# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 #TrackingRef 'jhCC3.cif' #======================================================= #AUTHOR INFORMATION #======================================================= _publ_contact_author_name 'Professor Daniel L. Reger' _publ_contact_author_address ; Department of Chemistry and Biochemistry University of South Carolina Columbia, South Carolina 29208 USA ; _publ_contact_author_phone '1 803 777 2587' _publ_contact_author_fax '1 803 777 9521' _publ_contact_author_email reger@mail.chem.sc.edu loop_ _publ_author_name _publ_author_address D.L.Reger ; Department of Chemistry and Biochemistry University of South Carolina Columbia, South Carolina, 29208 USA ; 'Horger Jacob' ; Department of Chemistry and Biochemistry University of South Carolina Columbia, South Carolina, 29208 USA ; M.D.Smith ; Department of Chemistry and Biochemistry University of South Carolina Columbia, South Carolina, 29208 USA ; #======================================================= #CRYSTAL DATA #======================================================= data_2 _database_code_depnum_ccdc_archive 'CCDC 799344' #TrackingRef 'jhCC3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C134 H97 Cu4 N17 O41, C4 H10 O, 2(C H4 O), 3(C H2 Cl2)' _chemical_formula_sum 'C143 H121 Cl6 Cu4 N17 O44' _chemical_formula_weight 3248.43 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 15.3235(5) _cell_length_b 21.9549(8) _cell_length_c 50.9472(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 17140.0(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8473 _cell_measurement_theta_min 2.277 _cell_measurement_theta_max 23.950 _exptl_crystal_description bar _exptl_crystal_colour blue-green _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.259 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6672 _exptl_absorpt_coefficient_mu 0.660 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8534 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS Version 2.05 (Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 218466 _diffrn_reflns_av_R_equivalents 0.0657 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -60 _diffrn_reflns_limit_l_max 60 _diffrn_reflns_theta_min 1.01 _diffrn_reflns_theta_max 25.07 _reflns_number_total 30385 _reflns_number_gt 26850 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART Version 5.625 (Bruker, 2001)' _computing_cell_refinement 'SAINT-Plus Version 6.45 (Bruker, 2001)' _computing_data_reduction 'SAINT-Plus Version 6.45 (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics various _computing_publication_material 'SHELXTL Version 6.14 (Bruker, 2000)' _refine_special_details ; # 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 0.043 0.569 0.117 829 200 ' ' 2 -0.052 0.069 0.383 829 200 ' ' 3 -0.001 0.431 0.617 829 200 ' ' 4 -0.060 0.842 0.680 166 51 ' ' 5 0.060 0.342 0.820 166 52 ' ' 6 0.002 0.931 0.883 829 200 ' ' 7 0.440 0.658 0.320 166 51 ' ' 8 0.560 0.158 0.180 166 51 ' ' 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^)+(0.0613P)^2^+2.0459P] 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 0.044(6) _refine_ls_number_reflns 30385 _refine_ls_number_parameters 1932 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0510 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1038 _refine_ls_wR_factor_gt 0.1007 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.95180(2) 0.430566(19) 0.304273(7) 0.02413(9) Uani 1 1 d . . . Cu2 Cu 0.92221(2) 0.410011(18) 0.356134(7) 0.02310(9) Uani 1 1 d . . . Cu3 Cu 0.54704(2) 0.541179(18) 0.462315(7) 0.02245(9) Uani 1 1 d . . . Cu4 Cu 0.56691(2) 0.516345(17) 0.411332(7) 0.02102(9) Uani 1 1 d . . . C1A C 0.6749(2) 0.42593(18) 0.27532(7) 0.0310(8) Uani 1 1 d . . . C2A C 0.6621(2) 0.43125(19) 0.24628(7) 0.0365(9) Uani 1 1 d . . . C3A C 0.6406(2) 0.48664(19) 0.23501(7) 0.0360(9) Uani 1 1 d . . . C4A C 0.6308(2) 0.53862(19) 0.25032(7) 0.0363(9) Uani 1 1 d . . . C5A C 0.6483(2) 0.53669(18) 0.27916(7) 0.0309(8) Uani 1 1 d . . . C6A C 0.6727(3) 0.3798(2) 0.23118(8) 0.0499(11) Uani 1 1 d . . . H6A H 0.6880 0.3421 0.2391 0.060 Uiso 1 1 calc R . . C7A C 0.6605(3) 0.3835(3) 0.20371(9) 0.0600(13) Uani 1 1 d . . . H7A H 0.6665 0.3481 0.1932 0.072 Uiso 1 1 calc R . . C8A C 0.6403(3) 0.4375(3) 0.19243(9) 0.0663(15) Uani 1 1 d . . . H8A H 0.6340 0.4393 0.1739 0.080 Uiso 1 1 calc R . . C9A C 0.6283(3) 0.4911(2) 0.20723(8) 0.0476(11) Uani 1 1 d . . . C10A C 0.6036(3) 0.5474(3) 0.19658(9) 0.0604(14) Uani 1 1 d . . . H10A H 0.5947 0.5508 0.1782 0.072 Uiso 1 1 calc R . . C11A C 0.5921(3) 0.5970(3) 0.21189(9) 0.0544(12) Uani 1 1 d . . . H11A H 0.5752 0.6346 0.2042 0.065 Uiso 1 1 calc R . . C12A C 0.6051(3) 0.5929(2) 0.23911(8) 0.0475(11) Uani 1 1 d . . . H12A H 0.5962 0.6277 0.2499 0.057 Uiso 1 1 calc R . . C13A C 0.6891(2) 0.47650(17) 0.31792(6) 0.0276(8) Uani 1 1 d . . . H13A H 0.6815 0.5185 0.3252 0.033 Uiso 1 1 calc R . . C14A C 0.6281(2) 0.43446(18) 0.33371(7) 0.0320(8) Uani 1 1 d . . . H14A H 0.5677 0.4397 0.3272 0.038 Uiso 1 1 calc R . . H14B H 0.6452 0.3916 0.3305 0.038 Uiso 1 1 calc R . . C15A C 0.6290(2) 0.44620(16) 0.36313(7) 0.0274(8) Uani 1 1 d . . . C16A C 0.7850(2) 0.45989(15) 0.32151(6) 0.0217(7) Uani 1 1 d . . . N1A N 0.66648(18) 0.47957(14) 0.28991(5) 0.0279(6) Uani 1 1 d . . . N2A N 0.65597(19) 0.40124(14) 0.37772(6) 0.0335(7) Uani 1 1 d . . . H2A1 H 0.6553 0.4047 0.3949 0.040 Uiso 1 1 calc R . . H2A2 H 0.6748 0.3674 0.3704 0.040 Uiso 1 1 calc R . . O1A O 0.69383(16) 0.37856(12) 0.28579(5) 0.0351(6) Uani 1 1 d . . . O2A O 0.6473(2) 0.58165(13) 0.29252(6) 0.0497(7) Uani 1 1 d . . . O3A O 0.60132(15) 0.49544(11) 0.37159(4) 0.0291(5) Uani 1 1 d . . . O4A O 0.83459(14) 0.46395(11) 0.30181(4) 0.0266(5) Uani 1 1 d . . . O5A O 0.80598(14) 0.44417(11) 0.34419(4) 0.0283(5) Uani 1 1 d . . . C1B C 0.9827(2) 0.21602(17) 0.30711(7) 0.0320(8) Uani 1 1 d . . . C2B C 1.0401(2) 0.18392(18) 0.28843(7) 0.0355(9) Uani 1 1 d . . . C3B C 1.0016(2) 0.15058(17) 0.26777(8) 0.0357(9) Uani 1 1 d . . . C4B C 0.9116(2) 0.14939(18) 0.26412(8) 0.0375(9) Uani 1 1 d . . . C5B C 0.8534(2) 0.18343(17) 0.28169(7) 0.0350(9) Uani 1 1 d . . . C6B C 1.1281(3) 0.1867(2) 0.29133(9) 0.0475(11) Uani 1 1 d . . . H6B H 1.1530 0.2095 0.3053 0.057 Uiso 1 1 calc R . . C7B C 1.1830(3) 0.1551(2) 0.27326(10) 0.0583(13) Uani 1 1 d . . . H7B H 1.2446 0.1574 0.2751 0.070 Uiso 1 1 calc R . . C8B C 1.1483(3) 0.1223(2) 0.25362(9) 0.0520(11) Uani 1 1 d . . . H8B H 1.1860 0.1011 0.2420 0.062 Uiso 1 1 calc R . . C9B C 1.0562(3) 0.11837(18) 0.24982(8) 0.0418(9) Uani 1 1 d . . . C10B C 1.0180(3) 0.08594(19) 0.22916(8) 0.0465(11) Uani 1 1 d . . . H10B H 1.0540 0.0644 0.2171 0.056 Uiso 1 1 calc R . . C11B C 0.9296(3) 0.08495(18) 0.22611(8) 0.0458(10) Uani 1 1 d . . . H11B H 0.9046 0.0626 0.2120 0.055 Uiso 1 1 calc R . . C12B C 0.8753(3) 0.11655(19) 0.24352(8) 0.0423(10) Uani 1 1 d . . . H12B H 0.8138 0.1155 0.2413 0.051 Uiso 1 1 calc R . . C13B C 0.8378(2) 0.25250(16) 0.31943(7) 0.0283(8) Uani 1 1 d . . . H13B H 0.7812 0.2592 0.3101 0.034 Uiso 1 1 calc R . . C14B C 0.8174(2) 0.21764(17) 0.34478(7) 0.0334(8) Uani 1 1 d . . . H14C H 0.7982 0.1758 0.3403 0.040 Uiso 1 1 calc R . . H14D H 0.8710 0.2145 0.3555 0.040 Uiso 1 1 calc R . . C15B C 0.7466(2) 0.24920(17) 0.36056(7) 0.0294(8) Uani 1 1 d . . . C16B C 0.8779(2) 0.31466(16) 0.32425(7) 0.0264(8) Uani 1 1 d . . . N1B N 0.89416(17) 0.21661(13) 0.30176(6) 0.0276(6) Uani 1 1 d . . . N2B N 0.7532(2) 0.24587(17) 0.38619(6) 0.0467(9) Uani 1 1 d . . . H2B1 H 0.7136 0.2632 0.3962 0.056 Uiso 1 1 calc R . . H2B2 H 0.7972 0.2263 0.3934 0.056 Uiso 1 1 calc R . . O1B O 1.01071(16) 0.24219(13) 0.32657(5) 0.0392(6) Uani 1 1 d . . . O2B O 0.77459(17) 0.18405(15) 0.27945(6) 0.0529(8) Uani 1 1 d . . . O3B O 0.68620(16) 0.27612(13) 0.34960(5) 0.0390(6) Uani 1 1 d . . . O4B O 0.90171(14) 0.34485(11) 0.30478(4) 0.0265(5) Uani 1 1 d . . . O5B O 0.87930(15) 0.33130(11) 0.34790(5) 0.0295(5) Uani 1 1 d . . . C1C C 1.2463(2) 0.45109(18) 0.30930(7) 0.0320(8) Uani 1 1 d . . . C2C C 1.2998(2) 0.47199(18) 0.28653(7) 0.0353(9) Uani 1 1 d . . . C3C C 1.3428(2) 0.42835(19) 0.27064(7) 0.0358(9) Uani 1 1 d . . . C4C C 1.3357(2) 0.36628(18) 0.27587(7) 0.0316(8) Uani 1 1 d . . . C5C C 1.2817(2) 0.34407(18) 0.29794(7) 0.0293(8) Uani 1 1 d . . . C6C C 1.3080(3) 0.5329(2) 0.28128(9) 0.0482(11) Uani 1 1 d . . . H6C H 1.2793 0.5619 0.2921 0.058 Uiso 1 1 calc R . . C7C C 1.3584(3) 0.5527(2) 0.26008(10) 0.0596(13) Uani 1 1 d . . . H7C H 1.3635 0.5950 0.2565 0.072 Uiso 1 1 calc R . . C8C C 1.3999(3) 0.5116(3) 0.24464(10) 0.0615(13) Uani 1 1 d . . . H8C H 1.4339 0.5260 0.2303 0.074 Uiso 1 1 calc R . . C9C C 1.3945(3) 0.4484(2) 0.24902(8) 0.0474(11) Uani 1 1 d . . . C10C C 1.4355(3) 0.4049(2) 0.23340(8) 0.0526(11) Uani 1 1 d . . . H10C H 1.4686 0.4176 0.2186 0.063 Uiso 1 1 calc R . . C11C C 1.4291(3) 0.3449(2) 0.23892(8) 0.0525(12) Uani 1 1 d . . . H11C H 1.4584 0.3161 0.2282 0.063 Uiso 1 1 calc R . . C12C C 1.3788(2) 0.3243(2) 0.26068(8) 0.0417(10) Uani 1 1 d . . . H12C H 1.3752 0.2820 0.2646 0.050 Uiso 1 1 calc R . . C13C C 1.1891(2) 0.36884(17) 0.33595(7) 0.0280(8) Uani 1 1 d . . . H13C H 1.1926 0.3234 0.3363 0.034 Uiso 1 1 calc R . . C14C C 1.2224(2) 0.39177(19) 0.36286(7) 0.0354(9) Uani 1 1 d . . . H14E H 1.2070 0.4353 0.3649 0.042 Uiso 1 1 calc R . . H14F H 1.1926 0.3688 0.3770 0.042 Uiso 1 1 calc R . . C15C C 1.3189(2) 0.38451(18) 0.36583(7) 0.0340(9) Uani 1 1 d . . . C16C C 1.0927(2) 0.38550(15) 0.33214(7) 0.0262(8) Uani 1 1 d . . . N1C N 1.24230(17) 0.38939(13) 0.31390(6) 0.0273(6) Uani 1 1 d . . . N2C N 1.3603(2) 0.43111(15) 0.37691(6) 0.0396(8) Uani 1 1 d . . . H2C1 H 1.4171 0.4294 0.3794 0.048 Uiso 1 1 calc R . . H2C2 H 1.3310 0.4637 0.3817 0.048 Uiso 1 1 calc R . . O1C O 1.20527(16) 0.48639(12) 0.32291(5) 0.0360(6) Uani 1 1 d . . . O2C O 1.27017(16) 0.29081(12) 0.30231(5) 0.0376(6) Uani 1 1 d . . . O3C O 1.35587(17) 0.33788(13) 0.35869(6) 0.0474(7) Uani 1 1 d . . . O4C O 1.06765(14) 0.39809(10) 0.30931(4) 0.0280(5) Uani 1 1 d . . . O5C O 1.04689(15) 0.38410(11) 0.35255(4) 0.0291(5) Uani 1 1 d . . . C1D C 0.8913(3) 0.63825(19) 0.33156(9) 0.0446(10) Uani 1 1 d . . . C2D C 0.8590(3) 0.6858(2) 0.31390(10) 0.0560(13) Uani 1 1 d . . . C3D C 0.9175(3) 0.72198(19) 0.29947(11) 0.0604(13) Uani 1 1 d . . . C4D C 1.0083(3) 0.71808(19) 0.30404(10) 0.0563(12) Uani 1 1 d . . . C5D C 1.0418(3) 0.67518(18) 0.32440(9) 0.0479(10) Uani 1 1 d . . . C6D C 0.7696(4) 0.6913(2) 0.31018(13) 0.0753(17) Uani 1 1 d . . . H6D H 0.7297 0.6669 0.3198 0.090 Uiso 1 1 calc R . . C7D C 0.7398(5) 0.7346(3) 0.29144(16) 0.100(2) Uani 1 1 d . . . H7D H 0.6789 0.7402 0.2890 0.120 Uiso 1 1 calc R . . C8D C 0.7968(5) 0.7682(3) 0.27702(16) 0.104(3) Uani 1 1 d . . . H8D H 0.7746 0.7960 0.2644 0.124 Uiso 1 1 calc R . . C9D C 0.8865(4) 0.7629(2) 0.28017(13) 0.0800(18) Uani 1 1 d . . . C10D C 0.9484(6) 0.7948(3) 0.26432(14) 0.100(2) Uani 1 1 d . . . H10D H 0.9283 0.8200 0.2504 0.119 Uiso 1 1 calc R . . C11D C 1.0338(5) 0.7897(2) 0.26863(13) 0.088(2) Uani 1 1 d . . . H11D H 1.0738 0.8116 0.2580 0.106 Uiso 1 1 calc R . . C12D C 1.0652(4) 0.7517(2) 0.28916(10) 0.0706(15) Uani 1 1 d . . . H12D H 1.1261 0.7495 0.2926 0.085 Uiso 1 1 calc R . . C13D C 1.0143(2) 0.58955(17) 0.35387(7) 0.0363(9) Uani 1 1 d . . . H13D H 1.0795 0.5905 0.3531 0.044 Uiso 1 1 calc R . . C14D C 0.9881(3) 0.60203(18) 0.38244(8) 0.0397(9) Uani 1 1 d . . . H14G H 0.9236 0.6029 0.3837 0.048 Uiso 1 1 calc R . . H14H H 1.0092 0.5681 0.3936 0.048 Uiso 1 1 calc R . . C15D C 1.0239(3) 0.6613(2) 0.39303(9) 0.0418(10) Uani 1 1 d . . . C16D C 0.9856(2) 0.52570(15) 0.34473(7) 0.0249(7) Uani 1 1 d . . . N1D N 0.9824(2) 0.63581(14) 0.33551(6) 0.0380(8) Uani 1 1 d . . . N2D N 1.0875(2) 0.65645(19) 0.41041(7) 0.0554(10) Uani 1 1 d . . . H2D1 H 1.1111 0.6894 0.4172 0.067 Uiso 1 1 calc R . . H2D2 H 1.1063 0.6202 0.4152 0.067 Uiso 1 1 calc R . . O1D O 0.84510(18) 0.60194(14) 0.34238(6) 0.0503(8) Uani 1 1 d . . . O2D O 1.1182(2) 0.67301(14) 0.33025(7) 0.0589(9) Uani 1 1 d . . . O3D O 0.9949(2) 0.71016(14) 0.38559(7) 0.0583(8) Uani 1 1 d . . . O4D O 0.99010(15) 0.51213(11) 0.32131(5) 0.0292(5) Uani 1 1 d . . . O5D O 0.96236(15) 0.49126(10) 0.36344(4) 0.0275(5) Uani 1 1 d . . . C1E C 0.7189(2) 0.37737(17) 0.48802(7) 0.0291(8) Uani 1 1 d . . . C2E C 0.7201(3) 0.34537(18) 0.51348(7) 0.0368(9) Uani 1 1 d . . . C3E C 0.7878(3) 0.35737(17) 0.53182(7) 0.0336(9) Uani 1 1 d . . . C4E C 0.8535(3) 0.40027(18) 0.52599(7) 0.0371(9) Uani 1 1 d . . . C5E C 0.8540(2) 0.43268(18) 0.50058(7) 0.0319(8) Uani 1 1 d . . . C6E C 0.6565(3) 0.3038(2) 0.51953(8) 0.0455(10) Uani 1 1 d . . . H6E H 0.6112 0.2960 0.5072 0.055 Uiso 1 1 calc R . . C7E C 0.6571(3) 0.2728(2) 0.54336(10) 0.0595(13) Uani 1 1 d . . . H7E H 0.6124 0.2442 0.5473 0.071 Uiso 1 1 calc R . . C8E C 0.7225(4) 0.2837(2) 0.56097(9) 0.0646(14) Uani 1 1 d . . . H8E H 0.7229 0.2619 0.5771 0.078 Uiso 1 1 calc R . . C9E C 0.7891(3) 0.3261(2) 0.55608(8) 0.0484(11) Uani 1 1 d . . . C10E C 0.8571(4) 0.3390(2) 0.57370(9) 0.0593(14) Uani 1 1 d . . . H10E H 0.8589 0.3186 0.5901 0.071 Uiso 1 1 calc R . . C11E C 0.9205(3) 0.3803(2) 0.56774(8) 0.0556(12) Uani 1 1 d . . . H11E H 0.9660 0.3878 0.5800 0.067 Uiso 1 1 calc R . . C12E C 0.9196(3) 0.4116(2) 0.54403(8) 0.0500(11) Uani 1 1 d . . . H12E H 0.9639 0.4405 0.5402 0.060 Uiso 1 1 calc R . . C13E C 0.7856(2) 0.44950(16) 0.45753(6) 0.0249(7) Uani 1 1 d . . . H13E H 0.8291 0.4834 0.4582 0.030 Uiso 1 1 calc R . . C14E C 0.8164(2) 0.40433(16) 0.43624(6) 0.0249(7) Uani 1 1 d . . . H14I H 0.8621 0.3782 0.4441 0.030 Uiso 1 1 calc R . . H14J H 0.7665 0.3775 0.4319 0.030 Uiso 1 1 calc R . . C15E C 0.8518(2) 0.42966(16) 0.41089(7) 0.0261(7) Uani 1 1 d . . . C16E C 0.6963(2) 0.47784(15) 0.45202(6) 0.0234(7) Uani 1 1 d . . . N1E N 0.78577(17) 0.41938(13) 0.48349(5) 0.0267(6) Uani 1 1 d . . . N2E N 0.8430(2) 0.48693(15) 0.40526(6) 0.0414(8) Uani 1 1 d . . . H2E1 H 0.8644 0.5014 0.3905 0.050 Uiso 1 1 calc R . . H2E2 H 0.8156 0.5113 0.4162 0.050 Uiso 1 1 calc R . . O1E O 0.66454(15) 0.36820(12) 0.47117(5) 0.0318(6) Uani 1 1 d . . . O2E O 0.90954(17) 0.47002(13) 0.49460(5) 0.0409(6) Uani 1 1 d . . . O3E O 0.88990(16) 0.39308(11) 0.39614(4) 0.0298(5) Uani 1 1 d . . . O4E O 0.65715(14) 0.50139(10) 0.47090(4) 0.0255(5) Uani 1 1 d . . . O5E O 0.67227(13) 0.47754(10) 0.42834(4) 0.0238(5) Uani 1 1 d . . . C1F C 0.3221(2) 0.38035(16) 0.45953(7) 0.0284(8) Uani 1 1 d . . . C2F C 0.2506(2) 0.37061(18) 0.47898(7) 0.0352(9) Uani 1 1 d . . . C3F C 0.2633(3) 0.33015(17) 0.50010(7) 0.0350(9) Uani 1 1 d . . . C4F C 0.3419(2) 0.29935(16) 0.50371(7) 0.0316(8) Uani 1 1 d . . . C5F C 0.4136(2) 0.30628(16) 0.48440(7) 0.0302(8) Uani 1 1 d . . . C6F C 0.1732(3) 0.4000(2) 0.47564(9) 0.0526(12) Uani 1 1 d . . . H6F H 0.1664 0.4280 0.4616 0.063 Uiso 1 1 calc R . . C7F C 0.1039(3) 0.3893(3) 0.49271(10) 0.0631(14) Uani 1 1 d . . . H7F H 0.0500 0.4099 0.4902 0.076 Uiso 1 1 calc R . . C8F C 0.1131(3) 0.3491(3) 0.51303(10) 0.0636(14) Uani 1 1 d . . . H8F H 0.0644 0.3408 0.5240 0.076 Uiso 1 1 calc R . . C9F C 0.1927(3) 0.31988(19) 0.51800(8) 0.0460(11) Uani 1 1 d . . . C10F C 0.2063(4) 0.2805(2) 0.53923(9) 0.0556(13) Uani 1 1 d . . . H10F H 0.1598 0.2725 0.5511 0.067 Uiso 1 1 calc R . . C11F C 0.2854(4) 0.25349(19) 0.54314(8) 0.0517(12) Uani 1 1 d . . . H11F H 0.2944 0.2286 0.5581 0.062 Uiso 1 1 calc R . . C12F C 0.3528(3) 0.26225(18) 0.52527(7) 0.0450(10) Uani 1 1 d . . . H12F H 0.4072 0.2424 0.5280 0.054 Uiso 1 1 calc R . . C13F C 0.4705(2) 0.35657(15) 0.44531(6) 0.0248(7) Uani 1 1 d . . . H13F H 0.5243 0.3397 0.4537 0.030 Uiso 1 1 calc R . . C14F C 0.4528(2) 0.31692(15) 0.42126(7) 0.0283(7) Uani 1 1 d . . . H14K H 0.4262 0.2782 0.4272 0.034 Uiso 1 1 calc R . . H14L H 0.4098 0.3379 0.4100 0.034 Uiso 1 1 calc R . . C15F C 0.5329(2) 0.30247(15) 0.40502(6) 0.0250(7) Uani 1 1 d . . . C16F C 0.48990(19) 0.42318(16) 0.43957(6) 0.0243(7) Uani 1 1 d . . . N1F N 0.40083(17) 0.34961(12) 0.46452(5) 0.0244(6) Uani 1 1 d . . . N2F N 0.51918(19) 0.29283(15) 0.37946(6) 0.0357(7) Uani 1 1 d . . . H2F1 H 0.5627 0.2816 0.3693 0.043 Uiso 1 1 calc R . . H2F2 H 0.4666 0.2977 0.3728 0.043 Uiso 1 1 calc R . . O1F O 0.31550(15) 0.41134(12) 0.44045(5) 0.0351(6) Uani 1 1 d . . . O2F O 0.47940(17) 0.27589(13) 0.48522(5) 0.0425(7) Uani 1 1 d . . . O3F O 0.60526(15) 0.29639(12) 0.41546(5) 0.0331(6) Uani 1 1 d . . . O4F O 0.49051(14) 0.45867(10) 0.45894(4) 0.0251(5) Uani 1 1 d . . . O5F O 0.50995(13) 0.43694(10) 0.41620(4) 0.0232(5) Uani 1 1 d . . . C1G C 0.4282(2) 0.72529(16) 0.42806(7) 0.0293(8) Uani 1 1 d . . . C2G C 0.4327(2) 0.78791(16) 0.43885(7) 0.0306(8) Uani 1 1 d . . . C3G C 0.3607(2) 0.81138(16) 0.45373(7) 0.0314(8) Uani 1 1 d . . . C4G C 0.2861(2) 0.77560(17) 0.45769(7) 0.0314(8) Uani 1 1 d . . . C5G C 0.2807(2) 0.71312(17) 0.44725(7) 0.0304(8) Uani 1 1 d . . . C6G C 0.5051(3) 0.82292(17) 0.43500(8) 0.0369(9) Uani 1 1 d . . . H6G H 0.5526 0.8074 0.4251 0.044 Uiso 1 1 calc R . . C7G C 0.5099(3) 0.88193(19) 0.44565(8) 0.0435(10) Uani 1 1 d . . . H7G H 0.5604 0.9061 0.4428 0.052 Uiso 1 1 calc R . . C8G C 0.4419(3) 0.90472(18) 0.46010(8) 0.0469(10) Uani 1 1 d . . . H8G H 0.4462 0.9445 0.4673 0.056 Uiso 1 1 calc R . . C9G C 0.3661(3) 0.87029(18) 0.46438(7) 0.0372(9) Uani 1 1 d . . . C10G C 0.2933(3) 0.89246(19) 0.47925(8) 0.0438(10) Uani 1 1 d . . . H10G H 0.2953 0.9321 0.4867 0.053 Uiso 1 1 calc R . . C11G C 0.2216(3) 0.8573(2) 0.48269(8) 0.0469(11) Uani 1 1 d . . . H11G H 0.1736 0.8728 0.4924 0.056 Uiso 1 1 calc R . . C12G C 0.2171(3) 0.79823(19) 0.47208(7) 0.0400(9) Uani 1 1 d . . . H12G H 0.1665 0.7740 0.4748 0.048 Uiso 1 1 calc R . . C13G C 0.3441(2) 0.63117(15) 0.42038(7) 0.0270(8) Uani 1 1 d . . . H13G H 0.2921 0.6110 0.4284 0.032 Uiso 1 1 calc R . . C14G C 0.3235(2) 0.63969(16) 0.39149(7) 0.0305(8) Uani 1 1 d . . . H14M H 0.3776 0.6512 0.3821 0.037 Uiso 1 1 calc R . . H14N H 0.2813 0.6735 0.3895 0.037 Uiso 1 1 calc R . . C15G C 0.2859(2) 0.58260(19) 0.37907(8) 0.0373(9) Uani 1 1 d . . . C16G C 0.4234(2) 0.58946(15) 0.42598(6) 0.0245(7) Uani 1 1 d . . . N1G N 0.35320(17) 0.69120(13) 0.43331(5) 0.0254(6) Uani 1 1 d . . . N2G N 0.2854(3) 0.58239(19) 0.35354(8) 0.0688(12) Uani 1 1 d . . . H2G1 H 0.2632 0.5512 0.3450 0.083 Uiso 1 1 calc R . . H2G2 H 0.3071 0.6135 0.3448 0.083 Uiso 1 1 calc R . . O1G O 0.48664(15) 0.70314(11) 0.41488(5) 0.0323(6) Uani 1 1 d . . . O2G O 0.21694(16) 0.68063(13) 0.45028(5) 0.0413(7) Uani 1 1 d . . . O3G O 0.25653(18) 0.54069(13) 0.39172(6) 0.0479(7) Uani 1 1 d . . . O4G O 0.44502(14) 0.58566(10) 0.44973(4) 0.0262(5) Uani 1 1 d . . . O5G O 0.45422(14) 0.56064(10) 0.40720(4) 0.0263(5) Uani 1 1 d . . . C1H C 0.8236(2) 0.64067(17) 0.44603(7) 0.0313(8) Uani 1 1 d . . . C2H C 0.9042(2) 0.64626(17) 0.46169(7) 0.0315(8) Uani 1 1 d . . . C3H C 0.9201(2) 0.70072(17) 0.47606(7) 0.0334(8) Uani 1 1 d . . . C4H C 0.8577(3) 0.74733(18) 0.47623(7) 0.0368(9) Uani 1 1 d . . . C5H C 0.7757(2) 0.74240(17) 0.46146(8) 0.0361(9) Uani 1 1 d . . . C6H C 0.9648(2) 0.60036(18) 0.46177(8) 0.0387(9) Uani 1 1 d . . . H6H H 0.9539 0.5642 0.4521 0.046 Uiso 1 1 calc R . . C7H C 1.0421(3) 0.6063(2) 0.47591(8) 0.0479(11) Uani 1 1 d . . . H7H H 1.0835 0.5741 0.4757 0.057 Uiso 1 1 calc R . . C8H C 1.0592(3) 0.6577(2) 0.49001(8) 0.0458(10) Uani 1 1 d . . . H8H H 1.1121 0.6608 0.4996 0.055 Uiso 1 1 calc R . . C9H C 0.9986(2) 0.7066(2) 0.49048(8) 0.0430(10) Uani 1 1 d . . . C10H C 1.0126(3) 0.7605(2) 0.50482(8) 0.0516(12) Uani 1 1 d . . . H10H H 1.0648 0.7652 0.5147 0.062 Uiso 1 1 calc R . . C11H C 0.9516(3) 0.8063(2) 0.50473(8) 0.0511(12) Uani 1 1 d . . . H11H H 0.9622 0.8425 0.5144 0.061 Uiso 1 1 calc R . . C12H C 0.8744(3) 0.80015(19) 0.49057(8) 0.0468(11) Uani 1 1 d . . . H12H H 0.8328 0.8322 0.4907 0.056 Uiso 1 1 calc R . . C13H C 0.6916(2) 0.68530(17) 0.42763(8) 0.0344(9) Uani 1 1 d . . . H13H H 0.6507 0.7190 0.4324 0.041 Uiso 1 1 calc R . . C14H C 0.7191(3) 0.69601(18) 0.39890(8) 0.0393(9) Uani 1 1 d . . . H14O H 0.7675 0.6681 0.3942 0.047 Uiso 1 1 calc R . . H14P H 0.6694 0.6874 0.3871 0.047 Uiso 1 1 calc R . . C15H C 0.7483(3) 0.76137(19) 0.39548(9) 0.0426(10) Uani 1 1 d . . . C16H C 0.6416(2) 0.62573(16) 0.43154(7) 0.0286(8) Uani 1 1 d . . . N1H N 0.76612(18) 0.68946(13) 0.44575(6) 0.0299(7) Uani 1 1 d . . . N2H N 0.8305(2) 0.77179(17) 0.39152(8) 0.0555(10) Uani 1 1 d . . . H2H1 H 0.8491 0.8094 0.3893 0.067 Uiso 1 1 calc R . . H2H2 H 0.8677 0.7413 0.3910 0.067 Uiso 1 1 calc R . . O1H O 0.80692(16) 0.59541(12) 0.43324(5) 0.0369(6) Uani 1 1 d . . . O2H O 0.71797(19) 0.78042(13) 0.46161(6) 0.0516(8) Uani 1 1 d . . . O3H O 0.6921(2) 0.80224(15) 0.39644(7) 0.0628(9) Uani 1 1 d . . . O4H O 0.61741(15) 0.61430(11) 0.45457(5) 0.0288(5) Uani 1 1 d . . . O5H O 0.62569(14) 0.59482(11) 0.41131(5) 0.0298(5) Uani 1 1 d . . . C21 C 0.9030(3) 0.4441(2) 0.24698(8) 0.0494(11) Uani 1 1 d . . . H21 H 0.8466 0.4385 0.2543 0.059 Uiso 1 1 calc R . . C22 C 0.9093(4) 0.4554(3) 0.22075(9) 0.0822(18) Uani 1 1 d . . . H22 H 0.8584 0.4568 0.2101 0.099 Uiso 1 1 calc R . . C23 C 0.9901(5) 0.4647(3) 0.21001(10) 0.088(2) Uani 1 1 d . . . H23 H 0.9960 0.4742 0.1919 0.105 Uiso 1 1 calc R . . C24 C 1.0627(4) 0.4601(2) 0.22582(10) 0.0708(15) Uani 1 1 d . . . H24 H 1.1197 0.4654 0.2188 0.085 Uiso 1 1 calc R . . C25 C 1.0501(3) 0.4475(2) 0.25225(8) 0.0494(11) Uani 1 1 d . . . H25 H 1.0999 0.4436 0.2632 0.059 Uiso 1 1 calc R . . N3 N 0.97149(19) 0.44049(14) 0.26285(6) 0.0334(7) Uani 1 1 d . . . C26 C 0.5423(4) 0.4978(3) 0.52014(9) 0.0818(18) Uani 1 1 d . . . H26A H 0.5247 0.4585 0.5127 0.123 Uiso 1 1 calc R . . H26B H 0.5165 0.5026 0.5376 0.123 Uiso 1 1 calc R . . H26C H 0.6061 0.4993 0.5215 0.123 Uiso 1 1 calc R . . O6 O 0.51288(17) 0.54578(13) 0.50346(5) 0.0396(6) Uani 1 1 d . . . H6M H 0.4603 0.5490 0.5073 0.059 Uiso 1 1 d R . . C27 C 0.2808(4) 0.5417(3) 0.48900(15) 0.097(2) Uani 1 1 d . . . H27A H 0.2263 0.5230 0.4951 0.146 Uiso 1 1 calc R . . H27B H 0.3074 0.5159 0.4755 0.146 Uiso 1 1 calc R . . H27C H 0.2683 0.5820 0.4816 0.146 Uiso 1 1 calc R . . O7 O 0.3402(2) 0.5479(2) 0.51086(9) 0.0945(14) Uani 1 1 d . . . H7M H 0.3545 0.5125 0.5161 0.142 Uiso 1 1 d R . . C28 C 0.0851(3) 0.4635(3) 0.41887(10) 0.0715(15) Uani 1 1 d . . . H28A H 0.1247 0.4291 0.4216 0.107 Uiso 1 1 calc R . . H28B H 0.0716 0.4672 0.4001 0.107 Uiso 1 1 calc R . . H28C H 0.0310 0.4567 0.4287 0.107 Uiso 1 1 calc R . . O8 O 0.1250(2) 0.51723(18) 0.42766(7) 0.0673(10) Uani 1 1 d . . . H8M H 0.1648 0.5347 0.4192 0.101 Uiso 1 1 d R . . C1S C 0.5909(3) 0.2491(2) 0.29492(8) 0.0462(10) Uani 1 1 d . . . H1S1 H 0.6258 0.2194 0.3051 0.055 Uiso 1 1 calc R . . H1S2 H 0.6275 0.2856 0.2919 0.055 Uiso 1 1 calc R . . Cl1 Cl 0.56251(9) 0.21702(7) 0.26451(2) 0.0711(4) Uani 1 1 d . . . Cl2 Cl 0.49866(8) 0.26975(8) 0.31309(2) 0.0735(4) Uani 1 1 d . . . C2S C 0.6328(5) 0.6988(3) 0.63179(12) 0.092(2) Uani 1 1 d . . . H2S1 H 0.5698 0.6940 0.6281 0.110 Uiso 1 1 calc R . . H2S2 H 0.6417 0.7395 0.6397 0.110 Uiso 1 1 calc R . . Cl3 Cl 0.66600(13) 0.64213(10) 0.65432(4) 0.1076(6) Uani 1 1 d . . . Cl4 Cl 0.69184(11) 0.69412(7) 0.60221(3) 0.0841(4) Uani 1 1 d . . . C3S C 1.0164(5) 0.6806(5) 0.63519(13) 0.128(3) Uani 1 1 d . . . H3S1 H 1.0397 0.7204 0.6293 0.154 Uiso 1 1 calc R . . H3S2 H 1.0349 0.6495 0.6223 0.154 Uiso 1 1 calc R . . Cl5 Cl 0.90366(11) 0.68420(9) 0.63546(3) 0.0956(5) Uani 1 1 d . . . Cl6 Cl 1.06099(16) 0.66294(12) 0.66557(3) 0.1308(8) Uani 1 1 d . . . C29 C 0.4714(7) 0.6332(5) 0.56904(14) 0.162(5) Uani 1 1 d D . . H29D H 0.4116 0.6460 0.5651 0.243 Uiso 1 1 calc R . . H29E H 0.4970 0.6136 0.5536 0.243 Uiso 1 1 calc R . . H29F H 0.5064 0.6689 0.5738 0.243 Uiso 1 1 calc R . . C30 C 0.4704(6) 0.5881(3) 0.59202(16) 0.131(3) Uani 1 1 d D . . H30C H 0.4332 0.5526 0.5877 0.158 Uiso 1 1 calc R . . H30D H 0.5303 0.5733 0.5956 0.158 Uiso 1 1 calc R . . C31 C 0.4300(6) 0.5842(4) 0.63762(17) 0.137(3) Uani 1 1 d D . . H31C H 0.4882 0.5689 0.6429 0.164 Uiso 1 1 calc R . . H31D H 0.3910 0.5489 0.6348 0.164 Uiso 1 1 calc R . . C32 C 0.3915(7) 0.6273(5) 0.65972(17) 0.158(4) Uani 1 1 d D . . H32D H 0.4343 0.6589 0.6641 0.237 Uiso 1 1 calc R . . H32E H 0.3784 0.6032 0.6754 0.237 Uiso 1 1 calc R . . H32F H 0.3378 0.6466 0.6533 0.237 Uiso 1 1 calc R . . O10 O 0.4368(3) 0.61893(17) 0.61426(8) 0.0892(12) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01950(18) 0.0333(2) 0.01960(19) -0.00006(17) 0.00129(16) 0.00182(17) Cu2 0.02074(19) 0.0288(2) 0.0197(2) -0.00313(17) 0.00179(16) 0.00013(16) Cu3 0.02001(19) 0.0270(2) 0.02030(19) -0.00259(16) 0.00132(16) 0.00079(16) Cu4 0.01848(19) 0.0245(2) 0.02006(19) -0.00060(16) 0.00163(15) -0.00091(16) C1A 0.0238(17) 0.043(2) 0.0267(19) -0.0021(18) -0.0033(14) -0.0016(16) C2A 0.0308(19) 0.058(3) 0.0206(18) -0.0123(18) 0.0039(15) -0.0054(18) C3A 0.0281(18) 0.055(3) 0.0248(18) 0.0073(18) -0.0053(15) -0.0087(18) C4A 0.0235(18) 0.051(2) 0.034(2) 0.0124(19) 0.0029(15) -0.0053(17) C5A 0.0216(17) 0.042(2) 0.0288(19) 0.0031(18) 0.0003(14) -0.0005(16) C6A 0.049(3) 0.065(3) 0.035(2) -0.007(2) -0.0012(19) 0.002(2) C7A 0.072(3) 0.079(4) 0.030(2) -0.015(2) 