0.9500 . ? C8 C9 1.384(9) . ? C8 H8 0.9500 . ? C9 C10 1.397(8) . ? C9 C12 1.504(7) . ? C10 C11 1.383(8) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13A 1.370(11) . ? C12 C13B 1.439(11) . ? C13A C14A 1.391(12) . ? C13A H13A 0.9500 . ? C14A C15A 1.512(12) . ? C15A C16A 1.489(12) . ? C15A H15A 0.9900 . ? C15A H15B 0.9900 . ? C16A H16A 0.9800 . ? C16A H16B 0.9800 . ? C16A H16C 0.9800 . ? C13B C14B 1.406(12) . ? C13B H13B 0.9500 . ? C14B C15B 1.516(12) . ? C15B C16B 1.498(12) . ? C15B H15C 0.9900 . ? C15B H15D 0.9900 . ? C16B H16D 0.9800 . ? C16B H16E 0.9800 . ? C16B H16F 0.9800 . ? C17 C18 1.507(13) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.523(8) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.395(9) . ? C20 C21 1.403(8) . ? C20 H20 0.9500 . ? C21 C22 1.490(8) . ? C22 C23 1.395(8) . ? C22 C27 1.405(8) . ? C23 C24 1.394(9) . ? C23 H23 0.9500 . ? C24 C25 1.392(8) . ? C24 H24 0.9500 . ? C25 C26 1.396(8) . ? C25 C28 1.507(8) . ? C26 C27 1.378(8) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C29 1.395(8) . ? C29 C30 1.385(9) . ? C29 H29 0.9500 . ? C30 C31 1.522(8) . ? C31 C32 1.487(12) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.528(10) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.518(8) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.386(8) . ? C36 C37 1.407(8) . ? C36 H36 0.9500 . ? C37 C38 1.498(7) . ? C38 C39 1.393(8) . ? C38 C43 1.396(8) . ? C39 C40 1.393(8) . ? C39 H39 0.9500 . ? C40 C41 1.397(8) . ? C40 H40 0.9500 . ? C41 C42 1.392(7) . ? C41 C44 1.495(8) . ? C42 C43 1.388(8) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 C45 1.401(7) . ? C45 C46 1.406(9) . ? C45 H45 0.9500 . ? C46 C47A 1.521(11) . ? C46 C47B 1.530(12) . ? C47A C48A 1.511(12) . ? C47A H47A 0.9900 . ? C47A H47B 0.9900 . ? C48A H48A 0.9800 . ? C48A H48B 0.9800 . ? C48A H48C 0.9800 . ? C47B C48B 1.507(13) . ? C47B H47C 0.9900 . ? C47B H47D 0.9900 . ? C48B H48D 0.9800 . ? C48B H48E 0.9800 . ? C48B H48F 0.9800 . ? C49 C50 1.390(8) . ? C49 H49 0.9500 . ? C50 C51 1.388(8) . ? C50 H50 0.9500 . ? C51 C52 1.395(8) . ? C51 C54 1.482(8) . ? C52 C53 1.385(8) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C54 C58 1.385(8) . ? C54 C55 1.392(8) . ? C55 C56 1.389(9) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 C58 1.387(8) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? O1T C1T 1.430(11) . ? O1T C4T 1.479(13) . ? C1T C2T 1.437(17) . ? C1T H1T1 0.9900 . ? C1T H1T2 0.9900 . ? C2T C3T 1.53(2) . ? C2T H2T1 0.9900 . ? C2T H2T2 0.9900 . ? C3T C4T 1.397(19) . ? C3T H3T1 0.9900 . ? C3T H3T2 0.9900 . ? C4T H4T1 0.9900 . ? C4T H4T2 0.9900 . ? O2T C5T 1.431(12) . ? O2T C8T 1.443(12) . ? C6T C5T 1.465(12) . ? C6T C7T 1.469(12) . ? C6T H6T1 0.9900 . ? C6T H6T2 0.9900 . ? C5T H5T1 0.9900 . ? C5T H5T2 0.9900 . ? C7T C8T 1.481(13) . ? C7T H7T1 0.9900 . ? C7T H7T2 0.9900 . ? C8T H8T1 0.9900 . ? C8T H8T2 0.9900 . ? O7T C28T 1.418(13) . ? O7T C27T 1.427(13) . ? C26T C25T 1.42(2) . ? C26T C27T 1.481(10) . ? C26T H26A 0.9900 . ? C26T H26B 0.9900 . ? C28T C25T 1.482(14) . ? C28T H28A 0.9900 . ? C28T H28B 0.9900 . ? C25T H25A 0.9900 . ? C25T H25B 0.9900 . ? C27T H27A 0.9900 . ? C27T H27B 0.9900 . ? O3T C12T 1.328(16) . ? O3T C9T 1.419(16) . ? C9T C10T 1.536(19) . ? C9T H9T1 0.9900 . ? C9T H9T2 0.9900 . ? C10T C11T 1.441(19) . ? C10T H10A 0.9900 . ? C10T H10B 0.9900 . ? C11T C12T 1.546(19) . ? C11T H11A 0.9900 . ? C11T H11B 0.9900 . ? C12T H12A 0.9900 . ? C12T H12B 0.9900 . ? O4T C13T 1.419(12) . ? O4T C16T 1.437(12) . ? C13T C14T 1.43(2) . ? C13T H13C 0.9900 . ? C13T H13D 0.9900 . ? C14T C15T 1.50(2) . ? C14T H14A 0.9900 . ? C14T H14B 0.9900 . ? C15T C16T 1.483(10) . ? C15T H15E 0.9900 . ? C15T H15F 0.9900 . ? C16T H16G 0.9900 . ? C16T H16H 0.9900 . ? O5T C20T 1.418(13) . ? O5T C17T 1.441(13) . ? C17T C18T 1.506(14) . ? C18T C19T 1.501(14) . ? C19T C20T 1.483(13) . ? O6T C24T 1.415(15) . ? O6T C21T 1.439(14) . ? C21T C22T 1.468(13) . ? C22T C23T 1.485(14) . ? C23T C24T 1.490(15) . ? 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 O11 Cu1 O12 92.64(16) . . ? O11 Cu1 O2 86.18(16) . . ? O12 Cu1 O2 171.30(18) . . ? O11 Cu1 O1 173.39(18) . . ? O12 Cu1 O1 87.46(17) . . ? O2 Cu1 O1 92.73(16) . . ? O11 Cu1 N1 91.19(17) . . ? O12 Cu1 N1 96.34(17) . . ? O2 Cu1 N1 92.30(17) . . ? O1 Cu1 N1 95.37(18) . . ? O4 Cu2 O3 93.49(19) . . ? O4 Cu2 O6 169.6(2) . . ? O3 Cu2 O6 86.09(18) . . ? O4 Cu2 O5 87.2(2) . . ? O3 Cu2 O5 176.3(2) . . ? O6 Cu2 O5 92.63(19) . . ? O4 Cu2 O1T 98.2(2) . . ? O3 Cu2 O1T 97.9(2) . . ? O6 Cu2 O1T 92.2(2) . . ? O5 Cu2 O1T 85.5(2) . . ? O10 Cu3 O8 173.35(18) . . ? O10 Cu3 O9 92.34(17) . . ? O8 Cu3 O9 86.36(18) . . ? O10 Cu3 O7 87.66(17) . . ? O8 Cu3 O7 92.89(17) . . ? O9 Cu3 O7 173.40(18) . . ? O10 Cu3 N2 91.46(17) . 1_655 ? O8 Cu3 N2 95.18(18) . 1_655 ? O9 Cu3 N2 97.48(19) . 1_655 ? O7 Cu3 N2 89.11(18) . 1_655 ? C53 N1 C49 117.0(5) . . ? C53 N1 Cu1 122.5(4) . . ? C49 N1 Cu1 120.5(4) . . ? C57 N2 C56 116.7(5) . . ? C57 N2 Cu3 119.3(4) . 1_455 ? C56 N2 Cu3 124.0(4) . 1_455 ? C3 O1 Cu1 126.4(3) . . ? C5 O2 Cu1 125.9(3) . . ? C12 O3 Cu2 125.4(4) . . ? C14A O4 Cu2 123.5(6) . . ? C14B O4 Cu2 123.5(6) . . ? C19 O5 Cu2 126.0(4) . . ? C21 O6 Cu2 126.7(4) . . ? C28 O7 Cu3 125.0(4) . . ? C30 O8 Cu3 125.0(4) . . ? C35 O9 Cu3 125.9(4) . . ? C37 O10 Cu3 126.3(4) . . ? C44 O11 Cu1 126.7(3) . . ? C46 O12 Cu1 125.4(4) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C1 117.2(6) . . ? C3 C2 H2A 108.0 . . ? C1 C2 H2A 108.0 . . ? C3 C2 H2B 108.0 . . ? C1 C2 H2B 108.0 . . ? H2A C2 H2B 107.2 . . ? O1 C3 C4 124.9(5) . . ? O1 C3 C2 114.8(5) . . ? C4 C3 C2 120.3(5) . . ? C3 C4 C5 124.2(5) . . ? C3 C4 H4 117.9 . . ? C5 C4 H4 117.9 . . ? O2 C5 C4 125.6(5) . . ? O2 C5 C6 115.1(5) . . ? C4 C5 C6 119.4(5) . . ? C7 C6 C11 118.8(5) . . ? C7 C6 C5 122.2(5) . . ? C11 C6 C5 119.0(5) . . ? C6 C7 C8 120.4(5) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C9 C8 C7 120.5(5) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C10 119.2(5) . . ? C8 C9 C12 121.9(5) . . ? C10 C9 C12 118.8(5) . . ? C11 C10 C9 120.4(5) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 C6 120.6(5) . . ? C10 C11 H11 119.7 . . ? C6 C11 H11 119.7 . . ? O3 C12 C13A 124.0(7) . . ? O3 C12 C13B 124.0(7) . . ? O3 C12 C9 115.3(5) . . ? C13A C12 C9 118.8(7) . . ? C13B C12 C9 119.5(7) . . ? C12 C13A C14A 123.9(11) . . ? C12 C13A H13A 118.0 . . ? C14A C13A H13A 118.0 . . ? O4 C14A C13A 126.5(10) . . ? O4 C14A C15A 116.5(10) . . ? C13A C14A C15A 116.1(11) . . ? C16A C15A C14A 112.0(11) . . ? C16A C15A H15A 109.2 . . ? C14A C15A H15A 109.2 . . ? C16A C15A H15B 109.2 . . ? C14A C15A H15B 109.2 . . ? H15A C15A H15B 107.9 . . ? C15A C16A H16A 109.5 . . ? C15A C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? C15A C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? C14B C13B C12 124.6(10) . . ? C14B C13B H13B 117.7 . . ? C12 C13B H13B 117.7 . . ? O4 C14B C13B 121.8(10) . . ? O4 C14B C15B 115.7(9) . . ? C13B C14B C15B 122.3(11) . . ? C16B C15B C14B 117.5(11) . . ? C16B C15B H15C 107.9 . . ? C14B C15B H15C 107.9 . . ? C16B C15B H15D 107.9 . . ? C14B C15B H15D 107.9 . . ? H15C C15B H15D 107.2 . . ? C15B C16B H16D 109.5 . . ? C15B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? C15B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? C18 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C18 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C17 C18 C19 110.5(7) . . ? C17 C18 H18A 109.6 . . ? C19 C18 H18A 109.6 . . ? C17 C18 H18B 109.6 . . ? C19 C18 H18B 109.6 . . ? H18A C18 H18B 108.1 . . ? O5 C19 C20 125.9(6) . . ? O5 C19 C18 115.6(6) . . ? C20 C19 C18 118.5(6) . . ? C19 C20 C21 124.0(6) . . ? C19 C20 H20 118.0 . . ? C21 C20 H20 118.0 . . ? O6 C21 C20 124.5(6) . . ? O6 C21 C22 114.9(5) . . ? C20 C21 C22 120.6(5) . . ? C23 C22 C27 118.3(5) . . ? C23 C22 C21 122.6(5) . . ? C27 C22 C21 119.1(5) . . ? C24 C23 C22 120.1(5) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C25 C24 C23 121.3(5) . . ? C25 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? C24 C25 C26 118.4(5) . . ? C24 C25 C28 123.0(5) . . ? C26 C25 C28 118.6(5) . . ? C27 C26 C25 120.7(5) . . ? C27 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C26 C27 C22 121.1(5) . . ? C26 C27 H27 119.4 . . ? C22 C27 H27 119.4 . . ? O7 C28 C29 125.5(5) . . ? O7 C28 C25 115.2(5) . . ? C29 C28 C25 119.3(5) . . ? C30 C29 C28 124.3(6) . . ? C30 C29 H29 117.8 . . ? C28 C29 H29 117.8 . . ? O8 C30 C29 126.1(5) . . ? O8 C30 C31 115.4(6) . . ? C29 C30 C31 118.5(6) . . ? C32 C31 C30 111.4(6) . . ? C32 C31 H31A 109.3 . . ? C30 C31 H31A 109.3 . . ? C32 C31 H31B 109.3 . . ? C30 C31 H31B 109.3 . . ? H31A C31 H31B 108.0 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 H33A 109.5 . . ? C34 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C34 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 C33 117.5(5) . . ? C35 C34 H34A 107.9 . . ? C33 C34 H34A 107.9 . . ? C35 C34 H34B 107.9 . . ? C33 C34 H34B 107.9 . . ? H34A C34 H34B 107.2 . . ? O9 C35 C36 125.9(5) . . ? O9 C35 C34 113.7(5) . . ? C36 C35 C34 120.5(6) . . ? C35 C36 C37 124.0(6) . . ? C35 C36 H36 118.0 . . ? C37 C36 H36 118.0 . . ? O10 C37 C36 125.0(5) . . ? O10 C37 C38 115.6(5) . . ? C36 C37 C38 119.4(5) . . ? C39 C38 C43 118.2(5) . . ? C39 C38 C37 123.7(5) . . ? C43 C38 C37 118.1(5) . . ? C38 C39 C40 121.2(5) . . ? C38 C39 H39 119.4 . . ? C40 C39 H39 119.4 . . ? C39 C40 C41 120.5(5) . . ? C39 C40 H40 119.8 . . ? C41 C40 H40 119.8 . . ? C42 C41 C40 118.1(5) . . ? C42 C41 C44 118.3(5) . . ? C40 C41 C44 123.6(5) . . ? C43 C42 C41 121.5(5) . . ? C43 C42 H42 119.3 . . ? C41 C42 H42 119.3 . . ? C42 C43 C38 120.5(5) . . ? C42 C43 H43 119.7 . . ? C38 C43 H43 119.7 . . ? O11 C44 C45 124.5(5) . . ? O11 C44 C41 114.7(5) . . ? C45 C44 C41 120.8(5) . . ? C44 C45 C46 123.6(5) . . ? C44 C45 H45 118.2 . . ? C46 C45 H45 118.2 . . ? O12 C46 C45 126.2(5) . . ? O12 C46 C47A 118.6(8) . . ? C45 C46 C47A 114.4(8) . . ? O12 C46 C47B 110.1(7) . . ? C45 C46 C47B 122.9(8) . . ? C48A C47A C46 106.6(10) . . ? C48A C47A H47A 110.4 . . ? C46 C47A H47A 110.4 . . ? C48A C47A H47B 110.4 . . ? C46 C47A H47B 110.4 . . ? H47A C47A H47B 108.6 . . ? C47A C48A H48A 109.5 . . ? C47A C48A H48B 109.5 . . ? H48A C48A H48B 109.5 . . ? C47A C48A H48C 109.5 . . ? H48A C48A H48C 109.5 . . ? H48B C48A H48C 109.5 . . ? C48B C47B C46 119.0(12) . . ? C48B C47B H47C 107.6 . . ? C46 C47B H47C 107.6 . . ? C48B C47B H47D 107.6 . . ? C46 C47B H47D 107.6 . . ? H47C C47B H47D 107.0 . . ? C47B C48B H48D 109.5 . . ? C47B C48B H48E 109.5 . . ? H48D C48B H48E 109.5 . . ? C47B C48B H48F 109.5 . . ? H48D C48B H48F 109.5 . . ? H48E C48B H48F 109.5 . . ? N1 C49 C50 123.4(5) . . ? N1 C49 H49 118.3 . . ? C50 C49 H49 118.3 . . ? C51 C50 C49 119.5(5) . . ? C51 C50 H50 120.3 . . ? C49 C50 H50 120.3 . . ? C50 C51 C52 117.0(5) . . ? C50 C51 C54 121.8(5) . . ? C52 C51 C54 121.2(5) . . ? C53 C52 C51 119.5(5) . . ? C53 C52 H52 120.3 . . ? C51 C52 H52 120.3 . . ? N1 C53 C52 123.6(5) . . ? N1 C53 H53 118.2 . . ? C52 C53 H53 118.2 . . ? C58 C54 C55 116.8(5) . . ? C58 C54 C51 121.0(5) . . ? C55 C54 C51 122.2(5) . . ? C56 C55 C54 119.4(6) . . ? C56 C55 H55 120.3 . . ? C54 C55 H55 120.3 . . ? N2 C56 C55 123.5(6) . . ? N2 C56 H56 118.3 . . ? C55 C56 H56 118.3 . . ? N2 C57 C58 123.4(5) . . ? N2 C57 H57 118.3 . . ? C58 C57 H57 118.3 . . ? C54 C58 C57 119.9(5) . . ? C54 C58 H58 120.0 . . ? C57 C58 H58 120.0 . . ? C1T O1T C4T 104.4(8) . . ? C1T O1T Cu2 115.5(6) . . ? C4T O1T Cu2 117.5(7) . . ? O1T C1T C2T 108.0(10) . . ? O1T C1T H1T1 110.1 . . ? C2T C1T H1T1 110.1 . . ? O1T C1T H1T2 110.1 . . ? C2T C1T H1T2 110.1 . . ? H1T1 C1T H1T2 108.4 . . ? C1T C2T C3T 102.0(11) . . ? C1T C2T H2T1 111.4 . . ? C3T C2T H2T1 111.4 . . ? C1T C2T H2T2 111.4 . . ? C3T C2T H2T2 111.4 . . ? H2T1 C2T H2T2 109.2 . . ? C4T C3T C2T 107.3(14) . . ? C4T C3T H3T1 110.3 . . ? C2T C3T H3T1 110.3 . . ? C4T C3T H3T2 110.3 . . ? C2T C3T H3T2 110.3 . . ? H3T1 C3T H3T2 108.5 . . ? C3T C4T O1T 108.4(12) . . ? C3T C4T H4T1 110.0 . . ? O1T C4T H4T1 110.0 . . ? C3T C4T H4T2 110.0 . . ? O1T C4T H4T2 110.0 . . ? H4T1 C4T H4T2 108.4 . . ? C5T O2T C8T 107.7(8) . . ? C5T C6T C7T 105.8(8) . . ? C5T C6T H6T1 110.6 . . ? C7T C6T H6T1 110.6 . . ? C5T C6T H6T2 110.6 . . ? C7T C6T H6T2 110.6 . . ? H6T1 C6T H6T2 108.7 . . ? O2T C5T C6T 108.0(8) . . ? O2T C5T H5T1 110.1 . . ? C6T C5T H5T1 110.1 . . ? O2T C5T H5T2 110.1 . . ? C6T C5T H5T2 110.1 . . ? H5T1 C5T H5T2 108.4 . . ? C6T C7T C8T 105.6(8) . . ? C6T C7T H7T1 110.6 . . ? C8T C7T H7T1 110.6 . . ? C6T C7T H7T2 110.6 . . ? C8T C7T H7T2 110.6 . . ? H7T1 C7T H7T2 108.8 . . ? O2T C8T C7T 104.4(8) . . ? O2T C8T H8T1 110.9 . . ? C7T C8T H8T1 110.9 . . ? O2T C8T H8T2 110.9 . . ? C7T C8T H8T2 110.9 . . ? H8T1 C8T H8T2 108.9 . . ? C28T O7T C27T 109.0(9) . . ? C25T C26T C27T 107.5(9) . . ? C25T C26T H26A 110.2 . . ? C27T C26T H26A 110.2 . . ? C25T C26T H26B 110.2 . . ? C27T C26T H26B 110.2 . . ? H26A C26T H26B 108.5 . . ? O7T C28T C25T 106.1(9) . . ? O7T C28T H28A 110.5 . . ? C25T C28T H28A 110.5 . . ? O7T C28T H28B 110.5 . . ? C25T C28T H28B 110.5 . . ? H28A C28T H28B 108.7 . . ? C26T C25T C28T 107.2(9) . . ? C26T C25T H25A 110.3 . . ? C28T C25T H25A 110.3 . . ? C26T C25T H25B 110.3 . . ? C28T C25T H25B 110.3 . . ? H25A C25T H25B 108.5 . . ? O7T C27T C26T 106.8(9) . . ? O7T C27T H27A 110.4 . . ? C26T C27T H27A 110.4 . . ? O7T C27T H27B 110.4 . . ? C26T C27T H27B 110.4 . . ? H27A C27T H27B 108.6 . . ? C12T O3T C9T 107.8(11) . . ? O3T C9T C10T 105.4(11) . . ? O3T C9T H9T1 110.7 . . ? C10T C9T H9T1 110.7 . . ? O3T C9T H9T2 110.7 . . ? C10T C9T H9T2 110.7 . . ? H9T1 C9T H9T2 108.8 . . ? C11T C10T C9T 102.5(12) . . ? C11T C10T H10A 111.3 . . ? C9T C10T H10A 111.3 . . ? C11T C10T H10B 111.3 . . ? C9T C10T H10B 111.3 . . ? H10A C10T H10B 109.2 . . ? C10T C11T C12T 102.1(12) . . ? C10T C11T H11A 111.3 . . ? C12T C11T H11A 111.3 . . ? C10T C11T H11B 111.3 . . ? C12T C11T H11B 111.3 . . ? H11A C11T H11B 109.2 . . ? O3T C12T C11T 110.9(12) . . ? O3T C12T H12A 109.5 . . ? C11T C12T H12A 109.5 . . ? O3T C12T H12B 109.5 . . ? C11T C12T H12B 109.5 . . ? H12A C12T H12B 108.0 . . ? C13T O4T C16T 104.4(8) . . ? O4T C13T C14T 109.6(9) . . ? O4T C13T H13C 109.7 . . ? C14T C13T H13C 109.7 . . ? O4T C13T H13D 109.7 . . ? C14T C13T H13D 109.7 . . ? H13C C13T H13D 108.2 . . ? C13T C14T C15T 106.3(8) . . ? C13T C14T H14A 110.5 . . ? C15T C14T H14A 110.5 . . ? C13T C14T H14B 110.5 . . ? C15T C14T H14B 110.5 . . ? H14A C14T H14B 108.7 . . ? C16T C15T C14T 102.7(9) . . ? C16T C15T H15E 111.2 . . ? C14T C15T H15E 111.2 . . ? C16T C15T H15F 111.2 . . ? C14T C15T H15F 111.2 . . ? H15E C15T H15F 109.1 . . ? O4T C16T C15T 106.1(8) . . ? O4T C16T H16G 110.5 . . ? C15T C16T H16G 110.5 . . ? O4T C16T H16H 110.5 . . ? C15T C16T H16H 110.5 . . ? H16G C16T H16H 108.7 . . ? C20T O5T C17T 107.7(8) . . ? O5T C17T C18T 104.0(10) . . ? C19T C18T C17T 100.1(10) . . ? C20T C19T C18T 102.0(10) . . ? O5T C20T C19T 107.6(9) . . ? C24T O6T C21T 106.4(14) . . ? O6T C21T C22T 107.2(10) . . ? C21T C22T C23T 104.0(9) . . ? C22T C23T C24T 107.3(11) . . ? O6T C24T C23T 105.6(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O11 Cu1 N1 C53 -105.8(5) . . . . ? O12 Cu1 N1 C53 -13.1(5) . . . . ? O2 Cu1 N1 C53 167.9(5) . . . . ? O1 Cu1 N1 C53 75.0(5) . . . . ? O11 Cu1 N1 C49 70.4(5) . . . . ? O12 Cu1 N1 C49 163.2(5) . . . . ? O2 Cu1 N1 C49 -15.8(5) . . . . ? O1 Cu1 N1 C49 -108.8(5) . . . . ? O12 Cu1 O1 C3 -174.9(5) . . . . ? O2 Cu1 O1 C3 -3.6(5) . . . . ? N1 Cu1 O1 C3 89.0(5) . . . . ? O11 Cu1 O2 C5 179.2(5) . . . . ? O1 Cu1 O2 C5 5.7(5) . . . . ? N1 Cu1 O2 C5 -89.8(4) . . . . ? O4 Cu2 O3 C12 -9.8(6) . . . . ? O6 Cu2 O3 C12 159.8(5) . . . . ? O1T Cu2 O3 C12 -108.5(5) . . . . ? O3 Cu2 O4 C14A -6.2(9) . . . . ? O6 Cu2 O4 C14A -93.5(14) . . . . ? O5 Cu2 O4 C14A 177.5(9) . . . . ? O1T Cu2 O4 C14A 92.4(9) . . . . ? O3 Cu2 O4 C14B 27.8(9) . . . . ? O6 Cu2 O4 C14B -59.5(14) . . . . ? O5 Cu2 O4 C14B -148.6(9) . . . . ? O1T Cu2 O4 C14B 126.3(9) . . . . ? O4 Cu2 O5 C19 165.5(6) . . . . ? O6 Cu2 O5 C19 -4.1(6) . . . . ? O1T Cu2 O5 C19 -96.1(6) . . . . ? O4 Cu2 O6 C21 -82.3(11) . . . . ? O3 Cu2 O6 C21 -170.3(5) . . . . ? O5 Cu2 O6 C21 6.2(5) . . . . ? O1T Cu2 O6 C21 91.9(5) . . . . ? O10 Cu3 O7 C28 -174.4(4) . . . . ? O8 Cu3 O7 C28 12.3(5) . . . . ? N2 Cu3 O7 C28 -82.9(4) 1_655 . . . ? O9 Cu3 O8 C30 178.4(5) . . . . ? O7 Cu3 O8 C30 -8.1(5) . . . . ? N2 Cu3 O8 C30 81.2(5) 1_655 . . . ? O10 Cu3 O9 C35 5.5(5) . . . . ? O8 Cu3 O9 C35 179.0(5) . . . . ? N2 Cu3 O9 C35 -86.3(5) 1_655 . . . ? O9 Cu3 O10 C37 -8.7(5) . . . . ? O7 Cu3 O10 C37 178.0(4) . . . . ? N2 Cu3 O10 C37 88.9(4) 1_655 . . . ? O12 Cu1 O11 C44 -10.1(5) . . . . ? O2 Cu1 O11 C44 178.6(5) . . . . ? N1 Cu1 O11 C44 86.4(5) . . . . ? O11 Cu1 O12 C46 5.5(5) . . . . ? O1 Cu1 O12 C46 178.9(5) . . . . ? N1 Cu1 O12 C46 -86.0(5) . . . . ? Cu1 O1 C3 C4 1.0(8) . . . . ? Cu1 O1 C3 C2 -178.4(4) . . . . ? C1 C2 C3 O1 175.2(6) . . . . ? C1 C2 C3 C4 -4.3(9) . . . . ? O1 C3 C4 C5 1.2(10) . . . . ? C2 C3 C4 C5 -179.4(6) . . . . ? Cu1 O2 C5 C4 -5.4(8) . . . . ? Cu1 O2 C5 C6 175.6(3) . . . . ? C3 C4 C5 O2 1.2(9) . . . . ? C3 C4 C5 C6 -179.9(5) . . . . ? O2 C5 C6 C7 -155.5(5) . . . . ? C4 C5 C6 C7 25.4(8) . . . . ? O2 C5 C6 C11 23.9(7) . . . . ? C4 C5 C6 C11 -155.2(6) . . . . ? C11 C6 C7 C8 0.3(9) . . . . ? C5 C6 C7 C8 179.7(5) . . . . ? C6 C7 C8 C9 1.1(9) . . . . ? C7 C8 C9 C10 -1.9(9) . . . . ? C7 C8 C9 C12 178.3(6) . . . . ? C8 C9 C10 C11 1.3(9) . . . . ? C12 C9 C10 C11 -178.9(6) . . . . ? C9 C10 C11 C6 0.1(9) . . . . ? C7 C6 C11 C10 -0.9(9) . . . . ? C5 C6 C11 C10 179.7(5) . . . . ? Cu2 O3 C12 C13A 20.8(11) . . . . ? Cu2 O3 C12 C13B -8.0(11) . . . . ? Cu2 O3 C12 C9 -175.1(4) . . . . ? C8 C9 C12 O3 169.9(6) . . . . ? C10 C9 C12 O3 -9.8(9) . . . . ? C8 C9 C12 C13A -25.1(11) . . . . ? C10 C9 C12 C13A 155.1(9) . . . . ? C8 C9 C12 C13B 2.2(11) . . . . ? C10 C9 C12 C13B -177.6(8) . . . . ? O3 C12 C13A C14A -15.4(19) . . . . ? C13B C12 C13A C14A 83(2) . . . . ? C9 C12 C13A C14A -178.9(11) . . . . ? C14B O4 C14A C13A -87(2) . . . . ? Cu2 O4 C14A C13A 13(2) . . . . ? C14B O4 C14A C15A 81.7(18) . . . . ? Cu2 O4 C14A C15A -178.7(8) . . . . ? C12 C13A C14A O4 -3(2) . . . . ? C12 C13A C14A C15A -171.8(12) . . . . ? O4 C14A C15A C16A -94.2(15) . . . . ? C13A C14A C15A C16A 75.8(16) . . . . ? O3 C12 C13B C14B 15.3(18) . . . . ? C13A C12 C13B C14B -83(2) . . . . ? C9 C12 C13B C14B -178.1(11) . . . . ? C14A O4 C14B C13B 71.3(18) . . . . ? Cu2 O4 C14B C13B -28.3(18) . . . . ? C14A O4 C14B C15B -103(2) . . . . ? Cu2 O4 C14B C15B 157.5(8) . . . . ? C12 C13B C14B O4 5(2) . . . . ? C12 C13B C14B C15B 178.4(12) . . . . ? O4 C14B C15B C16B 177.1(11) . . . . ? C13B C14B C15B C16B 3(2) . . . . ? Cu2 O5 C19 C20 0.6(11) . . . . ? Cu2 O5 C19 C18 178.6(5) . . . . ? C17 C18 C19 O5 -70.1(9) . . . . ? C17 C18 C19 C20 108.1(9) . . . . ? O5 C19 C20 C21 3.0(13) . . . . ? C18 C19 C20 C21 -175.0(7) . . . . ? Cu2 O6 C21 C20 -4.9(9) . . . . ? Cu2 O6 C21 C22 174.6(4) . . . . ? C19 C20 C21 O6 -0.7(11) . . . . ? C19 C20 C21 C22 179.8(6) . . . . ? O6 C21 C22 C23 166.9(6) . . . . ? C20 C21 C22 C23 -13.6(9) . . . . ? O6 C21 C22 C27 -13.0(8) . . . . ? C20 C21 C22 C27 166.5(6) . . . . ? C27 C22 C23 C24 -1.0(10) . . . . ? C21 C22 C23 C24 179.1(6) . . . . ? C22 C23 C24 C25 0.7(10) . . . . ? C23 C24 C25 C26 -0.3(10) . . . . ? C23 C24 C25 C28 178.1(6) . . . . ? C24 C25 C26 C27 0.3(9) . . . . ? C28 C25 C26 C27 -178.2(6) . . . . ? C25 C26 C27 C22 -0.6(10) . . . . ? C23 C22 C27 C26 0.9(10) . . . . ? C21 C22 C27 C26 -179.2(6) . . . . ? Cu3 O7 C28 C29 -10.9(8) . . . . ? Cu3 O7 C28 C25 168.0(4) . . . . ? C24 C25 C28 O7 -176.0(6) . . . . ? C26 C25 C28 O7 2.4(8) . . . . ? C24 C25 C28 C29 3.1(9) . . . . ? C26 C25 C28 C29 -178.5(6) . . . . ? O7 C28 C29 C30 1.5(10) . . . . ? C25 C28 C29 C30 -177.4(6) . . . . ? Cu3 O8 C30 C29 2.4(9) . . . . ? Cu3 O8 C30 C31 -175.6(4) . . . . ? C28 C29 C30 O8 3.3(10) . . . . ? C28 C29 C30 C31 -178.8(6) . . . . ? O8 C30 C31 C32 100.1(8) . . . . ? C29 C30 C31 C32 -78.1(9) . . . . ? Cu3 O9 C35 C36 -2.2(9) . . . . ? Cu3 O9 C35 C34 176.0(4) . . . . ? C33 C34 C35 O9 172.0(6) . . . . ? C33 C34 C35 C36 -9.7(9) . . . . ? O9 C35 C36 C37 -0.7(10) . . . . ? C34 C35 C36 C37 -178.8(6) . . . . ? Cu3 O10 C37 C36 8.6(8) . . . . ? Cu3 O10 C37 C38 -170.0(3) . . . . ? C35 C36 C37 O10 -2.7(9) . . . . ? C35 C36 C37 C38 175.8(5) . . . . ? O10 C37 C38 C39 169.8(5) . . . . ? C36 C37 C38 C39 -8.9(8) . . . . ? O10 C37 C38 C43 -8.4(7) . . . . ? C36 C37 C38 C43 172.9(5) . . . . ? C43 C38 C39 C40 -1.3(9) . . . . ? C37 C38 C39 C40 -179.4(6) . . . . ? C38 C39 C40 C41 0.2(9) . . . . ? C39 C40 C41 C42 1.2(9) . . . . ? C39 C40 C41 C44 -178.7(5) . . . . ? C40 C41 C42 C43 -1.6(9) . . . . ? C44 C41 C42 C43 178.4(5) . . . . ? C41 C42 C43 C38 0.5(9) . . . . ? C39 C38 C43 C42 1.0(9) . . . . ? C37 C38 C43 C42 179.2(5) . . . . ? Cu1 O11 C44 C45 8.7(8) . . . . ? Cu1 O11 C44 C41 -170.5(3) . . . . ? C42 C41 C44 O11 10.0(7) . . . . ? C40 C41 C44 O11 -170.1(5) . . . . ? C42 C41 C44 C45 -169.3(5) . . . . ? C40 C41 C44 C45 10.7(8) . . . . ? O11 C44 C45 C46 0.2(10) . . . . ? C41 C44 C45 C46 179.3(6) . . . . ? Cu1 O12 C46 C45 0.5(10) . . . . ? Cu1 O12 C46 C47A 169.7(6) . . . . ? Cu1 O12 C46 C47B -169.5(8) . . . . ? C44 C45 C46 O12 -5.1(11) . . . . ? C44 C45 C46 C47A -174.8(7) . . . . ? C44 C45 C46 C47B 