# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email dsun@sdu.edu.cn _publ_contact_author_name 'Di Sun' loop_ _publ_author_name 'Daofeng Sun' 'Di Sun' data_BPS-2 #TrackingRef 'web_deposit_cif_file_0_DiSun_1329271777.BPS-2-3-r2.cif' _database_code_depnum_ccdc_archive 'CCDC 830680' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C182 H280 Cl2 Cu9 N18 O96' _chemical_formula_weight 4899.05 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P -4 21 c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 31.010(4) _cell_length_b 31.010(4) _cell_length_c 28.765(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 27661(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 14532 _cell_measurement_theta_min 3.2957 _cell_measurement_theta_max 51.1957 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.934 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8004 _exptl_absorpt_coefficient_mu 0.749 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9288 _exptl_absorpt_correction_T_max 0.9288 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14894 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0218 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 26.37 _reflns_number_total 14894 _reflns_number_gt 13323 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. The Cu5/Cu5' was disordered with a ratio of 55/45. The one pyridine ligand was also disordered in two positions (N3, C77 > C81 and N3', C77' > C81') with a ratio of 55/45. The Cl2/Cl2' was disordered with a ratio of 80/20. The non-hydrogen atoms except some atoms with high thermal parameters due to disorder (C47, C48, C49 C50, C51, N3, C77, C78, C79, C80, C81, Cl2, Cl2') were refined anisotropically. In order to subtract the contribution from the disordered solvent molecules and cations, the SQUEEZE command was applied. ; _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^+0.0200P] 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 0.221(16) _refine_ls_number_reflns 14894 _refine_ls_number_parameters 993 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0846 _refine_ls_R_factor_gt 0.0801 _refine_ls_wR_factor_ref 0.2348 _refine_ls_wR_factor_gt 0.2281 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _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 1.08548(2) 0.82530(3) 0.52057(2) 0.03514(19) Uani 1 1 d . . . Cu2 Cu 1.20816(3) 0.71639(2) 0.25941(3) 0.03614(19) Uani 1 1 d . . . Cu3 Cu 1.0000 1.0000 0.24565(4) 0.0324(2) Uani 1 2 d S . . Cu4 Cu 0.86390(3) 0.63497(3) 0.27053(3) 0.0469(2) Uani 1 1 d . . . Cu5' Cu 0.98651(5) 0.76724(5) 0.02329(4) 0.0398(3) Uani 0.55 1 d P . . Cu5 Cu 0.92525(6) 0.80390(9) 0.01794(6) 0.0542(6) Uani 0.45 1 d P . . Cl1 Cl 1.0000 1.0000 0.33055(11) 0.0696(8) Uani 1 2 d S . . N1 N 1.17250(13) 0.70849(11) 0.20083(16) 0.066(2) Uani 1 1 d G . . C51 C 1.14216(14) 0.67550(10) 0.20135(15) 0.065(2) Uiso 1 1 d G . . H51A H 1.1391 0.6583 0.2276 0.078 Uiso 1 1 calc R . . C50 C 1.11641(15) 0.66820(10) 0.16259(14) 0.105(4) Uiso 1 1 d G . . H50A H 1.0961 0.6461 0.1629 0.126 Uiso 1 1 calc R . . C49 C 1.12099(16) 0.69390(11) 0.12331(14) 0.226(13) Uiso 1 1 d G . . H49A H 1.1038 0.6890 0.0974 0.272 Uiso 1 1 calc R . . C48 C 1.15133(15) 0.72690(12) 0.12279(14) 0.119(5) Uiso 1 1 d G . . H48A H 1.1544 0.7441 0.0965 0.143 Uiso 1 1 calc R . . C47 C 1.17708(13) 0.73419(11) 0.16155(15) 0.096(4) Uiso 1 1 d G . . H47A H 1.1974 0.7563 0.1612 0.115 Uiso 1 1 calc R . . N8 N 1.04588(12) 1.04741(9) 0.23570(19) 0.062(2) Uani 1 1 d G . . C82 C 1.06024(13) 1.06252(9) 0.27848(19) 0.067(2) Uiso 1 1 d G . . H82A H 1.0501 1.0501 0.3058 0.080 Uiso 1 1 calc R . . C83 C 1.08970(14) 1.09624(9) 0.2804(2) 0.102(4) Uiso 1 1 d G . . H83A H 1.0993 1.1064 0.3091 0.122 Uiso 1 1 calc R . . C84 C 1.10482(14) 1.11486(9) 0.2396(2) 0.114(5) Uiso 1 1 d G . . H84A H 1.1245 1.1374 0.2409 0.137 Uiso 1 1 calc R . . C85 C 1.09047(14) 1.09975(10) 0.1968(2) 0.104(4) Uiso 1 1 d G . . H85A H 1.1006 1.1122 0.1695 0.125 Uiso 1 1 calc R . . C86 C 1.06100(13) 1.06602(10) 0.19487(19) 0.085(3) Uiso 1 1 d G . . H86A H 1.0514 1.0559 0.1662 0.102 Uiso 1 1 calc R . . N5 N 0.87634(15) 0.65086(13) 0.3351(2) 0.075(3) Uani 1 1 d G . . C67 C 0.84630(16) 0.66996(15) 0.3644(2) 0.108(4) Uiso 1 1 d G . . C68 C 0.85790(17) 0.68113(15) 0.4095(2) 0.231(15) Uiso 1 1 d G . . C69 C 0.89954(18) 0.67321(15) 0.42526(19) 0.203(12) Uiso 1 1 d G . . C70 C 0.92958(17) 0.65411(13) 0.39589(17) 0.144(7) Uiso 1 1 d G . . C71 C 0.91798(16) 0.64294(13) 0.35079(18) 0.130(6) Uiso 1 1 d G . . H71A H 0.9381 0.6302 0.3311 0.156 Uiso 1 1 calc R . . C1 C 1.13264(19) 0.74439(19) 0.29718(18) 0.0306(11) Uani 1 1 d . . . C2 C 1.09851(18) 0.77554(17) 0.31387(18) 0.0275(11) Uani 1 1 d . . . C3 C 1.10393(17) 0.79236(18) 0.35927(18) 0.0277(10) Uani 1 1 d . . . C4 C 1.07259(18) 0.82207(16) 0.37396(17) 0.0270(10) Uani 1 1 d . . . C5 C 1.03848(17) 0.83539(16) 0.34552(19) 0.0267(10) Uani 1 1 d . . . C6 C 1.03458(17) 0.81846(16) 0.30018(17) 0.0243(10) Uani 1 1 d . . . C7 C 1.06631(16) 0.78869(16) 0.28409(18) 0.0229(9) Uani 1 1 d . . . C8 C 1.1405(2) 0.7786(2) 0.3898(2) 0.0440(15) Uani 1 1 d . . . H8A H 1.1355 0.7886 0.4209 0.066 Uiso 1 1 calc R . . H8B H 1.1669 0.7907 0.3783 0.066 Uiso 1 1 calc R . . H8C H 1.1425 0.7477 0.3897 0.066 Uiso 1 1 calc R . . C9 C 1.00733(17) 0.86900(17) 0.36443(18) 0.0272(10) Uani 1 1 d . . . H9A H 0.9786 0.8622 0.3545 0.041 Uiso 1 1 calc R . . H9B H 1.0152 0.8970 0.3529 0.041 Uiso 1 1 calc R . . H9C H 1.0086 0.8691 0.3978 0.041 Uiso 1 1 calc R . . C10 C 1.0651(2) 0.7712(2) 0.2352(2) 0.0377(13) Uani 1 1 d . . . H10A H 1.0860 0.7486 0.2320 0.057 Uiso 1 1 calc R . . H10B H 1.0716 0.7939 0.2136 0.057 Uiso 1 1 calc R . . H10C H 1.0369 0.7599 0.2287 0.057 Uiso 1 1 calc R . . C11 C 1.07980(19) 0.84099(19) 0.42210(19) 0.0315(12) Uani 1 1 d . . . C12 C 0.99873(17) 0.83659(15) 0.26905(18) 0.0247(10) Uani 1 1 d . . . H12A H 0.9781 0.8508 0.2893 0.030 Uiso 1 1 calc R . . H12B H 1.0116 0.8588 0.2498 0.030 Uiso 1 1 calc R . . C13 C 0.97307(16) 0.80712(16) 0.23675(18) 0.0246(10) Uani 1 1 d . . . C14 C 0.97474(18) 0.81205(19) 0.1885(2) 0.0311(11) Uani 1 1 d . . . C15 C 0.94948(19) 0.7845(2) 0.1611(2) 0.0388(14) Uani 1 1 d . . . C16 C 0.9226(2) 0.7543(3) 0.1791(2) 0.0417(15) Uani 1 1 d . . . C17 C 0.9207(2) 0.7499(2) 0.2283(2) 0.0415(15) Uani 1 1 d . . . C18 C 0.94609(19) 0.77573(19) 0.25681(18) 0.0314(12) Uani 1 1 d . . . C19 C 0.8931(2) 0.7150(3) 0.2476(2) 0.0454(16) Uani 1 1 d . . . C20 C 0.9521(3) 0.7886(3) 0.1083(2) 0.0504(18) Uani 1 1 d . . . C21 C 0.9435(2) 0.7700(2) 0.30929(19) 0.0390(14) Uani 1 1 d . . . H21A H 0.9225 0.7484 0.3166 0.058 Uiso 1 1 calc R . . H21B H 0.9353 0.7969 0.3234 0.058 Uiso 1 1 calc R . . H21C H 0.9712 0.7613 0.3210 0.058 Uiso 1 1 calc R . . C22 C 0.8975(3) 0.7224(3) 0.1482(3) 0.065(3) Uani 1 1 d . . . H22A H 0.9044 0.7277 0.1162 0.097 Uiso 1 1 calc R . . H22B H 0.8671 0.7262 0.1530 0.097 Uiso 1 1 calc R . . H22C H 0.9055 0.6934 0.1562 0.097 Uiso 1 1 calc R . . C23 C 1.00302(18) 0.84517(18) 0.1640(2) 0.0297(11) Uani 1 1 d . . . H23A H 1.0107 0.8676 0.1855 0.045 Uiso 1 1 calc