0.003(2) -0.018(3) C8A 0.064(3) 0.108(5) 0.027(2) -0.004(3) 0.000(2) -0.015(3) C9A 0.041(2) 0.076(3) 0.027(2) 0.001(2) -0.0024(17) -0.017(2) C10A 0.053(3) 0.094(4) 0.034(2) 0.024(3) -0.009(2) -0.015(3) C11A 0.046(3) 0.075(3) 0.043(3) 0.025(3) -0.009(2) -0.007(2) C12A 0.038(2) 0.063(3) 0.042(2) 0.015(2) 0.0009(18) -0.008(2) C13A 0.0239(17) 0.035(2) 0.0234(17) -0.0029(15) -0.0016(14) 0.0032(15) C14A 0.0254(17) 0.046(2) 0.0248(18) -0.0058(16) 0.0006(14) -0.0007(16) C15A 0.0208(16) 0.035(2) 0.0265(19) -0.0013(16) 0.0044(14) -0.0051(15) C16A 0.0277(16) 0.0211(16) 0.0163(16) -0.0051(13) 0.0002(13) 0.0035(14) N1A 0.0277(15) 0.0374(17) 0.0186(14) -0.0041(13) -0.0012(11) 0.0052(13) N2A 0.0371(17) 0.0389(18) 0.0245(15) -0.0019(14) 0.0067(13) 0.0058(15) O1A 0.0362(14) 0.0385(16) 0.0305(14) -0.0080(12) -0.0001(11) 0.0012(12) O2A 0.069(2) 0.0347(16) 0.0451(17) 0.0004(14) -0.0026(15) 0.0011(15) O3A 0.0359(13) 0.0305(14) 0.0210(12) -0.0002(10) 0.0045(10) 0.0031(11) O4A 0.0239(11) 0.0350(13) 0.0210(12) -0.0017(10) 0.0010(10) 0.0035(10) O5A 0.0206(11) 0.0403(15) 0.0239(13) -0.0014(11) -0.0001(9) 0.0041(10) C1B 0.0314(18) 0.033(2) 0.032(2) -0.0111(17) 0.0024(16) -0.0003(15) C2B 0.0306(19) 0.039(2) 0.036(2) -0.0102(17) 0.0059(16) 0.0055(17) C3B 0.035(2) 0.032(2) 0.040(2) -0.0068(17) 0.0083(17) 0.0009(17) C4B 0.038(2) 0.035(2) 0.040(2) -0.0133(17) 0.0103(17) -0.0004(17) C5B 0.034(2) 0.035(2) 0.036(2) -0.0135(17) 0.0026(17) -0.0008(17) C6B 0.036(2) 0.055(3) 0.051(3) -0.020(2) 0.0036(19) 0.008(2) C7B 0.031(2) 0.076(3) 0.068(3) -0.019(3) 0.011(2) 0.012(2) C8B 0.041(2) 0.057(3) 0.058(3) -0.020(2) 0.014(2) 0.011(2) C9B 0.047(2) 0.040(2) 0.038(2) -0.0091(18) 0.0143(19) 0.0008(19) C10B 0.059(3) 0.041(2) 0.039(2) -0.0137(19) 0.018(2) -0.001(2) C11B 0.055(3) 0.041(2) 0.042(2) -0.0181(19) 0.007(2) -0.006(2) C12B 0.044(2) 0.049(2) 0.034(2) -0.0110(19) 0.0037(18) -0.0013(19) C13B 0.0253(17) 0.0323(19) 0.0273(18) -0.0096(15) 0.0035(14) 0.0020(15) C14B 0.0310(18) 0.031(2) 0.038(2) -0.0077(17) 0.0058(16) 0.0036(16) C15B 0.0232(17) 0.034(2) 0.031(2) -0.0047(16) 0.0030(15) -0.0044(15) C16B 0.0185(16) 0.034(2) 0.0263(19) -0.0023(16) 0.0017(14) 0.0070(14) N1B 0.0228(14) 0.0294(16) 0.0305(16) -0.0109(13) 0.0043(12) 0.0013(12) N2B 0.0364(18) 0.071(3) 0.0330(19) -0.0044(17) 0.0031(15) 0.0248(18) O1B 0.0303(13) 0.0494(17) 0.0378(15) -0.0131(13) -0.0054(12) 0.0084(12) O2B 0.0259(14) 0.077(2) 0.0556(19) -0.0390(17) -0.0016(13) -0.0024(14) O3B 0.0292(13) 0.0566(17) 0.0312(14) -0.0037(13) 0.0038(11) 0.0096(13) O4B 0.0258(12) 0.0305(13) 0.0233(12) -0.0041(11) 0.0016(10) 0.0010(10) O5B 0.0279(12) 0.0340(14) 0.0265(13) -0.0055(11) 0.0022(10) -0.0023(11) C1C 0.0216(17) 0.041(2) 0.033(2) -0.0061(18) -0.0099(15) -0.0056(16) C2C 0.0288(18) 0.040(2) 0.037(2) 0.0019(18) -0.0080(16) -0.0077(16) C3C 0.0225(17) 0.053(2) 0.032(2) -0.0004(18) -0.0009(15) -0.0023(17) C4C 0.0211(17) 0.050(2) 0.0241(18) -0.0040(17) 0.0004(14) -0.0025(16) C5C 0.0195(16) 0.044(2) 0.0243(18) -0.0105(16) -0.0036(14) 0.0045(16) C6C 0.040(2) 0.051(3) 0.053(3) 0.002(2) -0.002(2) -0.009(2) C7C 0.056(3) 0.054(3) 0.069(3) 0.013(3) -0.002(3) -0.014(2) C8C 0.056(3) 0.080(4) 0.049(3) 0.013(3) 0.010(2) -0.018(3) C9C 0.032(2) 0.069(3) 0.042(2) 0.003(2) 0.0013(18) -0.009(2) C10C 0.042(2) 0.076(3) 0.040(2) 0.000(2) 0.009(2) -0.008(2) C11C 0.042(2) 0.085(4) 0.031(2) -0.014(2) 0.0083(19) 0.005(2) C12C 0.0285(19) 0.057(3) 0.040(2) -0.009(2) 0.0033(17) 0.0018(18) C13C 0.0269(18) 0.032(2) 0.0248(18) -0.0022(15) 0.0017(14) 0.0020(15) C14C 0.0293(19) 0.046(2) 0.031(2) -0.0028(17) 0.0002(16) 0.0040(17) C15C 0.0312(19) 0.038(2) 0.033(2) -0.0003(17) -0.0065(16) 0.0074(18) C16C 0.0240(17) 0.0241(18) 0.030(2) -0.0065(15) 0.0006(15) 0.0007(14) N1C 0.0188(14) 0.0367(17) 0.0265(16) -0.0023(13) -0.0002(11) 0.0008(12) N2C 0.0341(17) 0.0441(19) 0.0407(18) -0.0054(16) -0.0064(14) 0.0044(16) O1C 0.0354(14) 0.0338(14) 0.0388(15) -0.0113(12) -0.0017(12) 0.0029(12) O2C 0.0330(14) 0.0380(16) 0.0417(15) -0.0048(13) 0.0085(12) 0.0012(12) O3C 0.0339(14) 0.0540(18) 0.0543(18) -0.0218(15) -0.0166(13) 0.0178(14) O4C 0.0189(11) 0.0377(14) 0.0273(13) -0.0025(10) -0.0023(10) 0.0057(10) O5C 0.0216(11) 0.0390(13) 0.0268(13) -0.0012(10) 0.0031(10) 0.0040(11) C1D 0.038(2) 0.033(2) 0.062(3) -0.009(2) -0.010(2) 0.0021(19) C2D 0.061(3) 0.035(2) 0.071(3) -0.001(2) -0.026(3) 0.011(2) C3D 0.072(3) 0.028(2) 0.081(3) 0.006(2) -0.024(3) -0.001(2) C4D 0.078(3) 0.023(2) 0.068(3) 0.004(2) -0.012(3) -0.011(2) C5D 0.050(3) 0.033(2) 0.061(3) 0.002(2) -0.003(2) -0.007(2) C6D 0.066(3) 0.049(3) 0.111(5) 0.002(3) -0.032(3) 0.017(3) C7D 0.090(5) 0.067(4) 0.144(7) 0.003(4) -0.054(5) 0.023(4) C8D 0.108(5) 0.058(4) 0.145(7) 0.025(4) -0.062(5) 0.018(4) C9D 0.097(4) 0.031(3) 0.112(5) 0.013(3) -0.036(4) 0.000(3) C10D 0.137(6) 0.048(3) 0.114(5) 0.033(3) -0.045(5) -0.008(4) C11D 0.133(6) 0.036(3) 0.096(5) 0.020(3) -0.026(4) -0.021(3) C12D 0.097(4) 0.042(3) 0.073(3) 0.012(2) -0.011(3) -0.021(3) C13D 0.0315(18) 0.036(2) 0.041(2) 0.0050(18) -0.0015(16) -0.0007(16) C14D 0.042(2) 0.038(2) 0.039(2) -0.0054(18) -0.0029(18) -0.0080(18) C15D 0.032(2) 0.040(2) 0.053(3) -0.013(2) 0.0045(19) -0.0029(18) C16D 0.0198(15) 0.0273(19) 0.0275(19) -0.0018(15) -0.0038(14) 0.0001(13) N1D 0.0401(18) 0.0302(17) 0.0437(19) 0.0068(15) -0.0099(15) -0.0021(14) N2D 0.043(2) 0.065(2) 0.058(2) -0.019(2) -0.0100(19) -0.0073(19) O1D 0.0341(15) 0.0440(18) 0.073(2) -0.0017(16) -0.0045(15) -0.0014(14) O2D 0.0469(19) 0.053(2) 0.076(2) 0.0196(17) -0.0051(16) -0.0168(15) O3D 0.0512(18) 0.0368(18) 0.087(2) -0.0120(17) -0.0002(17) -0.0027(15) O4D 0.0291(12) 0.0297(13) 0.0288(14) -0.0002(11) -0.0017(10) -0.0040(11) O5D 0.0317(12) 0.0271(12) 0.0236(12) -0.0010(10) 0.0027(10) -0.0021(11) C1E 0.0281(18) 0.035(2) 0.0239(18) -0.0027(15) 0.0064(15) 0.0114(16) C2E 0.041(2) 0.044(2) 0.0248(19) 0.0009(17) 0.0016(16) 0.0167(19) C3E 0.047(2) 0.035(2) 0.0192(18) -0.0047(15) -0.0021(16) 0.0139(18) C4E 0.044(2) 0.040(2) 0.0272(19) -0.0089(17) -0.0095(17) 0.0197(19) C5E 0.0273(18) 0.041(2) 0.0277(19) -0.0123(17) -0.0042(15) 0.0099(18) C6E 0.046(2) 0.049(3) 0.041(2) 0.007(2) 0.0046(19) 0.006(2) C7E 0.073(3) 0.054(3) 0.051(3) 0.019(2) 0.008(3) 0.000(3) C8E 0.090(4) 0.069(3) 0.035(2) 0.018(2) 0.004(3) 0.023(3) C9E 0.068(3) 0.050(3) 0.028(2) 0.0000(19) 0.002(2) 0.020(2) C10E 0.088(4) 0.058(3) 0.032(2) 0.001(2) -0.021(2) 0.035(3) C11E 0.071(3) 0.059(3) 0.036(2) -0.005(2) -0.027(2) 0.008(3) C12E 0.054(3) 0.057(3) 0.039(2) -0.009(2) -0.021(2) 0.017(2) C13E 0.0201(15) 0.038(2) 0.0170(16) -0.0015(14) 0.0013(13) 0.0009(14) C14E 0.0260(16) 0.0322(19) 0.0166(16) -0.0029(14) 0.0003(13) 0.0069(15) C15E 0.0240(16) 0.0310(19) 0.0232(17) -0.0046(16) -0.0014(14) 0.0014(15) C16E 0.0211(16) 0.0243(17) 0.0247(18) -0.0019(14) -0.0006(14) -0.0032(14) N1E 0.0252(14) 0.0377(17) 0.0171(14) -0.0018(12) -0.0015(11) 0.0056(13) N2E 0.056(2) 0.0348(19) 0.0332(18) -0.0025(15) 0.0209(15) 0.0039(16) O1E 0.0273(13) 0.0420(15) 0.0259(13) 0.0027(11) -0.0016(11) 0.0019(11) O2E 0.0341(14) 0.0496(17) 0.0390(15) -0.0024(13) -0.0146(12) -0.0002(13) O3E 0.0371(13) 0.0307(13) 0.0216(12) -0.0053(10) 0.0073(10) 0.0019(11) O4E 0.0211(11) 0.0328(13) 0.0226(12) -0.0024(10) 0.0005(9) 0.0067(10) O5E 0.0203(11) 0.0316(13) 0.0195(12) 0.0022(10) -0.0024(9) 0.0020(10) C1F 0.0238(17) 0.0328(19) 0.029(2) 0.0028(17) 0.0046(15) -0.0009(15) C2F 0.0279(19) 0.047(2) 0.031(2) 0.0037(18) 0.0050(15) -0.0026(17) C3F 0.044(2) 0.031(2) 0.030(2) 0.0014(16) 0.0095(17) -0.0118(17) C4F 0.045(2) 0.0255(19) 0.0237(18) 0.0003(15) 0.0047(16) -0.0043(17) C5F 0.038(2) 0.0269(19) 0.0254(18) 0.0003(15) -0.0027(15) -0.0022(16) C6F 0.032(2) 0.076(3) 0.049(3) 0.008(2) 0.0073(19) 0.008(2) C7F 0.031(2) 0.096(4) 0.063(3) 0.000(3) 0.016(2) 0.004(2) C8F 0.043(3) 0.087(4) 0.060(3) -0.002(3) 0.027(2) -0.016(3) C9F 0.058(3) 0.043(2) 0.037(2) 0.0010(19) 0.023(2) -0.015(2) C10F 0.084(3) 0.045(3) 0.037(2) 0.001(2) 0.034(2) -0.016(3) C11F 0.092(4) 0.035(2) 0.028(2) 0.0087(18) 0.016(2) -0.012(2) C12F 0.077(3) 0.030(2) 0.029(2) 0.0067(17) 0.003(2) -0.006(2) C13F 0.0201(16) 0.0307(19) 0.0234(17) 0.0038(14) 0.0052(13) 0.0022(14) C14F 0.0258(17) 0.0242(17) 0.0350(19) -0.0027(15) 0.0003(15) -0.0019(15) C15F 0.0275(18) 0.0208(17) 0.0266(18) -0.0009(14) 0.0002(14) 0.0006(14) C16F 0.0153(14) 0.037(2) 0.0201(17) 0.0021(15) 0.0006(13) -0.0005(14) N1F 0.0241(14) 0.0235(14) 0.0257(15) 0.0048(12) 0.0002(12) 0.0002(11) N2F 0.0237(15) 0.056(2) 0.0270(16) -0.0085(15) -0.0001(12) 0.0077(14) O1F 0.0256(12) 0.0494(16) 0.0303(14) 0.0137(13) 0.0023(10) 0.0055(12) O2F 0.0417(15) 0.0443(16) 0.0415(16) 0.0131(13) -0.0005(12) 0.0112(13) O3F 0.0265(13) 0.0412(15) 0.0315(14) -0.0002(11) 0.0010(11) 0.0136(11) O4F 0.0247(11) 0.0297(12) 0.0209(12) -0.0016(10) 0.0046(9) -0.0045(10) O5F 0.0213(11) 0.0271(12) 0.0211(12) -0.0001(10) 0.0014(9) -0.0030(9) C1G 0.0275(18) 0.0342(19) 0.0260(18) 0.0030(15) -0.0040(15) 0.0010(16) C2G 0.0300(19) 0.032(2) 0.0295(18) -0.0021(15) -0.0041(15) 0.0015(16) C3G 0.0366(19) 0.031(2) 0.0267(19) -0.0016(15) -0.0066(15) 0.0067(16) C4G 0.0287(18) 0.0324(19) 0.033(2) -0.0071(16) -0.0024(15) 0.0070(15) C5G 0.0246(18) 0.040(2) 0.0261(19) -0.0005(16) -0.0001(14) 0.0067(16) C6G 0.038(2) 0.036(2) 0.037(2) -0.0018(17) -0.0029(17) -0.0006(17) C7G 0.046(2) 0.037(2) 0.048(2) -0.0056(19) 0.000(2) -0.0102(19) C8G 0.056(3) 0.029(2) 0.056(3) -0.0112(19) -0.011(2) -0.001(2) C9G 0.044(2) 0.037(2) 0.030(2) -0.0065(17) -0.0029(17) 0.0054(17) C10G 0.054(3) 0.039(2) 0.038(2) -0.0118(18) -0.0056(19) 0.015(2) C11G 0.045(2) 0.052(3) 0.044(2) -0.008(2) 0.005(2) 0.017(2) C12G 0.037(2) 0.048(2) 0.035(2) -0.0055(19) 0.0003(17) 0.0064(18) C13G 0.0219(17) 0.0274(19) 0.0318(19) -0.0031(15) 0.0005(14) -0.0016(14) C14G 0.0273(18) 0.032(2) 0.032(2) -0.0046(16) -0.0060(15) 0.0063(15) C15G 0.033(2) 0.039(2) 0.040(2) -0.0112(19) -0.0105(17) 0.0092(18) C16G 0.0221(16) 0.0247(17) 0.0269(18) 0.0000(14) 0.0031(14) -0.0054(14) N1G 0.0232(14) 0.0266(15) 0.0265(15) -0.0032(12) 0.0018(12) 0.0021(12) N2G 0.111(4) 0.050(2) 0.045(2) -0.012(2) -0.017(2) -0.014(2) O1G 0.0268(12) 0.0325(14) 0.0378(14) -0.0043(11) 0.0086(11) 0.0006(11) O2G 0.0264(13) 0.0478(17) 0.0497(16) -0.0153(13) 0.0074(12) -0.0056(12) O3G 0.0455(16) 0.0388(16) 0.0595(19) -0.0088(15) -0.0022(14) -0.0087(14) O4G 0.0274(12) 0.0281(12) 0.0232(12) -0.0047(10) -0.0008(10) 0.0052(10) O5G 0.0208(11) 0.0318(13) 0.0262(12) -0.0018(10) 0.0018(10) 0.0042(10) C1H 0.0246(17) 0.032(2) 0.037(2) -0.0067(17) 0.0057(15) -0.0014(15) C2H 0.0216(17) 0.041(2) 0.0322(19) -0.0042(17) 0.0063(15) -0.0093(15) C3H 0.0305(18) 0.042(2) 0.0279(18) -0.0056(16) 0.0096(15) -0.0095(17) C4H 0.040(2) 0.036(2) 0.035(2) -0.0047(17) 0.0060(17) -0.0123(18) C5H 0.037(2) 0.033(2) 0.039(2) -0.0101(18) 0.0144(17) -0.0096(17) C6H 0.0320(19) 0.043(2) 0.041(2) -0.0052(18) 0.0013(17) 0.0001(17) C7H 0.0275(19) 0.069(3) 0.047(2) 0.001(2) -0.0039(18) -0.002(2) C8H 0.028(2) 0.073(3) 0.036(2) -0.003(2) -0.0044(17) -0.010(2) C9H 0.031(2) 0.062(3) 0.036(2) -0.012(2) 0.0053(17) -0.021(2) C10H 0.049(2) 0.070(3) 0.036(2) -0.014(2) 0.0088(19) -0.032(2) C11H 0.063(3) 0.054(3) 0.036(2) -0.016(2) 0.010(2) -0.032(3) C12H 0.058(3) 0.040(2) 0.042(2) -0.0102(19) 0.015(2) -0.013(2) C13H 0.0230(17) 0.030(2) 0.051(2) -0.0049(18) 0.0007(16) -0.0043(15) C14H 0.035(2) 0.036(2) 0.047(2) 0.0080(18) -0.0062(18) -0.0090(17) C15H 0.035(2) 0.039(2) 0.054(3) 0.007(2) 0.0005(19) -0.0029(19) C16H 0.0232(17) 0.0268(19) 0.036(2) 0.0007(16) 0.0012(15) 0.0033(14) N1H 0.0246(14) 0.0258(16) 0.0391(18) -0.0055(13) 0.0051(13) -0.0062(12) N2H 0.042(2) 0.041(2) 0.083(3) 0.005(2) 0.0116(19) -0.0117(17) O1H 0.0323(13) 0.0309(14) 0.0475(16) -0.0162(13) -0.0076(12) 0.0024(11) O2H 0.0448(16) 0.0352(15) 0.075(2) -0.0196(15) 0.0040(16) 0.0062(14) O3H 0.0482(18) 0.0445(18) 0.096(3) 0.0153(18) 0.0124(17) 0.0006(16) O4H 0.0262(12) 0.0292(13) 0.0311(14) -0.0024(11) -0.0005(10) -0.0024(10) O5H 0.0263(12) 0.0310(13) 0.0321(13) 0.0023(12) -0.0006(10) -0.0059(10) C21 0.045(2) 0.069(3) 0.034(2) 0.001(2) -0.0016(19) 0.016(2) C22 0.100(4) 0.118(5) 0.028(2) 0.006(3) -0.004(3) 0.023(4) C23 0.124(6) 0.106(5) 0.033(3) 0.012(3) 0.022(3) 0.016(4) C24 0.080(4) 0.079(4) 0.054(3) 0.002(3) 0.041(3) -0.006(3) C25 0.050(2) 0.055(3) 0.043(2) 0.002(2) 0.014(2) 0.000(2) N3 0.0361(17) 0.0373(18) 0.0269(16) -0.0008(13) 0.0090(13) 0.0012(14) C26 0.084(4) 0.128(5) 0.034(3) 0.013(3) 0.012(3) 0.028(4) O6 0.0388(14) 0.0554(17) 0.0245(13) -0.0024(12) 0.0081(11) 0.0070(13) C27 0.072(4) 0.093(5) 0.127(6) 0.003(4) 0.007(4) -0.020(4) O7 0.047(2) 0.115(3) 0.122(4) 0.025(3) 0.017(2) 0.010(2) C28 0.055(3) 0.108(5) 0.052(3) 0.002(3) -0.019(2) 0.015(3) O8 0.0489(18) 0.095(3) 0.058(2) -0.021(2) -0.0004(15) 0.0080(19) C1S 0.039(2) 0.059(3) 0.040(2) -0.014(2) -0.0005(18) -0.005(2) Cl1 0.0621(8) 0.0920(9) 0.0592(7) -0.0301(7) -0.0097(6) 0.0185(7) Cl2 0.0433(6) 0.1381(13) 0.0391(6) -0.0143(7) -0.0027(5) 0.0157(7) C2S 0.110(5) 0.097(5) 0.069(4) 0.007(3) 0.007(4) 0.041(4) Cl3 0.1097(13) 0.1303(15) 0.0829(11) 0.0389(11) 0.0043(10) 0.0463(12) Cl4 0.0967(11) 0.0761(9) 0.0794(10) 0.0111(8) 0.0234(8) 0.0196(8) C3S 0.096(5) 0.229(10) 0.059(4) 0.030(5) -0.002(4) -0.024(6) Cl5 0.0915(11) 0.1198(14) 0.0755(10) 0.0127(9) 0.0140(9) -0.0069(10) Cl6 0.1300(17) 0.195(2) 0.0671(10) 0.0130(12) -0.0154(11) 0.0139(17) C29 0.242(12) 0.184(9) 0.059(4) -0.032(5) -0.017(6) 0.092(9) C30 0.150(7) 0.099(6) 0.145(8) -0.062(6) -0.036(6) 0.052(5) C31 0.134(7) 0.108(6) 0.168(8) 0.087(6) -0.029(6) 0.016(6) C32 0.187(10) 0.192(10) 0.095(6) 0.059(7) 0.013(6) 0.075(8) O10 0.097(3) 0.065(2) 0.106(3) -0.002(2) -0.025(3) 0.027(2) _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 O4C 1.930(2) . ? Cu1 O4A 1.944(2) . ? Cu1 O4B 2.033(2) . ? Cu1 O4D 2.075(2) . ? Cu1 N3 2.143(3) . ? Cu1 Cu2 2.7185(5) . ? Cu2 O5B 1.896(2) . ? Cu2 O5D 1.923(2) . ? Cu2 O5C 2.002(2) . ? Cu2 O5A 2.026(2) . ? Cu2 O3E 2.130(2) . ? Cu3 O4E 1.950(2) . ? Cu3 O4G 1.952(2) . ? Cu3 O4H 1.974(2) . ? Cu3 O4F 2.015(2) . ? Cu3 O6 2.163(2) . ? Cu3 Cu4 2.6714(5) . ? Cu4 O5H 1.944(2) . ? Cu4 O5F 1.965(2) . ? Cu4 O5G 1.993(2) . ? Cu4 O5E 2.021(2) . ? Cu4 O3A 2.142(2) . ? C1A O1A 1.204(4) . ? C1A N1A 1.399(5) . ? C1A C2A 1.497(5) . ? C2A C6A 1.377(6) . ? C2A C3A 1.385(6) . ? C3A C4A 1.390(6) . ? C3A C9A 1.431(5) . ? C4A C12A 1.379(6) . ? C4A C5A 1.494(5) . ? C5A O2A 1.199(5) . ? C5A N1A 1.396(5) . ? C6A C7A 1.414(6) . ? C6A H6A 0.9500 . ? C7A C8A 1.352(7) . ? C7A H7A 0.9500 . ? C8A C9A 1.409(7) . ? C8A H8A 0.9500 . ? C9A C10A 1.404(7) . ? C10A C11A 1.350(7) . ? C10A H10A 0.9500 . ? C11A C12A 1.404(6) . ? C11A H11A 0.9500 . ? C12A H12A 0.9500 . ? C13A N1A 1.470(4) . ? C13A C16A 1.525(5) . ? C13A C14A 1.541(5) . ? C13A H13A 1.0000 . ? C14A C15A 1.521(5) . ? C14A H14A 0.9900 . ? C14A H14B 0.9900 . ? C15A O3A 1.239(4) . ? C15A N2A 1.303(4) . ? C16A O5A 1.248(4) . ? C16A O4A 1.262(4) . ? N2A H2A1 0.8800 . ? N2A H2A2 0.8800 . ? C1B O1B 1.223(4) . ? C1B N1B 1.384(4) . ? C1B C2B 1.475(5) . ? C2B C6B 1.358(6) . ? C2B C3B 1.411(5) . ? C3B C4B 1.392(5) . ? C3B C9B 1.427(5) . ? C4B C12B 1.389(5) . ? C4B C5B 1.468(5) . ? C5B O2B 1.213(4) . ? C5B N1B 1.403(5) . ? C6B C7B 1.426(6) . ? C6B H6B 0.9500 . ? C7B C8B 1.343(6) . ? C7B H7B 0.9500 . ? C8B C9B 1.427(6) . ? C8B H8B 0.9500 . ? C9B C10B 1.399(6) . ? C10B C11B 1.363(6) . ? C10B H10B 0.9500 . ? C11B C12B 1.400(6) . ? C11B H11B 0.9500 . ? C12B H12B 0.9500 . ? C13B N1B 1.475(4) . ? C13B C16B 1.516(5) . ? C13B C14B 1.533(5) . ? C13B H13B 1.0000 . ? C14B C15B 1.517(5) . ? C14B H14C 0.9900 . ? C14B H14D 0.9900 . ? C15B O3B 1.233(4) . ? C15B N2B 1.312(5) . ? C16B O4B 1.247(4) . ? C16B O5B 1.259(4) . ? N2B H2B1 0.8800 . ? N2B H2B2 0.8800 . ? C1C O1C 1.215(4) . ? C1C N1C 1.376(5) . ? C1C C2C 1.492(5) . ? C2C C6C 1.370(6) . ? C2C C3C 1.417(6) . ? C3C C4C 1.393(6) . ? C3C C9C 1.427(6) . ? C4C C12C 1.374(5) . ? C4C C5C 1.479(5) . ? C5C O2C 1.203(5) . ? C5C N1C 1.419(4) . ? C6C C7C 1.396(6) . ? C6C H6C 0.9500 . ? C7C C8C 1.355(7) . ? C7C H7C 0.9500 . ? C8C C9C 1.408(7) . ? C8C H8C 0.9500 . ? C9C C10C 1.393(6) . ? C10C C11C 1.351(7) . ? C10C H10C 0.9500 . ? C11C C12C 1.424(6) . ? C11C H11C 0.9500 . ? C12C H12C 0.9500 . ? C13C N1C 1.460(4) . ? C13C C16C 1.533(5) . ? C13C C14C 1.547(5) . ? C13C H13C 1.0000 . ? C14C C15C 1.495(5) . ? C14C H14E 0.9900 . ? C14C H14F 0.9900 . ? C15C O3C 1.225(4) . ? C15C N2C 1.330(5) . ? C16C O5C 1.255(4) . ? C16C O4C 1.256(4) . ? N2C H2C1 0.8800 . ? N2C H2C2 0.8800 . ? C1D O1D 1.200(5) . ? C1D N1D 1.412(5) . ? C1D C2D 1.465(6) . ? C2D C6D 1.388(7) . ? C2D C3D 1.405(7) . ? C3D C4D 1.412(7) . ? C3D C9D 1.415(7) . ? C4D C12D 1.371(7) . ? C4D C5D 1.492(6) . ? C5D O2D 1.208(5) . ? C5D N1D 1.377(5) . ? C6D C7D 1.423(8) . ? C6D H6D 0.9500 . ? C7D C8D 1.358(10) . ? C7D H7D 0.9500 . ? C8D C9D 1.389(9) . ? C8D H8D 0.9500 . ? C9D C10D 1.429(10) . ? C10D C11D 1.330(9) . ? C10D H10D 0.9500 . ? C11D C12D 1.423(8) . ? C11D H11D 0.9500 . ? C12D H12D 0.9500 . ? C13D N1D 1.464(5) . ? C13D C14D 1.535(5) . ? C13D C16D 1.541(5) . ? C13D H13D 1.0000 . ? C14D C15D 1.512(5) . ? C14D H14G 0.9900 . ? C14D H14H 0.9900 . ? C15D O3D 1.221(5) . ? C15D N2D 1.321(5) . ? C16D O4D 1.232(4) . ? C16D O5D 1.268(4) . ? N2D H2D1 0.8800 . ? N2D H2D2 0.8800 . ? C1E O1E 1.213(4) . ? C1E N1E 1.398(5) . ? C1E C2E 1.476(5) . ? C2E C6E 1.372(6) . ? C2E C3E 1.420(5) . ? C3E C4E 1.410(6) . ? C3E C9E 1.415(5) . ? C4E C12E 1.390(5) . ? C4E C5E 1.477(5) . ? C5E O2E 1.220(5) . ? C5E N1E 1.392(4) . ? C6E C7E 1.392(6) . ? C6E H6E 0.9500 . ? C7E C8E 1.367(7) . ? C7E H7E 0.9500 . ? C8E C9E 1.403(7) . ? C8E H8E 0.9500 . ? C9E C10E 1.404(7) . ? C10E C11E 1.363(7) . ? C10E H10E 0.9500 . ? C11E C12E 1.390(6) . ? C11E H11E 0.9500 . ? C12E H12E 0.9500 . ? C13E N1E 1.479(4) . ? C13E C16E 1.529(4) . ? C13E C14E 1.544(4) . ? C13E H13E 1.0000 . ? C14E C15E 1.507(5) . ? C14E H14I 0.9900 . ? C14E H14J 0.9900 . ? C15E O3E 1.245(4) . ? C15E N2E 1.297(5) . ? C16E O4E 1.246(4) . ? C16E O5E 1.261(4) . ? N2E H2E1 0.8800 . ? N2E H2E2 0.8800 . ? C1F O1F 1.191(4) . ? C1F N1F 1.405(4) . ? C1F C2F 1.493(5) . ? C2F C6F 1.361(6) . ? C2F C3F 1.409(5) . ? C3F C4F 1.393(5) . ? C3F C9F 1.432(5) . ? C4F C12F 1.378(5) . ? C4F C5F 1.483(5) . ? C5F O2F 1.209(4) . ? C5F N1F 1.403(4) . ? C6F C7F 1.392(6) . ? C6F H6F 0.9500 . ? C7F C8F 1.368(7) . ? C7F H7F 0.9500 . ? C8F C9F 1.402(7) . ? C8F H8F 0.9500 . ? C9F C10F 1.401(6) . ? C10F C11F 1.364(7) . ? C10F H10F 0.9500 . ? C11F C12F 1.391(6) . ? C11F H11F 0.9500 . ? C12F H12F 0.9500 . ? C13F N1F 1.457(4) . ? C13F C16F 1.521(5) . ? C13F C14F 1.527(5) . ? C13F H13F 1.0000 . ? C14F C15F 1.514(5) . ? C14F H14K 0.9900 . ? C14F H14L 0.9900 . ? C15F O3F 1.237(4) . ? C15F N2F 1.336(4) . ? C16F O4F 1.257(4) . ? C16F O5F 1.266(4) . ? N2F H2F1 0.8800 . ? N2F H2F2 0.8800 . ? C1G O1G 1.220(4) . ? C1G N1G 1.397(4) . ? C1G C2G 1.482(5) . ? C2G C6G 1.364(5) . ? C2G C3G 1.434(5) . ? C3G C4G 1.402(5) . ? C3G C9G 1.405(5) . ? C4G C12G 1.380(5) . ? C4G C5G 1.474(5) . ? C5G O2G 1.219(4) . ? C5G N1G 1.404(4) . ? C6G C7G 1.407(6) . ? C6G H6G 0.9500 . ? C7G C8G 1.370(6) . ? C7G H7G 0.9500 . ? C8G C9G 1.403(6) . ? C8G H8G 0.9500 . ? C9G C10G 1.434(6) . ? C10G C11G 1.354(6) . ? C10G H10G 0.9500 . ? C11G C12G 1.407(6) . ? C11G H11G 0.9500 . ? C12G H12G 0.9500 . ? C13G N1G 1.480(4) . ? C13G C14G 1.517(5) . ? C13G C16G 1.549(5) . ? C13G H13G 1.0000 . ? C14G C15G 1.518(5) . ? C14G H14M 0.9900 . ? C14G H14N 0.9900 . ? C15G O3G 1.210(5) . ? C15G N2G 1.301(5) . ? C16G O5G 1.241(4) . ? C16G O4G 1.257(4) . ? N2G H2G1 0.8800 . ? N2G H2G2 0.8800 . ? C1H O1H 1.215(4) . ? C1H N1H 1.387(5) . ? C1H C2H 1.476(5) . ? C2H C6H 1.370(5) . ? C2H C3H 1.423(5) . ? C3H C4H 1.400(6) . ? C3H C9H 1.415(5) . ? C4H C12H 1.394(6) . ? C4H C5H 1.469(5) . ? C5H O2H 1.216(5) . ? C5H N1H 1.419(5) . ? C6H C7H 1.392(5) . ? C6H H6H 0.9500 . ? C7H C8H 1.364(6) . ? C7H H7H 0.9500 . ? C8H C9H 1.420(6) . ? C8H H8H 0.9500 . ? C9H C10H 1.406(6) . ? C10H C11H 1.373(7) . ? C10H H10H 0.9500 . ? C11H C12H 1.392(6) . ? C11H H11H 0.9500 . ? C12H H12H 0.9500 . ? C13H N1H 1.471(5) . ? C13H C16H 1.529(5) . ? C13H C14H 1.541(6) . ? C13H H13H 1.0000 . ? C14H C15H 1.513(6) . ? C14H H14O 0.9900 . ? C14H H14P 0.9900 . ? C15H O3H 1.244(5) . ? C15H N2H 1.296(5) . ? C16H O4H 1.256(4) . ? C16H O5H 1.258(4) . ? N2H H2H1 0.8800 . ? N2H H2H2 0.8800 . ? C21 N3 1.327(5) . ? C21 C22 1.362(6) . ? C21 H21 0.9500 . ? C22 C23 1.369(9) . ? C22 H22 0.9500 . ? C23 C24 1.377(8) . ? C23 H23 0.9500 . ? C24 C25 1.388(6) . ? C24 H24 0.9500 . ? C25 N3 1.329(5) . ? C25 H25 0.9500 . ? C26 O6 1.427(6) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? O6 H6M 0.8316 . ? C27 O7 1.445(8) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? O7 H7M 0.8493 . ? C28 O8 1.402(7) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? O8 H8M 0.8401 . ? C1S Cl2 1.749(4) . ? C1S Cl1 1.757(4) . ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? C2S Cl4 1.761(6) . ? C2S Cl3 1.767(6) . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? C3S Cl5 1.729(7) . ? C3S Cl6 1.736(7) . ? C3S H3S1 0.9900 . ? C3S H3S2 0.9900 . ? C29 C30 1.534(10) . ? C29 H29D 0.9800 . ? C29 H29E 0.9800 . ? C29 H29F 0.9800 . ? C30 O10 1.417(7) . ? C30 H30C 0.9900 . ? C30 H30D 0.9900 . ? C31 O10 1.417(7) . ? C31 C32 1.585(10) . ? C31 H31C 0.9900 . ? C31 H31D 0.9900 . ? C32 H32D 0.9800 . ? C32 H32E 0.9800 . ? C32 H32F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4C Cu1 O4A 176.06(9) . . ? O4C Cu1 O4B 90.20(9) . . ? O4A Cu1 O4B 90.06(9) . . ? O4C Cu1 O4D 90.18(9) . . ? O4A Cu1 O4D 87.87(9) . . ? O4B Cu1 O4D 154.24(9) . . ? O4C Cu1 N3 92.23(10) . . ? O4A Cu1 N3 91.61(10) . . ? O4B Cu1 N3 99.20(10) . . ? O4D Cu1 N3 106.52(11) . . ? O4C Cu1 Cu2 87.87(7) . . ? O4A Cu1 Cu2 88.36(7) . . ? O4B Cu1 Cu2 76.75(6) . . ? O4D Cu1 Cu2 77.52(7) . . ? N3 Cu1 Cu2 175.96(8) . . ? O5B Cu2 O5D 177.61(10) . . ? O5B Cu2 O5C 92.97(10) . . ? O5D Cu2 O5C 88.62(10) . . ? O5B Cu2 O5A 88.06(10) . . ? O5D Cu2 O5A 89.77(10) . . ? O5C Cu2 O5A 156.47(9) . . ? O5B Cu2 O3E 88.40(10) . . ? O5D Cu2 O3E 92.92(9) . . ? O5C Cu2 O3E 105.04(9) . . ? O5A Cu2 O3E 98.49(9) . . ? O5B Cu2 Cu1 89.66(7) . . ? O5D Cu2 Cu1 88.90(7) . . ? O5C Cu2 Cu1 78.43(7) . . ? O5A Cu2 Cu1 78.07(6) . . ? O3E Cu2 Cu1 176.11(7) . . ? O4E Cu3 O4G 172.36(10) . . ? O4E Cu3 O4H 86.35(10) . . ? O4G Cu3 O4H 87.99(10) . . ? O4E Cu3 O4F 89.33(9) . . ? O4G Cu3 O4F 94.45(9) . . ? O4H Cu3 O4F 161.60(9) . . ? O4E Cu3 O6 90.74(10) . . ? O4G Cu3 O6 95.81(9) . . ? O4H Cu3 O6 106.73(10) . . ? O4F Cu3 O6 91.19(10) . . ? O4E Cu3 Cu4 91.61(6) . . ? O4G Cu3 Cu4 82.76(6) . . ? O4H Cu3 Cu4 84.80(7) . . ? O4F Cu3 Cu4 77.44(6) . . ? O6 Cu3 Cu4 168.36(8) . . ? O5H Cu4 O5F 172.71(10) . . ? O5H Cu4 O5G 88.22(10) . . ? O5F Cu4 O5G 93.52(9) . . ? O5H Cu4 O5E 90.21(9) . . ? O5F Cu4 O5E 85.79(9) . . ? O5G Cu4 O5E 160.61(9) . . ? O5H Cu4 O3A 94.32(10) . . ? O5F Cu4 O3A 92.21(9) . . ? O5G Cu4 O3A 102.59(9) . . ? O5E Cu4 O3A 96.80(9) . . ? O5H Cu4 Cu3 82.68(7) . . ? O5F Cu4 Cu3 90.44(6) . . ? O5G Cu4 Cu3 84.51(6) . . ? O5E Cu4 Cu3 76.12(6) . . ? O3A Cu4 Cu3 172.24(7) . . ? O1A C1A N1A 120.9(3) . . ? O1A C1A C2A 122.5(4) . . ? N1A C1A C2A 116.6(3) . . ? C6A C2A C3A 121.1(4) . . ? C6A C2A C1A 118.2(4) . . ? C3A C2A C1A 120.6(3) . . ? C2A C3A C4A 120.9(3) . . ? C2A C3A C9A 120.1(4) . . ? C4A C3A C9A 119.0(4) . . ? C12A C4A C3A 120.5(4) . . ? C12A C4A C5A 118.9(4) . . ? C3A C4A C5A 120.6(3) . . ? O2A C5A N1A 121.3(3) . . ? O2A C5A C4A 122.2(4) . . ? N1A C5A C4A 116.5(3) . . ? C2A C6A C7A 119.3(5) . . ? C2A C6A H6A 120.3 . . ? C7A C6A H6A 120.3 . . ? C8A C7A C6A 120.1(5) . . ? C8A C7A H7A 119.9 . . ? C6A C7A H7A 119.9 . . ? C7A C8A C9A 122.2(4) . . ? C7A C8A H8A 118.9 . . ? C9A C8A H8A 118.9 . . ? C10A C9A C8A 124.3(4) . . ? C10A C9A C3A 118.5(4) . . ? C8A C9A C3A 117.1(4) . . ? C11A C10A C9A 121.5(4) . . ? C11A C10A H10A 119.3 . . ? C9A C10A H10A 119.3 . . ? C10A C11A C12A 120.0(5) . . ? C10A C11A H11A 120.0 . . ? C12A C11A H11A 120.0 . . ? C4A C12A C11A 120.3(5) . . ? C4A C12A H12A 119.8 . . ? C11A C12A H12A 119.8 . . ? N1A C13A C16A 110.8(3) . . ? N1A C13A C14A 113.0(3) . . ? C16A C13A C14A 112.3(3) . . ? N1A C13A H13A 106.8 . . ? C16A C13A H13A 106.8 . . ? C14A C13A H13A 106.8 . . ? C15A C14A C13A 114.0(3) . . ? C15A C14A H14A 108.7 . . ? C13A C14A H14A 108.7 . . ? C15A C14A H14B 108.7 . . ? C13A C14A H14B 108.7 . . ? H14A C14A H14B 107.6 . . ? O3A C15A N2A 124.8(3) . . ? O3A C15A C14A 119.2(3) . . ? N2A C15A C14A 115.9(3) . . ? O5A C16A O4A 126.9(3) . . ? O5A C16A C13A 115.2(3) . . ? O4A C16A C13A 117.9(3) . . ? C5A N1A C1A 124.5(3) . . ? C5A N1A C13A 118.0(3) . . ? C1A N1A C13A 117.1(3) . . ? C15A N2A H2A1 120.0 . . ? C15A N2A H2A2 120.0 . . ? H2A1 N2A H2A2 120.0 . . ? C15A O3A Cu4 126.9(2) . . ? C16A O4A Cu1 118.6(2) . . ? C16A O5A Cu2 127.4(2) . . ? O1B C1B N1B 119.9(3) . . ? O1B C1B C2B 122.6(3) . . ? N1B C1B C2B 117.5(3) . . ? C6B C2B C3B 121.3(3) . . ? C6B C2B C1B 120.0(4) . . ? C3B C2B C1B 118.7(3) . . ? C4B C3B C2B 121.6(3) . . ? C4B C3B C9B 119.1(4) . . ? C2B C3B C9B 119.3(3) . . ? C12B C4B C3B 120.5(4) . . ? C12B C4B C5B 118.8(4) . . ? C3B