163.7(10) . . . . ? O12 C46 C47A C48A 89.9(11) . . . . ? C45 C46 C47A C48A -99.6(11) . . . . ? C47B C46 C47A C48A 19(2) . . . . ? O12 C46 C47B C48B 172.3(13) . . . . ? C45 C46 C47B C48B 2(2) . . . . ? C47A C46 C47B C48B -69(3) . . . . ? C53 N1 C49 C50 -1.1(10) . . . . ? Cu1 N1 C49 C50 -177.5(5) . . . . ? N1 C49 C50 C51 -0.3(10) . . . . ? C49 C50 C51 C52 1.2(9) . . . . ? C49 C50 C51 C54 -177.5(6) . . . . ? C50 C51 C52 C53 -0.8(10) . . . . ? C54 C51 C52 C53 178.0(6) . . . . ? C49 N1 C53 C52 1.5(10) . . . . ? Cu1 N1 C53 C52 177.9(5) . . . . ? C51 C52 C53 N1 -0.6(11) . . . . ? C50 C51 C54 C58 147.8(6) . . . . ? C52 C51 C54 C58 -30.9(9) . . . . ? C50 C51 C54 C55 -29.3(9) . . . . ? C52 C51 C54 C55 152.0(7) . . . . ? C58 C54 C55 C56 3.8(11) . . . . ? C51 C54 C55 C56 -179.0(7) . . . . ? C57 N2 C56 C55 -5.0(12) . . . . ? Cu3 N2 C56 C55 176.6(6) 1_455 . . . ? C54 C55 C56 N2 0.4(13) . . . . ? C56 N2 C57 C58 5.5(10) . . . . ? Cu3 N2 C57 C58 -176.1(5) 1_455 . . . ? C55 C54 C58 C57 -3.3(10) . . . . ? C51 C54 C58 C57 179.4(6) . . . . ? N2 C57 C58 C54 -1.4(11) . . . . ? O4 Cu2 O1T C1T 40.1(7) . . . . ? O3 Cu2 O1T C1T 134.8(7) . . . . ? O6 Cu2 O1T C1T -138.8(7) . . . . ? O5 Cu2 O1T C1T -46.4(7) . . . . ? O4 Cu2 O1T C4T 164.0(7) . . . . ? O3 Cu2 O1T C4T -101.3(7) . . . . ? O6 Cu2 O1T C4T -14.9(7) . . . . ? O5 Cu2 O1T C4T 77.6(7) . . . . ? C4T O1T C1T C2T 29.8(14) . . . . ? Cu2 O1T C1T C2T 160.3(10) . . . . ? O1T C1T C2T C3T -31.4(18) . . . . ? C1T C2T C3T C4T 21(2) . . . . ? C2T C3T C4T O1T -4(2) . . . . ? C1T O1T C4T C3T -15.3(17) . . . . ? Cu2 O1T C4T C3T -144.6(13) . . . . ? C8T O2T C5T C6T 14(2) . . . . ? C7T C6T C5T O2T 4(2) . . . . ? C5T C6T C7T C8T -20(2) . . . . ? C5T O2T C8T C7T -27(2) . . . . ? C6T C7T C8T O2T 29(2) . . . . ? C27T O7T C28T C25T -18(3) . . . . ? C27T C26T C25T C28T -10(4) . . . . ? O7T C28T C25T C26T 18(3) . . . . ? C28T O7T C27T C26T 12(4) . . . . ? C25T C26T C27T O7T -1(4) . . . . ? C12T O3T C9T C10T 25.6(14) . . . . ? O3T C9T C10T C11T -34.2(14) . . . . ? C9T C10T C11T C12T 27.9(14) . . . . ? C9T O3T C12T C11T -7.6(15) . . . . ? C10T C11T C12T O3T -14.4(16) . . . . ? C16T O4T C13T C14T -24.5(18) . . . . ? O4T C13T C14T C15T 6(2) . . . . ? C13T C14T C15T C16T 14.2(19) . . . . ? C13T O4T C16T C15T 33.5(17) . . . . ? C14T C15T C16T O4T -29.3(18) . . . . ? C20T O5T C17T C18T -25(3) . . . . ? O5T C17T C18T C19T 41(2) . . . . ? C17T C18T C19T C20T -40(2) . . . . ? C17T O5T C20T C19T -1(3) . . . . ? C18T C19T C20T O5T 27(3) . . . . ? C24T O6T C21T C22T 32(3) . . . . ? O6T C21T C22T C23T -22(3) . . . . ? C21T C22T C23T C24T 5(3) . . . . ? C21T O6T C24T C23T -28(3) . . . . ? C22T C23T C24T O6T 14(4) . . . . ? _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.743 _refine_diff_density_min -0.953 _refine_diff_density_rms 0.126 # Attachment '(3)Cu3L3Bipybipy.CIF' data_lj44sad _database_code_depnum_ccdc_archive 'CCDC 292066' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H64 Cu3 N2 O13, C10 H8 N2, 0.75(C4 H8 O)' _chemical_formula_sum 'C75 H78 Cu3 N4 O13.75' _chemical_formula_weight 1446.03 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 -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.0012(16) _cell_length_b 14.1336(16) _cell_length_c 18.328(2) _cell_angle_alpha 72.259(2) _cell_angle_beta 88.496(2) _cell_angle_gamma 83.084(2) _cell_volume 3429.0(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5591 _cell_measurement_theta_min 2.235 _cell_measurement_theta_max 25.254 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.401 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1506 _exptl_absorpt_coefficient_mu 0.990 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.807 _exptl_absorpt_correction_T_max 0.990 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 125 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.14 _diffrn_reflns_number 34047 _diffrn_reflns_av_R_equivalents 0.0509 _diffrn_reflns_av_sigmaI/netI 0.0904 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 28.34 _reflns_number_total 15835 _reflns_number_gt 9906 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT and XPREP (Siemens, 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2003)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997), WINGX-32 (Farrugia, 1999)' _computing_publication_material 'enCIFer 1.0 (CCDC, 2003)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0958P)^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 15835 _refine_ls_number_parameters 874 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1032 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.1616 _refine_ls_wR_factor_gt 0.1332 _refine_ls_goodness_of_fit_ref 0.923 _refine_ls_restrained_S_all 0.926 _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 0.47381(3) -0.88527(3) 0.71807(2) 0.02145(12) Uani 1 1 d . . . Cu2 Cu -0.08388(3) -0.30199(3) 0.51653(2) 0.02099(12) Uani 1 1 d . . . Cu3 Cu -0.03115(3) -0.70392(3) 1.10544(2) 0.02623(13) Uani 1 1 d . . . O1 O 0.56805(18) -0.87425(18) 0.63722(14) 0.0259(6) Uani 1 1 d . . . O2 O 0.40008(18) -0.75977(18) 0.66172(14) 0.0241(6) Uani 1 1 d . . . O3 O 0.02038(18) -0.40690(18) 0.52372(13) 0.0225(5) Uani 1 1 d . . . O4 O -0.06549(18) -0.24027(18) 0.40807(14) 0.0257(6) Uani 1 1 d . . . O5 O -0.19858(18) -0.20828(19) 0.50521(14) 0.0266(6) Uani 1 1 d . . . O6 O -0.11092(17) -0.36735(18) 0.62353(13) 0.0228(6) Uani 1 1 d . . . O7 O -0.05531(19) -0.60553(19) 1.00697(14) 0.0289(6) Uani 1 1 d . . . O8 O -0.1233(2) -0.6346(2) 1.15662(14) 0.0326(7) Uani 1 1 d . . . O9 O 0.00342(19) -0.7977(2) 1.20427(14) 0.0303(6) Uani 1 1 d . . . O10 O 0.06886(19) -0.7641(2) 1.05451(14) 0.0302(6) Uani 1 1 d . . . O11 O 0.40810(18) -0.86999(18) 0.80925(14) 0.0252(6) Uani 1 1 d . . . O12 O 0.55452(17) -1.00552(18) 0.77594(14) 0.0246(6) Uani 1 1 d . . . C1 C 0.7139(3) -0.7423(3) 0.5264(3) 0.0418(11) Uani 1 1 d . . . H1A H 0.7685 -0.7444 0.4921 0.063 Uiso 1 1 calc R . . H1B H 0.7374 -0.7626 0.5795 0.063 Uiso 1 1 calc R . . H1C H 0.6807 -0.6741 0.5131 0.063 Uiso 1 1 calc R . . C2 C 0.6448(3) -0.8132(3) 0.5181(2) 0.0283(9) Uani 1 1 d . . . H2A H 0.6216 -0.7932 0.4644 0.034 Uiso 1 1 calc R . . H2B H 0.6786 -0.8820 0.5307 0.034 Uiso 1 1 calc R . . C3 C 0.5601(3) -0.8115(3) 0.5708(2) 0.0222(8) Uani 1 1 d . . . C4 C 0.4814(3) -0.7376(3) 0.5443(2) 0.0255(8) Uani 1 1 d . . . H4 H 0.4794 -0.6999 0.4915 0.031 Uiso 1 1 calc R . . C5 C 0.4061(2) -0.7160(3) 0.5902(2) 0.0202(7) Uani 1 1 d . . . C6 C 0.3250(3) -0.6352(3) 0.5565(2) 0.0206(7) Uani 1 1 d . . . C7 C 0.3208(3) -0.5752(3) 0.4802(2) 0.0307(9) Uani 1 1 d . . . H7 H 0.3724 -0.5834 0.4470 0.037 Uiso 1 1 calc R . . C8 C 0.2430(3) -0.5041(3) 0.4519(2) 0.0313(9) Uani 1 1 d . . . H8 H 0.2414 -0.4654 0.3994 0.038 Uiso 1 1 calc R . . C9 C 0.1672(3) -0.4885(3) 0.4991(2) 0.0205(8) Uani 1 1 d . . . C10 C 0.1711(3) -0.5482(3) 0.5750(2) 0.0258(8) Uani 1 1 d . . . H10 H 0.1198 -0.5396 0.6082 0.031 Uiso 1 1 calc R . . C11 C 0.2486(3) -0.6205(3) 0.6032(2) 0.0263(8) Uani 1 1 d . . . H11 H 0.2494 -0.6606 0.6553 0.032 Uiso 1 1 calc R . . C12 C 0.0833(3) -0.4099(3) 0.4730(2) 0.0208(8) Uani 1 1 d . . . C13 C 0.0773(3) -0.3442(3) 0.3978(2) 0.0264(8) Uani 1 1 d . . . H13 H 0.1267 -0.3541 0.3634 0.032 Uiso 1 1 calc R . . C14 C 0.0047(3) -0.2660(3) 0.3697(2) 0.0241(8) Uani 1 1 d . . . C15 C 0.0041(3) -0.2050(3) 0.2862(2) 0.0333(10) Uani 1 1 d . . . H15A H 0.0709 -0.2055 0.2669 0.040 Uiso 1 1 calc R . . H15B H -0.0217 -0.1348 0.2808 0.040 Uiso 1 1 calc R . . C16 C -0.0572(4) -0.2470(4) 0.2385(3) 0.0559(14) Uani 1 1 d . . . H16A H -0.0569 -0.2060 0.1847 0.084 Uiso 1 1 calc R . . H16B H -0.1234 -0.2461 0.2573 0.084 Uiso 1 1 calc R . . H16C H -0.0307 -0.3160 0.2429 0.084 Uiso 1 1 calc R . . C17 C -0.4115(3) -0.0981(3) 0.5885(2) 0.0346(10) Uani 1 1 d . . . H17A H -0.4590 -0.0410 0.5640 0.052 Uiso 1 1 calc R . . H17B H -0.3827 -0.0869 0.6329 0.052 Uiso 1 1 calc R . . H17C H -0.4433 -0.1591 0.6054 0.052 Uiso 1 1 calc R . . C18 C -0.3336(3) -0.1093(3) 0.5317(2) 0.0292(9) Uani 1 1 d . . . H18A H -0.3048 -0.0456 0.5138 0.035 Uiso 1 1 calc R . . H18B H -0.3648 -0.1180 0.4867 0.035 Uiso 1 1 calc R . . C19 C -0.2520(3) -0.1939(3) 0.5586(2) 0.0218(8) Uani 1 1 d . . . C20 C -0.2395(3) -0.2483(3) 0.6357(2) 0.0266(8) Uani 1 1 d . . . H20 H -0.2816 -0.2289 0.6715 0.032 Uiso 1 1 calc R . . C21 C -0.1687(3) -0.3300(3) 0.6640(2) 0.0210(8) Uani 1 1 d . . . C22 C -0.1576(3) -0.3784(3) 0.74895(19) 0.0209(8) Uani 1 1 d . . . C23 C -0.2029(3) -0.3374(3) 0.8023(2) 0.0323(9) Uani 1 1 d . . . H23 H -0.2429 -0.2755 0.7850 0.039 Uiso 1 1 calc R . . C24 C -0.1913(3) -0.3843(3) 0.8802(2) 0.0332(10) Uani 1 1 d . . . H24 H -0.2233 -0.3543 0.9154 0.040 Uiso 1 1 calc R . . C25 C -0.1330(3) -0.4757(3) 0.9076(2) 0.0226(8) Uani 1 1 d . . . C26 C -0.0846(3) -0.5152(3) 0.8543(2) 0.0305(9) Uani 1 1 d . . . H26 H -0.0423 -0.5755 0.8716 0.037 Uiso 1 1 calc R . . C27 C -0.0972(3) -0.4681(3) 0.7769(2) 0.0295(9) Uani 1 1 d . . . H27 H -0.0640 -0.4972 0.7417 0.035 Uiso 1 1 calc R . . C28 C -0.1215(3) -0.5317(3) 0.9907(2) 0.0261(8) Uani 1 1 d . . . C29 C -0.1816(3) -0.5047(3) 1.0451(2) 0.0342(10) Uani 1 1 d . . . H29 H -0.2275 -0.4473 1.0274 0.041 Uiso 1 1 calc R . . C30 C -0.1794(3) -0.5555(3) 1.1231(2) 0.0316(9) Uani 1 1 d . . . C31 C -0.2456(3) -0.5141(4) 1.1756(2) 0.0453(12) Uani 1 1 d . . . H31A H -0.2966 -0.4645 1.1448 0.054 Uiso 1 1 calc R . . H31B H -0.2768 -0.5690 1.2114 0.054 Uiso 1 1 calc R . . C32 C -0.1900(4) -0.4650(4) 1.2205(3) 0.0650(16) Uani 1 1 d . . . H32A H -0.2338 -0.4392 1.2545 0.097 Uiso 1 1 calc R . . H32B H -0.1603 -0.4097 1.1851 0.097 Uiso 1 1 calc R . . H32C H -0.1397 -0.5142 1.2513 0.097 Uiso 1 1 calc R . . C33 C 0.1692(3) -1.0101(3) 1.3246(2) 0.0411(11) Uani 1 1 d . . . H33A H 0.1694 -1.0426 1.3801 0.062 Uiso 1 1 calc R . . H33B H 0.2298 -0.9814 1.3098 0.062 Uiso 1 1 calc R . . H33C H 0.1625 -1.0596 1.2981 0.062 Uiso 1 1 calc R . . C34 C 0.0857(3) -0.9277(3) 1.3027(2) 0.0317(9) Uani 1 1 d . . . H34A H 0.0258 -0.9580 1.3204 0.038 Uiso 1 1 calc R . . H34B H 0.0930 -0.8800 1.3314 0.038 Uiso 1 1 calc R . . C35 C 0.0724(3) -0.8687(3) 1.2188(2) 0.0253(8) Uani 1 1 d . . . C36 C 0.1339(3) -0.8933(3) 1.1639(2) 0.0267(8) Uani 1 1 d . . . H36 H 0.1816 -0.9492 1.1808 0.032 Uiso 1 1 calc R . . C37 C 0.1288(3) -0.8404(3) 1.0857(2) 0.0253(8) Uani 1 1 d . . . C38 C 0.1999(3) -0.8694(3) 1.0319(2) 0.0244(8) Uani 1 1 d . . . C39 C 0.2531(3) -0.9640(3) 1.0498(2) 0.0294(9) Uani 1 1 d . . . H39 H 0.2429 -1.0131 1.0970 0.035 Uiso 1 1 calc R . . C40 C 0.3205(3) -0.9866(3) 0.9992(2) 0.0299(9) Uani 1 1 d . . . H40 H 0.3567 -1.0509 1.0125 0.036 Uiso 1 1 calc R . . C41 C 0.3362(3) -0.9168(3) 0.9293(2) 0.0232(8) Uani 1 1 d . . . C42 C 0.2818(3) -0.8232(3) 0.9112(2) 0.0285(9) Uani 1 1 d . . . H42 H 0.2911 -0.7747 0.8635 0.034 Uiso 1 1 calc R . . C43 C 0.2148(3) -0.7998(3) 0.9613(2) 0.0284(9) Uani 1 1 d . . . H43 H 0.1784 -0.7356 0.9476 0.034 Uiso 1 1 calc R . . C44 C 0.4074(3) -0.9389(3) 0.87268(19) 0.0215(8) Uani 1 1 d . . . C45 C 0.4671(3) -1.0295(3) 0.8913(2) 0.0313(9) Uani 1 1 d . . . H45 H 0.4596 -1.0760 0.9403 0.038 Uiso 1 1 calc R . . C46 C 0.5370(3) -1.0573(3) 0.8436(2) 0.0230(8) Uani 1 1 d . . . C47 C 0.5958(3) -1.1581(3) 0.8733(2) 0.0307(9) Uani 1 1 d . . . H47A H 0.5973 -1.1790 0.9300 0.037 Uiso 1 1 calc R . . H47B H 0.6628 -1.1528 0.8552 0.037 Uiso 1 1 calc R . . C48 C 0.5551(4) -1.2365(4) 0.8469(3) 0.0554(14) Uani 1 1 d . . . H48A H 0.5950 -1.3009 0.8672 0.083 Uiso 1 1 calc R . . H48B H 0.5547 -1.2166 0.7908 0.083 Uiso 1 1 calc R . . H48C H 0.4892 -1.2428 0.8655 0.083 Uiso 1 1 calc R . . N1 N 0.3623(2) -0.9734(2) 0.69089(16) 0.0228(7) Uani 1 1 d . . . N2 N 0.0254(2) -1.2184(2) 0.55793(17) 0.0234(7) Uani 1 1 d . . . C49 C 0.3821(3) -1.0701(3) 0.6947(2) 0.0249(8) Uani 1 1 d . . . H49 H 0.4436 -1.1035 0.7135 0.030 Uiso 1 1 calc R . . C50 C 0.3183(3) -1.1236(3) 0.6730(2) 0.0234(8) Uani 1 1 d . . . H50 H 0.3352 -1.1923 0.6776 0.028 Uiso 1 1 calc R . . C51 C 0.2286(3) -1.0752(3) 0.64411(19) 0.0208(8) Uani 1 1 d . . . C52 C 0.2067(3) -0.9758(3) 0.64152(19) 0.0232(8) Uani 1 1 d . . . H52 H 0.1456 -0.9406 0.6232 0.028 Uiso 1 1 calc R . . C53 C 0.2744(3) -0.9288(3) 0.6658(2) 0.0253(8) Uani 1 1 d . . . H53 H 0.2579 -0.8612 0.6647 0.030 Uiso 1 1 calc R . . C54 C 0.1597(3) -1.1265(3) 0.6146(2) 0.0210(8) Uani 1 1 d . . . C55 C 0.1367(3) -1.2213(3) 0.6562(2) 0.0233(8) Uani 1 1 d . . . H55 H 0.1670 -1.2563 0.7042 0.028 Uiso 1 1 calc R . . C56 C 0.0691(3) -1.2634(3) 0.6262(2) 0.0272(8) Uani 1 1 d . . . H56 H 0.0527 -1.3272 0.6553 0.033 Uiso 1 1 calc R . . C57 C 0.0496(3) -1.1286(3) 0.5179(2) 0.0245(8) Uani 1 1 d . . . H57 H 0.0206 -1.0967 0.4689 0.029 Uiso 1 1 calc R . . C58 C 0.1140(3) -1.0801(3) 0.54371(19) 0.0225(8) Uani 1 1 d . . . H58 H 0.1276 -1.0155 0.5137 0.027 Uiso 1 1 calc R . . N3 N 0.4234(3) -0.3625(3) 0.6645(2) 0.0521(11) Uani 1 1 d . . . N4 N 0.7618(3) -0.7983(3) 0.8035(3) 0.0598(12) Uani 1 1 d . . . C59 C 0.5034(5) -0.3633(4) 0.7003(3) 0.0734(19) Uani 1 1 d . . . H59 H 0.5139 -0.3031 0.7102 0.088 Uiso 1 1 calc R . . C60 C 0.5737(5) -0.4433(4) 0.7250(4) 0.082(2) Uani 1 1 d . . . H60 H 0.6311 -0.4360 0.7482 0.098 Uiso 1 1 calc R . . C61 C 0.5607(3) -0.5323(3) 0.7160(2) 0.0387(10) Uani 1 1 d . . . C62 C 0.4762(4) -0.5350(4) 0.6813(3) 0.0521(13) Uani 1 1 d . . . H62 H 0.4618 -0.5959 0.6748 0.062 Uiso 1 1 calc R . . C63 C 0.4114(4) -0.4490(4) 0.6556(3) 0.0563(14) Uani 1 1 d . . . H63 H 0.3547 -0.4531 0.6298 0.068 Uiso 1 1 calc R . . C64 C 0.6323(3) -0.6236(3) 0.7439(3) 0.0416(11) Uani 1 1 d . . . C65 C 0.7147(4) -0.6256(4) 0.7846(3) 0.0573(14) Uani 1 1 d . . . H65 H 0.7297 -0.5658 0.7927 0.069 Uiso 1 1 calc R . . C66 C 0.7745(4) -0.7117(4) 0.8132(3) 0.0554(14) Uani 1 1 d . . . H66 H 0.8291 -0.7095 0.8420 0.067 Uiso 1 1 calc R . . C67 C 0.6854(4) -0.7966(4) 0.7630(4) 0.080(2) Uani 1 1 d . . . H67 H 0.6730 -0.8576 0.7553 0.096 Uiso 1 1 calc R . . C68 C 0.6218(5) -0.7124(4) 0.7306(4) 0.075(2) Uani 1 1 d . . . H68 H 0.5704 -0.7158 0.6990 0.091 Uiso 1 1 calc R . . O1T O -0.1497(2) -0.7963(2) 1.07387(17) 0.0430(8) Uani 1 1 d . . . C1T C -0.1225(4) -0.8567(4) 1.0252(3) 0.0518(13) Uani 1 1 d . . . H1T1 H -0.0684 -0.8314 0.9921 0.062 Uiso 1 1 calc R . . H1T2 H -0.1773 -0.8572 0.9923 0.062 Uiso 1 1 calc R . . C2T C -0.0924(4) -0.9612(4) 1.0794(3) 0.0609(15) Uani 1 1 d . . . H2T1 H -0.1111 -1.0130 1.0582 0.073 Uiso 1 1 calc R . . H2T2 H -0.0220 -0.9724 1.0885 0.073 Uiso 1 1 calc R . . C3T C -0.1459(4) -0.9630(4) 1.1523(3) 0.0650(16) Uani 1 1 d . . . H3T1 H -0.1006 -0.9776 1.1960 0.078 Uiso 1 1 calc R . . H3T2 H -0.1913 -1.0141 1.1643 0.078 Uiso 1 1 calc R . . C4T C -0.1995(4) -0.8591(4) 1.1359(3) 0.0579(15) Uani 1 1 d . . . H4T1 H -0.2671 -0.8586 1.1211 0.070 Uiso 1 1 calc R . . H4T2 H -0.1990 -0.8358 1.1816 0.070 Uiso 1 1 calc R . . O2T O 0.5955(6) -0.7327(6) 0.9739(5) 0.118(2) Uani 0.75 1 d PD . . C5T C 0.5069(10) -0.6869(11) 0.9266(6) 0.170(9) Uani 0.75 1 d PD . . H5T1 H 0.5153 -0.6902 0.8736 0.204 Uiso 0.75 1 calc PR . . H5T2 H 0.4505 -0.7210 0.9493 0.204 Uiso 0.75 1 calc PR . . C6T C 0.4955(7) -0.5826(12) 0.9280(7) 0.154(7) Uani 0.75 1 d PD . . H6T1 H 0.4632 -0.5381 0.8804 0.185 Uiso 0.75 1 calc PR . . H6T2 H 0.4557 -0.5764 0.9722 0.185 Uiso 0.75 1 calc PR . . C7T C 0.5884(7) -0.5549(7) 0.9345(6) 0.095(3) Uani 0.75 1 d PD . . H7T1 H 0.5854 -0.5002 0.9580 0.115 Uiso 0.75 1 calc PR . . H7T2 H 0.6196 -0.5340 0.8839 0.115 Uiso 0.75 1 calc PR . . C8T C 0.6392(7) -0.6488(7) 0.9850(5) 0.091(3) Uani 0.75 1 d PD . . H8T1 H 0.7083 -0.6541 0.9721 0.109 Uiso 0.75 1 calc PR . . H8T2 H 0.6333 -0.6497 1.0392 0.109 Uiso 0.75 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0194(2) 0.0220(2) 0.0197(2) -0.00439(18) 0.00291(17) 0.00460(18) Cu2 0.0197(2) 0.0205(2) 0.0193(2) -0.00363(18) 0.00073(17) 0.00449(18) Cu3 0.0282(3) 0.0278(3) 0.0169(2) -0.00270(19) 0.00379(18) 0.0079(2) O1 0.0229(14) 0.0247(14) 0.0261(14) -0.0054(11) 0.0058(11) 0.0056(11) O2 0.0233(14) 0.0220(13) 0.0222(13) -0.0028(11) 0.0041(10) 0.0050(11) O3 0.0231(13) 0.0202(13) 0.0206(12) -0.0034(10) 0.0015(10) 0.0033(10) O4 0.0257(14) 0.0252(14) 0.0224(13) -0.0056(11) 0.0011(11) 0.0071(11) O5 0.0234(14) 0.0276(14) 0.0224(13) -0.0022(11) 0.0037(11) 0.0077(11) O6 0.0215(13) 0.0215(13) 0.0209(12) -0.0028(10) 0.0020(10) 0.0054(11) O7 0.0309(15) 0.0296(15) 0.0195(13) -0.0029(11) 0.0047(11) 0.0088(12) O8 0.0379(17) 0.0330(16) 0.0205(13) -0.0047(12) 0.0058(12) 0.0102(13) O9 0.0321(15) 0.0333(15) 0.0184(13) -0.0027(12) 0.0038(11) 0.0096(13) O10 0.0313(15) 0.0340(15) 0.0188(13) -0.0043(12) 0.0046(11) 0.0106(12) O11 0.0280(14) 0.0233(13) 0.0217(13) -0.0061(11) 0.0050(11) 0.0046(11) O12 0.0209(14) 0.0274(14) 0.0228(13) -0.0072(11) 0.0025(10) 0.0050(11) C1 0.030(2) 0.038(3) 0.055(3) -0.013(2) 0.015(2) -0.004(2) C2 0.025(2) 0.028(2) 0.028(2) -0.0067(17) 0.0062(16) 0.0061(17) C3 0.023(2) 0.0203(19) 0.0259(19) -0.0116(16) 0.0016(15) 0.0004(15) C4 0.024(2) 0.025(2) 0.0230(18) -0.0028(16) 0.0043(15) 0.0038(16) C5 0.0163(18) 0.0197(18) 0.0256(19) -0.0083(15) -0.0014(14) -0.0019(14) C6 0.0204(19) 0.0181(18) 0.0250(18) -0.0092(15) 0.0035(15) -0.0021(15) C7 0.024(2) 0.036(2) 0.0229(19) -0.0020(17) 0.0083(16) 0.0099(17) C8 0.031(2) 0.032(2) 0.0212(19) 0.0011(17) 0.0049(16) 0.0068(18) C9 0.0196(19) 0.0167(17) 0.0249(18) -0.0065(15) -0.0021(15) 0.0007(14) C10 0.023(2) 0.030(2) 0.0212(18) -0.0066(16) 0.0049(15) 0.0053(16) C11 0.028(2) 0.026(2) 0.0198(18) -0.0022(15) 0.0005(15) 0.0064(16) C12 0.0190(18) 0.0212(18) 0.0225(18) -0.0088(15) 0.0001(14) 0.0022(15) C13 0.023(2) 0.029(2) 0.0218(18) -0.0039(16) 0.0039(15) 0.0060(16) C14 0.025(2) 0.027(2) 0.0201(18) -0.0065(16) 0.0004(15) -0.0024(16) C15 0.036(2) 0.030(2) 0.025(2) -0.0011(17) 0.0026(17) 0.0072(19) C16 0.067(4) 0.072(4) 0.025(2) -0.009(2) -0.009(2) -0.004(3) C17 0.027(2) 0.038(2) 0.033(2) -0.0062(19) 0.0019(17) 0.0098(18) C18 0.027(2) 0.031(2) 0.0243(19) -0.0034(17) -0.0003(16) 0.0065(17) C19 0.0163(18) 0.0181(18) 0.0299(19) -0.0068(15) -0.0004(15) 0.0012(14) C20 0.024(2) 0.031(2) 0.0216(18) -0.0065(16) 0.0033(15) 0.0044(17) C21 0.0203(19) 0.0206(18) 0.0204(17) -0.0036(15) 0.0013(14) -0.0030(15) C22 0.0194(19) 0.0213(18) 0.0194(17) -0.0040(15) 0.0007(14) 0.0019(15) C23 0.035(2) 0.026(2) 0.030(2) -0.0056(17) -0.0008(17) 0.0124(18) C24 0.044(3) 0.028(2) 0.024(2) -0.0060(17) 0.0055(18) 0.0084(19) C25 0.023(2) 0.0230(19) 0.0190(17) -0.0042(15) 0.0003(15) 0.0014(15) C26 0.032(2) 0.027(2) 0.026(2) -0.0042(17) 0.0028(17) 0.0092(17) C27 0.028(2) 0.033(2) 0.0214(19) -0.0056(17) 0.0041(16) 0.0090(17) C28 0.028(2) 0.025(2) 0.0225(19) -0.0034(16) -0.0010(16) -0.0007(17) C29 0.035(2) 0.034(2) 0.027(2) -0.0049(18) 0.0039(17) 0.0128(19) C30 0.034(2) 0.035(2) 0.025(2) -0.0126(18) 0.0047(17) 0.0042(19) C31 0.054(3) 0.048(3) 0.024(2) -0.008(2) 0.007(2) 0.023(2) C32 0.093(5) 0.059(3) 0.046(3) -0.031(3) 0.011(3) 0.014(3) C33 0.036(3) 0.050(3) 0.025(2) 0.000(2) -0.0016(18) 0.015(2) C34 0.033(2) 0.037(2) 0.0170(18) -0.0007(17) 0.0024(16) 0.0063(19) C35 0.025(2) 0.027(2) 0.0201(18) -0.0022(16) -0.0003(15) 0.0004(16) C36 0.026(2) 0.029(2) 0.0218(18) -0.0060(16) 0.0006(15) 0.0050(17) C37 0.026(2) 0.030(2) 0.0175(17) -0.0062(16) 0.0028(15) 0.0023(17) C38 0.024(2) 0.030(2) 0.0178(17) -0.0071(16) 0.0006(15) 0.0046(16) C39 0.036(2) 0.028(2) 0.0189(18) -0.0021(16) 0.0031(16) 0.0027(18) C40 0.033(2) 0.028(2) 0.0250(19) -0.0066(17) 0.0031(17) 0.0080(17) C41 0.0197(19) 0.029(2) 0.0190(17) -0.0061(15) 0.0012(14) 0.0010(16) C42 0.029(2) 0.029(2) 0.0199(18) -0.0008(16) 0.0020(16) 0.0079(17) C43 0.034(2) 0.0212(19) 0.0235(19) -0.0023(16) 0.0010(16) 0.0088(17) C44 0.0202(19) 0.0250(19) 0.0185(17) -0.0070(15) -0.0009(14) 0.0018(15) C45 0.031(2) 0.030(2) 0.0244(19) -0.0005(17) 0.0077(16) 0.0074(18) C46 0.0191(19) 0.027(2) 0.0234(18) -0.0085(16) 0.0003(15) -0.0002(15) C47 0.026(2) 0.030(2) 0.029(2) -0.0044(17) -0.0001(17) 0.0098(17) C48 0.056(3) 0.040(3) 0.066(3) -0.016(3) -0.014(3) 0.016(2) N1 0.0212(16) 0.0264(17) 0.0198(15) -0.0067(13) 0.0016(12) 0.0004(13) N2 0.0225(17) 0.0211(16) 0.0251(16) -0.0062(13) -0.0005(13) 0.0015(13) C49 0.021(2) 0.029(2) 0.0221(18) -0.0068(16) -0.0017(15) 0.0058(16) C50 0.025(2) 0.0238(19) 0.0205(18) -0.0077(15) -0.0025(15) 0.0040(16) C51 0.0228(19) 0.0214(18) 0.0160(16) -0.0039(14) 0.0035(14) 0.0007(15) C52 0.0191(19) 0.028(2) 0.0182(17) -0.0020(15) -0.0001(14) 0.0029(16) C53 0.025(2) 0.0209(19) 0.028(2) -0.0074(16) 0.0033(16) 0.0016(16) C54 0.0179(18) 0.0234(19) 0.0201(17) -0.0071(15) 0.0033(14) 0.0047(15) C55 0.023(2) 0.026(2) 0.0173(17) -0.0021(15) -0.0006(14) -0.0009(16) C56 0.026(2) 0.0214(19) 0.030(2) -0.0020(16) 0.0037(16) -0.0011(16) C57 0.024(2) 0.026(2) 0.0188(18) -0.0034(15) -0.0021(15) 0.0060(16) C58 0.027(2) 0.0171(18) 0.0184(17) 0.0007(14) 0.0010(15) 0.0023(15) N3 0.072(3) 0.028(2) 0.051(3) -0.0064(19) -0.013(2) 0.001(2) N4 0.046(3) 0.049(3) 0.076(3) -0.008(2) -0.007(2) 0.003(2) C59 0.113(5) 0.029(3) 0.078(4) -0.018(3) -0.043(4) 0.006(3) C60 0.102(5) 0.045(3) 0.103(5) -0.025(3) -0.053(4) -0.005(3) C61 0.047(3) 0.031(2) 0.035(2) -0.0051(19) -0.001(2) -0.006(2) C62 0.051(3) 0.031(3) 0.078(4) -0.024(3) -0.018(3) 0.000(2) C63 0.050(3) 0.041(3) 0.077(4) -0.018(3) -0.017(3) 0.003(2) C64 0.039(3) 0.041(3) 0.043(3) -0.008(2) 0.001(2) -0.006(2) C65 0.047(3) 0.051(3) 0.080(4) -0.026(3) -0.005(3) -0.009(3) C66 0.038(3) 0.064(4) 