Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Li-Min Zheng' 'Feng-Tai Chen' 'Song Gao' 'Dong-Feng Li' 'Yizhi Li' 'Wen-Xia Tang' 'Xin-Yi Wang' _publ_contact_author_name 'Dr Li-Min Zheng' _publ_contact_author_address ; Coordination Chemistry Institute Nanjing University State Key Laboratory of Coordinatio Nanjing 210093 CHINA ; _publ_contact_author_email LMZHENG@NETRA.NJU.EDU.CN _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis, crystal structure and magnetic properties of a Cu(II)-W(V) bimetallic complex with a novel open framework structure ; data_wcu1 _database_code_CSD 208671 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C84 H137 Cu10 N34 O30 W3, 6(H2 O)' _chemical_formula_sum 'C84 H149 Cu10 N34 O36 W3' _chemical_formula_weight 3398.40 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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pbcn ' _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 32.349(2) _cell_length_b 20.892(2) _cell_length_c 21.162(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 14302(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1980 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 17.59 _exptl_crystal_description column _exptl_crystal_colour green _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6764 _exptl_absorpt_coefficient_mu 3.929 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.255 _exptl_absorpt_correction_T_max 0.459 _exptl_absorpt_process_details SADABS,Bruker(2000) _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 Apex CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 80241 _diffrn_reflns_av_R_equivalents 0.0506 _diffrn_reflns_av_sigmaI/netI 0.0909 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 27.02 _reflns_number_total 15528 _reflns_number_gt 9910 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0414P)^2^] 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 15528 _refine_ls_number_parameters 753 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0831 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.0887 _refine_ls_wR_factor_gt 0.0820 _refine_ls_goodness_of_fit_ref 0.891 _refine_ls_restrained_S_all 0.891 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.257910(7) 0.576270(10) 0.525790(10) 0.01928(6) Uani 1 1 d . . . W2 W 0.5000 0.178160(17) 0.2500 0.02833(9) Uani 1 2 d S . . Cu1 Cu 0.23047(2) 0.77948(3) 0.22781(3) 0.02876(18) Uani 1 1 d . . . Cu2 Cu 0.26126(2) 0.76130(3) 0.35570(3) 0.02952(17) Uani 1 1 d . . . Cu3 Cu 0.34867(2) 0.44265(3) 0.36726(3) 0.03068(18) Uani 1 1 d . . . Cu4 Cu 0.39623(2) 0.32413(3) 0.37096(3) 0.02906(17) Uani 1 1 d . . . Cu5 Cu 0.47991(2) 0.02960(3) 0.05422(3) 0.02833(17) Uani 1 1 d . . . C1 C 0.25771(18) 0.6315(2) 0.6147(2) 0.0252(13) Uani 1 1 d . . . C2 C 0.25760(16) 0.6508(2) 0.4574(2) 0.0193(12) Uani 1 1 d . . . C3 C 0.29555(16) 0.5222(3) 0.4600(3) 0.0244(13) Uani 1 1 d . . . C4 C 0.22046(16) 0.5054(3) 0.5742(2) 0.0193(12) Uani 1 1 d . . . C5 C 0.29792(16) 0.5197(2) 0.5828(2) 0.0193(12) Uani 1 1 d . . . C6 C 0.3169(2) 0.6249(3) 0.5288(3) 0.0361(15) Uani 1 1 d . . . C7 C 0.2002(2) 0.6205(3) 0.5412(3) 0.0375(16) Uani 1 1 d . . . C8 C 0.21650(17) 0.5426(3) 0.4531(3) 0.0283(14) Uani 1 1 d . . . C9 C 0.46271(17) 0.2454(3) 0.2935(2) 0.0272(14) Uani 1 1 d . . . C10 C 0.50059(17) 0.1084(3) 0.1811(3) 0.0283(14) Uani 1 1 d . . . C11 C 0.46680(17) 0.2201(3) 0.1752(3) 0.0283(14) Uani 1 1 d . . . C12 C 0.43869(18) 0.1347(3) 0.2548(3) 0.0294(14) Uani 1 1 d . . . C13 C 0.23148(19) 0.6874(3) 0.1244(3) 0.0427(17) Uani 1 1 d . . . H13A H 0.2191 0.6521 0.1014 0.051 Uiso 1 1 calc R . . H13D H 0.2356 0.7223 0.0948 0.051 Uiso 1 1 calc R . . C14 C 0.2715(2) 0.6673(3) 0.1487(3) 0.0445(18) Uani 1 1 d . . . H14A H 0.2907 0.6622 0.1139 0.053 Uiso 1 1 calc R . . H14D H 0.2687 0.6263 0.1697 0.053 Uiso 1 1 calc R . . C15 C 0.1651(2) 0.7360(3) 0.1502(3) 0.0405(17) Uani 1 1 d . . . H15A H 0.1481 0.7016 0.1336 0.049 Uiso 1 1 calc R . . H15B H 0.1731 0.7631 0.1151 0.049 Uiso 1 1 calc R . . C16 C 0.1409(2) 0.7733(3) 0.1945(3) 0.0404(16) Uani 1 1 