C4B C5B 120.7(4) . . ? O2B C5B N1B 120.4(3) . . ? O2B C5B C4B 123.6(3) . . ? N1B C5B C4B 116.0(3) . . ? C2B C6B C7B 119.6(4) . . ? C2B C6B H6B 120.2 . . ? C7B C6B H6B 120.2 . . ? C8B C7B C6B 120.5(4) . . ? C8B C7B H7B 119.8 . . ? C6B C7B H7B 119.8 . . ? C7B C8B C9B 121.7(4) . . ? C7B C8B H8B 119.2 . . ? C9B C8B H8B 119.2 . . ? C10B C9B C8B 123.1(4) . . ? C10B C9B C3B 119.3(4) . . ? C8B C9B C3B 117.6(4) . . ? C11B C10B C9B 120.6(4) . . ? C11B C10B H10B 119.7 . . ? C9B C10B H10B 119.7 . . ? C10B C11B C12B 120.7(4) . . ? C10B C11B H11B 119.7 . . ? C12B C11B H11B 119.7 . . ? C4B C12B C11B 119.8(4) . . ? C4B C12B H12B 120.1 . . ? C11B C12B H12B 120.1 . . ? N1B C13B C16B 110.1(3) . . ? N1B C13B C14B 111.5(3) . . ? C16B C13B C14B 113.3(3) . . ? N1B C13B H13B 107.2 . . ? C16B C13B H13B 107.2 . . ? C14B C13B H13B 107.2 . . ? C15B C14B C13B 111.4(3) . . ? C15B C14B H14C 109.4 . . ? C13B C14B H14C 109.4 . . ? C15B C14B H14D 109.4 . . ? C13B C14B H14D 109.4 . . ? H14C C14B H14D 108.0 . . ? O3B C15B N2B 122.4(3) . . ? O3B C15B C14B 121.1(3) . . ? N2B C15B C14B 116.6(3) . . ? O4B C16B O5B 127.0(3) . . ? O4B C16B C13B 117.9(3) . . ? O5B C16B C13B 115.0(3) . . ? C1B N1B C5B 125.1(3) . . ? C1B N1B C13B 117.3(3) . . ? C5B N1B C13B 117.5(3) . . ? C15B N2B H2B1 120.0 . . ? C15B N2B H2B2 120.0 . . ? H2B1 N2B H2B2 120.0 . . ? C16B O4B Cu1 127.8(2) . . ? C16B O5B Cu2 118.8(2) . . ? O1C C1C N1C 120.5(3) . . ? O1C C1C C2C 122.1(4) . . ? N1C C1C C2C 117.3(3) . . ? C6C C2C C3C 120.4(4) . . ? C6C C2C C1C 120.2(4) . . ? C3C C2C C1C 119.4(3) . . ? C4C C3C C2C 121.1(3) . . ? C4C C3C C9C 119.5(4) . . ? C2C C3C C9C 119.4(4) . . ? C12C C4C C3C 120.8(3) . . ? C12C C4C C5C 118.4(4) . . ? C3C C4C C5C 120.8(3) . . ? O2C C5C N1C 120.8(3) . . ? O2C C5C C4C 122.9(3) . . ? N1C C5C C4C 116.3(3) . . ? C2C C6C C7C 120.4(4) . . ? C2C C6C H6C 119.8 . . ? C7C C6C H6C 119.8 . . ? C8C C7C C6C 120.1(5) . . ? C8C C7C H7C 119.9 . . ? C6C C7C H7C 119.9 . . ? C7C C8C C9C 122.4(4) . . ? C7C C8C H8C 118.8 . . ? C9C C8C H8C 118.8 . . ? C10C C9C C8C 124.0(4) . . ? C10C C9C C3C 118.7(4) . . ? C8C C9C C3C 117.3(4) . . ? C11C C10C C9C 121.1(4) . . ? C11C C10C H10C 119.4 . . ? C9C C10C H10C 119.4 . . ? C10C C11C C12C 120.8(4) . . ? C10C C11C H11C 119.6 . . ? C12C C11C H11C 119.6 . . ? C4C C12C C11C 119.0(4) . . ? C4C C12C H12C 120.5 . . ? C11C C12C H12C 120.5 . . ? N1C C13C C16C 111.5(3) . . ? N1C C13C C14C 113.4(3) . . ? C16C C13C C14C 110.6(3) . . ? N1C C13C H13C 107.0 . . ? C16C C13C H13C 107.0 . . ? C14C C13C H13C 107.0 . . ? C15C C14C C13C 112.4(3) . . ? C15C C14C H14E 109.1 . . ? C13C C14C H14E 109.1 . . ? C15C C14C H14F 109.1 . . ? C13C C14C H14F 109.1 . . ? H14E C14C H14F 107.9 . . ? O3C C15C N2C 123.2(3) . . ? O3C C15C C14C 121.1(4) . . ? N2C C15C C14C 115.7(3) . . ? O5C C16C O4C 127.0(3) . . ? O5C C16C C13C 115.3(3) . . ? O4C C16C C13C 117.7(3) . . ? C1C N1C C5C 125.0(3) . . ? C1C N1C C13C 117.4(3) . . ? C5C N1C C13C 117.5(3) . . ? C15C N2C H2C1 120.0 . . ? C15C N2C H2C2 120.0 . . ? H2C1 N2C H2C2 120.0 . . ? C16C O4C Cu1 119.1(2) . . ? C16C O5C Cu2 127.1(2) . . ? O1D C1D N1D 119.5(4) . . ? O1D C1D C2D 123.8(4) . . ? N1D C1D C2D 116.6(4) . . ? C6D C2D C3D 120.6(5) . . ? C6D C2D C1D 118.6(5) . . ? C3D C2D C1D 120.6(4) . . ? C2D C3D C4D 120.5(4) . . ? C2D C3D C9D 120.5(5) . . ? C4D C3D C9D 119.0(5) . . ? C12D C4D C3D 120.2(5) . . ? C12D C4D C5D 120.3(5) . . ? C3D C4D C5D 119.5(4) . . ? O2D C5D N1D 120.9(4) . . ? O2D C5D C4D 122.0(4) . . ? N1D C5D C4D 117.0(4) . . ? C2D C6D C7D 117.8(6) . . ? C2D C6D H6D 121.1 . . ? C7D C6D H6D 121.1 . . ? C8D C7D C6D 121.3(6) . . ? C8D C7D H7D 119.4 . . ? C6D C7D H7D 119.4 . . ? C7D C8D C9D 121.9(6) . . ? C7D C8D H8D 119.0 . . ? C9D C8D H8D 119.0 . . ? C8D C9D C3D 117.8(6) . . ? C8D C9D C10D 123.5(6) . . ? C3D C9D C10D 118.7(6) . . ? C11D C10D C9D 121.3(6) . . ? C11D C10D H10D 119.4 . . ? C9D C10D H10D 119.4 . . ? C10D C11D C12D 120.2(6) . . ? C10D C11D H11D 119.9 . . ? C12D C11D H11D 119.9 . . ? C4D C12D C11D 120.4(6) . . ? C4D C12D H12D 119.8 . . ? C11D C12D H12D 119.8 . . ? N1D C13D C14D 113.2(3) . . ? N1D C13D C16D 110.1(3) . . ? C14D C13D C16D 112.0(3) . . ? N1D C13D H13D 107.1 . . ? C14D C13D H13D 107.1 . . ? C16D C13D H13D 107.1 . . ? C15D C14D C13D 113.4(3) . . ? C15D C14D H14G 108.9 . . ? C13D C14D H14G 108.9 . . ? C15D C14D H14H 108.9 . . ? C13D C14D H14H 108.9 . . ? H14G C14D H14H 107.7 . . ? O3D C15D N2D 123.2(4) . . ? O3D C15D C14D 120.8(4) . . ? N2D C15D C14D 115.9(4) . . ? O4D C16D O5D 126.9(3) . . ? O4D C16D C13D 119.8(3) . . ? O5D C16D C13D 113.3(3) . . ? C5D N1D C1D 124.8(4) . . ? C5D N1D C13D 118.5(3) . . ? C1D N1D C13D 116.5(3) . . ? C15D N2D H2D1 120.0 . . ? C15D N2D H2D2 120.0 . . ? H2D1 N2D H2D2 120.0 . . ? C16D O4D Cu1 126.7(2) . . ? C16D O5D Cu2 119.8(2) . . ? O1E C1E N1E 119.7(3) . . ? O1E C1E C2E 123.5(3) . . ? N1E C1E C2E 116.7(3) . . ? C6E C2E C3E 119.7(4) . . ? C6E C2E C1E 120.3(4) . . ? C3E C2E C1E 120.0(4) . . ? C4E C3E C9E 119.9(4) . . ? C4E C3E C2E 120.4(3) . . ? C9E C3E C2E 119.7(4) . . ? C12E C4E C3E 120.0(4) . . ? C12E C4E C5E 119.3(4) . . ? C3E C4E C5E 120.7(3) . . ? O2E C5E N1E 120.6(3) . . ? O2E C5E C4E 123.1(3) . . ? N1E C5E C4E 116.3(3) . . ? C2E C6E C7E 121.1(4) . . ? C2E C6E H6E 119.4 . . ? C7E C6E H6E 119.4 . . ? C8E C7E C6E 119.4(5) . . ? C8E C7E H7E 120.3 . . ? C6E C7E H7E 120.3 . . ? C7E C8E C9E 122.3(4) . . ? C7E C8E H8E 118.8 . . ? C9E C8E H8E 118.8 . . ? C8E C9E C10E 124.1(4) . . ? C8E C9E C3E 117.8(4) . . ? C10E C9E C3E 118.1(5) . . ? C11E C10E C9E 121.4(4) . . ? C11E C10E H10E 119.3 . . ? C9E C10E H10E 119.3 . . ? C10E C11E C12E 121.0(4) . . ? C10E C11E H11E 119.5 . . ? C12E C11E H11E 119.5 . . ? C4E C12E C11E 119.6(5) . . ? C4E C12E H12E 120.2 . . ? C11E C12E H12E 120.2 . . ? N1E C13E C16E 110.3(2) . . ? N1E C13E C14E 109.9(3) . . ? C16E C13E C14E 113.9(3) . . ? N1E C13E H13E 107.5 . . ? C16E C13E H13E 107.5 . . ? C14E C13E H13E 107.5 . . ? C15E C14E C13E 118.4(3) . . ? C15E C14E H14I 107.7 . . ? C13E C14E H14I 107.7 . . ? C15E C14E H14J 107.7 . . ? C13E C14E H14J 107.7 . . ? H14I C14E H14J 107.1 . . ? O3E C15E N2E 122.8(3) . . ? O3E C15E C14E 116.6(3) . . ? N2E C15E C14E 120.6(3) . . ? O4E C16E O5E 126.9(3) . . ? O4E C16E C13E 117.2(3) . . ? O5E C16E C13E 115.8(3) . . ? C5E N1E C1E 125.9(3) . . ? C5E N1E C13E 117.8(3) . . ? C1E N1E C13E 116.2(3) . . ? C15E N2E H2E1 120.0 . . ? C15E N2E H2E2 120.0 . . ? H2E1 N2E H2E2 120.0 . . ? C15E O3E Cu2 125.0(2) . . ? C16E O4E Cu3 115.4(2) . . ? C16E O5E Cu4 129.9(2) . . ? O1F C1F N1F 119.7(3) . . ? O1F C1F C2F 124.1(3) . . ? N1F C1F C2F 116.2(3) . . ? C6F C2F C3F 121.0(4) . . ? C6F C2F C1F 119.3(4) . . ? C3F C2F C1F 119.7(3) . . ? C4F C3F C2F 121.8(3) . . ? C4F C3F C9F 119.5(4) . . ? C2F C3F C9F 118.8(4) . . ? C12F C4F C3F 119.9(4) . . ? C12F C4F C5F 119.9(4) . . ? C3F C4F C5F 120.2(3) . . ? O2F C5F N1F 121.0(3) . . ? O2F C5F C4F 122.6(3) . . ? N1F C5F C4F 116.4(3) . . ? C2F C6F C7F 120.4(4) . . ? C2F C6F H6F 119.8 . . ? C7F C6F H6F 119.8 . . ? C8F C7F C6F 120.2(5) . . ? C8F C7F H7F 119.9 . . ? C6F C7F H7F 119.9 . . ? C7F C8F C9F 121.4(4) . . ? C7F C8F H8F 119.3 . . ? C9F C8F H8F 119.3 . . ? C10F C9F C8F 123.4(4) . . ? C10F C9F C3F 118.5(4) . . ? C8F C9F C3F 118.1(4) . . ? C11F C10F C9F 120.9(4) . . ? C11F C10F H10F 119.6 . . ? C9F C10F H10F 119.6 . . ? C10F C11F C12F 120.3(4) . . ? C10F C11F H11F 119.8 . . ? C12F C11F H11F 119.8 . . ? C4F C12F C11F 120.9(4) . . ? C4F C12F H12F 119.6 . . ? C11F C12F H12F 119.6 . . ? N1F C13F C16F 111.9(3) . . ? N1F C13F C14F 110.4(3) . . ? C16F C13F C14F 115.4(3) . . ? N1F C13F H13F 106.1 . . ? C16F C13F H13F 106.1 . . ? C14F C13F H13F 106.1 . . ? C15F C14F C13F 114.5(3) . . ? C15F C14F H14K 108.6 . . ? C13F C14F H14K 108.6 . . ? C15F C14F H14L 108.6 . . ? C13F C14F H14L 108.6 . . ? H14K C14F H14L 107.6 . . ? O3F C15F N2F 122.9(3) . . ? O3F C15F C14F 121.0(3) . . ? N2F C15F C14F 116.0(3) . . ? O4F C16F O5F 126.0(3) . . ? O4F C16F C13F 116.5(3) . . ? O5F C16F C13F 117.2(3) . . ? C5F N1F C1F 125.2(3) . . ? C5F N1F C13F 117.0(3) . . ? C1F N1F C13F 117.2(3) . . ? C15F N2F H2F1 120.0 . . ? C15F N2F H2F2 120.0 . . ? H2F1 N2F H2F2 120.0 . . ? C16F O4F Cu3 128.8(2) . . ? C16F O5F Cu4 116.0(2) . . ? O1G C1G N1G 119.7(3) . . ? O1G C1G C2G 122.6(3) . . ? N1G C1G C2G 117.7(3) . . ? C6G C2G C3G 119.9(3) . . ? C6G C2G C1G 120.5(3) . . ? C3G C2G C1G 119.6(3) . . ? C4G C3G C9G 120.5(3) . . ? C4G C3G C2G 120.1(3) . . ? C9G C3G C2G 119.3(3) . . ? C12G C4G C3G 120.0(3) . . ? C12G C4G C5G 118.9(3) . . ? C3G C4G C5G 121.1(3) . . ? O2G C5G N1G 119.8(3) . . ? O2G C5G C4G 123.0(3) . . ? N1G C5G C4G 117.2(3) . . ? C2G C6G C7G 120.4(4) . . ? C2G C6G H6G 119.8 . . ? C7G C6G H6G 119.8 . . ? C8G C7G C6G 120.3(4) . . ? C8G C7G H7G 119.8 . . ? C6G C7G H7G 119.8 . . ? C7G C8G C9G 121.1(4) . . ? C7G C8G H8G 119.5 . . ? C9G C8G H8G 119.5 . . ? C8G C9G C3G 119.0(4) . . ? C8G C9G C10G 122.9(4) . . ? C3G C9G C10G 118.1(4) . . ? C11G C10G C9G 120.4(4) . . ? C11G C10G H10G 119.8 . . ? C9G C10G H10G 119.8 . . ? C10G C11G C12G 121.1(4) . . ? C10G C11G H11G 119.5 . . ? C12G C11G H11G 119.5 . . ? C4G C12G C11G 119.9(4) . . ? C4G C12G H12G 120.1 . . ? C11G C12G H12G 120.1 . . ? N1G C13G C14G 110.0(3) . . ? N1G C13G C16G 111.7(3) . . ? C14G C13G C16G 114.5(3) . . ? N1G C13G H13G 106.7 . . ? C14G C13G H13G 106.7 . . ? C16G C13G H13G 106.7 . . ? C13G C14G C15G 112.4(3) . . ? C13G C14G H14M 109.1 . . ? C15G C14G H14M 109.1 . . ? C13G C14G H14N 109.1 . . ? C15G C14G H14N 109.1 . . ? H14M C14G H14N 107.9 . . ? O3G C15G N2G 121.8(4) . . ? O3G C15G C14G 123.2(4) . . ? N2G C15G C14G 115.0(4) . . ? O5G C16G O4G 127.5(3) . . ? O5G C16G C13G 117.2(3) . . ? O4G C16G C13G 115.1(3) . . ? C1G N1G C5G 124.4(3) . . ? C1G N1G C13G 118.0(3) . . ? C5G N1G C13G 117.1(3) . . ? C15G N2G H2G1 120.0 . . ? C15G N2G H2G2 120.0 . . ? H2G1 N2G H2G2 120.0 . . ? C16G O4G Cu3 124.1(2) . . ? C16G O5G Cu4 119.8(2) . . ? O1H C1H N1H 119.5(3) . . ? O1H C1H C2H 122.3(3) . . ? N1H C1H C2H 118.2(3) . . ? C6H C2H C3H 120.1(3) . . ? C6H C2H C1H 120.5(3) . . ? C3H C2H C1H 119.4(3) . . ? C4H C3H C9H 120.7(3) . . ? C4H C3H C2H 120.1(3) . . ? C9H C3H C2H 119.3(4) . . ? C12H C4H C3H 119.0(4) . . ? C12H C4H C5H 119.1(4) . . ? C3H C4H C5H 121.8(3) . . ? O2H C5H N1H 119.4(4) . . ? O2H C5H C4H 124.6(3) . . ? N1H C5H C4H 116.0(3) . . ? C2H C6H C7H 120.6(4) . . ? C2H C6H H6H 119.7 . . ? C7H C6H H6H 119.7 . . ? C8H C7H C6H 120.9(4) . . ? C8H C7H H7H 119.6 . . ? C6H C7H H7H 119.6 . . ? C7H C8H C9H 120.6(4) . . ? C7H C8H H8H 119.7 . . ? C9H C8H H8H 119.7 . . ? C10H C9H C3H 118.5(4) . . ? C10H C9H C8H 123.0(4) . . ? C3H C9H C8H 118.6(4) . . ? C11H C10H C9H 120.7(4) . . ? C11H C10H H10H 119.7 . . ? C9H C10H H10H 119.7 . . ? C10H C11H C12H 120.6(4) . . ? C10H C11H H11H 119.7 . . ? C12H C11H H11H 119.7 . . ? C11H C12H C4H 120.5(4) . . ? C11H C12H H12H 119.7 . . ? C4H C12H H12H 119.7 . . ? N1H C13H C16H 111.1(3) . . ? N1H C13H C14H 112.0(3) . . ? C16H C13H C14H 113.0(3) . . ? N1H C13H H13H 106.8 . . ? C16H C13H H13H 106.8 . . ? C14H C13H H13H 106.8 . . ? C15H C14H C13H 109.6(3) . . ? C15H C14H H14O 109.8 . . ? C13H C14H H14O 109.8 . . ? C15H C14H H14P 109.8 . . ? C13H C14H H14P 109.8 . . ? H14O C14H H14P 108.2 . . ? O3H C15H N2H 123.4(4) . . ? O3H C15H C14H 118.4(4) . . ? N2H C15H C14H 118.2(4) . . ? O4H C16H O5H 126.9(3) . . ? O4H C16H C13H 116.2(3) . . ? O5H C16H C13H 116.9(3) . . ? C1H N1H C5H 124.1(3) . . ? C1H N1H C13H 116.8(3) . . ? C5H N1H C13H 119.0(3) . . ? C15H N2H H2H1 120.0 . . ? C15H N2H H2H2 120.0 . . ? H2H1 N2H H2H2 120.0 . . ? C16H O4H Cu3 120.7(2) . . ? C16H O5H Cu4 124.6(2) . . ? N3 C21 C22 123.6(5) . . ? N3 C21 H21 118.2 . . ? C22 C21 H21 118.2 . . ? C21 C22 C23 118.9(5) . . ? C21 C22 H22 120.6 . . ? C23 C22 H22 120.6 . . ? C22 C23 C24 119.1(5) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 120.5 . . ? C23 C24 C25 118.0(5) . . ? C23 C24 H24 121.0 . . ? C25 C24 H24 121.0 . . ? N3 C25 C24 122.9(5) . . ? N3 C25 H25 118.6 . . ? C24 C25 H25 118.6 . . ? C21 N3 C25 117.5(3) . . ? C21 N3 Cu1 119.7(3) . . ? C25 N3 Cu1 122.6(3) . . ? O6 C26 H26A 109.5 . . ? O6 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O6 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C26 O6 Cu3 117.8(3) . . ? C26 O6 H6M 103.2 . . ? Cu3 O6 H6M 117.7 . . ? O7 C27 H27A 109.5 . . ? O7 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O7 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C27 O7 H7M 108.5 . . ? O8 C28 H28A 109.5 . . ? O8 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O8 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C28 O8 H8M 122.5 . . ? Cl2 C1S Cl1 111.7(2) . . ? Cl2 C1S H1S1 109.3 . . ? Cl1 C1S H1S1 109.3 . . ? Cl2 C1S H1S2 109.3 . . ? Cl1 C1S H1S2 109.3 . . ? H1S1 C1S H1S2 107.9 . . ? Cl4 C2S Cl3 111.5(3) . . ? Cl4 C2S H2S1 109.3 . . ? Cl3 C2S H2S1 109.3 . . ? Cl4 C2S H2S2 109.3 . . ? Cl3 C2S H2S2 109.3 . . ? H2S1 C2S H2S2 108.0 . . ? Cl5 C3S Cl6 113.4(4) . . ? Cl5 C3S H3S1 108.9 . . ? Cl6 C3S H3S1 108.9 . . ? Cl5 C3S H3S2 108.9 . . ? Cl6 C3S H3S2 108.9 . . ? H3S1 C3S H3S2 107.7 . . ? C30 C29 H29D 109.5 . . ? C30 C29 H29E 109.5 . . ? H29D C29 H29E 109.5 . . ? C30 C29 H29F 109.5 . . ? H29D C29 H29F 109.5 . . ? H29E C29 H29F 109.5 . . ? O10 C30 C29 107.7(6) . . ? O10 C30 H30C 110.2 . . ? C29 C30 H30C 110.2 . . ? O10 C30 H30D 110.2 . . ? C29 C30 H30D 110.2 . . ? H30C C30 H30D 108.5 . . ? O10 C31 C32 107.6(6) . . ? O10 C31 H31C 110.2 . . ? C32 C31 H31C 110.2 . . ? O10 C31 H31D 110.2 . . ? C32 C31 H31D 110.2 . . ? H31C C31 H31D 108.5 . . ? C31 C32 H32D 109.5 . . ? C31 C32 H32E 109.5 . . ? H32D C32 H32E 109.5 . . ? C31 C32 H32F 109.5 . . ? H32D C32 H32F 109.5 . . ? H32E C32 H32F 109.5 . . ? C31 O10 C30 116.1(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4C Cu1 Cu2 O5B -90.66(10) . . . . ? O4A Cu1 Cu2 O5B 90.51(10) . . . . ? O4B Cu1 Cu2 O5B 0.05(10) . . . . ? O4D Cu1 Cu2 O5B 178.69(10) . . . . ? O4C Cu1 Cu2 O5D 91.26(10) . . . . ? O4A Cu1 Cu2 O5D -87.58(10) . . . . ? O4B Cu1 Cu2 O5D -178.03(9) . . . . ? O4D Cu1 Cu2 O5D 0.61(10) . . . . ? O4C Cu1 Cu2 O5C 2.45(10) . . . . ? O4A Cu1 Cu2 O5C -176.39(10) . . . . ? O4B Cu1 Cu2 O5C 93.16(9) . . . . ? O4D Cu1 Cu2 O5C -88.21(10) . . . . ? O4C Cu1 Cu2 O5A -178.74(10) . . . . ? O4A Cu1 Cu2 O5A 2.42(10) . . . . ? O4B Cu1 Cu2 O5A -88.03(9) . . . . ? O4D Cu1 Cu2 O5A 90.61(10) . . . . ? O4E Cu3 Cu4 O5H -89.99(10) . . . . ? O4G Cu3 Cu4 O5H 84.83(10) . . . . ? O4H Cu3 Cu4 O5H -3.80(10) . . . . ? O4F Cu3 Cu4 O5H -178.95(10) . . . . ? O6 Cu3 Cu4 O5H 168.5(4) . . . . ? O4E Cu3 Cu4 O5F 87.61(9) . . . . ? O4G Cu3 Cu4 O5F -97.57(9) . . . . ? O4H Cu3 Cu4 O5F 173.80(9) . . . . ? O4F Cu3 Cu4 O5F -1.35(9) . . . . ? O6 Cu3 Cu4 O5F -13.9(4) . . . . ? O4E Cu3 Cu4 O5G -178.89(9) . . . . ? O4G Cu3 Cu4 O5G -4.07(9) . . . . ? O4H Cu3 Cu4 O5G -92.70(9) . . . . ? O4F Cu3 Cu4 O5G 92.15(9) . . . . ? O6 Cu3 Cu4 O5G 79.6(4) . . . . ? O4E Cu3 Cu4 O5E 2.05(10) . . . . ? O4G Cu3 Cu4 O5E 176.87(10) . . . . ? O4H Cu3 Cu4 O5E 88.24(9) . . . . ? O4F Cu3 Cu4 O5E -86.91(9) . . . . ? O6 Cu3 Cu4 O5E -99.5(4) . . . . ? O1A C1A C2A C6A 0.0(5) . . . . ? N1A C1A C2A C6A 177.9(3) . . . . ? O1A C1A C2A C3A -179.8(3) . . . . ? N1A C1A C2A C3A -1.9(5) . . . . ? C6A C2A C3A C4A -179.4(4) . . . . ? C1A C2A C3A C4A 0.5(5) . . . . ? C6A C2A C3A C9A 0.4(6) . . . . ? C1A C2A C3A C9A -179.8(3) . . . . ? C2A C3A C4A C12A -176.8(4) . . . . ? C9A C3A C4A C12A 3.5(5) . . . . ? C2A C3A C4A C5A 3.4(5) . . . . ? C9A C3A C4A C5A -176.3(3) . . . . ? C12A C4A C5A O2A -5.9(5) . . . . ? C3A C4A C5A O2A 173.9(4) . . . . ? C12A C4A C5A N1A 174.5(3) . . . . ? C3A C4A C5A N1A -5.7(5) . . . . ? C3A C2A C6A C7A -0.6(6) . . . . ? C1A C2A C6A C7A 179.6(4) . . . . ? C2A C6A C7A C8A 1.2(7) . . . . ? C6A C7A C8A C9A -1.7(8) . . . . ? C7A C8A C9A C10A -177.0(5) . . . . ? C7A C8A C9A C3A 1.5(7) . . . . ? C2A C3A C9A C10A 177.8(4) . . . . ? C4A C3A C9A C10A -2.4(6) . . . . ? C2A C3A C9A C8A -0.8(6) . . . . ? C4A C3A C9A C8A 178.9(4) . . . . ? C8A C9A C10A C11A 179.2(4) . . . . ? C3A C9A C10A C11A 0.7(6) . . . . ? C9A C10A C11A C12A 0.1(7) . . . . ? C3A C4A C12A C11A -2.8(6) . . . . ? C5A C4A C12A C11A 177.1(3) . . . . ? C10A C11A C12A C4A 0.9(6) . . . . ? N1A C13A C14A C15A -160.4(3) . . . . ? C16A C13A C14A C15A 73.4(4) . . . . ? C13A C14A C15A O3A 65.4(4) . . . . ? C13A C14A C15A N2A -117.7(3) . . . . ? N1A C13A C16A O5A -166.1(3) . . . . ? C14A C13A C16A O5A -38.7(4) . . . . ? N1A C13A C16A O4A 14.7(4) . . . . ? C14A C13A C16A O4A 142.1(3) . . . . ? O2A C5A N1A C1A -175.3(3) . . . . ? C4A C5A N1A C1A 4.4(5) . . . . ? O2A C5A N1A C13A -3.2(5) . . . . ? C4A C5A N1A C13A 176.4(3) . . . . ? O1A C1A N1A C5A 177.3(3) . . . . ? C2A C1A N1A C5A -0.7(5) . . . . ? O1A C1A N1A C13A 5.1(5) . . . . ? C2A C1A N1A C13A -172.9(3) . . . . ? C16A C13A N1A C5A -110.4(3) . . . . ? C14A C13A N1A C5A 122.6(3) . . . . ? C16A C13A N1A C1A 62.2(4) . . . . ? C14A C13A N1A C1A -64.7(4) . . . . ? N2A C15A O3A Cu4 -12.2(5) . . . . ? C14A C15A O3A Cu4 164.5(2) . . . . ? O5H Cu4 O3A C15A 135.5(3) . . . . ? O5F Cu4 O3A C15A -41.2(3) . . . . ? O5G Cu4 O3A C15A -135.3(3) . . . . ? O5E Cu4 O3A C15A 44.8(3) . . . . ? O5A C16A O4A Cu1 10.9(4) . . . . ? C13A C16A O4A Cu1 -170.0(2) . . . . ? O4B Cu1 O4A C16A 69.8(2) . . . . ? O4D Cu1 O4A C16A -84.5(2) . . . . ? N3 Cu1 O4A C16A 169.0(2) . . . . ? Cu2 Cu1 O4A C16A -7.0(2) . . . . ? O4A C16A O5A Cu2 -8.2(5) . . . . ? C13A C16A O5A Cu2 172.7(2) . . . . ? O5B Cu2 O5A C16A -88.4(3) . . . . ? O5D Cu2 O5A C16A 90.6(3) . . . . ? O5C Cu2 O5A C16A 4.5(4) . . . . ? O3E Cu2 O5A C16A -176.5(3) . . . . ? Cu1 Cu2 O5A C16A 1.6(3) . . . . ? O1B C1B C2B C6B -5.2(6) . . . . ? N1B C1B C2B C6B 173.8(4) . . . . ? O1B C1B C2B C3B 174.6(4) . . . . ? N1B C1B C2B C3B -6.3(5) . . . . ? C6B C2B C3B C4B -177.6(4) . . . . ? C1B C2B C3B C4B 2.6(6) . . . . ? C6B C2B C3B C9B 1.0(6) . . . . ? C1B C2B C3B C9B -178.9(4) . . . . ? C2B C3B C4B C12B 179.6(4) . . . . ? C9B C3B C4B C12B 1.0(6) . . . . ? C2B C3B C4B C5B 0.4(6) . . . . ? C9B C3B C4B C5B -178.2(4) . . . . ? C12B C4B C5B O2B 0.8(7) . . . . ? C3B C4B C5B O2B 180.0(4) . . . . ? C12B C4B C5B N1B -178.8(4) . . . . ? C3B C4B C5B N1B 0.4(6) . . . . ? C3B C2B C6B C7B -0.3(7) . . . . ? C1B C2B C6B C7B 179.6(4) . . . . ? C2B C6B C7B C8B -0.7(8) . . . . ? C6B C7B C8B C9B 0.9(8) . . . . ? C7B C8B C9B C10B 178.2(5) . . . . ? C7B C8B C9B C3B -0.2(7) . . . . ? C4B C3B C9B C10B -0.6(6) . . . . ? C2B C3B C9B C10B -179.2(4) . . . . ? C4B C3B C9B C8B 177.9(4) . . . . ? C2B C3B C9B C8B -0.7(6) . . . . ? C8B C9B C10B C11B -178.4(4) . . . . ? C3B C9B C10B C11B 0.0(6) . . . . ? C9B C10B C11B C12B 0.3(7) . . . . ? C3B C4B C12B C11B -0.7(7) . . . . ? C5B C4B C12B C11B 178.4(4) . . . . ? C10B C11B C12B C4B 0.1(7) . . . . ? N1B C13B C14B C15B -169.4(3) . . . . ? C16B C13B C14B C15B 65.7(4) . . . . ? C13B C14B C15B O3B 34.8(5) . . . . ? C13B C14B C15B N2B -145.6(3) . . . . ? N1B C13B C16B O4B 50.0(4) . . . . ? C14B C13B C16B O4B 175.7(3) . . . . ? N1B C13B C16B O5B -133.3(3) . . . . ? C14B C13B C16B O5B -7.7(4) . . . . ? O1B C1B N1B C5B -173.3(4) . . . . ? C2B C1B N1B C5B 7.7(6) . . . . ? O1B C1B N1B C13B 3.4(5) . . . . ? C2B C1B N1B C13B -175.7(3) . . . . ? O2B C5B N1B C1B 175.7(4) . . . . ? C4B C5B N1B C1B -4.7(6) . . . . ? O2B C5B N1B C13B -1.0(6) . . . . ? C4B C5B N1B C13B 178.6(3) . . . . ? C16B C13B N1B C1B 46.3(4) . . . . ? C14B C13B N1B C1B -80.4(4) . . . . ? C16B C13B N1B C5B -136.8(3) . . . . ? C14B C13B N1B C5B 96.6(4) . . . . ? O5B C16B O4B Cu1 0.6(5) . . . . ? C13B C16B O4B Cu1 176.7(2) . . . . ? O4C Cu1 O4B C16B 87.5(3) . . . . ? O4A Cu1 O4B C16B -88.6(3) . . . . ? O4D Cu1 O4B C16B -3.4(4) . . . . ? N3 Cu1 O4B C16B 179.8(3) . . . . ? Cu2 Cu1 O4B C16B -0.3(2) . . . . ? O4B C16B O5B Cu2 -0.4(4) . . . . ? C13B C16B O5B Cu2 -176.7(2) . . . . ? O5C Cu2 O5B C16B -78.2(2) . . . . ? O5A Cu2 O5B C16B 78.2(2) . . . . ? O3E Cu2 O5B C16B 176.8(2) . . . . ? Cu1 Cu2 O5B C16B 0.1(2) . . . . ? O1C C1C C2C C6C 3.8(5) . . . . ? N1C C1C C2C C6C -178.5(3) . . . . ? O1C C1C C2C C3C -177.0(3) . . . . ? N1C C1C C2C C3C 0.7(5) . . . . ? C6C C2C C3C C4C 179.4(4) . . . . ? C1C C2C C3C C4C 0.2(5) . . . . ? C6C C2C C3C C9C -0.2(5) . . . . ? C1C C2C C3C C9C -179.5(3) . . . . ? C2C C3C C4C C12C -178.8(3) . . . . ? C9C C3C C4C C12C 0.9(5) . . . . ? C2C C3C C4C C5C 1.1(5) . . . . ? C9C C3C C4C C5C -179.2(3) . . . . ? C12C C4C C5C O2C -4.0(5) . . . . ? C3C C4C C5C O2C 176.1(3) . . . . ? C12C C4C C5C N1C 176.7(3) . . . . ? C3C C4C C5C N1C -3.2(5) . . . . ? C3C C2C C6C C7C 0.4(6) . . . . ? C1C C2C C6C C7C 179.7(4) . . . . ? C2C C6C C7C C8C -0.4(7) . . . . ? C6C C7C C8C C9C 0.1(8) . . . . ? C7C C8C C9C C10C 179.3(5) . . . . ? C7C C8C C9C C3C 0.1(7) . . . . ? C4C C3C C9C C10C 1.0(6) . . . . ? C2C C3C C9C C10C -179.3(4) . . . . ? C4C C3C C9C C8C -179.7(4) . . . . ? C2C C3C C9C C8C 0.0(6) . . . . ? C8C C9C C10C C11C 178.8(4) . . . . ? C3C C9C C10C C11C -2.0(6) . . . . ? C9C C10C C11C C12C 1.0(7) . . . . ? C3C C4C C12C C11C -1.8(6) . . . . ? C5C C4C C12C C11C 178.2(3) . . . . ? C10C C11C C12C C4C 0.9(6) . . . . ? N1C C13C C14C C15C -45.6(4) . . . . ? C16C C13C C14C C15C -171.8(3) . . . . ? C13C C14C C15C O3C -43.0(5) . . . . ? C13C C14C C15C N2C 138.0(4) . . . . ? N1C C13C C16C O5C -162.3(3) . . . . ? C14C C13C C16C O5C -35.1(4) . . . . ? N1C C13C C16C O4C 18.7(4) . . . . ? C14C C13C C16C O4C 145.9(3) . . . . ? O1C C1C N1C C5C 174.5(3) . . . . ? C2C C1C N1C C5C -3.2(5) . . . . ? O1C C1C N1C C13C -1.5(5) . . . . ? C2C C1C N1C C13C -179.2(3) . . . . ? O2C C5C N1C C1C -174.9(3) . . . . ? C4C C5C N1C C1C 4.4(5) . . . . ? O2C C5C N1C C13C 1.1(5) . . . . ? C4C C5C N1C C13C -179.6(3) . . . . ? C16C C13C N1C C1C 62.4(4) . . . . ? C14C C13C N1C C1C -63.2(4) . . . . ? C16C C13C N1C C5C -113.9(3) . . . . ? C14C C13C N1C C5C 120.4(3) . . . . ? O5C C16C O4C Cu1 10.0(5) . . . . ? C13C C16C O4C Cu1 -171.1(2) . . . . ? O4B Cu1 O4C C16C -83.3(2) . . . . ? O4D Cu1 O4C C16C 70.9(2) . . . . ? N3 Cu1 O4C C16C 177.5(3) . . . . ? Cu2 Cu1 O4C C16C -6.6(2) . . . . ? O4C C16C O5C Cu2 -7.1(5) . . . . ? C13C C16C O5C Cu2 174.0(2) . . . . ? O5B Cu2 O5C C16C 90.1(3) . . . . ? O5D Cu2 O5C C16C -88.1(3) . . . . ? O5A Cu2 O5C C16C -1.8(4) . . . . ? O3E Cu2 O5C C16C 179.3(3) . . . . ? Cu1 Cu2 O5C C16C 1.1(3) . . . . ? O1D C1D C2D C6D 2.8(7) . . . . ? N1D C1D C2D C6D -177.7(4) . . . . ? O1D C1D C2D C3D -172.2(5) . . . . ? N1D C1D C2D C3D 7.2(7) . . . . ? C6D C2D C3D C4D 177.4(5) . . . . ? C1D C2D C3D C4D -7.6(7) . . . . ? C6D C2D C3D C9D -2.4(8) . . . . ? C1D C2D C3D C9D 172.5(5) . . . . ? C2D C3D C4D C12D 177.4(5) . . . . ? C9D C3D C4D C12D -2.8(8) . . . . ? C2D C3D C4D C5D 0.0(7) . . . . ? C9D C3D C4D C5D 179.8(5) . . . . ? C12D C4D C5D O2D 7.5(7) . . . . ? C3D C4D C5D O2D -175.1(5) . . . . ? C12D C4D C5D N1D -169.6(4) . . . . ? C3D C4D C5D N1D 7.8(7) . . . . ? C3D C2D C6D C7D -0.2(8) . . . . ? C1D C2D C6D C7D -175.3(5) . . . . ? C2D C6D C7D C8D 2.2(10) . . . . ? C6D C7D C8D C9D -1.4(12) . . . . ? C7D C8D C9D C3D -1.3(11) . . . . ? C7D C8D C9D C10D 176.2(7) . . . . ? C2D C3D C9D C8D 3.2(9) . . . . ? C4D C3D C9D C8D -176.7(6) . . . . ? C2D C3D C9D C10D -174.4(5) . . . . ? C4D C3D C9D C10D 5.7(8) . . . . ? C8D C9D C10D C11D 177.8(7) . . . . ? C3D C9D C10D C11D -4.7(10) . . . . ? C9D C10D C11D C12D 0.6(10) . . . . ? C3D C4D C12D C11D -1.4(8) . . . . ? C5D C4D C12D C11D 176.0(5) . . . . ? C10D C11D C12D C4D 2.5(9) . . . . ? N1D C13D C14D C15D -61.3(4) . . . . ? C16D C13D C14D C15D 173.6(3) . . . . ? C13D C14D C15D O3D 71.8(5) . . . . ? C13D C14D C15D N2D -107.9(4) . . . . ? N1D C13D C16D O4D 42.4(4) . . . . ? C14D C13D C16D O4D 169.3(3) . . . . ? N1D C13D C16D O5D -140.4(3) . . . . ? C14D C13D C16D O5D -13.5(4) . . . . ? O2D C5D N1D C1D 174.4(4) . . . . ? C4D C5D N1D C1D -8.4(6) . . . . ? O2D C5D N1D C13D -2.4(6) . . . . ? C4D C5D N1D C13D 174.8(4) . . . . ? O1D C1D N1D C5D -179.4(4) . . . . ? C2D C1D N1D C5D 1.1(6) . . . . ? O1D C1D N1D C13D -2.5(6) . . . . ? C2D C1D N1D C13D 178.0(4) . . . . ? C14D C13D N1D C5D 109.0(4) . . . . ? C16D C13D N1D C5D -124.8(4) . . . . ? C14D C13D N1D C1D -68.1(4) . . . . ? C16D C13D N1D C1D 58.1(4) . . . . ? O5D C16D O4D Cu1 5.3(5) . . . . ? C13D C16D O4D Cu1 -177.9(2) . . . . ? O4C Cu1 O4D C16D -90.8(3) . . . . ? O4A Cu1 O4D C16D 85.8(3) . . . . ? O4B Cu1 O4D C16D 0.1(4) . . . . ? N3 Cu1 O4D C16D 176.9(3) . . . . ? Cu2 Cu1 O4D C16D -3.0(2) . . . . ? O4D C16D O5D Cu2 -4.1(4) . . . . ? C13D C16D O5D Cu2 178.9(2) . . . . ? O5C Cu2 O5D C16D 79.7(2) . . . . ? O5A Cu2 O5D C16D -76.8(2) . . . . ? O3E Cu2 O5D C16D -175.3(2) . . . . ? Cu1 Cu2 O5D C16D 1.3(2) . . . . ? O1E C1E C2E C6E -1.7(6) . . . . ? N1E C1E C2E C6E 179.5(3) . . . . ? O1E C1E C2E C3E 177.9(3) . . . . ? N1E C1E C2E C3E -0.8(5) . . . . ? C6E C2E C3E C4E -179.6(4) . . . . ? C1E C2E C3E C4E 0.7(5) . . . . ? C6E C2E C3E C9E 0.3(5) . . . . ? C1E C2E C3E C9E -179.3(3) . . . . ? C9E C3E C4E C12E 0.2(5) . . . . ? C2E C3E C4E C12E -179.8(4) . . . . ? C9E C3E C4E C5E 179.0(3) . . . . ? C2E C3E C4E C5E -1.0(5) . . . . ? C12E C4E C5E O2E -1.0(5) . . . . ? C3E C4E C5E O2E -179.8(3) . . . . ? C12E C4E