R . . H23B H 0.9875 0.8574 0.1383 0.045 Uiso 1 1 calc R . . H23C H 1.0287 0.8314 0.1527 0.045 Uiso 1 1 calc R . . C24 C 1.23625(18) 0.6324(2) 0.24546(18) 0.0318(11) Uani 1 1 d . . . C25 C 1.26601(19) 0.59997(19) 0.2250(2) 0.0327(12) Uani 1 1 d . . . C26 C 1.28919(16) 0.57183(18) 0.25478(18) 0.0272(10) Uani 1 1 d . . . C27 C 1.31594(15) 0.53849(16) 0.23563(17) 0.0219(9) Uani 1 1 d . . . C28 C 1.32174(17) 0.53653(17) 0.18744(19) 0.0276(11) Uani 1 1 d . . . C29 C 1.29838(17) 0.56616(16) 0.15874(17) 0.0257(10) Uani 1 1 d . . . C30 C 1.26974(19) 0.59676(18) 0.1770(2) 0.0323(11) Uani 1 1 d . . . C31 C 1.2438(2) 0.6249(2) 0.1445(2) 0.0440(15) Uani 1 1 d . . . H31A H 1.2449 0.6131 0.1137 0.066 Uiso 1 1 calc R . . H31B H 1.2558 0.6535 0.1443 0.066 Uiso 1 1 calc R . . H31C H 1.2145 0.6261 0.1549 0.066 Uiso 1 1 calc R . . C32 C 1.2853(2) 0.5784(2) 0.30705(19) 0.0332(12) Uani 1 1 d . . . H32A H 1.2687 0.6039 0.3132 0.050 Uiso 1 1 calc R . . H32B H 1.3136 0.5817 0.3203 0.050 Uiso 1 1 calc R . . H32C H 1.2714 0.5539 0.3207 0.050 Uiso 1 1 calc R . . C33 C 1.3530(2) 0.50544(17) 0.1652(2) 0.0317(12) Uani 1 1 d . . . H33A H 1.3693 0.4911 0.1890 0.047 Uiso 1 1 calc R . . H33B H 1.3723 0.5210 0.1451 0.047 Uiso 1 1 calc R . . H33C H 1.3373 0.4845 0.1474 0.047 Uiso 1 1 calc R . . C34 C 1.30486(19) 0.56548(18) 0.10635(18) 0.0301(11) Uani 1 1 d . . . C35 C 1.33712(14) 0.50579(14) 0.26808(16) 0.0189(9) Uani 1 1 d . . . H35A H 1.3513 0.4838 0.2496 0.023 Uiso 1 1 calc R . . H35B H 1.3590 0.5203 0.2864 0.023 Uiso 1 1 calc R . . C36 C 1.30534(18) 0.48444(18) 0.30039(19) 0.0290(11) Uani 1 1 d . . . C37 C 1.31210(19) 0.48348(18) 0.3498(2) 0.0314(11) Uani 1 1 d . . . C38 C 1.2801(2) 0.4655(2) 0.3789(2) 0.0364(12) Uani 1 1 d . . . C39 C 1.2388(2) 0.4529(2) 0.3618(2) 0.0402(13) Uani 1 1 d . . . C40 C 1.2338(2) 0.45283(19) 0.3133(2) 0.0349(12) Uani 1 1 d . . . C41 C 1.2663(2) 0.46696(18) 0.28320(19) 0.0308(11) Uani 1 1 d . . . C42 C 1.2597(2) 0.4618(2) 0.2306(2) 0.0407(14) Uani 1 1 d . . . H42A H 1.2300 0.4552 0.2244 0.061 Uiso 1 1 calc R . . H42B H 1.2776 0.4388 0.2194 0.061 Uiso 1 1 calc R . . H42C H 1.2674 0.4881 0.2152 0.061 Uiso 1 1 calc R . . C43 C 1.3526(2) 0.5016(2) 0.3712(2) 0.0373(12) Uani 1 1 d . . . H43A H 1.3714 0.5117 0.3470 0.056 Uiso 1 1 calc R . . H43B H 1.3670 0.4794 0.3887 0.056 Uiso 1 1 calc R . . H43C H 1.3453 0.5250 0.3915 0.056 Uiso 1 1 calc R . . C44 C 1.2037(3) 0.4363(3) 0.3941(3) 0.0535(18) Uani 1 1 d . . . H44A H 1.1786 0.4292 0.3763 0.080 Uiso 1 1 calc R . . H44B H 1.1966 0.4583 0.4164 0.080 Uiso 1 1 calc R . . H44C H 1.2139 0.4111 0.4101 0.080 Uiso 1 1 calc R . . C45 C 1.2865(2) 0.4640(2) 0.4309(2) 0.0407(14) Uani 1 1 d . . . C46 C 1.1921(2) 0.4373(2) 0.2932(2) 0.0415(14) Uani 1 1 d . . . C52 C 1.2543(3) 0.7540(3) 0.3410(3) 0.0512(17) Uani 1 1 d . . . H52A H 1.2617 0.7759 0.3203 0.061 Uiso 1 1 calc R . . C53 C 1.2655(3) 0.7585(3) 0.3873(3) 0.062(2) Uani 1 1 d . . . H53A H 1.2795 0.7831 0.3979 0.075 Uiso 1 1 calc R . . C54 C 1.2548(3) 0.7241(3) 0.4185(3) 0.069(2) Uani 1 1 d . . . H54A H 1.2612 0.7261 0.4500 0.083 Uiso 1 1 calc R . . C55 C 1.2356(3) 0.6895(3) 0.4015(3) 0.062(2) Uani 1 1 d . . . H55A H 1.2300 0.6662 0.4211 0.074 Uiso 1 1 calc R . . C56 C 1.2235(3) 0.6870(3) 0.3543(3) 0.056(2) Uani 1 1 d . . . H56A H 1.2086 0.6628 0.3437 0.067 Uiso 1 1 calc R . . C57 C 1.1563(3) 0.7610(4) 0.5256(3) 0.074(3) Uani 1 1 d . . . H57A H 1.1722 0.7854 0.5332 0.089 Uiso 1 1 calc R . . C58 C 1.1767(4) 0.7218(4) 0.5242(3) 0.082(4) Uani 1 1 d . . . H58A H 1.2060 0.7188 0.5301 0.098 Uiso 1 1 calc R . . C59 C 1.1482(5) 0.6838(4) 0.5127(5) 0.094(4) Uani 1 1 d . . . H59A H 1.1593 0.6560 0.5131 0.113 Uiso 1 1 calc R . . C60 C 1.1073(5) 0.6905(4) 0.5020(5) 0.104(5) Uani 1 1 d . . . H60A H 1.0904 0.6675 0.4922 0.125 Uiso 1 1 calc R . . C61 C 1.0892(4) 0.7318(3) 0.5053(3) 0.079(3) Uani 1 1 d . . . H61A H 1.0599 0.7352 0.4997 0.094 Uiso 1 1 calc R . . C62 C 1.0605(2) 0.9111(2) 0.5581(2) 0.0442(15) Uani 1 1 d . . . H62A H 1.0893 0.9134 0.5668 0.053 Uiso 1 1 calc R . . C63 C 1.0329(3) 0.9408(2) 0.5727(3) 0.0504(17) Uani 1 1 d . . . H63A H 1.0432 0.9641 0.5898 0.060 Uiso 1 1 calc R . . C64 C 0.9898(3) 0.9382(2) 0.5634(3) 0.0519(18) Uani 1 1 d . . . H64A H 0.9702 0.9582 0.5749 0.062 Uiso 1 1 calc R . . C65 C 0.9774(2) 0.9049(3) 0.5365(3) 0.0540(19) Uani 1 1 d . . . H65A H 0.9484 0.9031 0.5282 0.065 Uiso 1 1 calc R . . C66 C 1.0051(2) 0.8734(2) 0.5204(2) 0.0417(14) Uani 1 1 d . . . H66A H 0.9949 0.8503 0.5030 0.050 Uiso 1 1 calc R . . C72 C 0.8044(3) 0.6362(3) 0.1896(3) 0.062(2) Uani 1 1 d . . . H72A H 0.7854 0.6489 0.2106 0.075 Uiso 1 1 calc R . . C73 C 0.7904(4) 0.6285(3) 0.1454(4) 0.074(3) Uani 1 1 d . . . H73A H 0.7619 0.6342 0.1376 0.089 Uiso 1 1 calc R . . C74 C 0.8177(4) 0.6125(4) 0.1129(3) 0.083(3) Uani 1 1 d . . . H74A H 0.8086 0.6061 0.0829 0.100 Uiso 1 1 calc R . . C75 C 0.8599(6) 0.6062(5) 0.1270(4) 0.106(5) Uani 1 1 d . . . H75A H 0.8800 0.5982 0.1047 0.128 Uiso 1 1 calc R . . C76 C 0.8743(4) 0.6112(4) 0.1725(4) 0.074(3) Uani 1 1 d . . . H76A H 0.9025 0.6046 0.1809 0.089 Uiso 1 1 calc R . . C87 C 1.0665(2) 0.93478(19) 0.2694(3) 0.0414(14) Uani 1 1 d . . . H87A H 1.0572 0.9407 0.2995 0.050 Uiso 1 1 calc R . . C88 C 1.0994(2) 0.9050(2) 0.2639(3) 0.0458(16) Uani 1 1 d . . . H88A H 1.1125 0.8925 0.2896 0.055 Uiso 1 1 calc R . . C89 C 1.1120(2) 0.8946(2) 0.2209(4) 0.057(2) Uani 1 1 d . . . H89A H 1.1334 0.8740 0.2163 0.068 Uiso 1 1 calc R . . C90 C 1.0925(2) 0.9154(2) 0.1822(3) 0.0492(17) Uani 1 1 d . . . H90A H 1.1008 0.9091 0.1519 0.059 Uiso 1 1 calc R . . C91 C 1.0605(2) 0.9453(2) 0.1916(3) 0.0441(15) Uani 1 1 d . . . H91A H 1.0473 0.9593 0.1669 0.053 Uiso 1 1 calc R . . N2 N 1.23281(19) 0.71857(18) 0.3246(2) 0.0412(12) Uani 1 1 d . . . N4 N 0.8450(2) 0.62625(18) 0.2046(2) 0.0454(14) Uani 1 1 d . . . N6 N 1.04813(17) 0.87732(17) 0.53088(17) 0.0358(11) Uani 1 1 d . . . N7 N 1.1120(2) 0.7653(2) 0.5158(2) 0.0538(16) Uani 1 1 d . . . N9 N 1.04770(14) 0.95483(15) 0.2356(2) 0.0404(13) Uani 1 1 d . . . O1 O 1.16707(15) 0.76164(16) 0.27768(15) 0.0409(10) Uani 1 1 d . . . O2 O 1.12765(16) 0.70644(15) 0.30181(16) 0.0425(11) Uani 1 1 d . . . O3 O 1.06447(14) 0.81941(14) 0.45533(14) 0.0345(9) Uani 1 1 d . . . O4 O 1.10208(17) 0.87453(14) 0.42650(14) 0.0411(10) Uani 1 1 d . . . O5 O 0.90834(17) 0.67686(17) 0.24993(19) 0.0525(13) Uani 1 1 d . . . O6 O 0.85348(18) 0.7233(2) 0.2581(2) 0.0659(18) Uani 1 1 d . . . O7 O 0.98274(19) 0.7643(2) 0.08904(18) 0.0608(15) Uani 1 1 d . . . O8 O 0.9259(3) 0.8103(3) 0.0874(2) 0.080(2) Uani 1 1 d . . . O9 O 1.24890(14) 0.67150(12) 0.24092(15) 0.0357(9) Uani 1 1 d . . . O10 O 1.20147(14) 0.62155(15) 0.26386(16) 0.0409(10) Uani 1 1 d . . . O11 O 1.28941(16) 0.53509(13) 0.08272(14) 0.0380(9) Uani 1 1 d . . . O12 O 1.32477(14) 0.59759(13) 0.08902(13) 0.0319(8) Uani 1 1 d . . . O13 O 1.27238(19) 0.49334(18) 0.45570(16) 0.0521(13) Uani 1 1 d . . . O14 O 1.3066(2) 0.4330(2) 0.44690(19) 0.0648(17) Uani 1 1 d . . . O15 O 1.18901(16) 0.39527(16) 0.29212(17) 0.0457(11) Uani 1 1 d . . . O16 O 1.16453(16) 0.46350(18) 