d . . . H16A H 0.1179 0.7930 0.1725 0.049 Uiso 1 1 calc R . . H16B H 0.1297 0.7453 0.2268 0.049 Uiso 1 1 calc R . . C17 C 0.1919(2) 0.6554(3) 0.2202(3) 0.0392(16) Uani 1 1 d . . . H17A H 0.1976 0.6153 0.1988 0.047 Uiso 1 1 calc R . . H17B H 0.1630 0.6556 0.2325 0.047 Uiso 1 1 calc R . . C18 C 0.2197(2) 0.6620(3) 0.2794(3) 0.0379(16) Uani 1 1 d . . . H18A H 0.2097 0.6340 0.3126 0.045 Uiso 1 1 calc R . . H18B H 0.2477 0.6495 0.2691 0.045 Uiso 1 1 calc R . . C19 C 0.31749(18) 0.8668(3) 0.3490(3) 0.0306(14) Uani 1 1 d . . . H19A H 0.3472 0.8721 0.3451 0.037 Uiso 1 1 calc R . . H19B H 0.3060 0.9061 0.3661 0.037 Uiso 1 1 calc R . . C20 C 0.29824(17) 0.8528(3) 0.2830(3) 0.0298(14) Uani 1 1 d . . . H20A H 0.2971 0.8918 0.2581 0.036 Uiso 1 1 calc R . . H20B H 0.3149 0.8217 0.2604 0.036 Uiso 1 1 calc R . . C21 C 0.29575(18) 0.8387(3) 0.4546(3) 0.0312(15) Uani 1 1 d . . . H21A H 0.2971 0.8047 0.4858 0.037 Uiso 1 1 calc R . . H21B H 0.3150 0.8720 0.4672 0.037 Uiso 1 1 calc R . . C22 C 0.25354(17) 0.8652(3) 0.4532(3) 0.0312(14) Uani 1 1 d . . . H22A H 0.2458 0.8792 0.4953 0.037 Uiso 1 1 calc R . . H22B H 0.2528 0.9021 0.4255 0.037 Uiso 1 1 calc R . . C23 C 0.34620(18) 0.7714(3) 0.3971(3) 0.0323(15) Uani 1 1 d . . . H23A H 0.3421 0.7402 0.4305 0.039 Uiso 1 1 calc R . . H23B H 0.3697 0.7978 0.4085 0.039 Uiso 1 1 calc R . . C24 C 0.35550(18) 0.7366(3) 0.3356(3) 0.0334(15) Uani 1 1 d . . . H24A H 0.3641 0.7671 0.3036 0.040 Uiso 1 1 calc R . . H24B H 0.3777 0.7061 0.3419 0.040 Uiso 1 1 calc R . . C25 C 0.3834(2) 0.4823(3) 0.2488(3) 0.0412(16) Uani 1 1 d . . . H25A H 0.4040 0.5127 0.2342 0.049 Uiso 1 1 calc R . . H25B H 0.3656 0.4717 0.2134 0.049 Uiso 1 1 calc R . . C26 C 0.40404(19) 0.4239(3) 0.2722(3) 0.0398(16) Uani 1 1 d . . . H26A H 0.4137 0.3990 0.2364 0.048 Uiso 1 1 calc R . . H26B H 0.4280 0.4360 0.2970 0.048 Uiso 1 1 calc R . . C27 C 0.3771(2) 0.5658(3) 0.3340(3) 0.0450(17) Uani 1 1 d . . . H27A H 0.3582 0.5793 0.3670 0.054 Uiso 1 1 calc R . . H27B H 0.3802 0.6013 0.3048 0.054 Uiso 1 1 calc R . . C28 C 0.4182(2) 0.5515(3) 0.3629(3) 0.0471(18) Uani 1 1 d . . . H28A H 0.4375 0.5335 0.3326 0.057 Uiso 1 1 calc R . . H28B H 0.4304 0.5888 0.3829 0.057 Uiso 1 1 calc R . . C29 C 0.31573(19) 0.5299(3) 0.2785(3) 0.0420(17) Uani 1 1 d . . . H29A H 0.3029 0.5554 0.3114 0.050 Uiso 1 1 calc R . . H29B H 0.3181 0.5567 0.2412 0.050 Uiso 1 1 calc R . . C30 C 0.2890(2) 0.4763(3) 0.2640(3) 0.0413(17) Uani 1 1 d . . . H30A H 0.2617 0.4920 0.2529 0.050 Uiso 1 1 calc R . . H30B H 0.2999 0.4534 0.2278 0.050 Uiso 1 1 calc R . . C31 C 0.37774(19) 0.3015(3) 0.5003(3) 0.0386(16) Uani 1 1 d . . . H31A H 0.3539 0.2736 0.5039 0.046 Uiso 1 1 calc R . . H31B H 0.3914 0.3025 0.5411 0.046 Uiso 1 1 calc R . . C32 C 0.36395(19) 0.3653(3) 0.4845(3) 0.0375(16) Uani 1 1 d . . . H32A H 0.3861 0.3957 0.4917 0.045 Uiso 1 1 calc R . . H32B H 0.3408 0.3771 0.5111 0.045 Uiso 1 1 calc R . . C33 C 0.45001(19) 0.2824(3) 0.4685(3) 0.0409(16) Uani 1 1 d . . . H33A H 0.4669 0.2676 0.4335 0.049 Uiso 1 1 calc R . . H33B H 0.4559 0.2549 0.5043 0.049 Uiso 1 1 calc R . . C34 C 0.4641(2) 0.3517(3) 0.4857(3) 0.0419(17) Uani 1 1 d . . . H34A H 0.4470 0.3698 0.5189 0.050 Uiso 1 1 calc R . . H34B H 0.4928 0.3525 0.4990 0.050 Uiso 1 1 calc R . . C35 C 0.39929(18) 0.2058(3) 0.4369(3) 0.0394(16) Uani 1 1 d . . . H35A H 0.3989 0.1812 0.4757 0.047 Uiso 1 1 calc R . . H35B H 0.4213 0.1893 0.4104 0.047 Uiso 1 1 calc R . . C36 C 0.35920(18) 0.1987(3) 0.4038(3) 0.0393(16) Uani 1 1 d . . . H36A H 0.3557 0.1544 0.3912 0.047 Uiso 1 1 calc R . . H36B H 0.3370 0.2093 0.4327 0.047 Uiso 1 1 calc R . . C37 C 0.42043(17) -0.0648(3) 0.1423(3) 0.0291(14) Uani 1 1 d . . . H37A H 0.4122 -0.0780 0.1843 0.035 Uiso 1 1 calc R . . H37B H 0.4079 -0.0944 0.1127 0.035 Uiso 1 1 calc R . . C38 C 0.40292(17) -0.0023(3) 0.1308(3) 0.0291(14) Uani 1 1 d . . . H38A H 0.4103 0.0258 0.1656 0.035 Uiso 1 1 calc R . . H38B H 0.3730 -0.0059 0.1301 0.035 Uiso 1 1 calc R . . C39 C 0.41293(17) 0.1337(3) 0.0281(3) 0.0291(14) Uani 1 1 d . . . H39A H 0.4043 0.1769 0.0383 0.035 