0.070(4) -0.032(3) -0.011(3) 0.004(3) C67 0.056(4) 0.043(3) 0.141(6) -0.029(4) -0.040(4) 0.009(3) C68 0.070(4) 0.043(3) 0.118(6) -0.031(3) -0.044(4) 0.001(3) O1T 0.0470(19) 0.0459(19) 0.0341(16) -0.0068(14) 0.0033(14) -0.0119(16) C1T 0.062(3) 0.069(4) 0.032(2) -0.020(2) 0.000(2) -0.023(3) C2T 0.058(4) 0.058(4) 0.072(4) -0.027(3) -0.017(3) -0.008(3) C3T 0.082(4) 0.055(3) 0.053(3) 0.000(3) -0.010(3) -0.027(3) C4T 0.055(3) 0.074(4) 0.046(3) -0.011(3) 0.009(2) -0.029(3) O2T 0.098(6) 0.132(6) 0.135(7) -0.051(6) 0.018(5) -0.036(5) C5T 0.176(15) 0.29(2) 0.056(6) -0.016(10) 0.031(8) -0.192(16) C6T 0.042(6) 0.31(2) 0.091(9) -0.036(12) -0.014(5) 0.008(10) C7T 0.090(8) 0.087(7) 0.123(9) -0.060(7) 0.017(6) 0.005(6) C8T 0.078(7) 0.117(9) 0.083(7) -0.035(6) 0.002(5) -0.021(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.941(2) . ? Cu1 O11 1.943(2) . ? Cu1 O2 1.943(2) . ? Cu1 O12 1.947(2) . ? Cu1 N1 2.264(3) . ? Cu2 O5 1.927(2) . ? Cu2 O3 1.928(2) . ? Cu2 O4 1.936(2) . ? Cu2 O6 1.945(2) . ? Cu2 N2 2.314(3) 1_565 ? Cu3 O10 1.919(3) . ? Cu3 O7 1.922(3) . ? Cu3 O8 1.923(3) . ? Cu3 O9 1.924(2) . ? Cu3 O1T 2.415(3) . ? O1 C3 1.268(4) . ? O2 C5 1.273(4) . ? O3 C12 1.269(4) . ? O4 C14 1.275(4) . ? O5 C19 1.267(4) . ? O6 C21 1.260(4) . ? O7 C28 1.276(4) . ? O8 C30 1.281(5) . ? O9 C35 1.276(4) . ? O10 C37 1.275(4) . ? O11 C44 1.270(4) . ? O12 C46 1.269(4) . ? C1 C2 1.516(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.512(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.408(5) . ? C4 C5 1.395(5) . ? C4 H4 0.9500 . ? C5 C6 1.506(5) . ? C6 C11 1.388(5) . ? C6 C7 1.396(5) . ? C7 C8 1.383(5) . ? C7 H7 0.9500 . ? C8 C9 1.392(5) . ? C8 H8 0.9500 . ? C9 C10 1.389(5) . ? C9 C12 1.495(5) . ? C10 C11 1.390(5) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.407(5) . ? C13 C14 1.389(5) . ? C13 H13 0.9500 . ? C14 C15 1.509(5) . ? C15 C16 1.528(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.517(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.522(5) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.392(5) . ? C20 C21 1.404(5) . ? C20 H20 0.9500 . ? C21 C22 1.501(5) . ? C22 C23 1.385(5) . ? C22 C27 1.398(5) . ? C23 C24 1.383(5) . ? C23 H23 0.9500 . ? C24 C25 1.400(5) . ? C24 H24 0.9500 . ? C25 C26 1.390(5) . ? C25 C28 1.489(5) . ? C26 C27 1.377(5) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C29 1.401(5) . ? C29 C30 1.389(5) . ? C29 H29 0.9500 . ? C30 C31 1.514(5) . ? C31 C32 1.509(7) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.515(5) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.513(5) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.404(5) . ? C36 C37 1.400(5) . ? C36 H36 0.9500 . ? C37 C38 1.493(5) . ? C38 C43 1.395(5) . ? C38 C39 1.398(5) . ? C39 C40 1.383(5) . ? C39 H39 0.9500 . ? C40 C41 1.389(5) . ? C40 H40 0.9500 . ? C41 C42 1.395(5) . ? C41 C44 1.495(5) . ? C42 C43 1.377(5) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 C45 1.395(5) . ? C45 C46 1.394(5) . ? C45 H45 0.9500 . ? C46 C47 1.508(5) . ? C47 C48 1.510(6) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? N1 C53 1.338(5) . ? N1 C49 1.342(5) . ? N2 C57 1.337(5) . ? N2 C56 1.343(5) . ? N2 Cu2 2.314(3) 1_545 ? C49 C50 1.375(5) . ? C49 H49 0.9500 . ? C50 C51 1.390(5) . ? C50 H50 0.9500 . ? C51 C52 1.388(5) . ? C51 C54 1.479(5) . ? C52 C53 1.375(5) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C54 C55 1.395(5) . ? C54 C58 1.397(5) . ? C55 C56 1.384(5) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 C58 1.370(5) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? N3 C59 1.310(7) . ? N3 C63 1.313(6) . ? N4 C67 1.311(7) . ? N4 C66 1.323(6) . ? C59 C60 1.377(8) . ? C59 H59 0.9500 . ? C60 C61 1.350(7) . ? C60 H60 0.9500 . ? C61 C62 1.369(6) . ? C61 C64 1.498(6) . ? C62 C63 1.389(7) . ? C62 H62 0.9500 . ? C63 H63 0.9500 . ? C64 C68 1.375(7) . ? C64 C65 1.382(7) . ? C65 C66 1.358(7) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C67 C68 1.380(7) . ? C67 H67 0.9500 . ? C68 H68 0.9500 . ? O1T C1T 1.427(6) . ? O1T C4T 1.434(5) . ? C1T C2T 1.524(7) . ? C1T H1T1 0.9900 . ? C1T H1T2 0.9900 . ? C2T C3T 1.511(8) . ? C2T H2T1 0.9900 . ? C2T H2T2 0.9900 . ? C3T C4T 1.512(8) . ? C3T H3T1 0.9900 . ? C3T H3T2 0.9900 . ? C4T H4T1 0.9900 . ? C4T H4T2 0.9900 . ? O2T C8T 1.467(10) . ? O2T C5T 1.494(13) . ? C5T C6T 1.472(14) . ? C5T H5T1 0.9900 . ? C5T H5T2 0.9900 . ? C6T C7T 1.420(11) . ? C6T H6T1 0.9900 . ? C6T H6T2 0.9900 . ? C7T C8T 1.477(10) . ? C7T H7T1 0.9900 . ? C7T H7T2 0.9900 . ? C8T H8T1 0.9900 . ? C8T H8T2 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 O11 160.88(11) . . ? O1 Cu1 O2 92.10(10) . . ? O11 Cu1 O2 86.99(10) . . ? O1 Cu1 O12 86.72(10) . . ? O11 Cu1 O12 92.86(10) . . ? O2 Cu1 O12 175.94(11) . . ? O1 Cu1 N1 105.32(11) . . ? O11 Cu1 N1 93.79(11) . . ? O2 Cu1 N1 91.08(11) . . ? O12 Cu1 N1 92.97(11) . . ? O5 Cu2 O3 172.38(11) . . ? O5 Cu2 O4 86.14(10) . . ? O3 Cu2 O4 93.29(10) . . ? O5 Cu2 O6 92.06(10) . . ? O3 Cu2 O6 87.99(10) . . ? O4 Cu2 O6 175.78(11) . . ? O5 Cu2 N2 100.90(11) . 1_565 ? O3 Cu2 N2 86.71(10) . 1_565 ? O4 Cu2 N2 96.09(11) . 1_565 ? O6 Cu2 N2 88.00(11) . 1_565 ? O10 Cu3 O7 85.16(11) . . ? O10 Cu3 O8 174.62(12) . . ? O7 Cu3 O8 93.70(11) . . ? O10 Cu3 O9 93.04(11) . . ? O7 Cu3 O9 175.01(12) . . ? O8 Cu3 O9 87.66(11) . . ? O10 Cu3 O1T 92.27(12) . . ? O7 Cu3 O1T 88.51(11) . . ? O8 Cu3 O1T 92.95(12) . . ? O9 Cu3 O1T 96.22(11) . . ? C3 O1 Cu1 125.8(2) . . ? C5 O2 Cu1 125.5(2) . . ? C12 O3 Cu2 126.2(2) . . ? C14 O4 Cu2 124.7(2) . . ? C19 O5 Cu2 126.6(2) . . ? C21 O6 Cu2 124.7(2) . . ? C28 O7 Cu3 126.3(2) . . ? C30 O8 Cu3 124.8(2) . . ? C35 O9 Cu3 126.4(2) . . ? C37 O10 Cu3 126.4(2) . . ? C44 O11 Cu1 124.6(2) . . ? C46 O12 Cu1 124.1(2) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C1 110.4(3) . . ? C3 C2 H2A 109.6 . . ? C1 C2 H2A 109.6 . . ? C3 C2 H2B 109.6 . . ? C1 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? O1 C3 C4 125.1(3) . . ? O1 C3 C2 116.7(3) . . ? C4 C3 C2 118.1(3) . . ? C5 C4 C3 124.4(3) . . ? C5 C4 H4 117.8 . . ? C3 C4 H4 117.8 . . ? O2 C5 C4 124.4(3) . . ? O2 C5 C6 115.1(3) . . ? C4 C5 C6 120.5(3) . . ? C11 C6 C7 117.7(3) . . ? C11 C6 C5 118.5(3) . . ? C7 C6 C5 123.8(3) . . ? C8 C7 C6 121.2(3) . . ? C8 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? C7 C8 C9 121.1(3) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C10 C9 C8 117.8(3) . . ? C10 C9 C12 118.5(3) . . ? C8 C9 C12 123.7(3) . . ? C9 C10 C11 121.2(3) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C6 C11 C10 121.1(3) . . ? C6 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? O3 C12 C13 123.7(3) . . ? O3 C12 C9 115.1(3) . . ? C13 C12 C9 121.2(3) . . ? C14 C13 C12 125.2(3) . . ? C14 C13 H13 117.4 . . ? C12 C13 H13 117.4 . . ? O4 C14 C13 125.8(3) . . ? O4 C14 C15 114.7(3) . . ? C13 C14 C15 119.5(3) . . ? C14 C15 C16 111.0(3) . . ? C14 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? C14 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C18 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C17 C18 C19 117.9(3) . . ? C17 C18 H18A 107.8 . . ? C19 C18 H18A 107.8 . . ? C17 C18 H18B 107.8 . . ? C19 C18 H18B 107.8 . . ? H18A C18 H18B 107.2 . . ? O5 C19 C20 124.7(3) . . ? O5 C19 C18 114.0(3) . . ? C20 C19 C18 121.3(3) . . ? C19 C20 C21 124.2(3) . . ? C19 C20 H20 117.9 . . ? C21 C20 H20 117.9 . . ? O6 C21 C20 125.2(3) . . ? O6 C21 C22 115.4(3) . . ? C20 C21 C22 119.4(3) . . ? C23 C22 C27 117.3(3) . . ? C23 C22 C21 123.3(3) . . ? C27 C22 C21 119.5(3) . . ? C24 C23 C22 121.7(3) . . ? C24 C23 H23 119.1 . . ? C22 C23 H23 119.1 . . ? C23 C24 C25 120.6(4) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C26 C25 C24 117.9(3) . . ? C26 C25 C28 119.2(3) . . ? C24 C25 C28 122.9(3) . . ? C27 C26 C25 120.9(3) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C26 C27 C22 121.6(3) . . ? C26 C27 H27 119.2 . . ? C22 C27 H27 119.2 . . ? O7 C28 C29 123.9(3) . . ? O7 C28 C25 115.0(3) . . ? C29 C28 C25 121.0(3) . . ? C30 C29 C28 125.0(4) . . ? C30 C29 H29 117.5 . . ? C28 C29 H29 117.5 . . ? O8 C30 C29 125.9(4) . . ? O8 C30 C31 115.1(3) . . ? C29 C30 C31 119.0(4) . . ? C32 C31 C30 110.6(4) . . ? C32 C31 H31A 109.5 . . ? C30 C31 H31A 109.5 . . ? C32 C31 H31B 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 108.1 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 H33A 109.5 . . ? C34 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C34 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 C33 117.7(3) . . ? C35 C34 H34A 107.9 . . ? C33 C34 H34A 107.9 . . ? C35 C34 H34B 107.9 . . ? C33 C34 H34B 107.9 . . ? H34A C34 H34B 107.2 . . ? O9 C35 C36 125.0(3) . . ? O9 C35 C34 114.8(3) . . ? C36 C35 C34 120.2(3) . . ? C37 C36 C35 123.9(3) . . ? C37 C36 H36 118.1 . . ? C35 C36 H36 118.1 . . ? O10 C37 C36 125.3(3) . . ? O10 C37 C38 114.6(3) . . ? C36 C37 C38 120.1(3) . . ? C43 C38 C39 118.4(3) . . ? C43 C38 C37 119.1(3) . . ? C39 C38 C37 122.5(3) . . ? C40 C39 C38 120.5(3) . . ? C40 C39 H39 119.8 . . ? C38 C39 H39 119.8 . . ? C39 C40 C41 121.1(4) . . ? C39 C40 H40 119.5 . . ? C41 C40 H40 119.5 . . ? C40 C41 C42 118.2(3) . . ? C40 C41 C44 122.7(3) . . ? C42 C41 C44 119.2(3) . . ? C43 C42 C41 121.2(3) . . ? C43 C42 H42 119.4 . . ? C41 C42 H42 119.4 . . ? C42 C43 C38 120.6(3) . . ? C42 C43 H43 119.7 . . ? C38 C43 H43 119.7 . . ? O11 C44 C45 124.7(3) . . ? O11 C44 C41 114.9(3) . . ? C45 C44 C41 120.3(3) . . ? C46 C45 C44 125.2(4) . . ? C46 C45 H45 117.4 . . ? C44 C45 H45 117.4 . . ? O12 C46 C45 125.5(3) . . ? O12 C46 C47 116.3(3) . . ? C45 C46 C47 118.2(3) . . ? C46 C47 C48 111.7(3) . . ? C46 C47 H47A 109.3 . . ? C48 C47 H47A 109.3 . . ? C46 C47 H47B 109.3 . . ? C48 C47 H47B 109.3 . . ? H47A C47 H47B 107.9 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C53 N1 C49 116.9(3) . . ? C53 N1 Cu1 120.7(2) . . ? C49 N1 Cu1 122.3(2) . . ? C57 N2 C56 117.3(3) . . ? C57 N2 Cu2 124.5(2) . 1_545 ? C56 N2 Cu2 118.2(2) . 1_545 ? N1 C49 C50 123.7(3) . . ? N1 C49 H49 118.2 . . ? C50 C49 H49 118.2 . . ? C49 C50 C51 118.8(3) . . ? C49 C50 H50 120.6 . . ? C51 C50 H50 120.6 . . ? C52 C51 C50 117.9(3) . . ? C52 C51 C54 120.8(3) . . ? C50 C51 C54 121.3(3) . . ? C53 C52 C51 119.3(3) . . ? C53 C52 H52 120.4 . . ? C51 C52 H52 120.4 . . ? N1 C53 C52 123.4(3) . . ? N1 C53 H53 118.3 . . ? C52 C53 H53 118.3 . . ? C55 C54 C58 117.7(3) . . ? C55 C54 C51 122.0(3) . . ? C58 C54 C51 120.4(3) . . ? C56 C55 C54 118.8(3) . . ? C56 C55 H55 120.6 . . ? C54 C55 H55 120.6 . . ? N2 C56 C55 123.3(3) . . ? N2 C56 H56 118.3 . . ? C55 C56 H56 118.3 . . ? N2 C57 C58 123.5(3) . . ? N2 C57 H57 118.2 . . ? C58 C57 H57 118.2 . . ? C57 C58 C54 119.4(3) . . ? C57 C58 H58 120.3 . . ? C54 C58 H58 120.3 . . ? C59 N3 C63 114.0(5) . . ? C67 N4 C66 115.0(5) . . ? N3 C59 C60 126.0(5) . . ? N3 C59 H59 117.0 . . ? C60 C59 H59 117.0 . . ? C61 C60 C59 119.7(5) . . ? C61 C60 H60 120.2 . . ? C59 C60 H60 120.2 . . ? C60 C61 C62 115.7(5) . . ? C60 C61 C64 122.7(5) . . ? C62 C61 C64 121.5(4) . . ? C61 C62 C63 120.3(4) . . ? C61 C62 H62 119.9 . . ? C63 C62 H62 119.9 . . ? N3 C63 C62 124.2(5) . . ? N3 C63 H63 117.9 . . ? C62 C63 H63 117.9 . . ? C68 C64 C65 114.3(5) . . ? C68 C64 C61 122.6(4) . . ? C65 C64 C61 123.1(4) . . ? C66 C65 C64 121.1(5) . . ? C66 C65 H65 119.4 . . ? C64 C65 H65 119.4 . . ? N4 C66 C65 124.4(5) . . ? N4 C66 H66 117.8 . . ? C65 C66 H66 117.8 . . ? N4 C67 C68 124.5(5) . . ? N4 C67 H67 117.7 . . ? C68 C67 H67 117.7 . . ? C64 C68 C67 120.3(5) . . ? C64 C68 H68 119.8 . . ? C67 C68 H68 119.8 . . ? C1T O1T C4T 104.7(4) . . ? C1T O1T Cu3 118.6(3) . . ? C4T O1T Cu3 117.7(3) . . ? O1T C1T C2T 105.1(4) . . ? O1T C1T H1T1 110.7 . . ? C2T C1T H1T1 110.7 . . ? O1T C1T H1T2 110.7 . . ? C2T C1T H1T2 110.7 . . ? H1T1 C1T H1T2 108.8 . . ? C3T C2T C1T 104.2(5) . . ? C3T C2T H2T1 110.9 . . ? C1T C2T H2T1 110.9 . . ? C3T C2T H2T2 110.9 . . ? C1T C2T H2T2 110.9 . . ? H2T1 C2T H2T2 108.9 . . ? C2T C3T C4T 104.5(4) . . ? C2T C3T H3T1 110.9 . . ? C4T C3T H3T1 110.9 . . ? C2T C3T H3T2 110.9 . . ? C4T C3T H3T2 110.9 . . ? H3T1 C3T H3T2 108.9 . . ? O1T C4T C3T 105.9(4) . . ? O1T C4T H4T1 110.6 . . ? C3T C4T H4T1 110.6 . . ? O1T C4T H4T2 110.6 . . ? C3T C4T H4T2 110.6 . . ? H4T1 C4T H4T2 108.7 . . ? C8T O2T C5T 105.7(8) . . ? C6T C5T O2T 103.5(8) . . ? C6T C5T H5T1 111.1 . . ? O2T C5T H5T1 111.1 . . ? C6T C5T H5T2 111.1 . . ? O2T C5T H5T2 111.1 . . ? H5T1 C5T H5T2 109.0 . . ? C7T C6T C5T 108.2(9) . . ? C7T C6T H6T1 110.1 . . ? C5T C6T H6T1 110.1 . . ? C7T C6T H6T2 110.1 . . ? C5T C6T H6T2 110.1 . . ? H6T1 C6T H6T2 108.4 . . ? C6T C7T C8T 102.0(8) . . ? C6T C7T H7T1 111.4 . . ? C8T C7T H7T1 111.4 . . ? C6T C7T H7T2 111.4 . . ? C8T C7T H7T2 111.4 . . ? H7T1 C7T H7T2 109.2 . . ? O2T C8T C7T 108.1(7) . . ? O2T C8T H8T1 110.1 . . ? C7T C8T H8T1 110.1 . . ? O2T C8T H8T2 110.1 . . ? C7T C8T H8T2 110.1 . . ? H8T1 C8T H8T2 108.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O11 Cu1 O1 C3 -97.4(4) . . . . ? O2 Cu1 O1 C3 -10.6(3) . . . . ? O12 Cu1 O1 C3 173.3(3) . . . . ? N1 Cu1 O1 C3 81.1(3) . . . . ? O1 Cu1 O2 C5 18.1(3) . . . . ? O11 Cu1 O2 C5 178.9(3) . . . . ? N1 Cu1 O2 C5 -87.3(3) . . . . ? O4 Cu2 O3 C12 11.9(3) . . . . ? O6 Cu2 O3 C12 -172.1(3) . . . . ? N2 Cu2 O3 C12 -84.0(3) 1_565 . . . ? O5 Cu2 O4 C14 179.9(3) . . . . ? O3 Cu2 O4 C14 -7.7(3) . . . . ? N2 Cu2 O4 C14 79.3(3) 1_565 . . . ? O4 Cu2 O5 C19 -172.4(3) . . . . ? O6 Cu2 O5 C19 11.5(3) . . . . ? N2 Cu2 O5 C19 -76.9(3) 1_565 . . . ? O5 Cu2 O6 C21 -17.5(3) . . . . ? O3 Cu2 O6 C21 170.2(3) . . . . ? N2 Cu2 O6 C21 83.4(3) 1_565 . . . ? O10 Cu3 O7 C28 177.8(3) . . . . ? O8 Cu3 O7 C28 -7.5(3) . . . . ? O1T Cu3 O7 C28 85.4(3) . . . . ? O7 Cu3 O8 C30 4.9(3) . . . . ? O9 Cu3 O8 C30 -179.9(3) . . . . ? O1T Cu3 O8 C30 -83.8(3) . . . . ? O10 Cu3 O9 C35 1.1(3) . . . . ? O8 Cu3 O9 C35 -173.6(3) . . . . ? O1T Cu3 O9 C35 93.7(3) . . . . ? O7 Cu3 O10 C37 176.3(3) . . . . ? O9 Cu3 O10 C37 0.9(3) . . . . ? O1T Cu3 O10 C37 -95.4(3) . . . . ? O1 Cu1 O11 C44 -106.2(4) . . . . ? O2 Cu1 O11 C44 166.1(3) . . . . ? O12 Cu1 O11 C44 -18.0(3) . . . . ? N1 Cu1 O11 C44 75.2(3) . . . . ? O1 Cu1 O12 C46 177.6(3) . . . . ? O11 Cu1 O12 C46 16.8(3) . . . . ? N1 Cu1 O12 C46 -77.2(3) . . . . ? Cu1 O1 C3 C4 0.8(5) . . . . ? Cu1 O1 C3 C2 177.1(2) . . . . ? C1 C2 C3 O1 -90.8(4) . . . . ? C1 C2 C3 C4 85.9(4) . . . . ? O1 C3 C4 C5 7.5(6) . . . . ? C2 C3 C4 C5 -168.8(3) . . . . ? Cu1 O2 C5 C4 -15.9(5) . . . . ? Cu1 O2 C5 C6 164.9(2) . . . . ? C3 C4 C5 O2 0.7(6) . . . . ? C3 C4 C5 C6 179.8(3) . . . . ? O2 C5 C6 C11 -4.8(5) . . . . ? C4 C5 C6 C11 176.0(3) . . . . ? O2 C5 C6 C7 176.7(3) . . . . ? C4 C5 C6 C7 -2.5(6) . . . . ? C11 C6 C7 C8 -0.4(6) . . . . ? C5 C6 C7 C8 178.1(4) . . . . ? C6 C7 C8 C9 1.4(6) . . . . ? C7 C8 C9 C10 -1.5(6) . . . . ? C7 C8 C9 C12 177.1(4) . . . . ? C8 C9 C10 C11 0.7(6) . . . . ? C12 C9 C10 C11 -178.0(3) . . . . ? C7 C6 C11 C10 -0.4(6) . . . . ? C5 C6 C11 C10 -179.0(3) . . . . ? C9 C10 C11 C6 0.2(6) . . . . ? Cu2 O3 C12 C13 -11.0(5) . . . . ? Cu2 O3 C12 C9 168.1(2) . . . . ? C10 C9 C12 O3 -1.9(5) . . . . ? C8 C9 C12 O3 179.4(3) . . . . ? C10 C9 C12 C13 177.3(3) . . . . ? C8 C9 C12 C13 -1.4(6) . . . . ? O3 C12 C13 C14 2.4(6) . . . . ? C9 C12 C13 C14 -176.6(4) . . . . ? Cu2 O4 C14 C13 2.7(5) . . . . ? Cu2 O4 C14 C15 -178.8(2) . . . . ? C12 C13 C14 O4 2.0(6) . . . . ? C12 C13 C14 C15 -176.4(4) . . . . ? O4 C14 C15 C16 -85.8(4) . . . . ? C13 C14 C15 C16 92.8(5) . . . . ? Cu2 O5 C19 C20 -3.8(5) . . . . ? Cu2 O5 C19 C18 175.9(2) . . . . ? C17 C18 C19 O5 169.3(3) . . . . ? C17 C18 C19 C20 -11.0(6) . . . . ? O5 C19 C20 C21 -3.4(6) . . . . ? C18 C19 C20 C21 177.0(4) . . . . ? Cu2 O6 C21 C20 16.4(5) . . . . ? Cu2 O6 C21 C22 -162.9(2) . . . . ? C19 C20 C21 O6 -3.6(6) . . . . ? C19 C20 C21 C22 175.7(3) . . . . ? O6 C21 C22 C23 168.6(4) . . . . ? C20 C21 C22 C23 -10.7(6) . . . . ? O6 C21 C22 C27 -9.9(5) . . . . ? C20 C21 C22 C27 170.8(4) . . . . ? C27 C22 C23 C24 -1.8(6) . . . . ? C21 C22 C23 C24 179.7(4) . . . . ? C22 C23 C24 C25 -0.1(7) . . . . ? C23 C24 C25 C26 2.4(6) . . . . ? C23 C24 C25 C28 -177.2(4) . . . . ? C24 C25 C26 C27 -2.9(6) . . . . ? C28 C25 C26 C27 176.7(4) . . . . ? C25 C26 C27 C22 1.0(6) . . . . ? C23 C22 C27 C26 1.4(6) . . . . ? C21 C22 C27 C26 179.9(4) . . . . ? Cu3 O7 C28 C29 7.0(6) . . . . ? Cu3 O7 C28 C25 -171.5(2) . . . . ? C26 C25 C28 O7 10.4(5) . . . . ? C24 C25 C28 O7 -170.1(4) . . . . ? C26 C25 C28 C29 -168.2(4) . . . . ? C24 C25 C28 C29 11.4(6) . . . . ? O7 C28 C29 C30 -1.8(7) . . . . ? C25 C28 C29 C30 176.6(4) . . . . ? Cu3 O8 C30 C29 -1.9(6) . . . . ? Cu3 O8 C30 C31 -179.7(3) . . . . ? C28 C29 C30 O8 -0.9(7) . . . . ? C28 C29 C30 C31 176.8(4) . . . . ? O8 C30 C31 C32 73.3(5) . . . . ? C29 C30 C31 C32 -104.6(5) . . . . ? Cu3 O9 C35 C36 -2.6(6) . . . . ? Cu3 O9 C35 C34 177.2(3) . . . . ? C33 C34 C35 O9 -177.3(4) . . . . ? C33 C34 C35 C36 2.5(6) . . . . ? O9 C35 C36 C37 2.2(7) . . . . ? C34 C35 C36 C37 -177.6(4) . . . . ? Cu3 O10 C37 C36 -1.5(6) . . . . ? Cu3 O10 C37 C38 -179.0(2) . . . . ? C35 C36 C37 O10 0.0(7) . . . . ? C35 C36 C37 C38 177.3(4) . . . . ? O10 C37 C38 C43 18.3(5) . . . . ? C36 C37 C38 C43 -159.3(4) . . . . ? O10 C37 C38 C39 -162.2(4) . . . . ? C36 C37 C38 C39 20.2(6) . . . . ? C43 C38 C39 C40 1.7(6) . . . . ? C37 C38 C39 C40 -177.9(4) . . . . ? C38 C39 C40 C41 -0.9(6) . . . . ? C39 C40 C41 C42 -0.2(6) . . . . ? C39 C40 C41 C44 -179.1(4) . . . . ? C40 C41 C42 C43 0.5(6) . . . . ? C44 C41 C42 C43 179.4(4) . . . . ? C41 C42 C43 C38 0.3(6) . . . . ? C39 C38 C43 C42 -1.4(6) . . . . ? C37 C38 C43 C42 178.2(4) . . . . ? Cu1 O11 C44 C45 12.5(5) . . . . ? Cu1 O11 C44 C41 -167.9(2) . . . . ? C40 C41 C44 O11 175.0(3) . . . . ? C42 C41 C44 O11 -3.8(5) . . . . ? C40 C41 C44 C45 -5.3(6) . . . . ? C42 C41 C44 C45 175.8(4) . . . . ? O11 C44 C45 C46 0.8(7) . . . . ? C41 C44 C45 C46 -178.8(4) . . . . ? Cu1 O12 C46 C45 -10.2(5) . . . . ? Cu1 O12 C46 C47 168.3(2) . . . . ? C44 C45 C46 O12 -2.0(7) . . . . ? C44 C45 C46 C47 179.6(4) . . . . ? O12 C46 C47 C48 -82.5(5) . . . . ? C45 C46 C47 C48 96.1(5) . . . . ? O1 Cu1 N1 C53 -108.7(3) . . . . ? O11 Cu1 N1 C53 70.8(3) . . . . ? O2 Cu1 N1 C53 -16.3(3) . . . . ? O12 Cu1 N1 C53 163.9(3) . . . . ? O1 Cu1 N1 C49 67.4(3) . . . . ? O11 Cu1 N1 C49 -113.1(3) . . . . ? O2 Cu1 N1 C49 159.8(3) . . . . ? O12 Cu1 N1 C49 -20.0(3) . . . . ? C53 N1 C49 C50 1.4(5) . . . . ? Cu1 N1 C49 C50 -174.8(3) . . . . ? N1 C49 C50 C51 1.2(5) . . . . ? C49 C50 C51 C52 -2.5(5) . . . . ? C49 C50 C51 C54 175.5(3) . . . . ? C50 C51 C52 C53 1.3(5) . . . . ? C54 C51 C52 C53 -176.7(3) . . . . ? C49 N1 C53 C52 -2.6(5) . . . . ? Cu1 N1 C53 C52 173.7(3) . . . . ? C51 C52 C53 N1 1.3(5) . . . . ? C52 C51 C54 C55 -132.8(4) . . . . ? C50 C51 C54 C55 49.2(5) . . . . ? C52 C51 C54 C58 46.3(5) . . . . ? C50 C51 C54 C58 -131.7(4) . . . . ? C58 C54 C55 C56 -1.3(5) . . . . ? C51 C54 C55 C56 177.8(3) . . . . ? C57 N2 C56 C55 0.0(5) . . . . ? Cu2 N2 C56 C55 178.9(3) 1_545 . . . ? C54 C55 C56 N2 1.4(5) . . . . ? C56 N2 C57 C58 -1.6(5) . . . . ? Cu2 N2 C57 C58 179.5(3) 1_545 . . . ? N2 C57 C58 C54 1.7(5) . . . . ? C55 C54 C58 C57 -0.1(5) . . . . ? C51 C54 C58 C57 -179.3(3) . . . . ? C63 N3 C59 C60 2.8(10) . . . . ? N3 C59 C60 C61 -3.3(12) . . . . ? C59 C60 C61 C62 0.6(9) . . . . ? C59 C60 C61 C64 -177.7(6) . . . . ? C60 C61 C62 C63 2.0(8) . . . . ? C64 C61 C62 C63 -179.6(5) . . . . ? C59 N3 C63 C62 0.2(9) . . . . ? C61 C62 C63 N3 -2.6(9) . . . . ? C60 C61 C64 C68 -175.9(6) . . . . ? C62 C61 C64 C68 5.8(8) . . . . ? C60 C61 C64 C65 3.6(8) . . . . ? C62 C61 C64 C65 -174.7(5) . . . . ? C68 C64 C65 C66 -4.8(8) . . . . ? C61 C64 C65 C66 175.6(5) . . . . ? C67 N4 C66 C65 0.2(9) . . . . ? C64 C65 C66 N4 1.9(9) . . . . ? C66 N4 C67 C68 1.0(10) . . . . ? C65 C64 C68 C67 5.9(9) . . . . ? C61 C64 C68 C67 -174.6(6) . . . . ? N4 C67 C68 C64 -4.3(12) . . . . ? O10 Cu3 O1T C1T -5.6(3) . . . . ? O7 Cu3 O1T C1T 79.5(3) . . . . ? O8 Cu3 O1T C1T 173.1(3) . . . . ? O9 Cu3 O1T C1T -98.9(3) . . . . ? O10 Cu3 O1T C4T 122.1(3) . . . . ? O7 Cu3 O1T C4T -152.8(3) . . . . ? O8 Cu3 O1T C4T -59.2(3) . . . . ? O9 Cu3 O1T C4T 28.8(3) . . . . ? C4T O1T C1T C2T -39.2(5) . . . . ? Cu3 O1T C1T C2T 94.4(4) . . . . ? O1T C1T C2T C3T 24.9(5) . . . . ? C1T C2T C3T C4T -2.0(5) . . . . ? C1T O1T C4T C3T 38.1(5) . . . . ? Cu3 O1T C4T C3T -96.0(4) . . . . ? C2T C3T C4T O1T -21.5(5) . . . . ? C8T O2T C5T C6T -11.6(12) . . . . ? O2T C5T C6T C7T 30.5(13) . . . . ? C5T C6T C7T C8T -36.1(12) . . . . ? C5T O2T C8T C7T -9.9(11) . . . . ? C6T C7T C8T O2T 28.0(11) . . . . ? _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.944 _refine_diff_density_min -0.397 _refine_diff_density_rms 0.096 # Attachment '(4)Cu3L3pyrnew.CIF' data_lj43twin _database_code_depnum_ccdc_archive 'CCDC 292067' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H52 Cu3 N2 O12, (C4 H8 O)' _chemical_formula_sum 'C56 H60 Cu3 N2 O13' _chemical_formula_weight 1159.68 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 12.571(3) _cell_length_b 13.202(3) _cell_length_c 19.105(4) _cell_angle_alpha 109.55(3) _cell_angle_beta 100.89(3) _cell_angle_gamma 102.37(3) _cell_volume 2799.1(15) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 24786 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 24.155 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1202 _exptl_absorpt_coefficient_mu 1.192 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 85 