0.2814(2) 0.0577(14) Uani 1 1 d . . . O17 O 1.0384(5) 0.7184(5) 0.0183(6) 0.157(5) Uiso 1 1 d . . . Cl2 Cl 1.0128(3) 1.0190(3) 0.1004(4) 0.102(2) Uiso 0.40 1 d P . . Cl2' Cl 1.0581(11) 1.0195(11) 0.0612(13) 0.093(8) Uiso 0.10 1 d P . . O2W O 1.2573(2) 0.76707(17) 0.2274(2) 0.0567(14) Uani 1 1 d . . . O22 O 1.14966(19) 0.8613(2) 0.5047(2) 0.0580(14) Uani 1 1 d . . . O1W O 0.9111(3) 0.5774(3) 0.2701(3) 0.0799(19) Uiso 1 1 d . . . C81 C 0.9373(4) 0.7050(6) 0.0198(8) 0.073(6) Uiso 0.45 1 d PG . . H81A H 0.9675 0.7116 0.0222 0.087 Uiso 0.45 1 d PR . . N3 N 0.9075(6) 0.7385(4) 0.0183(6) 0.054(4) Uiso 0.45 1 d PG . . C80 C 0.8637(5) 0.7294(6) 0.0150(12) 0.21(4) Uiso 0.45 1 d PG . . H80A H 0.8431 0.7525 0.0140 0.258 Uiso 0.45 1 d PR . . C79 C 0.8497(4) 0.6868(7) 0.0131(14) 0.26(5) Uiso 0.45 1 d PG . . H79A H 0.8195 0.6806 0.0108 0.315 Uiso 0.45 1 d PR . . C78 C 0.8795(6) 0.6534(5) 0.0146(10) 0.084(7) Uiso 0.45 1 d PG . . H78A H 0.8699 0.6240 0.0132 0.101 Uiso 0.45 1 d PR . . C77 C 0.9233(6) 0.6625(5) 0.0179(8) 0.079(6) Uiso 0.45 1 d PG . . H77A H 0.9439 0.6394 0.0189 0.094 Uiso 0.45 1 d PR . . N3' N 0.9362(4) 0.7241(7) 0.0201(7) 0.086(5) Uiso 0.55 1 d PG . . C81' C 0.8984(5) 0.7481(4) 0.0177(7) 0.093(8) Uiso 0.55 1 d PG . . H81B H 0.8998 0.7790 0.0170 0.112 Uiso 0.55 1 d PR . . C80' C 0.8587(4) 0.7274(5) 0.0163(7) 0.070(5) Uiso 0.55 1 d PG . . H80B H 0.8326 0.7440 0.0146 0.084 Uiso 0.55 1 d PR . . C79' C 0.8567(5) 0.6826(5) 0.0172(8) 0.090(7) Uiso 0.55 1 d PG . . H79B H 0.8293 0.6683 0.0162 0.108 Uiso 0.55 1 d PR . . C78' C 0.8945(7) 0.6586(4) 0.0196(11) 0.177(19) Uiso 0.55 1 d PG . . H78B H 0.8931 0.6276 0.0203 0.212 Uiso 0.55 1 d PR . . C77' C 0.9342(5) 0.6793(7) 0.0211(10) 0.172(17) Uiso 0.55 1 d PG . . H77B H 0.9603 0.6627 0.0228 0.206 Uiso 0.55 1 d 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 0.0336(3) 0.0558(4) 0.0160(3) 0.0011(3) 0.0023(3) 0.0118(3) Cu2 0.0418(4) 0.0410(4) 0.0256(4) -0.0033(3) 0.0048(3) 0.0179(3) Cu3 0.0207(4) 0.0260(4) 0.0506(6) 0.000 0.000 0.0033(3) Cu4 0.0481(5) 0.0485(5) 0.0441(5) 0.0050(4) 0.0026(4) -0.0233(4) Cu5' 0.0457(7) 0.0589(8) 0.0146(5) -0.0017(6) 0.0013(5) -0.0120(6) Cu5 0.0475(10) 0.1013(17) 0.0139(7) 0.0048(9) -0.0010(7) -0.0266(10) Cl1 0.0704(18) 0.090(2) 0.0480(15) 0.000 0.000 0.0311(17) N1 0.064(4) 0.104(6) 0.032(3) -0.009(3) -0.003(3) 0.057(4) N8 0.031(3) 0.032(3) 0.123(7) 0.001(3) 0.015(3) 0.015(2) N5 0.079(5) 0.093(6) 0.053(4) 0.002(4) -0.009(4) -0.069(5) C1 0.035(3) 0.039(3) 0.018(2) -0.006(2) 0.001(2) 0.017(2) C2 0.035(3) 0.027(2) 0.021(2) -0.0058(19) 0.007(2) 0.013(2) C3 0.031(2) 0.032(3) 0.020(2) -0.007(2) -0.0003(19) 0.012(2) C4 0.039(3) 0.026(2) 0.016(2) -0.0049(19) 0.004(2) 0.005(2) C5 0.028(2) 0.022(2) 0.030(3) -0.0054(19) 0.005(2) 0.0009(19) C6 0.030(2) 0.025(2) 0.017(2) -0.0039(18) 0.0034(19) 0.005(2) C7 0.023(2) 0.024(2) 0.021(2) -0.0086(19) -0.0017(18) 0.0050(18) C8 0.055(4) 0.056(4) 0.021(3) -0.005(3) -0.008(3) 0.022(3) C9 0.031(3) 0.031(2) 0.020(2) -0.0097(19) -0.0046(19) 0.006(2) C10 0.046(3) 0.045(3) 0.022(3) -0.013(2) -0.005(2) 0.016(3) C11 0.034(3) 0.039(3) 0.022(2) -0.005(2) 0.002(2) 0.015(2) C12 0.026(2) 0.020(2) 0.028(3) -0.0022(18) -0.007(2) 0.0021(18) C13 0.024(2) 0.027(2) 0.023(2) -0.0023(19) -0.0028(19) -0.0055(18) C14 0.027(3) 0.035(3) 0.031(3) 0.000(2) -0.002(2) -0.012(2) C15 0.030(3) 0.055(4) 0.031(3) -0.009(3) -0.002(2) -0.022(3) C16 0.040(3) 0.070(4) 0.016(2) -0.005(3) 0.002(2) -0.026(3) C17 0.044(3) 0.056(4) 0.024(3) -0.002(3) -0.002(2) -0.029(3) C18 0.040(3) 0.041(3) 0.013(2) -0.009(2) 0.006(2) -0.015(2) C19 0.051(4) 0.068(4) 0.017(3) -0.012(3) 0.004(2) -0.021(3) C20 0.063(4) 0.059(4) 0.029(3) -0.001(3) 0.005(3) -0.024(4) C21 0.050(3) 0.055(4) 0.012(2) -0.004(2) 0.005(2) -0.021(3) C22 0.079(5) 0.084(6) 0.031(3) -0.007(4) -0.012(3) -0.058(5) C23 0.027(2) 0.034(3) 0.027(3) 0.007(2) 0.004(2) -0.012(2) C24 0.034(3) 0.043(3) 0.018(2) 0.004(2) -0.001(2) 0.015(2) C25 0.037(3) 0.037(3) 0.024(3) 0.001(2) 0.007(2) 0.008(2) C26 0.025(2) 0.038(3) 0.018(2) 0.000(2) 0.0033(19) 0.011(2) C27 0.019(2) 0.027(2) 0.020(2) 0.0049(19) 0.0026(18) 0.0077(18) C28 0.027(2) 0.026(2) 0.030(3) 0.000(2) 0.007(2) 0.017(2) C29 0.034(3) 0.026(2) 0.018(2) 0.0072(18) 0.0033(19) 0.006(2) C30 0.032(3) 0.033(3) 0.033(3) -0.002(2) 0.005(2) 0.010(2) C31 0.049(4) 0.050(4) 0.033(3) 0.001(3) -0.007(3) 0.030(3) C32 0.038(3) 0.040(3) 0.022(2) -0.005(2) 0.000(2) 0.009(2) C33 0.043(3) 0.025(2) 0.027(3) 0.003(2) 0.018(2) 0.011(2) C34 0.036(3) 0.034(3) 0.020(2) 0.000(2) 0.006(2) 0.014(2) C35 0.0184(19) 0.0164(19) 0.022(2) 0.0034(17) 0.0010(16) -0.0024(15) C36 0.033(3) 0.034(3) 0.020(2) -0.001(2) 0.004(2) 0.000(2) C37 0.037(3) 0.032(3) 0.026(3) 0.003(2) 0.000(2) -0.004(2) C38 0.043(3) 0.038(3) 0.028(3) 0.000(2) -0.005(2) -0.003(2) C39 0.045(3) 0.046(3) 0.029(3) 0.000(2) 0.003(3) -0.009(3) C40 0.043(3) 0.035(3) 0.026(3) -0.004(2) -0.004(2) -0.011(2) C41 0.044(3) 0.029(2) 0.019(2) -0.002(2) 0.000(2) -0.001(2) C42 0.053(4) 0.048(3) 0.020(3) -0.002(2) -0.006(2) -0.015(3) C43 0.038(3) 0.042(3) 0.032(3) 0.004(3) -0.008(2) -0.007(3) C44 0.053(4) 0.069(5) 0.039(4) 0.001(3) 0.008(3) -0.019(4) C45 0.057(4) 0.037(3) 0.028(3) 0.005(2) 0.004(3) -0.004(3) C46 0.052(4) 0.037(3) 0.035(3) -0.003(3) 0.004(3) -0.017(3) C52 0.054(4) 0.056(4) 0.044(4) 0.000(3) -0.007(3) 0.004(3) C53 0.084(6) 0.062(5) 0.040(4) -0.002(4) -0.016(4) -0.001(4) C54 0.077(6) 0.085(6) 0.045(4) -0.005(4) -0.011(4) 0.026(5) C55 0.086(6) 0.060(4) 0.039(4) -0.001(3) -0.008(4) 0.010(4) C56 0.076(5) 0.050(4) 0.042(4) -0.003(3) -0.009(4) 0.031(4) C57 0.064(5) 0.113(8) 0.046(4) 0.011(5) 0.007(4) 0.048(5) C58 0.081(6) 0.114(9) 0.051(5) -0.008(5) 0.006(4) 0.063(7) C59 0.122(10) 0.075(7) 0.087(8) 0.001(6) 0.000(7) 0.052(7) C60 0.139(12) 0.055(6) 0.119(11) -0.021(6) -0.026(9) 0.042(7) C61 0.133(9) 0.041(4) 0.062(5) -0.014(4) -0.039(6) 0.028(5) C62 0.055(4) 0.054(4) 0.023(3) 0.009(3) -0.002(3) -0.005(3) C63 0.063(4) 0.045(4) 0.043(4) -0.005(3) 0.010(3) 0.008(3) C64 0.067(5) 0.041(3) 0.048(4) 0.011(3) 0.011(3) 0.013(3) C65 0.036(3) 0.082(5) 0.044(4) 0.005(4) 0.010(3) 0.023(3) C66 0.051(4) 0.044(3) 0.030(3) 0.002(3) 0.008(3) 0.012(3) C72 0.074(6) 0.065(5) 0.048(4) 0.007(4) 0.013(4) -0.032(4) C73 0.077(6) 0.082(6) 0.063(6) 0.000(5) -0.016(5) -0.037(5) C74 0.091(7) 0.117(9) 0.043(5) -0.007(5) -0.003(5) -0.049(7) C75 0.162(14) 0.113(10) 0.045(5) -0.027(6) 0.017(7) -0.020(10) C76 0.079(6) 0.086(7) 0.057(5) -0.018(5) 0.011(5) -0.034(5) C87 0.041(3) 0.027(3) 0.056(4) 0.010(3) 0.003(3) -0.006(2) C88 0.027(3) 0.039(3) 0.071(5) 0.009(3) 0.000(3) -0.006(2) C89 0.035(3) 0.029(3) 0.106(7) -0.016(4) 0.009(4) -0.013(3) C90 0.038(3) 0.036(3) 0.073(5) -0.017(3) 0.003(3) -0.002(3) C91 0.037(3) 0.031(3) 0.065(4) -0.009(3) 0.004(3) 0.000(2) N2 0.050(3) 0.039(3) 0.034(3) -0.007(2) -0.004(2) 0.023(2) N4 0.060(4) 0.037(3) 0.040(3) -0.007(2) 0.016(3) -0.032(3) N6 0.040(3) 0.041(3) 0.026(2) 0.004(2) -0.0025(19) 0.004(2) N7 0.063(4) 0.068(4) 0.030(3) 0.008(3) 0.012(3) 0.025(3) N9 0.0187(19) 0.025(2) 0.077(4) 0.001(2) -0.003(2) 0.0040(17) O1 0.045(2) 0.054(3) 