Uiso 1 1 calc R . . H39B H 0.4003 0.1222 -0.0119 0.035 Uiso 1 1 calc R . . C40 C 0.39786(18) 0.0911(3) 0.0763(3) 0.0288(14) Uani 1 1 d . . . H40A H 0.3681 0.0867 0.0730 0.035 Uiso 1 1 calc R . . H40B H 0.4045 0.1078 0.1178 0.035 Uiso 1 1 calc R . . C41 C 0.39838(17) -0.0089(3) 0.0139(2) 0.0288(14) Uani 1 1 d . . . H41A H 0.3813 -0.0426 0.0313 0.035 Uiso 1 1 calc R . . H41B H 0.3809 0.0188 -0.0115 0.035 Uiso 1 1 calc R . . C42 C 0.43142(17) -0.0374(3) -0.0265(3) 0.0288(13) Uani 1 1 d . . . H42A H 0.4381 -0.0792 -0.0093 0.035 Uiso 1 1 calc R . . H42B H 0.4198 -0.0443 -0.0682 0.035 Uiso 1 1 calc R . . N1 N 0.25755(14) 0.6615(2) 0.6581(2) 0.0255(11) Uani 1 1 d . . . N2 N 0.25881(13) 0.69183(19) 0.41899(19) 0.0198(10) Uani 1 1 d . . . N3 N 0.31638(13) 0.4938(2) 0.4260(2) 0.0247(11) Uani 1 1 d . . . N4 N 0.20270(14) 0.4648(2) 0.5976(2) 0.0261(11) Uani 1 1 d . . . N5 N 0.32130(14) 0.4849(2) 0.6101(2) 0.0256(11) Uani 1 1 d . . . N6 N 0.34879(17) 0.6510(2) 0.5262(2) 0.0383(13) Uani 1 1 d . . . N7 N 0.16971(16) 0.6454(3) 0.5510(2) 0.0389(13) Uani 1 1 d . . . N8 N 0.19662(14) 0.5243(2) 0.4143(2) 0.0305(12) Uani 1 1 d . . . N9 N 0.43969(14) 0.2843(2) 0.3198(2) 0.0276(11) Uani 1 1 d . . . N10 N 0.49853(13) 0.0762(2) 0.1349(2) 0.0283(11) Uani 1 1 d . . . N11 N 0.45136(14) 0.2418(2) 0.1287(2) 0.0308(12) Uani 1 1 d . . . N12 N 0.40617(15) 0.1086(2) 0.2599(2) 0.0315(12) Uani 1 1 d . . . N13 N 0.20057(16) 0.7099(2) 0.1776(2) 0.0407(14) Uani 1 1 d . . . N14 N 0.30818(14) 0.8129(2) 0.3915(2) 0.0312(12) Uani 1 1 d . . . N15 N 0.35865(16) 0.5113(2) 0.2999(3) 0.0427(14) Uani 1 1 d . . . N16 N 0.40737(16) 0.2737(3) 0.4516(2) 0.0396(13) Uani 1 1 d . . . N17 N 0.41765(14) 0.0294(2) 0.0671(2) 0.0288(11) Uani 1 1 d . . . O1 O 0.21904(12) 0.72474(19) 0.29994(18) 0.0362(10) Uani 1 1 d . . . O2 O 0.28750(13) 0.7145(2) 0.19295(19) 0.0459(12) Uani 1 1 d . . . H2C H 0.2997 0.6975 0.2244 0.055 Uiso 1 1 d R . . O3 O 0.16530(13) 0.82163(19) 0.22340(19) 0.0401(11) Uani 1 1 d . . . H3D H 0.1567 0.8299 0.2605 0.048 Uiso 1 1 d R . . O4 O 0.25846(12) 0.82889(17) 0.29250(17) 0.0289(9) Uani 1 1 d . . . O5 O 0.22502(12) 0.81914(17) 0.43175(17) 0.0311(10) Uani 1 1 d . . . H5D H 0.2037 0.8368 0.4158 0.037 Uiso 1 1 d R . . O6 O 0.32026(12) 0.70529(18) 0.31613(18) 0.0341(10) Uani 1 1 d . . . O7 O 0.37782(12) 0.38555(19) 0.30941(19) 0.0382(11) Uani 1 1 d . . . O8 O 0.28593(12) 0.43623(19) 0.31316(19) 0.0406(11) Uani 1 1 d . . . H8D H 0.2814 0.3980 0.3012 0.049 Uiso 1 1 d R . . O9 O 0.40473(13) 0.5057(2) 0.4076(2) 0.0489(12) Uani 1 1 d . . . H9B H 0.4276 0.4778 0.4185 0.059 Uiso 1 1 d R . . O10 O 0.35162(12) 0.36689(19) 0.41851(18) 0.0366(10) Uani 1 1 d . . . O11 O 0.45841(12) 0.3857(2) 0.4263(2) 0.0447(11) Uani 1 1 d . . . H11C H 0.4419 0.3732 0.4092 0.054 Uiso 1 1 d R . . O12 O 0.35632(12) 0.2367(2) 0.35174(18) 0.0390(11) Uani 1 1 d . . . H12D H 0.3314 0.2479 0.3451 0.047 Uiso 1 1 d R . . O13 O 0.46400(11) -0.07183(18) 0.13782(17) 0.0307(9) Uani 1 1 d . . . H13E H 0.4727 -0.0444 0.1128 0.037 Uiso 0.50 1 d PR . . O14 O 0.45745(11) 0.13293(18) 0.02061(17) 0.0307(9) Uani 1 1 d . . . H14B H 0.4676 0.1609 0.0453 0.037 Uiso 1 1 d R . . O15 O 0.46647(11) -0.00575(18) -0.03365(17) 0.0307(9) Uani 1 1 d . . . O1W O 0.35945(11) 0.77405(17) 0.14863(16) 0.0295(9) Uani 1 1 d . . . H111 H 0.3480 0.7900 0.1161 0.035 Uiso 1 1 d R . . H112 H 0.3415 0.7689 0.1775 0.035 Uiso 1 1 d R . . O2W O 0.42852(11) 0.69814(17) 0.50363(17) 0.0295(9) Uani 1 1 d . . . H212 H 0.4387 0.6984 0.5406 0.035 Uiso 1 1 d R . . H211 H 0.4025 0.7038 0.5058 0.035 Uiso 1 1 d R . . O3W O 0.36631(11) 0.00364(17) 0.31113(17) 0.0295(9) Uani 1 1 d . . . H312 H 0.3785 0.0357 0.2948 0.035 Uiso 1 1 d R . . H311 H 0.3682 0.0056 0.3512 0.035 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 W1 0.02805(12) 0.01802(11) 0.01176(10) -0.00054(10) 0.00118(10) 0.00227(11) W2 0.02540(19) 0.0327(2) 0.02689(19) 0.000 0.00035(15) 0.000 Cu1 0.0365(4) 0.0283(4) 0.0216(4) 0.0001(3) -0.0001(3) 0.0001(3) Cu2 0.0398(4) 0.0297(4) 0.0191(4) 0.0055(3) -0.0016(3) -0.0070(3) Cu3 