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.16 _diffrn_reflns_number 21985 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1130 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 27.85 _reflns_number_total 21993 _reflns_number_gt 10179 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT and XPREP (Siemens, 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEP-3 (Farrugia, 1997) WINGX-32 (Farrugia, 1999) ; _computing_publication_material 'enCIFer 1.0 (CCDC, 2003)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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 21993 _refine_ls_number_parameters 710 _refine_ls_number_restraints 469 _refine_ls_R_factor_all 0.1934 _refine_ls_R_factor_gt 0.1069 _refine_ls_wR_factor_ref 0.3313 _refine_ls_wR_factor_gt 0.2662 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 1.011 _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 -0.41605(6) 0.78405(7) 0.30740(4) 0.0376(3) Uani 1 1 d U . . Cu2 Cu 0.22022(7) 0.41876(8) 0.45048(5) 0.0467(3) Uani 1 1 d U . . Cu3 Cu -0.43803(10) -0.01753(8) -0.07203(5) 0.0679(4) Uani 1 1 d U . . O1 O -0.3810(4) 0.9273(4) 0.3931(2) 0.0401(11) Uani 1 1 d U . . O2 O -0.2837(3) 0.7523(3) 0.3530(2) 0.0349(10) Uani 1 1 d U . . O3 O 0.1140(4) 0.5051(4) 0.4503(3) 0.0405(11) Uani 1 1 d U . . O4 O 0.3059(4) 0.5118(4) 0.5581(3) 0.0517(13) Uani 1 1 d U . . O5 O 0.3181(4) 0.3227(5) 0.4527(3) 0.0577(14) Uani 1 1 d U . . O6 O 0.1216(4) 0.3154(4) 0.3498(3) 0.0497(12) Uani 1 1 d U . . O7 O -0.3018(5) 0.0374(4) 0.0115(3) 0.0610(14) Uani 1 1 d U . . O8 O -0.4014(6) -0.1461(5) -0.1305(3) 0.0758(18) Uani 1 1 d U . . O9 O -0.5620(5) -0.0573(5) -0.1641(3) 0.0693(16) Uani 1 1 d U . . O10 O -0.4747(5) 0.1158(4) -0.0160(3) 0.0566(14) Uani 1 1 d U . . O11 O -0.4317(3) 0.6565(4) 0.2150(2) 0.0389(11) Uani 1 1 d U . . O12 O -0.5385(4) 0.8240(4) 0.2568(3) 0.0441(11) Uani 1 1 d U B . C1 C -0.1909(7) 1.1365(7) 0.5846(4) 0.059(2) Uani 1 1 d U . . H1A H -0.1951 1.2104 0.6162 0.088 Uiso 1 1 calc R . . H1B H -0.1182 1.1453 0.5722 0.088 Uiso 1 1 calc R . . H1C H -0.1970 1.0876 0.6136 0.088 Uiso 1 1 calc R . . C2 C -0.2883(6) 1.0834(6) 0.5097(4) 0.0510(18) Uani 1 1 d U . . H2A H -0.3606 1.0783 0.5237 0.061 Uiso 1 1 calc R . . H2B H -0.2820 1.1354 0.4824 0.061 Uiso 1 1 calc R . . C3 C -0.2959(6) 0.9687(5) 0.4536(4) 0.0399(15) Uani 1 1 d U . . C4 C -0.2146(6) 0.9162(5) 0.4684(4) 0.0412(16) Uani 1 1 d U . . H4 H -0.1552 0.9550 0.5155 0.049 Uiso 1 1 calc R . . C5 C -0.2131(5) 0.8120(5) 0.4202(3) 0.0315(14) Uani 1 1 d U . . C6 C -0.1238(5) 0.7596(5) 0.4442(3) 0.0294(13) Uani 1 1 d U . . C7 C -0.0493(5) 0.8052(5) 0.5184(4) 0.0385(15) Uani 1 1 d U . . H7 H -0.0522 0.8727 0.5558 0.046 Uiso 1 1 calc R . . C8 C 0.0292(5) 0.7528(5) 0.5384(4) 0.0390(15) Uani 1 1 d U . . H8 H 0.0780 0.7836 0.5897 0.047 Uiso 1 1 calc R . . C9 C 0.0372(5) 0.6564(5) 0.4845(3) 0.0318(14) Uani 1 1 d U . . C10 C -0.0368(5) 0.6124(5) 0.4116(4) 0.0411(16) Uani 1 1 d U . . H10 H -0.0326 0.5460 0.3738 0.049 Uiso 1 1 calc R . . C11 C -0.1171(5) 0.6623(5) 0.3919(4) 0.0400(16) Uani 1 1 d U . . H11 H -0.1685 0.6287 0.3413 0.048 Uiso 1 1 calc R . . C12 C 0.1239(5) 0.5986(5) 0.5027(4) 0.0352(14) Uani 1 1 d U . . C13 C 0.2087(6) 0.6499(6) 0.5727(4) 0.0527(19) Uani 1 1 d U . . H13 H 0.2099 0.7219 0.6067 0.063 Uiso 1 1 calc R . . C14 C 0.2937(6) 0.6042(7) 0.5978(5) 0.0549(19) Uani 1 1 d U . . C15 C 0.3740(8) 0.6671(8) 0.6764(5) 0.076(3) Uani 1 1 d U . . H15A H 0.4422 0.6409 0.6798 0.091 Uiso 1 1 calc R . . H15B H 0.3983 0.7486 0.6871 0.091 Uiso 1 1 calc R . . C16 C 0.3188(10) 0.6485(9) 0.7314(6) 0.098(3) Uani 1 1 d U . . H16A H 0.3714 0.6895 0.7836 0.148 Uiso 1 1 calc R . . H16B H 0.2952 0.5677 0.7205 0.148 Uiso 1 1 calc R . . H16C H 0.2520 0.6755 0.7281 0.148 Uiso 1 1 calc R . . C17 C 0.4141(13) 0.0873(12) 0.3594(9) 0.141(5) Uani 1 1 d U . . H17A H 0.4794 0.0660 0.3802 0.211 Uiso 1 1 calc R . . H17B H 0.4264 0.1093 0.3168 0.211 Uiso 1 1 calc R . . H17C H 0.3452 0.0230 0.3404 0.211 Uiso 1 1 calc R . . C18 C 0.4017(10) 0.1769(9) 0.4173(6) 0.090(3) Uani 1 1 d U . . H18A H 0.4746 0.2380 0.4376 0.108 Uiso 1 1 calc R . . H18B H 0.3919 0.1524 0.4599 0.108 Uiso 1 1 calc R . . C19 C 0.3070(8) 0.2294(8) 0.4008(5) 0.063(2) Uani 1 1 d U . . C20 C 0.2207(8) 0.1774(8) 0.3308(6) 0.072(2) Uani 1 1 d U . . H20 H 0.2207 0.1071 0.2952 0.086 Uiso 1 1 calc R . . C21 C 0.1338(7) 0.2223(7) 0.3098(5) 0.0537(19) Uani 1 1 d U . . C22 C 0.0439(7) 0.1585(6) 0.2323(5) 0.0531(19) Uani 1 1 d U . . C23 C 0.0580(8) 0.0753(8) 0.1722(5) 0.073(2) Uani 1 1 d U . . H23 H 0.1267 0.0558 0.1779 0.087 Uiso 1 1 calc R . . C24 C -0.0267(9) 0.0202(8) 0.1039(6) 0.078(3) Uani 1 1 d U . . H24 H -0.0155 -0.0382 0.0633 0.094 Uiso 1 1 calc R . . C25 C -0.1301(7) 0.0464(6) 0.0911(5) 0.058(2) Uani 1 1 d U . . C26 C -0.1407(7) 0.1342(6) 0.1528(4) 0.057(2) Uani 1 1 d U . . H26 H -0.2080 0.1561 0.1471 0.068 Uiso 1 1 calc R . . C27 C -0.0555(7) 0.1894(6) 0.2214(5) 0.055(2) Uani 1 1 d U . . H27 H -0.0645 0.2495 0.2620 0.066 Uiso 1 1 calc R . . C28 C -0.2258(8) -0.0121(7) 0.0178(5) 0.059(2) Uani 1 1 d U . . C29 C -0.2281(8) -0.1152(8) -0.0385(5) 0.075(3) Uani 1 1 d U . . H29 H -0.1685 -0.1473 -0.0299 0.090 Uiso 1 1 calc R . . C30 C -0.3225(9) -0.1733(7) -0.1110(5) 0.074(3) Uani 1 1 d DU . . C32A C -0.2263(17) -0.3239(15) -0.1600(13) 0.050(2) Uiso 0.40 1 d PD A 1 H32A H -0.2524 -0.4062 -0.1780 0.075 Uiso 0.40 1 calc PR A 1 H32B H -0.1797 -0.2914 -0.1059 0.075 Uiso 0.40 1 calc PR A 1 H32C H -0.1809 -0.3027 -0.1921 0.075 Uiso 0.40 1 calc PR A 1 C31A C -0.317(2) -0.2845(17) -0.1654(12) 0.050(2) Uiso 0.40 1 d PD A 1 H31A H -0.3805 -0.3432 -0.1650 0.060 Uiso 0.40 1 calc PR A 1 H31B H -0.3359 -0.2836 -0.2178 0.060 Uiso 0.40 1 calc PR A 1 C31B C -0.338(3) -0.280(2) -0.1807(12) 0.050(2) Uiso 0.30 1 d PD A 2 H31C H -0.3184 -0.2612 -0.2236 0.060 Uiso 0.30 1 calc PR A 2 H31D H -0.4171 -0.3296 -0.1992 0.060 Uiso 0.30 1 calc PR A 2 C32B C -0.253(2) -0.3395(19) -0.1505(16) 0.050(2) Uiso 0.30 1 d PD A 2 H32D H -0.2601 -0.4101 -0.1924 0.075 Uiso 0.30 1 calc PR A 2 H32E H -0.2726 -0.3556 -0.1071 0.075 Uiso 0.30 1 calc PR A 2 H32F H -0.1753 -0.2896 -0.1331 0.075 Uiso 0.30 1 calc PR A 2 C31C C -0.267(3) -0.281(2) -0.1415(16) 0.050(2) Uiso 0.30 1 d P A 3 H31E H -0.1892 -0.2555 -0.1449 0.060 Uiso 0.30 1 calc PR A 3 H31F H -0.2684 -0.3252 -0.1083 0.060 Uiso 0.30 1 calc PR A 3 C32C C -0.356(2) -0.350(2) -0.2245(14) 0.050(2) Uiso 0.30 1 d P A 3 H32G H -0.3342 -0.4154 -0.2526 0.075 Uiso 0.30 1 calc PR A 3 H32H H -0.3579 -0.3014 -0.2535 0.075 Uiso 0.30 1 calc PR A 3 H32I H -0.4320 -0.3757 -0.2185 0.075 Uiso 0.30 1 calc PR A 3 C33 C -0.7799(8) 0.0204(7) -0.2748(5) 0.071(2) Uani 1 1 d U . . H33A H -0.8228 -0.0156 -0.3298 0.106 Uiso 1 1 calc R . . H33B H -0.7436 0.1005 -0.2615 0.106 Uiso 1 1 calc R . . H33C H -0.8317 0.0126 -0.2433 0.106 Uiso 1 1 calc R . . C34 C -0.6899(7) -0.0357(7) -0.2594(4) 0.065(2) Uani 1 1 d U . . H34A H -0.7284 -0.1168 -0.2747 0.078 Uiso 1 1 calc R . . H34B H -0.6410 -0.0301 -0.2938 0.078 Uiso 1 1 calc R . . C35 C -0.6139(7) 0.0094(7) -0.1776(4) 0.060(2) Uani 1 1 d U . . C36 C -0.6047(7) 0.1177(7) -0.1254(4) 0.059(2) Uani 1 1 d U . . H36 H -0.6451 0.1616 -0.1432 0.071 Uiso 1 1 calc R . . C37 C -0.5375(7) 0.1636(6) -0.0474(4) 0.0529(19) Uani 1 1 d U . . C38 C -0.5332(6) 0.2783(6) 0.0026(4) 0.0474(17) Uani 1 1 d U . . C39 C -0.6175(6) 0.3271(7) -0.0158(4) 0.056(2) Uani 1 1 d U . . H39 H -0.6785 0.2864 -0.0618 0.067 Uiso 1 1 calc R . . C40 C -0.6128(6) 0.4339(6) 0.0324(4) 0.0534(19) Uani 1 1 d U . . H40 H -0.6710 0.4654 0.0192 0.064 Uiso 1 1 calc R . . C41 C -0.5237(6) 0.4964(6) 0.1002(4) 0.0420(16) Uani 1 1 d U . . C42 C -0.4406(6) 0.4474(5) 0.1171(4) 0.0437(16) Uani 1 1 d U . . H42 H -0.3790 0.4885 0.1627 0.052 Uiso 1 1 calc R . . C43 C -0.4443(6) 0.3416(6) 0.0702(4) 0.0495(18) Uani 1 1 d U . . H43 H -0.3855 0.3109 0.0838 0.059 Uiso 1 1 calc R . . C44 C -0.5187(5) 0.6086(5) 0.1559(4) 0.0395(15) Uani 1 1 d U . . C45 C -0.6058(6) 0.6577(7) 0.1428(4) 0.056(2) Uani 1 1 d U B . H45 H -0.6679 0.6152 0.0976 0.067 Uiso 1 1 calc R . . C46 C -0.6094(7) 0.7613(7) 0.1893(5) 0.059(2) Uani 1 1 d U . . C47A C -0.6952(12) 0.8200(11) 0.1606(8) 0.116(4) Uiso 0.50 1 d P B 1 H47A H -0.7452 0.8252 0.1952 0.139 Uiso 0.50 1 calc PR B 1 H47B H -0.6485 0.8983 0.1746 0.139 Uiso 0.50 1 calc PR B 1 C48A C -0.765(2) 0.790(2) 0.0895(15) 0.109(5) Uiso 0.50 1 d P B 1 C47B C -0.6952(12) 0.8200(11) 0.1606(8) 0.116(4) Uiso 0.50 1 d P B 2 H47C H -0.6892 0.8162 0.1089 0.139 Uiso 0.50 1 calc PR B 2 H47D H -0.7725 0.7724 0.1527 0.139 Uiso 0.50 1 calc PR B 2 C48B C -0.690(2) 0.925(2) 0.2014(15) 0.109(5) Uiso 0.50 1 d P B 2 N1 N -0.5294(5) 0.6699(5) 0.3511(3) 0.0460(14) Uani 1 1 d U . . N2 N -0.6665(5) 0.5284(5) 0.4011(4) 0.0533(16) Uani 1 1 d U . . C49 C -0.4897(7) 0.6025(7) 0.3818(5) 0.057(2) Uani 1 1 d U . . H49 H -0.4135 0.6018 0.3857 0.069 Uiso 1 1 calc R . . C50 C -0.5564(7) 0.5351(7) 0.4077(5) 0.062(2) Uani 1 1 d U . . H50 H -0.5239 0.4915 0.4312 0.074 Uiso 1 1 calc R . . C51 C -0.7045(7) 0.5950(7) 0.3728(4) 0.0536(19) Uani 1 1 d U . . H51 H -0.7807 0.5953 0.3695 0.064 Uiso 1 1 calc R . . C52 C -0.6386(6) 0.6654(7) 0.3474(4) 0.0529(19) Uani 1 1 d U . . H52 H -0.6711 0.7117 0.3267 0.064 Uiso 1 1 calc R . . O1T O -0.1328(10) 0.6661(9) 0.1186(6) 0.098(4) Uani 0.60 1 d PDU . . C1T C -0.1518(12) 0.6813(13) 0.1907(8) 0.079(4) Uani 0.60 1 d PDU . . H1T1 H -0.1641 0.6095 0.1982 0.094 Uiso 0.60 1 calc PR . . H1T2 H -0.2202 0.7065 0.1937 0.094 Uiso 0.60 1 calc PR . . C2T C -0.0521(12) 0.7666(13) 0.2505(8) 0.076(4) Uani 0.60 1 d PDU . . H2T1 H -0.0756 0.8196 0.2906 0.091 Uiso 0.60 1 calc PR . . H2T2 H -0.0047 0.7304 0.2756 0.091 Uiso 0.60 1 calc PR . . C3T C 0.0111(12) 0.8259(12) 0.2127(8) 0.081(5) Uani 0.60 1 d PDU . . H3T1 H 0.0894 0.8203 0.2206 0.098 Uiso 0.60 1 calc PR . . H3T2 H 0.0144 0.9064 0.2322 0.098 Uiso 0.60 1 calc PR . . C4T C -0.0549(15) 0.7667(14) 0.1301(9) 0.097(6) Uani 0.60 1 d PDU . . H4T1 H -0.0955 0.8153 0.1141 0.117 Uiso 0.60 1 calc PR . . H4T2 H -0.0027 0.7508 0.0979 0.117 Uiso 0.60 1 calc PR . . C6T C -0.009(2) 0.456(2) 0.1876(13) 0.096(8) Uani 0.40 1 d PDU . . H6T1 H -0.0372 0.5098 0.2241 0.115 Uiso 0.40 1 calc PR . . H6T2 H 0.0170 0.4075 0.2124 0.115 Uiso 0.40 1 calc PR . . C5T C 0.080(2) 0.515(2) 0.1668(15) 0.110(10) Uani 0.40 1 d PDU . . H5T1 H 0.0848 0.5957 0.1847 0.132 Uiso 0.40 1 calc PR . . H5T2 H 0.1537 0.5092 0.1927 0.132 Uiso 0.40 1 calc PR . . C8T C -0.031(3) 0.378(2) 0.0629(18) 0.136(12) Uani 0.40 1 d PDU . . H8T1 H -0.0051 0.3106 0.0569 0.163 Uiso 0.40 1 calc PR . . H8T2 H -0.0766 0.3673 0.0113 0.163 Uiso 0.40 1 calc PR . . C7T C -0.101(2) 0.387(3) 0.1139(16) 0.140(13) Uani 0.40 1 d PDU . . H7T1 H -0.1402 0.3121 0.1126 0.168 Uiso 0.40 1 calc PR . . H7T2 H -0.1571 0.4258 0.1034 0.168 Uiso 0.40 1 calc PR . . O2T O 0.063(2) 0.471(2) 0.0882(15) 0.163(10) Uani 0.40 1 d PDU . . 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) 0.0475(5) 0.0288(4) 0.0091(3) -0.0068(3) 0.0109(3) Cu2 0.0373(5) 0.0582(6) 0.0555(6) 0.0298(4) 0.0130(4) 0.0237(4) Cu3 0.0982(8) 0.0432(6) 0.0300(5) -0.0045(4) 0.0158(5) -0.0095(5) O1 0.032(2) 0.049(2) 0.037(2) 0.0138(18) 0.0024(18) 0.0200(19) O2 0.0230(19) 0.041(2) 0.027(2) 0.0056(17) -0.0076(16) 0.0094(17) O3 0.031(2) 0.047(2) 0.046(2) 0.0186(19) 0.0080(18) 0.0171(18) O4 0.036(2) 0.062(3) 0.061(3) 0.030(2) 0.004(2) 0.023(2) O5 0.051(3) 0.071(3) 0.071(3) 0.038(3) 0.021(2) 0.037(2) O6 0.049(3) 0.048(3) 0.056(3) 0.017(2) 0.020(2) 0.022(2) O7 0.078(3) 0.046(3) 0.045(3) 0.007(2) 0.021(2) 0.007(2) O8 0.100(4) 0.055(3) 0.049(3) 0.002(2) 0.026(3) 0.002(3) O9 0.081(3) 0.057(3) 0.035(2) 0.000(2) 0.011(2) -0.013(3) O10 0.070(3) 0.047(3) 0.033(2) 0.005(2) 0.011(2) 0.001(2) O11 0.027(2) 0.044(2) 0.031(2) 0.0080(17) -0.0084(17) 0.0081(17) O12 0.034(2) 0.051(2) 0.039(2) 0.0143(19) -0.0061(18) 0.0159(19) C1 0.052(4) 0.059(4) 0.057(4) 0.016(3) 0.009(3) 0.018(3) C2 0.044(3) 0.050(3) 0.048(3) 0.009(3) 0.001(3) 0.021(3) C3 0.039(3) 0.042(3) 0.034(3) 0.012(2) 0.004(2) 0.012(3) C4 0.035(3) 0.044(3) 0.034(3) 0.008(2) -0.002(2) 0.013(3) C5 0.024(3) 0.039(3) 0.028(3) 0.011(2) 0.003(2) 0.010(2) C6 0.024(3) 0.034(3) 0.026(3) 0.011(2) -0.003(2) 0.008(2) C7 0.034(3) 0.042(3) 0.032(3) 0.006(2) 0.003(2) 0.018(2) C8 0.031(3) 0.048(3) 0.029(3) 0.012(2) -0.006(2) 0.013(2) C9 0.020(2) 0.041(3) 0.031(3) 0.012(2) 0.002(2) 0.009(2) C10 0.034(3) 0.039(3) 0.036(3) 0.005(2) -0.004(2) 0.010(2) C11 0.032(3) 0.040(3) 0.035(3) 0.008(2) -0.006(2) 0.012(2) C12 0.026(3) 0.040(3) 0.041(3) 0.019(2) 0.008(2) 0.010(2) C13 0.043(3) 0.054(3) 0.051(3) 0.015(3) -0.008(3) 0.021(3) C14 0.046(3) 0.057(4) 0.057(4) 0.024(3) -0.003(3) 0.019(3) C15 0.065(4) 0.074(4) 0.077(4) 0.027(3) -0.011(3) 0.030(3) C16 0.103(5) 0.090(5) 0.086(5) 0.043(4) -0.013(4) 0.016(4) C17 0.139(7) 0.141(7) 0.151(7) 0.061(5) 0.043(5) 0.050(5) C18 0.099(5) 0.087(5) 0.097(5) 0.039(4) 0.023(4) 0.051(4) C19 0.069(4) 0.069(4) 0.072(4) 0.040(3) 0.024(3) 0.037(3) C20 0.076(4) 0.065(4) 0.081(4) 0.028(3) 0.025(4) 0.032(3) C21 0.054(4) 0.056(4) 0.057(4) 0.022(3) 0.027(3) 0.021(3) C22 0.052(4) 0.049(3) 0.060(4) 0.015(3) 0.024(3) 0.021(3) C23 0.075(4) 0.071(4) 0.074(4) 0.022(3) 0.026(3) 0.033(3) C24 0.085(5) 0.075(4) 0.075(4) 0.015(3) 0.035(4) 0.034(4) C25 0.063(4) 0.053(4) 0.061(4) 0.015(3) 0.031(3) 0.020(3) C26 0.051(4) 0.051(3) 0.060(4) 0.011(3) 0.021(3) 0.013(3) C27 0.052(4) 0.046(3) 0.060(4) 0.012(3) 0.020(3) 0.011(3) C28 0.066(4) 0.051(4) 0.056(4) 0.014(3) 0.033(3) 0.008(3) C29 0.076(4) 0.070(4) 0.077(4) 0.019(3) 0.042(4) 0.014(3) C30 0.089(5) 0.059(4) 0.062(4) 0.009(3) 0.048(4) -0.002(3) C33 0.068(4) 0.072(4) 0.047(4) 0.013(3) 0.007(3) -0.003(3) C34 0.065(4) 0.066(4) 0.041(3) 0.008(3) 0.015(3) -0.006(3) C35 0.062(4) 0.059(4) 0.039(3) 0.010(3) 0.016(3) -0.009(3) C36 0.061(4) 0.061(4) 0.037(3) 0.012(3) 0.011(3) -0.003(3) C37 0.053(4) 0.052(3) 0.038(3) 0.009(3) 0.018(3) -0.005(3) C38 0.047(3) 0.046(3) 0.034(3) 0.010(2) 0.008(3) -0.003(3) C39 0.043(3) 0.064(4) 0.041(3) 0.009(3) 0.005(3) 0.002(3) C40 0.044(3) 0.063(4) 0.041(3) 0.012(3) 0.005(3) 0.013(3) C41 0.039(3) 0.050(3) 0.028(3) 0.013(2) 0.003(2) 0.007(3) C42 0.044(3) 0.041(3) 0.035(3) 0.012(2) -0.002(2) 0.008(3) C43 0.052(3) 0.049(3) 0.035(3) 0.011(3) 0.000(3) 0.009(3) C44 0.031(3) 0.046(3) 0.032(3) 0.016(2) -0.001(2) 0.000(2) C45 0.039(3) 0.064(4) 0.051(4) 0.015(3) -0.007(3) 0.017(3) C46 0.046(3) 0.068(4) 0.055(4) 0.021(3) -0.003(3) 0.023(3) N1 0.036(3) 0.055(3) 0.048(3) 0.020(2) 0.011(2) 0.018(2) N2 0.044(3) 0.065(3) 0.063(3) 0.032(3) 0.018(3) 0.030(3) C49 0.050(4) 0.066(4) 0.074(4) 0.042(3) 0.018(3) 0.027(3) C50 0.054(4) 0.072(4) 0.079(4) 0.047(3) 0.022(3) 0.030(3) C51 0.045(3) 0.063(4) 0.063(4) 0.034(3) 0.014(3) 0.022(3) C52 0.049(4) 0.062(4) 0.060(4) 0.033(3) 0.014(3) 0.027(3) O1T 0.092(5) 0.097(5) 0.093(5) 0.032(4) 0.001(4) 0.038(4) C1T 0.071(6) 0.084(6) 0.077(6) 0.032(4) 0.022(4) 0.014(4) C2T 0.072(6) 0.081(6) 0.070(6) 0.031(4) 0.020(4) 0.010(4) C3T 0.079(6) 0.082(6) 0.081(6) 0.036(5) 0.024(5) 0.012(4) C4T 0.109(7) 0.099(7) 0.091(7) 0.047(5) 0.029(5) 0.027(5) C6T 0.102(9) 0.094(9) 0.095(9) 0.041(6) 0.025(5) 0.031(5) C5T 0.112(11) 0.105(10) 0.114(11) 0.046(6) 0.026(6) 0.035(6) C8T 0.138(13) 0.134(13) 0.136(13) 0.053(7) 0.038(6) 0.041(6) C7T 0.142(14) 0.134(14) 0.148(14) 0.063(7) 0.038(6) 0.038(6) O2T 0.162(11) 0.162(11) 0.165(11) 0.067(6) 0.042(6) 0.051(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O2 1.923(4) . ? Cu1 O12 1.926(4) . ? Cu1 O11 1.931(4) . ? Cu1 O1 1.936(4) . ? Cu1 N1 2.318(6) . ? Cu2 O6 1.928(5) . ? Cu2 O3 1.932(4) . ? Cu2 O4 1.951(5) . ? Cu2 O5 1.951(5) . ? Cu2 N2 2.356(7) 1_655 ? Cu3 O8 1.898(6) . ? Cu3 O7 1.915(6) . ? Cu3 O10 1.931(5) . ? Cu3 O9 1.948(6) . ? O1 C3 1.280(7) . ? O2 C5 1.284(7) . ? O3 C12 1.265(7) . ? O4 C14 1.261(9) . ? O5 C19 1.256(10) . ? O6 C21 1.271(8) . ? O7 C28 1.277(10) . ? O8 C30 1.163(11) . ? O9 C35 1.266(10) . ? O10 C37 1.293(10) . ? O11 C44 1.277(7) . ? O12 C46 1.294(8) . ? C1 C2 1.530(10) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.505(9) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.389(9) . ? C4 C5 1.383(9) . ? C4 H4 0.9500 . ? C5 C6 1.516(8) . ? C6 C11 1.370(8) . ? C6 C7 1.391(8) . ? C7 C8 1.386(9) . ? C7 H7 0.9500 . ? C8 C9 1.381(8) . ? C8 H8 0.9500 . ? C9 C10 1.370(8) . ? C9 C12 1.511(8) . ? C10 C11 1.380(9) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.389(9) . ? C13 C14 1.418(9) . ? C13 H13 0.9500 . ? C14 C15 1.481(11) . ? C15 C16 1.422(13) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.385(16) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.535(12) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.397(12) . ? C20 C21 1.405(11) . ? C20 H20 0.9500 . ? C21 C22 1.518(11) . ? C22 C23 1.368(11) . ? C22 C27 1.396(10) . ? C23 C24 1.369(13) . ? C23 H23 0.9500 . ? C24 C25 1.413(12) . ? C24 H24 0.9500 . ? C25 C26 1.401(10) . ? C25 C28 1.499(12) . ? C26 C27 1.376(11) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C29 1.416(11) . ? C29 C30 1.480(13) . ? C29 H29 0.9500 . ? C30 C31A 1.515(16) . ? C30 C31B 1.527(17) . ? C30 C31C 1.70(3) . ? C32A C31A 1.35(3) . ? C32A H32A 0.9800 . ? C32A H32B 0.9800 . ? C32A H32C 0.9800 . ? C31A H31A 0.9900 . ? C31A H31B 0.9900 . ? C31B C32B 1.581(18) . ? C31B H31C 0.9900 . ? C31B H31D 0.9900 . ? C32B H32D 0.9800 . ? C32B H32E 0.9800 . ? C32B H32F 0.9800 . ? C31C C32C 1.59(3) . ? C31C H31E 0.9900 . ? C31C H31F 0.9900 . ? C32C H32G 0.9800 . ? C32C H32H 0.9800 . ? C32C H32I 0.9800 . ? C33 C34 1.516(12) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.511(11) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.408(11) . ? C36 C37 1.415(10) . ? C36 H36 0.9500 . ? C37 C38 1.478(10) . ? C38 C43 1.395(9) . ? C38 C39 1.403(11) . ? C39 C40 1.383(10) . ? C39 H39 0.9500 . ? C40 C41 1.397(9) . ? C40 H40 0.9500 . ? C41 C42 1.384(9) . ? C41 C44 1.487(9) . ? C42 C43 1.369(9) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 C45 1.411(10) . ? C45 C46 1.374(11) . ? C45 H45 0.9500 . ? C46 C47A 1.576(15) . ? C47A C48A 1.35(3) . ? C47A H47A 0.9900 . ? C47A H47B 0.9900 . ? N1 C49 1.347(9) . ? N1 C52 1.348(9) . ? N2 C51 1.302(9) . ? N2 C50 1.347(10) . ? N2 Cu2 2.356(7) 1_455 ? C49 C50 1.367(11) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 C52 1.382(11) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? O1T C4T 1.391(14) . ? O1T C1T 1.398(14) . ? C1T C2T 1.462(14) . ? C1T H1T1 0.9900 . ? C1T H1T2 0.9900 . ? C2T C3T 1.447(14) . ? C2T H2T1 0.9900 . ? C2T H2T2 0.9900 . ? C3T C4T 1.480(15) . ? C3T H3T1 0.9900 . ? C3T H3T2 0.9900 . ? C4T H4T1 0.9900 . ? C4T H4T2 0.9900 . ? C6T C5T 1.428(18) . ? C6T C7T 1.489(18) . ? C6T H6T1 0.9900 . ? C6T H6T2 0.9900 . ? C5T O2T 1.371(18) . ? C5T H5T1 0.9900 . ? C5T H5T2 0.9900 . ? C8T O2T 1.374(18) . ? C8T C7T 1.426(18) . ? C8T H8T1 0.9900 . ? C8T H8T2 0.9900 . ? C7T H7T1 0.9900 . ? C7T H7T2 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cu1 O12 173.9(2) . . ? O2 Cu1 O11 86.08(17) . . ? O12 Cu1 O11 92.98(18) . . ? O2 Cu1 O1 92.71(17) . . ? O12 Cu1 O1 87.10(18) . . ? O11 Cu1 O1 169.4(2) . . ? O2 Cu1 N1 90.95(19) . . ? O12 Cu1 N1 95.1(2) . . ? O11 Cu1 N1 91.3(2) . . ? O1 Cu1 N1 99.3(2) . . ? O6 Cu2 O3 86.0(2) . . ? O6 Cu2 O4 172.0(2) . . ? O3 Cu2 O4 93.3(2) . . ? O6 Cu2 O5 92.9(2) . . ? O3 Cu2 O5 175.1(2) . . ? O4 Cu2 O5 87.1(2) . . ? O6 Cu2 N2 94.1(2) . 1_655 ? O3 Cu2 N2 90.8(2) . 1_655 ? O4 Cu2 N2 93.8(2) . 1_655 ? O5 Cu2 N2 94.1(2) . 