0.0229(19) -0.0006(18) 0.0039(18) 0.023(2) O2 0.056(3) 0.037(2) 0.034(2) -0.0095(18) -0.0070(19) 0.022(2) O3 0.039(2) 0.047(2) 0.0185(18) 0.0020(17) 0.0014(16) 0.0032(18) O4 0.065(3) 0.038(2) 0.0200(19) -0.0034(16) -0.0042(19) 0.000(2) O5 0.054(3) 0.052(3) 0.051(3) 0.018(2) -0.008(2) -0.025(2) O6 0.060(3) 0.086(4) 0.051(3) -0.033(3) 0.026(3) -0.053(3) O7 0.062(3) 0.090(4) 0.031(2) -0.016(3) 0.005(2) -0.013(3) O8 0.100(5) 0.111(5) 0.028(3) 0.011(3) 0.005(3) 0.011(5) O9 0.045(2) 0.0291(18) 0.033(2) -0.0025(16) 0.0141(18) 0.0174(17) O10 0.035(2) 0.049(2) 0.039(2) -0.0004(19) 0.0108(18) 0.0173(18) O11 0.061(3) 0.033(2) 0.0197(18) -0.0034(16) 0.0015(18) 0.0030(19) O12 0.044(2) 0.0322(19) 0.0192(18) 0.0001(15) 0.0043(16) 0.0040(17) O13 0.069(3) 0.061(3) 0.026(2) -0.010(2) 0.007(2) -0.010(3) O14 0.101(5) 0.061(3) 0.033(3) 0.001(2) -0.003(3) 0.028(3) O15 0.049(3) 0.044(2) 0.044(3) -0.015(2) 0.005(2) -0.025(2) O16 0.038(2) 0.052(3) 0.083(4) -0.003(3) -0.010(3) -0.013(2) O2W 0.064(3) 0.043(3) 0.063(4) 0.011(2) 0.007(3) 0.019(2) O22 0.056(3) 0.077(4) 0.040(3) 0.005(3) 0.000(2) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O3 1.995(4) . ? Cu1 O12 2.005(4) 8_545 ? Cu1 N6 2.008(5) . ? Cu1 N7 2.039(7) . ? Cu1 O22 2.327(6) . ? Cu2 O9 1.954(4) . ? Cu2 O1 1.967(4) . ? Cu2 N2 2.026(6) . ? Cu2 N1 2.030(5) . ? Cu2 O2W 2.375(6) . ? Cu3 N9 2.057(5) 2_775 ? Cu3 N9 2.057(5) . ? Cu3 N8 2.066(4) 2_775 ? Cu3 N8 2.066(4) . ? Cu3 Cl1 2.442(3) . ? Cu4 N5 1.959(6) . ? Cu4 O5 1.984(5) . ? Cu4 O15 1.989(4) 2_765 ? Cu4 N4 2.003(6) . ? Cu4 O1W 2.310(8) . ? Cu5' O7 1.897(6) . ? Cu5' O13 1.962(5) 8_544 ? Cu5' N3' 2.058(15) . ? Cu5' O17 2.215(16) . ? Cu5' C81 2.462(15) . ? Cu5 O8 2.008(6) . ? Cu5 O14 2.059(6) 8_544 ? Cu5 N3 2.102(13) . ? N1 C51 1.3900 . ? N1 C47 1.3900 . ? C51 C50 1.3900 . ? C50 C49 1.3900 . ? C49 C48 1.3900 . ? C48 C47 1.3900 . ? N8 C82 1.3900 . ? N8 C86 1.3900 . ? C82 C83 1.3900 . ? C83 C84 1.3900 . ? C84 C85 1.3900 . ? C85 C86 1.3900 . ? N5 C67 1.3900 . ? N5 C71 1.3900 . ? C67 C68 1.3900 . ? C68 C69 1.3900 . ? C69 C70 1.3900 . ? C70 C71 1.3900 . ? C1 O2 1.194(8) . ? C1 O1 1.319(8) . ? C1 C2 1.511(7) . ? C2 C7 1.377(7) . ? C2 C3 1.416(7) . ? C3 C4 1.404(7) . ? C3 C8 1.496(8) . ? C4 C5 1.400(8) . ? C4 C11 1.521(7) . ? C5 C6 1.411(7) . ? C5 C9 1.521(7) . ? C6 C7 1.426(7) . ? C6 C12 1.534(7) . ? C7 C10 1.509(7) . ? C11 O4 1.255(8) . ? C11 O3 1.260(7) . ? C12 C13 1.527(7) . ? C13 C14 1.397(8) . ? C13 C18 1.407(7) . ? C14 C15 1.401(8) . ? C14 C23 1.523(7) . ? C15 C16 1.358(9) . ? C15 C20 1.526(9) . ? C16 C17 1.422(8) . ? C16 C22 1.539(8) . ? C17 C18 1.392(8) . ? C17 C19 1.486(9) . ? C18 C21 1.522(7) . ? C19 O5 1.277(10) . ? C19 O6 1.290(10) . ? C20 O8 1.215(11) . ? C20 O7 1.333(11) . ? C24 O10 1.248(8) . ? C24 O9 1.281(8) . ? C24 C25 1.487(8) . ? C25 C30 1.389(8) . ? C25 C26 1.419(8) . ? C26 C27 1.435(7) . ? C26 C32 1.522(7) . ? C27 C28 1.399(7) . ? C27 C35 1.527(6) . ? C28 C29 1.432(7) . ? C28 C33 1.510(6) . ? C29 C30 1.402(7) . ? C29 C34 1.520(7) . ? C30 C31 1.511(8) . ? C34 O11 1.257(7) . ? C34 O12 1.273(7) . ? C35 C36 1.508(7) . ? C36 C41 1.416(8) . ? C36 C37 1.437(8) . ? C37 C38 1.414(9) . ? C37 C43 1.507(8) . ? C38 C39 1.425(9) . ? C38 C45 1.510(8) . ? C39 C40 1.405(9) . ? C39 C44 1.519(9) . ? C40 C41 1.399(9) . ? C40 C46 1.498(9) . ? C41 C42 1.535(7) . ? C45 O14 1.234(9) . ? C45 O13 1.236(9) . ? C46 O16 1.226(10) . ? C46 O15 1.307(8) . ? C52 N2 1.370(10) . ? C52 C53 1.382(12) . ? C53 C54 1.433(15) . ? C54 C55 1.323(14) . ? C55 C56 1.411(11) . ? C56 N2 1.331(11) . ? C57 C58 1.368(14) . ? C57 N7 1.409(12) . ? C58 C59 1.51(2) . ? C59 C60 1.32(2) . ? C60 C61 1.402(13) . ? C61 N7 1.293(14) . ? C62 C63 1.325(11) . ? C62 N6 1.364(9) . ? C63 C64 1.367(12) . ? C64 C65 1.345(12) . ? C65 C66 1.381(10) . ? C66 N6 1.375(9) . ? C72 N4 1.365(12) . ? C72 C73 1.365(13) . ? C73 C74 1.357(16) . ? C74 C75 1.39(2) . ? C75 C76 1.390(17) . ? C76 N4 1.377(12) . ? C87 N9 1.292(9) . ? C87 C88 1.386(10) . ? C88 C89 1.336(13) . ? C89 C90 1.420(13) . ? C90 C91 1.383(10) . ? C91 N9 1.361(11) . ? O12 Cu1 2.005(4) 8_544 ? O13 Cu5' 1.962(5) 8_545 ? O14 Cu5 2.059(6) 8_545 ? O15 Cu4 1.989(4) 2_765 ? Cl2 Cl2 1.420(19) 2_775 ? C81 N3 1.3900 . ? C81 C77 1.3900 . ? N3 C80 1.3900 . ? C80 C79 1.3900 . ? C79 C78 1.3900 . ? C78 C77 1.3900 . ? N3' C81' 1.3900 . ? N3' C77' 1.3900 . ? C81' C80' 1.3900 . ? C80' C79' 1.3900 . ? C79' C78' 1.3900 . ? C78' C77' 1.3900 . ? 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 O3 Cu1 O12 169.89(18) . 8_545 ? O3 Cu1 N6 91.38(19) . . ? O12 Cu1 N6 88.25(19) 8_545 . ? O3 Cu1 N7 89.1(2) . . ? O12 Cu1 N7 89.1(2) 8_545 . ? N6 Cu1 N7 167.4(3) . . ? O3 Cu1 O22 98.00(19) . . ? O12 Cu1 O22 92.06(19) 8_545 . ? N6 Cu1 O22 97.8(2) . . ? N7 Cu1 O22 94.5(3) . . ? O9 Cu2 O1 179.7(2) . . ? O9 Cu2 N2 91.8(2) . . ? O1 Cu2 N2 88.47(19) . . ? O9 Cu2 N1 92.31(16) . . ? O1 Cu2 N1 87.42(16) . . ? N2 Cu2 N1 167.9(2) . . ? O9 Cu2 O2W 87.17(18) . . ? O1 Cu2 O2W 92.72(19) . . ? N2 Cu2 O2W 95.4(3) . . ? N1 Cu2 O2W 96.2(2) . . ? N9 Cu3 N9 163.9(4) 2_775 . ? N9 Cu3 N8 88.28(15) 2_775 2_775 ? N9 Cu3 N8 89.50(15) . 2_775 ? N9 Cu3 N8 89.50(16) 2_775 . ? N9 Cu3 N8 88.28(16) . . ? N8 Cu3 N8 164.1(3) 2_775 . ? N9 Cu3 Cl1 98.0(2) 2_775 . ? N9 Cu3 Cl1 98.0(2) . . ? N8 Cu3 Cl1 97.97(15) 2_775 . ? N8 Cu3 Cl1 97.97(15) . . ? N5 Cu4 O5 88.94(19) . . ? N5 Cu4 O15 89.14(18) . 2_765 ? O5 Cu4 O15 167.1(2) . 2_765 ? N5 Cu4 N4 171.3(3) . . ? O5 Cu4 N4 90.5(2) . . ? O15 Cu4 N4 89.4(2) 2_765 . ? N5 Cu4 O1W 94.3(3) . . ? O5 Cu4 O1W 93.7(3) . . ? O15 Cu4 O1W 99.2(3) 2_765 . ? N4 Cu4 O1W 94.4(3) . . ? O7 Cu5' O13 176.7(3) . 8_544 ? O7 Cu5' N3' 88.1(6) . . ? O13 Cu5' N3' 95.2(6) 8_544 . ? O7 Cu5' O17 94.4(5) . . ? O13 Cu5' O17 85.0(5) 8_544 . ? N3' Cu5' O17 95.9(7) . . ? O7 Cu5' Cu5 92.3(2) . . ? O13 Cu5' Cu5 88.98(19) 8_544 . ? N3' Cu5' Cu5 71.4(5) . . ? O17 Cu5' Cu5 165.5(4) . . ? O7 Cu5' C81 88.0(5) . . ? O13 Cu5' C81 95.2(5) 8_544 . ? N3' Cu5' C81 11.0(5) . . ? O17 Cu5' C81 85.0(6) . . ? Cu5 Cu5' C81 82.4(4) . . ? C81' Cu5 O8 95.5(6) . . ? C81' Cu5 O14 94.8(6) . 8_544 ? O8 Cu5 O14 169.2(3) . 