0.0365(4) 0.0300(4) 0.0256(4) -0.0037(3) 0.0024(3) 0.0037(3) Cu4 0.0353(4) 0.0287(4) 0.0232(4) -0.0016(3) 0.0021(3) 0.0039(3) Cu5 0.0254(4) 0.0327(4) 0.0269(4) 0.0000(3) 0.0004(3) 0.0000(3) C1 0.044(4) 0.016(3) 0.016(3) -0.003(2) -0.008(3) 0.011(3) C2 0.028(3) 0.018(3) 0.012(3) -0.001(2) 0.001(2) 0.002(2) C3 0.027(3) 0.018(3) 0.028(3) -0.011(3) -0.008(3) 0.010(2) C4 0.028(3) 0.018(3) 0.012(3) -0.001(2) 0.001(2) 0.002(3) C5 0.028(3) 0.018(3) 0.012(3) -0.001(2) 0.001(2) 0.002(2) C6 0.056(5) 0.025(3) 0.027(3) -0.009(3) 0.005(3) -0.009(3) C7 0.032(4) 0.039(4) 0.041(4) -0.007(3) -0.005(3) -0.004(3) C8 0.022(3) 0.037(4) 0.026(3) -0.004(3) 0.001(3) -0.003(3) C9 0.031(3) 0.038(4) 0.013(3) 0.006(3) 0.000(3) -0.004(3) C10 0.025(3) 0.033(4) 0.027(3) 0.000(3) 0.000(3) 0.000(3) C11 0.025(3) 0.033(4) 0.027(3) 0.000(3) 0.000(3) 0.000(3) C12 0.034(4) 0.018(3) 0.037(4) 0.014(3) 0.003(3) 0.006(3) C13 0.056(5) 0.041(4) 0.031(4) 0.002(3) -0.014(3) -0.004(3) C14 0.058(5) 0.043(4) 0.032(4) 0.003(3) -0.014(3) -0.003(3) C15 0.053(4) 0.039(4) 0.030(4) 0.002(3) -0.014(3) -0.005(3) C16 0.053(4) 0.039(4) 0.030(4) 0.003(3) -0.015(3) -0.005(3) C17 0.053(4) 0.038(4) 0.027(4) 0.003(3) -0.013(3) -0.006(3) C18 0.051(4) 0.037(4) 0.026(3) 0.004(3) -0.012(3) -0.007(3) C19 0.038(4) 0.024(3) 0.030(4) 0.000(3) -0.005(3) 0.001(3) C20 0.037(4) 0.024(3) 0.029(4) -0.001(3) -0.005(3) 0.001(3) C21 0.038(4) 0.025(4) 0.031(4) 0.000(3) -0.004(3) 0.002(3) C22 0.038(4) 0.025(3) 0.030(3) 0.000(3) -0.004(3) 0.003(3) C23 0.039(4) 0.026(3) 0.032(4) 0.000(3) -0.004(3) 0.002(3) C24 0.040(4) 0.027(4) 0.033(4) 0.000(3) -0.003(3) 0.003(3) C25 0.049(4) 0.032(4) 0.043(4) -0.003(3) 0.000(3) -0.005(3) C26 0.048(4) 0.030(4) 0.041(4) -0.004(3) 0.000(3) -0.004(3) C27 0.052(4) 0.035(4) 0.048(4) -0.002(3) -0.001(3) -0.006(3) C28 0.054(5) 0.037(4) 0.050(5) -0.003(4) -0.001(4) -0.006(3) C29 0.049(4) 0.032(4) 0.044(4) -0.002(3) 0.000(3) -0.006(3) C30 0.048(4) 0.032(4) 0.043(4) -0.003(3) 0.000(3) -0.006(3) C31 0.039(4) 0.047(4) 0.030(4) 0.001(3) -0.003(3) 0.008(3) C32 0.038(4) 0.046(4) 0.029(4) 0.000(3) -0.003(3) 0.008(3) C33 0.040(4) 0.049(4) 0.033(4) 0.001(3) -0.004(3) 0.008(3) C34 0.041(4) 0.050(4) 0.035(4) 0.001(3) -0.004(3) 0.007(3) C35 0.039(4) 0.046(4) 0.032(4) 0.001(3) -0.003(3) 0.006(3) C36 0.039(4) 0.046(4) 0.033(4) 0.000(3) -0.003(3) 0.006(3) C37 0.035(4) 0.029(4) 0.023(3) -0.002(3) 0.002(3) 0.004(3) C38 0.035(4) 0.029(3) 0.023(3) -0.002(3) 0.002(3) 0.004(3) C39 0.035(4) 0.029(3) 0.023(3) -0.002(3) 0.002(3) 0.004(3) C40 0.036(4) 0.028(4) 0.022(3) 0.000(3) 0.000(3) 0.000(3) C41 0.036(4) 0.028(3) 0.022(3) 0.000(3) 0.000(3) 0.000(3) C42 0.036(4) 0.028(3) 0.022(3) 0.000(3) 0.000(3) 0.000(3) N1 0.044(3) 0.016(3) 0.016(2) -0.0038(19) -0.008(2) 0.011(2) N2 0.029(3) 0.019(2) 0.012(2) 0.0001(18) 0.001(2) 0.002(2) N3 0.027(3) 0.019(3) 0.029(3) -0.011(2) -0.008(2) 0.010(2) N4 0.034(3) 0.025(3) 0.019(3) 0.003(2) 0.001(2) 0.002(2) N5 0.035(3) 0.024(3) 0.018(3) -0.002(2) -0.001(2) 0.004(2) N6 0.058(4) 0.028(3) 0.029(3) -0.009(2) 0.005(3) -0.009(3) N7 0.034(3) 0.041(3) 0.042(3) -0.006(3) -0.005(3) -0.004(3) N8 0.024(3) 0.039(3) 0.028(3) -0.003(2) 0.002(2) -0.002(2) N9 0.031(3) 0.038(3) 0.013(2) 0.006(2) 0.000(2) -0.003(2) N10 0.025(3) 0.033(3) 0.027(3) 0.000(2) 0.000(2) 0.000(2) N11 0.027(3) 0.033(3) 0.032(3) -0.001(2) 0.003(2) 0.008(2) N12 0.036(3) 0.021(3) 0.038(3) 0.014(2) 0.003(2) 0.006(2) N13 0.054(4) 0.039(3) 0.029(3) 0.003(3) -0.014(3) -0.005(3) N14 0.038(3) 0.025(3) 0.031(3) 0.000(2) -0.004(2) 0.002(2) N15 0.050(4) 0.033(3) 0.045(4) -0.003(3) 0.000(3) -0.005(3) N16 0.039(3) 0.047(4) 0.032(3) 0.001(3) -0.003(2) 0.007(3) N17 0.036(3) 0.028(3) 0.022(3) 0.000(2) 0.000(2) 0.000(2) O1 0.050(3) 0.035(3) 0.023(2) 0.005(2) -0.0125(19) -0.007(2) O2 0.059(3) 0.045(3) 0.033(3) 0.003(2) -0.016(2) -0.003(2) O3 0.052(3) 0.038(3) 0.030(2) 0.002(2) -0.015(2) -0.005(2) O4 0.037(2) 0.023(2) 0.028(2) -0.0006(17) -0.0053(18) -0.0003(19) O5 0.037(2) 0.025(2) 0.030(2) 0.0010(19) -0.0050(19) 0.0028(19) O6 0.041(3) 0.028(2) 0.033(3) -0.0003(19) -0.0031(19) 