1_655 ? O8 Cu3 O7 94.3(3) . . ? O8 Cu3 O10 177.6(2) . . ? O7 Cu3 O10 86.7(2) . . ? O8 Cu3 O9 86.1(3) . . ? O7 Cu3 O9 170.3(2) . . ? O10 Cu3 O9 92.6(3) . . ? C3 O1 Cu1 125.9(4) . . ? C5 O2 Cu1 126.4(4) . . ? C12 O3 Cu2 125.9(4) . . ? C14 O4 Cu2 124.8(4) . . ? C19 O5 Cu2 126.7(5) . . ? C21 O6 Cu2 125.2(5) . . ? C28 O7 Cu3 126.0(5) . . ? C30 O8 Cu3 126.1(6) . . ? C35 O9 Cu3 124.8(5) . . ? C37 O10 Cu3 124.9(4) . . ? C44 O11 Cu1 125.6(4) . . ? C46 O12 Cu1 125.0(5) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C1 117.1(6) . . ? C3 C2 H2A 108.0 . . ? C1 C2 H2A 108.0 . . ? C3 C2 H2B 108.0 . . ? C1 C2 H2B 108.0 . . ? H2A C2 H2B 107.3 . . ? O1 C3 C4 124.9(6) . . ? O1 C3 C2 114.2(6) . . ? C4 C3 C2 120.9(6) . . ? C5 C4 C3 125.3(6) . . ? C5 C4 H4 117.4 . . ? C3 C4 H4 117.4 . . ? O2 C5 C4 124.6(5) . . ? O2 C5 C6 114.6(5) . . ? C4 C5 C6 120.8(5) . . ? C11 C6 C7 118.2(5) . . ? C11 C6 C5 119.3(5) . . ? C7 C6 C5 122.5(5) . . ? C8 C7 C6 120.5(6) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C9 C8 C7 120.7(5) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C10 C9 C8 118.1(6) . . ? C10 C9 C12 119.2(5) . . ? C8 C9 C12 122.7(5) . . ? C9 C10 C11 121.5(6) . . ? C9 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? C6 C11 C10 120.9(5) . . ? C6 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? O3 C12 C13 124.4(6) . . ? O3 C12 C9 115.7(5) . . ? C13 C12 C9 119.8(6) . . ? C12 C13 C14 125.7(7) . . ? C12 C13 H13 117.1 . . ? C14 C13 H13 117.1 . . ? O4 C14 C13 124.6(7) . . ? O4 C14 C15 116.5(7) . . ? C13 C14 C15 118.8(7) . . ? C16 C15 C14 108.8(8) . . ? C16 C15 H15A 109.9 . . ? C14 C15 H15A 109.9 . . ? C16 C15 H15B 109.9 . . ? C14 C15 H15B 109.9 . . ? H15A C15 H15B 108.3 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C18 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C17 C18 C19 120.8(11) . . ? C17 C18 H18A 107.1 . . ? C19 C18 H18A 107.1 . . ? C17 C18 H18B 107.1 . . ? C19 C18 H18B 107.1 . . ? H18A C18 H18B 106.8 . . ? O5 C19 C20 124.7(8) . . ? O5 C19 C18 114.5(8) . . ? C20 C19 C18 120.7(8) . . ? C19 C20 C21 124.3(8) . . ? C19 C20 H20 117.8 . . ? C21 C20 H20 117.8 . . ? O6 C21 C20 126.2(8) . . ? O6 C21 C22 113.8(7) . . ? C20 C21 C22 120.0(7) . . ? C23 C22 C27 119.0(8) . . ? C23 C22 C21 122.8(7) . . ? C27 C22 C21 118.1(6) . . ? C22 C23 C24 120.1(9) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C25 122.8(8) . . ? C23 C24 H24 118.6 . . ? C25 C24 H24 118.6 . . ? C26 C25 C24 115.8(8) . . ? C26 C25 C28 119.3(8) . . ? C24 C25 C28 124.9(7) . . ? C27 C26 C25 121.3(8) . . ? C27 C26 H26 119.3 . . ? C25 C26 H26 119.3 . . ? C26 C27 C22 120.9(7) . . ? C26 C27 H27 119.5 . . ? C22 C27 H27 119.5 . . ? O7 C28 C29 124.4(8) . . ? O7 C28 C25 115.3(7) . . ? C29 C28 C25 120.3(9) . . ? C28 C29 C30 120.4(9) . . ? C28 C29 H29 119.8 . . ? C30 C29 H29 119.8 . . ? O8 C30 C29 128.6(8) . . ? O8 C30 C31A 116.1(12) . . ? C29 C30 C31A 115.3(12) . . ? O8 C30 C31B 102.5(11) . . ? C29 C30 C31B 128.8(12) . . ? O8 C30 C31C 139.8(12) . . ? C29 C30 C31C 91.6(12) . . ? C31A C32A H32A 109.5 . . ? C31A C32A H32B 109.5 . . ? H32A C32A H32B 109.5 . . ? C31A C32A H32C 109.5 . . ? H32A C32A H32C 109.5 . . ? H32B C32A H32C 109.5 . . ? C32A C31A C30 125.8(19) . . ? C32A C31A H31A 105.9 . . ? C30 C31A H31A 105.9 . . ? C32A C31A H31B 105.9 . . ? C30 C31A H31B 105.9 . . ? H31A C31A H31B 106.2 . . ? C30 C31B C32B 105.2(14) . . ? C30 C31B H31C 110.7 . . ? C32B C31B H31C 110.7 . . ? C30 C31B H31D 110.7 . . ? C32B C31B H31D 110.7 . . ? H31C C31B H31D 108.8 . . ? C31B C32B H32D 109.5 . . ? C31B C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C31B C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? C32C C31C C30 98(2) . . ? C32C C31C H31E 112.1 . . ? C30 C31C H31E 112.1 . . ? C32C C31C H31F 112.1 . . ? C30 C31C H31F 112.1 . . ? H31E C31C H31F 109.8 . . ? C31C C32C H32G 109.5 . . ? C31C C32C H32H 109.5 . . ? H32G C32C H32H 109.5 . . ? C31C C32C H32I 109.5 . . ? H32G C32C H32I 109.5 . . ? H32H C32C H32I 109.5 . . ? C34 C33 H33A 109.5 . . ? C34 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C34 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 C33 117.2(7) . . ? C35 C34 H34A 108.0 . . ? C33 C34 H34A 108.0 . . ? C35 C34 H34B 108.0 . . ? C33 C34 H34B 108.0 . . ? H34A C34 H34B 107.2 . . ? O9 C35 C36 126.6(8) . . ? O9 C35 C34 113.7(7) . . ? C36 C35 C34 119.7(9) . . ? C35 C36 C37 122.4(8) . . ? C35 C36 H36 118.8 . . ? C37 C36 H36 118.8 . . ? O10 C37 C36 125.7(7) . . ? O10 C37 C38 116.0(6) . . ? C36 C37 C38 118.2(8) . . ? C43 C38 C39 117.8(7) . . ? C43 C38 C37 120.7(7) . . ? C39 C38 C37 121.6(7) . . ? C40 C39 C38 120.7(7) . . ? C40 C39 H39 119.6 . . ? C38 C39 H39 119.6 . . ? C39 C40 C41 121.1(7) . . ? C39 C40 H40 119.5 . . ? C41 C40 H40 119.5 . . ? C42 C41 C40 117.5(6) . . ? C42 C41 C44 119.6(6) . . ? C40 C41 C44 122.8(6) . . ? C43 C42 C41 122.2(6) . . ? C43 C42 H42 118.9 . . ? C41 C42 H42 118.9 . . ? C42 C43 C38 120.8(7) . . ? C42 C43 H43 119.6 . . ? C38 C43 H43 119.6 . . ? O11 C44 C45 122.9(6) . . ? O11 C44 C41 116.0(6) . . ? C45 C44 C41 121.0(6) . . ? C46 C45 C44 126.2(6) . . ? C46 C45 H45 116.9 . . ? C44 C45 H45 116.9 . . ? O12 C46 C45 124.6(7) . . ? O12 C46 C47A 113.4(8) . . ? C45 C46 C47A 121.8(8) . . ? C48A C47A C46 129.7(15) . . ? C48A C47A H47A 104.8 . . ? C46 C47A H47A 104.8 . . ? C48A C47A H47B 104.8 . . ? C46 C47A H47B 104.8 . . ? H47A C47A H47B 105.8 . . ? C49 N1 C52 115.4(7) . . ? C49 N1 Cu1 121.6(5) . . ? C52 N1 Cu1 123.0(5) . . ? C51 N2 C50 116.1(7) . . ? C51 N2 Cu2 121.1(5) . 1_455 ? C50 N2 Cu2 122.5(5) . 1_455 ? N1 C49 C50 121.7(7) . . ? N1 C49 H49 119.1 . . ? C50 C49 H49 119.1 . . ? N2 C50 C49 122.2(8) . . ? N2 C50 H50 118.9 . . ? C49 C50 H50 118.9 . . ? N2 C51 C52 122.9(7) . . ? N2 C51 H51 118.6 . . ? C52 C51 H51 118.6 . . ? N1 C52 C51 121.5(7) . . ? N1 C52 H52 119.2 . . ? C51 C52 H52 119.2 . . ? C4T O1T C1T 105.2(11) . . ? O1T C1T C2T 108.0(11) . . ? O1T C1T H1T1 110.1 . . ? C2T C1T H1T1 110.1 . . ? O1T C1T H1T2 110.1 . . ? C2T C1T H1T2 110.1 . . ? H1T1 C1T H1T2 108.4 . . ? C3T C2T C1T 107.1(11) . . ? C3T C2T H2T1 110.3 . . ? C1T C2T H2T1 110.3 . . ? C3T C2T H2T2 110.3 . . ? C1T C2T H2T2 110.3 . . ? H2T1 C2T H2T2 108.5 . . ? C2T C3T C4T 103.2(10) . . ? C2T C3T H3T1 111.1 . . ? C4T C3T H3T1 111.1 . . ? C2T C3T H3T2 111.1 . . ? C4T C3T H3T2 111.1 . . ? H3T1 C3T H3T2 109.1 . . ? O1T C4T C3T 110.2(12) . . ? O1T C4T H4T1 109.6 . . ? C3T C4T H4T1 109.6 . . ? O1T C4T H4T2 109.6 . . ? C3T C4T H4T2 109.6 . . ? H4T1 C4T H4T2 108.1 . . ? C5T C6T C7T 105.9(16) . . ? C5T C6T H6T1 110.6 . . ? C7T C6T H6T1 110.6 . . ? C5T C6T H6T2 110.6 . . ? C7T C6T H6T2 110.6 . . ? H6T1 C6T H6T2 108.7 . . ? O2T C5T C6T 110.5(16) . . ? O2T C5T H5T1 109.5 . . ? C6T C5T H5T1 109.5 . . ? O2T C5T H5T2 109.5 . . ? C6T C5T H5T2 109.5 . . ? H5T1 C5T H5T2 108.1 . . ? O2T C8T C7T 113.4(19) . . ? O2T C8T H8T1 108.9 . . ? C7T C8T H8T1 108.9 . . ? O2T C8T H8T2 108.9 . . ? C7T C8T H8T2 108.9 . . ? H8T1 C8T H8T2 107.7 . . ? C8T C7T C6T 97.5(18) . . ? C8T C7T H7T1 112.3 . . ? C6T C7T H7T1 112.3 . . ? C8T C7T H7T2 112.3 . . ? C6T C7T H7T2 112.3 . . ? H7T1 C7T H7T2 109.9 . . ? C5T O2T C8T 103.3(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Cu1 O1 C3 -1.0(6) . . . . ? O12 Cu1 O1 C3 -174.9(6) . . . . ? O11 Cu1 O1 C3 -84.2(11) . . . . ? N1 Cu1 O1 C3 90.4(6) . . . . ? O11 Cu1 O2 C5 174.2(5) . . . . ? O1 Cu1 O2 C5 4.7(5) . . . . ? N1 Cu1 O2 C5 -94.6(5) . . . . ? O6 Cu2 O3 C12 -177.2(5) . . . . ? O4 Cu2 O3 C12 10.7(5) . . . . ? N2 Cu2 O3 C12 -83.1(5) 1_655 . . . ? O3 Cu2 O4 C14 -10.6(6) . . . . ? O5 Cu2 O4 C14 174.4(6) . . . . ? N2 Cu2 O4 C14 80.4(6) 1_655 . . . ? O6 Cu2 O5 C19 0.4(7) . . . . ? O4 Cu2 O5 C19 172.4(7) . . . . ? N2 Cu2 O5 C19 -94.0(7) 1_655 . . . ? O3 Cu2 O6 C21 -175.5(6) . . . . ? O5 Cu2 O6 C21 -0.3(6) . . . . ? N2 Cu2 O6 C21 94.0(6) 1_655 . . . ? O8 Cu3 O7 C28 -4.2(6) . . . . ? O10 Cu3 O7 C28 178.0(6) . . . . ? O7 Cu3 O8 C30 4.1(8) . . . . ? O9 Cu3 O8 C30 174.4(8) . . . . ? O8 Cu3 O9 C35 -160.8(7) . . . . ? O10 Cu3 O9 C35 17.1(7) . . . . ? O7 Cu3 O10 C37 152.8(6) . . . . ? O9 Cu3 O10 C37 -17.5(6) . . . . ? O2 Cu1 O11 C44 168.0(5) . . . . ? O12 Cu1 O11 C44 -18.1(5) . . . . ? O1 Cu1 O11 C44 -108.2(10) . . . . ? N1 Cu1 O11 C44 77.1(5) . . . . ? O11 Cu1 O12 C46 11.7(6) . . . . ? O1 Cu1 O12 C46 -178.9(6) . . . . ? N1 Cu1 O12 C46 -79.8(6) . . . . ? Cu1 O1 C3 C4 -1.0(10) . . . . ? Cu1 O1 C3 C2 178.3(5) . . . . ? C1 C2 C3 O1 178.0(7) . . . . ? C1 C2 C3 C4 -2.7(11) . . . . ? O1 C3 C4 C5 0.2(12) . . . . ? C2 C3 C4 C5 -179.0(7) . . . . ? Cu1 O2 C5 C4 -6.7(9) . . . . ? Cu1 O2 C5 C6 173.7(4) . . . . ? C3 C4 C5 O2 3.9(11) . . . . ? C3 C4 C5 C6 -176.5(6) . . . . ? O2 C5 C6 C11 6.7(9) . . . . ? C4 C5 C6 C11 -172.9(7) . . . . ? O2 C5 C6 C7 -171.9(6) . . . . ? C4 C5 C6 C7 8.5(9) . . . . ? C11 C6 C7 C8 -0.1(10) . . . . ? C5 C6 C7 C8 178.5(6) . . . . ? C6 C7 C8 C9 1.9(10) . . . . ? C7 C8 C9 C10 -1.9(10) . . . . ? C7 C8 C9 C12 177.9(6) . . . . ? C8 C9 C10 C11 0.2(10) . . . . ? C12 C9 C10 C11 -179.6(6) . . . . ? C7 C6 C11 C10 -1.6(10) . . . . ? C5 C6 C11 C10 179.8(6) . . . . ? C9 C10 C11 C6 1.6(11) . . . . ? Cu2 O3 C12 C13 -6.1(10) . . . . ? Cu2 O3 C12 C9 172.5(4) . . . . ? C10 C9 C12 O3 -7.1(9) . . . . ? C8 C9 C12 O3 173.1(6) . . . . ? C10 C9 C12 C13 171.6(7) . . . . ? C8 C9 C12 C13 -8.2(10) . . . . ? O3 C12 C13 C14 -2.8(13) . . . . ? C9 C12 C13 C14 178.6(7) . . . . ? Cu2 O4 C14 C13 6.0(12) . . . . ? Cu2 O4 C14 C15 -174.7(6) . . . . ? C12 C13 C14 O4 2.8(14) . . . . ? C12 C13 C14 C15 -176.5(8) . . . . ? O4 C14 C15 C16 -100.7(10) . . . . ? C13 C14 C15 C16 78.6(11) . . . . ? Cu2 O5 C19 C20 0.1(13) . . . . ? Cu2 O5 C19 C18 176.6(6) . . . . ? C17 C18 C19 O5 -166.5(11) . . . . ? C17 C18 C19 C20 10.2(17) . . . . ? O5 C19 C20 C21 -0.8(15) . . . . ? C18 C19 C20 C21 -177.1(9) . . . . ? Cu2 O6 C21 C20 -0.2(11) . . . . ? Cu2 O6 C21 C22 -179.5(5) . . . . ? C19 C20 C21 O6 0.8(14) . . . . ? C19 C20 C21 C22 -179.9(8) . . . . ? O6 C21 C22 C23 160.9(8) . . . . ? C20 C21 C22 C23 -18.5(12) . . . . ? O6 C21 C22 C27 -16.8(10) . . . . ? C20 C21 C22 C27 163.8(8) . . . . ? C27 C22 C23 C24 -2.9(14) . . . . ? C21 C22 C23 C24 179.4(8) . . . . ? C22 C23 C24 C25 1.1(15) . . . . ? C23 C24 C25 C26 0.8(14) . . . . ? C23 C24 C25 C28 -179.3(9) . . . . ? C24 C25 C26 C27 -0.9(12) . . . . ? C28 C25 C26 C27 179.3(7) . . . . ? C25 C26 C27 C22 -0.9(12) . . . . ? C23 C22 C27 C26 2.9(12) . . . . ? C21 C22 C27 C26 -179.4(7) . . . . ? Cu3 O7 C28 C29 2.8(11) . . . . ? Cu3 O7 C28 C25 -177.0(5) . . . . ? C26 C25 C28 O7 13.3(11) . . . . ? C24 C25 C28 O7 -166.6(8) . . . . ? C26 C25 C28 C29 -166.6(8) . . . . ? C24 C25 C28 C29 13.6(13) . . . . ? O7 C28 C29 C30 0.1(13) . . . . ? C25 C28 C29 C30 179.9(7) . . . . ? Cu3 O8 C30 C29 -2.7(15) . . . . ? Cu3 O8 C30 C31A 175.3(14) . . . . ? Cu3 O8 C30 C31B -179.6(15) . . . . ? Cu3 O8 C30 C31C 174.2(17) . . . . ? C28 C29 C30 O8 -0.2(15) . . . . ? C28 C29 C30 C31A -178.2(15) . . . . ? C28 C29 C30 C31B 176(2) . . . . ? C28 C29 C30 C31C -178.2(12) . . . . ? O8 C30 C31A C32A 170(2) . . . . ? C29 C30 C31A C32A -12(3) . . . . ? C31B C30 C31A C32A 149(12) . . . . ? C31C C30 C31A C32A -12(3) . . . . ? O8 C30 C31B C32B -165(2) . . . . ? C29 C30 C31B C32B 18(3) . . . . ? C31A C30 C31B C32B -4(8) . . . . ? C31C C30 C31B C32B 8(2) . . . . ? O8 C30 C31C C32C 7(3) . . . . ? C29 C30 C31C C32C -175.8(16) . . . . ? C31A C30 C31C C32C 4(4) . . . . ? C31B C30 C31C C32C -3(3) . . . . ? Cu3 O9 C35 C36 -10.0(12) . . . . ? Cu3 O9 C35 C34 168.5(5) . . . . ? C33 C34 C35 O9 162.6(7) . . . . ? C33 C34 C35 C36 -18.8(11) . . . . ? O9 C35 C36 C37 -3.4(13) . . . . ? C34 C35 C36 C37 178.2(7) . . . . ? Cu3 O10 C37 C36 10.9(10) . . . . ? Cu3 O10 C37 C38 -166.0(5) . . . . ? C35 C36 C37 O10 2.9(12) . . . . ? C35 C36 C37 C38 179.7(7) . . . . ? O10 C37 C38 C43 17.6(10) . . . . ? C36 C37 C38 C43 -159.6(7) . . . . ? O10 C37 C38 C39 -162.3(7) . . . . ? C36 C37 C38 C39 20.5(10) . . . . ? C43 C38 C39 C40 -0.9(11) . . . . ? C37 C38 C39 C40 179.0(7) . . . . ? C38 C39 C40 C41 0.5(12) . . . . ? C39 C40 C41 C42 0.1(11) . . . . ? C39 C40 C41 C44 -176.4(7) . . . . ? C40 C41 C42 C43 -0.4(11) . . . . ? C44 C41 C42 C43 176.3(7) . . . . ? C41 C42 C43 C38 0.0(11) . . . . ? C39 C38 C43 C42 0.6(11) . . . . ? C37 C38 C43 C42 -179.3(7) . . . . ? Cu1 O11 C44 C45 14.6(9) . . . . ? Cu1 O11 C44 C41 -165.6(4) . . . . ? C42 C41 C44 O11 4.2(10) . . . . ? C40 C41 C44 O11 -179.3(6) . . . . ? C42 C41 C44 C45 -175.9(7) . . . . ? C40 C41 C44 C45 0.6(11) . . . . ? O11 C44 C45 C46 1.0(13) . . . . ? C41 C44 C45 C46 -178.9(8) . . . . ? Cu1 O12 C46 C45 -1.9(12) . . . . ? Cu1 O12 C46 C47A -176.1(6) . . . . ? C44 C45 C46 O12 -7.8(14) . . . . ? C44 C45 C46 C47A 165.9(9) . . . . ? O12 C46 C47A C48A 166.5(18) . . . . ? C45 C46 C47A C48A -8(2) . . . . ? O2 Cu1 N1 C49 -9.9(6) . . . . ? O12 Cu1 N1 C49 169.3(6) . . . . ? O11 Cu1 N1 C49 76.2(6) . . . . ? O1 Cu1 N1 C49 -102.8(6) . . . . ? O2 Cu1 N1 C52 170.5(6) . . . . ? O12 Cu1 N1 C52 -10.3(6) . . . . ? O11 Cu1 N1 C52 -103.4(6) . . . . ? O1 Cu1 N1 C52 77.6(6) . . . . ? C52 N1 C49 C50 -0.4(11) . . . . ? Cu1 N1 C49 C50 180.0(6) . . . . ? C51 N2 C50 C49 -4.0(12) . . . . ? Cu2 N2 C50 C49 -177.2(6) 1_455 . . . ? N1 C49 C50 N2 2.9(14) . . . . ? C50 N2 C51 C52 2.9(12) . . . . ? Cu2 N2 C51 C52 176.2(6) 1_455 . . . ? C49 N1 C52 C51 -0.7(11) . . . . ? Cu1 N1 C52 C51 178.9(6) . . . . ? N2 C51 C52 N1 -0.6(13) . . . . ? C4T O1T C1T C2T -25.0(18) . . . . ? O1T C1T C2T C3T 17.1(19) . . . . ? C1T C2T C3T C4T -2(2) . . . . ? C1T O1T C4T C3T 24(2) . . . . ? C2T C3T C4T O1T -13(2) . . . . ? C7T C6T C5T O2T -13(4) . . . . ? O2T C8T C7T C6T -32(4) . . . . ? C5T C6T C7T C8T 25(3) . . . . ? C6T C5T O2T C8T -6(4) . . . . ? C7T C8T O2T C5T 25(4) . . . . ? _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.724 _refine_diff_density_min -2.371 _refine_diff_density_rms 0.203 # Attachment '(5)Cu3L3dabco.CIF' data_lj59 _database_code_depnum_ccdc_archive 'CCDC 292068' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C78 H108 Cu3 N6 O12, 3(C4 H10 O)' _chemical_formula_sum 'C90 H138 Cu3 N6 O15' _chemical_formula_weight 1734.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/m _symmetry_space_group_name_Hall '-P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 7.5941(8) _cell_length_b 33.013(3) _cell_length_c 21.558(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.130(2) _cell_angle_gamma 90.00 _cell_volume 5404.8(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 12465 _cell_measurement_theta_min 4.25 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.066 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1854 _exptl_absorpt_coefficient_mu 0.639 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 197 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.20 _diffrn_reflns_number 52355 _diffrn_reflns_av_R_equivalents 0.0696 _diffrn_reflns_av_sigmaI/netI 0.0710 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 28.10 _reflns_number_total 12961 _reflns_number_gt 8377 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT and XPREP (Siemens, 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997), WINGX-32 (Farrugia, 1999)' _computing_publication_material 'enCIFer 1.0 (CCDC, 2003)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1387P)^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 12961 _refine_ls_number_parameters 486 _refine_ls_number_restraints 92 _refine_ls_R_factor_all 0.0993 _refine_ls_R_factor_gt 0.0718 _refine_ls_wR_factor_ref 0.2178 _refine_ls_wR_factor_gt 0.2029 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.031 _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 0.4022(11) -0.0425(3) 0.7987(4) 0.0321(7) Uiso 0.60 1 d PD A 1 H1A H 0.5102 -0.0389 0.7745 0.048 Uiso 0.60 1 calc PR A 1 H1B H 0.3876 -0.0712 0.8090 0.048 Uiso 0.60 1 calc PR A 1 H1C H 0.4101 -0.0266 0.8370 0.048 Uiso 0.60 1 calc PR A 1 C2 C 0.0765(10) -0.0413(3) 0.7912(4) 0.0321(7) Uiso 0.60 1 d PD A 1 H2A H 0.0729 -0.0710 0.7919 0.048 Uiso 0.60 1 calc PR A 1 H2B H -0.0268 -0.0310 0.7689 0.048 Uiso 0.60 1 calc PR A 1 H2C H 0.0759 -0.0310 0.8338 0.048 Uiso 0.60 1 calc PR A 1 C3 C 0.2719(12) -0.0459(4) 0.6941(4) 0.0321(7) Uiso 0.60 1 d PD A 1 H3A H 0.3815 -0.0350 0.6771 0.048 Uiso 0.60 1 calc PR A 1 H3B H 0.1735 -0.0389 0.6666 0.048 Uiso 0.60 1 calc PR A 1 H3C H 0.2812 -0.0755 0.6973 0.048 Uiso 0.60 1 calc PR A 1 C4 C 0.2392(11) -0.0277(4) 0.7593(5) 0.0321(7) Uiso 0.60 1 d PD A 1 C1A C 0.4650(13) -0.0394(4) 0.7817(6) 0.0321(7) Uiso 0.40 1 d PD A 2 H1A1 H 0.4924 -0.0265 0.8214 0.048 Uiso 0.40 1 calc PR A 2 H1A2 H 0.5494 -0.0304 0.7503 0.048 Uiso 0.40 1 calc PR A 2 H1A3 H 0.4728 -0.0689 0.7863 0.048 Uiso 0.40 1 calc PR A 2 C2A C 0.2221(16) -0.0459(6) 0.6984(6) 0.0321(7) Uiso 0.40 1 d PD A 2 H2A1 H 0.1936 -0.0747 0.7037 0.048 Uiso 0.40 1 calc PR A 2 H2A2 H 0.3185 -0.0431 0.6686 0.048 Uiso 0.40 1 calc PR A 2 H2A3 H 0.1182 -0.0314 0.6830 0.048 Uiso 0.40 1 calc PR A 2 C3A C 0.1457(15) -0.0464(4) 0.8071(5) 0.0321(7) Uiso 0.40 1 d PD A 2 H3A1 H 0.1847 -0.0413 0.8498 0.048 Uiso 0.40 1 calc PR A 2 H3A2 H 0.1377 -0.0756 0.8001 0.048 Uiso 0.40 1 calc PR A 2 H3A3 H 0.0298 -0.0340 0.8006 0.048 Uiso 0.40 1 calc PR A 2 C4A C 0.2788(14) -0.0279(6) 0.7615(7) 0.0321(7) Uiso 0.40 1 d PD A 2 C5 C 0.2530(7) 0.01857(10) 0.76135(17) 0.0253(7) Uani 1 1 d . . . C6 C 0.2525(8) 0.04094(10) 0.70654(16) 0.0282(8) Uani 1 1 d . A . H6 H 0.2545 0.0265 0.6684 0.034 Uiso 1 1 calc R . . C7 C 0.2491(8) 0.08353(10) 0.70411(16) 0.0242(7) Uani 1 1 d . . . C8 C 0.2498(8) 0.10442(11) 0.64199(17) 0.0279(8) Uani 1 1 d D A . C9 C 0.1879(10) 0.0861(2) 0.5876(4) 0.0256(6) Uiso 0.60 1 d PD A 1 H9 H 0.1482 0.0588 0.5885 0.031 Uiso 0.60 1 calc PR A 1 C10 C 0.1844(10) 0.1079(2) 0.5318(4) 0.0256(6) Uiso 0.60 1 d PD A 1 H10 H 0.1394 0.0955 0.4953 0.031 Uiso 0.60 1 calc PR A 1 C12 C 0.3154(11) 0.1654(2) 0.5843(4) 0.0256(6) Uiso 0.60 1 d PD A 1 H12 H 0.3631 0.1920 0.5825 0.031 Uiso 0.60 1 calc PR A 1 C13 C 0.3135(11) 0.1448(2) 0.6393(4) 0.0256(6) Uiso 0.60 1 d PD A 1 H13 H 0.3552 0.1575 0.6760 0.031 Uiso 0.60 1 calc PR A 1 C9A C 0.2766(14) 0.0837(3) 0.5869(5) 0.0256(6) Uiso 0.40 1 d PD A 2 H9A H 0.3017 0.0555 0.5870 0.031 Uiso 0.40 1 calc PR A 2 C10A C 0.2659(17) 0.1053(3) 0.5312(5) 0.0256(6) Uiso 0.40 1 d PD A 2 H10A H 0.2727 0.0909 0.4932 0.031 Uiso 0.40 1 calc PR A 2 C12A C 0.2251(17) 0.1673(3) 0.5850(5) 0.0256(6) Uiso 0.40 1 d PD A 2 H12A H 0.2171 0.1960 0.5850 0.031 Uiso 0.40 1 calc PR A 2 C13A C 0.2156(17) 0.1459(3) 0.6424(5) 0.0256(6) Uiso 0.40 1 d PD A 2 H13A H 0.1868 0.1595 0.6798 0.031 Uiso 0.40 1 calc PR A 2 C11 C 0.2456(8) 0.14706(10) 0.52947(16) 0.0244(7) Uani 1 1 d D . . C14 C 0.2401(7) 0.17138(10) 0.47122(16) 0.0233(7) Uani 1 1 d . A . C15 C 0.2460(8) 0.15139(11) 0.41404(16) 0.0301(8) Uani 1 1 d . . . H15 H 0.2514 0.1226 0.4142 0.036 Uiso 1 1 calc R A . C16 C 0.2445(8) 0.17125(11) 0.35616(17) 0.0275(8) Uani 1 1 d . A . C17 C 0.2338(10) 0.1469(3) 0.2958(5) 0.0370(7) Uiso 0.70 1 d PD A 1 C18 C 0.0635(9) 0.1573(2) 0.2609(4) 0.0370(7) Uiso 0.70 1 d PD A 1 H18A H 0.0482 0.1868 0.2600 0.055 Uiso 0.70 1 calc PR A 1 H18B H -0.0369 0.1449 0.2819 0.055 Uiso 0.70 1 calc PR A 1 H18C H 0.0707 0.1471 0.2183 0.055 Uiso 0.70 1 calc PR A 1 C19 C 0.3929(9) 0.1599(2) 0.2563(4) 0.0370(7) Uiso 0.70 1 d PD A 1 H19A H 0.3863 0.1891 0.2483 0.055 Uiso 0.70 1 calc PR A 1 H19B H 0.3914 0.1452 0.2169 0.055 Uiso 0.70 1 calc PR A 1 H19C H 0.5021 0.1538 0.2787 0.055 Uiso 0.70 1 calc PR A 1 C20 C 0.2610(12) 0.1011(3) 0.3051(5) 0.0370(7) Uiso 0.70 1 d PD A 1 H20A H 0.2799 0.0881 0.2648 0.055 Uiso 0.70 1 calc PR A 1 H20B H 0.1564 0.0894 0.3248 0.055 Uiso 0.70 1 calc PR A 1 H20C H 0.3640 0.0965 0.3317 0.055 Uiso 0.70 1 calc PR A 1 C17A C 0.2743(19) 0.1474(7) 0.2949(12) 0.0370(7) Uiso 0.30 1 d PD A 2 C18A C 0.4562(17) 0.1540(6) 0.2698(9) 0.0370(7) Uiso 0.30 1 d PD A 2 H18D H 0.4722 0.1377 0.2323 0.055 Uiso 0.30 1 calc PR A 2 H18E H 0.5433 0.1460 0.3011 0.055 Uiso 0.30 1 calc PR A 2 H18F H 0.4718 0.1827 0.2597 0.055 Uiso 0.30 1 calc PR A 2 C19A C 0.134(2) 0.1646(5) 0.2490(8) 0.0370(7) Uiso 0.30 1 d PD A 2 H19D H 0.1301 0.1477 0.2116 0.055 Uiso 0.30 1 calc PR A 2 H19E H 0.1653 0.1924 0.2376 0.055 Uiso 0.30 1 calc PR A 2 H19F H 0.0180 0.1644 0.2689 0.055 Uiso 0.30 1 calc PR A 2 C20A C 0.217(2) 0.1027(6) 0.3037(13) 0.0370(7) Uiso 0.30 1 d PD A 2 H20D H 0.2318 0.0880 0.2646 0.055 Uiso 0.30 1 calc PR A 2 H20E H 0.0925 0.1018 0.3159 0.055 Uiso 0.30 1 calc PR A 2 H20F H 0.2890 0.0901 0.3360 0.055 Uiso 0.30 1 calc PR A 2 C21 C 0.0597(11) 0.0526(3) 1.0338(5) 0.0397(8) Uiso 0.50 1 d PD B 1 H21A H 0.0528 0.0345 0.9979 0.060 Uiso 0.50 1 calc PR B 1 H21B H -0.0380 0.0720 1.0322 0.060 Uiso 0.50 1 calc PR B 1 H21C H 0.0520 0.0367 1.0720 0.060 Uiso 0.50 1 calc PR B 1 C22 C 0.3818(12) 0.0432(3) 1.0338(5) 0.0397(8) Uiso 0.50 1 d PD B 1 H22A H 0.4134 0.0372 1.0770 0.060 Uiso 0.50 1 calc PR B 1 H22B H 0.4847 0.0541 1.0122 0.060 Uiso 0.50 1 calc PR B 1 H22C H 0.3425 0.0184 1.0132 0.060 Uiso 0.50 1 calc PR B 1 C23 C 0.2737(15) 0.1015(4) 1.0902(7) 0.0397(8) Uiso 0.50 1 d PD B 1 H23A H 0.1759 0.1202 1.0980 0.060 Uiso 0.50 1 calc PR B 1 H23B H 0.3814 0.1170 1.0825 0.060 Uiso 0.50 1 calc PR B 1 H23C H 0.2908 0.0840 1.1265 0.060 Uiso 0.50 1 calc PR B 1 C24 C 0.2307(14) 0.0750(3) 1.0326(6) 0.0397(8) Uiso 0.50 1 d PD B 1 C21A C 0.1901(12) 0.0368(3) 1.0321(5) 0.0397(8) Uiso 0.50 1 d PD B 2 H21D H 0.2360 0.0182 1.0006 0.060 Uiso 0.50 1 calc PR B 2 H21E H 0.0669 0.0432 1.0227 0.060 Uiso 0.50 1 calc PR B 2 H21F H 0.1977 0.0240 1.0730 0.060 Uiso 0.50 1 calc PR B 2 C22A C 0.4914(11) 0.0633(3) 1.0363(5) 0.0397(8) Uiso 0.50 1 d PD B 2 H22D H 0.5215 0.0570 1.0794 0.060 Uiso 0.50 1 calc PR B 2 H22E H 0.5641 0.0859 1.0218 0.060 Uiso 0.50 1 calc PR B 2 H22F H 0.5133 0.0395 1.0103 0.060 Uiso 0.50 1 calc PR B 2 C23A C 0.2239(14) 0.1003(4) 1.0883(7) 0.0397(8) Uiso 0.50 1 d PD B 2 H23D H 0.1088 0.1118 1.0774 0.060 Uiso 0.50 1 calc PR B 2 H23E H 0.3060 0.1224 1.0980 0.060 Uiso 0.50 1 calc PR B 2 H23F H 0.2115 0.0827 1.1246 0.060 Uiso 0.50 1 calc PR B 2 C24A C 0.2967(13) 0.0750(4) 1.0321(6) 0.0397(8) Uiso 0.50 1 d PD B 2 C25 C 0.2575(9) 0.09778(11) 0.96996(17) 0.0317(9) Uani 1 1 d . . . C26 C 0.2567(8) 0.13978(10) 0.96799(17) 0.0281(8) Uani 1 1 d . B . H26 H 0.2545 0.1540 1.0063 0.034 Uiso 1 1 calc R . . C27 C 0.2590(7) 0.16240(10) 0.91329(16) 0.0231(7) Uani 1 1 d . . . C28 C 0.2639(7) 0.20770(10) 0.91558(16) 0.0217(8) Uani 1 1 d . . . C30 C 0.2070(15) 0.2286(3) 0.9692(6) 0.0220(8) Uiso 0.35 1 d P . 1 H30A H 0.1692 0.2141 1.0048 0.026 Uiso 0.35 1 calc PR . 1 C29 C 0.269(2) 0.2288(4) 0.8635(6) 0.0220(8) Uiso 0.35 1 d P . 1 H29 H 0.2735 0.2148 0.8251 0.026 Uiso 0.35 1 calc PR . 1 C30A C 0.3291(9) 0.2290(2) 0.9661(3) 0.0220(8) Uiso 0.65 1 d P . 2 H30B H 0.3740 0.2148 1.0009 0.026 Uiso 0.65 1 calc PR . 2 C29A C 0.1920(10) 0.2290(2) 0.8642(4) 0.0220(8) Uiso 0.65 1 d P . 2 H29A H 0.1440 0.2146 0.8300 0.026 Uiso 0.65 1 calc PR . 