C5E N1E -179.7(3) . . . . ? C3E C4E C5E N1E 1.5(5) . . . . ? C3E C2E C6E C7E -0.2(6) . . . . ? C1E C2E C6E C7E 179.4(4) . . . . ? C2E C6E C7E C8E -0.4(7) . . . . ? C6E C7E C8E C9E 0.9(8) . . . . ? C7E C8E C9E C10E 179.5(5) . . . . ? C7E C8E C9E C3E -0.8(7) . . . . ? C4E C3E C9E C8E -179.9(4) . . . . ? C2E C3E C9E C8E 0.2(6) . . . . ? C4E C3E C9E C10E -0.1(6) . . . . ? C2E C3E C9E C10E 179.9(4) . . . . ? C8E C9E C10E C11E 179.4(5) . . . . ? C3E C9E C10E C11E -0.3(6) . . . . ? C9E C10E C11E C12E 0.6(7) . . . . ? C3E C4E C12E C11E 0.1(6) . . . . ? C5E C4E C12E C11E -178.7(4) . . . . ? C10E C11E C12E C4E -0.5(7) . . . . ? N1E C13E C14E C15E -158.3(3) . . . . ? C16E C13E C14E C15E 77.2(4) . . . . ? C13E C14E C15E O3E 167.8(3) . . . . ? C13E C14E C15E N2E -11.6(5) . . . . ? N1E C13E C16E O4E 37.3(4) . . . . ? C14E C13E C16E O4E 161.5(3) . . . . ? N1E C13E C16E O5E -146.3(3) . . . . ? C14E C13E C16E O5E -22.1(4) . . . . ? O2E C5E N1E C1E 179.6(3) . . . . ? C4E C5E N1E C1E -1.7(5) . . . . ? O2E C5E N1E C13E 3.1(5) . . . . ? C4E C5E N1E C13E -178.1(3) . . . . ? O1E C1E N1E C5E -177.4(3) . . . . ? C2E C1E N1E C5E 1.4(5) . . . . ? O1E C1E N1E C13E -0.9(4) . . . . ? C2E C1E N1E C13E 177.9(3) . . . . ? C16E C13E N1E C5E -130.6(3) . . . . ? C14E C13E N1E C5E 102.9(3) . . . . ? C16E C13E N1E C1E 52.6(4) . . . . ? C14E C13E N1E C1E -73.9(3) . . . . ? N2E C15E O3E Cu2 -14.5(5) . . . . ? C14E C15E O3E Cu2 166.1(2) . . . . ? O5B Cu2 O3E C15E -134.6(3) . . . . ? O5D Cu2 O3E C15E 43.4(3) . . . . ? O5C Cu2 O3E C15E 132.7(3) . . . . ? O5A Cu2 O3E C15E -46.8(3) . . . . ? O5E C16E O4E Cu3 0.4(4) . . . . ? C13E C16E O4E Cu3 176.4(2) . . . . ? O4H Cu3 O4E C16E -86.7(2) . . . . ? O4F Cu3 O4E C16E 75.4(2) . . . . ? O6 Cu3 O4E C16E 166.6(2) . . . . ? Cu4 Cu3 O4E C16E -2.0(2) . . . . ? O4E C16E O5E Cu4 2.6(5) . . . . ? C13E C16E O5E Cu4 -173.4(2) . . . . ? O5H Cu4 O5E C16E 79.4(3) . . . . ? O5F Cu4 O5E C16E -94.5(3) . . . . ? O5G Cu4 O5E C16E -5.9(5) . . . . ? O3A Cu4 O5E C16E 173.7(3) . . . . ? Cu3 Cu4 O5E C16E -3.0(3) . . . . ? O1F C1F C2F C6F -2.3(6) . . . . ? N1F C1F C2F C6F 178.6(4) . . . . ? O1F C1F C2F C3F 176.2(4) . . . . ? N1F C1F C2F C3F -2.9(5) . . . . ? C6F C2F C3F C4F 179.6(4) . . . . ? C1F C2F C3F C4F 1.1(6) . . . . ? C6F C2F C3F C9F 0.6(6) . . . . ? C1F C2F C3F C9F -177.8(4) . . . . ? C2F C3F C4F C12F 177.2(4) . . . . ? C9F C3F C4F C12F -3.9(6) . . . . ? C2F C3F C4F C5F -3.0(5) . . . . ? C9F C3F C4F C5F 176.0(3) . . . . ? C12F C4F C5F O2F 7.6(6) . . . . ? C3F C4F C5F O2F -172.3(4) . . . . ? C12F C4F C5F N1F -173.6(3) . . . . ? C3F C4F C5F N1F 6.6(5) . . . . ? C3F C2F C6F C7F -1.8(7) . . . . ? C1F C2F C6F C7F 176.6(4) . . . . ? C2F C6F C7F C8F 0.1(8) . . . . ? C6F C7F C8F C9F 2.9(8) . . . . ? C7F C8F C9F C10F 177.1(5) . . . . ? C7F C8F C9F C3F -4.0(7) . . . . ? C4F C3F C9F C10F 2.2(6) . . . . ? C2F C3F C9F C10F -178.8(4) . . . . ? C4F C3F C9F C8F -176.7(4) . . . . ? C2F C3F C9F C8F 2.3(6) . . . . ? C8F C9F C10F C11F -179.8(5) . . . . ? C3F C9F C10F C11F 1.4(7) . . . . ? C9F C10F C11F C12F -3.3(7) . . . . ? C3F C4F C12F C11F 2.0(6) . . . . ? C5F C4F C12F C11F -177.8(4) . . . . ? C10F C11F C12F C4F 1.6(6) . . . . ? N1F C13F C14F C15F -158.8(3) . . . . ? C16F C13F C14F C15F 73.1(4) . . . . ? C13F C14F C15F O3F 32.9(4) . . . . ? C13F C14F C15F N2F -151.5(3) . . . . ? N1F C13F C16F O4F 41.3(4) . . . . ? C14F C13F C16F O4F 168.7(3) . . . . ? N1F C13F C16F O5F -143.6(3) . . . . ? C14F C13F C16F O5F -16.2(4) . . . . ? O2F C5F N1F C1F 169.9(3) . . . . ? C4F C5F N1F C1F -9.0(5) . . . . ? O2F C5F N1F C13F -0.7(5) . . . . ? C4F C5F N1F C13F -179.6(3) . . . . ? O1F C1F N1F C5F -171.9(3) . . . . ? C2F C1F N1F C5F 7.2(5) . . . . ? O1F C1F N1F C13F -1.4(5) . . . . ? C2F C1F N1F C13F 177.8(3) . . . . ? C16F C13F N1F C5F -135.9(3) . . . . ? C14F C13F N1F C5F 94.1(3) . . . . ? C16F C13F N1F C1F 52.7(4) . . . . ? C14F C13F N1F C1F -77.3(4) . . . . ? O5F C16F O4F Cu3 -15.3(5) . . . . ? C13F C16F O4F Cu3 159.3(2) . . . . ? O4E Cu3 O4F C16F -83.5(3) . . . . ? O4G Cu3 O4F C16F 89.8(3) . . . . ? O4H Cu3 O4F C16F -7.2(5) . . . . ? O6 Cu3 O4F C16F -174.2(3) . . . . ? Cu4 Cu3 O4F C16F 8.3(2) . . . . ? O4F C16F O5F Cu4 11.8(4) . . . . ? C13F C16F O5F Cu4 -162.8(2) . . . . ? O5G Cu4 O5F C16F -88.6(2) . . . . ? O5E Cu4 O5F C16F 71.9(2) . . . . ? O3A Cu4 O5F C16F 168.6(2) . . . . ? Cu3 Cu4 O5F C16F -4.1(2) . . . . ? O1G C1G C2G C6G -2.1(5) . . . . ? N1G C1G C2G C6G 178.3(3) . . . . ? O1G C1G C2G C3G 178.7(3) . . . . ? N1G C1G C2G C3G -0.9(5) . . . . ? C6G C2G C3G C4G 179.9(3) . . . . ? C1G C2G C3G C4G -0.9(5) . . . . ? C6G C2G C3G C9G -0.5(5) . . . . ? C1G C2G C3G C9G 178.7(3) . . . . ? C9G C3G C4G C12G 0.2(5) . . . . ? C2G C3G C4G C12G 179.8(3) . . . . ? C9G C3G C4G C5G -178.3(3) . . . . ? C2G C3G C4G C5G 1.3(5) . . . . ? C12G C4G C5G O2G 1.5(5) . . . . ? C3G C4G C5G O2G -180.0(3) . . . . ? C12G C4G C5G N1G -178.4(3) . . . . ? C3G C4G C5G N1G 0.2(5) . . . . ? C3G C2G C6G C7G 0.3(6) . . . . ? C1G C2G C6G C7G -178.9(4) . . . . ? C2G C6G C7G C8G 0.3(6) . . . . ? C6G C7G C8G C9G -0.7(6) . . . . ? C7G C8G C9G C3G 0.4(6) . . . . ? C7G C8G C9G C10G -179.7(4) . . . . ? C4G C3G C9G C8G 179.7(4) . . . . ? C2G C3G C9G C8G 0.1(5) . . . . ? C4G C3G C9G C10G -0.2(5) . . . . ? C2G C3G C9G C10G -179.8(3) . . . . ? C8G C9G C10G C11G 179.8(4) . . . . ? C3G C9G C10G C11G -0.3(6) . . . . ? C9G C10G C11G C12G 0.6(6) . . . . ? C3G C4G C12G C11G 0.1(6) . . . . ? C5G C4G C12G C11G 178.7(4) . . . . ? C10G C11G C12G C4G -0.6(6) . . . . ? N1G C13G C14G C15G -162.0(3) . . . . ? C16G C13G C14G C15G 71.2(4) . . . . ? C13G C14G C15G O3G 16.4(5) . . . . ? C13G C14G C15G N2G -165.2(4) . . . . ? N1G C13G C16G O5G -135.8(3) . . . . ? C14G C13G C16G O5G -9.9(4) . . . . ? N1G C13G C16G O4G 49.1(4) . . . . ? C14G C13G C16G O4G 175.0(3) . . . . ? O1G C1G N1G C5G -177.1(3) . . . . ? C2G C1G N1G C5G 2.5(5) . . . . ? O1G C1G N1G C13G -5.9(5) . . . . ? C2G C1G N1G C13G 173.8(3) . . . . ? O2G C5G N1G C1G 177.9(3) . . . . ? C4G C5G N1G C1G -2.2(5) . . . . ? O2G C5G N1G C13G 6.6(5) . . . . ? C4G C5G N1G C13G -173.5(3) . . . . ? C14G C13G N1G C1G -73.0(4) . . . . ? C16G C13G N1G C1G 55.3(4) . . . . ? C14G C13G N1G C5G 98.9(3) . . . . ? C16G C13G N1G C5G -132.8(3) . . . . ? O5G C16G O4G Cu3 9.9(5) . . . . ? C13G C16G O4G Cu3 -175.6(2) . . . . ? O4H Cu3 O4G C16G 84.3(3) . . . . ? O4F Cu3 O4G C16G -77.5(3) . . . . ? O6 Cu3 O4G C16G -169.1(2) . . . . ? Cu4 Cu3 O4G C16G -0.7(2) . . . . ? O4G C16G O5G Cu4 -15.2(4) . . . . ? C13G C16G O5G Cu4 170.4(2) . . . . ? O5H Cu4 O5G C16G -72.6(2) . . . . ? O5F Cu4 O5G C16G 100.3(2) . . . . ? O5E Cu4 O5G C16G 13.0(4) . . . . ? O3A Cu4 O5G C16G -166.6(2) . . . . ? Cu3 Cu4 O5G C16G 10.2(2) . . . . ? O1H C1H C2H C6H 1.6(6) . . . . ? N1H C1H C2H C6H -177.4(3) . . . . ? O1H C1H C2H C3H 179.5(3) . . . . ? N1H C1H C2H C3H 0.5(5) . . . . ? C6H C2H C3H C4H -179.2(3) . . . . ? C1H C2H C3H C4H 2.9(5) . . . . ? C6H C2H C3H C9H -0.4(5) . . . . ? C1H C2H C3H C9H -178.3(3) . . . . ? C9H C3H C4H C12H 0.8(5) . . . . ? C2H C3H C4H C12H 179.7(3) . . . . ? C9H C3H C4H C5H -180.0(3) . . . . ? C2H C3H C4H C5H -1.1(5) . . . . ? C12H C4H C5H O2H -3.4(6) . . . . ? C3H C4H C5H O2H 177.3(4) . . . . ? C12H C4H C5H N1H 175.3(3) . . . . ? C3H C4H C5H N1H -3.9(5) . . . . ? C3H C2H C6H C7H 0.2(6) . . . . ? C1H C2H C6H C7H 178.1(4) . . . . ? C2H C6H C7H C8H 0.2(6) . . . . ? C6H C7H C8H C9H -0.4(6) . . . . ? C4H C3H C9H C10H -0.4(6) . . . . ? C2H C3H C9H C10H -179.2(3) . . . . ? C4H C3H C9H C8H 179.0(3) . . . . ? C2H C3H C9H C8H 0.2(5) . . . . ? C7H C8H C9H C10H 179.6(4) . . . . ? C7H C8H C9H C3H 0.2(6) . . . . ? C3H C9H C10H C11H -0.2(6) . . . . ? C8H C9H C10H C11H -179.6(4) . . . . ? C9H C10H C11H C12H 0.4(6) . . . . ? C10H C11H C12H C4H 0.0(6) . . . . ? C3H C4H C12H C11H -0.6(6) . . . . ? C5H C4H C12H C11H -179.9(4) . . . . ? N1H C13H C14H C15H -67.0(4) . . . . ? C16H C13H C14H C15H 166.5(3) . . . . ? C13H C14H C15H O3H -70.6(5) . . . . ? C13H C14H C15H N2H 109.9(4) . . . . ? N1H C13H C16H O4H 53.0(4) . . . . ? C14H C13H C16H O4H 179.9(3) . . . . ? N1H C13H C16H O5H -130.1(3) . . . . ? C14H C13H C16H O5H -3.2(4) . . . . ? O1H C1H N1H C5H 174.9(3) . . . . ? C2H C1H N1H C5H -6.1(5) . . . . ? O1H C1H N1H C13H -5.8(5) . . . . ? C2H C1H N1H C13H 173.2(3) . . . . ? O2H C5H N1H C1H -173.5(4) . . . . ? C4H C5H N1H C1H 7.7(5) . . . . ? O2H C5H N1H C13H 7.2(5) . . . . ? C4H C5H N1H C13H -171.6(3) . . . . ? C16H C13H N1H C1H 52.5(4) . . . . ? C14H C13H N1H C1H -74.9(4) . . . . ? C16H C13H N1H C5H -128.2(3) . . . . ? C14H C13H N1H C5H 104.4(4) . . . . ? O5H C16H O4H Cu3 0.3(5) . . . . ? C13H C16H O4H Cu3 176.8(2) . . . . ? O4E Cu3 O4H C16H 95.1(2) . . . . ? O4G Cu3 O4H C16H -79.8(2) . . . . ? O4F Cu3 O4H C16H 18.3(5) . . . . ? O6 Cu3 O4H C16H -175.2(2) . . . . ? Cu4 Cu3 O4H C16H 3.1(2) . . . . ? O4H C16H O5H Cu4 -5.7(5) . . . . ? C13H C16H O5H Cu4 177.7(2) . . . . ? O5G Cu4 O5H C16H 90.6(3) . . . . ? O5E Cu4 O5H C16H -70.0(3) . . . . ? O3A Cu4 O5H C16H -166.9(3) . . . . ? Cu3 Cu4 O5H C16H 5.9(2) . . . . ? N3 C21 C22 C23 -1.2(9) . . . . ? C21 C22 C23 C24 2.4(10) . . . . ? C22 C23 C24 C25 -1.4(9) . . . . ? C23 C24 C25 N3 -0.9(8) . . . . ? C22 C21 N3 C25 -1.1(7) . . . . ? C22 C21 N3 Cu1 174.4(4) . . . . ? C24 C25 N3 C21 2.1(6) . . . . ? C24 C25 N3 Cu1 -173.2(4) . . . . ? O4C Cu1 N3 C21 159.1(3) . . . . ? O4A Cu1 N3 C21 -21.8(3) . . . . ? O4B Cu1 N3 C21 68.5(3) . . . . ? O4D Cu1 N3 C21 -110.1(3) . . . . ? O4C Cu1 N3 C25 -25.7(3) . . . . ? O4A Cu1 N3 C25 153.4(3) . . . . ? O4B Cu1 N3 C25 -116.3(3) . . . . ? O4D Cu1 N3 C25 65.1(3) . . . . ? O4E Cu3 O6 C26 -32.7(4) . . . . ? O4G Cu3 O6 C26 151.2(4) . . . . ? O4H Cu3 O6 C26 -119.1(4) . . . . ? O4F Cu3 O6 C26 56.6(4) . . . . ? Cu4 Cu3 O6 C26 68.9(5) . . . . ? C32 C31 O10 C30 179.9(7) . . . . ? C29 C30 O10 C31 179.5(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2A H2A1 O5E 0.88 2.35 3.085(4) 141 . N2A H2A1 O5F 0.88 2.58 3.076(4) 117 . N2A H2A2 O3B 0.88 2.27 3.133(4) 165 . N2B H2B1 O3F 0.88 2.06 2.932(4) 170 . N2E H2E1 O5D 0.88 2.05 2.810(4) 144 . N2E H2E2 O1H 0.88 2.04 2.830(4) 148 . N2E H2E2 O5E 0.88 2.40 2.876(4) 114 . N2F H2F1 O3B 0.88 2.15 3.000(4) 164 . N2H H2H2 O3D 0.88 2.08 2.875(5) 149 . O6 H6M O7 0.83 1.85 2.673(4) 170 . N2C H2C1 O5F 0.88 2.36 3.047(4) 135 1_655 N2C H2C2 O3G 0.88 2.10 2.981(4) 177 1_655 N2D H2D1 O2G 0.88 2.35 2.888(4) 120 1_655 N2D H2D2 O8 0.88 2.37 3.232(6) 168 1_655 N2F H2F2 O3C 0.88 2.04 2.891(4) 161 1_455 N2G H2G1 O1C 0.88 2.02 2.895(5) 174 1_455 N2H H2H1 O10 0.88 2.08 2.915(5) 159 4_566 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.531 _refine_diff_density_min -0.316 _refine_diff_density_rms 0.060 _vrf_PLAT602_2 ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: Solvent species in some regions of the asymmetric unit could not be resolved due to disorder. These were treated as diffusely scattering volumes, and their contributions to the structure factors were removed with the SQUEEZE program implemented in PLATON. The voids found by CHECKCIF are actually filled with the disordered solvent removed by Squeeze. ; #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 799345' #TrackingRef 'jhCC3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C138 H103 Cu4 N17 O43, 3(C5 H10 O3) ' _chemical_formula_sum 'C153 H133 Cu4 N17 O52' _chemical_formula_weight 3295.92 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 15.1091(8) _cell_length_b 21.4458(12) _cell_length_c 52.381(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 16972.8(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4043 _cell_measurement_theta_min 2.266 _cell_measurement_theta_max 15.533 _exptl_crystal_description 'rectangular bar' _exptl_crystal_colour blue _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.290 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6808 _exptl_absorpt_coefficient_mu 0.579 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 167453 _diffrn_reflns_av_R_equivalents 0.2058 _diffrn_reflns_av_sigmaI/netI 0.2214 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -56 _diffrn_reflns_limit_l_max 56 _diffrn_reflns_theta_min 0.78 _diffrn_reflns_theta_max 22.59 _reflns_number_total 22429 _reflns_number_gt 9535 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART Version 5.625 (Bruker, 2001)' _computing_cell_refinement 'SAINT-Plus Version 6.45 (Bruker, 2001)' _computing_data_reduction 'SAINT-Plus Version 6.45 (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics various _computing_publication_material 'SHELXTL Version 6.14 (Bruker, 2000)' _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^)+(0.0940P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(2) _refine_ls_number_reflns 22429 _refine_ls_number_parameters 850 _refine_ls_number_restraints 1351 _refine_ls_R_factor_all 0.1534 _refine_ls_R_factor_gt 0.0866 _refine_ls_wR_factor_ref 0.2220 _refine_ls_wR_factor_gt 0.1940 _refine_ls_goodness_of_fit_ref 0.846 _refine_ls_restrained_S_all 0.854 _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 0.96193(9) 0.41574(7) 0.30634(3) 0.0413(4) Uani 1 1 d D . . Cu2 Cu 0.92841(10) 0.40402(7) 0.35698(3) 0.0415(4) Uani 1 1 d . A . Cu3 Cu 0.55116(9) 0.54425(7) 0.45920(3) 0.0369(4) Uani 1 1 d . A . Cu4 Cu 0.57194(9) 0.51860(7) 0.41089(3) 0.0349(4) Uani 1 1 d D . . C1G C 0.4290(7) 0.7299(5) 0.4290(2) 0.048(4) Uiso 1 1 d D . . C2G C 0.4366(7) 0.7924(5) 0.4412(2) 0.055(4) Uiso 1 1 d D . . C3G C 0.3645(7) 0.8119(5) 0.4557(2) 0.049(4) Uiso 1 1 d D . . C4G C 0.2878(7) 0.7799(5) 0.4578(2) 0.053(4) Uiso 1 1 d D . . C5G C 0.2791(8) 0.7187(5) 0.4452(2) 0.061(4) Uiso 1 1 d D . . C6G C 0.5119(8) 0.8269(5) 0.4384(2) 0.055(4) Uiso 1 1 d D . . H6G H 0.5592 0.8129 0.4279 0.065 Uiso 1 1 calc R . . C7G C 0.5169(9) 0.8858(6) 0.4520(3) 0.071(5) Uiso 1 1 d D . . H7G H 0.5688 0.9107 0.4511 0.085 Uiso 1 1 calc R . . C8G C 0.4488(9) 0.9041(7) 0.4656(3) 0.093(5) Uiso 1 1 d D . . H8G H 0.4542 0.9437 0.4736 0.111 Uiso 1 1 calc R . . C9G C 0.3715(8) 0.8734(6) 0.4696(3) 0.066(4) Uiso 1 1 d D . . C10G C 0.2972(8) 0.8884(6) 0.4828(3) 0.077(5) Uiso 1 1 d D . . H10G H 0.2986 0.9277 0.4911 0.093 Uiso 1 1 calc R . . C11G C 0.2239(8) 0.8568(6) 0.4857(2) 0.057(4) Uiso 1 1 d D . . H11G H 0.1771 0.8724 0.4960 0.068 Uiso 1 1 calc R . . C12G C 0.2164(8) 0.7989(6) 0.4730(2) 0.066(4) Uiso 1 1 d D . . H12G H 0.1649 0.7739 0.4747 0.079 Uiso 1 1 calc R . . C13G C 0.3482(8) 0.6340(5) 0.4188(2) 0.041(3) Uiso 1 1 d D . . H13G H 0.2939 0.6129 0.4255 0.049 Uiso 1 1 calc R . . N1G N 0.3530(6) 0.6964(4) 0.43244(18) 0.045(3) Uiso 1 1 d D . . O1G O 0.4901(5) 0.7097(4) 0.41568(16) 0.054(2) Uiso 1 1 d D . . O2G O 0.2133(6) 0.6868(4) 0.44469(18) 0.072(3) Uiso 1 1 d D . . C14G C 0.3286(10) 0.6488(7) 0.3908(3) 0.066(4) Uiso 1 1 d . . . H14O H 0.2845 0.6829 0.3899 0.079 Uiso 1 1 calc R . . H14P H 0.3835 0.6634 0.3824 0.079 Uiso 1 1 calc R . . C15G C 0.2939(9) 0.5930(7) 0.3769(3) 0.061(4) Uiso 1 1 d . . . C16G C 0.4223(8) 0.5918(6) 0.4247(2) 0.043(3) Uiso 1 1 d . . . N2G N 0.3098(8) 0.5900(6) 0.3522(2) 0.092(4) Uiso 1 1 d . . . H2G1 H 0.2934 0.5570 0.3435 0.110 Uiso 1 1 calc R . . H2G2 H 0.3369 0.6210 0.3445 0.110 Uiso 1 1 calc R . . O3G O 0.2551(7) 0.5485(5) 0.38798(19) 0.079(3) Uiso 1 1 d . . . O4G O 0.4460(5) 0.5876(3) 0.44762(13) 0.040(2) Uiso 1 1 d . A . O5G O 0.4554(5) 0.5630(3) 0.40650(14) 0.038(2) Uiso 1 1 d . . . C1A C 0.6867(10) 0.3881(6) 0.2844(3) 0.0993(14) Uiso 1 1 d D A . C2A C 0.6777(7) 0.3626(6) 0.2578(2) 0.0993(14) Uiso 1 1 d D . . C3A C 0.6605(7) 0.4056(6) 0.2387(2) 0.0993(14) Uiso 1 1 d D . . C4A C 0.6493(11) 0.4670(6) 0.2426(2) 0.0993(14) Uiso 1 1 d D . . C5A C 0.6578(11) 0.4927(6) 0.2692(2) 0.0993(14) Uiso 1 1 d D A . C6A C 0.6851(11) 0.2986(7) 0.2553(3) 0.0993(14) Uiso 1 1 d D . . H6A H 0.6982 0.2722 0.2694 0.119 Uiso 1 1 calc R . . C7A C 0.6714(11) 0.2739(7) 0.2294(3) 0.0993(14) Uiso 1 1 d D . . H7A H 0.6665 0.2305 0.2261 0.119 Uiso 1 1 calc R . . C8A C 0.6664(11) 0.3150(7) 0.2114(3) 0.0993(14) Uiso 1 1 d D . . H8A H 0.6711 0.2980 0.1947 0.119 Uiso 1 1 calc R . . C9A C 0.6560(11) 0.3765(6) 0.2118(3) 0.0993(14) Uiso 1 1 d D . . C10A C 0.6355(10) 0.4217(7) 0.1968(3) 0.0993(14) Uiso 1 1 d D . . H10A H 0.6247 0.4080 0.1799 0.119 Uiso 1 1 calc R . . C11A C 0.6260(11) 0.4814(7) 0.1992(3) 0.0993(14) Uiso 1 1 d D . . H11A H 0.6133 0.5061 0.1846 0.119 Uiso 1 1 calc R . . C12A C 0.6344(10) 0.5095(7) 0.2230(3) 0.0993(14) Uiso 1 1 d D . . H12A H 0.6304 0.5532 0.2256 0.119 Uiso 1 1 calc R . . C16A C 0.7898(8) 0.4500(6) 0.3197(2) 0.043(3) Uiso 1 1 d D . . N1A N 0.6761(9) 0.4509(6) 0.2894(2) 0.0993(14) Uiso 1 1 d D . . O1A O 0.7032(7) 0.3512(5) 0.3016(2) 0.0993(14) Uiso 1 1 d D . . O2A O 0.6495(7) 0.5480(5) 0.2750(2) 0.0993(14) Uiso 1 1 d D . . O4A O 0.8456(5) 0.4498(4) 0.30175(16) 0.051(2) Uiso 1 1 d . A . O5A O 0.8126(5) 0.4389(4) 0.34326(14) 0.040(2) Uiso 1 1 d . A . C13A C 0.7000(7) 0.4697(6) 0.3150(2) 0.0417(17) Uiso 0.50 1 d PD A 3 H13A H 0.6953 0.5160 0.3167 0.050 Uiso 0.50 1 calc PR A 3 C14A C 0.6356(14) 0.4374(11) 0.3337(3) 0.0417(17) Uiso 0.50 1 d PD A 3 H14A H 0.5751 0.4493 0.3283 0.050 Uiso 0.50 1 calc PR A 3 H14B H 0.6411 0.3920 0.3307 0.050 Uiso 0.50 1 calc PR A 3 C15A C 0.6396(14) 0.4468(8) 0.3625(3) 0.0417(17) Uiso 0.50 1 d PD A 3 N2A N 0.6689(11) 0.3997(8) 0.3780(3) 0.0417(17) Uiso 0.50 1 d PD A 3 H2A1 H 0.6632 0.4029 0.3947 0.050 Uiso 0.50 1 calc PR A 3 H2A2 H 0.6935 0.3663 0.3713 0.050 Uiso 0.50 1 calc PR A 3 O3A O 0.6048(10) 0.4939(8) 0.3728(2) 0.0417(17) Uiso 0.50 1 d PD A 3 C13Z C 0.7000(7) 0.4697(6) 0.3150(2) 0.0417(17) Uiso 0.50 1 d PD A 4 H13Z H 0.7092 0.5154 0.3124 0.050 Uiso 0.50 1 calc PR A 4 C14Z C 0.6302(13) 0.4708(11) 0.3345(3) 0.0417(17) Uiso 0.50 1 d PD A 4 H14Z H 0.6183 0.4267 0.3389 0.050 Uiso 0.50 1 calc PR A 4 H14Y H 0.5764 0.4865 0.3259 0.050 Uiso 0.50 1 calc PR A 4 C15Z C 0.6363(12) 0.5051(9) 0.3594(3) 0.0417(17) Uiso 0.50 1 d PD A 4 N2Z N 0.7007(11) 0.5473(8) 0.3608(3) 0.0417(17) Uiso 0.50 1 d PD A 4 H2Z1 H 0.7008 0.5749 0.3732 0.050 Uiso 0.50 1 calc PR A 4 H2Z2 H 0.7431 0.5476 0.3493 0.050 Uiso 0.50 1 calc PR A 4 O3Z O 0.5701(10) 0.4928(8) 0.37196(18) 0.0417(17) Uiso 0.50 1 d PD A 4 C1B C 0.9871(8) 0.1950(7) 0.3126(3) 0.0788(12) Uiso 1 1 d D . . C2B C 1.0464(8) 0.1589(7) 0.2945(2) 0.0788(12) Uiso 1 1 d D . . C3B C 1.0051(8) 0.1276(7) 0.2751(3) 0.0788(12) Uiso 1 1 d D . . C4B C 0.9190(8) 0.1306(7) 0.2698(2) 0.0788(12) Uiso 1 1 d D . . C5B C 0.8560(8) 0.1654(7) 0.2878(2) 0.0788(12) Uiso 1 1 d D . . C6B C 1.1343(8) 0.1581(7) 0.2988(3) 0.0788(12) Uiso 1 1 d D . . H6B H 1.1597 0.1811 0.3124 0.095 Uiso 1 1 calc R . . C7B C 1.1902(9) 0.1198(7) 0.2814(3) 0.0788(12) Uiso 1 1 d D . . H7B H 1.2523 0.1155 0.2837 0.095 Uiso 1 1 calc R . . C8B C 1.1484(8) 0.0930(7) 0.2631(3) 0.0788(12) Uiso 1 1 d D . . H8B H 1.1856 0.0701 0.2519 0.095 Uiso 1 1 calc R . . C9B C 1.0643(8) 0.0911(7) 0.2568(2) 0.0788(12) Uiso 1 1 d D . . C10B C 1.0189(9) 0.0653(7) 0.2378(3) 0.0788(12) Uiso 1 1 d D . . H10B H 1.0532 0.0403 0.2265 0.095 Uiso 1 1 calc R . . C11B C 0.9374(9) 0.0687(6) 0.2322(2) 0.0788(12) Uiso 1 1 d D . . H11B H 0.9143 0.0497 0.2172 0.095 Uiso 1 1 calc R . . C12B C 0.8820(9) 0.1021(7) 0.2494(2) 0.0788(12) Uiso 1 1 d D . . H12B H 0.8199 0.1044 0.2466 0.095 Uiso 1 1 calc R . . C13B C 0.8446(10) 0.2387(7) 0.3244(3) 0.0788(12) Uiso 1 1 d D B . H13B H 0.7853 0.2445 0.3162 0.095 Uiso 1 1 calc R . . N1B N 0.8982(7) 0.1968(6) 0.3077(2) 0.0788(12) Uiso 1 1 d D . . O1B O 1.0196(6) 0.2215(5) 0.33077(19) 0.0788(12) Uiso 1 1 d D . . O2B O 0.7787(6) 0.1738(5) 0.28386(18) 0.0788(12) Uiso 1 1 d D . . C14B C 0.8315(9) 0.2040(6) 0.3490(2) 0.057(4) Uiso 1 1 d . . . H14C H 0.8865 0.2062 0.3592 0.068 Uiso 1 1 calc R . . H14D H 0.8194 0.1596 0.3453 0.068 Uiso 1 1 calc R . . C15B C 0.7511(10) 0.2327(7) 0.3651(3) 0.066(4) Uiso 1 1 d . . . C16B C 0.8860(8) 0.3014(6) 0.3275(2) 0.043(3) Uiso 1 1 d . . . N2B N 0.7611(8) 0.2321(6) 0.3889(2) 0.076(4) Uiso 1 1 d . . . H2B1 H 0.7234 0.2520 0.3988 0.091 Uiso 1 1 calc R . . H2B2 H 0.8059 0.2117 0.3957 0.091 Uiso 1 1 calc R . . O3B O 0.6895(7) 0.2604(5) 0.3544(2) 0.092(4) Uiso 1 1 d . . . O4B O 0.9136(5) 0.3286(3) 0.30763(14) 0.040(2) Uiso 1 1 d . B . O5B O 0.8851(5) 0.3221(4) 0.34994(15) 0.039(2) Uiso 1 1 d . A . C1C C 1.2567(11) 0.4452(6) 0.3125(3) 0.0982(16) Uiso 1 1 d D . . C2C C 1.3061(11) 0.4680(6) 0.2888(3) 0.0982(16) Uiso 1 1 d D . . C3C C 1.3471(11) 0.4213(6) 0.2747(3) 0.0982(16) Uiso 1 1 d D . . C4C C 1.3433(11) 0.3600(6) 0.2800(3) 0.0982(16) Uiso 1 1 d D . . C5C C 1.2876(11) 0.3362(6) 0.3015(3) 0.0982(16) Uiso 1 1 d D . . C6C C 1.3110(10) 0.5301(7) 0.2846(3) 0.0982(16) Uiso 1 1 d D . . H6C H 1.2838 0.5588 0.2960 0.118 Uiso 1 1 calc R . . C7C C 1.3605(11) 0.5523(7) 0.2615(3) 0.0982(16) Uiso 1 1 d D . . H7C H 1.3646 0.5949 0.2566 0.118 Uiso 1 1 calc R . . C8C C 1.3973(11) 0.5063(7) 0.2490(3) 0.0982(16) Uiso 1 1 d D . . H8C H 1.4322 0.5206 0.2351 0.118 Uiso 1 1 calc R . . C9C C 1.3981(11) 0.4446(7) 0.2509(3) 0.0982(16) Uiso 1 1 d D . . C10C C 1.4274(11) 0.3952(7) 0.2383(3) 0.0982(16) Uiso 1 1 d D . . H10C H 1.4574 0.4047 0.2228 0.118 Uiso 1 1 calc R . . C11C C 1.4223(11) 0.3372(7) 0.2432(3) 0.0982(16) Uiso 1 1 d D . . H11C H 1.4479 0.3088 0.2315 0.118 Uiso 1 1 calc R . . C12C C 1.3801(10) 0.3121(7) 0.2656(3) 0.0982(16) Uiso 1 1 d D . . H12C H 1.3777 0.2691 0.2699 0.118 Uiso 1 1 calc R . . C13C C 1.2021(11) 0.3618(8) 0.3406(3) 0.0982(16) Uiso 1 1 d D B . H13C H 1.2075 0.3154 0.3418 0.118 Uiso 1 1 calc R . . N1C N 1.2526(9) 0.3833(5) 0.3181(2) 0.0982(16) Uiso 1 1 d D . . O1C O 1.2154(7) 0.4823(5) 0.32542(19) 0.085(3) Uiso 1 1 d D . . O2C O 1.2766(7) 0.2835(5) 0.3072(2) 0.103(4) Uiso 1 1 d D . . C14C C 1.2327(8) 0.3905(7) 0.3663(3) 0.062(4) Uiso 1 1 d . . . H14E H 1.2151 0.4349 0.3671 0.074 Uiso 1 1 calc R . . H14F H 1.2045 0.3682 0.3807 0.074 Uiso 1 1 calc R . . C15C C 1.3346(9) 0.3847(7) 0.3682(3) 0.060(4) Uiso 1 1 d . . . C16C C 1.1050(8) 0.3782(6) 0.3358(2) 0.046(4) Uiso 1 1 d . . . N2C N 1.3756(8) 0.4346(6) 0.3756(2) 0.071(4) Uiso 1 1 d . . . H2C1 H 1.4336 0.4344 0.3772 0.085 Uiso 1 1 calc R . . H2C2 H 1.3455 0.4688 0.3789 0.085 Uiso 1 1 calc R . . O3C O 1.3693(7) 0.3364(5) 0.3632(2) 0.086(3) Uiso 1 1 d . . . O4C O 1.0779(5) 0.3856(4) 0.31395(15) 0.049(2) Uiso 1 1 d . B . O5C O 1.0560(5) 0.3773(4) 0.35570(15) 0.047(2) Uiso 1 1 d . A . C1D C 0.9055(7) 0.6295(6) 0.3228(2) 0.064(4) Uiso 1 1 d D . . C2D C 0.8775(7) 0.6708(5) 0.3016(2) 0.048(4) Uiso 1 1 d D . . C3D C 0.9394(7) 0.7048(6) 0.2884(2) 0.064(4) Uiso 1 1 d D . . C4D C 1.0255(8) 0.7051(6) 0.2951(2) 0.068(4) Uiso 1 1 d D . . C5D C 1.0567(9) 0.6666(7) 0.3169(3) 0.108(6) Uiso 1 1 d D . . C6D C 0.7894(8) 0.6690(7) 0.2953(3) 0.080(5) Uiso 1 1 d D . . H6D H 0.7488 0.6424 0.3038 0.097 Uiso 1 1 calc R . . C7D C 0.7620(10) 0.7108(8) 0.2747(3) 0.112(7) Uiso 1 1 d D . . H7D H 0.7011 0.7177 0.2713 0.135 Uiso 1 1 calc R . . C8D C 0.8228(9) 0.7383(8) 0.2612(3) 0.095(6) Uiso 1 1 d D . . H8D H 0.8029 0.7577 0.2459 0.114 Uiso 1 1 calc R . . C9D C 0.9106(8) 0.7431(6) 0.2660(2) 0.070(5) Uiso 1 1 d D . . C10D C 0.9786(8) 0.7706(6) 0.2532(3) 0.067(4) Uiso 1 1 d D . . H10D H 0.9633 0.7930 0.2381 0.080 Uiso 1 1 calc R . . C11D C 1.0618(10) 0.7696(7) 0.2592(3) 0.100(6) Uiso 1 1 d D . . H11D H 1.1044 0.7894 0.2486 0.120 Uiso 1 1 calc R . . C12D C 1.0883(9) 0.7382(7) 0.2819(3) 0.086(5) Uiso 1 1 d D . . H12D H 1.1478 0.7402 0.2877 0.104 Uiso 1 1 calc R . . C13D C 1.0238(9) 0.5848(6) 0.3482(2) 0.068(4) Uiso 1 1 d D B . H13D H 1.0900 0.5852 0.3486 0.082 Uiso 1 1 calc R . . N1D N 0.9945(6) 0.6289(5) 0.3291(2) 0.057(3) Uiso 1 1 d D . . O1D O 0.8559(6) 0.5940(4) 0.33409(17) 0.067(3) Uiso 1 1 d D . . O2D O 1.1328(8) 0.6670(6) 0.3250(2) 0.127(5) Uiso 1 1 d D . . C14D C 0.9870(11) 0.6057(8) 0.3759(3) 0.095(6) Uiso 1 1 d . . . H14G H 0.9216 0.6066 0.3753 0.114 Uiso 1 1 calc R . . H14H H 1.0048 0.5740 0.3886 0.114 Uiso 1 1 calc R . . C15D C 1.0194(14) 0.6672(10) 0.3844(4) 0.107(7) Uiso 1 1 d . . . C16D C 0.9935(8) 0.5196(6) 0.3427(2) 0.045(4) Uiso 1 1 d . . . N2D N 1.0916(10) 0.6635(7) 0.4009(3) 0.116(5) Uiso 1 1 d . . . H2D1 H 1.1125 0.6976 0.4081 0.139 Uiso 1 1 calc R . . H2D2 H 1.1164 0.6272 0.4041 0.139 Uiso 1 1 calc R . . O3D O 0.9847(10) 0.7140(7) 0.3796(3) 0.141(5) Uiso 1 1 d . . . O4D O 0.9974(5) 0.5028(4) 0.32006(15) 0.043(2) Uiso 1 1 d . B . O5D O 0.9719(5) 0.4869(4) 0.36132(15) 0.051(2) Uiso 1 1 d . A . C1E C 0.7299(7) 0.3828(5) 0.48725(19) 0.045(4) Uiso 1 1 d D . . C2E C 0.7377(8) 0.3513(6) 0.5128(2) 0.058(4) Uiso 1 1 d D . . C3E C 0.8080(8) 0.3676(6) 0.5286(2) 0.063(4) Uiso 1 1 d D . . C4E C 0.8720(8) 0.4072(7) 0.5217(2) 0.073(5) Uiso 1 1 d D . . C5E C 0.8677(8) 0.4382(6) 0.4968(2) 0.053(4) Uiso 1 1 d D . . C6E C 0.6760(9) 0.3094(6) 0.5199(2) 0.070(5) Uiso 1 1 d D . . H6E H 0.6296 0.2987 0.5085 0.084 Uiso 1 1 calc R . . C7E C 0.6800(10) 0.2798(8) 0.5456(3) 0.102(6) Uiso 1 1 d D . . H7E H 0.6357 0.2521 0.5516 0.122 Uiso 1 1 calc R . . C8E C 0.7482(10) 0.2948(8) 0.5588(3) 0.100(6) Uiso 1 1 d D . . H8E H 0.7533 0.2729 0.5746 0.120 Uiso 1 1 calc R . . C9E C 0.8130(10) 0.3354(7) 0.5545(3) 0.087(5) Uiso 1 1 d D . . C10E C 