0.002(2) O7 0.046(3) 0.029(2) 0.039(3) -0.004(2) 0.000(2) -0.004(2) O8 0.048(3) 0.032(3) 0.042(3) -0.003(2) 0.000(2) -0.006(2) O9 0.056(3) 0.039(3) 0.052(3) -0.003(2) -0.002(2) -0.006(2) O10 0.037(2) 0.045(3) 0.028(2) 0.000(2) -0.0027(19) 0.008(2) O11 0.044(3) 0.051(3) 0.039(3) 0.000(2) -0.003(2) 0.007(2) O12 0.039(3) 0.046(3) 0.032(3) 0.000(2) -0.003(2) 0.005(2) O13 0.036(2) 0.030(2) 0.026(2) -0.0037(19) 0.0024(17) 0.0037(19) O14 0.036(2) 0.030(2) 0.026(2) -0.0037(19) 0.0024(18) 0.0037(18) O15 0.036(2) 0.030(2) 0.026(2) -0.0037(18) 0.0024(18) 0.0037(19) O1W 0.040(2) 0.030(2) 0.019(2) 0.0055(17) -0.0016(17) -0.0070(19) O2W 0.040(2) 0.030(2) 0.019(2) 0.0055(18) -0.0016(18) -0.0070(19) O3W 0.040(2) 0.030(2) 0.019(2) 0.0055(18) -0.0016(18) -0.0070(19) _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 W1 C7 2.107(7) . ? W1 C2 2.126(5) . ? W1 C5 2.128(5) . ? W1 C8 2.157(6) . ? W1 C6 2.162(7) . ? W1 C3 2.168(5) . ? W1 C4 2.170(5) . ? W1 C1 2.208(5) . ? W2 C10 2.062(6) . ? W2 C10 2.062(6) 3_655 ? W2 C9 2.068(6) 3_655 ? W2 C9 2.068(6) . ? W2 C11 2.105(6) 3_655 ? W2 C11 2.105(6) . ? W2 C12 2.183(6) 3_655 ? W2 C12 2.183(6) . ? Cu1 O4 1.939(4) . ? Cu1 O1 1.943(4) . ? Cu1 N1 1.961(4) 2_564 ? Cu1 N13 2.044(5) . ? Cu1 O3 2.287(4) . ? Cu1 O2 2.407(4) . ? Cu1 Cu2 2.9088(10) . ? Cu2 O4 1.947(4) . ? Cu2 O1 1.960(4) . ? Cu2 N2 1.977(4) . ? Cu2 N14 2.010(5) . ? Cu2 O5 2.329(4) . ? Cu2 O6 2.390(4) . ? Cu3 O10 1.921(4) . ? Cu3 N3 1.943(4) . ? Cu3 O7 1.952(4) . ? Cu3 N15 2.049(5) . ? Cu3 O8 2.334(4) . ? Cu3 O9 2.398(4) . ? Cu3 Cu4 2.9162(10) . ? Cu4 O7 1.923(4) . ? Cu4 N9 1.960(5) . ? Cu4 O10 1.973(4) . ? Cu4 N16 2.038(5) . ? Cu4 O12 2.274(4) . ? Cu4 H11C 1.9728 . ? Cu5 O15 1.856(4) 5_655 ? Cu5 N17 2.032(5) . ? Cu5 O15 2.047(4) . ? Cu5 N10 2.056(5) . ? Cu5 O14 2.386(4) . ? Cu5 Cu5 2.9129(14) 5_655 ? Cu5 H13E 1.9965 . ? C1 N1 1.112(6) . ? C2 N2 1.182(6) . ? C3 N3 1.150(6) . ? C4 N4 1.138(6) . ? C5 N5 1.197(6) . ? C6 N6 1.168(7) . ? C7 N7 1.135(7) . ? C8 N8 1.111(6) . ? C9 N9 1.235(7) . ? C10 N10 1.188(7) . ? C11 N11 1.193(7) . ? C12 N12 1.190(7) . ? C13 C14 1.454(8) . ? C13 N13 1.577(8) . ? C13 H13A 0.9700 . ? C13 H13D 0.9700 . ? C14 O2 1.455(7) . ? C14 H14A 0.9700 . ? C14 H14D 0.9700 . ? C15 N13 1.398(7) . ? C15 C16 1.448(8) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 O3 1.420(7) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 N13 1.479(7) . ? C17 C18 1.547(8) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 O1 1.381(7) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 N14 1.474(7) . ? C19 C20 1.558(7) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 O4 1.395(6) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.474(7) . ? C21 N14 1.495(7) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 O5 1.408(6) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 N14 1.509(7) . ? C23 C24 1.520(7) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 O6 1.378(6) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 N15 1.476(8) . ? C25 C26 1.477(8) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 O7 1.408(7) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 N15 1.474(7) . ? C27 C28 1.495(8) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 O9 1.413(7) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.449(8) . ? C29 N15 1.511(7) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 O8 1.340(7) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.446(8) . ? C31 N16 1.522(7) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 O10 1.452(6) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 N16 1.436(7) . ? C33 C34 1.562(8) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 O11 1.456(7) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 N16 1.475(8) . ? C35 C36 1.482(8) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 O12 1.361(7) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 O13 1.420(6) . ? C37 C38 1.444(7) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 N17 1.576(7) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.438(7) . ? C39 