2 C37 C -0.3432(15) 0.1279(4) 0.8694(6) 0.0613(9) Uiso 0.60 1 d P C 1 H37A H -0.3964 0.1288 0.9113 0.074 Uiso 0.60 1 calc PR C 1 H37B H -0.3730 0.1534 0.8477 0.074 Uiso 0.60 1 calc PR C 1 C38 C -0.3425(15) 0.0569(4) 0.8595(6) 0.0613(9) Uiso 0.60 1 d P C 1 H38A H -0.4085 0.0333 0.8431 0.074 Uiso 0.60 1 calc PR C 1 H38B H -0.3531 0.0569 0.9052 0.074 Uiso 0.60 1 calc PR C 1 C39 C -0.3484(15) 0.0968(4) 0.7685(6) 0.0613(9) Uiso 0.60 1 d P C 1 H39A H -0.4138 0.1182 0.7460 0.074 Uiso 0.60 1 calc PR C 1 H39B H -0.3659 0.0708 0.7465 0.074 Uiso 0.60 1 calc PR C 1 C40 C -0.1415(16) 0.1240(4) 0.8752(6) 0.0613(9) Uiso 0.60 1 d P C 1 H40A H -0.0863 0.1503 0.8648 0.074 Uiso 0.60 1 calc PR C 1 H40B H -0.1105 0.1174 0.9187 0.074 Uiso 0.60 1 calc PR C 1 C41 C -0.1412(15) 0.0534(4) 0.8405(6) 0.0613(9) Uiso 0.60 1 d P C 1 H41A H -0.0753 0.0381 0.8725 0.074 Uiso 0.60 1 calc PR C 1 H41B H -0.1302 0.0388 0.8005 0.074 Uiso 0.60 1 calc PR C 1 C42 C -0.1472(15) 0.1076(4) 0.7714(6) 0.0613(9) Uiso 0.60 1 d P C 1 H42A H -0.0840 0.0940 0.7371 0.074 Uiso 0.60 1 calc PR C 1 H42B H -0.1310 0.1372 0.7671 0.074 Uiso 0.60 1 calc PR C 1 C43 C -0.349(2) 0.0833(5) 0.9026(8) 0.0613(9) Uiso 0.40 1 d P C 2 H43A H -0.3639 0.1069 0.9305 0.074 Uiso 0.40 1 calc PR C 2 H43B H -0.4132 0.0599 0.9198 0.074 Uiso 0.40 1 calc PR C 2 C44 C -0.343(2) 0.0578(5) 0.8049(9) 0.0613(9) Uiso 0.40 1 d PD C 2 H44A H -0.4155 0.0496 0.7687 0.074 Uiso 0.40 1 calc PR C 2 H44B H -0.3338 0.0348 0.8342 0.074 Uiso 0.40 1 calc PR C 2 C45 C -0.347(2) 0.1316(5) 0.8219(9) 0.0613(9) Uiso 0.40 1 d P C 2 H45A H -0.4149 0.1522 0.8454 0.074 Uiso 0.40 1 calc PR C 2 H45B H -0.3627 0.1374 0.7772 0.074 Uiso 0.40 1 calc PR C 2 C46 C -0.149(2) 0.0732(6) 0.8933(9) 0.0613(9) Uiso 0.40 1 d P C 2 H46A H -0.0822 0.0826 0.9301 0.074 Uiso 0.40 1 calc PR C 2 H46B H -0.1348 0.0434 0.8904 0.074 Uiso 0.40 1 calc PR C 2 C47 C -0.147(2) 0.0741(6) 0.7832(8) 0.0613(9) Uiso 0.40 1 d PD C 2 H47A H -0.0728 0.0511 0.7696 0.074 Uiso 0.40 1 calc PR C 2 H47B H -0.1582 0.0935 0.7484 0.074 Uiso 0.40 1 calc PR C 2 C48 C -0.147(2) 0.1353(5) 0.8392(9) 0.0613(9) Uiso 0.40 1 d P C 2 H48A H -0.0863 0.1537 0.8100 0.074 Uiso 0.40 1 calc PR C 2 H48B H -0.1332 0.1461 0.8818 0.074 Uiso 0.40 1 calc PR C 2 C62 C 0.633(3) 0.2500 0.4811(15) 0.0398(13) Uiso 0.25 2 d SPD D 3 H62A H 0.5930 0.2255 0.5036 0.048 Uiso 0.13 1 calc PR D 3 H62B H 0.5930 0.2745 0.5036 0.048 Uiso 0.13 1 calc PR D 3 C49 C 0.830(3) 0.2500 0.4732(15) 0.0398(13) Uiso 0.25 2 d SPD D 3 H49A H 0.8743 0.2740 0.4959 0.048 Uiso 0.13 1 calc PR D 3 H49B H 0.8743 0.2260 0.4959 0.048 Uiso 0.13 1 calc PR D 3 C50 C 0.836(4) 0.2500 0.3544(16) 0.0398(13) Uiso 0.25 2 d SP D 3 H50A H 0.8789 0.2258 0.3318 0.048 Uiso 0.13 1 calc PR D 3 H50B H 0.8789 0.2742 0.3318 0.048 Uiso 0.13 1 calc PR D 3 C51 C 0.636(5) 0.2500 0.3538(18) 0.0398(13) Uiso 0.25 2 d SP D 3 H51A H 0.5923 0.2743 0.3318 0.048 Uiso 0.13 1 calc PR D 3 H51B H 0.5923 0.2257 0.3318 0.048 Uiso 0.13 1 calc PR D 3 C52 C 0.813(3) 0.2076(7) 0.3968(12) 0.0398(13) Uiso 0.25 1 d P D 4 H52A H 0.8749 0.1943 0.3620 0.048 Uiso 0.25 1 calc PR D 4 H52B H 0.8091 0.1885 0.4323 0.048 Uiso 0.25 1 calc PR D 4 C53 C 0.648(3) 0.2182(7) 0.3797(11) 0.0398(13) Uiso 0.25 1 d P D 4 H53A H 0.5714 0.1940 0.3817 0.048 Uiso 0.25 1 calc PR D 4 H53B H 0.6505 0.2276 0.3361 0.048 Uiso 0.25 1 calc PR D 4 C54 C 0.648(4) 0.2126(9) 0.4437(13) 0.0398(13) Uiso 0.25 1 d P D 5 H54A H 0.6159 0.1896 0.4164 0.048 Uiso 0.25 1 calc PR D 5 H54B H 0.5975 0.2074 0.4852 0.048 Uiso 0.25 1 calc PR D 5 C55 C 0.847(4) 0.2149(9) 0.4490(13) 0.0398(13) Uiso 0.25 1 d P D 5 H55A H 0.8805 0.2164 0.4933 0.048 Uiso 0.25 1 calc PR D 5 H55B H 0.8994 0.1901 0.4312 0.048 Uiso 0.25 1 calc PR D 5 C56 C 0.644(4) 0.2331(7) 0.3624(13) 0.0398(13) Uiso 0.25 1 d P D 6 H56A H 0.6045 0.2501 0.3271 0.048 Uiso 0.50 2 calc SPR D 6 H56B H 0.5927 0.2058 0.3564 0.048 Uiso 0.25 1 calc PR D 6 C57 C 0.854(3) 0.2296(7) 0.3604(12) 0.0398(13) Uiso 0.25 1 d P D 6 H57A H 0.8910 0.2008 0.3603 0.048 Uiso 0.25 1 calc PR D 6 H57B H 0.9015 0.2431 0.3231 0.048 Uiso 0.25 1 calc PR D 6 C58 C 0.648(3) 0.2250(7) 0.4691(12) 0.0398(13) Uiso 0.25 1 d P D 7 H58A H 0.6040 0.1969 0.4645 0.048 Uiso 0.25 1 calc PR D 7 H58B H 0.6050 0.2356 0.5092 0.048 Uiso 0.25 1 calc PR D 7 C59 C 0.848(4) 0.2240(8) 0.4706(13) 0.0398(13) Uiso 0.25 1 d P D 7 H59A H 0.8913 0.1959 0.4661 0.048 Uiso 0.25 1 calc PR D 7 H59B H 0.8923 0.2350 0.5105 0.048 Uiso 0.25 1 calc PR D 7 C60 C 0.851(4) 0.2123(8) 0.4249(14) 0.0398(13) Uiso 0.25 1 d P D 8 H60A H 0.8907 0.2021 0.4658 0.048 Uiso 0.25 1 calc PR D 8 H60B H 0.9026 0.1944 0.3927 0.048 Uiso 0.25 1 calc PR D 8 C61 C 0.644(4) 0.2095(8) 0.4212(13) 0.0398(13) Uiso 0.25 1 d P D 8 H61A H 0.6086 0.1941 0.3838 0.048 Uiso 0.25 1 calc PR D 8 H61B H 0.5982 0.1952 0.4582 0.048 Uiso 0.25 1 calc PR D 8 O7 O 0.7380(13) 0.0559(2) 0.5504(3) 0.0555(18) Uani 0.50 1 d PU E 1 C31 C 0.746(3) 0.0124(4) 0.6345(7) 0.084(4) Uani 0.50 1 d PU E 1 H31A H 0.7554 0.0128 0.6798 0.126 Uiso 0.50 1 calc PR E 1 H31B H 0.8462 -0.0027 0.6173 0.126 Uiso 0.50 1 calc PR E 1 H31C H 0.6361 -0.0008 0.6222 0.126 Uiso 0.50 1 calc PR E 1 C32 C 0.749(3) 0.0515(4) 0.6122(6) 0.082(4) Uani 0.50 1 d PU E 1 H32A H 0.6491 0.0663 0.6311 0.099 Uiso 0.50 1 calc PR E 1 H32B H 0.8585 0.0646 0.6265 0.099 Uiso 0.50 1 calc PR E 1 C33 C 0.713(2) 0.0971(5) 0.5266(7) 0.089(5) Uani 0.50 1 d PU E 1 H33A H 0.8049 0.1151 0.5444 0.107 Uiso 0.50 1 calc PR E 1 H33B H 0.5969 0.1074 0.5398 0.107 Uiso 0.50 1 calc PR E 1 C34 C 0.725(2) 0.0980(4) 0.4528(6) 0.076(4) Uani 0.50 1 d PU E 1 H34A H 0.7116 0.1260 0.4381 0.114 Uiso 0.50 1 calc PR E 1 H34B H 0.6317 0.0811 0.4351 0.114 Uiso 0.50 1 calc PR E 1 H34C H 0.8402 0.0876 0.4397 0.114 Uiso 0.50 1 calc PR E 1 O8 O -0.180(3) 0.2500 0.6364(12) 0.066(7) Uani 0.25 2 d SPU . 2 C35 C -0.179(4) 0.3167(8) 0.6354(13) 0.066(7) Uani 0.25 1 d PU . 2 H35A H -0.0926 0.3385 0.6416 0.099 Uiso 0.25 1 calc PR . 2 H35B H -0.2761 0.3201 0.6647 0.099 Uiso 0.25 1 calc PR . 2 H35C H -0.2242 0.3179 0.5929 0.099 Uiso 0.25 1 calc PR . 2 C36 C -0.102(4) 0.2811(10) 0.6451(16) 0.082(9) Uani 0.25 1 d PU . 2 H36A H 0.0049 0.2803 0.6187 0.098 Uiso 0.25 1 calc PR . 2 H36B H -0.0606 0.2808 0.6887 0.098 Uiso 0.25 1 calc PR . 2 N1 N -0.0722(6) 0.09301(14) 0.8349(3) 0.0378(11) Uani 1 1 d . . . N2 N -0.4147(6) 0.09354(13) 0.8348(3) 0.0398(12) Uani 1 1 d . . . N3 N 0.5737(8) 0.2500 0.4185(3) 0.0389(16) Uani 1 2 d S . . N4 N 0.9137(8) 0.2500 0.4168(4) 0.0394(16) Uani 1 2 d S . . O1 O 0.2567(5) 0.03376(7) 0.81499(11) 0.0271(6) Uani 1 1 d . A . O2 O 0.2535(6) 0.10707(7) 0.75032(11) 0.0279(6) Uani 1 1 d . A . O3 O 0.2449(6) 0.20934(7) 0.47928(10) 0.0257(5) Uani 1 1 d . . . O4 O 0.2428(6) 0.20921(7) 0.34890(11) 0.0291(6) Uani 1 1 d . . . O5 O 0.2573(6) 0.07455(7) 0.92369(11) 0.0333(7) Uani 1 1 d . B . O6 O 0.2571(6) 0.14795(7) 0.85843(11) 0.0270(6) Uani 1 1 d . B . Cu1 Cu 0.25558(10) 0.090848(11) 0.83695(2) 0.02422(14) Uani 1 1 d . . . Cu2 Cu 0.24448(13) 0.2500 0.41420(3) 0.02301(16) 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 C5 0.0300(19) 0.0197(15) 0.0262(18) 0.0021(14) -0.002(3) 0.002(2) C6 0.045(2) 0.0173(16) 0.0223(17) -0.0014(13) -0.001(3) -0.006(3) C7 0.0318(19) 0.0190(16) 0.0216(17) 0.0039(13) -0.003(3) 0.003(2) C8 0.036(2) 0.0238(17) 0.0236(17) 0.0019(14) -0.002(3) -0.008(3) C11 0.0285(19) 0.0248(16) 0.0199(17) 0.0006(13) 0.006(2) -0.006(2) C14 0.026(2) 0.0205(16) 0.0228(17) 0.0013(13) -0.003(2) -0.004(2) C15 0.045(2) 0.0241(17) 0.0207(17) 0.0005(14) 0.001(3) 0.011(3) C16 0.037(2) 0.0251(18) 0.0205(16) -0.0047(14) 0.005(3) 0.000(3) C25 0.052(3) 0.0226(17) 0.0208(18) 0.0036(14) 0.003(3) 0.001(3) C26 0.046(2) 0.0182(16) 0.0202(17) -0.0021(13) -0.004(3) 0.002(3) C27 0.028(2) 0.0185(15) 0.0228(17) -0.0009(13) 0.004(2) -0.001(2) C28 0.024(2) 0.0161(15) 0.0248(18) 0.0016(13) 0.003(2) 0.0022(19) O7 0.049(3) 0.067(4) 0.051(3) -0.003(3) -0.007(4) 0.002(4) C31 0.089(5) 0.081(5) 0.081(5) 0.011(4) 0.001(5) -0.003(5) C32 0.081(5) 0.089(5) 0.076(5) 0.006(4) 0.002(5) 0.003(5) C33 0.087(7) 0.090(6) 0.090(6) -0.005(4) 0.008(5) 0.009(5) C34 0.080(6) 0.074(5) 0.074(5) -0.006(4) -0.009(4) 0.003(4) O8 0.063(8) 0.072(8) 0.063(8) 0.000 0.002(5) 0.000 C35 0.066(8) 0.069(8) 0.065(8) -0.008(5) 0.001(5) -0.003(5) C36 0.080(10) 0.085(10) 0.080(10) -0.001(5) -0.001(5) 0.005(5) N1 0.032(2) 0.036(3) 0.045(3) 0.000(2) 0.002(2) -0.0055(19) N2 0.034(2) 0.029(2) 0.057(3) 0.002(2) 0.000(2) -0.0040(19) N3 0.030(3) 0.053(4) 0.034(4) 0.000 0.004(3) 0.000 N4 0.036(4) 0.044(4) 0.038(4) 0.000 0.004(3) 0.000 O1 0.0421(16) 0.0174(11) 0.0217(12) 0.0032(9) -0.0051(18) -0.0037(18) O2 0.0476(16) 0.0162(11) 0.0198(12) 0.0013(9) 0.0024(19) -0.0062(19) O3 0.0405(15) 0.0211(11) 0.0155(12) -0.0023(9) 0.0015(18) 0.0034(18) O4 0.0489(17) 0.0224(12) 0.0160(12) -0.0019(9) 0.0034(19) -0.0021(18) O5 0.0627(19) 0.0186(12) 0.0186(13) 0.0030(10) -0.005(2) -0.001(2) O6 0.0454(16) 0.0150(11) 0.0207(12) 0.0015(9) 0.0013(18) -0.0026(18) Cu1 0.0410(3) 0.0140(2) 0.0177(2) 0.00153(15) -0.0001(3) -0.0018(3) Cu2 0.0369(4) 0.0184(3) 0.0138(3) 0.000 0.0013(4) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C4 1.576(11) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C4 1.486(11) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.551(11) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.532(13) . ? C1A C4A 1.527(13) . ? C1A H1A1 0.9800 . ? C1A H1A2 0.9800 . ? C1A H1A3 0.9800 . ? C2A C4A 1.546(15) . ? C2A H2A1 0.9800 . ? C2A H2A2 0.9800 . ? C2A H2A3 0.9800 . ? C3A C4A 1.538(14) . ? C3A H3A1 0.9800 . ? C3A H3A2 0.9800 . ? C3A H3A3 0.9800 . ? C4A C5 1.545(19) . ? C5 O1 1.261(4) . ? C5 C6 1.393(5) . ? C6 C7 1.407(5) . ? C6 H6 0.9500 . ? C7 O2 1.264(4) . ? C7 C8 1.506(5) . ? C8 C9A 1.385(12) . ? C8 C13A 1.393(12) . ? C8 C9 1.401(9) . ? C8 C13 1.418(9) . ? C9 C10 1.402(12) . ? C9 H9 0.9500 . ? C10 C11 1.376(9) . ? C10 H10 0.9500 . ? C12 C13 1.370(12) . ? C12 C11 1.428(9) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C9A C10A 1.398(15) . ? C9A H9A 0.9500 . ? C10A C11 1.387(11) . ? C10A H10A 0.9500 . ? C12A C11 1.380(11) . ? C12A C13A 1.426(16) . ? C12A H12A 0.9500 . ? C13A H13A 0.9500 . ? C11 C14 1.491(5) . ? C14 O3 1.266(4) . ? C14 C15 1.399(5) . ? C15 C16 1.410(5) . ? C15 H15 0.9500 . ? C16 O4 1.263(4) . ? C16 C17 1.531(12) . ? C16 C17A 1.55(3) . ? C17 C18 1.535(10) . ? C17 C20 1.538(9) . ? C17 C19 1.541(10) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C17A C18A 1.501(16) . ? C17A C20A 1.549(17) . ? C17A C19A 1.561(17) . ? C18A H18D 0.9800 . ? C18A H18E 0.9800 . ? C18A H18F 0.9800 . ? C19A H19D 0.9800 . ? C19A H19E 0.9800 . ? C19A H19F 0.9800 . ? C20A H20D 0.9800 . ? C20A H20E 0.9800 . ? C20A H20F 0.9800 . ? C21 C24 1.495(12) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.555(12) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.554(12) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.559(13) . ? C21A C24A 1.498(12) . ? C21A H21D 0.9800 . ? C21A H21E 0.9800 . ? C21A H21F 0.9800 . ? C22A C24A 1.531(12) . ? C22A H22D 0.9800 . ? C22A H22E 0.9800 . ? C22A H22F 0.9800 . ? C23A C24A 1.575(13) . ? C23A H23D 0.9800 . ? C23A H23E 0.9800 . ? C23A H23F 0.9800 . ? C24A C25 1.563(14) . ? C25 O5 1.258(4) . ? C25 C26 1.387(5) . ? C26 C27 1.396(5) . ? C26 H26 0.9500 . ? C27 O6 1.275(4) . ? C27 C28 1.497(5) . ? C28 C29 1.321(13) . ? C28 C30A 1.387(8) . ? C28 C30 1.415(12) . ? C28 C29A 1.421(8) . ? C30 C30 1.41(2) 4_565 ? C30 H30A 0.9500 . ? C29 C29 1.40(2) 4_565 ? C29 H29 0.9500 . ? C30A C30A 1.384(13) 4_565 ? C30A H30B 0.9500 . ? C29A C29A 1.384(15) 4_565 ? C29A H29A 0.9500 . ? C37 N2 1.461(13) . ? C37 C40 1.542(13) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 N2 1.431(12) . ? C38 C41 1.587(14) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 N2 1.520(13) . ? C39 C42 1.570(14) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 N1 1.441(13) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 N1 1.415(12) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 N1 1.558(13) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C46 1.57(2) . ? C43 N2 1.579(18) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 N2 1.451(17) . ? C44 C47 1.653(15) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 N2 1.386(18) . ? C45 C48 1.57(2) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 N1 1.536(18) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 N1 1.397(17) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 N1 1.510(18) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C62 N3 1.42(3) . ? C62 C49 1.503(18) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C49 N4 1.37(3) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 N4 1.47(4) . ? C50 C51 1.52(4) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 N3 1.48(4) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.35(3) . ? C52 N4 1.65(2) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 N3 1.46(2) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 N3 1.46(3) . ? C54 C55 1.51(3) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 N4 1.44(3) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 N3 1.43(3) . ? C56 C57 1.60(3) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 N4 1.46(3) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 N3 1.48(3) . ? C58 C59 1.52(3) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 N4 1.53(3) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 N4 1.34(3) . ? C60 C61 1.58(3) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 N3 1.44(3) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? O7 C32 1.343(14) . ? O7 C33 1.464(16) . ? C31 C32 1.377(18) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.596(19) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? O8 C36 1.20(3) 4_565 ? O8 C36 1.20(3) . ? C35 C36 1.33(4) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? N1 Cu1 2.491(4) . ? N3 C56 1.43(3) 4_565 ? N3 C61 1.44(3) 4_565 ? N3 C53 1.46(2) 4_565 ? N3 C54 1.46(3) 4_565 ? N3 C58 1.48(3) 4_565 ? N4 C60 1.34(3) 4_565 ? N4 C55 1.44(3) 4_565 ? N4 C57 1.46(3) 4_565 ? N4 C59 1.53(3) 4_565 ? N4 C52 1.65(2) 4_565 ? O1 Cu1 1.943(2) . ? O2 Cu1 1.943(2) . ? O3 Cu2 1.942(2) . ? O4 Cu2 1.948(2) . ? O5 Cu1 1.946(2) . ? O6 Cu1 1.941(2) . ? Cu1 N2 36.574(7) 3 ? Cu2 O3 1.942(2) 4_565 ? Cu2 O4 1.948(2) 4_565 ? Cu2 N4 25.886(6) 3 ? 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 C2 C4 C5 110.2(8) . . ? C2 C4 C3 115.9(8) . . ? C5 C4 C3 113.7(8) . . ? C2 C4 C1 108.1(7) . . ? C5 C4 C1 103.9(7) . . ? C3 C4 C1 103.9(7) . . ? C4A C1A H1A1 109.5 . . ? C4A C1A H1A2 109.5 . . ? H1A1 C1A H1A2 109.5 . . ? C4A C1A H1A3 109.5 . . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? C4A C2A H2A1 109.5 . . ? C4A C2A H2A2 109.5 . . ? H2A1 C2A H2A2 109.5 . . ? C4A C2A H2A3 109.5 . . ? H2A1 C2A H2A3 109.5 . . ? H2A2 C2A H2A3 109.5 . . ? C4A C3A H3A1 109.5 . . ? C4A C3A H3A2 109.5 . . ? H3A1 C3A H3A2 109.5 . . ? C4A C3A H3A3 109.5 . . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? C1A C4A C3A 109.2(11) . . ? C1A C4A C5 111.5(11) . . ? C3A C4A C5 108.2(10) . . ? C1A C4A C2A 114.2(11) . . ? C3A C4A C2A 103.1(10) . . ? C5 C4A C2A 110.2(12) . . ? O1 C5 C6 124.5(3) . . ? O1 C5 C4 115.1(5) . . ? C6 C5 C4 120.3(5) . . ? O1 C5 C4A 112.9(6) . . ? C6 C5 C4A 121.9(6) . . ? C5 C6 C7 124.1(3) . . ? C5 C6 H6 117.9 . . ? C7 C6 H6 117.9 . . ? O2 C7 C6 125.8(3) . . ? O2 C7 C8 114.8(3) . . ? C6 C7 C8 119.4(3) . . ? C9A C8 C13A 121.1(7) . . ? C13A C8 C9 111.6(6) . . ? C9A C8 C13 112.2(6) . . ? C9 C8 C13 119.1(6) . . ? C9A C8 C7 122.5(6) . . ? C13A C8 C7 116.3(6) . . ? C9 C8 C7 123.0(5) . . ? C13 C8 C7 117.9(5) . . ? C8 C9 C10 120.1(7) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C11 C10 C9 120.5(7) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C13 C12 C11 120.1(7) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C8 120.4(7) . . ? C12 C13 H13 119.8 . . ? C8 C13 H13 119.8 . . ? C8 C9A C10A 118.5(9) . . ? C8 C9A H9A 120.8 . . ? C10A C9A H9A 120.8 . . ? C11 C10A C9A 122.4(9) . . ? C11 C10A H10A 118.8 . . ? C9A C10A H10A 118.8 . . ? C11 C12A C13A 121.2(9) . . ? C11 C12A H12A 119.4 . . ? C13A C12A H12A 119.4 . . ? C8 C13A C12A 118.2(10) . . ? C8 C13A H13A 120.9 . . ? C12A C13A H13A 120.9 . . ? C10 C11 C12A 112.6(6) . . ? C12A C11 C10A 118.0(7) . . ? C10 C11 C12 119.6(5) . . ? C10A C11 C12 111.0(6) . . ? C10 C11 C14 121.9(5) . . ? C12A C11 C14 117.8(5) . . ? C10A C11 C14 124.1(5) . . ? C12 C11 C14 118.5(4) . . ? O3 C14 C15 125.9(3) . . ? O3 C14 C11 114.6(3) . . ? C15 C14 C11 119.2(3) . . ? C14 C15 C16 124.1(3) . . ? C14 C15 H15 118.0 . . ? C16 C15 H15 118.0 . . ? O4 C16 C15 124.8(3) . . ? O4 C16 C17 114.6(4) . . ? C15 C16 C17 120.5(4) . . ? O4 C16 C17A 113.6(8) . . ? C15 C16 C17A 121.0(8) . . ? C16 C17 C18 110.0(7) . . ? C16 C17 C20 113.5(8) . . ? C18 C17 C20 113.5(7) . . ? C16 C17 C19 106.4(7) . . ? C18 C17 C19 109.0(7) . . ? C20 C17 C19 104.0(7) . . ? C18A C17A C20A 116.4(15) . . ? C18A C17A C16 111.6(15) . . ? C20A C17A C16 109.7(17) . . ? C18A C17A C19A 110.2(14) . . ? C20A C17A C19A 103.3(13) . . ? C16 C17A C19A 104.7(13) . . ? C17A C18A H18D 109.5 . . ? C17A C18A H18E 109.5 . . ? H18D C18A H18E 109.5 . . ? C17A C18A H18F 109.5 . . ? H18D C18A H18F 109.5 . . ? H18E C18A H18F 109.5 . . ? C17A C19A H19D 109.5 . . ? C17A C19A H19E 109.5 . . ? H19D C19A H19E 109.5 . . ? C17A C19A H19F 109.5 . . ? H19D C19A H19F 109.5 . . ? H19E C19A H19F 109.5 . . ? C17A C20A H20D 109.5 . . ? C17A C20A H20E 109.5 . . ? H20D C20A H20E 109.5 . . ? C17A C20A H20F 109.5 . . ? H20D C20A H20F 109.5 . . ? H20E C20A H20F 109.5 . . ? C21 C24 C23 116.5(10) . . ? C21 C24 C22 107.9(9) . . ? C23 C24 C22 102.3(8) . . ? C21 C24 C25 111.6(9) . . ? C23 C24 C25 113.1(10) . . ? C22 C24 C25 104.0(8) . . ? C24A C21A H21D 109.5 . . ? C24A C21A H21E 109.5 . . ? H21D C21A H21E 109.5 . . ? C24A C21A H21F 109.5 . . ? H21D C21A H21F 109.5 . . ? H21E C21A H21F 109.5 . . ? C24A C22A H22D 109.5 . . ? C24A C22A H22E 109.5 . . ? H22D C22A H22E 109.5 . . ? C24A C22A H22F 109.5 . . ? H22D C22A H22F 109.5 . . ? H22E C22A H22F 109.5 . . ? C24A C23A H23D 109.5 . . ? C24A C23A H23E 109.5 . . ? H23D C23A H23E 109.5 . . ? C24A C23A H23F 109.5 . . ? H23D C23A H23F 109.5 . . ? H23E C23A H23F 109.5 . . ? C21A C24A C22A 108.0(9) . . ? C21A C24A C25 107.7(9) . . ? C22A C24A C25 110.7(9) . . ? C21A C24A C23A 104.9(9) . . ? C22A C24A C23A 115.4(9) . . ? C25 C24A C23A 109.7(10) . . ? O5 C25 C26 125.8(3) . . ? O5 C25 C24 113.1(5) . . ? C26 C25 C24 120.5(5) . . ? O5 C25 C24A 112.7(5) . . ? C26 C25 C24A 120.5(5) . . ? C25 C26 C27 124.1(3) . . ? C25 C26 H26 118.0 . . ? C27 C26 H26 118.0 . . ? O6 C27 C26 125.7(3) . . ? O6 C27 C28 113.9(3) . . ? C26 C27 C28 120.5(3) . . ? C29 C28 C30A 112.8(7) . . ? C29 C28 C30 116.5(8) . . ? C30A C28 C29A 119.7(5) . . ? C30 C28 C29A 106.1(6) . . ? C29 C28 C27 119.9(6) . . ? C30A C28 C27 122.8(4) . . ? C30 C28 C27 120.5(6) . . ? C29A C28 C27 117.4(4) . . ? C30 C30 C28 119.2(5) 4_565 . ? C30 C30 H30A 120.4 4_565 . ? C28 C30 H30A 120.4 . . ? C28 C29 C29 121.8(6) . 