0.8853(10) 0.3520(8) 0.5681(3) 0.112(7) Uiso 1 1 d D . . H10E H 0.8904 0.3341 0.5846 0.135 Uiso 1 1 calc R . . C11E C 0.9485(11) 0.3893(7) 0.5614(3) 0.100(6) Uiso 1 1 d D . . H11E H 0.9978 0.3960 0.5723 0.121 Uiso 1 1 calc R . . C12E C 0.9427(9) 0.4197(7) 0.5375(3) 0.090(5) Uiso 1 1 d D . . H12E H 0.9871 0.4485 0.5324 0.108 Uiso 1 1 calc R . . C13E C 0.7908(8) 0.4489(6) 0.45451(19) 0.043(3) Uiso 1 1 d D A . H13E H 0.8369 0.4822 0.4537 0.051 Uiso 1 1 calc R . . N1E N 0.7968(6) 0.4215(4) 0.48006(16) 0.042(3) Uiso 1 1 d D . . O1E O 0.6705(5) 0.3693(4) 0.47200(15) 0.048(2) Uiso 1 1 d D . . O2E O 0.9227(6) 0.4740(4) 0.48841(17) 0.079(3) Uiso 1 1 d D . . C14E C 0.8181(10) 0.3990(7) 0.4350(3) 0.072(5) Uiso 1 1 d . . . H14I H 0.7647 0.3751 0.4301 0.087 Uiso 1 1 calc R . . H14J H 0.8592 0.3696 0.4435 0.087 Uiso 1 1 calc R . . C15E C 0.8629(13) 0.4234(10) 0.4104(4) 0.106(6) Uiso 1 1 d . B . C16E C 0.7040(8) 0.4802(6) 0.4499(2) 0.036(3) Uiso 1 1 d . . . N2E N 0.8620(10) 0.4849(8) 0.4066(3) 0.133(6) Uiso 1 1 d . . . H2E1 H 0.8852 0.5007 0.3925 0.159 Uiso 1 1 calc R . . H2E2 H 0.8383 0.5098 0.4181 0.159 Uiso 1 1 calc R . . O3E O 0.8922(6) 0.3940(4) 0.39605(18) 0.062(3) Uiso 1 1 d . . . O4E O 0.6643(5) 0.5045(4) 0.46775(14) 0.043(2) Uiso 1 1 d . A . O5E O 0.6821(5) 0.4808(4) 0.42622(14) 0.040(2) Uiso 1 1 d . A . C1F C 0.3245(8) 0.3771(7) 0.4564(3) 0.0796(12) Uiso 1 1 d D . . C2F C 0.2445(8) 0.3643(7) 0.4729(2) 0.0796(12) Uiso 1 1 d D . . C3F C 0.2580(8) 0.3346(7) 0.4957(2) 0.0796(12) Uiso 1 1 d D . . C4F C 0.3339(8) 0.3083(7) 0.5028(2) 0.0796(12) Uiso 1 1 d D . . C5F C 0.4127(8) 0.3128(7) 0.4855(2) 0.0796(12) Uiso 1 1 d D . . C6F C 0.1667(8) 0.3888(7) 0.4640(3) 0.0796(12) Uiso 1 1 d D . . H6F H 0.1623 0.4124 0.4487 0.096 Uiso 1 1 calc R . . C7F C 0.0894(9) 0.3744(7) 0.4808(3) 0.0796(12) Uiso 1 1 d D . . H7F H 0.0312 0.3875 0.4765 0.096 Uiso 1 1 calc R . . C8F C 0.1050(9) 0.3436(7) 0.5015(3) 0.0796(12) Uiso 1 1 d D . . H8F H 0.0525 0.3322 0.5103 0.096 Uiso 1 1 calc R . . C9F C 0.1773(8) 0.3243(7) 0.5131(3) 0.0796(12) Uiso 1 1 d D . . C10F C 0.1957(9) 0.2885(7) 0.5332(3) 0.0796(12) Uiso 1 1 d D . . H10F H 0.1464 0.2766 0.5434 0.096 Uiso 1 1 calc R . . C11F C 0.2707(9) 0.2680(7) 0.5407(3) 0.0796(12) Uiso 1 1 d D . . H11F H 0.2758 0.2486 0.5569 0.096 Uiso 1 1 calc R . . C12F C 0.3470(9) 0.2742(7) 0.5248(2) 0.0796(12) Uiso 1 1 d D . . H12F H 0.4025 0.2562 0.5291 0.096 Uiso 1 1 calc R . . C13F C 0.4760(9) 0.3550(7) 0.4453(3) 0.0796(12) Uiso 1 1 d D A . H13F H 0.5295 0.3382 0.4542 0.096 Uiso 1 1 calc R . . N1F N 0.4019(7) 0.3484(5) 0.4632(2) 0.0796(12) Uiso 1 1 d D . . O1F O 0.3212(6) 0.4078(5) 0.43682(19) 0.0796(12) Uiso 1 1 d D . . O2F O 0.4823(6) 0.2854(5) 0.48831(18) 0.0796(12) Uiso 1 1 d D . . C14F C 0.4613(8) 0.3143(6) 0.4219(2) 0.044(3) Uiso 1 1 d . . . H14K H 0.4343 0.2744 0.4273 0.053 Uiso 1 1 calc R . . H14L H 0.4190 0.3354 0.4103 0.053 Uiso 1 1 calc R . . C15F C 0.5463(10) 0.3009(6) 0.4074(3) 0.058(4) Uiso 1 1 d . . . C16F C 0.4935(7) 0.4236(6) 0.4405(2) 0.035(3) Uiso 1 1 d . . . N2F N 0.5395(9) 0.2943(5) 0.3821(2) 0.088(4) Uiso 1 1 d . . . H2F1 H 0.5866 0.2853 0.3730 0.105 Uiso 1 1 calc R . . H2F2 H 0.4878 0.2990 0.3746 0.105 Uiso 1 1 calc R . . O3F O 0.6193(6) 0.2943(4) 0.41780(16) 0.053(2) Uiso 1 1 d . . . O4F O 0.4959(5) 0.4605(4) 0.45781(15) 0.039(2) Uiso 1 1 d . A . O5F O 0.5194(5) 0.4379(3) 0.41746(14) 0.041(2) Uiso 1 1 d . A . C1H C 0.8300(7) 0.6477(5) 0.4434(2) 0.052(4) Uiso 1 1 d D . . C2H C 0.9126(7) 0.6501(5) 0.4590(2) 0.048(3) Uiso 1 1 d D . . C3H C 0.9245(7) 0.7030(5) 0.4743(2) 0.049(4) Uiso 1 1 d D . . C4H C 0.8635(7) 0.7491(5) 0.4763(2) 0.044(3) Uiso 1 1 d D . . C5H C 0.7792(7) 0.7458(5) 0.4619(2) 0.042(3) Uiso 1 1 d D . . C6H C 0.9755(7) 0.6054(6) 0.4559(2) 0.062(4) Uiso 1 1 d D . . H6H H 0.9666 0.5719 0.4443 0.074 Uiso 1 1 calc R . . C7H C 1.0575(9) 0.6099(6) 0.4710(3) 0.081(5) Uiso 1 1 d D . . H7H H 1.1021 0.5787 0.4700 0.097 Uiso 1 1 calc R . . C8H C 1.0664(9) 0.6591(6) 0.4859(3) 0.075(5) Uiso 1 1 d D . . H8H H 1.1197 0.6613 0.4954 0.090 Uiso 1 1 calc R . . C9H C 1.0094(8) 0.7065(6) 0.4893(3) 0.072(5) Uiso 1 1 d D . . C10H C 1.0148(9) 0.7578(6) 0.5047(3) 0.074(5) Uiso 1 1 d D . . H10H H 1.0661 0.7614 0.5151 0.089 Uiso 1 1 calc R . . C11H C 0.9569(8) 0.8018(6) 0.5064(2) 0.066(4) Uiso 1 1 d D . . H11H H 0.9685 0.8366 0.5171 0.079 Uiso 1 1 calc R . . C12H C 0.8766(8) 0.7991(5) 0.4927(2) 0.051(4) Uiso 1 1 d D . . H12H H 0.8328 0.8305 0.4947 0.061 Uiso 1 1 calc R . . C13H C 0.6944(8) 0.6935(6) 0.4265(2) 0.052(4) Uiso 1 1 d D A . H13H H 0.6527 0.7274 0.4318 0.062 Uiso 1 1 calc R . . N1H N 0.7712(6) 0.6963(4) 0.44447(17) 0.043(3) Uiso 1 1 d D . . O1H O 0.8153(5) 0.6032(4) 0.42897(15) 0.051(2) Uiso 1 1 d D . . O2H O 0.7182(6) 0.7830(4) 0.46331(17) 0.066(3) Uiso 1 1 d D . . C14H C 0.7231(10) 0.7083(7) 0.3985(3) 0.065(4) Uiso 1 1 d . . . H14M H 0.7745 0.6821 0.3938 0.078 Uiso 1 1 calc R . . H14N H 0.6740 0.6986 0.3867 0.078 Uiso 1 1 calc R . . C15H C 0.7468(13) 0.7740(10) 0.3963(3) 0.100(6) Uiso 1 1 d . . . C16H C 0.6431(8) 0.6304(6) 0.4295(2) 0.043(3) Uiso 1 1 d . . . N2H N 0.8320(10) 0.7881(7) 0.3903(3) 0.104(5) Uiso 1 1 d . . . H2H1 H 0.8495 0.8272 0.3900 0.124 Uiso 1 1 calc R . . H2H2 H 0.8697 0.7581 0.3867 0.124 Uiso 1 1 calc R . . O3H O 0.6943(8) 0.8193(6) 0.4014(2) 0.101(4) Uiso 1 1 d . . . O4H O 0.6216(5) 0.6195(4) 0.45234(15) 0.040(2) Uiso 1 1 d . A . O5H O 0.6294(4) 0.6009(3) 0.40981(14) 0.0330(19) Uiso 1 1 d . A . N3I N 0.9749(11) 0.4176(11) 0.26561(19) 0.056(2) Uiso 0.50 1 d PGD B 1 C21I C 0.9028(9) 0.4229(11) 0.2493(3) 0.056(2) Uiso 0.50 1 d PG B 1 H21I H 0.8445 0.4238 0.2560 0.067 Uiso 0.50 1 calc PR B 1 C22I C 0.9161(10) 0.4269(10) 0.2231(3) 0.056(2) Uiso 0.50 1 d PG B 1 H22I H 0.8668 0.4305 0.2119 0.067 Uiso 0.50 1 calc PR B 1 C23I C 1.0014(12) 0.4255(9) 0.21319(19) 0.056(2) Uiso 0.50 1 d PG B 1 H23I H 1.0105 0.4283 0.1953 0.067 Uiso 0.50 1 calc PR B 1 C24I C 1.0736(9) 0.4203(10) 0.2295(3) 0.056(2) Uiso 0.50 1 d PG B 1 H24I H 1.1319 0.4194 0.2228 0.067 Uiso 0.50 1 calc PR B 1 C25I C 1.0603(9) 0.4163(11) 0.2557(3) 0.056(2) Uiso 0.50 1 d PG B 1 H25I H 1.1096 0.4127 0.2669 0.067 Uiso 0.50 1 calc PR B 1 N3J N 1.0046(11) 0.4177(11) 0.2671(2) 0.056(2) Uiso 0.50 1 d PGD B 2 C21J C 0.9400(8) 0.4250(11) 0.2485(3) 0.056(2) Uiso 0.50 1 d PG B 2 H21J H 0.8791 0.4242 0.2531 0.067 Uiso 0.50 1 calc PR B 2 C22J C 0.9643(10) 0.4335(10) 0.2231(3) 0.056(2) Uiso 0.50 1 d PG B 2 H22J H 0.9202 0.4385 0.2104 0.067 Uiso 0.50 1 calc PR B 2 C23J C 1.0533(12) 0.4347(9) 0.2164(2) 0.056(2) Uiso 0.50 1 d PG B 2 H23J H 1.0700 0.4405 0.1991 0.067 Uiso 0.50 1 calc PR B 2 C24J C 1.1180(8) 0.4274(10) 0.2351(3) 0.056(2) Uiso 0.50 1 d PG B 2 H24J H 1.1788 0.4282 0.2305 0.067 Uiso 0.50 1 calc PR B 2 C25J C 1.0936(10) 0.4189(11) 0.2604(3) 0.056(2) Uiso 0.50 1 d PG B 2 H25J H 1.1378 0.4139 0.2732 0.067 Uiso 0.50 1 calc PR B 2 O36 O 0.5122(6) 0.5484(5) 0.50055(17) 0.069(3) Uiso 1 1 d D . . O37 O 0.4011(8) 0.4844(6) 0.5144(3) 0.148(5) Uiso 1 1 d D . . O38 O 0.6373(8) 0.4761(6) 0.5217(2) 0.126(5) Uiso 1 1 d D A . C31 C 0.4898(12) 0.5004(9) 0.5124(4) 0.120(7) Uiso 1 1 d D A . C32 C 0.3246(11) 0.5271(9) 0.5014(4) 0.132(8) Uiso 1 1 d D A . H32A H 0.3416 0.5717 0.5016 0.158 Uiso 1 1 calc R . . H32B H 0.3136 0.5141 0.4835 0.158 Uiso 1 1 calc R . . C33 C 0.2489(12) 0.5167(10) 0.5168(4) 0.154(9) Uiso 1 1 d D . . H33A H 0.2043 0.4938 0.5069 0.231 Uiso 1 1 calc R A . H33B H 0.2243 0.5568 0.5223 0.231 Uiso 1 1 calc R . . H33C H 0.2656 0.4922 0.5318 0.231 Uiso 1 1 calc R . . C34 C 0.5499(10) 0.4517(7) 0.5213(3) 0.095(5) Uiso 1 1 d D . . H34 H 0.5481 0.4166 0.5087 0.114 Uiso 1 1 calc R A . C35 C 0.5233(11) 0.4268(8) 0.5469(3) 0.118(7) Uiso 1 1 d D A . H35A H 0.5556 0.3880 0.5503 0.176 Uiso 1 1 calc R . . H35B H 0.4595 0.4184 0.5470 0.176 Uiso 1 1 calc R . . H35C H 0.5374 0.4575 0.5601 0.176 Uiso 1 1 calc R . . O46 O 0.6823(10) 0.7066(8) 0.6073(3) 0.166(6) Uiso 1 1 d D . . O47 O 0.5571(10) 0.6491(7) 0.6028(3) 0.165(6) Uiso 1 1 d D . . O48 O 0.6761(10) 0.6975(8) 0.6584(3) 0.182(7) Uiso 1 1 d D . . C41 C 0.6186(15) 0.6795(13) 0.6182(4) 0.207(13) Uiso 1 1 d D . . C42 C 0.5504(16) 0.6654(10) 0.5725(3) 0.166(9) Uiso 1 1 d D . . H42A H 0.5289 0.7085 0.5697 0.199 Uiso 1 1 calc R . . H42B H 0.6082 0.6601 0.5639 0.199 Uiso 1 1 calc R . . C43 C 0.4884(15) 0.6210(11) 0.5641(4) 0.176(10) Uiso 1 1 d D . . H43A H 0.5065 0.5795 0.5698 0.264 Uiso 1 1 calc R . . H43B H 0.4855 0.6218 0.5454 0.264 Uiso 1 1 calc R . . H43C H 0.4300 0.6310 0.5711 0.264 Uiso 1 1 calc R . . C44 C 0.6141(12) 0.6603(9) 0.6454(3) 0.140(8) Uiso 1 1 d D . . H44 H 0.6307 0.6154 0.6470 0.168 Uiso 1 1 calc R . . C45 C 0.5224(12) 0.6700(11) 0.6553(4) 0.183(11) Uiso 1 1 d D . . H45A H 0.5154 0.6478 0.6715 0.274 Uiso 1 1 calc R . . H45B H 0.4796 0.6538 0.6428 0.274 Uiso 1 1 calc R . . H45C H 0.5120 0.7146 0.6579 0.274 Uiso 1 1 calc R . . O56 O 0.7690(13) 0.5810(9) 0.6327(3) 0.230(3) Uiso 1 1 d D . . O57 O 0.8194(13) 0.5889(8) 0.5927(3) 0.230(3) Uiso 1 1 d D . . O58 O 0.8407(12) 0.6963(9) 0.6434(4) 0.230(3) Uiso 1 1 d D . . C51 C 0.8286(17) 0.6032(12) 0.6186(4) 0.230(3) Uiso 1 1 d D . . C52 C 0.7350(15) 0.5507(12) 0.5805(5) 0.230(3) Uiso 1 1 d D . . H52A H 0.6797 0.5574 0.5903 0.276 Uiso 1 1 calc R . . H52B H 0.7253 0.5606 0.5623 0.276 Uiso 1 1 calc R . . C53 C 0.7707(18) 0.4903(10) 0.5842(5) 0.230(3) Uiso 1 1 d D . . H53A H 0.8349 0.4933 0.5865 0.345 Uiso 1 1 calc R . . H53B H 0.7577 0.4644 0.5692 0.345 Uiso 1 1 calc R . . H53C H 0.7441 0.4713 0.5994 0.345 Uiso 1 1 calc R . . C54 C 0.8773(15) 0.6616(10) 0.6230(5) 0.230(3) Uiso 1 1 d D . . H54 H 0.8700 0.6874 0.6072 0.276 Uiso 1 1 calc R . . C55 C 0.9749(14) 0.6485(12) 0.6257(5) 0.230(3) Uiso 1 1 d D . . H55A H 1.0031 0.6826 0.6351 0.345 Uiso 1 1 calc R . . H55B H 1.0018 0.6450 0.6087 0.345 Uiso 1 1 calc R . . H55C H 0.9833 0.6093 0.6350 0.345 Uiso 1 1 calc R . . O66 O 0.5212(12) 0.7884(9) 0.3140(4) 0.230(3) Uiso 1 1 d D . . O67 O 0.6426(12) 0.7645(8) 0.3371(4) 0.230(3) Uiso 1 1 d D . . O68 O 0.4205(12) 0.7029(9) 0.3362(4) 0.230(3) Uiso 1 1 d D . . C61 C 0.5591(16) 0.7507(11) 0.3285(5) 0.230(3) Uiso 1 1 d D . . C62 C 0.7151(15) 0.8159(12) 0.3274(6) 0.230(3) Uiso 1 1 d D . . H62A H 0.7745 0.8082 0.3347 0.276 Uiso 1 1 calc R . . H62B H 0.7189 0.8177 0.3086 0.276 Uiso 1 1 calc R . . C63 C 0.6751(19) 0.8699(10) 0.3378(6) 0.230(3) Uiso 1 1 d D . . H63A H 0.6106 0.8650 0.3376 0.345 Uiso 1 1 calc R . . H63B H 0.6916 0.9063 0.3276 0.345 Uiso 1 1 calc R . . H63C H 0.6954 0.8757 0.3554 0.345 Uiso 1 1 calc R . . C64 C 0.5128(15) 0.6994(10) 0.3412(5) 0.230(3) Uiso 1 1 d D . . H64 H 0.5226 0.7028 0.3601 0.276 Uiso 1 1 calc R . . C65 C 0.5509(16) 0.6387(10) 0.3320(5) 0.230(3) Uiso 1 1 d D . . H65A H 0.5190 0.6040 0.3399 0.345 Uiso 1 1 calc R . . H65B H 0.6137 0.6365 0.3366 0.345 Uiso 1 1 calc R . . H65C H 0.5449 0.6362 0.3134 0.345 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0346(9) 0.0552(11) 0.0341(9) -0.0045(8) -0.0005(7) 0.0051(9) Cu2 0.0373(9) 0.0562(10) 0.0311(8) -0.0052(8) -0.0019(7) 0.0108(9) Cu3 0.0304(9) 0.0500(10) 0.0303(8) -0.0011(8) 0.0015(7) 0.0012(8) Cu4 0.0272(8) 0.0482(9) 0.0294(8) 0.0016(7) -0.0005(7) -0.0011(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O4C 1.910(8) . ? Cu1 O4A 1.918(8) . ? Cu1 O4B 2.008(8) . ? Cu1 O4D 2.071(8) . ? Cu1 N3I 2.143(10) . ? Cu1 N3J 2.152(10) . ? Cu1 Cu2 2.712(2) . ? Cu2 O5D 1.908(9) . ? Cu2 O5B 1.910(8) . ? Cu2 O5C 2.013(8) . ? Cu2 O5A 2.034(8) . ? Cu2 O3E 2.129(10) . ? Cu3 O4G 1.939(7) . ? Cu3 O4E 1.962(8) . ? Cu3 O4H 1.967(8) . ? Cu3 O4F 1.982(8) . ? Cu3 O36 2.246(9) . ? Cu3 Cu4 2.6088(19) . ? Cu4 O5F 1.935(8) . ? Cu4 O5H 1.967(7) . ? Cu4 O5G 2.016(8) . ? Cu4 O5E 2.018(8) . ? Cu4 O3Z 2.113(9) . ? Cu4 O3A 2.125(9) . ? C1G O1G 1.235(10) . ? C1G N1G 1.366(10) . ? C1G C2G 1.490(11) . ? C2G C6G 1.366(11) . ? C2G C3G 1.390(11) . ? C3G C4G 1.351(11) . ? C3G C9G 1.513(12) . ? C4G C12G 1.400(12) . ? C4G C5G 1.477(11) . ? C5G O2G 1.207(10) . ? C5G N1G 1.387(11) . ? C6G C7G 1.453(12) . ? C6G H6G 0.9500 . ? C7G C8G 1.312(12) . ? C7G H7G 0.9500 . ? C8G C9G 1.356(12) . ? C8G H8G 0.9500 . ? C9G C10G 1.356(12) . ? C10G C11G 1.307(12) . ? C10G H10G 0.9500 . ? C11G C12G 1.412(12) . ? C11G H11G 0.9500 . ? C12G H12G 0.9500 . ? C13G C16G 1.472(15) . ? C13G N1G 1.520(10) . ? C13G C14G 1.530(16) . ? C13G H13G 1.0000 . ? C14G C15G 1.494(18) . ? C14G H14O 0.9900 . ? C14G H14P 0.9900 . ? C15G O3G 1.262(15) . ? C15G N2G 1.318(16) . ? C16G O5G 1.242(12) . ? C16G O4G 1.254(12) . ? N2G H2G1 0.8800 . ? N2G H2G2 0.8800 . ? C1A O1A 1.222(11) . ? C1A N1A 1.380(12) . ? C1A C2A 1.505(12) . ? C2A C3A 1.383(12) . ? C2A C6A 1.385(12) . ? C3A C4A 1.343(12) . ? C3A C9A 1.542(13) . ? C4A C12A 1.389(12) . ? C4A C5A 1.505(12) . ? C5A O2A 1.231(12) . ? C5A N1A 1.415(12) . ? C6A C7A 1.471(13) . ? C6A H6A 0.9500 . ? C7A C8A 1.292(13) . ? C7A H7A 0.9500 . ? C8A C9A 1.329(12) . ? C8A H8A 0.9500 . ? C9A C10A 1.286(12) . ? C10A C11A 1.293(12) . ? C10A H10A 0.9500 . ? C11A C12A 1.391(13) . ? C11A H11A 0.9500 . ? C12A H12A 0.9500 . ? C16A O4A 1.264(13) . ? C16A O5A 1.303(12) . ? C16A C13A 1.442(15) . ? N1A C13A 1.445(15) . ? C13A C14A 1.546(13) . ? C13A H13A 1.0000 . ? C14A C15A 1.523(13) . ? C14A H14A 0.9900 . ? C14A H14B 0.9900 . ? C15A O3A 1.259(9) . ? C15A N2A 1.370(9) . ? N2A H2A1 0.8800 . ? N2A H2A2 0.8800 . ? C14Z C15Z 1.500(13) . ? C14Z H14Z 0.9900 . ? C14Z H14Y 0.9900 . ? C15Z O3Z 1.226(9) . ? C15Z N2Z 1.330(9) . ? N2Z H2Z1 0.8800 . ? N2Z H2Z2 0.8800 . ? C1B O1B 1.212(11) . ? C1B N1B 1.368(11) . ? C1B C2B 1.517(12) . ? C2B C6B 1.348(12) . ? C2B C3B 1.367(11) . ? C3B C4B 1.331(12) . ? C3B C9B 1.529(12) . ? C4B C12B 1.351(12) . ? C4B C5B 1.533(12) . ? C5B O2B 1.199(11) . ? C5B N1B 1.396(11) . ? C6B C7B 1.489(12) . ? C6B H6B 0.9500 . ? C7B C8B 1.284(12) . ? C7B H7B 0.9500 . ? C8B C9B 1.313(12) . ? C8B H8B 0.9500 . ? C9B C10B 1.329(12) . ? C10B C11B 1.267(12) . ? C10B H10B 0.9500 . ? C11B C12B 1.425(12) . ? C11B H11B 0.9500 . ? C12B H12B 0.9500 . ? C13B N1B 1.492(12) . ? C13B C16B 1.492(18) . ? C13B C14B 1.503(18) . ? C13B H13B 1.0000 . ? C14B C15B 1.604(18) . ? C14B H14C 0.9900 . ? C14B H14D 0.9900 . ? C15B O3B 1.238(15) . ? C15B N2B 1.253(16) . ? C16B O5B 1.256(13) . ? C16B O4B 1.265(13) . ? N2B H2B1 0.8800 . ? N2B H2B2 0.8800 . ? C1C O1C 1.217(11) . ? C1C N1C 1.361(12) . ? C1C C2C 1.529(12) . ? C2C C6C 1.350(12) . ? C2C C3C 1.389(12) . ? C3C C4C 1.343(12) . ? C3C C9C 1.548(13) . ? C4C C12C 1.391(13) . ? C4C C5C 1.496(12) . ? C5C O2C 1.182(11) . ? C5C N1C 1.435(12) . ? C6C C7C 1.500(13) . ? C6C H6C 0.9500 . ? C7C C8C 1.309(13) . ? C7C H7C 0.9500 . ? C8C C9C 1.325(12) . ? C8C H8C 0.9500 . ? C9C C10C 1.327(12) . ? C10C C11C 1.274(12) . ? C10C H10C 0.9500 . ? C11C C12C 1.437(13) . ? C11C H11C 0.9500 . ? C12C H12C 0.9500 . ? C13C N1C 1.478(12) . ? C13C C16C 1.530(19) . ? C13C C14C 1.549(19) . ? C13C H13C 1.0000 . ? C14C C15C 1.548(18) . ? C14C H14E 0.9900 . ? C14C H14F 0.9900 . ? C15C O3C 1.189(15) . ? C15C N2C 1.296(16) . ? C16C O4C 1.225(13) . ? C16C O5C 1.279(13) . ? N2C H2C1 0.8800 . ? N2C H2C2 0.8800 . ? C1D O1D 1.221(10) . ? C1D N1D 1.383(11) . ? C1D C2D 1.483(11) . ? C2D C3D 1.372(11) . ? C2D C6D 1.372(12) . ? C3D C4D 1.347(11) . ? C3D C9D 1.497(12) . ? C4D C12D 1.374(12) . ? C4D C5D 1.488(12) . ? C5D O2D 1.226(12) . ? C5D N1D 1.393(12) . ? C6D C7D 1.462(13) . ? C6D H6D 0.9500 . ? C7D C8D 1.301(13) . ? C7D H7D 0.9500 . ? C8D C9D 1.355(12) . ? C8D H8D 0.9500 . ? C9D C10D 1.362(12) . ? C10D C11D 1.296(12) . ? C10D H10D 0.9500 . ? C11D C12D 1.424(13) . ? C11D H11D 0.9500 . ? C12D H12D 0.9500 . ? C13D N1D 1.446(11) . ? C13D C16D 1.500(17) . ? C13D C14D 1.619(19) . ? C13D H13D 1.0000 . ? C14D C15D 1.48(2) . ? C14D H14G 0.9900 . ? C14D H14H 0.9900 . ? C15D O3D 1.16(2) . ? C15D N2D 1.40(2) . ? C16D O4D 1.241(13) . ? C16D O5D 1.244(13) . ? N2D H2D1 0.8800 . ? N2D H2D2 0.8800 . ? C1E O1E 1.235(10) . ? C1E N1E 1.361(10) . ? C1E C2E 1.505(11) . ? C2E C6E 1.347(12) . ? C2E C3E 1.390(11) . ? C3E C4E 1.337(11) . ? C3E C9E 1.527(12) . ? C4E C12E 1.377(12) . ? C4E C5E 1.466(11) . ? C5E O2E 1.213(10) . ? C5E N1E 1.430(10) . ? C6E C7E 1.486(13) . ? C6E H6E 0.9500 . ? C7E C8E 1.285(13) . ? C7E H7E 0.9500 . ? C8E C9E 1.329(12) . ? C8E H8E 0.9500 . ? C9E C10E 1.350(13) . ? C10E C11E 1.293(13) . ? C10E H10E 0.9500 . ? C11E C12E 1.414(12) . ? C11E H11E 0.9500 . ? C12E H12E 0.9500 . ? C13E N1E 1.464(10) . ? C13E C16E 1.493(15) . ? C13E C14E 1.533(17) . ? C13E H13E 1.0000 . ? C14E C15E 1.55(2) . ? C14E H14I 0.9900 . ? C14E H14J 0.9900 . ? C15E O3E 1.07(2) . ? C15E N2E 1.33(2) . ? C16E O4E 1.226(12) . ? C16E O5E 1.286(12) . ? N2E H2E1 0.8800 . ? N2E H2E2 0.8800 . ? C1F O1F 1.220(11) . ? C1F N1F 1.367(11) . ? C1F C2F 1.512(12) . ? C2F C3F 1.367(12) . ? C2F C6F 1.370(12) . ? C3F C4F 1.332(12) . ? C3F C9F 1.539(12) . ? C4F C12F 1.379(12) . ? C4F C5F 1.499(12) . ? C5F O2F 1.214(11) . ? C5F N1F 1.408(11) . ? C6F C7F 1.495(12) . ? C6F H6F 0.9500 . ? C7F C8F 1.291(12) . ? C7F H7F 0.9500 . ? C8F C9F 1.317(12) . ? C8F H8F 0.9500 . ? C9F C10F 1.334(12) . ? C10F C11F 1.276(12) . ? C10F H10F 0.9500 . ? C11F C12F 1.428(12) . ? C11F H11F 0.9500 . ? C12F H12F 0.9500 . ? C13F N1F 1.465(11) . ? C13F C16F 1.516(18) . ? C13F C14F 1.523(17) . ? C13F H13F 1.0000 . ? C14F C15F 1.519(17) . ? C14F H14K 0.9900 . ? C14F H14L 0.9900 . ? C15F O3F 1.238(14) . ? C15F N2F 1.335(15) . ? C16F O4F 1.205(12) . ? C16F O5F 1.304(12) . ? N2F H2F1 0.8800 . ? N2F H2F2 0.8800 . ? C1H O1H 1.237(10) . ? C1H N1H 1.370(10) . ? C1H C2H 1.492(11) . ? C2H C6H 1.360(11) . ? C2H C3H 1.400(11) . ? C3H C4H 1.356(11) . ? C3H C9H 1.507(12) . ? C4H C12H 1.388(11) . ? C4H C5H 1.485(11) . ? C5H O2H 1.221(10) . ? C5H N1H 1.405(10) . ? C6H C7H 1.473(12) . ? C6H H6H 0.9500 . ? C7H C8H 1.321(12) . ? C7H H7H 0.9500 . ? C8H C9H 1.343(12) . ? C8H H8H 0.9500 . ? C9H C10H 1.366(12) . ? C10H C11H 1.290(12) . ? C10H H10H 0.9500 . ? C11H C12H 1.411(12) . ? C11H H11H 0.9500 . ? C12H H12H 0.9500 . ? C13H N1H 1.495(11) . ? C13H C14H 1.559(17) . ? C13H C16H 1.568(17) . ? C13H H13H 1.0000 . ? C14H C15H 1.46(2) . ? C14H H14M 0.9900 . ? C14H H14N 0.9900 . ? C15H O3H 1.28(2) . ? C15H N2H 1.36(2) . ? C16H O5H 1.229(13) . ? C16H O4H 1.261(13) . ? N2H H2H1 0.8800 . ? N2H H2H2 0.8800 . ? N3I C21I 1.3900 . ? N3I C25I 1.3900 . ? C21I C22I 1.3900 . ? C21I H21I 0.9500 . ? C22I C23I 1.3900 . ? C22I H22I 0.9500 . ? C23I C24I 1.3900 . ? C23I H23I 0.9500 . ? C24I C25I 1.3900 . ? C24I H24I 0.9500 . ? C25I H25I 0.9500 . ? N3J C21J 1.3900 . ? N3J C25J 1.3900 . ? C21J C22J 1.3900 . ? C21J H21J 0.9500 . ? C22J C23J 1.3900 . ? C22J H22J 0.9500 . ? C23J C24J 1.3900 . ? C23J H23J 0.9500 . ? C24J C25J 1.3900 . ? C24J H24J 0.9500 . ? C25J H25J 0.9500 . ? O36 C31 1.249(16) . ? O37 C31 1.387(16) . ? O37 C32 1.624(15) . ? O38 C34 1.420(14) . ? C31 C34 1.459(17) . ? C32 C33 1.419(16) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.498(15) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? O46 C41 1.261(17) . ? O47 C41 1.389(17) . ? O47 C42 1.631(15) . ? O48 C44 1.406(15) . ? C41 C44 1.486(18) . ? C42 C43 1.407(16) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.493(16) . ? C44 H44 1.0000 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? O56 C51 1.258(18) . ? O57 C51 1.399(17) . ? O57 C52 1.644(16) . ? O58 C54 1.417(16) . ? C51 C54 1.470(18) . ? C52 C53 1.418(17) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 C55 1.509(17) . ? C54 H54 1.0000 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? O66 C61 1.247(17) . ? O67 C61 1.372(17) . ? O67 C62 1.633(16) . ? O68 C64 1.421(16) . ? C61 C64 1.466(18) . ? C62 C63 1.415(17) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 C65 1.503(17) . ? C64 H64 1.0000 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4C Cu1 O4A 174.7(3) . . ? O4C Cu1 O4B 90.6(3) . . ? O4A Cu1 O4B 91.4(3) . . ? O4C Cu1 O4D 89.8(3) . . ? O4A Cu1 O4D 86.4(3) . . ? O4B Cu1 O4D 157.2(3) . . ? O4C Cu1 N3I 97.5(5) . . ? O4A Cu1 N3I 87.2(6) . . ? O4B Cu1 N3I 94.8(7) . . ? O4D Cu1 N3I 107.7(7) . . ? O4C Cu1 N3J 86.0(5) . . ? O4A Cu1 N3J 98.5(5) . . ? O4B Cu1 N3J 99.2(7) . . ? O4D Cu1 N3J 103.6(7) . . ? N3I Cu1 N3J 12.2(7) . . ? O4C Cu1 Cu2 86.3(2) . . ? O4A Cu1 Cu2 89.3(3) . . ? O4B Cu1 Cu2 79.2(2) . . ? O4D Cu1 Cu2 78.0(2) . . ? N3I Cu1 Cu2 173.0(5) . . ? N3J Cu1 Cu2 172.2(5) . . ? O5D Cu2 O5B 175.7(3) . . ? O5D Cu2 O5C 86.5(3) . . ? O5B Cu2 O5C 93.4(3) . . ? O5D Cu2 O5A 89.8(3) . . ? O5B Cu2 O5A 88.6(3) . . ? O5C Cu2 O5A 156.5(3) . . ? O5D Cu2 O3E 93.9(4) . . ? O5B Cu2 O3E 90.3(3) . . ? O5C Cu2 O3E 104.4(3) . . ? O5A Cu2 O3E 99.0(3) . . ? O5D Cu2 Cu1 88.1(3) . . ? O5B Cu2 Cu1 87.7(2) . . ? O5C Cu2 Cu1 79.3(2) . . ? O5A Cu2 Cu1 77.3(2) . . ? O3E Cu2 Cu1 175.8(3) . . ? O4G Cu3 O4E 173.8(3) . . ? O4G Cu3 O4H 89.6(3) . . ? O4E Cu3 O4H 85.8(3) . . ? O4G Cu3 O4F 94.5(3) . . ? O4E Cu3 O4F 89.0(3) . . ? O4H Cu3 O4F 164.8(3) . . ? O4G Cu3 O36 93.9(3) . . ? O4E Cu3 O36 91.4(3) . . ? O4H Cu3 O36 106.6(3) . . ? O4F Cu3 O36 87.8(3) . . ? O4G Cu3 Cu4 84.1(2) . . ? O4E Cu3 Cu4 91.4(2) . . ? O4H Cu3 Cu4 86.0(2) . . ? O4F Cu3 Cu4 79.9(2) . . ? O36 Cu3 Cu4 167.3(3) . . ? O5F Cu4 O5H 171.2(3) . . ? O5F Cu4 O5G 94.8(3) . . ? O5H Cu4 O5G 87.6(3) . . ? O5F Cu4 O5E 84.8(3) . . ? O5H Cu4 O5E 90.4(3) . . ? O5G Cu4 O5E 162.9(3) . . ? O5F Cu4 O3Z 86.1(5) . . ? O5H Cu4 O3Z 102.3(5) . . ? O5G Cu4 O3Z 90.1(5) . . ? O5E Cu4 O3Z 106.8(5) . . ? O5F Cu4 O3A 92.3(5) . . ? O5H Cu4 O3A 95.3(5) . . ? O5G Cu4 O3A 102.4(5) . . ? O5E Cu4 O3A 94.7(5) . . ? O3Z Cu4 O3A 14.3(6) . . ? O5F Cu4 Cu3 88.1(2) . . ? O5H Cu4 Cu3 83.8(2) . . ? O5G Cu4 Cu3 84.6(2) . . ? O5E Cu4 Cu3 78.3(2) . . ? O3Z Cu4 Cu3 171.8(4) . . ? O3A Cu4 Cu3 172.9(4) . . ? O1G C1G N1G 121.2(9) . . ? O1G C1G C2G 120.0(9) . . ? N1G C1G C2G 118.7(9) . . ? C6G C2G C3G 123.4(10) . . ? C6G C2G C1G 120.3(9) . . ? C3G C2G C1G 116.3(9) . . ? C4G C3G C2G 124.5(9) . . ? C4G C3G C9G 117.5(9) . . ? C2G C3G C9G 118.0(9) . . ? C3G C4G C12G 124.1(10) . . ? C3G C4G C5G 119.3(9) . . ? C12G C4G C5G 116.4(10) . . ? O2G C5G N1G 117.1(10) . . ? O2G C5G C4G 126.0(10) . . ? N1G C5G C4G 116.8(9) . . ? C2G C6G C7G 117.3(10) . . ? C2G C6G H6G 121.3 . . ? C7G C6G H6G 121.3 . . ? C8G C7G C6G 119.2(12) . . ? C8G C7G H7G 120.4 . . ? C6G C7G H7G 120.4 . . ? C7G C8G C9G 127.9(13) . . ? C7G C8G H8G 116.1 . . ? C9G C8G H8G 116.1 . . ? C10G C9G C8G 132.6(12) . . ? C10G C9G C3G 113.2(10) . . ? C8G C9G C3G 114.1(10) . . ? C11G C10G C9G 129.6(13) . . ? C11G C10G H10G 115.2 . . ? C9G C10G H10G 115.2 . . ? C10G C11G C12G 118.0(12) . . ? C10G C11G H11G 121.0 . . ? C12G C11G H11G 121.0 . . ? C4G C12G C11G 117.4(11) . . ? C4G C12G H12G 121.3 . . ? C11G C12G H12G 121.3 . . ? C16G C13G N1G 114.0(9) . . ? C16G C13G C14G 118.5(10) . . ? N1G C13G C14G 106.1(9) . . ? C16G C13G H13G 105.8 . . ? N1G C13G H13G 105.8 . . ? C14G C13G H13G 105.8 . . ? C1G N1G C5G 124.0(9) . . ? C1G N1G C13G 116.2(8) . . ? C5G N1G C13G 119.5(9) . . ? C15G C14G C13G 111.5(11) . . ? C15G C14G H14O 109.3 . . ? C13G C14G H14O 109.3 . . ? C15G C14G H14P 109.3 . . ? C13G C14G H14P 109.3 . . ? H14O C14G H14P 108.0 . . ? O3G C15G N2G 119.9(14) . . ? O3G C15G C14G 123.1(13) . . ? N2G C15G C14G 116.9(14) . . ? O5G C16G O4G 125.8(11) . . ? O5G C16G C13G 116.7(10) . . ? O4G C16G C13G 117.6(11) . . ? C15G N2G H2G1 120.0 . . ? C15G N2G H2G2 120.0 . . ? H2G1 N2G H2G2 120.0 . . ? C16G O4G Cu3 124.6(8) . . ? C16G O5G Cu4 119.9(7) . . ? O1A C1A N1A 121.0(12) . . ? O1A C1A C2A 117.7(12) . . ? N1A C1A C2A 121.2(11) . . ? C3A C2A C6A 127.4(12) . . ? C3A C2A C1A 116.4(11) . . ? C6A C2A C1A 116.1(11) . . ? C4A C3A C2A 124.7(12) . . ? C4A C3A C9A 121.8(11) . . ? C2A C3A C9A 113.5(11) . . ? C3A C4A C12A 123.6(12) . . ? C3A C4A C5A 119.1(11) . . ? C12A C4A C5A 117.2(11) . . ? O2A C5A N1A 116.4(12) . . ? O2A C5A C4A 125.0(12) . . ? N1A C5A C4A 118.6(11) . . ? C2A C6A C7A 115.6(12) . . ? C2A C6A H6A 122.2 . . ? C7A C6A H6A 122.2 . . ? C8A C7A C6A 115.9(14) . . ? C8A C7A H7A 122.0 . . ? C6A C7A H7A 122.0 . . ? C7A C8A C9A 132.1(15) . . ? C7A C8A H8A 114.0 . . ? C9A C8A H8A 114.0 . . ? C10A C9A C8A 140.0(15) . . ? C10A C9A C3A 105.3(12) . . ? C8A C9A C3A 114.3(12) . . ? C9A C10A C11A 135.5(15) . . ? C9A C10A H10A 112.2 . . ? C11A C10A H10A 112.2 . . ? C10A C11A C12A 120.3(14) . . ? C10A C11A H11A 119.9 . . ? C12A C11A H11A 119.9 . . ? C4A C12A C11A 113.1(12) . . ? C4A C12A H12A 123.5 . . ? C11A C12A H12A 123.5 . . ? O4A C16A O5A 121.8(11) . . ? O4A C16A C13A 120.1(11) . . ? O5A C16A C13A 117.7(11) . . ? C1A N1A C5A 119.9(11) . . ? C1A N1A C13A 114.8(11) . . ? C5A N1A C13A 124.4(11) . . ? C16A O4A Cu1 121.3(8) . . ? C16A O5A Cu2 129.0(8) . . ? C16A C13A N1A 108.2(10) . . ? C16A C13A C14A 110.6(13) . . ? N1A C13A C14A 107.8(11) . . ? C16A C13A H13A 110.1 . . ? N1A C13A H13A 110.1 . . ? C14A C13A H13A 110.1 . . ? C15A C14A C13A 123.0(15) . . ? C15A C14A H14A 106.6 . . ? C13A C14A H14A 106.6 . . ? C15A C14A H14B 106.6 . . ? C13A C14A H14B 106.6 . . ? H14A C14A H14B 106.6 . . ? O3A C15A N2A 118.2(15) . . ? O3A C15A C14A 120.8(15) . . ? N2A C15A C14A 120.2(16) . . ? C15A N2A H2A1 120.0 . . ? C15A N2A H2A2 120.0 . . ? H2A1 