O14 1.449(6) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 N17 1.452(7) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.493(7) . ? C41 N17 1.515(7) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 O15 1.321(6) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? N1 Cu1 1.961(4) 2_565 ? O2 H2C 0.8504 . ? O3 H3D 0.8499 . ? O5 H5D 0.8501 . ? O8 H8D 0.8501 . ? O9 H9B 0.9700 . ? O11 H11C 0.6948 . ? O12 H12D 0.8501 . ? O13 H13E 0.8281 . ? O14 H14B 0.8499 . ? O15 Cu5 1.856(4) 5_655 ? O1W H111 0.8493 . ? O1W H112 0.8506 . ? O2W H212 0.8498 . ? O2W H211 0.8501 . ? O3W H312 0.8498 . ? O3W H311 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 C7 W1 C2 77.3(2) . . ? C7 W1 C5 134.0(2) . . ? C2 W1 C5 142.7(2) . . ? C7 W1 C8 72.8(2) . . ? C2 W1 C8 75.6(2) . . ? C5 W1 C8 126.9(2) . . ? C7 W1 C6 124.7(2) . . ? C2 W1 C6 71.3(2) . . ? C5 W1 C6 73.0(2) . . ? C8 W1 C6 136.2(2) . . ? C7 W1 C3 145.6(2) . . ? C2 W1 C3 87.0(2) . . ? C5 W1 C3 74.55(19) . . ? C8 W1 C3 73.8(2) . . ? C6 W1 C3 76.6(2) . . ? C7 W1 C4 74.5(2) . . ? C2 W1 C4 144.9(2) . . ? C5 W1 C4 72.12(19) . . ? C8 W1 C4 76.5(2) . . ? C6 W1 C4 143.1(2) . . ? C3 W1 C4 105.1(2) . . ? C7 W1 C1 68.7(2) . . ? C2 W1 C1 101.36(19) . . ? C5 W1 C1 78.95(19) . . ? C8 W1 C1 140.9(2) . . ? C6 W1 C1 74.5(2) . . ? C3 W1 C1 145.3(2) . . ? C4 W1 C1 87.3(2) . . ? C10 W2 C10 90.0(3) . 3_655 ? C10 W2 C9 99.2(2) . 3_655 ? C10 W2 C9 143.2(2) 3_655 3_655 ? C10 W2 C9 143.2(2) . . ? C10 W2 C9 99.2(2) 3_655 . ? C9 W2 C9 94.4(3) 3_655 . ? C10 W2 C11 145.3(2) . 3_655 ? C10 W2 C11 76.5(2) 3_655 3_655 ? C9 W2 C11 75.8(2) 3_655 3_655 ? C9 W2 C11 71.3(2) . 3_655 ? C10 W2 C11 76.5(2) . . ? C10 W2 C11 145.3(2) 3_655 . ? C9 W2 C11 71.3(2) 3_655 . ? C9 W2 C11 75.8(2) . . ? C11 W2 C11 130.8(3) 3_655 . ? C10 W2 C12 70.4(2) . 3_655 ? C10 W2 C12 75.4(2) 3_655 3_655 ? C9 W2 C12 74.4(2) 3_655 3_655 ? C9 W2 C12 146.4(2) . 3_655 ? C11 W2 C12 75.2(2) 3_655 3_655 ? C11 W2 C12 127.0(2) . 3_655 ? C10 W2 C12 75.4(2) . . ? C10 W2 C12 70.4(2) 3_655 . ? C9 W2 C12 146.4(2) 3_655 . ? C9 W2 C12 74.4(2) . . ? C11 W2 C12 127.0(2) 3_655 . ? C11 W2 C12 75.2(2) . . ? C12 W2 C12 130.9(3) 3_655 . ? O4 Cu1 O1 81.23(15) . . ? O4 Cu1 N1 95.98(17) . 2_564 ? O1 Cu1 N1 176.99(18) . 2_564 ? O4 Cu1 N13 165.14(18) . . ? O1 Cu1 N13 84.22(18) . . ? N1 Cu1 N13 98.62(19) 2_564 . ? O4 Cu1 O3 104.73(15) . . ? O1 Cu1 O3 94.78(16) . . ? N1 Cu1 O3 84.80(17) 2_564 . ? N13 Cu1 O3 79.42(18) . . ? O4 Cu1 O2 99.15(15) . . ? O1 Cu1 O2 93.12(16) . . ? N1 Cu1 O2 88.44(16) 2_564 . ? N13 Cu1 O2 78.58(18) . . ? O3 Cu1 O2 155.72(14) . . ? O4 Cu1 Cu2 41.64(11) . . ? O1 Cu1 Cu2 42.04(11) . . ? N1 Cu1 Cu2 135.59(14) 2_564 . ? N13 Cu1 Cu2 123.55(14) . . ? O3 Cu1 Cu2 113.83(11) . . ? O2 Cu1 Cu2 87.08(10) . . ? O4 Cu2 O1 80.60(15) . . ? O4 Cu2 N2 174.98(17) . . ? O1 Cu2 N2 95.39(17) . . ? O4 Cu2 N14 84.58(17) . . ? O1 Cu2 N14 164.22(18) . . ? N2 Cu2 N14 99.69(18) . . ? O4 Cu2 O5 94.30(14) . . ? O1 Cu2 O5 105.51(16) . . ? N2 Cu2 O5 83.83(15) . . ? N14 Cu2 O5 80.86(17) . . ? O4 Cu2 O6 98.72(15) . . ? O1 Cu2 O6 98.90(16) . . ? N2 Cu2 O6 84.83(15) . . ? N14 Cu2 O6 77.98(17) . . ? O5 Cu2 O6 153.90(13) . . ? O4 Cu2 Cu1 41.43(11) . . ? O1 Cu2 Cu1 41.59(11) . . ? N2 Cu2 Cu1 135.45(12) . . ? N14 Cu2 Cu1 122.66(14) . . ? O5 Cu2 Cu1 113.75(10) . . ? O6 Cu2 Cu1 90.65(9) . . ? O10 Cu3 N3 96.81(18) . . ? O10 Cu3 O7 80.01(17) . . ? N3 Cu3 O7 175.24(18) . . ? O10 Cu3 N15 164.21(19) . . ? N3 Cu3 N15 98.3(2) . . ? O7 Cu3 N15 85.15(19) . . ? O10 Cu3 O8 105.83(16) . . ? N3 Cu3 O8 82.99(16) . . ? O7 Cu3 O8 94.43(15) . . ? N15 Cu3 O8 80.55(18) . . ? O10 Cu3 O9 102.37(16) . . ? N3 Cu3 O9 82.94(17) . . ? O7 Cu3 O9 101.16(16) . . ? N15 Cu3 O9 75.14(18) . . ? O8 Cu3 O9 149.71(15) . . ? O10 Cu3 Cu4 42.19(11) . . ? N3 Cu3 Cu4 137.15(14) . . ? O7 Cu3 Cu4 40.81(12) . . ? N15 Cu3 Cu4 122.03(15) . . ? O8 Cu3 Cu4 115.03(10) . . ? O9 Cu3 Cu4 93.32(11) . . ? O7 Cu4 N9 97.52(18) . . ? O7 Cu4 O10 79.44(17) . . ? N9 Cu4 O10 176.95(18) . . ? O7 Cu4 N16 165.26(19) . . ? N9 Cu4 N16 96.70(19) . . ? O10 Cu4 N16 86.35(18) . . ? O7 Cu4 