8_544 ? C81' Cu5 N3 10.5(6) . . ? O8 Cu5 N3 95.3(6) . . ? O14 Cu5 N3 94.3(6) 8_544 . ? C81' Cu5 Cu5' 84.8(5) . . ? O8 Cu5 Cu5' 88.5(2) . . ? O14 Cu5 Cu5' 89.40(19) 8_544 . ? N3 Cu5 Cu5' 74.3(5) . . ? C51 N1 C47 120.0 . . ? N1 C51 C50 120.0 . . ? C49 C50 C51 120.0 . . ? C48 C49 C50 120.0 . . ? C49 C48 C47 120.0 . . ? C48 C47 N1 120.0 . . ? C82 N8 C86 120.0 . . ? C86 N8 Cu3 130.16(15) . . ? N8 C82 C83 120.0 . . ? C82 C83 C84 120.0 . . ? C85 C84 C83 120.0 . . ? C84 C85 C86 120.0 . . ? C85 C86 N8 120.0 . . ? C67 N5 C71 120.0 . . ? N5 C67 C68 120.0 . . ? C69 C68 C67 120.0 . . ? C68 C69 C70 120.0 . . ? C71 C70 C69 120.0 . . ? C70 C71 N5 120.0 . . ? O2 C1 O1 123.5(5) . . ? O2 C1 C2 120.2(6) . . ? O1 C1 C2 116.3(5) . . ? C7 C2 C3 123.4(4) . . ? C7 C2 C1 120.0(4) . . ? C3 C2 C1 116.4(5) . . ? C4 C3 C2 115.9(5) . . ? C4 C3 C8 122.3(5) . . ? C2 C3 C8 121.7(5) . . ? C5 C4 C3 122.7(5) . . ? C5 C4 C11 122.0(5) . . ? C3 C4 C11 115.2(5) . . ? C4 C5 C6 119.7(5) . . ? C4 C5 C9 118.2(5) . . ? C6 C5 C9 122.1(5) . . ? C5 C6 C7 118.8(5) . . ? C5 C6 C12 117.7(4) . . ? C7 C6 C12 123.2(4) . . ? C2 C7 C6 119.3(4) . . ? C2 C7 C10 119.5(4) . . ? C6 C7 C10 121.2(5) . . ? O4 C11 O3 124.8(5) . . ? O4 C11 C4 119.5(5) . . ? O3 C11 C4 115.5(5) . . ? C13 C12 C6 120.9(4) . . ? C14 C13 C18 120.3(5) . . ? C14 C13 C12 121.3(5) . . ? C18 C13 C12 118.3(5) . . ? C13 C14 C15 118.1(5) . . ? C13 C14 C23 123.7(5) . . ? C15 C14 C23 118.2(5) . . ? C16 C15 C14 123.4(6) . . ? C16 C15 C20 117.9(5) . . ? C14 C15 C20 118.7(6) . . ? C15 C16 C17 118.1(5) . . ? C15 C16 C22 122.2(5) . . ? C17 C16 C22 119.5(6) . . ? C18 C17 C16 120.5(5) . . ? C18 C17 C19 121.6(5) . . ? C16 C17 C19 117.8(5) . . ? C17 C18 C13 119.6(5) . . ? C17 C18 C21 119.2(5) . . ? C13 C18 C21 121.2(5) . . ? O5 C19 O6 121.7(7) . . ? O5 C19 C17 118.7(6) . . ? O6 C19 C17 119.4(8) . . ? O8 C20 O7 125.7(7) . . ? O8 C20 C15 120.3(8) . . ? O7 C20 C15 113.9(7) . . ? O10 C24 O9 124.3(5) . . ? O10 C24 C25 121.5(6) . . ? O9 C24 C25 114.2(5) . . ? C30 C25 C26 121.0(5) . . ? C30 C25 C24 119.6(5) . . ? C26 C25 C24 119.4(5) . . ? C25 C26 C27 120.3(5) . . ? C25 C26 C32 118.3(5) . . ? C27 C26 C32 121.4(5) . . ? C28 C27 C26 119.1(4) . . ? C28 C27 C35 121.4(4) . . ? C26 C27 C35 119.5(4) . . ? C27 C28 C29 118.6(4) . . ? C27 C28 C33 122.0(5) . . ? C29 C28 C33 119.4(5) . . ? C30 C29 C28 122.6(5) . . ? C30 C29 C34 117.7(5) . . ? C28 C29 C34 119.7(4) . . ? C25 C30 C29 118.3(5) . . ? C25 C30 C31 122.0(5) . . ? C29 C30 C31 119.8(5) . . ? O11 C34 O12 124.0(5) . . ? O11 C34 C29 119.7(5) . . ? O12 C34 C29 116.2(5) . . ? C36 C35 C27 112.8(4) . . ? C41 C36 C37 117.5(5) . . ? C41 C36 C35 120.8(5) . . ? C37 C36 C35 121.6(5) . . ? C38 C37 C36 119.4(5) . . ? C38 C37 C43 119.4(5) . . ? C36 C37 C43 121.2(5) . . ? C37 C38 C39 122.3(6) . . ? C37 C38 C45 120.3(6) . . ? C39 C38 C45 116.9(6) . . ? C40 C39 C38 116.3(6) . . ? C40 C39 C44 121.8(6) . . ? C38 C39 C44 121.6(6) . . ? C41 C40 C39 122.4(6) . . ? C41 C40 C46 118.9(5) . . ? C39 C40 C46 118.7(6) . . ? C40 C41 C36 121.3(5) . . ? C40 C41 C42 118.8(5) . . ? C36 C41 C42 119.9(5) . . ? O14 C45 O13 122.5(6) . . ? O14 C45 C38 117.3(6) . . ? O13 C45 C38 120.1(6) . . ? O16 C46 O15 127.2(7) . . ? O16 C46 C40 119.7(6) . . ? O15 C46 C40 113.1(6) . . ? N2 C52 C53 122.3(8) . . ? C52 C53 C54 118.1(9) . . ? C55 C54 C53 118.5(8) . . ? C54 C55 C56 121.3(9) . . ? N2 C56 C55 121.3(8) . . ? C58 C57 N7 121.9(12) . . ? C57 C58 C59 115.4(10) . . ? C60 C59 C58 119.3(10) . . ? C59 C60 C61 120.8(14) . . ? N7 C61 C60 122.1(12) . . ? C63 C62 N6 122.3(7) . . ? C62 C63 C64 121.9(8) . . ? C65 C64 C63 116.1(7) . . ? C64 C65 C66 123.8(8) . . ? N6 C66 C65 117.9(7) . . ? N4 C72 C73 123.3(9) . . ? C74 C73 C72 120.5(10) . . ? C73 C74 C75 116.0(9) . . ? C74 C75 C76 124.3(13) . . ? N4 C76 C75 117.3(12) . . ? N9 C87 C88 124.4(8) . . ? C89 C88 C87 118.9(8) . . ? C88 C89 C90 119.4(7) . . ? C91 C90 C89 117.2(8) . . ? N9 C91 C90 122.5(8) . . ? C56 N2 C52 118.3(7) . . ? C56 N2 Cu2 119.2(5) . . ? C52 N2 Cu2 122.0(5) . . ? C72 N4 C76 118.2(8) . . ? C72 N4 Cu4 122.6(5) . . ? C76 N4 Cu4 119.2(7) . . ? C62 N6 C66 117.9(6) . . ? C62 N6 Cu1 122.7(5) . . ? C66 N6 Cu1 117.2(4) . . ? C61 N7 C57 120.2(9) . . ? C61 N7 Cu1 121.9(6) . . ? C57 N7 Cu1 117.9(7) . . ? C87 N9 C91 117.6(6) . . ? C87 N9 Cu3 123.1(6) . . ? C91 N9 Cu3 119.3(5) . . ? C1 O1 Cu2 110.4(4) . . ? C11 O3 Cu1 122.8(4) . . ? C19 O5 Cu4 111.4(5) . . ? C20 O7 Cu5' 115.6(5) . . ? C20 O8 Cu5 116.4(6) . . ? C24 O9 Cu2 116.7(4) . . ? C34 O12 Cu1 104.0(3) . 8_544 ? C45 O13 Cu5' 121.4(5) . 8_545 ? C45 O14 Cu5 116.1(5) . 8_545 ? C46 O15 Cu4 122.5(5) . 2_765 ? Cl2 Cl2 Cl2' 116.3(13) 2_775 . ? N3' C81 C77' 169(4) . . ? C77' C81 N3 131.5(15) . . ? N3' C81 C77 158.4(19) . . ? N3 C81 C77 120.0 . . ? C77' C81 C81' 131.2(18) . . ? C77 C81 C81' 119.6(8) . . ? N3' C81 C78' 134(2) . . ? N3 C81 C78' 95.7(8) . . ? C81' C81 C78' 95.3(8) . . ? C77' C81 Cu5' 148.1(18) . . ? N3 C81 Cu5' 80.1(9) . . ? C77 C81 Cu5' 159.9(9) . . ? C81' C81 Cu5' 80.5(8) . . ? C78' C81 Cu5' 175.2(12) . . ? N3' N3 C80 141.6(11) . . ? C80 N3 C81 120.0 . . ? N3' N3 C80' 140.5(16) . . ? C80 N3 C80' 2.1(17) . . ? C81 N3 C80' 118.9(9) . . ? N3' N3 Cu5 101.5(16) . . ? C80 N3 Cu5 116.8(10) . . ? C81 N3 Cu5 123.1(10) . . ? C80' N3 Cu5 118.0(10) . . ? C81' C80 N3 16.6(8) . . ? C81' C80 C79 136.6(8) . . ? N3 C80 C79 120.0 . . ? C81' C80 C79' 126.5(14) . . ? N3 C80 C79' 110.0(9) . . ? C80' C79 C78 125.6(8) . . ? C78 C79 C80 120.0 . . ? C80 C79 C78' 103.7(7) . . ? C78' C78 C79' 107(3) . . ? C78' C78 C79 112(2) . . ? C79' C78 C77 115.8(10) . . ? C79 C78 C77 120.0 . . ? C77' C77 C78' 130(3) . . ? C77' C77 C78 134.8(17) . . ? C78' C77 C81 115.7(12) . . ? C78 C77 C81 120.0 . . ? C78' C77 N3' 109.4(14) . . ? C78 C77 N3' 113.6(6) . . ? C81' N3' C77' 120.0 . . ? C81 N3' C77 15.2(13) . . ? N3 N3' C77 104.8(13) . . ? N3 N3' Cu5' 112.7(16) . . ? C81' N3' Cu5' 107.0(11) . . ? C77' N3' Cu5' 133.0(11) . . ? C80 C81' N3' 119.3(10) . . ? C80' C81' N3' 120.0 . . ? C80 C81' C81 103.8(11) . . ? C80 C81' Cu5 143.8(14) . . ? C80' C81' Cu5 143.2(10) . . ? N3' C81' Cu5 96.8(10) . . ? C81 C81' Cu5 112.3(10) . . ? C79 C80' C81' 130.0(10) . . ? C81' C80' C79' 120.0 . . ? C79 C80' N3 115.4(13) . . ? C79' C80' N3 105.3(6) . . ? C78 C79' C80' 139.3(11) . . ? C80' C79' C78' 120.0 . . ? C78 C79' C80 133.2(17) . . ? C78' C79' C80 114.1(7) . . ? C78 C78' C77 157(7) . . ? C78 C78' C77' 163(5) . . ? C77 C78' C79' 139.3(12) . . ? C77' C78' C79' 120.0 . . ? C77 C78' C79 138.9(19) . . ? C77' C78' C79 120.2(8) . . ? C79' C78' C79 3.7(19) . . ? C78 C78' C81 148(4) . . ? C79' C78' C81 100.1(5) . . ? C79 C78' C81 100.3(9) . . ? C77 C77' C81 152(4) . . ? C81 C77' C78' 124.2(13) . . ? C77 C77' N3' 148(2) . . ? C78' C77' N3' 120.0 . . ? C81 C77' C78 121.6(18) . . ? N3' C77' C78 117.6(8) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.216 _refine_diff_density_min -0.758 _refine_diff_density_rms 0.115 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.009 0.154 0.011 11737 3999 ' ' _platon_squeeze_details ; ? ; data_bps-3 #TrackingRef 'web_deposit_cif_file_0_DiSun_1329271777.BPS-2-3-r2.cif' _database_code_depnum_ccdc_archive 'CCDC 830681' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H62 Cu2 N4 O21' _chemical_formula_weight 1146.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4190(7) _cell_length_b 12.9822(8) _cell_length_c 17.2565(11) _cell_angle_alpha 89.9860(10) _cell_angle_beta 79.2290(10) _cell_angle_gamma 80.3940(10) _cell_volume 2476.