N2A H2A2 120.0 . . ? C15A O3A Cu4 134.3(12) . . ? C15Z C14Z H14Z 106.2 . . ? C15Z C14Z H14Y 106.2 . . ? H14Z C14Z H14Y 106.4 . . ? O3Z C15Z N2Z 135.5(16) . . ? O3Z C15Z C14Z 108.2(12) . . ? N2Z C15Z C14Z 115.2(15) . . ? C15Z N2Z H2Z1 120.0 . . ? C15Z N2Z H2Z2 120.0 . . ? H2Z1 N2Z H2Z2 120.0 . . ? C15Z O3Z Cu4 116.8(11) . . ? O1B C1B N1B 122.1(11) . . ? O1B C1B C2B 119.4(11) . . ? N1B C1B C2B 118.4(10) . . ? C6B C2B C3B 124.6(11) . . ? C6B C2B C1B 118.9(11) . . ? C3B C2B C1B 116.5(10) . . ? C4B C3B C2B 125.2(11) . . ? C4B C3B C9B 117.7(10) . . ? C2B C3B C9B 116.8(10) . . ? C3B C4B C12B 123.2(11) . . ? C3B C4B C5B 120.1(11) . . ? C12B C4B C5B 116.6(11) . . ? O2B C5B N1B 120.0(11) . . ? O2B C5B C4B 124.9(11) . . ? N1B C5B C4B 114.2(10) . . ? C2B C6B C7B 117.7(11) . . ? C2B C6B H6B 121.2 . . ? C7B C6B H6B 121.2 . . ? C8B C7B C6B 115.0(12) . . ? C8B C7B H7B 122.5 . . ? C6B C7B H7B 122.5 . . ? C7B C8B C9B 132.8(14) . . ? C7B C8B H8B 113.6 . . ? C9B C8B H8B 113.6 . . ? C8B C9B C10B 134.5(13) . . ? C8B C9B C3B 113.0(11) . . ? C10B C9B C3B 112.4(11) . . ? C11B C10B C9B 130.5(14) . . ? C11B C10B H10B 114.8 . . ? C9B C10B H10B 114.8 . . ? C10B C11B C12B 117.1(13) . . ? C10B C11B H11B 121.5 . . ? C12B C11B H11B 121.5 . . ? C4B C12B C11B 118.9(12) . . ? C4B C12B H12B 120.5 . . ? C11B C12B H12B 120.5 . . ? N1B C13B C16B 112.3(12) . . ? N1B C13B C14B 106.0(12) . . ? C16B C13B C14B 113.9(12) . . ? N1B C13B H13B 108.1 . . ? C16B C13B H13B 108.1 . . ? C14B C13B H13B 108.1 . . ? C1B N1B C5B 125.1(10) . . ? C1B N1B C13B 116.2(10) . . ? C5B N1B C13B 118.6(10) . . ? C13B C14B C15B 111.2(11) . . ? C13B C14B H14C 109.4 . . ? C15B C14B H14C 109.4 . . ? C13B C14B H14D 109.4 . . ? C15B C14B H14D 109.4 . . ? H14C C14B H14D 108.0 . . ? O3B C15B N2B 123.1(15) . . ? O3B C15B C14B 120.9(14) . . ? N2B C15B C14B 115.3(14) . . ? O5B C16B O4B 127.6(12) . . ? O5B C16B C13B 114.8(11) . . ? O4B C16B C13B 117.5(12) . . ? C15B N2B H2B1 120.0 . . ? C15B N2B H2B2 120.0 . . ? H2B1 N2B H2B2 120.0 . . ? C16B O4B Cu1 125.2(8) . . ? C16B O5B Cu2 120.2(8) . . ? O1C C1C N1C 119.6(12) . . ? O1C C1C C2C 119.6(12) . . ? N1C C1C C2C 120.6(11) . . ? C6C C2C C3C 126.9(12) . . ? C6C C2C C1C 118.2(11) . . ? C3C C2C C1C 114.7(11) . . ? C4C C3C C2C 125.3(12) . . ? C4C C3C C9C 120.1(11) . . ? C2C C3C C9C 114.6(10) . . ? C3C C4C C12C 126.6(12) . . ? C3C C4C C5C 120.8(12) . . ? C12C C4C C5C 112.3(11) . . ? O2C C5C N1C 117.9(12) . . ? O2C C5C C4C 126.6(13) . . ? N1C C5C C4C 115.1(11) . . ? C2C C6C C7C 118.1(12) . . ? C2C C6C H6C 120.9 . . ? C7C C6C H6C 120.9 . . ? C8C C7C C6C 112.0(13) . . ? C8C C7C H7C 124.0 . . ? C6C C7C H7C 124.0 . . ? C7C C8C C9C 136.0(15) . . ? C7C C8C H8C 112.0 . . ? C9C C8C H8C 112.0 . . ? C8C C9C C10C 139.7(14) . . ? C8C C9C C3C 112.2(12) . . ? C10C C9C C3C 108.1(11) . . ? C11C C10C C9C 131.1(15) . . ? C11C C10C H10C 114.4 . . ? C9C C10C H10C 114.4 . . ? C10C C11C C12C 124.1(14) . . ? C10C C11C H11C 117.9 . . ? C12C C11C H11C 117.9 . . ? C4C C12C C11C 109.9(12) . . ? C4C C12C H12C 125.1 . . ? C11C C12C H12C 125.1 . . ? N1C C13C C16C 106.9(13) . . ? N1C C13C C14C 114.4(13) . . ? C16C C13C C14C 109.7(12) . . ? N1C C13C H13C 108.5 . . ? C16C C13C H13C 108.5 . . ? C14C C13C H13C 108.5 . . ? C1C N1C C5C 122.6(11) . . ? C1C N1C C13C 120.1(12) . . ? C5C N1C C13C 117.0(11) . . ? C15C C14C C13C 108.8(12) . . ? C15C C14C H14E 109.9 . . ? C13C C14C H14E 109.9 . . ? C15C C14C H14F 109.9 . . ? C13C C14C H14F 109.9 . . ? H14E C14C H14F 108.3 . . ? O3C C15C N2C 125.0(15) . . ? O3C C15C C14C 119.5(14) . . ? N2C C15C C14C 115.4(14) . . ? O4C C16C O5C 124.8(12) . . ? O4C C16C C13C 120.3(12) . . ? O5C C16C C13C 114.6(11) . . ? C15C N2C H2C1 120.0 . . ? C15C N2C H2C2 120.0 . . ? H2C1 N2C H2C2 120.0 . . ? C16C O4C Cu1 123.0(8) . . ? C16C O5C Cu2 125.2(8) . . ? O1D C1D N1D 118.5(10) . . ? O1D C1D C2D 124.0(10) . . ? N1D C1D C2D 117.3(10) . . ? C3D C2D C6D 123.6(10) . . ? C3D C2D C1D 120.1(9) . . ? C6D C2D C1D 116.2(10) . . ? C4D C3D C2D 122.0(10) . . ? C4D C3D C9D 118.7(10) . . ? C2D C3D C9D 119.3(9) . . ? C3D C4D C12D 122.6(11) . . ? C3D C4D C5D 120.2(11) . . ? C12D C4D C5D 117.1(10) . . ? O2D C5D N1D 118.6(12) . . ? O2D C5D C4D 124.0(12) . . ? N1D C5D C4D 117.3(11) . . ? C2D C6D C7D 115.9(12) . . ? C2D C6D H6D 122.1 . . ? C7D C6D H6D 122.1 . . ? C8D C7D C6D 118.6(14) . . ? C8D C7D H7D 120.7 . . ? C6D C7D H7D 120.7 . . ? C7D C8D C9D 128.7(14) . . ? C7D C8D H8D 115.7 . . ? C9D C8D H8D 115.7 . . ? C8D C9D C10D 132.8(12) . . ? C8D C9D C3D 112.9(11) . . ? C10D C9D C3D 114.0(10) . . ? C11D C10D C9D 127.2(13) . . ? C11D C10D H10D 116.4 . . ? C9D C10D H10D 116.4 . . ? C10D C11D C12D 118.9(13) . . ? C10D C11D H11D 120.6 . . ? C12D C11D H11D 120.6 . . ? C4D C12D C11D 118.1(12) . . ? C4D C12D H12D 120.9 . . ? C11D C12D H12D 120.9 . . ? N1D C13D C16D 112.6(11) . . ? N1D C13D C14D 109.6(11) . . ? C16D C13D C14D 108.9(11) . . ? N1D C13D H13D 108.6 . . ? C16D C13D H13D 108.6 . . ? C14D C13D H13D 108.6 . . ? C1D N1D C5D 122.9(10) . . ? C1D N1D C13D 117.8(10) . . ? C5D N1D C13D 119.2(10) . . ? C15D C14D C13D 113.8(14) . . ? C15D C14D H14G 108.8 . . ? C13D C14D H14G 108.8 . . ? C15D C14D H14H 108.8 . . ? C13D C14D H14H 108.8 . . ? H14G C14D H14H 107.7 . . ? O3D C15D N2D 122(2) . . ? O3D C15D C14D 124(2) . . ? N2D C15D C14D 113.3(19) . . ? O4D C16D O5D 126.7(12) . . ? O4D C16D C13D 116.0(12) . . ? O5D C16D C13D 117.2(12) . . ? C15D N2D H2D1 120.0 . . ? C15D N2D H2D2 120.0 . . ? H2D1 N2D H2D2 120.0 . . ? C16D O4D Cu1 125.5(8) . . ? C16D O5D Cu2 121.4(8) . . ? O1E C1E N1E 120.2(9) . . ? O1E C1E C2E 121.8(9) . . ? N1E C1E C2E 117.5(9) . . ? C6E C2E C3E 122.1(10) . . ? C6E C2E C1E 119.5(10) . . ? C3E C2E C1E 118.4(9) . . ? C4E C3E C2E 123.5(10) . . ? C4E C3E C9E 119.4(10) . . ? C2E C3E C9E 117.0(10) . . ? C3E C4E C12E 121.6(11) . . ? C3E C4E C5E 119.7(10) . . ? C12E C4E C5E 118.7(11) . . ? O2E C5E N1E 116.7(10) . . ? O2E C5E C4E 125.4(10) . . ? N1E C5E C4E 117.7(9) . . ? C2E C6E C7E 120.4(12) . . ? C2E C6E H6E 119.8 . . ? C7E C6E H6E 119.8 . . ? C8E C7E C6E 114.6(13) . . ? C8E C7E H7E 122.7 . . ? C6E C7E H7E 122.7 . . ? C7E C8E C9E 131.5(15) . . ? C7E C8E H8E 114.2 . . ? C9E C8E H8E 114.2 . . ? C8E C9E C10E 132.9(13) . . ? C8E C9E C3E 114.2(11) . . ? C10E C9E C3E 112.8(12) . . ? C11E C10E C9E 128.2(15) . . ? C11E C10E H10E 115.9 . . ? C9E C10E H10E 115.9 . . ? C10E C11E C12E 118.7(14) . . ? C10E C11E H11E 120.7 . . ? C12E C11E H11E 120.7 . . ? C4E C12E C11E 119.2(12) . . ? C4E C12E H12E 120.4 . . ? C11E C12E H12E 120.4 . . ? N1E C13E C16E 112.4(9) . . ? N1E C13E C14E 108.1(10) . . ? C16E C13E C14E 116.3(10) . . ? N1E C13E H13E 106.4 . . ? C16E C13E H13E 106.4 . . ? C14E C13E H13E 106.4 . . ? C1E N1E C5E 122.7(8) . . ? C1E N1E C13E 116.8(8) . . ? C5E N1E C13E 120.4(8) . . ? C13E C14E C15E 115.9(14) . . ? C13E C14E H14I 108.3 . . ? C15E C14E H14I 108.3 . . ? C13E C14E H14J 108.3 . . ? C15E C14E H14J 108.3 . . ? H14I C14E H14J 107.4 . . ? O3E C15E N2E 119(2) . . ? O3E C15E C14E 124(2) . . ? N2E C15E C14E 117.0(19) . . ? O4E C16E O5E 127.2(11) . . ? O4E C16E C13E 120.0(10) . . ? O5E C16E C13E 112.7(10) . . ? C15E N2E H2E1 120.0 . . ? C15E N2E H2E2 120.0 . . ? H2E1 N2E H2E2 120.0 . . ? C15E O3E Cu2 135.8(14) . . ? C16E O4E Cu3 115.9(7) . . ? C16E O5E Cu4 127.0(7) . . ? O1F C1F N1F 119.7(11) . . ? O1F C1F C2F 123.1(11) . . ? N1F C1F C2F 117.0(10) . . ? C3F C2F C6F 127.1(11) . . ? C3F C2F C1F 117.7(10) . . ? C6F C2F C1F 114.9(10) . . ? C4F C3F C2F 124.8(11) . . ? C4F C3F C9F 117.1(10) . . ? C2F C3F C9F 117.8(10) . . ? C3F C4F C12F 125.6(11) . . ? C3F C4F C5F 119.2(11) . . ? C12F C4F C5F 115.2(11) . . ? O2F C5F N1F 117.7(11) . . ? O2F C5F C4F 125.7(11) . . ? N1F C5F C4F 116.4(10) . . ? C2F C6F C7F 113.0(11) . . ? C2F C6F H6F 123.5 . . ? C7F C6F H6F 123.5 . . ? C8F C7F C6F 117.2(12) . . ? C8F C7F H7F 121.4 . . ? C6F C7F H7F 121.4 . . ? C7F C8F C9F 134.4(14) . . ? C7F C8F H8F 112.8 . . ? C9F C8F H8F 112.8 . . ? C8F C9F C10F 136.0(13) . . ? C8F C9F C3F 109.8(11) . . ? C10F C9F C3F 112.7(11) . . ? C11F C10F C9F 128.6(14) . . ? C11F C10F H10F 115.7 . . ? C9F C10F H10F 115.7 . . ? C10F C11F C12F 120.5(13) . . ? C10F C11F H11F 119.8 . . ? C12F C11F H11F 119.8 . . ? C4F C12F C11F 114.9(12) . . ? C4F C12F H12F 122.6 . . ? C11F C12F H12F 122.6 . . ? N1F C13F C16F 109.5(12) . . ? N1F C13F C14F 110.4(12) . . ? C16F C13F C14F 116.5(11) . . ? N1F C13F H13F 106.6 . . ? C16F C13F H13F 106.6 . . ? C14F C13F H13F 106.6 . . ? C1F N1F C5F 124.0(10) . . ? C1F N1F C13F 116.4(10) . . ? C5F N1F C13F 119.6(10) . . ? C15F C14F C13F 112.8(10) . . ? C15F C14F H14K 109.0 . . ? C13F C14F H14K 109.0 . . ? C15F C14F H14L 109.0 . . ? C13F C14F H14L 109.0 . . ? H14K C14F H14L 107.8 . . ? O3F C15F N2F 119.5(13) . . ? O3F C15F C14F 123.8(12) . . ? N2F C15F C14F 116.7(13) . . ? O4F C16F O5F 122.2(11) . . ? O4F C16F C13F 121.2(11) . . ? O5F C16F C13F 115.8(11) . . ? C15F N2F H2F1 120.0 . . ? C15F N2F H2F2 120.0 . . ? H2F1 N2F H2F2 120.0 . . ? C16F O4F Cu3 129.5(8) . . ? C16F O5F Cu4 119.9(7) . . ? O1H C1H N1H 119.7(9) . . ? O1H C1H C2H 120.7(9) . . ? N1H C1H C2H 119.6(9) . . ? C6H C2H C3H 123.3(9) . . ? C6H C2H C1H 119.7(9) . . ? C3H C2H C1H 116.6(9) . . ? C4H C3H C2H 123.3(9) . . ? C4H C3H C9H 120.0(9) . . ? C2H C3H C9H 116.7(9) . . ? C3H C4H C12H 121.1(9) . . ? C3H C4H C5H 120.5(9) . . ? C12H C4H C5H 118.4(9) . . ? O2H C5H N1H 118.0(9) . . ? O2H C5H C4H 125.8(9) . . ? N1H C5H C4H 116.2(9) . . ? C2H C6H C7H 118.6(11) . . ? C2H C6H H6H 120.7 . . ? C7H C6H H6H 120.7 . . ? C8H C7H C6H 117.0(12) . . ? C8H C7H H7H 121.5 . . ? C6H C7H H7H 121.5 . . ? C7H C8H C9H 128.2(13) . . ? C7H C8H H8H 115.9 . . ? C9H C8H H8H 115.9 . . ? C8H C9H C10H 130.5(12) . . ? C8H C9H C3H 116.0(10) . . ? C10H C9H C3H 113.5(10) . . ? C11H C10H C9H 126.2(13) . . ? C11H C10H H10H 116.9 . . ? C9H C10H H10H 116.9 . . ? C10H C11H C12H 121.1(12) . . ? C10H C11H H11H 119.4 . . ? C12H C11H H11H 119.4 . . ? C4H C12H C11H 118.0(10) . . ? C4H C12H H12H 121.0 . . ? C11H C12H H12H 121.0 . . ? N1H C13H C14H 111.6(10) . . ? N1H C13H C16H 110.7(10) . . ? C14H C13H C16H 114.1(10) . . ? N1H C13H H13H 106.6 . . ? C14H C13H H13H 106.6 . . ? C16H C13H H13H 106.6 . . ? C1H N1H C5H 123.1(9) . . ? C1H N1H C13H 116.6(9) . . ? C5H N1H C13H 120.3(9) . . ? C15H C14H C13H 109.9(13) . . ? C15H C14H H14M 109.7 . . ? C13H C14H H14M 109.7 . . ? C15H C14H H14N 109.7 . . ? C13H C14H H14N 109.7 . . ? H14M C14H H14N 108.2 . . ? O3H C15H N2H 117.8(18) . . ? O3H C15H C14H 124.3(18) . . ? N2H C15H C14H 117.7(18) . . ? O5H C16H O4H 131.1(12) . . ? O5H C16H C13H 116.3(11) . . ? O4H C16H C13H 112.5(11) . . ? C15H N2H H2H1 120.0 . . ? C15H N2H H2H2 120.0 . . ? H2H1 N2H H2H2 120.0 . . ? C16H O4H Cu3 117.7(8) . . ? C16H O5H Cu4 120.9(8) . . ? C21I N3I C25I 120.0 . . ? C21I N3I Cu1 122.9(9) . . ? C25I N3I Cu1 117.1(9) . . ? C22I C21I N3I 120.0 . . ? C22I C21I H21I 120.0 . . ? N3I C21I H21I 120.0 . . ? C21I C22I C23I 120.0 . . ? C21I C22I H22I 120.0 . . ? C23I C22I H22I 120.0 . . ? C22I C23I C24I 120.0 . . ? C22I C23I H23I 120.0 . . ? C24I C23I H23I 120.0 . . ? C25I C24I C23I 120.0 . . ? C25I C24I H24I 120.0 . . ? C23I C24I H24I 120.0 . . ? C24I C25I N3I 120.0 . . ? C24I C25I H25I 120.0 . . ? N3I C25I H25I 120.0 . . ? C21J N3J C25J 120.0 . . ? C21J N3J Cu1 117.5(9) . . ? C25J N3J Cu1 122.1(9) . . ? C22J C21J N3J 120.0 . . ? C22J C21J H21J 120.0 . . ? N3J C21J H21J 120.0 . . ? C21J C22J C23J 120.0 . . ? C21J C22J H22J 120.0 . . ? C23J C22J H22J 120.0 . . ? C24J C23J C22J 120.0 . . ? C24J C23J H23J 120.0 . . ? C22J C23J H23J 120.0 . . ? C23J C24J C25J 120.0 . . ? C23J C24J H24J 120.0 . . ? C25J C24J H24J 120.0 . . ? C24J C25J N3J 120.0 . . ? C24J C25J H25J 120.0 . . ? N3J C25J H25J 120.0 . . ? C31 O36 Cu3 121.1(12) . . ? C31 O37 C32 121.1(13) . . ? O36 C31 O37 120.2(15) . . ? O36 C31 C34 125.5(15) . . ? O37 C31 C34 113.5(15) . . ? C33 C32 O37 104.3(13) . . ? C33 C32 H32A 110.9 . . ? O37 C32 H32A 110.9 . . ? C33 C32 H32B 110.9 . . ? O37 C32 H32B 110.9 . . ? H32A C32 H32B 108.9 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O38 C34 C31 108.7(13) . . ? O38 C34 C35 111.5(13) . . ? C31 C34 C35 112.0(13) . . ? O38 C34 H34 108.2 . . ? C31 C34 H34 108.2 . . ? C35 C34 H34 108.2 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C41 O47 C42 120.3(14) . . ? O46 C41 O47 117.8(18) . . ? O46 C41 C44 126.6(18) . . ? O47 C41 C44 113.2(17) . . ? C43 C42 O47 101.7(14) . . ? C43 C42 H42A 111.4 . . ? O47 C42 H42A 111.4 . . ? C43 C42 H42B 111.4 . . ? O47 C42 H42B 111.4 . . ? H42A C42 H42B 109.3 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? O48 C44 C41 106.2(15) . . ? O48 C44 C45 111.8(16) . . ? C41 C44 C45 109.6(16) . . ? O48 C44 H44 109.7 . . ? C41 C44 H44 109.7 . . ? C45 C44 H44 109.7 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C51 O57 C52 124.3(17) . . ? O56 C51 O57 114.6(18) . . ? O56 C51 C54 126(2) . . ? O57 C51 C54 112.8(19) . . ? C53 C52 O57 96.2(12) . . ? C53 C52 H52A 112.5 . . ? O57 C52 H52A 112.5 . . ? C53 C52 H52B 112.5 . . ? O57 C52 H52B 112.5 . . ? H52A C52 H52B 110.0 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? O58 C54 C51 111.8(18) . . ? O58 C54 C55 114.1(18) . . ? C51 C54 C55 110.2(18) . . ? O58 C54 H54 106.8 . . ? C51 C54 H54 106.8 . . ? C55 C54 H54 106.8 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C61 O67 C62 131.3(18) . . ? O66 C61 O67 118.8(19) . . ? O66 C61 C64 123(2) . . ? O67 C61 C64 116.9(19) . . ? C63 C62 O67 98.4(15) . . ? C63 C62 H62A 112.1 . . ? O67 C62 H62A 112.1 . . ? C63 C62 H62B 112.1 . . ? O67 C62 H62B 112.1 . . ? H62A C62 H62B 109.7 . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? O68 C64 C61 110.2(17) . . ? O68 C64 C65 111.3(18) . . ? C61 C64 C65 108.7(18) . . ? O68 C64 H64 108.9 . . ? C61 C64 H64 108.9 . . ? C65 C64 H64 108.9 . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4C Cu1 Cu2 O5D 88.4(3) . . . . ? O4A Cu1 Cu2 O5D -88.6(3) . . . . ? O4B Cu1 Cu2 O5D 179.8(3) . . . . ? O4D Cu1 Cu2 O5D -2.1(3) . . . . ? O4C Cu1 Cu2 O5B -92.3(3) . . . . ? O4A Cu1 Cu2 O5B 90.7(3) . . . . ? O4B Cu1 Cu2 O5B -0.9(3) . . . . ? O4D Cu1 Cu2 O5B 177.2(3) . . . . ? O4C Cu1 Cu2 O5C 1.6(3) . . . . ? O4A Cu1 Cu2 O5C -175.4(3) . . . . ? O4B Cu1 Cu2 O5C 92.9(3) . . . . ? O4D Cu1 Cu2 O5C -88.9(3) . . . . ? O4C Cu1 Cu2 O5A 178.6(3) . . . . ? O4A Cu1 Cu2 O5A 1.6(3) . . . . ? O4B Cu1 Cu2 O5A -90.0(3) . . . . ? O4D Cu1 Cu2 O5A 88.1(3) . . . . ? O4G Cu3 Cu4 O5F -98.4(3) . . . . ? O4E Cu3 Cu4 O5F 85.9(3) . . . . ? O4H Cu3 Cu4 O5F 171.6(3) . . . . ? O4F Cu3 Cu4 O5F -2.8(3) . . . . ? O36 Cu3 Cu4 O5F -17.1(12) . . . . ? O4G Cu3 Cu4 O5H 84.9(3) . . . . ? O4E Cu3 Cu4 O5H -90.8(3) . . . . ? O4H Cu3 Cu4 O5H -5.1(3) . . . . ? O4F Cu3 Cu4 O5H -179.5(3) . . . . ? O36 Cu3 Cu4 O5H 166.1(12) . . . . ? O4G Cu3 Cu4 O5G -3.3(3) . . . . ? O4E Cu3 Cu4 O5G -179.0(3) . . . . ? O4H Cu3 Cu4 O5G -93.3(3) . . . . ? O4F Cu3 Cu4 O5G 92.3(3) . . . . ? O36 Cu3 Cu4 O5G 77.9(12) . . . . ? O4G Cu3 Cu4 O5E 176.6(3) . . . . ? O4E Cu3 Cu4 O5E 0.9(3) . . . . ? O4H Cu3 Cu4 O5E 86.6(3) . . . . ? O4F Cu3 Cu4 O5E -87.8(3) . . . . ? O36 Cu3 Cu4 O5E -102.1(12) . . . . ? O1G C1G C2G C6G -1.7(19) . . . . ? N1G C1G C2G C6G 179.4(12) . . . . ? O1G C1G C2G C3G 179.4(12) . . . . ? N1G C1G C2G C3G 0.5(17) . . . . ? C6G C2G C3G C4G 176.9(13) . . . . ? C1G C2G C3G C4G -4(2) . . . . ? C6G C2G C3G C9G -2(2) . . . . ? C1G C2G C3G C9G 176.6(11) . . . . ? C2G C3G C4G C12G 178.1(13) . . . . ? C9G C3G C4G C12G -3(2) . . . . ? C2G C3G C4G C5G 3(2) . . . . ? C9G C3G C4G C5G -178.0(12) . . . . ? C3G C4G C5G O2G -176.5(14) . . . . ? C12G C4G C5G O2G 8(2) . . . . ? C3G C4G C5G N1G 2.4(19) . . . . ? C12G C4G C5G N1G -173.2(12) . . . . ? C3G C2G C6G C7G 2(2) . . . . ? C1G C2G C6G C7G -176.6(11) . . . . ? C2G C6G C7G C8G -2(2) . . . . ? C6G C7G C8G C9G 2(3) . . . . ? C7G C8G C9G C10G -178.6(16) . . . . ? C7G C8G C9G C3G -2(2) . . . . ? C4G C3G C9G C10G -0.2(19) . . . . ? C2G C3G C9G C10G 179.0(13) . . . . ? C4G C3G C9G C8G -177.1(13) . . . . ? C2G C3G C9G C8G 2.1(19) . . . . ? C8G C9G C10G C11G 178.9(17) . . . . ? C3G C9G C10G C11G 3(2) . . . . ? C9G C10G C11G C12G -2(3) . . . . ? C3G C4G C12G C11G 3(2) . . . . ? C5G C4G C12G C11G 178.9(12) . . . . ? C10G C11G C12G C4G -1(2) . . . . ? O1G C1G N1G C5G -174.0(12) . . . . ? C2G C1G N1G C5G 4.9(18) . . . . ? O1G C1G N1G C13G -0.7(17) . . . . ? C2G C1G N1G C13G 178.2(10) . . . . ? O2G C5G N1G C1G 172.8(12) . . . . ? C4G C5G N1G C1G -6.3(19) . . . . ? O2G C5G N1G C13G -0.4(18) . . . . ? C4G C5G N1G C13G -179.4(11) . . . . ? C16G C13G N1G C1G 55.3(14) . . . . ? C14G C13G N1G C1G -76.9(13) . . . . ? C16G C13G N1G C5G -131.0(12) . . . . ? C14G C13G N1G C5G 96.8(13) . . . . ? C16G C13G C14G C15G 68.6(15) . . . . ? N1G C13G C14G C15G -161.8(11) . . . . ? C13G C14G C15G O3G 25(2) . . . . ? C13G C14G C15G N2G -151.6(13) . . . . ? N1G C13G C16G O5G -137.0(11) . . . . ? C14G C13G C16G O5G -11.2(16) . . . . ? N1G C13G C16G O4G 43.4(15) . . . . ? C14G C13G C16G O4G 169.3(11) . . . . ? O5G C16G O4G Cu3 9.3(18) . . . . ? C13G C16G O4G Cu3 -171.2(7) . . . . ? O4H Cu3 O4G C16G 84.9(9) . . . . ? O4F Cu3 O4G C16G -80.5(9) . . . . ? O36 Cu3 O4G C16G -168.6(9) . . . . ? Cu4 Cu3 O4G C16G -1.2(9) . . . . ? O4G C16G O5G Cu4 -13.4(17) . . . . ? C13G C16G O5G Cu4 167.1(7) . . . . ? O5F Cu4 O5G C16G 96.6(9) . . . . ? O5H Cu4 O5G C16G -75.0(9) . . . . ? O5E Cu4 O5G C16G 8.7(16) . . . . ? O3Z Cu4 O5G C16G -177.3(10) . . . . ? O3A Cu4 O5G C16G -169.9(9) . . . . ? Cu3 Cu4 O5G C16G 9.0(8) . . . . ? O1A C1A C2A C3A -178.9(13) . . . . ? N1A C1A C2A C3A 1.5(13) . . . . ? O1A C1A C2A C6A 2.8(15) . . . . ? N1A C1A C2A C6A -176.8(15) . . . . ? C6A C2A C3A C4A 176.2(15) . . . . ? C1A C2A C3A C4A -1.8(13) . . . . ? C6A C2A C3A C9A -4.3(15) . . . . ? C1A C2A C3A C9A 177.6(10) . . . . ? C2A C3A C4A C12A 178.3(12) . . . . ? C9A C3A C4A C5A -177.9(13) . . . . ? C3A C4A C5A O2A 179.5(16) . . . . ? C12A C4A C5A N1A -177.8(15) . . . . ? C1A C2A C6A C7A 176.8(11) . . . . ? C2A C3A C9A C10A 176.9(12) . . . . ? C4A C3A C9A C8A -178.5(15) . . . . ? C2A C3A C9A C8A 2.0(18) . . . . ? C5A C4A C12A C11A -179.0(15) . . . . ? O1A C1A N1A C5A 179.4(15) . . . . ? C2A C1A N1A C13A -170.9(9) . . . . ? O2A C5A N1A C1A -179.7(15) . . . . ? C4A C5A N1A C13A 169.5(13) . . . . ? O5A C16A O4A Cu1 13.8(16) . . . . ? C13A C16A O4A Cu1 -173.4(9) . . . . ? O4B Cu1 O4A C16A 71.0(9) . . . . ? O4D Cu1 O4A C16A -86.2(9) . . . . ? N3I Cu1 O4A C16A 165.8(11) . . . . ? N3J Cu1 O4A C16A 170.5(11) . . . . ? Cu2 Cu1 O4A C16A -8.2(9) . . . . ? O4A C16A O5A Cu2 -12.4(17) . . . . ? C13A C16A O5A Cu2 174.5(8) . . . . ? O5D Cu2 O5A C16A 92.7(10) . . . . ? O5B Cu2 O5A C16A -83.4(10) . . . . ? O5C Cu2 O5A C16A 11.9(14) . . . . ? O3E Cu2 O5A C16A -173.4(10) . . . . ? Cu1 Cu2 O5A C16A 4.6(9) . . . . ? O4A C16A C13A N1A 34.1(16) . . . . ? O5A C16A C13A N1A -152.7(11) . . . . ? O4A C16A C13A C14A 151.9(13) . . . . ? O5A C16A C13A C14A -34.9(17) . . . . ? C1A N1A C13A C16A 55.1(16) . . . . ? C5A N1A C13A C16A -114.2(16) . . . . ? C1A N1A C13A C14A -64.5(18) . . . . ? C5A N1A C13A C14A 126.1(17) . . . . ? N1A C13A C14A C15A -179.2(17) . . . . ? C13A C14A C15A N2A -108(2) . . . . ? C14A C15A O3A Cu4 166.1(13) . . . . ? C14Z C15Z O3Z Cu4 167.3(15) . . . . ? O5F Cu4 O3Z C15Z -137.2(18) . . . . ? O5H Cu4 O3Z C15Z 40.3(18) . . . . ? O5G Cu4 O3Z C15Z 127.9(18) . . . . ? O5E Cu4 O3Z C15Z -53.9(18) . . . . ? N1B C1B C2B C6B 178.4(15) . . . . ? O1B C1B C2B C3B 176.9(15) . . . . ? C6B C2B C3B C4B -176.2(17) . . . . ? C1B C2B C3B C9B -179.9(13) . . . . ? C2B C3B C4B C12B 175.4(16) . . . . ? C9B C3B C4B C5B 178.8(13) . . . . ? C3B C4B C5B O2B 175.4(17) . . . . ? C12B C4B C5B N1B -176.7(14) . . . . ? C1B C2B C6B C7B 177.0(13) . . . . ? C7B C8B C9B C10B 178.1(19) . . . . ? C4B C3B C9B C8B 177.3(16) . . . . ? C2B C3B C9B C10B -176.2(15) . . . . ? C8B C9B C10B C11B -175.4(19) . . . . ? C9B C10B C11B C12B -4(3) . . . . ? C3B C4B C12B C11B -2(3) . . . . ? C5B C4B C12B C11B -179.5(13) . . . . ? C10B C11B C12B C4B 3(2) . . . . ? O1B C1B N1B C5B -177.4(15) . . . . ? C2B C1B N1B C5B 3(2) . . . . ? O1B C1B N1B C13B 6(2) . . . . ? C2B C1B N1B C13B -173.2(13) . . . . ? O2B C5B N1B C1B -174.3(15) . . . . ? C4B C5B N1B C1B -4(2) . . . . ? O2B C5B N1B C13B 2(2) . . . . ? C4B C5B N1B C13B 172.3(13) . . . . ? C16B C13B N1B C1B 46.2(19) . . . . ? C14B C13B N1B C1B -78.8(16) . . . . ? C16B C13B N1B C5B -130.4(14) . . . . ? C14B C13B N1B C5B 104.6(15) . . . . ? N1B C13B C14B C15B -161.9(11) . . . . ? C16B C13B C14B C15B 74.1(15) . . . . ? C13B C14B C15B O3B 27(2) . . . . ? C13B C14B C15B N2B -144.6(14) . . . . ? N1B C13B C16B O5B -136.2(12) . . . . ? C14B C13B C16B O5B -15.7(17) . . . . ? N1B C13B C16B O4B 47.1(17) . . . . ? C14B C13B C16B O4B 167.6(11) . . . . ? O5B C16B O4B Cu1 -1.8(18) . . . . ? C13B C16B O4B Cu1 174.4(8) . . . . ? O4C Cu1 O4B C16B 87.7(9) . . . . ? O4A Cu1 O4B C16B -87.4(9) . . . . ? O4D Cu1 O4B C16B -3.2(14) . . . . ? N3I Cu1 O4B C16B -174.7(10) . . . . ? N3J Cu1 O4B C16B 173.8(10) . . . . ? Cu2 Cu1 O4B C16B 1.6(9) . . . . ? O4B C16B O5B Cu2 0.4(17) . . . . ? C13B C16B O5B Cu2 -175.9(8) . . . . ? O5C Cu2 O5B C16B -78.5(9) . . . . ? O5A Cu2 O5B C16B 78.0(9) . . . . ? O3E Cu2 O5B C16B 177.0(9) . . . . ? Cu1 Cu2 O5B C16B 0.7(8) . . . . ? N1C C1C C2C C6C -177.5(17) . . . . ? O1C C1C C2C C3C -176.8(17) . . . . ? C6C C2C C3C C4C 177.5(19) . . . . ? C1C C2C C3C C9C -179.2(14) . . . . ? C2C C3C C4C C12C 176.7(18) . . . . ? C9C C3C C4C C5C -174.4(15) . . . . ? C3C C4C C5C O2C 176.9(19) . . . . ? C12C C4C C5C N1C 175.9(15) . . . . ? C1C C2C C6C C7C 179.2(14) . . . . ? C7C C8C C9C C10C 173(2) . . . . ? C4C C3C C9C C8C -178.2(18) . . . . ? C2C C3C C9C C10C -174.9(16) . . . . ? C8C C9C C10C C11C 180(2) . . . . ? C5C C4C C12C C11C 171.9(15) . . . . ? C10C C11C C12C C4C 3(3) . . . . ? O1C C1C N1C C5C 169.8(16) . . . . ? C2C C1C N1C C13C -178.0(15) . . . . ? O2C C5C N1C C1C -175.7(17) . . . . ? C4C C5C N1C C13C -176.1(15) . . . . ? C16C C13C N1C C5C -109.5(16) . . . . ? C14C C13C N1C C5C 128.8(16) . . . . ? N1C C13C C14C C15C -48.6(18) . . . . ? C16C C13C C14C C15C -168.8(12) . . . . ? C13C C14C C15C O3C -47.0(18) . . . . ? C13C C14C C15C N2C 133.8(14) . . . . ? N1C C13C C16C O4C 23.3(19) . . . . ? C14C C13C C16C O4C 147.9(12) . . . . ? N1C C13C C16C O5C -163.2(11) . . . . ? C14C C13C C16C O5C -38.6(17) . . . . ? O5C C16C O4C Cu1 14.9(18) . . . . ? C13C C16C O4C Cu1 -172.3(10) . . . . ? O4B Cu1 O4C C16C -87.6(10) . . . . ? O4D Cu1 O4C C16C 69.6(10) . . . . ? N3I Cu1 O4C C16C 177.4(11) . . . . ? N3J Cu1 O4C C16C 173.3(12) . . . . ? Cu2 Cu1 O4C C16C -8.4(9) . . . . ? O4C C16C O5C Cu2 -12.8(18) . . . . ? C13C C16C O5C Cu2 174.0(9) . . . . ? O5D Cu2 O5C C16C -84.2(10) . . . . ? O5B Cu2 O5C C16C 91.5(9) . . . . ? O5A Cu2 O5C C16C -2.8(14) . . . . ? O3E Cu2 O5C C16C -177.3(9) . . . . ? Cu1 Cu2 O5C C16C 4.5(9) . . . . ? O1D C1D C2D C3D -173.7(14) . . . . ? N1D C1D C2D C6D 178.0(13) . . . . ? C6D C2D C3D C4D -179.6(14) . . . . ? C1D C2D C3D C9D 176.2(12) . . . . ? C2D C3D C4D C12D 179.0(14) . . . . ? C9D C3D C4D C5D -178.7(14) . . . . ? C3D C4D C5D O2D -175.8(17) . . . . ? C12D C4D C5D N1D -174.8(14) . . . . ? C1D C2D C6D C7D 178.8(14) . . . . ? C7D C8D C9D C10D 179.9(19) . . . . ? C4D C3D C9D C8D 179.6(15) . . . . ? C2D C3D C9D C10D -174.8(13) . . . . ? C8D C9D C10D C11D -176.6(19) . . . . ? C5D C4D C12D C11D 172.7(15) . . . . ? O1D C1D N1D C5D 178.4(14) . . . . ? C2D C1D N1D C13D -174.6(11) . . . . ? O2D C5D N1D C1D 174.0(16) . . . . ? C4D C5D N1D C13D 172.2(13) . . . . ? C16D C13D N1D C1D 51.1(17) . . . . ? C14D C13D N1D C1D -70.3(16) . . . . ? C16D C13D N1D C5D -125.9(14) . . . . ? C14D C13D N1D C5D 112.7(15) . . . . ? N1D C13D C14D C15D -61.5(18) . . . . ? C16D C13D C14D C15D 174.9(15) . . . . ? C13D C14D C15D O3D 88(2) . . . . ? C13D C14D C15D N2D -97.7(18) . . . . ? N1D C13D C16D O4D 41.1(16) . . . . ? C14D C13D C16D O4D 162.8(11) . . . . ? N1D C13D C16D O5D -142.8(11) . . . . ? C14D C13D C16D O5D -21.1(16) . . . . ? O5D C16D O4D Cu1 3.7(18) . . . . ? C13D C16D O4D Cu1 179.3(8) . . . . ? O4C Cu1 O4D C16D -86.1(9) . . . . ? O4A Cu1 O4D C16D 90.2(9) . . . . ? O4B Cu1 O4D C16D 5.0(14) . . . . ? N3I Cu1 O4D C16D 176.1(10) . . . . ? N3J Cu1 O4D C16D -172.0(10) . . . . ? Cu2 Cu1 O4D C16D 0.2(9) . . . . ? O4D C16D O5D Cu2 -6.5(18) . . . . ? C13D C16D O5D Cu2 177.9(8) . . . . ? O5C Cu2 O5D C16D 84.3(9) . . . . ? O5A Cu2 O5D C16D -72.5(9) . . . . ? O3E Cu2 O5D C16D -171.5(9) . . . . ? Cu1 Cu2 O5D C16D 4.8(9) . . . . ? N1E C1E C2E C6E -175.5(12) . . . . ? O1E C1E C2E C3E 177.9(12) . . . . ? N1E C1E C2E C3E 5.8(19) . . . . ? C6E C2E C3E C4E 177.4(14) . . . . ? C1E C2E C3E C9E 179.1(12) . . . . ? C2E C3E C4E C12E -176.9(15) . . . . ? C9E C3E C4E C5E 180.0(13) . . . . ? C3E C4E C5E O2E -178.6(14) . . . . ? C12E C4E C5E N1E 176.1(13) . . . . ? C1E C2E C6E C7E -177.2(13) . . . . ? C4E C3E C9E C8E -176.8(16) . . . . ? C2E C3E C9E C10E 177.3(15) . . . . ? C8E C9E C10E C11E 175(2) . . . . ? C5E C4E C12E C11E -178.9(14) . . . . ? O1E C1E N1E C5E -179.3(11) . . . . ? C2E C1E N1E C5E -7.1(17) . . . . ? O1E C1E N1E C13E 4.3(17) . . . . ? C2E