O12 103.83(16) . . ? N9 Cu4 O12 88.13(17) . . ? O10 Cu4 O12 92.28(16) . . ? N16 Cu4 O12 80.48(18) . . ? O7 Cu4 Cu3 41.57(12) . . ? N9 Cu4 Cu3 136.38(13) . . ? O10 Cu4 Cu3 40.83(12) . . ? N16 Cu4 Cu3 123.70(15) . . ? O12 Cu4 Cu3 112.20(11) . . ? O7 Cu4 H11C 99.4 . . ? N9 Cu4 H11C 84.9 . . ? O10 Cu4 H11C 95.9 . . ? N16 Cu4 H11C 78.0 . . ? O12 Cu4 H11C 156.4 . . ? Cu3 Cu4 H11C 88.0 . . ? O15 Cu5 N17 163.09(18) 5_655 . ? O15 Cu5 O15 83.61(17) 5_655 . ? N17 Cu5 O15 84.85(16) . . ? O15 Cu5 N10 92.76(17) 5_655 . ? N17 Cu5 N10 100.39(18) . . ? O15 Cu5 N10 170.89(17) . . ? O15 Cu5 O14 117.22(15) 5_655 . ? N17 Cu5 O14 74.91(16) . . ? O15 Cu5 O14 89.48(14) . . ? N10 Cu5 O14 84.75(16) . . ? O15 Cu5 Cu5 44.31(12) 5_655 5_655 ? N17 Cu5 Cu5 123.14(13) . 5_655 ? O15 Cu5 Cu5 39.30(10) . 5_655 ? N10 Cu5 Cu5 136.44(13) . 5_655 ? O14 Cu5 Cu5 106.57(9) . 5_655 ? O15 Cu5 H13E 92.7 5_655 . ? N17 Cu5 H13E 78.4 . . ? O15 Cu5 H13E 105.1 . . ? N10 Cu5 H13E 83.4 . . ? O14 Cu5 H13E 148.3 . . ? Cu5 Cu5 H13E 102.3 5_655 . ? N1 C1 W1 177.2(5) . . ? N2 C2 W1 177.7(5) . . ? N3 C3 W1 178.2(5) . . ? N4 C4 W1 174.9(5) . . ? N5 C5 W1 174.1(4) . . ? N6 C6 W1 175.7(5) . . ? N7 C7 W1 177.9(6) . . ? N8 C8 W1 177.0(5) . . ? N9 C9 W2 178.3(5) . . ? N10 C10 W2 168.9(5) . . ? N11 C11 W2 173.0(5) . . ? N12 C12 W2 176.1(5) . . ? C14 C13 N13 113.5(5) . . ? C14 C13 H13A 108.9 . . ? N13 C13 H13A 108.9 . . ? C14 C13 H13D 108.9 . . ? N13 C13 H13D 108.9 . . ? H13A C13 H13D 107.7 . . ? C13 C14 O2 110.4(5) . . ? C13 C14 H14A 109.6 . . ? O2 C14 H14A 109.6 . . ? C13 C14 H14D 109.6 . . ? O2 C14 H14D 109.6 . . ? H14A C14 H14D 108.1 . . ? N13 C15 C16 112.6(5) . . ? N13 C15 H15A 109.1 . . ? C16 C15 H15A 109.1 . . ? N13 C15 H15B 109.1 . . ? C16 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? O3 C16 C15 111.2(5) . . ? O3 C16 H16A 109.4 . . ? C15 C16 H16A 109.4 . . ? O3 C16 H16B 109.4 . . ? C15 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? N13 C17 C18 108.3(5) . . ? N13 C17 H17A 110.0 . . ? C18 C17 H17A 110.0 . . ? N13 C17 H17B 110.0 . . ? C18 C17 H17B 110.0 . . ? H17A C17 H17B 108.4 . . ? O1 C18 C17 109.3(5) . . ? O1 C18 H18A 109.8 . . ? C17 C18 H18A 109.8 . . ? O1 C18 H18B 109.8 . . ? C17 C18 H18B 109.8 . . ? H18A C18 H18B 108.3 . . ? N14 C19 C20 108.8(5) . . ? N14 C19 H19A 109.9 . . ? C20 C19 H19A 109.9 . . ? N14 C19 H19B 109.9 . . ? C20 C19 H19B 109.9 . . ? H19A C19 H19B 108.3 . . ? O4 C20 C19 107.8(5) . . ? O4 C20 H20A 110.1 . . ? C19 C20 H20A 110.1 . . ? O4 C20 H20B 110.1 . . ? C19 C20 H20B 110.1 . . ? H20A C20 H20B 108.5 . . ? C22 C21 N14 111.5(5) . . ? C22 C21 H21A 109.3 . . ? N14 C21 H21A 109.3 . . ? C22 C21 H21B 109.3 . . ? N14 C21 H21B 109.3 . . ? H21A C21 H21B 108.0 . . ? O5 C22 C21 110.9(5) . . ? O5 C22 H22A 109.5 . . ? C21 C22 H22A 109.5 . . ? O5 C22 H22B 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 108.0 . . ? N14 C23 C24 111.7(5) . . ? N14 C23 H23A 109.3 . . ? C24 C23 H23A 109.3 . . ? N14 C23 H23B 109.3 . . ? C24 C23 H23B 109.3 . . ? H23A C23 H23B 107.9 . . ? O6 C24 C23 108.6(5) . . ? O6 C24 H24A 110.0 . . ? C23 C24 H24A 110.0 . . ? O6 C24 H24B 110.0 . . ? C23 C24 H24B 110.0 . . ? H24A C24 H24B 108.4 . . ? N15 C25 C26 109.8(5) . . ? N15 C25 H25A 109.7 . . ? C26 C25 H25A 109.7 . . ? N15 C25 H25B 109.7 . . ? C26 C25 H25B 109.7 . . ? H25A C25 H25B 108.2 . . ? O7 C26 C25 112.7(5) . . ? O7 C26 H26A 109.1 . . ? C25 C26 H26A 109.1 . . ? O7 C26 H26B 109.1 . . ? C25 C26 H26B 109.1 . . ? H26A C26 H26B 107.8 . . ? N15 C27 C28 114.0(5) . . ? N15 C27 H27A 108.8 . . ? C28 C27 H27A 108.8 . . ? N15 C27 H27B 108.8 . . ? C28 C27 H27B 108.8 . . ? H27A C27 H27B 107.7 . . ? O9 C28 C27 97.8(5) . . ? O9 C28 H28A 112.2 . . ? C27 C28 H28A 112.2 . . ? O9 C28 H28B 112.2 . . ? C27 C28 H28B 112.2 . . ? H28A C28 H28B 109.8 . . ? C30 C29 N15 114.4(5) . . ? C30 C29 H29A 108.7 . . ? N15 C29 H29A 108.7 . . ? C30 C29 H29B 108.7 . . ? N15 C29 H29B 108.7 . . ? H29A C29 H29B 107.6 . . ? O8 C30 C29 111.3(5) . . ? O8 C30 H30A 109.4 . . ? C29 C30 H30A 109.4 . . ? O8 C30 H30B 109.4 . . ? C29 C30 H30B 109.4 . . ? H30A C30 H30B 