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 18055 _cell_measurement_theta_min 6.07 _cell_measurement_theta_max 50.03 _exptl_crystal_description BLOCK _exptl_crystal_colour GREEN _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1186 _exptl_absorpt_coefficient_mu 0.945 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8636 _exptl_absorpt_correction_T_max 0.9283 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17084 _diffrn_reflns_av_R_equivalents 0.0214 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 24.84 _reflns_number_total 8438 _reflns_number_gt 6689 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. During the refinement, the command 'isor' was used to restrain the non-H atoms (o10w o11w o12w). The non-hydrogen atoms except some atoms with high thermal parameters due to disorder (O9W and O13W) were refined anisotropically. ; _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^+8.6994P] 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 8438 _refine_ls_number_parameters 666 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0836 _refine_ls_R_factor_gt 0.0680 _refine_ls_wR_factor_ref 0.1938 _refine_ls_wR_factor_gt 0.1808 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.114 _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 0.29888(5) 0.24981(5) 0.03113(4) 0.02605(19) Uani 1 1 d . . . Cu2 Cu 0.66991(6) 0.71387(5) -0.52002(4) 0.0295(2) Uani 1 1 d . . . C1 C 0.2471(5) 0.0854(4) 0.1510(3) 0.0349(13) Uani 1 1 d . . . H1A H 0.1657 0.1151 0.1582 0.042 Uiso 1 1 calc R . . C2 C 0.2815(6) -0.0014(5) 0.1947(3) 0.0415(14) Uani 1 1 d . . . H2A H 0.2237 -0.0285 0.2305 0.050 Uiso 1 1 calc R . . C3 C 0.4013(6) -0.0465(4) 0.1842(3) 0.0407(15) Uani 1 1 d . . . H3A H 0.4246 -0.1056 0.2118 0.049 Uiso 1 1 calc R . . C4 C 0.4874(5) -0.0040(4) 0.1326(3) 0.0342(13) Uani 1 1 d . . . C5 C 0.4445(5) 0.0843(4) 0.0910(3) 0.0280(11) Uani 1 1 d . . . C6 C 0.6154(6) -0.0424(4) 0.1175(4) 0.0399(15) Uani 1 1 d . . . H6A H 0.6452 -0.1010 0.1434 0.048 Uiso 1 1 calc R . . C7 C 0.6936(5) 0.0045(4) 0.0668(3) 0.0375(14) Uani 1 1 d . . . H7A H 0.7758 -0.0221 0.0592 0.045 Uiso 1 1 calc R . . C8 C 0.6531(5) 0.0940(4) 0.0244(3) 0.0314(12) Uani 1 1 d . . . C9 C 0.5271(5) 0.1329(4) 0.0374(3) 0.0283(11) Uani 1 1 d . . . C10 C 0.7288(5) 0.1468(4) -0.0289(3) 0.0362(13) Uani 1 1 d . . . H10A H 0.8121 0.1249 -0.0385 0.043 Uiso 1 1 calc R . . C11 C 0.6786(5) 0.2317(5) -0.0671(3) 0.0376(13) Uani 1 1 d . . . H11A H 0.7275 0.2674 -0.1028 0.045 Uiso 1 1 calc R . . C12 C 0.5533(5) 0.2629(4) -0.0512(3) 0.0329(12) Uani 1 1 d . . . H12A H 0.5203 0.3199 -0.0775 0.040 Uiso 1 1 calc R . . C13 C 0.7936(7) 0.9031(5) -0.5055(4) 0.0516(17) Uani 1 1 d . . . H13A H 0.8620 0.8682 -0.5393 0.062 Uiso 1 1 calc R . . C14 C 0.7952(9) 1.0023(6) -0.4728(5) 0.066(2) Uani 1 1 d . . . H14A H 0.8657 1.0309 -0.4840 0.079 Uiso 1 1 calc R . . C15 C 0.6971(10) 1.0562(6) -0.4258(5) 0.072(3) Uani 1 1 d . . . H15A H 0.6997 1.1219 -0.4053 0.086 Uiso 1 1 calc R . . C16 C 0.5964(6) 0.9129(4) -0.4412(3) 0.0422(15) Uani 1 1 d . . . C17 C 0.5909(8) 1.0132(5) -0.4077(4) 0.057(2) Uani 1 1 d . . . C18 C 0.4785(10) 1.0630(6) -0.3608(4) 0.073(3) Uani 1 1 d . . . H18A H 0.4738 1.1292 -0.3387 0.087 Uiso 1 1 calc R . . C19 C 0.3787(9) 1.0168(6) -0.3476(4) 0.067(2) Uani 1 1 d . . . H19A H 0.3071 1.0522 -0.3176 0.081 Uiso 1 1 calc R . . C20 C 0.3823(7) 0.9147(5) -0.3790(3) 0.0518(19) Uani 1 1 d . . . C21 C 0.4924(6) 0.8639(5) -0.4251(3) 0.0396(14) Uani 1 1 d . . . C22 C 0.2849(7) 0.8619(7) -0.3692(4) 0.060(2) Uani 1 1 d . . . H22A H 0.2100 0.8939 -0.3413 0.072 Uiso 1 1 calc R . . C23 C 0.2985(6) 0.7638(6) -0.3999(4) 0.0528(18) Uani 1 1 d . . . H23A H 0.2330 0.7284 -0.3930 0.063 Uiso 1 1 calc R . . C24 C 0.4107(5) 0.7160(5) -0.4420(3) 0.0383(13) Uani 1 1 d . . . H24A H 0.4198 0.6475 -0.4610 0.046 Uiso 1 1 calc R . . C25 C 0.1476(5) 0.7348(4) -0.1020(3) 0.0266(11) Uani 1 1 d . . . C26 C 0.0719(4) 0.6972(4) -0.0380(3) 0.0253(11) Uani 1 1 d . . . C27 C 0.1111(4) 0.6094(4) 0.0025(3) 0.0236(10) Uani 1 1 d . . . C28 C 0.2303(4) 0.5572(4) -0.0241(3) 0.0237(10) Uani 1 1 d . . . C29 C 0.3085(4) 0.5936(4) -0.0867(3) 0.0234(10) Uani 1 1 d . . . C30 C 0.2657(4) 0.6810(4) -0.1271(3) 0.0233(10) Uani 1 1 d . . . C31 C 0.2699(4) 0.4549(4) 0.0126(3) 0.0256(11) Uani 1 1 d . . . C32 C 0.0294(4) 0.5713(4) 0.0715(3) 0.0315(12) Uani 1 1 d . . . H32A H -0.0533 0.5906 0.0656 0.047 Uiso 1 1 calc R . . H32B H 0.0402 0.6024 0.1196 0.047 Uiso 1 1 calc R . . H32C H 0.0492 0.4966 0.0733 0.047 Uiso 1 1 calc R . . C33 C 0.4389(4) 0.5399(4) -0.1063(3) 0.0290(11) Uani 1 1 d . . . H33A H 0.4904 0.5914 -0.1187 0.044 Uiso 1 1 calc R . . H33B H 0.4498 0.4928 -0.1510 0.044 Uiso 1 1 calc R . . H33C H 0.4595 0.5015 -0.0618 0.044 Uiso 1 1 calc R . . C34 C 0.3450(5) 0.7219(4) -0.1977(3) 0.0309(12) Uani 1 1 d . . . H34A H 0.2919 0.7678 -0.2255 0.037 Uiso 1 1 calc R . . H34B H 0.3950 0.7646 -0.1773 0.037 Uiso 1 1 calc R . . C35 C 0.4277(5) 0.6447(4) -0.2582(3) 0.0256(11) Uani 1 1 d . . . C36 C 0.5482(5) 0.6579(4) -0.2834(3) 0.0266(11) Uani 1 1 d . . . C37 C 0.6263(4) 0.5859(4) -0.3382(3) 0.0257(11) Uani 1 1 d . . . C38 C 0.5877(5) 0.4998(4) -0.3669(3) 0.0276(11) Uani 1 1 d . . . C39 C 0.6793(5) 0.4209(4) -0.4216(3) 0.0380(13) Uani 1 1 d . . . H39A H 0.7538 0.4080 -0.4022 0.057 Uiso 1 1 calc R . . H39B H 0.6936 0.4482 -0.4736 0.057 Uiso 1 1 calc R . . H39C H 0.6484 0.3568 -0.4236 0.057 Uiso 1 1 calc R . . C40 C 0.3846(5) 0.5630(4) -0.2917(3) 0.0271(11) Uani 1 1 d . . . C41 C 0.0995(5) 0.8330(4) -0.1408(3) 0.0318(12) Uani 1 1 d . . . H41A H 0.1576 0.8794 -0.1466 0.048 Uiso 1 1 calc R . . H41B H 0.0251 0.8669 -0.1087 0.048 Uiso 1 1 calc R . . H41C H 0.0852 0.8153 -0.1918 0.048 Uiso 1 1 calc R . . C42 C 0.5988(5) 0.7470(4) -0.2525(3) 0.0350(12) Uani 1 1 d . . . H42A H 0.5432 0.8111 -0.2529 0.052 Uiso 1 1 calc R . . H42B H 0.6750 0.7527 -0.2855 0.052 Uiso 1 1 calc R . . H42C H 0.6104 0.7336 -0.1995 0.052 Uiso 1 1 calc R . . C43 C 0.2532(5) 0.5511(4) -0.2722(3) 0.0338(12) Uani 1 1 d . . . H43A H 0.2325 0.5169 -0.3158 0.051 Uiso 1 1 calc R . . H43B H 0.2035 0.6188 -0.2621 0.051 Uiso 1 1 calc R . . H43C H 0.2400 0.5099 -0.2261 0.051 Uiso 1 1 calc R . . C45 C 0.4661(5) 0.4909(4) -0.3449(3) 0.0267(11) Uani 1 1 d . . . C46 C 0.4233(5) 0.3980(4) -0.3766(3) 0.0317(12) Uani 1 1 d . . . C47 C 0.7549(5) 0.5995(4) -0.3665(3) 0.0300(12) Uani 1 1 d . . . C48 C -0.0604(5) 0.7483(4) -0.0154(3) 0.0307(12) Uani 1 1 d . . . N1 N 0.3257(4) 0.1268(3) 0.1000(2) 0.0276(9) Uani 1 1 d . . . N2 N 0.4791(4) 0.2158(3) -0.0007(3) 0.0284(10) Uani 1 1 d . . . N3 N 0.5053(4) 0.7653(4) -0.4558(2) 0.0338(11) Uani 1 1 d . . . N4 N 0.6955(5) 0.8590(4) -0.4886(3) 0.0391(12) Uani 1 1 d . . . O1 O 0.2827(3) 0.4485(3) 0.0821(2) 0.0339(9) Uani 1 1 d . . . O1W O 0.8275(4) 0.6861(4) -0.5901(2) 0.0480(11) Uani 1 1 d . . . H1WB H 0.8673 0.6247 -0.5899 0.058 Uiso 1 1 d R . . H1WA H 0.8384 0.7036 -0.6380 0.058 Uiso 1 1 d R . . O2 O 0.2864(3) 0.3734(3) -0.0334(2) 0.0298(8) Uani 1 1 d . . . O2W O 0.2314(7) 0.5821(4) 0.2120(3) 0.098(2) Uani 1 1 d . . . H2WA H 0.2488 0.5451 0.1695 0.117 Uiso 1 1 d R . . H2WB H 0.2108 0.5432 0.2500 0.117 Uiso 1 1 d R . . O3 O 0.8329(3) 0.5580(3) -0.3271(2) 0.0410(10) Uani 1 1 d . . . O3W O 0.9391(5) 0.6762(4) 0.7716(3) 0.0615(13) Uani 1 1 d . . . H3WA H 0.9215 0.6739 0.8215 0.074 Uiso 1 1 d R . . H3WB H 0.9095 0.6273 0.7537 0.074 Uiso 1 1 d R . . O4 O 0.7790(3) 0.6490(3) -0.4285(2) 0.0360(9) Uani 1 1 d . . . O4W O 0.0132(5) 0.7148(4) 0.5306(3) 0.0592(13) Uani 1 1 d . . . H4WA H 0.0320 0.7447 0.4873 0.11(4) Uiso 1 1 d R . . H4WB H -0.0573 0.6995 0.5433 0.10(4) Uiso 1 1 d R . . O5 O 0.3823(3) 0.4100(3) -0.4405(2) 0.0306(8) Uani 