C1E N1E C13E 176.5(11) . . . . ? O2E C5E N1E C1E -178.6(12) . . . . ? C4E C5E N1E C1E 6.2(18) . . . . ? O2E C5E N1E C13E -2.3(18) . . . . ? C4E C5E N1E C13E -177.5(11) . . . . ? C16E C13E N1E C1E 52.1(14) . . . . ? C14E C13E N1E C1E -77.7(13) . . . . ? C16E C13E N1E C5E -124.4(11) . . . . ? C14E C13E N1E C5E 105.8(12) . . . . ? N1E C13E C14E C15E -149.2(12) . . . . ? C16E C13E C14E C15E 83.2(16) . . . . ? C13E C14E C15E O3E 172.6(17) . . . . ? N1E C13E C16E O4E 31.1(16) . . . . ? C14E C13E C16E O4E 156.6(11) . . . . ? N1E C13E C16E O5E -152.5(10) . . . . ? C14E C13E C16E O5E -27.0(15) . . . . ? C14E C15E O3E Cu2 160.7(11) . . . . ? O5D Cu2 O3E C15E 39.6(19) . . . . ? O5B Cu2 O3E C15E -139.4(19) . . . . ? O5C Cu2 O3E C15E 127.0(19) . . . . ? O5A Cu2 O3E C15E -50.8(19) . . . . ? O5E C16E O4E Cu3 4.0(16) . . . . ? C13E C16E O4E Cu3 179.8(8) . . . . ? O4H Cu3 O4E C16E -88.5(9) . . . . ? O4F Cu3 O4E C16E 77.2(8) . . . . ? O36 Cu3 O4E C16E 165.0(9) . . . . ? Cu4 Cu3 O4E C16E -2.6(8) . . . . ? O4E C16E O5E Cu4 -3.2(18) . . . . ? C13E C16E O5E Cu4 -179.3(7) . . . . ? O5F Cu4 O5E C16E -88.5(9) . . . . ? O5H Cu4 O5E C16E 84.2(9) . . . . ? O5G Cu4 O5E C16E 0.9(17) . . . . ? O3Z Cu4 O5E C16E -172.8(10) . . . . ? O3A Cu4 O5E C16E 179.6(10) . . . . ? Cu3 Cu4 O5E C16E 0.6(9) . . . . ? O1F C1F C2F C3F -173.6(16) . . . . ? N1F C1F C2F C6F -173.6(14) . . . . ? C6F C2F C3F C4F 175.7(17) . . . . ? C1F C2F C3F C9F 177.2(14) . . . . ? C2F C3F C4F C12F -175.0(17) . . . . ? C9F C3F C4F C5F 175.3(14) . . . . ? C3F C4F C5F O2F -171.4(16) . . . . ? C12F C4F C5F N1F -178.7(14) . . . . ? C1F C2F C6F C7F 179.4(13) . . . . ? C7F C8F C9F C10F -173.6(19) . . . . ? C4F C3F C9F C8F -169.3(16) . . . . ? C2F C3F C9F C10F 172.5(16) . . . . ? C5F C4F C12F C11F -177.6(14) . . . . ? O1F C1F N1F C5F 179.0(15) . . . . ? C2F C1F N1F C13F 172.8(13) . . . . ? O2F C5F N1F C1F 173.9(15) . . . . ? C4F C5F N1F C13F 179.9(13) . . . . ? C16F C13F N1F C1F 55.5(17) . . . . ? C14F C13F N1F C1F -74.1(17) . . . . ? C16F C13F N1F C5F -125.9(14) . . . . ? C14F C13F N1F C5F 104.5(15) . . . . ? N1F C13F C14F C15F -159.8(11) . . . . ? C16F C13F C14F C15F 74.5(15) . . . . ? C13F C14F C15F O3F 34.2(18) . . . . ? C13F C14F C15F N2F -147.9(12) . . . . ? N1F C13F C16F O4F 45.4(17) . . . . ? C14F C13F C16F O4F 171.5(11) . . . . ? N1F C13F C16F O5F -145.1(10) . . . . ? C14F C13F C16F O5F -19.0(16) . . . . ? O5F C16F O4F Cu3 -9.6(17) . . . . ? C13F C16F O4F Cu3 159.3(9) . . . . ? O4G Cu3 O4F C16F 90.4(10) . . . . ? O4E Cu3 O4F C16F -84.3(10) . . . . ? O4H Cu3 O4F C16F -14.6(18) . . . . ? O36 Cu3 O4F C16F -175.8(10) . . . . ? Cu4 Cu3 O4F C16F 7.3(9) . . . . ? O4F C16F O5F Cu4 4.8(15) . . . . ? C13F C16F O5F Cu4 -164.6(8) . . . . ? O5G Cu4 O5F C16F -84.2(8) . . . . ? O5E Cu4 O5F C16F 78.7(8) . . . . ? O3Z Cu4 O5F C16F -174.0(9) . . . . ? O3A Cu4 O5F C16F 173.1(9) . . . . ? Cu3 Cu4 O5F C16F 0.2(8) . . . . ? O1H C1H C2H C6H 4.9(19) . . . . ? N1H C1H C2H C6H -173.0(12) . . . . ? O1H C1H C2H C3H 178.6(12) . . . . ? N1H C1H C2H C3H 0.7(18) . . . . ? C6H C2H C3H C4H 176.7(13) . . . . ? C1H C2H C3H C4H 3.2(19) . . . . ? C6H C2H C3H C9H -4.4(19) . . . . ? C1H C2H C3H C9H -177.8(11) . . . . ? C2H C3H C4H C12H 176.9(12) . . . . ? C9H C3H C4H C5H -179.4(12) . . . . ? C3H C4H C5H O2H 176.1(12) . . . . ? C3H C4H C5H N1H -6.0(18) . . . . ? C12H C4H C5H N1H 176.5(11) . . . . ? C1H C2H C6H C7H 178.2(12) . . . . ? C7H C8H C9H C10H 178.9(16) . . . . ? C4H C3H C9H C8H -179.4(13) . . . . ? C2H C3H C9H C8H 1.6(19) . . . . ? C2H C3H C9H C10H -177.1(13) . . . . ? C8H C9H C10H C11H 179.0(16) . . . . ? C3H C4H C12H C11H 2.5(19) . . . . ? C5H C4H C12H C11H 180.0(11) . . . . ? O1H C1H N1H C5H 174.4(11) . . . . ? C2H C1H N1H C5H -7.6(18) . . . . ? O1H C1H N1H C13H -3.7(17) . . . . ? C2H C1H N1H C13H 174.2(11) . . . . ? O2H C5H N1H C1H -171.8(11) . . . . ? C4H C5H N1H C1H 10.1(17) . . . . ? O2H C5H N1H C13H 6.3(17) . . . . ? C4H C5H N1H C13H -171.8(11) . . . . ? C14H C13H N1H C1H -74.0(14) . . . . ? C16H C13H N1H C1H 54.2(14) . . . . ? C14H C13H N1H C5H 107.8(12) . . . . ? C16H C13H N1H C5H -123.9(11) . . . . ? N1H C13H C14H C15H -69.7(16) . . . . ? C16H C13H C14H C15H 163.8(13) . . . . ? C13H C14H C15H N2H 116.2(16) . . . . ? N1H C13H C16H O5H -128.6(11) . . . . ? C14H C13H C16H O5H -1.7(16) . . . . ? N1H C13H C16H O4H 52.4(14) . . . . ? C14H C13H C16H O4H 179.3(11) . . . . ? O5H C16H O4H Cu3 -2.0(18) . . . . ? C13H C16H O4H Cu3 176.8(7) . . . . ? O4G Cu3 O4H C16H -78.8(8) . . . . ? O4E Cu3 O4H C16H 97.0(9) . . . . ? O4F Cu3 O4H C16H 26.9(17) . . . . ? O36 Cu3 O4H C16H -172.7(8) . . . . ? Cu4 Cu3 O4H C16H 5.3(8) . . . . ? O4H C16H O5H Cu4 -4.8(18) . . . . ? C13H C16H O5H Cu4 176.4(7) . . . . ? O5G Cu4 O5H C16H 91.3(9) . . . . ? O5E Cu4 O5H C16H -71.7(9) . . . . ? O3Z Cu4 O5H C16H -179.1(9) . . . . ? O3A Cu4 O5H C16H -166.4(9) . . . . ? Cu3 Cu4 O5H C16H 6.5(8) . . . . ? O4C Cu1 N3I C21I 165.0(11) . . . . ? O4A Cu1 N3I C21I -17.5(11) . . . . ? O4B Cu1 N3I C21I 73.7(11) . . . . ? O4D Cu1 N3I C21I -102.8(11) . . . . ? O4C Cu1 N3I C25I -18.0(11) . . . . ? O4A Cu1 N3I C25I 159.5(11) . . . . ? O4B Cu1 N3I C25I -109.3(10) . . . . ? O4D Cu1 N3I C25I 74.2(11) . . . . ? C25I N3I C21I C22I 0.0 . . . . ? Cu1 N3I C21I C22I 176.9(16) . . . . ? N3I C21I C22I C23I 0.0 . . . . ? C21I C22I C23I C24I 0.0 . . . . ? C22I C23I C24I C25I 0.0 . . . . ? C23I C24I C25I N3I 0.0 . . . . ? C21I N3I C25I C24I 0.0 . . . . ? Cu1 N3I C25I C24I -177.1(15) . . . . ? O4C Cu1 N3J C21J 166.7(11) . . . . ? O4A Cu1 N3J C21J -16.1(11) . . . . ? O4B Cu1 N3J C21J 76.7(10) . . . . ? O4D Cu1 N3J C21J -104.5(10) . . . . ? O4C Cu1 N3J C25J -20.5(11) . . . . ? O4A Cu1 N3J C25J 156.6(11) . . . . ? O4B Cu1 N3J C25J -110.5(11) . . . . ? O4D Cu1 N3J C25J 68.3(12) . . . . ? C25J N3J C21J C22J 0.0 . . . . ? Cu1 N3J C21J C22J 172.9(15) . . . . ? N3J C21J C22J C23J 0.0 . . . . ? C21J C22J C23J C24J 0.0 . . . . ? C22J C23J C24J C25J 0.0 . . . . ? C23J C24J C25J N3J 0.0 . . . . ? C21J N3J C25J C24J 0.0 . . . . ? Cu1 N3J C25J C24J -172.6(16) . . . . ? O4G Cu3 O36 C31 110.1(12) . . . . ? O4E Cu3 O36 C31 -73.1(12) . . . . ? O4H Cu3 O36 C31 -159.1(12) . . . . ? O4F Cu3 O36 C31 15.8(12) . . . . ? Cu3 O36 C31 O37 -94.3(19) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2G H2G2 O68 0.88 2.20 3.06(2) 163.4 . N2A H2A1 O5E 0.88 2.37 3.07(2) 137.4 . N2A H2A1 O5F 0.88 2.59 3.17(2) 124.1 . N2A H2A2 O3B 0.88 2.44 3.25(2) 153.3 . N2Z H2Z1 O5H 0.88 2.27 3.01(2) 142.1 . N2Z H2Z2 O1D 0.88 2.13 2.909(19) 147.5 . N2B H2B1 O3F 0.88 2.07 2.944(15) 170.7 . N2E H2E1 O5D 0.88 2.12 2.893(18) 146.8 . N2E H2E2 O1H 0.88 2.11 2.883(19) 145.7 . N2F H2F1 O3B 0.88 1.91 2.789(17) 176.0 . N2H H2H2 O3D 0.88 2.01 2.86(2) 160.4 . N2G H2G1 O1C 0.88 2.20 3.057(17) 163.9 1_455 N2F H2F2 O3C 0.88 2.05 2.900(17) 161.7 1_455 N2C H2C1 O3Z 0.88 2.43 3.198(19) 146.1 1_655 N2C H2C2 O3G 0.88 2.24 3.114(16) 173.3 1_655 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 22.59 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.720 _refine_diff_density_min -0.703 _refine_diff_density_rms 0.103 _vrf_THETM01_3 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: No observable diffraction at high angle due to small available crystal size, extensive disorder and large cell. ; _vrf_PLAT023_3 ; PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6].. 22.59 Deg. RESPONSE: No observable diffraction at high angle due to small available crystal size, extensive disorder and large cell. ; _vrf_PLAT201_3 ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 187 RESPONSE: Due to the weak data, only the copper atoms refined anisotropically; carbon, nitrogen and oxygen atoms were refined isotropically to avoid a low data-to-parameter ratio and some physically unreasonable displacement parameters. ; _vrf_PLAT602_3 ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: The voids contain heavily disordered guest species, which could not be modeled and were therefore accounted for with the Squeeze program. The voids found by the the CHECKCIF program are actually filled with the disordered guests. ; #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 799346' #TrackingRef 'jhCC3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C138 H103 Cu4 N17 O43' _chemical_formula_sum 'C138 H103 Cu4 N17 O43' _chemical_formula_weight 2941.53 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ab 2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 15.1728(15) _cell_length_b 21.670(2) _cell_length_c 52.697(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 17327(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1470 _cell_measurement_theta_min 2.149 _cell_measurement_theta_max 19.740 _exptl_crystal_description 'rectanglur bar' _exptl_crystal_colour blue-green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.128 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6040 _exptl_absorpt_coefficient_mu 0.556 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 75115 _diffrn_reflns_av_R_equivalents 0.2005 _diffrn_reflns_av_sigmaI/netI 0.2089 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 1.02 _diffrn_reflns_theta_max 18.00 _reflns_number_total 11917 _reflns_number_gt 6196 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART Version 5.625 (Bruker, 2001)' _computing_cell_refinement 'SAINT-Plus Version 6.45 (Bruker, 2001)' _computing_data_reduction 'SAINT-Plus Version 6.45 (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics various _computing_publication_material 'SHELXTL Version 6.14 (Bruker, 2000)' _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^)+(0.0554P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.06(3) _refine_ls_number_reflns 11917 _refine_ls_number_parameters 742 _refine_ls_number_restraints 1041 _refine_ls_R_factor_all 0.1232 _refine_ls_R_factor_gt 0.0782 _refine_ls_wR_factor_ref 0.1814 _refine_ls_wR_factor_gt 0.1660 _refine_ls_goodness_of_fit_ref 0.879 _refine_ls_restrained_S_all 0.865 _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 Cu1 Cu 0.96585(14) 0.42331(11) 0.30566(4) 0.0486(7) Uani 1 1 d D . . Cu2 Cu 0.93582(15) 0.41252(11) 0.35582(4) 0.0546(8) Uani 1 1 d . B . Cu3 Cu 0.55385(14) 0.54477(10) 0.45881(4) 0.0420(7) Uani 1 1 d . A . Cu4 Cu 0.57589(14) 0.52072(10) 0.41078(4) 0.0392(7) Uani 1 1 d D . . C1G C 0.4273(10) 0.7295(6) 0.4291(3) 0.065(6) Uiso 1 1 d D . . C2G C 0.4254(9) 0.7926(6) 0.4403(3) 0.057(6) Uiso 1 1 d D . . C3G C 0.3584(9) 0.8105(7) 0.4550(3) 0.072(3) Uiso 1 1 d D . . C4G C 0.2862(9) 0.7767(6) 0.4568(3) 0.062(6) Uiso 1 1 d D . . C5G C 0.2741(10) 0.7178(7) 0.4446(3) 0.073(7) Uiso 1 1 d D . . C6G C 0.5034(10) 0.8232(7) 0.4373(3) 0.072(3) Uiso 1 1 d D . . H6G H 0.5502 0.8070 0.4274 0.087 Uiso 1 1 calc R . . C7G C 0.5104(10) 0.8830(7) 0.4504(3) 0.072(3) Uiso 1 1 d D . . H7G H 0.5617 0.9081 0.4494 0.087 Uiso 1 1 calc R . . C8G C 0.4387(10) 0.8996(7) 0.4639(3) 0.072(3) Uiso 1 1 d D . . H8G H 0.4417 0.9400 0.4708 0.087 Uiso 1 1 calc R . . C9G C 0.3643(10) 0.8696(7) 0.4692(3) 0.072(3) Uiso 1 1 d D . . C10G C 0.2915(11) 0.8807(7) 0.4825(3) 0.072(3) Uiso 1 1 d D . . H10G H 0.2933 0.9169 0.4926 0.087 Uiso 1 1 calc R . . C11G C 0.2194(11) 0.8501(7) 0.4837(3) 0.080(7) Uiso 1 1 d D . . H11G H 0.1717 0.8649 0.4937 0.096 Uiso 1 1 calc R . . C12G C 0.2110(10) 0.7937(7) 0.4700(3) 0.076(7) Uiso 1 1 d D . . H12G H 0.1585 0.7699 0.4699 0.091 Uiso 1 1 calc R . . C13G C 0.3503(10) 0.6328(6) 0.4197(3) 0.037(5) Uiso 1 1 d D . . H13G H 0.2971 0.6113 0.4265 0.044 Uiso 1 1 calc R . . N1G N 0.3532(8) 0.6938(6) 0.4316(2) 0.049(5) Uiso 1 1 d D . . O1G O 0.4865(7) 0.7099(5) 0.4154(2) 0.056(4) Uiso 1 1 d D . . O2G O 0.2147(8) 0.6800(6) 0.4447(2) 0.073(4) Uiso 1 1 d D . . C14G C 0.3293(15) 0.6484(10) 0.3893(4) 0.098(8) Uiso 1 1 d . . . H14O H 0.2859 0.6824 0.3882 0.117 Uiso 1 1 calc R . . H14P H 0.3842 0.6622 0.3808 0.117 Uiso 1 1 calc R . . C15G C 0.2933(14) 0.5920(11) 0.3756(4) 0.080(7) Uiso 1 1 d . . . C16G C 0.4256(13) 0.5904(9) 0.4231(4) 0.057(6) Uiso 1 1 d . . . N2G N 0.3126(11) 0.5872(9) 0.3519(4) 0.114(7) Uiso 1 1 d . . . H2G1 H 0.3030 0.5522 0.3438 0.137 Uiso 1 1 calc R . . H2G2 H 0.3353 0.6189 0.3437 0.137 Uiso 1 1 calc R . . O3G O 0.2613(10) 0.5463(7) 0.3866(3) 0.096(5) Uiso 1 1 d . . . O4G O 0.4480(7) 0.5855(5) 0.4466(2) 0.042(3) Uiso 1 1 d . A . O5G O 0.4578(7) 0.5620(5) 0.4061(2) 0.043(3) Uiso 1 1 d . . . C1A C 0.6875(11) 0.3896(10) 0.2832(4) 0.135(3) Uiso 1 1 d D A . C2A C 0.6747(8) 0.3721(9) 0.2558(3) 0.135(3) Uiso 1 1 d D . . C3A C 0.6563(8) 0.4153(7) 0.2390(3) 0.135(3) Uiso 1 1 d D . . C4A C 0.6475(16) 0.4738(8) 0.2460(4) 0.135(3) Uiso 1 1 d D . . C5A C 0.6625(17) 0.4972(11) 0.2712(4) 0.135(3) Uiso 1 1 d D A . C6A C 0.6866(15) 0.3094(9) 0.2525(4) 0.135(3) Uiso 1 1 d D . . H6A H 0.7037 0.2830 0.2660 0.162 Uiso 1 1 calc R . . C7A C 0.6710(15) 0.2860(9) 0.2265(4) 0.135(3) Uiso 1 1 d D . . H7A H 0.6691 0.2437 0.2219 0.162 Uiso 1 1 calc R . . C8A C 0.6596(15) 0.3336(10) 0.2101(4) 0.135(3) Uiso 1 1 d D . . H8A H 0.6608 0.3206 0.1929 0.162 Uiso 1 1 calc R . . C9A C 0.6472(16) 0.3942(10) 0.2123(4) 0.135(3) Uiso 1 1 d D . . C10A C 0.6311(15) 0.4434(10) 0.1985(4) 0.135(3) Uiso 1 1 d D . . H10A H 0.6294 0.4352 0.1808 0.162 Uiso 1 1 calc R . . C11A C 0.6173(15) 0.4999(10) 0.2040(4) 0.135(3) Uiso 1 1 d D . . H11A H 0.5988 0.5276 0.1911 0.162 Uiso 1 1 calc R . . C12A C 0.6293(15) 0.5224(9) 0.2296(4) 0.135(3) Uiso 1 1 d D . . H12A H 0.6254 0.5645 0.2345 0.162 Uiso 1 1 calc R . . N1A N 0.6787(13) 0.4560(6) 0.2892(4) 0.135(3) Uiso 1 1 d D . . O1A O 0.7036(11) 0.3570(7) 0.3001(3) 0.135(3) Uiso 1 1 d D . . O2A O 0.6516(11) 0.5546(7) 0.2782(3) 0.135(3) Uiso 1 1 d D . . O4A O 0.8490(8) 0.4572(5) 0.3022(2) 0.063(4) Uiso 1 1 d . A . O5A O 0.8218(8) 0.4493(6) 0.3440(3) 0.073(4) Uiso 1 1 d . . . C16A C 0.7973(15) 0.4584(10) 0.3215(4) 0.083(8) Uiso 1 1 d . A . C13A C 0.7057(11) 0.4768(6) 0.3153(3) 0.051(3) Uiso 0.50 1 d PD A 3 H13A H 0.6975 0.5224 0.3173 0.061 Uiso 0.50 1 calc PR A 3 C14A C 0.646(2) 0.4409(15) 0.3338(4) 0.051(3) Uiso 0.50 1 d PD A 3 H14A H 0.5844 0.4483 0.3283 0.061 Uiso 0.50 1 calc PR A 3 H14B H 0.6579 0.3965 0.3311 0.061 Uiso 0.50 1 calc PR A 3 C15A C 0.649(2) 0.4516(11) 0.3621(4) 0.051(3) Uiso 0.50 1 d PD A 3 N2A N 0.6771(16) 0.4065(11) 0.3776(5) 0.051(3) Uiso 0.50 1 d PD A 3 H2A1 H 0.6734 0.4112 0.3942 0.061 Uiso 0.50 1 calc PR A 3 H2A2 H 0.6995 0.3725 0.3712 0.061 Uiso 0.50 1 calc PR A 3 O3A O 0.6180(15) 0.4978(12) 0.3733(3) 0.051(3) Uiso 0.50 1 d PD A 3 C13Z C 0.7057(11) 0.4768(6) 0.3153(3) 0.051(3) Uiso 0.50 1 d PD A 4 H13Z H 0.7098 0.5227 0.3135 0.061 Uiso 0.50 1 calc PR A 4 C14Z C 0.642(2) 0.4685(14) 0.3377(5) 0.051(3) Uiso 0.50 1 d PD A 4 H14Y H 0.5813 0.4692 0.3306 0.061 Uiso 0.50 1 calc PR A 4 H14Z H 0.6514 0.4264 0.3445 0.061 Uiso 0.50 1 calc PR A 4 C15Z C 0.6425(18) 0.5117(13) 0.3599(5) 0.051(3) Uiso 0.50 1 d PD A 4 N2Z N 0.7102(15) 0.5522(11) 0.3599(5) 0.051(3) Uiso 0.50 1 d PD A 4 H2Z1 H 0.7176 0.5775 0.3728 0.061 Uiso 0.50 1 calc PR A 4 H2Z2 H 0.7469 0.5533 0.3469 0.061 Uiso 0.50 1 calc PR A 4 O3Z O 0.5777(14) 0.4925(11) 0.3720(3) 0.051(3) Uiso 0.50 1 d PD A 4 C1B C 0.9918(10) 0.2020(9) 0.3125(3) 0.0789(17) Uiso 1 1 d D . . C2B C 1.0464(10) 0.1671(8) 0.2937(3) 0.0789(17) Uiso 1 1 d D . . C3B C 1.0085(10) 0.1348(9) 0.2753(3) 0.0789(17) Uiso 1 1 d D . . C4B C 0.9222(10) 0.1366(9) 0.2714(3) 0.0789(17) Uiso 1 1 d D . . C5B C 0.8603(10) 0.1680(8) 0.2884(3) 0.0789(17) Uiso 1 1 d D . . C6B C 1.1326(10) 0.1683(8) 0.2982(3) 0.0789(17) Uiso 1 1 d D . . H6B H 1.1565 0.1908 0.3121 0.095 Uiso 1 1 calc R . . C7B C 1.1885(11) 0.1335(8) 0.2809(3) 0.0789(17) Uiso 1 1 d D . . H7B H 1.2509 0.1321 0.2825 0.095 Uiso 1 1 calc R . . C8B C 1.1456(11) 0.1039(9) 0.2627(3) 0.0789(17) Uiso 1 1 d D . . H8B H 1.1829 0.0813 0.2516 0.095 Uiso 1 1 calc R . . C9B C 1.0621(10) 0.0997(8) 0.2571(3) 0.0789(17) Uiso 1 1 d D . . C10B C 1.0143(11) 0.0720(9) 0.2391(3) 0.0789(17) Uiso 1 1 d D . . H10B H 1.0473 0.0457 0.2283 0.095 Uiso 1 1 calc R . . C11B C 0.9319(11) 0.0743(8) 0.2339(3) 0.0789(17) Uiso 1 1 d D . . H11B H 0.9079 0.0558 0.2191 0.095 Uiso 1 1 calc R . . C12B C 0.8781(11) 0.1068(8) 0.2520(3) 0.0789(17) Uiso 1 1 d D . . H12B H 0.8156 0.1078 0.2507 0.095 Uiso 1 1 calc R . . C13B C 0.8507(12) 0.2490(9) 0.3239(4) 0.0789(17) Uiso 1 1 d D B . H13B H 0.7931 0.2567 0.3153 0.095 Uiso 1 1 calc R . . N1B N 0.9030(9) 0.2085(7) 0.3072(3) 0.0789(17) Uiso 1 1 d D . . O1B O 1.0246(8) 0.2330(6) 0.3298(2) 0.0789(17) Uiso 1 1 d D . . O2B O 0.7827(8) 0.1818(6) 0.2853(2) 0.0789(17) Uiso 1 1 d D . . C14B C 0.8307(12) 0.2137(9) 0.3488(3) 0.061(6) Uiso 1 1 d . . . H14C H 0.8130 0.1710 0.3446 0.073 Uiso 1 1 calc R . . H14D H 0.8852 0.2115 0.3591 0.073 Uiso 1 1 calc R . . C15B C 0.7577(17) 0.2436(11) 0.3648(5) 0.104(9) Uiso 1 1 d . . . C16B C 0.8894(11) 0.3053(9) 0.3280(4) 0.045(6) Uiso 1 1 d . . . N2B N 0.7730(11) 0.2413(7) 0.3885(3) 0.084(6) Uiso 1 1 d . . . H2B1 H 0.7397 0.2623 0.3991 0.100 Uiso 1 1 calc R . . H2B2 H 0.8168 0.2188 0.3943 0.100 Uiso 1 1 calc R . . O3B O 0.6987(10) 0.2733(7) 0.3543(3) 0.096(5) Uiso 1 1 d . . . O4B O 0.9146(7) 0.3374(5) 0.3076(2) 0.044(3) Uiso 1 1 d . B . O5B O 0.8917(7) 0.3336(5) 0.3491(2) 0.040(3) Uiso 1 1 d . B . C1C C 1.2606(15) 0.4481(8) 0.3099(4) 0.114(3) Uiso 1 1 d D . . C2C C 1.3078(15) 0.4663(8) 0.2859(3) 0.114(3) Uiso 1 1 d D . . C3C C 1.3459(15) 0.4230(8) 0.2716(4) 0.114(3) Uiso 1 1 d D . . C4C C 1.3419(15) 0.3641(8) 0.2770(4) 0.114(3) Uiso 1 1 d D . . C5C C 1.2907(15) 0.3383(8) 0.2979(4) 0.114(3) Uiso 1 1 d D . . C6C C 1.3132(14) 0.5275(8) 0.2823(4) 0.114(3) Uiso 1 1 d D . . H6C H 1.2921 0.5559 0.2946 0.137 Uiso 1 1 calc R . . C7C C 1.3546(14) 0.5486(8) 0.2579(4) 0.114(3) Uiso 1 1 d D . . H7C H 1.3505 0.5895 0.2515 0.137 Uiso 1 1 calc R . . C8C C 1.3989(14) 0.5017(8) 0.2459(4) 0.114(3) Uiso 1 1 d D . . H8C H 1.4431 0.5156 0.2345 0.137 Uiso 1 1 calc R . . C9C C 1.3919(15) 0.4408(8) 0.2472(4) 0.114(3) Uiso 1 1 d D . . C10C C 1.4247(15) 0.3926(9) 0.2338(4) 0.114(3) Uiso 1 1 d D . . H10C H 1.4539 0.4019 0.2184 0.137 Uiso 1 1 calc R . . C11C C 1.4200(15) 0.3355(9) 0.2401(4) 0.114(3) Uiso 1 1 d D . . H11C H 1.4413 0.3051 0.2287 0.137 Uiso 1 1 calc R . . C12C C 1.3836(14) 0.3163(8) 0.2639(4) 0.114(3) Uiso 1 1 d D . . H12C H 1.3873 0.2752 0.2701 0.137 Uiso 1 1 calc R . . C13C C 1.2059(15) 0.3649(10) 0.3376(4) 0.114(3) Uiso 1 1 d D B . H13C H 1.2113 0.3190 0.3387 0.137 Uiso 1 1 calc R . . N1C N 1.2578(12) 0.3863(7) 0.3155(3) 0.114(3) Uiso 1 1 d D . . O1C O 1.2219(8) 0.4856(6) 0.3236(2) 0.075(4) Uiso 1 1 d D . . O2C O 1.2821(10) 0.2872(6) 0.3060(3) 0.114(6) Uiso 1 1 d D . . C14C C 1.2376(15) 0.3946(11) 0.3645(4) 0.114(9) Uiso 1 1 d . . . H14E H 1.2232 0.4392 0.3649 0.137 Uiso 1 1 calc R . . H14F H 1.2057 0.3743 0.3787 0.137 Uiso 1 1 calc R . . C15C C 1.3384(15) 0.3857(12) 0.3681(4) 0.078(8) Uiso 1 1 d . . . C16C C 1.1085(12) 0.3812(8) 0.3349(4) 0.043(6) Uiso 1 1 d . . . N2C N 1.3811(10) 0.4341(7) 0.3753(3) 0.068(5) Uiso 1 1 d . . . H2C1 H 1.4389 0.4329 0.3768 0.081 Uiso 1 1 calc R . . H2C2 H 1.3525 0.4684 0.3788 0.081 Uiso 1 1 calc R . . O3C O 1.3677(11) 0.3370(8) 0.3628(3) 0.119(6) Uiso 1 1 d . . . O4C O 1.0810(8) 0.3921(5) 0.3122(2) 0.057(4) Uiso 1 1 d . B . O5C O 1.0595(8) 0.3844(5) 0.3543(2) 0.054(3) Uiso 1 1 d . B . C1D C 0.9170(10) 0.6369(8) 0.3224(3) 0.079(7) Uiso 1 1 d D . . C2D C 0.8855(10) 0.6775(8) 0.3009(3) 0.065(6) Uiso 1 1 d D . . C3D C 0.9421(10) 0.7105(8) 0.2873(3) 0.066(6) Uiso 1 1 d D . . C4D C 1.0274(10) 0.7093(9) 0.2920(3) 0.084(7) Uiso 1 1 d D . . C5D C 1.0665(11) 0.6721(11) 0.3119(4) 0.139(10) Uiso 1 1 d D . . C6D C 0.7980(11) 0.6763(10) 0.2959(4) 0.127(10) Uiso 1 1 d D . . H6D H 0.7591 0.6504 0.3052 0.153 Uiso 1 1 calc R . . C7D C 0.7657(12) 0.7168(10) 0.2755(4) 0.125 Uiso 1 1 d D . . H7D H 0.7047 0.7223 0.2721 0.150 Uiso 1 1 calc R . . C8D C 0.8290(12) 0.7453(10) 0.2619(4) 0.112(9) Uiso 1 1 d D . . H8D H 0.8090 0.7654 0.2469 0.134 Uiso 1 1 calc R . . C9D C 0.9140(11) 0.7496(9) 0.2661(3) 0.077(7) Uiso 1 1 d D . . C10D C 0.9808(12) 0.7756(9) 0.2528(4) 0.096(8) Uiso 1 1 d D . . H10D H 0.9639 0.7966 0.2378 0.115 Uiso 1 1 calc R . . C11D C 1.0648(12) 0.7759(9) 0.2577(3) 0.098(8) Uiso 1 1 d D . . H11D H 1.1054 0.7964 0.2468 0.117 Uiso 1 1 calc R . . C12D C 1.0937(12) 0.7442(10) 0.2799(4) 0.131(10) Uiso 1 1 d D . . H12D H 1.1525 0.7464 0.2860 0.157 Uiso 1 1 calc R . . C13D C 1.0385(12) 0.5890(8) 0.3449(3) 0.071(6) Uiso 1 1 d D B . H13D H 1.1041 0.5866 0.3435 0.085 Uiso 1 1 calc R . . N1D N 1.0062(8) 0.6335(7) 0.3263(3) 0.067(5) Uiso 1 1 d D . . O1D O 0.8672(8) 0.6036(6) 0.3349(3) 0.089(5) Uiso 1 1 d D . . O2D O 1.1427(10) 0.6643(8) 0.3171(3) 0.125 Uiso 1 1 d D . . C14D C 1.0142(15) 0.6119(8) 0.3715(3) 0.125 Uiso 1 1 d D . . H14G H 0.9495 0.6068 0.3727 0.150 Uiso 1 1 calc R . . H14H H 1.0397 0.5810 0.3832 0.150 Uiso 1 1 calc R . . C15D C 1.0324(11) 0.6716(9) 0.3833(3) 0.125 Uiso 1 1 d D . . N2D N 1.1034(11) 0.6691(8) 0.3985(3) 0.125 Uiso 1 1 d D . . H2D1 H 1.1207 0.7023 0.4067 0.150 Uiso 1 1 calc R . . H2D2 H 1.1326 0.6343 0.4002 0.150 Uiso 1 1 calc R . . O3D O 0.9944(10) 0.7198(7) 0.3814(3) 0.125 Uiso 1 1 d D . . C16D C 1.0030(12) 0.5278(10) 0.3439(4) 0.064(7) Uiso 1 1 d . . . O4D O 1.0033(7) 0.5073(5) 0.3194(2) 0.052(4) Uiso 1 1 d . B . O5D O 0.9794(8) 0.4942(6) 0.3595(2) 0.058(4) Uiso 1 1 d . B . C1E C 0.7429(9) 0.3851(6) 0.4856(3) 0.074(7) Uiso 1 1 d D . . C2E C 0.7529(8) 0.3547(5) 0.5106(2) 0.039(5) Uiso 1 1 d D . . C3E C 0.8199(9) 0.3671(6) 0.5262(3) 0.067(3) Uiso 1 1 d D . . C4E C 0.8802(10) 0.4070(8) 0.5190(3) 0.067(3) Uiso 1 1 d D . . C5E C 0.8774(10) 0.4447(8) 0.4961(3) 0.067(3) Uiso 1 1 d D . . C6E C 0.6919(11) 0.3125(8) 0.5164(3) 0.080(7) Uiso 1 1 d D . . H6E H 0.6467 0.3019 0.5047 0.096 Uiso 1 1 calc R . . C7E C 0.6969(13) 0.2831(9) 0.5415(4) 0.125 Uiso 1 1 d D . . H7E H 0.6518 0.2562 0.5473 0.150 Uiso 1 1 calc R . . C8E C 0.7682(12) 0.2957(8) 0.5559(3) 0.086(8) Uiso 1 1 d D . . H8E H 0.7766 0.2712 0.5706 0.103 Uiso 1 1 calc R . . C9E C 0.8269(10) 0.3386(7) 0.5514(3) 0.052(6) Uiso 1 1 d D . . C10E C 0.9017(10) 0.3528(8) 0.5642(3) 0.067(3) Uiso 1 1 d D . . H10E H 0.9130 0.3298 0.5792 0.080 Uiso 1 1 calc R . . C11E C 0.9590(11) 0.3940(7) 0.5582(3) 0.067(3) Uiso 1 1 d D . . H11E H 1.0061 0.4036 0.5694 0.080 Uiso 1 1 calc R . . C12E C 0.9507(10) 0.4251(7) 0.5346(3) 0.067(3) Uiso 1 1 d D . . H12E H 0.9908 0.4565 0.5296 0.080 Uiso 1 1 calc R . . C13E C 0.7982(11) 0.4537(8) 0.4524(3) 0.054(6) Uiso 1 1 d D A . H13E H 0.8427 0.4877 0.4516 0.065 Uiso 1 1 calc R . . N1E N 0.8069(8) 0.4271(6) 0.4782(2) 0.042(4) Uiso 1 1 d D . . O1E O 0.6835(8) 0.3738(5) 0.4699(2) 0.065(4) Uiso 1 1 d D . . O2E O 0.9300(8) 0.4815(6) 0.4868(2) 0.086(4) Uiso 1 1 d D . . C14E C 0.8268(14) 0.4094(10) 0.4341(4) 0.095(8) Uiso 1 1 d . . . H14I H 0.7759 0.3824 0.4303 0.114 Uiso 1 1 calc R . . H14J H 0.8718 0.3832 0.4424 0.114 Uiso 1 1 calc R . . C15E C 0.8674(16) 0.4315(12) 0.4072(5) 0.099(9) Uiso 1 1 d . B . C16E C 0.7123(11) 0.4839(8) 0.4478(3) 0.035(5) Uiso 1 1 d . . . N2E N 0.8648(12) 0.4974(9) 0.4037(3) 0.112(7) Uiso 1 1 d . . . H2E1 H 0.8900 0.5141 0.3903 0.135 Uiso 1 1 calc R . . H2E2 H 0.8380 0.5209 0.4149 0.135 Uiso 1 1 calc R . . O3E O 0.8999(8) 0.4048(6) 0.3935(2) 0.057(4) Uiso 1 1 d . . . O4E O 0.6701(7) 0.5072(5) 0.4673(2) 0.048(4) Uiso 1 1 d . A . O5E O 0.6856(7) 0.4852(5) 0.4252(2) 0.041(3) Uiso 1 1 d . A . C1F C 0.3329(10) 0.3743(8) 0.4591(3) 0.0709(16) Uiso 1 1 d D . . C2F C 0.2617(10) 0.3616(9) 0.4778(3) 0.0709(16) Uiso 1 1 d D . . C3F C 0.2745(10) 0.3286(8) 0.4987(3) 0.0709(16) Uiso 1 1 d D . . C4F C 0.3517(10) 0.3037(9) 0.5032(3) 0.0709(16) Uiso 1 1 d D . . C5F C 0.4283(10) 0.3100(8) 0.4864(3) 0.0709(16) Uiso 1 1 d D . . C6F C 0.1815(10) 0.3819(8) 0.4708(3) 0.0709(16) Uiso 1 1 d D . . H6F H 0.1717 0.4025 0.4551 0.085 Uiso 1 1 calc R . . C7F C 0.1097(10) 0.3698(8) 0.4890(3) 0.0709(16) Uiso 1 1 d D . . H7F H 0.0516 0.3835 0.4853 0.085 Uiso 1 1 calc R . . C8F C 0.1264(10) 0.3393(8) 0.5110(3) 0.0709(16) Uiso 1 1 d D . . H8F H 0.0795 0.3359 0.5228 0.085 Uiso 1 1 calc R . . C9F C 0.2017(10) 0.3140(9) 0.5171(3) 0.0709(16) Uiso 1 1 d D . . C10F C 0.2253(11) 0.2800(8) 0.5368(3) 0.0709(16) Uiso 1 1 d D . . H10F H 0.1806 0.2726 0.5491 0.085 Uiso 1 1 calc R . . C11F C 0.3008(11) 0.2557(8) 0.5415(3) 0.0709(16) Uiso 1 1 d D . . H11F H 0.3088 0.2286 0.5555 0.085 Uiso 1 1 calc R . . C12F C 0.3722(11) 0.2708(8) 0.5250(3) 0.0709(16) Uiso 1 1 d D . . H12F H 0.4310 0.2589 0.5287 0.085 Uiso 1 1 calc R . . C13F C 0.4824(11) 0.3584(9) 0.4451(3) 0.0709(16) Uiso 1 1 d D A . H13F H 0.5370 0.3419 0.4532 0.085 Uiso 1 1 calc R . . N1F N 0.4130(9) 0.3475(6) 0.4639(3) 0.0709(16) Uiso 1 1 d D . . O1F O 0.3259(8) 0.4067(6) 0.4397(2) 0.0709(16) Uiso 1 1 d D . . O2F O 0.4990(8) 0.2863(6) 0.4867(2) 0.0709(16) Uiso 1 1 d D . . C14F C 0.4644(11) 0.3137(8) 0.4227(3) 0.047(6) Uiso 1 1 d . . . H14K H 0.4450 0.2732 0.4293 0.056 Uiso 1 1 calc R . . H14L H 0.4170 0.3305 0.4118 0.056 Uiso 1 1 calc R . . C15F C 0.5481(13) 0.3062(8) 0.4074(4) 0.053(6) Uiso 1 1 d . . . C16F C 0.5028(10) 0.4224(8) 0.4397(3) 0.034(5) Uiso 1 1 d . . . N2F