108.0 . . ? C32 C31 N16 112.9(5) . . ? C32 C31 H31A 109.0 . . ? N16 C31 H31A 109.0 . . ? C32 C31 H31B 109.0 . . ? N16 C31 H31B 109.0 . . ? H31A C31 H31B 107.8 . . ? C31 C32 O10 109.2(5) . . ? C31 C32 H32A 109.8 . . ? O10 C32 H32A 109.8 . . ? C31 C32 H32B 109.8 . . ? O10 C32 H32B 109.8 . . ? H32A C32 H32B 108.3 . . ? N16 C33 C34 117.1(5) . . ? N16 C33 H33A 108.0 . . ? C34 C33 H33A 108.0 . . ? N16 C33 H33B 108.0 . . ? C34 C33 H33B 108.0 . . ? H33A C33 H33B 107.3 . . ? O11 C34 C33 102.3(5) . . ? O11 C34 H34A 111.3 . . ? C33 C34 H34A 111.3 . . ? O11 C34 H34B 111.3 . . ? C33 C34 H34B 111.3 . . ? H34A C34 H34B 109.2 . . ? N16 C35 C36 110.6(5) . . ? N16 C35 H35A 109.5 . . ? C36 C35 H35A 109.5 . . ? N16 C35 H35B 109.5 . . ? C36 C35 H35B 109.5 . . ? H35A C35 H35B 108.1 . . ? O12 C36 C35 112.6(5) . . ? O12 C36 H36A 109.1 . . ? C35 C36 H36A 109.1 . . ? O12 C36 H36B 109.1 . . ? C35 C36 H36B 109.1 . . ? H36A C36 H36B 107.8 . . ? O13 C37 C38 118.2(5) . . ? O13 C37 H37A 107.8 . . ? C38 C37 H37A 107.8 . . ? O13 C37 H37B 107.8 . . ? C38 C37 H37B 107.8 . . ? H37A C37 H37B 107.1 . . ? C37 C38 N17 113.9(5) . . ? C37 C38 H38A 108.8 . . ? N17 C38 H38A 108.8 . . ? C37 C38 H38B 108.8 . . ? N17 C38 H38B 108.8 . . ? H38A C38 H38B 107.7 . . ? C40 C39 O14 114.1(5) . . ? C40 C39 H39A 108.7 . . ? O14 C39 H39A 108.7 . . ? C40 C39 H39B 108.7 . . ? O14 C39 H39B 108.7 . . ? H39A C39 H39B 107.6 . . ? C39 C40 N17 107.7(5) . . ? C39 C40 H40A 110.2 . . ? N17 C40 H40A 110.2 . . ? C39 C40 H40B 110.2 . . ? N17 C40 H40B 110.2 . . ? H40A C40 H40B 108.5 . . ? C42 C41 N17 110.0(5) . . ? C42 C41 H41A 109.7 . . ? N17 C41 H41A 109.7 . . ? C42 C41 H41B 109.7 . . ? N17 C41 H41B 109.7 . . ? H41A C41 H41B 108.2 . . ? O15 C42 C41 118.7(5) . . ? O15 C42 H42A 107.6 . . ? C41 C42 H42A 107.6 . . ? O15 C42 H42B 107.6 . . ? C41 C42 H42B 107.6 . . ? H42A C42 H42B 107.1 . . ? C1 N1 Cu1 167.1(5) . 2_565 ? C2 N2 Cu2 179.1(5) . . ? C3 N3 Cu3 176.5(5) . . ? C9 N9 Cu4 163.9(4) . . ? C10 N10 Cu5 165.4(4) . . ? C15 N13 C17 113.4(5) . . ? C15 N13 C13 109.9(5) . . ? C17 N13 C13 109.1(5) . . ? C15 N13 Cu1 109.1(4) . . ? C17 N13 Cu1 108.7(4) . . ? C13 N13 Cu1 106.4(4) . . ? C19 N14 C21 108.9(4) . . ? C19 N14 C23 108.7(4) . . ? C21 N14 C23 110.9(4) . . ? C19 N14 Cu2 109.5(3) . . ? C21 N14 Cu2 109.1(4) . . ? C23 N14 Cu2 109.7(3) . . ? C27 N15 C25 117.1(5) . . ? C27 N15 C29 108.7(5) . . ? C25 N15 C29 112.6(5) . . ? C27 N15 Cu3 105.3(4) . . ? C25 N15 Cu3 107.9(4) . . ? C29 N15 Cu3 104.1(4) . . ? C33 N16 C35 110.1(5) . . ? C33 N16 C31 112.8(5) . . ? C35 N16 C31 113.4(5) . . ? C33 N16 Cu4 108.2(4) . . ? C35 N16 Cu4 106.8(4) . . ? C31 N16 Cu4 105.0(4) . . ? C40 N17 C41 112.8(4) . . ? C40 N17 C38 97.1(4) . . ? C41 N17 C38 106.8(4) . . ? C40 N17 Cu5 116.9(4) . . ? C41 N17 Cu5 108.0(3) . . ? C38 N17 Cu5 114.5(3) . . ? C18 O1 Cu1 108.0(3) . . ? C18 O1 Cu2 123.3(4) . . ? Cu1 O1 Cu2 96.37(17) . . ? C14 O2 Cu1 107.9(3) . . ? C14 O2 H2C 112.7 . . ? Cu1 O2 H2C 110.5 . . ? C16 O3 Cu1 104.9(3) . . ? C16 O3 H3D 111.2 . . ? Cu1 O3 H3D 110.0 . . ? C20 O4 Cu1 121.3(3) . . ? C20 O4 Cu2 108.4(3) . . ? Cu1 O4 Cu2 96.93(16) . . ? C22 O5 Cu2 104.3(3) . . ? C22 O5 H5D 111.2 . . ? Cu2 O5 H5D 111.0 . . ? C24 O6 Cu2 108.9(3) . . ? C26 O7 Cu4 124.9(4) . . ? C26 O7 Cu3 107.1(3) . . ? Cu4 O7 Cu3 97.62(18) . . ? C30 O8 Cu3 106.3(4) . . ? C30 O8 H8D 111.5 . . ? Cu3 O8 H8D 110.5 . . ? C28 O9 Cu3 111.6(4) . . ? C28 O9 H9B 109.3 . . ? Cu3 O9 H9B 109.3 . . ? C32 O10 Cu3 125.1(4) . . ? C32 O10 Cu4 106.2(3) . . ? Cu3 O10 Cu4 96.98(17) . . ? C34 O11 H11C 111.4 . . ? C36 O12 Cu4 106.6(3) . . ? C36 O12 H12D 111.1 . . ? Cu4 O12 H12D 110.3 . . ? C37 O13 H13E 107.8 . . ? C39 O14 Cu5 106.3(3) . . ? C39 O14 H14B 107.9 . . ? Cu5 O14 H14B 108.8 . . ? C42 O15 Cu5 134.0(3) . 5_655 ? C42 O15 Cu5 105.0(3) . . ? Cu5 O15 Cu5 96.39(17) 5_655 . ? H111 O1W H112 109.5 . . ? H212 O2W H211 109.5 . . ? H312 O3W H311 109.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.02 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 4.955 _refine_diff_density_min -3.785 _refine_diff_density_rms 0.117