1 1 d . . . O5W O 0.9487(4) 0.4964(4) 0.4263(3) 0.0698(15) Uani 1 1 d . . . H5WA H 1.0185 0.4869 0.3971 0.084 Uiso 1 1 d R . . H5WB H 0.9325 0.4375 0.4423 0.084 Uiso 1 1 d R . . O6 O 0.4338(5) 0.3152(3) -0.3414(3) 0.0600(14) Uani 1 1 d . . . O6W O 0.9009(5) 0.1930(4) 0.6135(3) 0.0721(15) Uani 1 1 d . . . H6WA H 0.8811 0.2383 0.6512 0.086 Uiso 1 1 d R . . H6WB H 0.9470 0.1361 0.6192 0.086 Uiso 1 1 d R . . O7 O -0.1253(3) 0.7264(3) -0.0644(2) 0.0325(8) Uani 1 1 d . . . O7W O 0.9773(7) 0.8342(5) 0.6703(3) 0.094(2) Uani 1 1 d . . . H7WA H 0.9619 0.7856 0.7016 0.113 Uiso 1 1 d R . . H7WB H 0.9758 0.8132 0.6239 0.113 Uiso 1 1 d R . . O8 O -0.0993(4) 0.8025(4) 0.0442(3) 0.0516(12) Uani 1 1 d . . . O8W O 0.0150(5) 0.0302(5) 0.6963(4) 0.0830(18) Uani 1 1 d . . . H8WA H -0.0128 -0.0235 0.6849 0.100 Uiso 1 1 d R . . H8WB H 0.0111 0.0537 0.7428 0.100 Uiso 1 1 d R . . O9W O 0.8262(7) 0.7664(6) -0.7327(4) 0.105(2) Uiso 1 1 d . . . H9WC H 0.7885 0.7451 -0.7660 0.126 Uiso 1 1 d R . . H9WD H 0.9017 0.7528 -0.7512 0.126 Uiso 1 1 d R . . O10W O 0.3433(8) -0.2687(6) 0.2667(5) 0.116(2) Uani 1 1 d U . . H10B H 0.3144 -0.3205 0.2529 0.140 Uiso 1 1 d R . . H10C H 0.4038 -0.2913 0.2878 0.140 Uiso 1 1 d R . . O11W O 0.9877(9) 0.1187(9) -0.1529(6) 0.154(3) Uani 1 1 d U . . H11D H 0.9651 0.1680 -0.1820 0.184 Uiso 1 1 d R . . H11E H 1.0228 0.1431 -0.1194 0.184 Uiso 1 1 d R . . O12W O 0.6693(7) -0.2839(5) 0.1854(4) 0.097(2) Uani 1 1 d U . . H12B H 0.6697 -0.3233 0.1460 0.116 Uiso 1 1 d R . . H12C H 0.6311 -0.3079 0.2267 0.116 Uiso 1 1 d R . . O13W O 0.9234(14) 0.2597(13) -0.2358(9) 0.245(7) Uiso 1 1 d . . . H13D H 0.9345 0.2180 -0.1988 0.294 Uiso 1 1 d R . . H13E H 0.8675 0.3102 -0.2176 0.294 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0215(3) 0.0252(3) 0.0296(3) -0.0021(3) -0.0101(3) 0.0075(2) Cu2 0.0334(4) 0.0296(4) 0.0262(3) -0.0052(3) -0.0054(3) -0.0072(3) C1 0.038(3) 0.031(3) 0.037(3) -0.005(2) -0.013(3) -0.002(2) C2 0.058(4) 0.033(3) 0.036(3) 0.002(2) -0.014(3) -0.008(3) C3 0.062(4) 0.026(3) 0.038(3) -0.001(2) -0.029(3) 0.005(3) C4 0.046(3) 0.025(3) 0.033(3) -0.008(2) -0.022(3) 0.006(2) C5 0.033(3) 0.023(3) 0.027(3) -0.010(2) -0.016(2) 0.009(2) C6 0.052(4) 0.026(3) 0.041(3) -0.010(2) -0.030(3) 0.018(3) C7 0.037(3) 0.031(3) 0.043(3) -0.014(3) -0.022(3) 0.016(2) C8 0.030(3) 0.028(3) 0.036(3) -0.015(2) -0.019(2) 0.011(2) C9 0.030(3) 0.025(3) 0.029(3) -0.014(2) -0.015(2) 0.008(2) C10 0.025(3) 0.040(3) 0.040(3) -0.015(3) -0.010(2) 0.008(2) C11 0.031(3) 0.040(3) 0.041(3) -0.011(3) -0.010(2) 0.001(2) C12 0.033(3) 0.030(3) 0.034(3) -0.007(2) -0.010(2) 0.007(2) C13 0.064(4) 0.042(4) 0.061(4) 0.011(3) -0.033(4) -0.021(3) C14 0.091(6) 0.052(4) 0.077(5) 0.015(4) -0.053(5) -0.034(4) C15 0.133(8) 0.032(4) 0.067(5) 0.003(4) -0.061(6) -0.016(5) C16 0.068(4) 0.029(3) 0.031(3) -0.004(2) -0.027(3) 0.006(3) C17 0.103(6) 0.034(3) 0.045(4) -0.001(3) -0.048(4) 0.000(4) C18 0.135(8) 0.034(4) 0.044(4) -0.014(3) -0.045(5) 0.031(5) C19 0.092(6) 0.055(5) 0.043(4) -0.012(3) -0.021(4) 0.031(5) C20 0.069(5) 0.051(4) 0.026(3) -0.005(3) -0.016(3) 0.027(4) C21 0.052(4) 0.037(3) 0.027(3) -0.005(2) -0.016(3) 0.010(3) C22 0.047(4) 0.082(6) 0.035(4) 0.010(4) -0.003(3) 0.025(4) C23 0.039(4) 0.079(5) 0.036(3) 0.017(3) -0.007(3) 0.004(3) C24 0.036(3) 0.053(4) 0.026(3) 0.006(3) -0.011(2) -0.005(3) C25 0.028(3) 0.023(2) 0.030(3) -0.007(2) -0.014(2) 0.001(2) C26 0.019(2) 0.026(3) 0.030(3) -0.008(2) -0.008(2) 0.005(2) C27 0.020(2) 0.027(3) 0.022(2) -0.007(2) -0.0057(19) 0.003(2) C28 0.019(2) 0.028(3) 0.022(2) -0.006(2) -0.0079(19) 0.005(2) C29 0.021(2) 0.026(3) 0.023(2) -0.008(2) -0.007(2) 0.003(2) C30 0.024(2) 0.024(2) 0.020(2) -0.0077(19) -0.0066(19) 0.001(2) C31 0.011(2) 0.035(3) 0.028(3) 0.002(2) -0.0017(19) 0.001(2) C32 0.019(2) 0.043(3) 0.028(3) -0.007(2) -0.005(2) 0.006(2) C33 0.022(3) 0.036(3) 0.027(3) 0.000(2) -0.004(2) 0.003(2) C34 0.035(3) 0.026(3) 0.029(3) -0.003(2) -0.004(2) 0.000(2) C35 0.032(3) 0.022(2) 0.021(2) -0.0006(19) -0.005(2) 0.000(2) C36 0.029(3) 0.028(3) 0.023(2) -0.003(2) -0.008(2) -0.002(2) C37 0.028(3) 0.030(3) 0.019(2) 0.001(2) -0.009(2) 0.002(2) C38 0.033(3) 0.025(3) 0.024(3) -0.002(2) -0.010(2) 0.004(2) C39 0.039(3) 0.032(3) 0.042(3) -0.013(2) -0.014(3) 0.003(2) C40 0.033(3) 0.026(3) 0.022(2) 0.000(2) -0.006(2) -0.004(2) C41 0.028(3) 0.022(3) 0.043(3) 0.001(2) -0.007(2) 0.003(2) C42 0.034(3) 0.032(3) 0.038(3) -0.010(2) -0.005(2) -0.005(2) C43 0.036(3) 0.034(3) 0.032(3) -0.004(2) -0.005(2) -0.011(2) C45 0.039(3) 0.018(2) 0.024(2) -0.0008(19) -0.011(2) -0.001(2) C46 0.047(3) 0.023(3) 0.025(3) -0.002(2) -0.005(2) -0.008(2) C47 0.029(3) 0.032(3) 0.026(3) -0.010(2) -0.004(2) -0.001(2) C48 0.027(3) 0.026(3) 0.036(3) -0.002(2) -0.008(2) 0.007(2) N1 0.030(2) 0.023(2) 0.029(2) -0.0050(18) -0.0130(19) 0.0042(18) N2 0.028(2) 0.024(2) 0.031(2) -0.0058(18) -0.0112(19) 0.0074(18) N3 0.041(3) 0.037(3) 0.022(2) -0.0019(19) -0.011(2) 0.003(2) N4 0.052(3) 0.032(3) 0.040(3) 0.003(2) -0.024(2) -0.008(2) O1 0.030(2) 0.046(2) 0.0256(19) 0.0034(16) -0.0109(15) 0.0012(17) O1W 0.048(3) 0.057(3) 0.037(2) -0.012(2) 0.0074(19) -0.019(2) O2 0.0288(19) 0.0274(19) 0.0275(18) -0.0016(15) -0.0049(15) 0.0112(15) O2W 0.214(8) 0.044(3) 0.051(3) 0.003(2) -0.061(4) -0.029(4) O3 0.033(2) 0.054(3) 0.034(2) -0.0066(18) -0.0132(17) 0.0053(18) O3W 0.080(4) 0.069(3) 0.045(3) -0.005(2) -0.014(2) -0.036(3) O4 0.028(2) 0.045(2) 0.035(2) -0.0007(18) -0.0065(16) -0.0064(17) O4W 0.052(3) 0.080(4) 0.051(3) 0.002(3) -0.010(2) -0.027(3) O5 0.035(2) 0.0311(19) 0.0274(19) -0.0029(15) -0.0083(16) -0.0070(16) O5W 0.041(3) 0.071(3) 0.085(4) -0.029(3) 0.003(3) 0.009(2) O6 0.124(5) 0.028(2) 0.039(2) 0.0061(19) -0.029(3) -0.028(3) O6W 0.076(4) 0.067(3) 0.074(4) -0.004(3) -0.007(3) -0.024(3) O7 0.0230(18) 0.036(2) 0.039(2) 0.0037(16) -0.0129(16) 0.0014(15) O7W 0.155(7) 0.081(4) 0.058(3) 0.006(3) -0.019(4) -0.054(4) O8 0.033(2) 0.054(3) 0.058(3) -0.028(2) -0.010(2) 0.021(2) O8W 0.079(4) 0.083(4) 0.082(4) -0.027(3) 0.002(3) -0.020(3) O10W 0.157(5) 0.094(4) 0.117(4) 0.021(3) -0.065(4) -0.030(4) O11W 0.142(5) 0.179(6) 0.145(5) -0.035(4) -0.051(4) -0.019(4) O12W 0.150(4) 0.075(3) 0.062(3) 0.007(3) -0.005(3) -0.026(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O7 1.930(4) 2_565 ? Cu1 O2 1.954(4) . ? Cu1 N2 2.001(4) . ? Cu1 N1 2.008(4) . ? Cu2 O1W 1.949(4) . ? Cu2 O5 1.969(4) 2_664 ? Cu2 N3 2.003(5) . ? Cu2 N4 2.043(5) . ? Cu2 O4 2.267(4) . ? C1 N1 1.316(7) . ? C1 C2 1.399(8) . ? C1 H1A 0.9300 . ? C2 C3 1.374(9) . ? C2 H2A 0.9300 . ? C3 C4 1.384(9) . ? C3 H3A 0.9300 . ? C4 C5 1.419(7) . ? C4 C6 1.438(8) . ? C5 N1 1.357(6) . ? C5 C9 1.420(8) . ? C6 C7 1.350(9) . ? C6 H6A 0.9300 . ? C7 C8 1.430(8) . ? C7 H7A 0.9300 . ? C8 C10 1.402(9) . ? C8 C9 1.418(7) . ? C9 N2 1.353(7) . ? C10 C11 1.380(8) . ? C10 H10A 0.9300 . ? C11 C12 1.395(8) . ? C11 H11A 0.9300 . ? C12 N2 1.323(7) . ? C12 H12A 0.9300 . ? C13 N4 1.326(8) . ? C13 C14 1.411(10) . ? C13 H13A 0.9300 . ? C14 C15 1.342(12) . ? C14 H14A 0.9300 . ? C15 C17 1.402(12) . ? C15 H15A 0.9300 . ? C16 N4 1.352(8) . ? C16 C17 1.412(9) . ? C16 C21 