4_565 ? C28 C29 H29 119.1 . . ? C29 C29 H29 119.1 4_565 . ? C30A C30A C28 120.5(3) 4_565 . ? C30A C30A H30B 119.7 4_565 . ? C28 C30A H30B 119.7 . . ? C29A C29A C28 119.7(3) 4_565 . ? C29A C29A H29A 120.1 4_565 . ? C28 C29A H29A 120.1 . . ? N2 C37 C40 110.1(10) . . ? N2 C37 H37A 109.6 . . ? C40 C37 H37A 109.6 . . ? N2 C37 H37B 109.6 . . ? C40 C37 H37B 109.6 . . ? H37A C37 H37B 108.2 . . ? N2 C38 C41 109.5(9) . . ? N2 C38 H38A 109.8 . . ? C41 C38 H38A 109.8 . . ? N2 C38 H38B 109.8 . . ? C41 C38 H38B 109.8 . . ? H38A C38 H38B 108.2 . . ? N2 C39 C42 107.6(10) . . ? N2 C39 H39A 110.2 . . ? C42 C39 H39A 110.2 . . ? N2 C39 H39B 110.2 . . ? C42 C39 H39B 110.2 . . ? H39A C39 H39B 108.5 . . ? N1 C40 C37 112.0(11) . . ? N1 C40 H40A 109.2 . . ? C37 C40 H40A 109.2 . . ? N1 C40 H40B 109.2 . . ? C37 C40 H40B 109.2 . . ? H40A C40 H40B 107.9 . . ? N1 C41 C38 108.1(9) . . ? N1 C41 H41A 110.1 . . ? C38 C41 H41A 110.1 . . ? N1 C41 H41B 110.1 . . ? C38 C41 H41B 110.1 . . ? H41A C41 H41B 108.4 . . ? N1 C42 C39 108.6(10) . . ? N1 C42 H42A 110.0 . . ? C39 C42 H42A 110.0 . . ? N1 C42 H42B 110.0 . . ? C39 C42 H42B 110.0 . . ? H42A C42 H42B 108.4 . . ? C46 C43 N2 103.5(14) . . ? C46 C43 H43A 111.1 . . ? N2 C43 H43A 111.1 . . ? C46 C43 H43B 111.1 . . ? N2 C43 H43B 111.1 . . ? H43A C43 H43B 109.0 . . ? N2 C44 C47 101.5(12) . . ? N2 C44 H44A 111.5 . . ? C47 C44 H44A 111.5 . . ? N2 C44 H44B 111.5 . . ? C47 C44 H44B 111.5 . . ? H44A C44 H44B 109.3 . . ? N2 C45 C48 112.3(15) . . ? N2 C45 H45A 109.1 . . ? C48 C45 H45A 109.1 . . ? N2 C45 H45B 109.1 . . ? C48 C45 H45B 109.1 . . ? H45A C45 H45B 107.9 . . ? N1 C46 C43 112.5(14) . . ? N1 C46 H46A 109.1 . . ? C43 C46 H46A 109.1 . . ? N1 C46 H46B 109.1 . . ? C43 C46 H46B 109.1 . . ? H46A C46 H46B 107.8 . . ? N1 C47 C44 106.6(12) . . ? N1 C47 H47A 110.4 . . ? C44 C47 H47A 110.4 . . ? N1 C47 H47B 110.4 . . ? C44 C47 H47B 110.4 . . ? H47A C47 H47B 108.6 . . ? N1 C48 C45 106.3(13) . . ? N1 C48 H48A 110.5 . . ? C45 C48 H48A 110.5 . . ? N1 C48 H48B 110.5 . . ? C45 C48 H48B 110.5 . . ? H48A C48 H48B 108.7 . . ? N3 C62 C49 102(2) . . ? N3 C62 H62A 111.4 . . ? C49 C62 H62A 111.4 . . ? N3 C62 H62B 111.4 . . ? C49 C62 H62B 111.4 . . ? H62A C62 H62B 109.3 . . ? N4 C49 C62 124(3) . . ? N4 C49 H49A 106.3 . . ? C62 C49 H49A 106.3 . . ? N4 C49 H49B 106.3 . . ? C62 C49 H49B 106.3 . . ? H49A C49 H49B 106.4 . . ? N4 C50 C51 114(3) . . ? N4 C50 H50A 108.8 . . ? C51 C50 H50A 108.8 . . ? N4 C50 H50B 108.8 . . ? C51 C50 H50B 108.8 . . ? H50A C50 H50B 107.7 . . ? N3 C51 C50 108(3) . . ? N3 C51 H51A 110.0 . . ? C50 C51 H51A 110.0 . . ? N3 C51 H51B 110.0 . . ? C50 C51 H51B 110.0 . . ? H51A C51 H51B 108.4 . . ? C53 C52 N4 106.3(17) . . ? C53 C52 H52A 110.5 . . ? N4 C52 H52A 110.5 . . ? C53 C52 H52B 110.5 . . ? N4 C52 H52B 110.5 . . ? H52A C52 H52B 108.7 . . ? C52 C53 N3 113(2) . . ? C52 C53 H53A 109.0 . . ? N3 C53 H53A 109.0 . . ? C52 C53 H53B 109.0 . . ? N3 C53 H53B 109.0 . . ? H53A C53 H53B 107.8 . . ? N3 C54 C55 112(3) . . ? N3 C54 H54A 109.3 . . ? C55 C54 H54A 109.3 . . ? N3 C54 H54B 109.3 . . ? C55 C54 H54B 109.3 . . ? H54A C54 H54B 107.9 . . ? N4 C55 C54 111(3) . . ? N4 C55 H55A 109.5 . . ? C54 C55 H55A 109.5 . . ? N4 C55 H55B 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 108.0 . . ? N3 C56 C57 115(2) . . ? N3 C56 H56A 108.5 . . ? C57 C56 H56A 108.5 . . ? N3 C56 H56B 108.5 . . ? C57 C56 H56B 108.5 . . ? H56A C56 H56B 107.5 . . ? N4 C57 C56 105(2) . . ? N4 C57 H57A 110.8 . . ? C56 C57 H57A 110.8 . . ? N4 C57 H57B 110.8 . . ? C56 C57 H57B 110.8 . . ? H57A C57 H57B 108.9 . . ? N3 C58 C59 114(2) . . ? N3 C58 H58A 108.7 . . ? C59 C58 H58A 108.7 . . ? N3 C58 H58B 108.7 . . ? C59 C58 H58B 108.7 . . ? H58A C58 H58B 107.6 . . ? C58 C59 N4 107(2) . . ? C58 C59 H59A 110.3 . . ? N4 C59 H59A 110.3 . . ? C58 C59 H59B 110.3 . . ? N4 C59 H59B 110.3 . . ? H59A C59 H59B 108.5 . . ? N4 C60 C61 113(2) . . ? N4 C60 H60A 108.9 . . ? C61 C60 H60A 108.9 . . ? N4 C60 H60B 108.9 . . ? C61 C60 H60B 108.9 . . ? H60A C60 H60B 107.7 . . ? N3 C61 C60 109(2) . . ? N3 C61 H61A 110.0 . . ? C60 C61 H61A 110.0 . . ? N3 C61 H61B 110.0 . . ? C60 C61 H61B 110.0 . . ? H61A C61 H61B 108.4 . . ? C32 O7 C33 117.1(10) . . ? C32 C31 H31A 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C32 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O7 C32 C31 116.6(13) . . ? O7 C32 H32A 108.1 . . ? C31 C32 H32A 108.1 . . ? O7 C32 H32B 108.1 . . ? C31 C32 H32B 108.1 . . ? H32A C32 H32B 107.3 . . ? O7 C33 C34 111.1(11) . . ? O7 C33 H33A 109.4 . . ? C34 C33 H33A 109.4 . . ? O7 C33 H33B 109.4 . . ? C34 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 O8 C36 118(4) 4_565 . ? C36 C35 H35A 109.5 . . ? C36 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C36 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O8 C36 C35 121(3) . . ? O8 C36 H36A 107.1 . . ? C35 C36 H36A 107.1 . . ? O8 C36 H36B 107.1 . . ? C35 C36 H36B 107.1 . . ? H36A C36 H36B 106.8 . . ? C47 N1 C41 60.3(9) . . ? C47 N1 C40 130.5(9) . . ? C41 N1 C40 118.0(8) . . ? C47 N1 C48 108.0(11) . . ? C41 N1 C48 135.2(9) . . ? C47 N1 C46 108.0(10) . . ? C41 N1 C46 52.8(8) . . ? C40 N1 C46 70.6(9) . . ? C48 N1 C46 101.5(10) . . ? C41 N1 C42 103.0(7) . . ? C40 N1 C42 100.2(7) . . ? C48 N1 C42 68.4(8) . . ? C46 N1 C42 135.5(8) . . ? C47 N1 Cu1 113.9(7) . . ? C41 N1 Cu1 110.0(5) . . ? C40 N1 Cu1 112.1(6) . . ? C48 N1 Cu1 113.7(7) . . ? C46 N1 Cu1 110.8(7) . . ? C42 N1 Cu1 112.8(5) . . ? C45 N2 C38 134.5(9) . . ? C45 N2 C44 120.7(11) . . ? C38 N2 C44 48.2(8) . . ? C38 N2 C37 109.0(8) . . ? C44 N2 C37 136.0(9) . . ? C45 N2 C39 68.0(9) . . ? C38 N2 C39 106.4(7) . . ? C44 N2 C39 60.9(8) . . ? C37 N2 C39 107.6(7) . . ? C45 N2 C43 105.2(10) . . ? C38 N2 C43 49.9(8) . . ? C44 N2 C43 96.9(10) . . ? C37 N2 C43 65.0(8) . . ? C39 N2 C43 141.2(8) . . ? C62 N3 C56 133.1(14) . . ? C62 N3 C56 133.1(14) . 4_565 ? C56 N3 C56 46(2) . 4_565 ? C62 N3 C61 81.1(12) . . ? C56 N3 C61 62.4(14) . . ? C56 N3 C61 104.8(17) 4_565 . ? C62 N3 C61 81.1(12) . 4_565 ? C56 N3 C61 104.8(17) . 4_565 ? C56 N3 C61 62.4(14) 4_565 4_565 ? C61 N3 C61 136(2) . 4_565 ? C62 N3 C53 114.9(12) . . ? C56 N3 C53 69.5(16) 4_565 . ? C61 N3 C53 123.1(16) 4_565 . ? C62 N3 C53 114.9(12) . 4_565 ? C56 N3 C53 69.5(16) . 4_565 ? C61 N3 C53 123.1(16) . 4_565 ? C53 N3 C53 92(2) . 4_565 ? C62 N3 C54 61.7(11) . . ? C56 N3 C54 80.9(14) . . ? C56 N3 C54 119.8(17) 4_565 . ? C61 N3 C54 128.7(14) 4_565 . ? C53 N3 C54 56.9(13) . . ? C53 N3 C54 132.1(16) 4_565 . ? C62 N3 C54 61.7(11) . 4_565 ? C56 N3 C54 119.8(17) . 4_565 ? C56 N3 C54 80.9(14) 4_565 4_565 ? C61 N3 C54 128.7(14) . 4_565 ? C53 N3 C54 132.1(16) . 4_565 ? C53 N3 C54 56.9(13) 4_565 4_565 ? C54 N3 C54 115(2) . 4_565 ? C62 N3 C51 142.6(18) . . ? C61 N3 C51 85.3(13) . . ? C61 N3 C51 85.3(13) 4_565 . ? C53 N3 C51 48.0(10) . . ? C53 N3 C51 48.0(10) 4_565 . ? C54 N3 C51 103.1(14) . . ? C54 N3 C51 103.1(14) 4_565 . ? C56 N3 C58 134.2(16) . 4_565 ? C56 N3 C58 105.3(13) 4_565 4_565 ? C61 N3 C58 110.3(16) . 4_565 ? C61 N3 C58 46.5(14) 4_565 4_565 ? C53 N3 C58 132.6(14) . 4_565 ? C53 N3 C58 82.7(13) 4_565 4_565 ? C54 N3 C58 92.9(16) . 4_565 ? C51 N3 C58 125.0(15) . 4_565 ? C56 N3 C58 105.3(13) . . ? C56 N3 C58 134.2(16) 4_565 . ? C61 N3 C58 46.5(14) . . ? C61 N3 C58 110.3(16) 4_565 . ? C53 N3 C58 82.7(13) . . ? C53 N3 C58 132.6(14) 4_565 . ? C54 N3 C58 92.9(16) 4_565 . ? C51 N3 C58 125.0(15) . . ? C58 N3 C58 68(2) 4_565 . ? C60 N4 C60 136(2) . 4_565 ? C60 N4 C49 73.9(13) . . ? C60 N4 C49 73.9(13) 4_565 . ? C60 N4 C55 123.8(16) 4_565 . ? C49 N4 C55 53.8(11) . . ? C60 N4 C55 123.8(16) . 4_565 ? C49 N4 C55 53.8(11) . 4_565 ? C55 N4 C55 107(2) . 4_565 ? C60 N4 C57 64.6(16) . . ? C60 N4 C57 115.2(17) 4_565 . ? C49 N4 C57 126.3(14) . . ? C55 N4 C57 85.5(14) . . ? C55 N4 C57 131.3(16) 4_565 . ? C60 N4 C57 115.2(17) . 4_565 ? C60 N4 C57 64.6(16) 4_565 4_565 ? C49 N4 C57 126.3(14) . 4_565 ? C55 N4 C57 131.3(16) . 4_565 ? C55 N4 C57 85.5(14) 4_565 4_565 ? C57 N4 C57 54.9(19) . 4_565 ? C60 N4 C50 88.8(14) . . ? C60 N4 C50 88.8(14) 4_565 . ? C49 N4 C50 128.9(18) . . ? C55 N4 C50 107.5(14) . . ? C55 N4 C50 107.5(14) 4_565 . ? C60 N4 C59 107.9(18) . 4_565 ? C55 N4 C59 88.2(16) . 4_565 ? C57 N4 C59 142.2(15) . 4_565 ? C57 N4 C59 105.8(13) 4_565 4_565 ? C50 N4 C59 124.6(14) . 4_565 ? C60 N4 C59 107.9(18) 4_565 . ? C55 N4 C59 88.2(16) 4_565 . ? C57 N4 C59 105.8(13) . . ? C57 N4 C59 142.2(15) 4_565 . ? C50 N4 C59 124.6(14) . . ? C59 N4 C59 68(2) 4_565 . ? C60 N4 C52 131.0(14) 4_565 . ? C49 N4 C52 90.9(11) . . ? C55 N4 C52 129.8(15) 4_565 . ? C57 N4 C52 91.7(13) 4_565 . ? C50 N4 C52 64.9(10) . . ? C59 N4 C52 121.5(13) 4_565 . ? C59 N4 C52 64.6(12) . . ? C60 N4 C52 131.0(14) . 4_565 ? C49 N4 C52 90.9(11) . 4_565 ? C55 N4 C52 129.8(15) . 4_565 ? C57 N4 C52 91.7(13) . 4_565 ? C50 N4 C52 65.0(10) . 4_565 ? C59 N4 C52 64.6(12) 4_565 4_565 ? C59 N4 C52 121.5(13) . 4_565 ? C52 N4 C52 115.8(16) . 4_565 ? C5 O1 Cu1 127.5(2) . . ? C7 O2 Cu1 126.1(2) . . ? C14 O3 Cu2 125.8(2) . . ? C16 O4 Cu2 126.6(2) . . ? C25 O5 Cu1 126.4(2) . . ? C27 O6 Cu1 125.8(2) . . ? O6 Cu1 O2 87.80(10) . . ? O6 Cu1 O1 179.34(17) . . ? O2 Cu1 O1 91.90(10) . . ? O6 Cu1 O5 92.26(10) . . ? O2 Cu1 O5 179.90(17) . . ? O1 Cu1 O5 88.04(10) . . ? O6 Cu1 N1 88.95(17) . . ? O2 Cu1 N1 88.24(18) . . ? O1 Cu1 N1 91.63(17) . . ? O5 Cu1 N1 91.69(19) . . ? O6 Cu1 N2 113.36(7) . 3 ? O2 Cu1 N2 25.69(7) . 3 ? O1 Cu1 N2 66.32(7) . 3 ? O5 Cu1 N2 154.26(8) . 3 ? N1 Cu1 N2 91.30(13) . 3 ? O3 Cu2 O3 87.46(13) . 4_565 ? O3 Cu2 O4 92.54(10) . . ? O3 Cu2 O4 179.73(18) 4_565 . ? O3 Cu2 O4 179.73(18) . 4_565 ? O3 Cu2 O4 92.54(10) 4_565 4_565 ? O4 Cu2 O4 87.46(14) . 4_565 ? O3 Cu2 N3 88.46(18) . . ? O3 Cu2 N3 88.46(18) 4_565 . ? O4 Cu2 N3 91.81(18) . . ? O4 Cu2 N3 91.81(18) 4_565 . ? O3 Cu2 N4 93.40(8) . 3 ? O3 Cu2 N4 160.21(13) 4_565 3 ? O4 Cu2 N4 19.52(14) . 3 ? O4 Cu2 N4 86.51(9) 4_565 3 ? N3 Cu2 N4 111.33(12) . 3 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 C4 C5 O1 59.3(8) . . . . ? C3 C4 C5 O1 -168.6(6) . . . . ? C1 C4 C5 O1 -56.3(8) . . . . ? C2 C4 C5 C6 -117.8(8) . . . . ? C3 C4 C5 C6 14.3(10) . . . . ? C1 C4 C5 C6 126.6(7) . . . . ? C2 C4 C5 C4A 141(5) . . . . ? C3 C4 C5 C4A -87(4) . . . . ? C1 C4 C5 C4A 25(4) . . . . ? C1A C4A C5 O1 -67.9(11) . . . . ? C3A C4A C5 O1 52.2(10) . . . . ? C2A C4A C5 O1 164.2(8) . . . . ? C1A C4A C5 C6 103.2(11) . . . . ? C3A C4A C5 C6 -136.7(9) . . . . ? C2A C4A C5 C6 -24.6(11) . . . . ? C1A C4A C5 C4 -171(5) . . . . ? C3A C4A C5 C4 -51(4) . . . . ? C2A C4A C5 C4 61(4) . . . . ? O1 C5 C6 C7 -2.6(10) . . . . ? C4 C5 C6 C7 174.2(6) . . . . ? C4A C5 C6 C7 -172.7(7) . . . . ? C5 C6 C7 O2 3.2(11) . . . . ? C5 C6 C7 C8 179.7(6) . . . . ? O2 C7 C8 C9A 168.3(7) . . . . ? C6 C7 C8 C9A -8.6(10) . . . . ? O2 C7 C8 C13A -13.9(10) . . . . ? C6 C7 C8 C13A 169.2(8) . . . . ? O2 C7 C8 C9 -158.0(6) . . . . ? C6 C7 C8 C9 25.1(9) . . . . ? O2 C7 C8 C13 20.8(9) . . . . ? C6 C7 C8 C13 -156.1(6) . . . . ? C9A C8 C9 C10 -84.8(15) . . . . ? C13A C8 C9 C10 31.3(9) . . . . ? C13 C8 C9 C10 -1.9(9) . . . . ? C7 C8 C9 C10 176.9(6) . . . . ? C8 C9 C10 C11 1.6(9) . . . . ? C11 C12 C13 C8 2.8(12) . . . . ? C9A C8 C13 C12 30.0(11) . . . . ? C13A C8 C13 C12 -83.9(15) . . . . ? C9 C8 C13 C12 -0.4(11) . . . . ? C7 C8 C13 C12 -179.2(7) . . . . ? C13A C8 C9A C10A -1.0(11) . . . . ? C9 C8 C9A C10A 76.4(15) . . . . ? C13 C8 C9A C10A -34.1(10) . . . . ? C7 C8 C9A C10A 176.7(8) . . . . ? C8 C9A C10A C11 6.0(13) . . . . ? C9A C8 C13A C12A -5.8(15) . . . . ? C9 C8 C13A C12A -35.5(13) . . . . ? C13 C8 C13A C12A 75.5(16) . . . . ? C7 C8 C13A C12A 176.4(9) . . . . ? C11 C12A C13A C8 8.0(17) . . . . ? C9 C10 C11 C12A -29.9(10) . . . . ? C9 C10 C11 C10A 77.9(15) . . . . ? C9 C10 C11 C12 0.8(10) . . . . ? C9 C10 C11 C14 -178.6(6) . . . . ? C13A C12A C11 C10 25.1(14) . . . . ? C13A C12A C11 C10A -3.2(16) . . . . ? C13A C12A C11 C12 -85.6(17) . . . . ? C13A C12A C11 C14 175.3(9) . . . . ? C9A C10A C11 C10 -88.5(18) . . . . ? C9A C10A C11 C12A -3.9(15) . . . . ? C9A C10A C11 C12 26.3(12) . . . . ? C9A C10A C11 C14 177.7(8) . . . . ? C13 C12 C11 C10 -3.1(11) . . . . ? C13 C12 C11 C12A 80.0(15) . . . . ? C13 C12 C11 C10A -30.4(11) . . . . ? C13 C12 C11 C14 176.4(7) . . . . ? C10 C11 C14 O3 158.0(6) . . . . ? C12A C11 C14 O3 10.7(10) . . . . ? C10A C11 C14 O3 -170.8(8) . . . . ? C12 C11 C14 O3 -21.5(8) . . . . ? C10 C11 C14 C15 -27.6(9) . . . . ? C12A C11 C14 C15 -174.8(7) . . . . ? C10A C11 C14 C15 3.6(10) . . . . ? C12 C11 C14 C15 153.0(6) . . . . ? O3 C14 C15 C16 -5.2(10) . . . . ? C11 C14 C15 C16 -179.0(6) . . . . ? C14 C15 C16 O4 2.2(11) . . . . ? C14 C15 C16 C17 -174.2(6) . . . . ? C14 C15 C16 C17A 172.5(8) . . . . ? O4 C16 C17 C18 -59.4(8) . . . . ? C15 C16 C17 C18 117.3(7) . . . . ? C17A C16 C17 C18 -147(6) . . . . ? O4 C16 C17 C20 172.3(6) . . . . ? C15 C16 C17 C20 -11.0(10) . . . . ? C17A C16 C17 C20 85(5) . . . . ? O4 C16 C17 C19 58.5(8) . . . . ? C15 C16 C17 C19 -124.8(7) . . . . ? C17A C16 C17 C19 -29(5) . . . . ? O4 C16 C17A C18A 67.4(14) . . . . ? C15 C16 C17A C18A -104.0(13) . . . . ? C17 C16 C17A C18A 165(6) . . . . ? O4 C16 C17A C20A -162.2(10) . . . . ? C15 C16 C17A C20A 26.5(14) . . . . ? C17 C16 C17A C20A -64(5) . . . . ? O4 C16 C17A C19A -51.8(12) . . . . ? C15 C16 C17A C19A 136.8(10) . . . . ? C17 C16 C17A C19A 46(5) . . . . ? C21 C24 C25 O5 -59.6(10) . . . . ? C23 C24 C25 O5 166.6(8) . . . . ? C22 C24 C25 O5 56.5(9) . . . . ? C21 C24 C25 C26 112.3(9) . . . . ? C23 C24 C25 C26 -21.4(12) . . . . ? C22 C24 C25 C26 -131.6(8) . . . . ? C21 C24 C25 C24A -152(3) . . . . ? C23 C24 C25 C24A 74(2) . . . . ? C22 C24 C25 C24A -36(2) . . . . ? C21A C24A C25 O5 -44.3(9) . . . . ? C22A C24A C25 O5 73.6(10) . . . . ? C23A C24A C25 O5 -157.9(8) . . . . ? C21A C24A C25 C26 146.5(8) . . . . ? C22A C24A C25 C26 -95.6(10) . . . . ? C23A C24A C25 C26 33.0(11) . . . . ? C21A C24A C25 C24 51(2) . . . . ? C22A C24A C25 C24 169(3) . . . . ? C23A C24A C25 C24 -63(2) . . . . ? O5 C25 C26 C27 -1.3(12) . . . . ? C24 C25 C26 C27 -172.1(7) . . . . ? C24A C25 C26 C27 166.4(7) . . . . ? C25 C26 C27 O6 2.1(10) . . . . ? C25 C26 C27 C28 -178.0(6) . . . . ? O6 C27 C28 C29 -1.3(11) . . . . ? C26 C27 C28 C29 178.7(9) . . . . ? O6 C27 C28 C30A -156.0(5) . . . . ? C26 C27 C28 C30A 24.1(8) . . . . ? O6 C27 C28 C30 158.3(7) . . . . ? C26 C27 C28 C30 -21.7(9) . . . . ? O6 C27 C28 C29A 26.4(8) . . . . ? C26 C27 C28 C29A -153.5(6) . . . . ? C29 C28 C30 C30 -17.4(10) . . . 4_565 ? C30A C28 C30 C30 76.6(9) . . . 4_565 ? C29A C28 C30 C30 -41.2(6) . . . 4_565 ? C27 C28 C30 C30 -177.7(3) . . . 4_565 ? C30A C28 C29 C29 -24.7(9) . . . 4_565 ? C30 C28 C29 C29 17.9(10) . . . 4_565 ? C29A C28 C29 C29 87.4(18) . . . 4_565 ? C27 C28 C29 C29 178.3(3) . . . 4_565 ? C29 C28 C30A C30A 24.4(9) . . . 4_565 ? C30 C28 C30A C30A -80.2(10) . . . 4_565 ? C29A C28 C30A C30A -1.8(6) . . . 4_565 ? C27 C28 C30A C30A -179.4(3) . . . 4_565 ? C29 C28 C29A C29A -77.9(18) . . . 4_565 ? C30A C28 C29A C29A 1.8(6) . . . 4_565 ? C30 C28 C29A C29A 41.4(7) . . . 4_565 ? C27 C28 C29A C29A 179.5(3) . . . 4_565 ? N2 C37 C40 N1 12.2(16) . . . . ? N2 C38 C41 N1 29.9(12) . . . . ? N2 C39 C42 N1 24.2(11) . . . . ? N2 C43 C46 N1 24.4(17) . . . . ? N2 C44 C47 N1 48.4(14) . . . . ? N2 C45 C48 N1 26.7(19) . . . . ? N3 C62 C49 N4 0.000(5) . . . . ? N4 C50 C51 N3 0.000(8) . . . . ? N4 C52 C53 N3 -39(2) . . . . ? N3 C54 C55 N4 -11(3) . . . . ? N3 C56 C57 N4 -7(3) . . . . ? N3 C58 C59 N4 -1(3) . . . . ? N4 C60 C61 N3 -8(4) . . . . ? C33 O7 C32 C31 171.1(17) . . . . ? C32 O7 C33 C34 173.5(16) . . . . ? C36 O8 C36 C35 178.8(19) 4_565 . . . ? C44 C47 N1 C41 51.5(10) . . . . ? C44 C47 N1 C40 -51.3(17) . . . . ? C44 C47 N1 C48 -80.8(13) . . . . ? C44 C47 N1 C46 28.2(14) . . . . ? C44 C47 N1 C42 -109.3(15) . . . . ? C44 C47 N1 Cu1 151.8(8) . . . . ? C38 C41 N1 C47 -90.2(11) . . . . ? C38 C41 N1 C40 32.7(12) . . . . ? C38 C41 N1 C48 -4.2(18) . . . . ? C38 C41 N1 C46 61.6(11) . . . . ? C38 C41 N1 C42 -76.5(10) . . . . ? C38 C41 N1 Cu1 163.0(7) . . . . ? C37 C40 N1 C47 17.6(18) . . . . ? C37 C40 N1 C41 -55.9(14) . . . . ? C37 C40 N1 C48 74.7(17) . . . . ? C37 C40 N1 C46 -79.9(13) . . . . ? C37 C40 N1 C42 54.9(12) . . . . ? C37 C40 N1 Cu1 174.8(9) . . . . ? C45 C48 N1 C47 39.7(17) . . . . ? C45 C48 N1 C41 -26(2) . . . . ? C45 C48 N1 C40 -98(2) . . . . ? C45 C48 N1 C46 -73.7(15) . . . . ? C45 C48 N1 C42 60.9(13) . . . . ? C45 C48 N1 Cu1 167.2(10) . . . . ? C43 C46 N1 C47 -69.1(16) . . . . ? C43 C46 N1 C41 -94.7(15) . . . . ? C43 C46 N1 C40 58.4(13) . . . . ? C43 C46 N1 C48 44.4(15) . . . . ? C43 C46 N1 C42 -26(2) . . . . ? C43 C46 N1 Cu1 165.5(11) . . . . ? C39 C42 N1 C47 63.3(12) . . . . ? C39 C42 N1 C41 46.3(10) . . . . ? C39 C42 N1 C40 -75.8(10) . . . . ? C39 C42 N1 C48 -87.5(11) . . . . ? C39 C42 N1 C46 -3.1(16) . . . . ? C39 C42 N1 Cu1 164.8(7) . . . . ? C48 C45 N2 C38 -1(2) . . . . ? C48 C45 N2 C44 -60.7(19) . . . . ? C48 C45 N2 C37 65.4(15) . . . . ? C48 C45 N2 C39 -92.5(15) . . . . ? C48 C45 N2 C43 47.1(17) . . . . ? C41 C38 N2 C45 -31.1(18) . . . . ? C41 C38 N2 C44 63.6(12) . . . . ? C41 C38 N2 C37 -71.9(11) . . . . ? C41 C38 N2 C39 43.8(10) . . . . ? C41 C38 N2 C43 -100.8(13) . . . . ? C47 C44 N2 C45 21.0(17) . . . . ? C47 C44 N2 C38 -103.3(14) . . . . ? C47 C44 N2 C37 -30.6(19) . . . . ? C47 C44 N2 C39 54.9(10) . . . . ? C47 C44 N2 C43 -91.3(12) . . . . ? C40 C37 N2 C45 -88.2(16) . . . . ? C40 C37 N2 C38 48.1(13) . . . . ? C40 C37 N2 C44 -1(2) . . . . ? C40 C37 N2 C39 -66.8(13) . . . . ? C40 C37 N2 C43 72.2(13) . . . . ? C42 C39 N2 C45 59.9(11) . . . . ? C42 C39 N2 C38 -72.2(10) . . . . ? C42 C39 N2 C44 -88.9(11) . . . . ? C42 C39 N2 C37 44.5(10) . . . . ? C42 C39 N2 C43 -27.2(17) . . . . ? C46 C43 N2 C45 -74.6(14) . . . . ? C46 C43 N2 C38 61.6(12) . . . . ? C46 C43 N2 C44 49.9(13) . . . . ? C46 C43 N2 C37 -88.1(13) . . . . ? C46 C43 N2 C39 -1(2) . . . . ? C49 C62 N3 C56 32.1(16) . . . . ? C49 C62 N3 C56 -32.1(16) . . . 4_565 ? C49 C62 N3 C61 69.9(11) . . . . ? C49 C62 N3 C61 -69.9(11) . . . 4_565 ? C49 C62 N3 C53 52.6(12) . . . . ? C49 C62 N3 C53 -52.6(12) . . . 4_565 ? C49 C62 N3 C54 73.6(14) . . . . ? C49 C62 N3 C54 -73.6(14) . . . 4_565 ? C49 C62 N3 C51 0.000(11) . . . . ? C49 C62 N3 C58 -77(2) . . . 4_565 ? C49 C62 N3 C58 77(2) . . . . ? C57 C56 N3 C62 -29(3) . . . . ? C57 C56 N3 C56 84(2) . . . 4_565 ? C57 C56 N3 C61 -72(2) . . . . ? C57 C56 N3 C61 62(2) . . . 4_565 ? C57 C56 N3 C53 -79(4) . . . . ? C57 C56 N3 C53 76(2) . . . 4_565 ? C57 C56 N3 C54 -66(2) . . . . ? C57 C56 N3 C54 48(3) . . . 4_565 ? C57 C56 N3 C51 96(6) . . . . ? C57 C56 N3 C58 20(3) . . . 4_565 ? C57 C56 N3 C58 -54(2) . . . . ? C60 C61 N3 C62 -70(2) . . . . ? C60 C61 N3 C56 79(3) . . . . ? C60 C61 N3 C56 62(3) . . . 4_565 ? C60 C61 N3 C61 -3(5) . . . 4_565 ? C60 C61 N3 C53 83(3) . . . . ? C60 C61 N3 C53 44(3) . . . 4_565 ? C60 C61 N3 C54 -80(6) . . . . ? C60 C61 N3 C54 -28(4) . . . 4_565 ? C60 C61 N3 C51 75(3) . . . . ? C60 C61 N3 C58 -51(3) . . . 4_565 ? C60 C61 N3 C58 -76(3) . . . . ? C52 C53 N3 C62 -31(2) . . . . ? C52 C53 N3 C56 112(5) . . . . ? C52 C53 N3 C56 98(2) . . . 4_565 ? C52 C53 N3 C61 -59(2) . . . . ? C52 C53 N3 C61 65(3) . . . 4_565 ? C52 C53 N3 C53 88(2) . . . 4_565 ? C52 C53 N3 C54 -52.9(19) . . . . ? C52 C53 N3 C54 43(3) . . . 4_565 ? C52 C53 N3 C51 109(3) . . . . ? C52 C53 N3 C58 6(3) . . . 4_565 ? C52 C53 N3 C58 -45(2) . . . . ? C55 C54 N3 C62 -75(2) . . . . ? C55 C54 N3 C56 76(2) . . . . ? C55 C54 N3 C56 51(3) . . . 4_565 ? C55 C54 N3 C61 94(6) . . . . ? C55 C54 N3 C61 -26(4) . . . 4_565 ? C55 C54 N3 C53 82(2) . . . . ? C55 C54 N3 C53 24(4) . . . 4_565 ? C55 C54 N3 C54 -43(4) . . . 4_565 ? C55 C54 N3 C51 68(3) . . . . ? C55 C54 N3 C58 -59(3) . . . 4_565 ? C55 C54 N3 C58 -79(4) . . . . ? C50 C51 N3 C62 0.000(11) . . . . ? C50 C51 N3 C56 -79(6) . . . . ? C50 C51 N3 C56 79(6) . . . 4_565 ? C50 C51 N3 C61 -68.6(11) . . . . ? C50 C51 N3 C61 68.6(11) . . . 4_565 ? C50 C51 N3 C53 -75.8(17) . . . . ? C50 C51 N3 C53 75.8(17) . . . 4_565 ? C50 C51 N3 C54 -60.1(12) . . . . ? C50 C51 N3 C54 60.1(12) . . . 4_565 ? C50 C51 N3 C58 43.0(14) . . . 4_565 ? C50 C51 N3 C58 -43.0(14) . . . . ? C59 C58 N3 C62 -90(3) . . . . ? C59 C58 N3 C56 58(3) . . . . ? C59 C58 N3 C56 16(4) . . . 4_565 ? C59 C58 N3 C61 80(3) . . . . ? C59 C58 N3 C61 -55(3) . . . 4_565 ? C59 C58 N3 C53 68(2) . . . . ? C59 C58 N3 C53 -18(4) . . . 4_565 ? C59 C58 N3 C54 83(4) . . . . ? C59 C58 N3 C54 -64(3) . . . 4_565 ? C59 C58 N3 C51 44(3) . . . . ? C59 C58 N3 C58 -74(3) . . . 4_565 ? C61 C60 N4 C60 25(6) . . . 4_565 ? C61 C60 N4 C49 69(3) . . . . ? C61 C60 N4 C55 89(6) . . . . ? C61 C60 N4 C55 49(4) . . . 4_565 ? C61 C60 N4 C57 -76(3) . . . . ? C61 C60 N4 C57 -54(3) . . . 4_565 ? C61 C60 N4 C50 -62(3) . . . . ? C61 C60 N4 C59 64(3) . . . 4_565 ? C61 C60 N4 C59 87(3) . . . . ? C61 C60 N4 C52 -64(4) . . . . ? C61 C60 N4 C52 -7(4) . . . 4_565 ? C62 C49 N4 C60 -74.8(13) . . . . ? C62 C49 N4 C60 74.8(13) . . . 4_565 ? C62 C49 N4 C55 -83.6(17) . . . . ? C62 C49 N4 C55 83.6(17) . . . 4_565 ? C62 C49 N4 C57 -34.9(13) . . . . ? C62 C49 N4 C57 34.9(13) . . . 4_565 ? C62 C49 N4 C50 0.000(9) . . . . ? C62 C49 N4 C59 97(3) . . . 4_565 ? C62 C49 N4 C59 -97(3) . . . . ? C62 C49 N4 C52 -57.9(8) . . . . ? C62 C49 N4 C52 57.9(8) . . . 4_565 ? C54 C55 N4 C60 -81(6) . . . . ? C54 C55 N4 C60 51(3) . . . 4_565 ? C54 C55 N4 C49 76(3) . . . . ? C54 C55 N4 C55 65(3) . . . 4_565 ? C54 C55 N4 C57 -67(2) . . . . ? C54 C55 N4 C57 -34(3) . . . 4_565 ? C54 C55 N4 C50 -50(3) . . . . ? C54 C55 N4 C59 76(3) . . . 4_565 ? C54 C55 N4 C59 96(6) . . . . ? C54 C55 N4 C52 -66(2) . . . . ? C54 C55 N4 C52 22(3) . . . 4_565 ? C56 C57 N4 C60 78(2) . . . . ? C56 C57 N4 C60 -53(2) . . . 4_565 ? C56 C57 N4 C49 35(2) . . . . ? C56 C57 N4 C55 73(2) . . . . ? C56 C57 N4 C55 -36(3) . . . 4_565 ? C56 C57 N4 C57 -77.2(19) . . . 4_565 ? C56 C57 N4 C50 -71(4) . . . . ? C56 C57 N4 C59 -9(4) . . . 4_565 ? C56 C57 N4 C59 66(2) . . . . ? C56 C57 N4 C52 71(2) . . . . ? C56 C57 N4 C52 -57(2) . . . 4_565 ? C51 C50 N4 C60 68.0(12) . . . . ? C51 C50 N4 C60 -68.0(12) . . . 4_565 ? C51 C50 N4 C49 0.000(9) . . . . ? C51 C50 N4 C55 57.2(13) . . . . ? C51 C50 N4 C55 -57.2(13) . . . 4_565 ? C51 C50 N4 C57 96(4) . . . . ? C51 C50 N4 C57 -96(4) . . . 4_565 ? C51 C50 N4 C59 -43.0(14) . . . 4_565 ? C51 C50 N4 C59 43.0(14) . . . . ? C51 C50 N4 C52 69.2(10) . . . . ? C51 C50 N4 C52 -69.2(10) . . . 4_565 ? C58 C59 N4 C60 -80(3) . . . . ? C58 C59 N4 C60 60(3) . . . 4_565 ? C58 C59 N4 C49 68(3) . . . . ? C58 C59 N4 C55 -82(5) . . . . ? C58 C59 N4 C55 68(2) . . . 4_565 ? C58 C59 N4 C57 -64(2) . . . . ? C58 C59 N4 C57 -12(4) . . . 4_565 ? C58 C59 N4 C50 -42(3) . . . . ? C58 C59 N4 C59 76(2) . . . 4_565 ? C58 C59 N4 C52 -68(2) . . . . ? C58 C59 N4 C52 38(3) . . . 4_565 ? C53 C52 N4 C60 122(4) . . . . ? C53 C52 N4 C60 9(3) . . . 4_565 ? C53 C52 N4 C49 78(2) . . . . ? C53 C52 N4 C55 109(3) . . . . ? C53 C52 N4 C55 38(3) . . . 4_565 ? C53 C52 N4 C57 -73(2) . . . . ? C53 C52 N4 C57 -48(2) . . . 4_565 ? C53 C52 N4 C50 -55(2) . . . . ? C53 C52 N4 C59 62(3) . . . 4_565 ? C53 C52 N4 C59 101(2) . . . . ? C53 C52 N4 C52 -13(3) . . . 4_565 ? C6 C5 O1 Cu1 2.0(9) . . . . ? C4 C5 O1 Cu1 -175.0(4) . . . . ? C4A C5 O1 Cu1 172.8(5) . . . . ? C6 C7 O2 Cu1 -2.9(9) . . . . ? C8 C7 O2 Cu1 -179.6(4) . . . . ? C15 C14 O3 Cu2 4.8(9) . . . . ? C11 C14 O3 Cu2 178.8(4) . . . . ? C15 C16 O4 Cu2 0.7(9) . . . . ? C17 C16 O4 Cu2 177.3(4) . . . . ? C17A C16 O4 Cu2 -170.2(6) . . . . ? C26 C25 O5 Cu1 -0.1(10) . . . . ? C24 C25 O5 Cu1 171.4(5) . . . . ? C24A C25 O5 Cu1 -168.6(5) . . . . ? C26 C27 O6 Cu1 -1.4(8) . . . . ? C28 C27 O6 Cu1 178.7(3) . . . . ? C27 O6 Cu1 O2 -179.9(5) . . . . ? C27 O6 Cu1 O5 0.1(5) . . . . ? C27 O6 Cu1 N1 91.8(5) . . . . ? C27 O6 Cu1 N2 -177.2(4) . . . 3 ? C7 O2 Cu1 O6 -178.8(5) . . . . ? C7 O2 Cu1 O1 1.8(5) . . . . ? C7 O2 Cu1 N1 -89.8(5) . . . . ? C7 O2 Cu1 N2 6.9(4) . . . 3 ? C5 O1 Cu1 O2 -1.4(5) . . . . ? C5 O1 Cu1 O5 178.6(5) . . . . ? C5 O1 Cu1 N1 86.9(5) . . . . ? C5 O1 Cu1 N2 -3.8(4) . . . 