1.422(10) . ? C17 C18 1.434(12) . ? C18 C19 1.357(13) . ? C18 H18A 0.9300 . ? C19 C20 1.423(11) . ? C19 H19A 0.9300 . ? C20 C22 1.386(11) . ? C20 C21 1.414(9) . ? C21 N3 1.359(7) . ? C22 C23 1.353(11) . ? C22 H22A 0.9300 . ? C23 C24 1.394(9) . ? C23 H23A 0.9300 . ? C24 N3 1.329(8) . ? C24 H24A 0.9300 . ? C25 C30 1.401(7) . ? C25 C26 1.410(8) . ? C25 C41 1.510(7) . ? C26 C27 1.392(7) . ? C26 C48 1.523(7) . ? C27 C28 1.408(6) . ? C27 C32 1.507(7) . ? C28 C29 1.403(7) . ? C28 C31 1.508(7) . ? C29 C30 1.398(7) . ? C29 C33 1.511(6) . ? C30 C34 1.528(7) . ? C31 O1 1.236(6) . ? C31 O2 1.290(6) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C35 1.517(7) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.403(7) . ? C35 C40 1.408(7) . ? C36 C37 1.404(7) . ? C36 C42 1.515(7) . ? C37 C38 1.391(7) . ? C37 C47 1.498(7) . ? C38 C45 1.393(8) . ? C38 C39 1.519(7) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 C45 1.406(7) . ? C40 C43 1.509(7) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C45 C46 1.513(7) . ? C46 O6 1.235(7) . ? C46 O5 1.276(6) . ? C47 O4 1.258(7) . ? C47 O3 1.269(6) . ? C48 O8 1.214(6) . ? C48 O7 1.285(6) . ? O1W H1WB 0.8501 . ? O1W H1WA 0.8498 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8500 . ? O3W H3WA 0.8499 . ? O3W H3WB 0.8499 . ? O4W H4WA 0.8501 . ? O4W H4WB 0.8500 . ? O5 Cu2 1.969(3) 2_664 ? O5W H5WA 0.8500 . ? O5W H5WB 0.8499 . ? O6W H6WA 0.8500 . ? O6W H6WB 0.8500 . ? O7 Cu1 1.930(4) 2_565 ? O7W H7WA 0.8500 . ? O7W H7WB 0.8499 . ? O8W H8WA 0.8499 . ? O8W H8WB 0.8499 . ? O9W H9WC 0.8500 . ? O9W H9WD 0.8500 . ? O10W H10B 0.8500 . ? O10W H10C 0.8499 . ? O11W H11D 0.8499 . ? O11W H11E 0.8499 . ? O12W H12B 0.8500 . ? O12W H12C 0.8500 . ? O13W H13D 0.8500 . ? O13W H13E 0.8500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Cu1 O2 90.01(15) 2_565 . ? O7 Cu1 N2 176.29(17) 2_565 . ? O2 Cu1 N2 93.58(16) . . ? O7 Cu1 N1 94.15(17) 2_565 . ? O2 Cu1 N1 174.64(16) . . ? N2 Cu1 N1 82.32(18) . . ? O1W Cu2 O5 93.15(16) . 2_664 ? O1W Cu2 N3 170.7(2) . . ? O5 Cu2 N3 92.24(17) 2_664 . ? O1W Cu2 N4 92.1(2) . . ? O5 Cu2 N4 168.22(17) 2_664 . ? N3 Cu2 N4 81.3(2) . . ? O1W Cu2 O4 82.75(17) . . ? O5 Cu2 O4 103.57(15) 2_664 . ? N3 Cu2 O4 103.34(15) . . ? N4 Cu2 O4 87.56(16) . . ? N1 C1 C2 122.4(5) . . ? N1 C1 H1A 118.8 . . ? C2 C1 H1A 118.8 . . ? C3 C2 C1 119.4(6) . . ? C3 C2 H2A 120.3 . . ? C1 C2 H2A 120.3 . . ? C2 C3 C4 120.1(5) . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? C3 C4 C5 116.7(5) . . ? C3 C4 C6 125.5(5) . . ? C5 C4 C6 117.8(6) . . ? N1 C5 C4 123.0(5) . . ? N1 C5 C9 116.9(4) . . ? C4 C5 C9 120.1(5) . . ? C7 C6 C4 121.7(5) . . ? C7 C6 H6A 119.1 . . ? C4 C6 H6A 119.1 . . ? C6 C7 C8 121.7(5) . . ? C6 C7 H7A 119.1 . . ? C8 C7 H7A 119.1 . . ? C10 C8 C9 117.3(5) . . ? C10 C8 C7 124.9(5) . . ? C9 C8 C7 117.8(5) . . ? N2 C9 C8 122.6(5) . . ? N2 C9 C5 116.6(4) . . ? C8 C9 C5 120.8(5) . . ? C11 C10 C8 119.5(5) . . ? C11 C10 H10A 120.3 . . ? C8 C10 H10A 120.3 . . ? C10 C11 C12 118.9(6) . . ? C10 C11 H11A 120.5 . . ? C12 C11 H11A 120.5 . . ? N2 C12 C11 123.4(5) . . ? N2 C12 H12A 118.3 . . ? C11 C12 H12A 118.3 . . ? N4 C13 C14 120.5(8) . . ? N4 C13 H13A 119.7 . . ? C14 C13 H13A 119.7 . . ? C15 C14 C13 121.4(8) . . ? C15 C14 H14A 119.3 . . ? C13 C14 H14A 119.3 . . ? C14 C15 C17 119.8(7) . . ? C14 C15 H15A 120.1 . . ? C17 C15 H15A 120.1 . . ? N4 C16 C17 124.1(7) . . ? N4 C16 C21 116.8(5) . . ? C17 C16 C21 119.1(6) . . ? C15 C17 C16 115.8(7) . . ? C15 C17 C18 125.9(7) . . ? C16 C17 C18 118.2(8) . . ? C19 C18 C17 122.2(7) . . ? C19 C18 H18A 118.9 . . ? C17 C18 H18A 118.9 . . ? C18 C19 C20 120.9(7) . . ? C18 C19 H19A 119.6 . . ? C20 C19 H19A 119.6 . . ? C22 C20 C21 117.2(6) . . ? C22 C20 C19 124.8(7) . . ? C21 C20 C19 117.9(8) . . ? N3 C21 C20 122.1(6) . . ? N3 C21 C16 116.3(5) . . ? C20 C21 C16 121.6(6) . . ? C23 C22 C20 120.3(6) . . ? C23 C22 H22A 119.9 . . ? C20 C22 H22A 119.9 . . ? C22 C23 C24 119.8(7) . . ? C22 C23 H23A 120.1 . . ? C24 C23 H23A 120.1 . . ? N3 C24 C23 122.0(6) . . ? N3 C24 H24A 119.0 . . ? C23 C24 H24A 119.0 . . ? C30 C25 C26 119.2(5) . . ? C30 C25 C41 121.8(5) . . ? C26 C25 C41 119.0(4) . . ? C27 C26 C25 122.3(4) . . ? C27 C26 C48 117.8(5) . . ? C25 C26 C48 119.7(4) . . ? C26 C27 C28 117.1(5) . . ? C26 C27 C32 121.5(4) . . ? C28 C27 C32 121.4(4) . . ? C29 C28 C27 122.0(4) . . ? C29 C28 C31 119.9(4) . . ? C27 C28 C31 117.9(4) . . ? C30 C29 C28 119.5(4) . . ? C30 C29 C33 121.6(4) . . ? C28 C29 C33 118.9(4) . . ? C29 C30 C25 119.8(5) . . ? C29 C30 C34 122.0(4) . . ? C25 C30 C34 118.2(4) . . ? O1 C31 O2 122.0(5) . . ? O1 C31 C28 123.0(5) . . ? O2 C31 C28 114.9(4) . . ? C27 C32 H32A 109.5 . . ? C27 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C27 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C29 C33 H33A 109.5 . . ? C29 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C29 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 C30 119.4(4) . . ? C35 C34 H34A 107.5 . . ? C30 C34 H34A 107.5 . . ? C35 C34 H34B 107.5 . . ? C30 C34 H34B 107.5 . . ? H34A C34 H34B 107.0 . . ? C36 C35 C40 119.5(4) . . ? C36 C35 C34 119.1(4) . . ? C40 C35 C34 121.3(5) . . ? C35 C36 C37 119.6(5) . . ? C35 C36 C42 122.3(4) . . ? C37 C36 C42 118.1(5) . . ? C38 C37 C36 121.4(5) . . ? C38 C37 C47 118.2(4) . . ? C36 C37 C47 120.3(4) . . ? C37 C38 C45 118.3(4) . . ? C37 C38 C39 118.6(5) . . ? C45 C38 C39 123.1(5) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C45 C40 C35 119.1(5) . . ? C45 C40 C43 119.2(5) . . ? C35 C40 C43 121.7(5) . . ? C25 C41 H41A 109.5 . . ? C25 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C25 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C36 C42 H42A 109.5 . . ? C36 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C36 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C38 C45 C40 121.7(5) . . ? C38 C45 C46 118.5(4) . . ? C40 C45 C46 119.7(5) . . ? O6 C46 O5 124.2(5) . . ? O6 C46 C45 118.8(5) . . ? O5 C46 C45 116.9(4) . . ? O4 C47 O3 124.3(5) . . ? O4 C47 C37 118.1(5) . . ? O3 C47 C37 117.6(5) . . ? O8 C48 O7 124.3(5) . . ? O8 C48 C26 122.3(5) . . ? O7 C48 C26 113.3(4) . . ? C1 N1 C5 118.4(5) . . ? C1 N1 Cu1 129.8(4) . . ? C5 N1 Cu1 111.9(4) . . ? C12 N2 C9 118.3(4) . . ? C12 N2 Cu1 129.3(4) . . ? C9 N2 Cu1 112.4(4) . . ? C24 N3 C21 118.5(5) . . ? C24 N3 Cu2 128.0(4) . . ? C21 N3 Cu2 113.4(4) . . ? C13 N4 C16 118.4(6) . . ? C13 N4 Cu2 129.5(5) . . ? C16 N4 Cu2 112.1(4) . . ? Cu2 O1W H1WB 116.3 . . ? Cu2 O1W H1WA 122.8 . . ? H1WB O1W H1WA 105.8 . . ? C31 O2 Cu1 108.1(3) . . ? H2WA O2W H2WB 108.2 . . ? H3WA O3W H3WB 105.9 . . ? C47 O4 Cu2 133.4(3) . . ? H4WA O4W H4WB 119.2 . . ? C46 O5 Cu2 115.3(3) . 2_664 ? H5WA O5W H5WB 108.7 . . ? H6WA O6W H6WB 119.0 . . ? C48 O7 Cu1 118.5(3) . 2_565 ? H7WA O7W H7WB 107.9 . . ? H8WA O8W H8WB 125.0 . . ? H9WC O9W H9WD 108.8 . . ? H10B O10W H10C 108.7 . . ? H11D O11W H11E 108.4 . . ? H12B O12W H12C 108.9 . . ? H13D O13W H13E 108.8 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 24.84 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 2.835 _refine_diff_density_min -1.033 _refine_diff_density_rms 0.110