3 ? C25 O5 Cu1 O6 0.6(6) . . . . ? C25 O5 Cu1 O1 180.0(6) . . . . ? C25 O5 Cu1 N1 -88.5(6) . . . . ? C25 O5 Cu1 N2 175.0(4) . . . 3 ? C47 N1 Cu1 O6 133.9(9) . . . . ? C41 N1 Cu1 O6 -160.6(6) . . . . ? C40 N1 Cu1 O6 -27.3(7) . . . . ? C48 N1 Cu1 O6 9.5(9) . . . . ? C46 N1 Cu1 O6 -104.0(8) . . . . ? C42 N1 Cu1 O6 85.0(5) . . . . ? C47 N1 Cu1 O2 46.1(9) . . . . ? C41 N1 Cu1 O2 111.5(6) . . . . ? C40 N1 Cu1 O2 -115.1(7) . . . . ? C48 N1 Cu1 O2 -78.3(9) . . . . ? C46 N1 Cu1 O2 168.1(8) . . . . ? C42 N1 Cu1 O2 -2.9(5) . . . . ? C47 N1 Cu1 O1 -45.8(9) . . . . ? C41 N1 Cu1 O1 19.7(6) . . . . ? C40 N1 Cu1 O1 153.0(7) . . . . ? C48 N1 Cu1 O1 -170.2(9) . . . . ? C46 N1 Cu1 O1 76.3(8) . . . . ? C42 N1 Cu1 O1 -94.7(5) . . . . ? C47 N1 Cu1 O5 -133.8(9) . . . . ? C41 N1 Cu1 O5 -68.4(6) . . . . ? C40 N1 Cu1 O5 64.9(7) . . . . ? C48 N1 Cu1 O5 101.8(9) . . . . ? C46 N1 Cu1 O5 -11.8(8) . . . . ? C42 N1 Cu1 O5 177.2(5) . . . . ? C47 N1 Cu1 N2 20.6(9) . . . 3 ? C41 N1 Cu1 N2 86.0(6) . . . 3 ? C40 N1 Cu1 N2 -140.6(7) . . . 3 ? C48 N1 Cu1 N2 -103.8(9) . . . 3 ? C46 N1 Cu1 N2 142.6(8) . . . 3 ? C42 N1 Cu1 N2 -28.4(5) . . . 3 ? C14 O3 Cu2 O3 178.0(4) . . . 4_565 ? C14 O3 Cu2 O4 -1.7(5) . . . . ? C14 O3 Cu2 N3 -93.5(5) . . . . ? C14 O3 Cu2 N4 17.8(5) . . . 3 ? C16 O4 Cu2 O3 -0.9(5) . . . . ? C16 O4 Cu2 O4 179.4(4) . . . 4_565 ? C16 O4 Cu2 N3 87.6(5) . . . . ? C16 O4 Cu2 N4 -93.9(6) . . . 3 ? C62 N3 Cu2 O3 -43.75(7) . . . . ? C56 N3 Cu2 O3 111.9(10) . . . . ? C56 N3 Cu2 O3 160.6(11) 4_565 . . . ? C61 N3 Cu2 O3 44.6(13) . . . . ? C61 N3 Cu2 O3 -132.1(13) 4_565 . . . ? C53 N3 Cu2 O3 85.5(11) . . . . ? C53 N3 Cu2 O3 -173.0(11) 4_565 . . . ? C54 N3 Cu2 O3 23.3(12) . . . . ? C54 N3 Cu2 O3 -110.8(12) 4_565 . . . ? C51 N3 Cu2 O3 136.25(7) . . . . ? C58 N3 Cu2 O3 -81.5(11) 4_565 . . . ? C58 N3 Cu2 O3 -6.1(11) . . . . ? C62 N3 Cu2 O3 43.75(7) . . . 4_565 ? C56 N3 Cu2 O3 -160.6(11) . . . 4_565 ? C56 N3 Cu2 O3 -111.9(10) 4_565 . . 4_565 ? C61 N3 Cu2 O3 132.1(13) . . . 4_565 ? C61 N3 Cu2 O3 -44.6(13) 4_565 . . 4_565 ? C53 N3 Cu2 O3 173.0(11) . . . 4_565 ? C53 N3 Cu2 O3 -85.5(11) 4_565 . . 4_565 ? C54 N3 Cu2 O3 110.8(12) . . . 4_565 ? C54 N3 Cu2 O3 -23.3(12) 4_565 . . 4_565 ? C51 N3 Cu2 O3 -136.25(7) . . . 4_565 ? C58 N3 Cu2 O3 6.1(11) 4_565 . . 4_565 ? C58 N3 Cu2 O3 81.5(11) . . . 4_565 ? C62 N3 Cu2 O4 -136.24(7) . . . . ? C56 N3 Cu2 O4 19.4(11) . . . . ? C56 N3 Cu2 O4 68.1(10) 4_565 . . . ? C61 N3 Cu2 O4 -47.9(13) . . . . ? C61 N3 Cu2 O4 135.4(13) 4_565 . . . ? C53 N3 Cu2 O4 -7.0(11) . . . . ? C53 N3 Cu2 O4 94.5(11) 4_565 . . . ? C54 N3 Cu2 O4 -69.2(12) . . . . ? C54 N3 Cu2 O4 156.7(12) 4_565 . . . ? C51 N3 Cu2 O4 43.76(7) . . . . ? C58 N3 Cu2 O4 -173.9(11) 4_565 . . . ? C58 N3 Cu2 O4 -98.5(11) . . . . ? C62 N3 Cu2 O4 136.24(7) . . . 4_565 ? C56 N3 Cu2 O4 -68.1(10) . . . 4_565 ? C56 N3 Cu2 O4 -19.4(11) 4_565 . . 4_565 ? C61 N3 Cu2 O4 -135.4(13) . . . 4_565 ? C61 N3 Cu2 O4 47.9(13) 4_565 . . 4_565 ? C53 N3 Cu2 O4 -94.5(11) . . . 4_565 ? C53 N3 Cu2 O4 7.0(11) 4_565 . . 4_565 ? C54 N3 Cu2 O4 -156.7(12) . . . 4_565 ? C54 N3 Cu2 O4 69.2(12) 4_565 . . 4_565 ? C51 N3 Cu2 O4 -43.76(7) . . . 4_565 ? C58 N3 Cu2 O4 98.5(11) 4_565 . . 4_565 ? C58 N3 Cu2 O4 173.9(11) . . . 4_565 ? C62 N3 Cu2 N4 -136.80(5) . . . 3 ? C56 N3 Cu2 N4 18.8(11) . . . 3 ? C56 N3 Cu2 N4 67.6(10) 4_565 . . 3 ? C61 N3 Cu2 N4 -48.4(13) . . . 3 ? C61 N3 Cu2 N4 134.8(13) 4_565 . . 3 ? C53 N3 Cu2 N4 -7.6(11) . . . 3 ? C53 N3 Cu2 N4 94.0(11) 4_565 . . 3 ? C54 N3 Cu2 N4 -69.7(13) . . . 3 ? C54 N3 Cu2 N4 156.1(12) 4_565 . . 3 ? C51 N3 Cu2 N4 43.20(5) . . . 3 ? C58 N3 Cu2 N4 -174.5(11) 4_565 . . 3 ? C58 N3 Cu2 N4 -99.1(12) . . . 3 ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.726 _refine_diff_density_min -0.847 _refine_diff_density_rms 0.111 # Attachment '(6)Cu3L3hmtnew.cif' data_lflj60c _database_code_depnum_ccdc_archive 'CCDC 292069' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H72 Cu3 N4 O12' _chemical_formula_sum 'C60 H72 Cu3 N4 O12' _chemical_formula_weight 1231.23 _chemical_absolute_configuration ad 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 Cubic _symmetry_space_group_name_H-M P213 _symmetry_space_group_name_Hall 'P 2ac 2ab 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' 'z, x, y' 'y, z, x' '-z+1/2, -x, y+1/2' '-y, z+1/2, -x+1/2' 'z+1/2, -x+1/2, -y' '-y+1/2, -z, x+1/2' '-z, x+1/2, -y+1/2' 'y+1/2, -z+1/2, -x' _cell_length_a 18.206(1) _cell_length_b 18.206(1) _cell_length_c 18.206(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6034.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7250 _cell_measurement_theta_min 2.2375 _cell_measurement_theta_max 19.9935 _exptl_crystal_description tetrahedron _exptl_crystal_colour green _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.356 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2572 _exptl_absorpt_coefficient_mu 1.110 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 25 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 49783 _diffrn_reflns_av_R_equivalents 0.1051 _diffrn_reflns_av_sigmaI/netI 0.0880 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 28.30 _reflns_number_total 4995 _reflns_number_gt 2903 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT and XPREP (Siemens, 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEP-3 (Farrugia, 1997) WINGX-32 (Farrugia, 1999) ; _computing_publication_material 'enCIFer 1.0 (CCDC, 2003)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0814P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(2) _refine_ls_number_reflns 4995 _refine_ls_number_parameters 219 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1040 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1394 _refine_ls_wR_factor_gt 0.1246 _refine_ls_goodness_of_fit_ref 0.900 _refine_ls_restrained_S_all 0.921 _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 0.0756(6) 0.1585(6) 0.4742(6) 0.0741(12) Uiso 0.60 1 d PD A 1 H1A H 0.1057 0.1419 0.4328 0.111 Uiso 0.60 1 calc PR A 1 H1B H 0.0247 0.1649 0.4580 0.111 Uiso 0.60 1 calc PR A 1 H1C H 0.0774 0.1217 0.5135 0.111 Uiso 0.60 1 calc PR A 1 C2 C 0.0989(6) 0.2157(6) 0.4967(6) 0.0741(12) Uiso 0.60 1 d PD A 1 H2A H 0.0967 0.2515 0.4558 0.089 Uiso 0.60 1 calc PR A 1 H2B H 0.1514 0.2085 0.5088 0.089 Uiso 0.60 1 calc PR A 1 C3 C 0.0640(6) 0.2494(7) 0.5599(6) 0.0741(12) Uiso 0.60 1 d PD A 1 H3A H 0.0122 0.2603 0.5475 0.089 Uiso 0.60 1 calc PR A 1 H3B H 0.0887 0.2967 0.5703 0.089 Uiso 0.60 1 calc PR A 1 C1A C -0.0050(9) 0.0814(8) 0.5044(9) 0.0741(12) Uiso 0.40 1 d PD A 2 H1A1 H -0.0038 0.0436 0.4661 0.111 Uiso 0.40 1 calc PR A 2 H1A2 H -0.0560 0.0956 0.5140 0.111 Uiso 0.40 1 calc PR A 2 H1A3 H 0.0170 0.0618 0.5495 0.111 Uiso 0.40 1 calc PR A 2 C2A C 0.0317(10) 0.1381(8) 0.4829(9) 0.0741(12) Uiso 0.40 1 d PD A 2 H2A1 H 0.0073 0.1566 0.4380 0.089 Uiso 0.40 1 calc PR A 2 H2A2 H 0.0809 0.1203 0.4678 0.089 Uiso 0.40 1 calc PR A 2 C3A C 0.0452(10) 0.2100(9) 0.5372(9) 0.0741(12) Uiso 0.40 1 d PD A 2 H3A1 H 0.0878 0.2384 0.5190 0.089 Uiso 0.40 1 calc PR A 2 H3A2 H 0.0015 0.2423 0.5351 0.089 Uiso 0.40 1 calc PR A 2 C4 C 0.0657(9) 0.2030(8) 0.6284(9) 0.0741(12) Uiso 0.60 1 d P A 1 C5 C 0.0100(9) 0.2062(8) 0.6805(8) 0.0741(12) Uiso 0.60 1 d P A 1 H5 H -0.0294 0.2392 0.6716 0.089 Uiso 0.60 1 calc PR A 1 C4A C 0.0592(15) 0.1873(12) 0.6180(14) 0.0741(12) Uiso 0.40 1 d P A 2 C5A C 0.0005(14) 0.1889(11) 0.6702(13) 0.0741(12) Uiso 0.40 1 d P A 2 H5A H -0.0459 0.2069 0.6545 0.089 Uiso 0.40 1 calc PR A 2 C6 C 0.0076(3) 0.1653(3) 0.7440(3) 0.0463(12) Uani 1 1 d . . . C7 C -0.0549(3) 0.1734(3) 0.7950(3) 0.0427(11) Uani 1 1 d . A . C8 C -0.0636(3) 0.1243(3) 0.8536(3) 0.0580(15) Uani 1 1 d . . . H8 H -0.0288 0.0859 0.8600 0.070 Uiso 1 1 calc R A . C9 C -0.1203(3) 0.1301(3) 0.9015(3) 0.0599(15) Uani 1 1 d . A . H9 H -0.1250 0.0950 0.9397 0.072 Uiso 1 1 calc R . . C10 C -0.1719(3) 0.1866(2) 0.8959(3) 0.0396(11) Uani 1 1 d . . . C11 C -0.1632(3) 0.2353(3) 0.8393(3) 0.0561(14) Uani 1 1 d . A . H11 H -0.1970 0.2747 0.8341 0.067 Uiso 1 1 calc R . . C12 C -0.1057(3) 0.2285(3) 0.7891(3) 0.0590(15) Uani 1 1 d . . . H12 H -0.1018 0.2629 0.7500 0.071 Uiso 1 1 calc R A . C13 C -0.2322(2) 0.1912(2) 0.9510(3) 0.0365(11) Uani 1 1 d . A . C14 C -0.2947(3) 0.2343(3) 0.9363(3) 0.0462(12) Uani 1 1 d . . . H14 H -0.2960 0.2610 0.8915 0.055 Uiso 1 1 calc R A . C15 C -0.3554(3) 0.2402(3) 0.9836(3) 0.0444(11) Uani 1 1 d . A . C16 C -0.4184(3) 0.2864(3) 0.9604(3) 0.0667(13) Uiso 0.50 1 d PD A 1 H16A H -0.4115 0.3366 0.9801 0.080 Uiso 0.50 1 calc PR A 1 H16B H -0.4185 0.2898 0.9061 0.080 Uiso 0.50 1 calc PR A 1 C17 C -0.4902(6) 0.2584(7) 0.9849(8) 0.0667(13) Uiso 0.50 1 d PD A 1 H17A H -0.4957 0.2797 1.0346 0.080 Uiso 0.50 1 calc PR A 1 H17B H -0.5256 0.2854 0.9537 0.080 Uiso 0.50 1 calc PR A 1 C18 C -0.5199(7) 0.1933(6) 0.9913(7) 0.0667(13) Uiso 0.50 1 d PD A 1 H18A H -0.5694 0.1981 1.0119 0.100 Uiso 0.50 1 calc PR A 1 H18B H -0.4897 0.1629 1.0240 0.100 Uiso 0.50 1 calc PR A 1 H18C H -0.5227 0.1700 0.9429 0.100 Uiso 0.50 1 calc PR A 1 C16A C -0.4184(3) 0.2864(3) 0.9604(3) 0.0667(13) Uiso 0.25 1 d PD A 2 H16C H -0.4349 0.3164 1.0026 0.080 Uiso 0.25 1 calc PR A 2 H16D H -0.4019 0.3204 0.9213 0.080 Uiso 0.25 1 calc PR A 2 C17A C -0.4768(12) 0.2456(12) 0.9347(15) 0.0667(13) Uiso 0.25 1 d PD A 2 H17C H -0.5195 0.2772 0.9463 0.080 Uiso 0.25 1 calc PR A 2 H17D H -0.4710 0.2490 0.8808 0.080 Uiso 0.25 1 calc PR A 2 C18A C -0.5029(14) 0.1803(12) 0.9435(15) 0.0667(13) Uiso 0.25 1 d PD A 2 H18D H -0.5496 0.1759 0.9170 0.100 Uiso 0.25 1 calc PR A 2 H18E H -0.5111 0.1711 0.9959 0.100 Uiso 0.25 1 calc PR A 2 H18F H -0.4679 0.1442 0.9242 0.100 Uiso 0.25 1 calc PR A 2 C16B C -0.4184(3) 0.2864(3) 0.9604(3) 0.0667(13) Uiso 0.25 1 d PD A 3 H16E H -0.4640 0.2570 0.9626 0.080 Uiso 0.25 1 calc PR A 3 H16F H -0.4111 0.3021 0.9088 0.080 Uiso 0.25 1 calc PR A 3 C17B C -0.4270(13) 0.3572(10) 1.0113(12) 0.0667(13) Uiso 0.25 1 d PD A 3 H17E H -0.4459 0.3411 1.0596 0.080 Uiso 0.25 1 calc PR A 3 H17F H -0.3776 0.3783 1.0194 0.080 Uiso 0.25 1 calc PR A 3 C18B C -0.4717(13) 0.4116(12) 0.9858(13) 0.0667(13) Uiso 0.25 1 d PD A 3 H18G H -0.4697 0.4537 1.0194 0.100 Uiso 0.25 1 calc PR A 3 H18H H -0.5223 0.3934 0.9829 0.100 Uiso 0.25 1 calc PR A 3 H18I H -0.4553 0.4269 0.9369 0.100 Uiso 0.25 1 calc PR A 3 C19 C 0.2787(3) 0.1181(3) 0.8064(3) 0.0442(12) Uani 1 1 d . . . H19A H 0.2995 0.0773 0.7770 0.053 Uiso 1 1 calc R . . H19B H 0.2486 0.0964 0.8461 0.053 Uiso 1 1 calc R . . C20 C 0.2010(2) 0.2230(3) 0.8037(2) 0.0395(11) Uani 1 1 d . . . H20A H 0.1699 0.2021 0.8431 0.047 Uiso 1 1 calc R . . H20B H 0.1696 0.2544 0.7724 0.047 Uiso 1 1 calc R . . N1 N 0.2315(2) 0.1629(2) 0.7592(2) 0.0394(9) Uani 1 1 d . . . N2 N 0.3394(2) 0.1606(2) 0.8394(2) 0.0416(16) Uani 1 3 d S . . O1 O 0.1221(2) 0.1600(2) 0.6316(2) 0.0606(10) Uani 1 1 d . . . O2 O 0.05860(18) 0.12202(18) 0.76481(17) 0.0424(8) Uani 1 1 d . A . O3 O -0.22317(16) 0.15287(18) 1.00859(17) 0.0415(8) Uani 1 1 d . . . O4 O -0.36008(17) 0.2110(2) 1.04591(18) 0.0477(8) Uani 1 1 d . . . Cu1 Cu 0.14190(3) 0.08958(3) 0.70848(3) 0.04110(18) Uani 1 1 d . A . 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 C6 0.050(3) 0.046(3) 0.043(3) 0.009(2) 0.005(2) 0.002(2) C7 0.046(3) 0.039(3) 0.043(3) 0.002(2) 0.004(2) -0.003(2) C8 0.062(3) 0.049(3) 0.062(4) 0.009(3) 0.025(3) 0.022(3) C9 0.070(4) 0.052(3) 0.058(3) 0.016(3) 0.025(3) 0.020(3) C10 0.040(3) 0.035(3) 0.045(3) -0.005(2) 0.001(2) 0.001(2) C11 0.052(3) 0.051(3) 0.065(4) 0.016(3) 0.010(3) 0.015(3) C12 0.047(3) 0.061(4) 0.069(4) 0.019(3) 0.014(3) 0.006(3) C13 0.035(2) 0.031(2) 0.044(3) -0.008(2) -0.002(2) 0.0016(19) C14 0.049(3) 0.040(3) 0.050(3) -0.002(2) -0.004(2) 0.005(2) C15 0.036(3) 0.048(3) 0.049(3) -0.002(2) -0.008(2) 0.003(2) C19 0.048(3) 0.038(3) 0.046(3) -0.003(2) 0.006(2) -0.006(2) C20 0.037(2) 0.045(3) 0.036(3) -0.010(2) 0.009(2) -0.018(2) N1 0.045(2) 0.040(2) 0.033(2) -0.0010(17) 0.0064(17) -0.0135(18) N2 0.0416(16) 0.0416(16) 0.0416(16) -0.0080(19) 0.0080(19) -0.0080(19) O1 0.051(2) 0.082(3) 0.050(2) 0.018(2) 0.0151(18) 0.006(2) O2 0.0440(19) 0.0443(19) 0.0388(18) 0.0026(15) 0.0026(15) -0.0048(16) O3 0.0373(18) 0.047(2) 0.0404(19) -0.0091(16) -0.0018(14) 0.0098(15) O4 0.0310(17) 0.066(2) 0.046(2) -0.0050(18) -0.0041(16) 0.0153(17) Cu1 0.0457(4) 0.0421(4) 0.0355(3) 0.0004(3) 0.0073(3) -0.0081(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 C2 1.198(12) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.450(12) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.51(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C1A C2A 1.291(15) . ? C1A H1A1 0.9800 . ? C1A H1A2 0.9800 . ? C1A H1A3 0.9800 . ? C2A C3A 1.659(16) . ? C2A H2A1 0.9900 . ? C2A H2A2 0.9900 . ? C3A C4A 1.55(3) . ? C3A H3A1 0.9900 . ? C3A H3A2 0.9900 . ? C4 O1 1.292(18) . ? C4 C5 1.39(2) . ? C5 C6 1.375(17) . ? C5 H5 0.9500 . ? C4A O1 1.27(3) . ? C4A C5A 1.43(4) . ? C5A C6 1.42(2) . ? C5A H5A 0.9500 . ? C6 O2 1.276(6) . ? C6 C7 1.475(7) . ? C7 C12 1.370(7) . ? C7 C8 1.402(7) . ? C8 C9 1.355(7) . ? C8 H8 0.9500 . ? C9 C10 1.396(7) . ? C9 H9 0.9500 . ? C10 C11 1.370(7) . ? C10 C13 1.488(6) . ? C11 C12 1.395(7) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 O3 1.271(5) . ? C13 C14 1.407(7) . ? C14 C15 1.405(7) . ? C14 H14 0.9500 . ? C15 O4 1.256(6) . ? C15 C16 1.484(8) . ? C16 C17 1.472(11) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.308(13) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C17A C18A 1.291(17) . ? C17A H17C 0.9900 . ? C17A H17D 0.9900 . ? C18A H18D 0.9800 . ? C18A H18E 0.9800 . ? C18A H18F 0.9800 . ? C17B C18B 1.363(18) . ? C17B H17E 0.9900 . ? C17B H17F 0.9900 . ? C18B H18G 0.9800 . ? C18B H18H 0.9800 . ? C18B H18I 0.9800 . ? C19 N1 1.463(7) . ? C19 N2 1.477(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 N1 1.470(6) . ? C20 N1 1.475(5) 9_456 ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? N1 C20 1.475(5) 10_565 ? N1 Cu1 2.301(4) . ? N2 C19 1.477(5) 9_456 ? N2 C19 1.477(5) 10_565 ? O1 Cu1 1.931(4) . ? O2 Cu1 1.924(3) . ? O3 Cu1 1.940(3) 5_456 ? O4 Cu1 1.942(3) 5_456 ? Cu1 O3 1.940(3) 6_546 ? Cu1 O4 1.942(3) 6_546 ? 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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C1 C2 C3 119.0(12) . . ? C1 C2 H2A 107.6 . . ? C3 C2 H2A 107.6 . . ? C1 C2 H2B 107.6 . . ? C3 C2 H2B 107.6 . . ? H2A C2 H2B 107.0 . . ? C2 C3 C4 114.3(11) . . ? C2 C3 H3A 108.7 . . ? C4 C3 H3A 108.7 . . ? C2 C3 H3B 108.7 . . ? C4 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? C2A C1A C1A 140.9(18) . 7 ? C2A C1A C1A 159.1(18) . 8_545 ? C1A C1A C1A 60.000(2) 7 8_545 ? C2A C1A H1A1 109.5 . . ? C1A C1A H1A1 90.7 7 . ? C1A C1A H1A1 61.4 8_545 . ? C2A C1A H1A2 109.5 . . ? C1A C1A H1A2 93.7 7 . ? C1A C1A H1A2 61.2 8_545 . ? H1A1 C1A H1A2 109.5 . . ? C2A C1A H1A3 109.5 . . ? C1A C1A H1A3 91.4 8_545 . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? C1A C2A C3A 121.8(15) . . ? C1A C2A H2A1 106.9 . . ? C3A C2A H2A1 106.9 . . ? C1A C2A H2A2 106.9 . . ? C3A C2A H2A2 106.9 . . ? H2A1 C2A H2A2 106.7 . . ? C4A C3A C2A 112.3(14) . . ? C4A C3A H3A1 109.1 . . ? C2A C3A H3A1 109.1 . . ? C4A C3A H3A2 109.1 . . ? C2A C3A H3A2 109.1 . . ? H3A1 C3A H3A2 107.9 . . ? O1 C4 C5 125.0(16) . . ? O1 C4 C3 113.2(13) . . ? C5 C4 C3 121.8(15) . . ? C6 C5 C4 125.1(15) . . ? C6 C5 H5 117.4 . . ? C4 C5 H5 117.4 . . ? O1 C4A C5A 123(2) . . ? O1 C4A C3A 116(2) . . ? C5A C4A C3A 120(2) . . ? C6 C5A C4A 124(2) . . ? C6 C5A H5A 118.1 . . ? C4A C5A H5A 118.1 . . ? O2 C6 C5 124.1(8) . . ? O2 C6 C5A 122.4(11) . . ? O2 C6 C7 115.8(4) . . ? C5 C6 C7 120.0(8) . . ? C5A C6 C7 119.8(12) . . ? C12 C7 C8 116.8(5) . . ? C12 C7 C6 123.0(5) . . ? C8 C7 C6 120.2(4) . . ? C9 C8 C7 121.7(5) . . ? C9 C8 H8 119.1 . . ? C7 C8 H8 119.1 . . ? C8 C9 C10 121.6(5) . . ? C8 C9 H9 119.2 . . ? C10 C9 H9 119.2 . . ? C11 C10 C9 116.9(4) . . ? C11 C10 C13 123.8(4) . . ? C9 C10 C13 119.3(4) . . ? C10 C11 C12 121.6(5) . . ? C10 C11 H11 119.2 . . ? C12 C11 H11 119.2 . . ? C7 C12 C11 121.3(5) . . ? C7 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? O3 C13 C14 124.6(4) . . ? O3 C13 C10 115.4(4) . . ? C14 C13 C10 120.0(4) . . ? C15 C14 C13 124.2(5) . . ? C15 C14 H14 117.9 . . ? C13 C14 H14 117.9 . . ? O4 C15 C14 125.1(4) . . ? O4 C15 C16 116.4(5) . . ? C14 C15 C16 118.5(5) . . ? C17 C16 C15 113.8(7) . . ? C17 C16 H16A 108.8 . . ? C15 C16 H16A 108.8 . . ? C17 C16 H16B 108.8 . . ? C15 C16 H16B 108.8 . . ? H16A C16 H16B 107.7 . . ? C18 C17 C16 135.1(12) . . ? C18 C17 H17A 103.4 . . ? C16 C17 H17A 103.4 . . ? C18 C17 H17B 103.4 . . ? C16 C17 H17B 103.4 . . ? H17A C17 H17B 105.2 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C18A C17A H17C 102.7 . . ? C18A C17A H17D 102.7 . . ? H17C C17A H17D 105.0 . . ? C17A C18A H18D 109.5 . . ? C17A C18A H18E 109.5 . . ? H18D C18A H18E 109.5 . . ? C17A C18A H18F 109.5 . . ? H18D C18A H18F 109.5 . . ? H18E C18A H18F 109.5 . . ? C18B C17B H17E 108.1 . . ? C18B C17B H17F 108.1 . . ? H17E C17B H17F 107.3 . . ? C17B C18B H18G 109.5 . . ? C17B C18B H18H 109.5 . . ? H18G C18B H18H 109.5 . . ? C17B C18B H18I 109.5 . . ? H18G C18B H18I 109.5 . . ? H18H C18B H18I 109.5 . . ? N1 C19 N2 112.7(4) . . ? N1 C19 H19A 109.1 . . ? N2 C19 H19A 109.1 . . ? N1 C19 H19B 109.1 . . ? N2 C19 H19B 109.1 . . ? H19A C19 H19B 107.8 . . ? N1 C20 N1 112.0(4) . 9_456 ? N1 C20 H20A 109.2 . . ? N1 C20 H20A 109.2 9_456 . ? N1 C20 H20B 109.2 . . ? N1 C20 H20B 109.2 9_456 . ? H20A C20 H20B 107.9 . . ? C19 N1 C20 108.2(4) . . ? C19 N1 C20 108.7(4) . 10_565 ? C20 N1 C20 107.5(4) . 10_565 ? C19 N1 Cu1 109.1(3) . . ? C20 N1 Cu1 112.7(3) . . ? C20 N1 Cu1 110.4(3) 10_565 . ? C19 N2 C19 107.5(3) 9_456 . ? C19 N2 C19 107.5(3) 9_456 10_565 ? C19 N2 C19 107.5(3) . 10_565 ? C4A O1 Cu1 124.7(12) . . ? C4 O1 Cu1 125.7(8) . . ? C6 O2 Cu1 127.3(3) . . ? C13 O3 Cu1 126.9(3) . 5_456 ? C15 O4 Cu1 126.9(3) . 5_456 ? O2 Cu1 O1 92.01(14) . . ? O2 Cu1 O3 88.42(14) . 6_546 ? O1 Cu1 O3 171.24(16) . 6_546 ? O2 Cu1 O4 168.20(15) . 6_546 ? O1 Cu1 O4 85.82(14) . 6_546 ? O3 Cu1 O4 91.98(14) 6_546 6_546 ? O2 Cu1 N1 99.59(14) . . ? O1 Cu1 N1 92.21(16) . . ? O3 Cu1 N1 96.35(14) 6_546 . ? O4 Cu1 N1 92.09(14) 6_546 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C2 C3 C4 60.1(17) . . . . ? C1A C1A C2A C3A -59(2) 7 . . . ? C1A C1A C2A C3A 124(2) 8_545 . . . ? C1A C2A C3A C4A 38(3) . . . . ? C2 C3 C4 O1 29.5(15) . . . . ? C2 C3 C4 C5 -148.7(12) . . . . ? O1 C4 C5 C6 1.6(19) . . . . ? C3 C4 C5 C6 179.6(10) . . . . ? C2A C3A C4A O1 74(2) . . . . ? C2A C3A C4A C5A -98(2) . . . . ? O1 C4A C5A C6 5(3) . . . . ? C3A C4A C5A C6 176.4(15) . . . . ? C4 C5 C6 O2 4.0(15) . . . . ? C4 C5 C6 C5A -86(6) . . . . ? C4 C5 C6 C7 -179.7(10) . . . . ? C4A C5A C6 O2 -21(2) . . . . ? C4A C5A C6 C5 81(6) . . . . ? C4A C5A C6 C7 176.2(14) . . . . ? O2 C6 C7 C12 165.5(5) . . . . ? C5 C6 C7 C12 -11.1(9) . . . . ? C5A C6 C7 C12 -30.2(11) . . . . ? O2 C6 C7 C8 -13.3(7) . . . . ? C5 C6 C7 C8 170.2(7) . . . . ? C5A C6 C7 C8 151.0(10) . . . . ? C12 C7 C8 C9 1.2(9) . . . . ? C6 C7 C8 C9 180.0(5) . . . . ? C7 C8 C9 C10 -1.7(10) . . . . ? C8 C9 C10 C11 0.7(9) . . . . ? C8 C9 C10 C13 -178.7(5) . . . . ? C9 C10 C11 C12 0.6(8) . . . . ? C13 C10 C11 C12 -180.0(5) . . . . ? C8 C7 C12 C11 0.2(9) . . . . ? C6 C7 C12 C11 -178.6(5) . . . . ? C10 C11 C12 C7 -1.1(9) . . . . ? C11 C10 C13 O3 -164.5(5) . . . . ? C9 C10 C13 O3 14.9(7) . . . . ? C11 C10 C13 C14 17.3(7) . . . . ? C9 C10 C13 C14 -163.3(5) . . . . ? O3 C13 C14 C15 -0.1(8) . . . . ? C10 C13 C14 C15 177.8(4) . . . . ? C13 C14 C15 O4 3.5(8) . . . . ? C13 C14 C15 C16 -178.7(5) . . . . ? O4 C15 C16 C17 -36.2(9) . . . . ? C14 C15 C16 C17 145.7(8) . . . . ? C15 C16 C17 C18 -39(2) . . . . ? N2 C19 N1 C20 -58.9(4) . . . . ? N2 C19 N1 C20 57.6(4) . . . 10_565 ? N2 C19 N1 Cu1 178.1(2) . . . . ? N1 C20 N1 C19 58.0(5) 9_456 . . . ? N1 C20 N1 C20 -59.3(6) 9_456 . . 10_565 ? N1 C20 N1 Cu1 178.8(2) 9_456 . . . ? N1 C19 N2 C19 58.1(5) . . . 9_456 ? N1 C19 N2 C19 -57.4(5) . . . 10_565 ? C5A C4A O1 C4 -78(6) . . . . ? C3A C4A O1 C4 110(7) . . . . ? C5A C4A O1 Cu1 21(2) . . . . ? C3A C4A O1 Cu1 -151.0(11) . . . . ? C5 C4 O1 C4A 93(7) . . . . ? C3 C4 O1 C4A -85(7) . . . . ? C5 C4 O1 Cu1 0.6(16) . . . . ? C3 C4 O1 Cu1 -177.5(7) . . . . ? C5 C6 O2 Cu1 -11.3(9) . . . . ? C5A C6 O2 Cu1 8.4(11) . . . . ? C7 C6 O2 Cu1 172.3(3) . . . . ? C14 C13 O3 Cu1 1.0(6) . . . 5_456 ? C10 C13 O3 Cu1 -177.1(3) . . . 5_456 ? C14 C15 O4 Cu1 -7.2(7) . . . 5_456 ? C16 C15 O4 Cu1 174.9(3) . . . 5_456 ? C6 O2 Cu1 O1 10.4(4) . . . . ? C6 O2 Cu1 O3 -160.8(4) . . . 6_546 ? C6 O2 Cu1 O4 -68.7(8) . . . 6_546 ? C6 O2 Cu1 N1 103.0(4) . . . . ? C4A O1 Cu1 O2 -24.9(11) . . . . ? C4 O1 Cu1 O2 -5.1(8) . . . . ? C4A O1 Cu1 O4 143.5(12) . . . 6_546 ? C4 O1 Cu1 O4 163.3(8) . . . 6_546 ? C4A O1 Cu1 N1 -124.6(11) . . . . ? C4 O1 Cu1 N1 -104.7(8) . . . . ? C19 N1 Cu1 O2 106.6(3) . . . . ? C20 N1 Cu1 O2 -13.7(3) . . . . ? C20 N1 Cu1 O2 -133.9(3) 10_565 . . . ? C19 N1 Cu1 O1 -161.0(3) . . . . ? C20 N1 Cu1 O1 78.8(3) . . . . ? C20 N1 Cu1 O1 -41.5(3) 10_565 . . . ? C19 N1 Cu1 O3 17.2(3) . . . 6_546 ? C20 N1 Cu1 O3 -103.1(3) . . . 6_546 ? C20 N1 Cu1 O3 136.6(3) 10_565 . . 6_546 ? C19 N1 Cu1 O4 -75.1(3) . . . 6_546 ? C20 N1 Cu1 O4 164.7(3) . . . 6_546 ? C20 N1 Cu1 O4 44.4(3) 10_565 . . 6_546 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.549 _refine_diff_density_min -0.729 _refine_diff_density_rms 0.085