N 0.5411(10) 0.2971(6) 0.3824(3) 0.069(5) Uiso 1 1 d . . . H2F1 H 0.5875 0.2857 0.3735 0.083 Uiso 1 1 calc R . . H2F2 H 0.4901 0.3025 0.3748 0.083 Uiso 1 1 calc R . . O3F O 0.6227(9) 0.2977(5) 0.4169(2) 0.065(4) Uiso 1 1 d . . . O4F O 0.5014(6) 0.4629(5) 0.45825(19) 0.038(3) Uiso 1 1 d . A . O5F O 0.5264(7) 0.4400(5) 0.41730(19) 0.039(3) Uiso 1 1 d . A . C1H C 0.8293(9) 0.6522(7) 0.4435(3) 0.056(6) Uiso 1 1 d D . . C2H C 0.9097(9) 0.6576(7) 0.4600(3) 0.049(6) Uiso 1 1 d D . . C3H C 0.9206(9) 0.7062(6) 0.4754(3) 0.038(5) Uiso 1 1 d D . . C4H C 0.8579(9) 0.7489(7) 0.4778(3) 0.048(6) Uiso 1 1 d D . . C5H C 0.7789(10) 0.7506(7) 0.4626(3) 0.047(6) Uiso 1 1 d D . . C6H C 0.9713(10) 0.6135(7) 0.4566(3) 0.071(7) Uiso 1 1 d D . . H6H H 0.9636 0.5814 0.4446 0.085 Uiso 1 1 calc R . . C7H C 1.0516(11) 0.6172(8) 0.4726(3) 0.088(7) Uiso 1 1 d D . . H7H H 1.0949 0.5856 0.4727 0.105 Uiso 1 1 calc R . . C8H C 1.0594(11) 0.6686(8) 0.4871(3) 0.083(7) Uiso 1 1 d D . . H8H H 1.1133 0.6727 0.4962 0.100 Uiso 1 1 calc R . . C9H C 1.0024(11) 0.7134(8) 0.4903(4) 0.089(8) Uiso 1 1 d D . . C10H C 1.0053(12) 0.7646(8) 0.5047(4) 0.094(8) Uiso 1 1 d D . . H10H H 1.0556 0.7686 0.5153 0.112 Uiso 1 1 calc R . . C11H C 0.9492(12) 0.8091(8) 0.5060(3) 0.088(7) Uiso 1 1 d D . . H11H H 0.9609 0.8450 0.5157 0.105 Uiso 1 1 calc R . . C12H C 0.8693(11) 0.8026(7) 0.4923(3) 0.066(7) Uiso 1 1 d D . . H12H H 0.8250 0.8336 0.4929 0.079 Uiso 1 1 calc R . . C13H C 0.6928(10) 0.6977(8) 0.4266(3) 0.064(7) Uiso 1 1 d D A . H13H H 0.6507 0.7307 0.4320 0.077 Uiso 1 1 calc R . . N1H N 0.7683(8) 0.6993(6) 0.4445(2) 0.054(5) Uiso 1 1 d D . . O1H O 0.8136(7) 0.6061(5) 0.4304(2) 0.048(4) Uiso 1 1 d D . . O2H O 0.7148(8) 0.7833(6) 0.4631(2) 0.087(5) Uiso 1 1 d D . . C14H C 0.7204(14) 0.7115(9) 0.3979(3) 0.079(7) Uiso 1 1 d D . . H14M H 0.7716 0.6857 0.3931 0.094 Uiso 1 1 calc R . . H14N H 0.6709 0.7018 0.3864 0.094 Uiso 1 1 calc R . . C15H C 0.7438(16) 0.7783(13) 0.3960(2) 0.150 Uiso 1 1 d D . . O3H O 0.6933(13) 0.8227(9) 0.4003(3) 0.150 Uiso 1 1 d D . . N2H N 0.8306(14) 0.7847(10) 0.3887(4) 0.150 Uiso 1 1 d D . . H2H1 H 0.8535 0.8217 0.3868 0.180 Uiso 1 1 calc R . . H2H2 H 0.8630 0.7517 0.3859 0.180 Uiso 1 1 calc R . . C16H C 0.6424(11) 0.6320(8) 0.4297(4) 0.038(5) Uiso 1 1 d . . . O4H O 0.6215(7) 0.6220(5) 0.4523(2) 0.047(4) Uiso 1 1 d . A . O5H O 0.6300(6) 0.6013(4) 0.4105(2) 0.030(3) Uiso 1 1 d . A . N3I N 0.9788(18) 0.4253(16) 0.2645(2) 0.057(3) Uiso 0.50 1 d PGD B 1 C21I C 0.9063(14) 0.4365(16) 0.2491(4) 0.057(3) Uiso 0.50 1 d PG B 1 H21I H 0.8501 0.4438 0.2564 0.068 Uiso 0.50 1 calc PR B 1 C22I C 0.9160(14) 0.4371(14) 0.2228(4) 0.057(3) Uiso 0.50 1 d PG B 1 H22I H 0.8664 0.4447 0.2123 0.068 Uiso 0.50 1 calc PR B 1 C23I C 0.9982(17) 0.4264(12) 0.2121(2) 0.057(3) Uiso 0.50 1 d PG B 1 H23I H 1.0049 0.4268 0.1941 0.068 Uiso 0.50 1 calc PR B 1 C24I C 1.0707(13) 0.4153(11) 0.2275(4) 0.057(3) Uiso 0.50 1 d PG B 1 H24I H 1.1269 0.4080 0.2202 0.068 Uiso 0.50 1 calc PR B 1 C25I C 1.0610(15) 0.4147(13) 0.2538(4) 0.057(3) Uiso 0.50 1 d PG B 1 H25I H 1.1106 0.4071 0.2643 0.068 Uiso 0.50 1 calc PR B 1 N3J N 1.0012(18) 0.4209(15) 0.2660(2) 0.057(3) Uiso 0.50 1 d PGD B 2 C21J C 0.9350(13) 0.4276(16) 0.2480(4) 0.057(3) Uiso 0.50 1 d PG B 2 H21J H 0.8749 0.4243 0.2529 0.068 Uiso 0.50 1 calc PR B 2 C22J C 0.9567(14) 0.4390(14) 0.2228(4) 0.057(3) Uiso 0.50 1 d PG B 2 H22J H 0.9115 0.4436 0.2105 0.068 Uiso 0.50 1 calc PR B 2 C23J C 1.0446(16) 0.4438(11) 0.2156(3) 0.057(3) Uiso 0.50 1 d PG B 2 H23J H 1.0595 0.4516 0.1984 0.068 Uiso 0.50 1 calc PR B 2 C24J C 1.1108(12) 0.4371(11) 0.2337(4) 0.057(3) Uiso 0.50 1 d PG B 2 H24J H 1.1709 0.4403 0.2288 0.068 Uiso 0.50 1 calc PR B 2 C25J C 1.0891(16) 0.4256(13) 0.2588(4) 0.057(3) Uiso 0.50 1 d PG B 2 H25J H 1.1343 0.4210 0.2712 0.068 Uiso 0.50 1 calc PR B 2 O36 O 0.5139(11) 0.5533(8) 0.4996(3) 0.119(3) Uiso 1 1 d . . . O37 O 0.4090(11) 0.4825(7) 0.5150(3) 0.119(3) Uiso 1 1 d D . . O38 O 0.6379(11) 0.4762(7) 0.5215(3) 0.119(3) Uiso 1 1 d . A . C31 C 0.5023(14) 0.5071(13) 0.5120(5) 0.119(3) Uiso 1 1 d D A . C32 C 0.3409(13) 0.5236(11) 0.5009(4) 0.119(3) Uiso 1 1 d D A . H32A H 0.3272 0.5055 0.4841 0.143 Uiso 1 1 calc R . . H32B H 0.3654 0.5655 0.4982 0.143 Uiso 1 1 calc R . . C33 C 0.2549(14) 0.5272(11) 0.5175(4) 0.119(3) Uiso 1 1 d D . . H33A H 0.2067 0.5059 0.5087 0.179 Uiso 1 1 calc R A . H33B H 0.2388 0.5705 0.5201 0.179 Uiso 1 1 calc R . . H33C H 0.2655 0.5074 0.5339 0.179 Uiso 1 1 calc R . . C34 C 0.5535(17) 0.4505(11) 0.5217(5) 0.119(3) Uiso 1 1 d . . . H34 H 0.5515 0.4183 0.5081 0.143 Uiso 1 1 calc R A . C35 C 0.5316(15) 0.4204(10) 0.5459(4) 0.119(3) Uiso 1 1 d . A . H35A H 0.5666 0.3826 0.5478 0.179 Uiso 1 1 calc R . . H35B H 0.4688 0.4099 0.5461 0.179 Uiso 1 1 calc R . . H35C H 0.5447 0.4485 0.5600 0.179 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0303(15) 0.076(2) 0.0394(16) -0.0023(14) -0.0027(12) 0.0116(14) Cu2 0.0461(17) 0.082(2) 0.0357(16) -0.0105(14) -0.0046(13) 0.0247(17) Cu3 0.0324(15) 0.0558(17) 0.0377(15) -0.0042(12) 0.0097(13) -0.0018(14) Cu4 0.0311(15) 0.0506(16) 0.0359(15) -0.0021(12) 0.0069(13) -0.0011(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O4C 1.905(12) . ? Cu1 O4A 1.928(12) . ? Cu1 O4B 2.020(11) . ? Cu1 O4D 2.039(12) . ? Cu1 N3J 2.158(12) . ? Cu1 N3I 2.177(12) . ? Cu1 Cu2 2.692(3) . ? Cu2 O5B 1.870(11) . ? Cu2 O5D 1.899(13) . ? Cu2 O5C 1.975(12) . ? Cu2 O5A 2.003(13) . ? Cu2 O3E 2.064(13) . ? Cu3 O4G 1.943(11) . ? Cu3 O4F 1.946(10) . ? Cu3 O4H 1.993(11) . ? Cu3 O4E 1.993(11) . ? Cu3 O36 2.242(16) . ? Cu3 Cu4 2.606(3) . ? Cu4 O5H 1.929(10) . ? Cu4 O5F 1.934(10) . ? Cu4 O5E 1.984(11) . ? Cu4 O5G 2.018(11) . ? Cu4 O3Z 2.133(13) . ? Cu4 O3A 2.136(13) . ? C1G O1G 1.229(12) . ? C1G N1G 1.372(12) . ? C1G C2G 1.490(12) . ? C2G C3G 1.334(10) . ? C2G C6G 1.367(11) . ? C3G C4G 1.322(10) . ? C3G C9G 1.484(13) . ? C4G C12G 1.385(11) . ? C4G C5G 1.441(12) . ? C5G O2G 1.217(12) . ? C5G N1G 1.479(13) . ? C6G C7G 1.471(12) . ? C6G H6G 0.9500 . ? C7G C8G 1.348(13) . ? C7G H7G 0.9500 . ? C8G C9G 1.332(13) . ? C8G H8G 0.9500 . ? C9G C10G 1.331(13) . ? C10G C11G 1.282(13) . ? C10G H10G 0.9500 . ? C11G C12G 1.425(12) . ? C11G H11G 0.9500 . ? C12G H12G 0.9500 . ? C13G N1G 1.462(12) . ? C13G C16G 1.48(2) . ? C13G C14G 1.67(2) . ? C13G H13G 1.0000 . ? C14G C15G 1.52(3) . ? C14G H14O 0.9900 . ? C14G H14P 0.9900 . ? C15G O3G 1.25(2) . ? C15G N2G 1.29(2) . ? C16G O5G 1.190(18) . ? C16G O4G 1.290(17) . ? N2G H2G1 0.8800 . ? N2G H2G2 0.8800 . ? C1A O1A 1.16(2) . ? C1A N1A 1.48(2) . ? C1A C2A 1.506(16) . ? C2A C3A 1.316(12) . ? C2A C6A 1.383(13) . ? C3A C4A 1.327(12) . ? C3A C9A 1.486(16) . ? C4A C12A 1.390(13) . ? C4A C5A 1.439(16) . ? C5A O2A 1.31(2) . ? C5A N1A 1.33(2) . ? C6A C7A 1.480(13) . ? C6A H6A 0.9500 . ? C7A C8A 1.356(16) . ? C7A H7A 0.9500 . ? C8A C9A 1.332(16) . ? C8A H8A 0.9500 . ? C9A C10A 1.312(16) . ? C10A C11A 1.276(16) . ? C10A H10A 0.9500 . ? C11A C12A 1.446(13) . ? C11A H11A 0.9500 . ? C12A H12A 0.9500 . ? N1A C13A 1.50(2) . ? O4A C16A 1.29(2) . ? O5A C16A 1.26(2) . ? C16A C13A 1.48(2) . ? C13A C14A 1.542(14) . ? C13A H13A 1.0000 . ? C14A C15A 1.506(14) . ? C14A H14A 0.9900 . ? C14A H14B 0.9900 . ? C15A O3A 1.251(10) . ? C15A N2A 1.347(10) . ? N2A H2A1 0.8800 . ? N2A H2A2 0.8800 . ? C14Z C15Z 1.499(14) . ? C14Z H14Y 0.9900 . ? C14Z H14Z 0.9900 . ? C15Z O3Z 1.245(10) . ? C15Z N2Z 1.351(10) . ? N2Z H2Z1 0.8800 . ? N2Z H2Z2 0.8800 . ? C1B O1B 1.235(13) . ? C1B N1B 1.383(13) . ? C1B C2B 1.499(14) . ? C2B C3B 1.327(13) . ? C2B C6B 1.331(13) . ? C3B C4B 1.326(13) . ? C3B C9B 1.470(14) . ? C4B C12B 1.378(13) . ? C4B C5B 1.467(14) . ? C5B O2B 1.226(13) . ? C5B N1B 1.474(13) . ? C6B C7B 1.459(14) . ? C6B H6B 0.9500 . ? C7B C8B 1.323(14) . ? C7B H7B 0.9500 . ? C8B C9B 1.304(14) . ? C8B H8B 0.9500 . ? C9B C10B 1.334(13) . ? C10B C11B 1.281(14) . ? C10B H10B 0.9500 . ? C11B C12B 1.442(14) . ? C11B H11B 0.9500 . ? C12B H12B 0.9500 . ? C13B C16B 1.37(2) . ? C13B N1B 1.474(13) . ? C13B C14B 1.55(2) . ? C13B H13B 1.0000 . ? C14B C15B 1.54(3) . ? C14B H14C 0.9900 . ? C14B H14D 0.9900 . ? C15B O3B 1.23(2) . ? C15B N2B 1.27(3) . ? C16B O5B 1.272(18) . ? C16B O4B 1.334(18) . ? N2B H2B1 0.8800 . ? N2B H2B2 0.8800 . ? C1C O1C 1.235(13) . ? C1C N1C 1.372(13) . ? C1C C2C 1.508(14) . ? C2C C3C 1.336(13) . ? C2C C6C 1.341(14) . ? C3C C4C 1.311(13) . ? C3C C9C 1.512(14) . ? C4C C12C 1.397(14) . ? C4C C5C 1.458(14) . ? C5C O2C 1.193(13) . ? C5C N1C 1.482(14) . ? C6C C7C 1.505(14) . ? C6C H6C 0.9500 . ? C7C C8C 1.373(15) . ? C7C H7C 0.9500 . ? C8C C9C 1.326(14) . ? C8C H8C 0.9500 . ? C9C C10C 1.355(14) . ? C10C C11C 1.282(14) . ? C10C H10C 0.9500 . ? C11C C12C 1.430(14) . ? C11C H11C 0.9500 . ? C12C H12C 0.9500 . ? C13C N1C 1.477(14) . ? C13C C16C 1.53(2) . ? C13C C14C 1.63(3) . ? C13C H13C 1.0000 . ? C14C C15C 1.55(3) . ? C14C H14E 0.9900 . ? C14C H14F 0.9900 . ? C15C O3C 1.18(2) . ? C15C N2C 1.29(2) . ? C16C O5C 1.266(17) . ? C16C O4C 1.290(17) . ? N2C H2C1 0.8800 . ? N2C H2C2 0.8800 . ? C1D O1D 1.236(13) . ? C1D N1D 1.371(13) . ? C1D C2D 1.511(13) . ? C2D C3D 1.329(13) . ? C2D C6D 1.354(14) . ? C3D C4D 1.317(13) . ? C3D C9D 1.466(13) . ? C4D C12D 1.410(14) . ? C4D C5D 1.448(14) . ? C5D O2D 1.201(14) . ? C5D N1D 1.456(14) . ? C6D C7D 1.473(15) . ? C6D H6D 0.9500 . ? C7D C8D 1.349(15) . ? C7D H7D 0.9500 . ? C8D C9D 1.312(14) . ? C8D H8D 0.9500 . ? C9D C10D 1.354(14) . ? C10D C11D 1.299(14) . ? C10D H10D 0.9500 . ? C11D C12D 1.427(14) . ? C11D H11D 0.9500 . ? C12D H12D 0.9500 . ? C13D C16D 1.43(2) . ? C13D N1D 1.457(13) . ? C13D C14D 1.533(11) . ? C13D H13D 1.0000 . ? C14D C15D 1.462(15) . ? C14D H14G 0.9900 . ? C14D H14H 0.9900 . ? C15D O3D 1.198(15) . ? C15D N2D 1.343(15) . ? N2D H2D1 0.8800 . ? N2D H2D2 0.8800 . ? C16D O5D 1.16(2) . ? C16D O4D 1.368(19) . ? C1E O1E 1.247(13) . ? C1E N1E 1.386(13) . ? C1E C2E 1.482(13) . ? C2E C3E 1.335(13) . ? C2E C6E 1.337(13) . ? C3E C4E 1.315(13) . ? C3E C9E 1.465(13) . ? C4E C12E 1.405(13) . ? C4E C5E 1.459(13) . ? C5E O2E 1.231(13) . ? C5E N1E 1.477(13) . ? C6E C7E 1.468(14) . ? C6E H6E 0.9500 . ? C7E C8E 1.347(15) . ? C7E H7E 0.9500 . ? C8E C9E 1.309(14) . ? C8E H8E 0.9500 . ? C9E C10E 1.357(13) . ? C10E C11E 1.287(13) . ? C10E H10E 0.9500 . ? C11E C12E 1.419(13) . ? C11E H11E 0.9500 . ? C12E H12E 0.9500 . ? C13E C14E 1.43(2) . ? C13E C16E 1.48(2) . ? C13E N1E 1.484(12) . ? C13E H13E 1.0000 . ? C14E C15E 1.62(3) . ? C14E H14I 0.9900 . ? C14E H14J 0.9900 . ? C15E O3E 1.05(2) . ? C15E N2E 1.44(3) . ? C16E O5E 1.259(16) . ? C16E O4E 1.312(17) . ? N2E H2E1 0.8800 . ? N2E H2E2 0.8800 . ? C1F O1F 1.245(13) . ? C1F N1F 1.369(13) . ? C1F C2F 1.486(13) . ? C2F C3F 1.331(13) . ? C2F C6F 1.345(13) . ? C3F C4F 1.310(13) . ? C3F C9F 1.501(14) . ? C4F C12F 1.387(13) . ? C4F C5F 1.468(14) . ? C5F O2F 1.190(13) . ? C5F N1F 1.456(13) . ? C6F C7F 1.474(14) . ? C6F H6F 0.9500 . ? C7F C8F 1.358(14) . ? C7F H7F 0.9500 . ? C8F C9F 1.308(14) . ? C8F H8F 0.9500 . ? C9F C10F 1.324(13) . ? C10F C11F 1.284(14) . ? C10F H10F 0.9500 . ? C11F C12F 1.430(14) . ? C11F H11F 0.9500 . ? C12F H12F 0.9500 . ? C13F C16F 1.45(2) . ? C13F N1F 1.464(13) . ? C13F C14F 1.55(2) . ? C13F H13F 1.0000 . ? C14F C15F 1.51(2) . ? C14F H14K 0.9900 . ? C14F H14L 0.9900 . ? C15F O3F 1.252(19) . ? C15F N2F 1.338(18) . ? C16F O5F 1.292(16) . ? C16F O4F 1.314(17) . ? N2F H2F1 0.8800 . ? N2F H2F2 0.8800 . ? C1H O1H 1.237(12) . ? C1H N1H 1.380(12) . ? C1H C2H 1.501(13) . ? C2H C3H 1.340(12) . ? C2H C6H 1.349(13) . ? C3H C4H 1.334(12) . ? C3H C9H 1.477(14) . ? C4H C12H 1.400(13) . ? C4H C5H 1.442(13) . ? C5H O2H 1.204(12) . ? C5H N1H 1.472(12) . ? C6H C7H 1.484(14) . ? C6H H6H 0.9500 . ? C7H C8H 1.356(14) . ? C7H H7H 0.9500 . ? C8H C9H 1.311(14) . ? C8H H8H 0.9500 . ? C9H C10H 1.344(14) . ? C10H C11H 1.287(14) . ? C10H H10H 0.9500 . ? C11H C12H 1.418(14) . ? C11H H11H 0.9500 . ? C12H H12H 0.9500 . ? C13H N1H 1.484(13) . ? C13H C14H 1.599(15) . ? C13H C16H 1.62(2) . ? C13H H13H 1.0000 . ? C14H C15H 1.49(3) . ? C14H H14M 0.9900 . ? C14H H14N 0.9900 . ? C15H O3H 1.251(17) . ? C15H N2H 1.379(17) . ? N2H H2H1 0.8800 . ? N2H H2H2 0.8800 . ? C16H O5H 1.227(17) . ? C16H O4H 1.251(17) . ? N3I C21I 1.3900 . ? N3I C25I 1.3900 . ? C21I C22I 1.3900 . ? C21I H21I 0.9500 . ? C22I C23I 1.3900 . ? C22I H22I 0.9500 . ? C23I C24I 1.3900 . ? C23I H23I 0.9500 . ? C24I C25I 1.3900 . ? C24I H24I 0.9500 . ? C25I H25I 0.9500 . ? N3J C21J 1.3900 . ? N3J C25J 1.3900 . ? C21J C22J 1.3900 . ? C21J H21J 0.9500 . ? C22J C23J 1.3900 . ? C22J H22J 0.9500 . ? C23J C24J 1.3900 . ? C23J H23J 0.9500 . ? C24J C25J 1.3900 . ? C24J H24J 0.9500 . ? C25J H25J 0.9500 . ? O36 C31 1.21(3) . ? O37 C31 1.521(16) . ? O37 C32 1.555(15) . ? O38 C34 1.40(3) . ? C31 C34 1.54(3) . ? C32 C33 1.574(16) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.47(2) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4C Cu1 O4A 174.8(5) . . ? O4C Cu1 O4B 91.0(5) . . ? O4A Cu1 O4B 90.1(5) . . ? O4C Cu1 O4D 89.8(5) . . ? O4A Cu1 O4D 87.1(5) . . ? O4B Cu1 O4D 155.8(4) . . ? O4C Cu1 N3J 86.5(8) . . ? O4A Cu1 N3J 98.4(8) . . ? O4B Cu1 N3J 97.0(9) . . ? O4D Cu1 N3J 107.2(9) . . ? O4C Cu1 N3I 96.0(8) . . ? O4A Cu1 N3I 88.9(8) . . ? O4B Cu1 N3I 96.0(10) . . ? O4D Cu1 N3I 108.0(10) . . ? N3J Cu1 N3I 9.6(13) . . ? O4C Cu1 Cu2 86.9(4) . . ? O4A Cu1 Cu2 88.3(4) . . ? O4B Cu1 Cu2 78.7(3) . . ? O4D Cu1 Cu2 77.1(3) . . ? N3J Cu1 Cu2 172.1(8) . . ? N3I Cu1 Cu2 174.0(8) . . ? O5B Cu2 O5D 174.8(5) . . ? O5B Cu2 O5C 92.9(5) . . ? O5D Cu2 O5C 87.7(5) . . ? O5B Cu2 O5A 89.8(5) . . ? O5D Cu2 O5A 87.8(5) . . ? O5C Cu2 O5A 158.6(5) . . ? O5B Cu2 O3E 90.8(5) . . ? O5D Cu2 O3E 94.0(5) . . ? O5C Cu2 O3E 105.3(5) . . ? O5A Cu2 O3E 95.9(5) . . ? O5B Cu2 Cu1 87.3(3) . . ? O5D Cu2 Cu1 87.7(4) . . ? O5C Cu2 Cu1 80.0(3) . . ? O5A Cu2 Cu1 78.9(4) . . ? O3E Cu2 Cu1 174.4(4) . . ? O4G Cu3 O4F 94.1(4) . . ? O4G Cu3 O4H 89.3(4) . . ? O4F Cu3 O4H 166.9(5) . . ? O4G Cu3 O4E 172.5(5) . . ? O4F Cu3 O4E 89.6(4) . . ? O4H Cu3 O4E 85.7(4) . . ? O4G Cu3 O36 93.2(5) . . ? O4F Cu3 O36 88.8(5) . . ? O4H Cu3 O36 103.6(5) . . ? O4E Cu3 O36 93.3(5) . . ? O4G Cu3 Cu4 82.8(3) . . ? O4F Cu3 Cu4 81.7(3) . . ? O4H Cu3 Cu4 86.2(3) . . ? O4E Cu3 Cu4 91.3(3) . . ? O36 Cu3 Cu4 169.4(4) . . ? O5H Cu4 O5F 170.1(4) . . ? O5H Cu4 O5E 89.9(4) . . ? O5F Cu4 O5E 84.7(4) . . ? O5H Cu4 O5G 88.6(4) . . ? O5F Cu4 O5G 94.4(4) . . ? O5E Cu4 O5G 164.5(4) . . ? O5H Cu4 O3Z 104.3(7) . . ? O5F Cu4 O3Z 85.2(7) . . ? O5E Cu4 O3Z 104.1(7) . . ? O5G Cu4 O3Z 91.2(7) . . ? O5H Cu4 O3A 94.3(8) . . ? O5F Cu4 O3A 94.1(7) . . ? O5E Cu4 O3A 90.7(7) . . ? O5G Cu4 O3A 104.8(7) . . ? O3Z Cu4 O3A 16.9(9) . . ? O5H Cu4 Cu3 83.2(3) . . ? O5F Cu4 Cu3 87.6(3) . . ? O5E Cu4 Cu3 79.3(3) . . ? O5G Cu4 Cu3 85.2(3) . . ? O3Z Cu4 Cu3 171.7(6) . . ? O3A Cu4 Cu3 169.7(7) . . ? O1G C1G N1G 117.4(12) . . ? O1G C1G C2G 124.4(12) . . ? N1G C1G C2G 117.7(11) . . ? C3G C2G C6G 125.9(12) . . ? C3G C2G C1G 120.8(12) . . ? C6G C2G C1G 112.4(11) . . ? C4G C3G C2G 120.8(13) . . ? C4G C3G C9G 119.4(11) . . ? C2G C3G C9G 119.8(11) . . ? C3G C4G C12G 124.8(12) . . ? C3G C4G C5G 124.4(12) . . ? C12G C4G C5G 110.7(11) . . ? O2G C5G C4G 133.6(13) . . ? O2G C5G N1G 111.4(12) . . ? C4G C5G N1G 114.6(11) . . ? C2G C6G C7G 115.8(12) . . ? C2G C6G H6G 122.1 . . ? C7G C6G H6G 122.1 . . ? C8G C7G C6G 115.1(13) . . ? C8G C7G H7G 122.5 . . ? C6G C7G H7G 122.5 . . ? C9G C8G C7G 131.6(14) . . ? C9G C8G H8G 114.2 . . ? C7G C8G H8G 114.2 . . ? C10G C9G C8G 136.5(15) . . ? C10G C9G C3G 111.8(12) . . ? C8G C9G C3G 111.5(12) . . ? C11G C10G C9G 129.9(15) . . ? C11G C10G H10G 115.0 . . ? C9G C10G H10G 115.0 . . ? C10G C11G C12G 119.5(14) . . ? C10G C11G H11G 120.2 . . ? C12G C11G H11G 120.2 . . ? C4G C12G C11G 114.2(12) . . ? C4G C12G H12G 122.9 . . ? C11G C12G H12G 122.9 . . ? N1G C13G C16G 119.1(14) . . ? N1G C13G C14G 103.6(13) . . ? C16G C13G C14G 112.9(14) . . ? N1G C13G H13G 106.8 . . ? C16G C13G H13G 106.8 . . ? C14G C13G H13G 106.8 . . ? C1G N1G C13G 119.6(11) . . ? C1G N1G C5G 120.7(11) . . ? C13G N1G C5G 119.5(11) . . ? C15G C14G C13G 111.1(17) . . ? C15G C14G H14O 109.4 . . ? C13G C14G H14O 109.4 . . ? C15G C14G H14P 109.4 . . ? C13G C14G H14P 109.4 . . ? H14O C14G H14P 108.0 . . ? O3G C15G N2G 118(2) . . ? O3G C15G C14G 124(2) . . ? N2G C15G C14G 116(2) . . ? O5G C16G O4G 124.9(18) . . ? O5G C16G C13G 123.2(17) . . ? O4G C16G C13G 111.8(16) . . ? C15G N2G H2G1 120.0 . . ? C15G N2G H2G2 120.0 . . ? H2G1 N2G H2G2 120.0 . . ? C16G O4G Cu3 125.0(11) . . ? C16G O5G Cu4 120.1(12) . . ? O1A C1A N1A 116.5(18) . . ? O1A C1A C2A 127.5(19) . . ? N1A C1A C2A 116.0(18) . . ? C3A C2A C6A 129.8(16) . . ? C3A C2A C1A 119.6(17) . . ? C6A C2A C1A 110.6(14) . . ? C2A C3A C4A 120.9(18) . . ? C2A C3A C9A 116.0(14) . . ? C4A C3A C9A 123.1(15) . . ? C3A C4A C12A 124.9(16) . . ? C3A C4A C5A 125.2(18) . . ? C12A C4A C5A 109.7(15) . . ? O2A C5A N1A 117.3(18) . . ? O2A C5A C4A 125.2(18) . . ? N1A C5A C4A 117(2) . . ? C2A C6A C7A 115.6(16) . . ? C2A C6A H6A 122.2 . . ? C7A C6A H6A 122.2 . . ? C8A C7A C6A 110.5(17) . . ? C8A C7A H7A 124.7 . . ? C6A C7A H7A 124.7 . . ? C9A C8A C7A 135(2) . . ? C9A C8A H8A 112.3 . . ? C7A C8A H8A 112.3 . . ? C10A C9A C8A 141(2) . . ? C10A C9A C3A 107.1(16) . . ? C8A C9A C3A 111.9(17) . . ? C11A C10A C9A 133(2) . . ? C11A C10A H10A 113.5 . . ? C9A C10A H10A 113.5 . . ? C10A C11A C12A 121.1(18) . . ? C10A C11A H11A 119.5 . . ? C12A C11A H11A 119.5 . . ? C4A C12A C11A 110.4(16) . . ? C4A C12A H12A 124.8 . . ? C11A C12A H12A 124.8 . . ? C5A N1A C1A 121(2) . . ? C5A N1A C13A 120.2(14) . . ? C1A N1A C13A 117.7(12) . . ? C16A O4A Cu1 119.5(14) . . ? C16A O5A Cu2 127.6(14) . . ? O5A C16A O4A 124(2) . . ? O5A C16A C13A 122(2) . . ? O4A C16A C13A 113.7(19) . . ? C16A C13A N1A 112.1(15) . . ? C16A C13A C14A 106.1(19) . . ? N1A C13A C14A 105.4(15) . . ? C16A C13A H13A 111.0 . . ? N1A C13A H13A 111.0 . . ? C14A C13A H13A 111.0 . . ? C15A C14A C13A 122(2) . . ? C15A C14A H14A 106.8 . . ? C13A C14A H14A 106.8 . . ? C15A C14A H14B 106.8 . . ? C13A C14A H14B 106.8 . . ? H14A C14A H14B 106.6 . . ? O3A C15A N2A 114(2) . . ? O3A C15A C14A 125(2) . . ? N2A C15A C14A 120(2) . . ? C15A N2A H2A1 120.0 . . ? C15A N2A H2A2 120.0 . . ? H2A1 N2A H2A2 120.0 . . ? C15A O3A Cu4 137.1(18) . . ? C15Z C14Z H14Y 107.0 . . ? C15Z C14Z H14Z 107.0 . . ? H14Y C14Z H14Z 106.7 . . ? O3Z C15Z N2Z 145(2) . . ? O3Z C15Z C14Z 100.6(16) . . ? N2Z C15Z C14Z 114(2) . . ? C15Z N2Z H2Z1 120.0 . . ? C15Z N2Z H2Z2 120.0 . . ? H2Z1 N2Z H2Z2 120.0 . . ? C15Z O3Z Cu4 113.8(15) . . ? O1B C1B N1B 119.1(14) . . ? O1B C1B C2B 122.7(14) . . ? N1B C1B C2B 117.1(13) . . ? C3B C2B C6B 124.7(14) . . ? C3B C2B C1B 120.8(13) . . ? C6B C2B C1B 114.4(13) . . ? C4B C3B C2B 121.7(14) . . ? C4B C3B C9B 117.4(13) . . ? C2B C3B C9B 120.6(13) . . ? C3B C4B C12B 125.5(14) . . ? C3B C4B C5B 123.4(13) . . ? C12B C4B C5B 111.0(13) . . ? O2B C5B C4B 130.2(15) . . ? O2B C5B N1B 111.6(13) . . ? C4B C5B N1B 114.0(12) . . ? C2B C6B C7B 116.6(14) . . ? C2B C6B H6B 121.7 . . ? C7B C6B H6B 121.7 . . ? C8B C7B C6B 114.7(15) . . ? C8B C7B H7B 122.6 . . ? C6B C7B H7B 122.6 . . ? C9B C8B C7B 132.5(16) . . ? C9B C8B H8B 113.7 . . ? C7B C8B H8B 113.7 . . ? C8B C9B C10B 136.1(16) . . ? C8B C9B C3B 110.7(13) . . ? C10B C9B C3B 113.2(14) . . ? C11B C10B C9B 131.7(16) . . ? C11B C10B H10B 114.1 . . ? C9B C10B H10B 114.1 . . ? C10B C11B C12B 115.4(15) . . ? C10B C11B H11B 122.3 . . ? C12B C11B H11B 122.3 . . ? C4B C12B C11B 116.3(14) . . ? C4B C12B H12B 121.8 . . ? C11B C12B H12B 121.8 . . ? C16B C13B N1B 113.0(16) . . ? C16B C13B C14B 113.1(16) . . ? N1B C13B C14B 108.6(16) . . ? C16B C13B H13B 107.3 . . ? N1B C13B H13B 107.3 . . ? C14B C13B H13B 107.3 . . ? C1B N1B C5B 120.2(12) . . ? C1B N1B C13B 117.7(13) . . ? C5B N1B C13B 121.3(13) . . ? C15B C14B C13B 113.5(17) . . ? C15B C14B H14C 108.9 . . ? C13B C14B H14C 108.9 . . ? C15B C14B H14D 108.9 . . ? C13B C14B H14D 108.9 . . ? H14C C14B H14D 107.7 . . ? O3B C15B N2B 127(3) . . ? O3B C15B C14B 120(2) . . ? N2B C15B C14B 113(2) . . ? O5B C16B O4B 116.4(17) . . ? O5B C16B C13B 125.2(18) . . ? O4B C16B C13B 117.6(18) . . ? C15B N2B H2B1 120.0 . . ? C15B N2B H2B2 120.0 . . ? H2B1 N2B H2B2 120.0 . . ? C16B O4B Cu1 129.2(11) . . ? C16B O5B Cu2 128.1(12) . . ? O1C C1C N1C 120.1(14) . . ? O1C C1C C2C 123.0(14) . . ? N1C C1C C2C 116.8(13) . . ? C3C C2C C6C 126.1(15) . . ? C3C C2C C1C 119.8(14) . . ? C6C C2C C1C 113.8(14) . . ? C4C C3C C2C 122.7(15) . . ? C4C C3C C9C 117.2(14) . . ? C2C C3C C9C 120.0(14) . . ? C3C C4C C12C 126.3(15) . . ? C3C C4C C5C 124.3(15) . . ? C12C C4C C5C 109.4(14) . . ? O2C C5C C4C 133.1(16) . . ? O2C C5C N1C 113.1(14) . . ? C4C C5C N1C 112.5(13) . . ? C2C C6C C7C 116.5(15) . . ? C2C C6C H6C 121.8 . . ? C7C C6C H6C 121.8 . . ? C8C C7C C6C 111.9(15) . . ? C8C C7C H7C 124.0 . . ? C6C C7C H7C 124.0 . . ? C9C C8C C7C 132.3(18) . . ? C9C C8C H8C 113.8 . . ? C7C C8C H8C 113.8 . . ? C8C C9C C10C 135.4(17) . . ? C8C C9C C3C 109.6(14) . . ? C10C C9C C3C 114.4(14) . . ? C11C C10C C9C 126.1(17) . . ? C11C C10C H10C 116.9 . . ? C9C C10C H10C 116.9 . . ? C10C C11C C12C 121.9(16) . . ? C10C C11C H11C 119.0 . . ? C12C C11C H11C 119.0 . . ? C4C C12C C11C 113.2(15) . . ? C4C C12C H12C 123.4 . . ? C11C C12C H12C 123.4 . . ? N1C C13C C16C 111.9(18) . . ? N1C C13C C14C 113.8(18) . . ? C16C C13C C14C 105.8(16) . . ? N1C C13C H13C 108.4 . . ? C16C C13C H13C 108.4 . . ? C14C C13C H13C 108.4 . . ? C1C N1C C13C 119.5(14) . . ? C1C N1C C5C 122.7(14) . . ? C13C N1C C5C 116.8(14) . . ? C15C C14C C13C 110.3(19) . . ? C15C C14C H14E 109.6 . . ? C13C C14C H14E 109.6 . . ? C15C C14C H14F 109.6 . . ? C13C C14C H14F 109.6 . . ? H14E C14C H14F 108.1 . . ? O3C C15C N2C 128(2) . . ? O3C C15C C14C 117(2) . . ? N2C C15C C14C 115(2) . . ? O5C C16C O4C 123.3(17) . . ? O5C C16C C13C 120.6(16) . . ? O4C C16C C13C 116.1(16) . . ? C15C N2C H2C1 120.0 . . ? C15C N2C H2C2 120.0 . . ? H2C1 N2C H2C2 120.0 . . ? C16C O4C Cu1 122.0(11) . . ? C16C O5C Cu2 127.4(11) . . ? O1D C1D N1D 119.4(14) . . ? O1D C1D C2D 123.1(14) . . ? N1D C1D C2D 117.2(13) . . ? C3D C2D C6D 122.6(14) . . ? C3D C2D C1D 120.9(13) . . ? C6D C2D C1D 116.5(13) . . ? C4D C3D C2D 121.6(14) . . ? C4D C3D C9D 116.1(13) . . ? C2D C3D C9D 122.3(13) . . ? C3D C4D C12D 127.3(14) . . ? C3D C4D C5D 123.2(14) . . ? C12D C4D C5D 109.5(13) . . ? O2D C5D C4D 129.8(16) . . ? O2D C5D N1D 113.7(15) . . ? C4D C5D N1D 116.2(13) . . ? C2D C6D C7D 117.3(15) . . ? C2D C6D H6D 121.3 . . ? C7D C6D H6D 121.3 . . ? C8D C7D C6D 115.0(16) . . ? C8D C7D H7D 122.5 . . ? C6D C7D H7D 122.5 . . ? C9D C8D C7D 130.0(17) . . ? C9D C8D H8D 115.0 . . ? C7D C8D H8D 115.0 . . ? C8D C9D C10D 132.7(16) . . ? C8D C9D C3D 112.0(14) . . ? C10D C9D C3D 114.6(14) . . ? C11D C10D C9D 129.4(17) . . ? C11D C10D H10D 115.3 . . ? C9D C10D H10D 115.3 . . ? C10D C11D C12D 117.4(16) . . ? C10D C11D H11D 121.3 . . ? C12D C11D H11D 121.3 . . ? C4D C12D C11D 114.2(15) . . ? C4D C12D H12D 122.9 . . ? C11D C12D H12D 122.9 . . ? C16D C13D N1D 117.5(16) . . ? C16D C13D C14D 104.0(15) . . ? N1D C13D C14D 108.6(16) . . ? C16D C13D H13D 108.8 . . ? N1D C13D H13D 108.8 . . ? C14D C13D H13D 108.8 . . ? C1D N1D C5D 120.6(12) . . ? C1D N1D C13D 118.0(13) . . ? C5D N1D C13D 121.4(13) . . ? C15D C14D C13D 128.9(15) . . ? C15D C14D H14G 105.1 . . ? C13D C14D H14G 105.1 . . ? C15D C14D H14H 105.1 . . ? C13D C14D H14H 105.1 . . ? H14G C14D H14H 105.9 . . ? O3D C15D N2D 118.0(17) . . ? O3D C15D C14D 130.3(19) . . ? N2D C15D C14D 111.6(19) . . ? C15D N2D H2D1 120.0 . . ? C15D N2D H2D2 120.0 . . ? H2D1 N2D H2D2 120.0 . . ? O5D C16D O4D 118(2) . . ? O5D C16D C13D 133(2) . . ? O4D C16D C13D 109.5(18) . . ? C16D O4D Cu1 128.6(12) . . ? C16D O5D Cu2 128.6(15) . . ? O1E C1E N1E 116.7(13) . . ? O1E C1E C2E 125.1(13) . . ? N1E C1E C2E 118.1(12) . . ? C3E C2E C6E 121.5(13) . . ? C3E C2E C1E 122.5(12) . . ? C6E C2E C1E 116.0(12) . . ? C4E C3E C2E 118.9(13) . . ? C4E C3E C9E 119.2(12) . . ? C2E C3E C9E 121.9(12) . . ? C3E C4E C12E 123.0(13) . . ? C3E C4E C5E 126.0(13) . . ? C12E C4E C5E 110.5(12) . . ? O2E C5E C4E 132.5(14) . . ? O2E C5E N1E 112.4(12) . . ? C4E C5E N1E 114.0(12) . . ? C2E C6E C7E 117.9(14) . . ? C2E C6E H6E 121.1 . . ? C7E C6E H6E 121.1 . . ? C8E C7E C6E 117.3(16) . . ? C8E C7E H7E 121.4 . . ? C6E C7E H7E 121.4 . . ? C9E C8E C7E 126.1(16) . . ? C9E C8E H8E 117.0 . . ? C7E C8E H8E 117.0 . . ? C8E C9E C10E 129.8(15) . . ? C8E C9E C3E 114.4(13) . . ? C10E C9E C3E 114.6(13) . . ? C11E C10E C9E 126.8(15) . . ? C11E C10E H10E 116.6 . . ? C9E C10E H10E 116.6 . . ? C10E C11E C12E 119.1(14) . . ? C10E C11E H11E 120.5 . . ? C12E C11E H11E 120.5 . . ? C4E C12E C11E 116.5(13) . . ? C4E C12E H12E 121.7 . . ? C11E C12E H12E 121.7 . . ? C14E C13E C16E 117.0(16) . . ? C14E C13E N1E 109.4(15) . . ? C16E C13E N1E 113.6(13) . . ? C14E C13E H13E 105.2 . . ? C16E C13E H13E 105.2 . . ? N1E C13E H13E 105.2 . . ? C1E N1E C5E 119.8(11) . . ? C1E N1E C13E 116.8(11) . . ? C5E N1E C13E 123.4(11) . . ? C13E C14E C15E 120.6(19) . . ? C13E C14E H14I 107.2 . . ? C15E C14E H14I 107.2 . . ? C13E C14E H14J 107.2 . . ? C15E C14E H14J 107.2 . . ? H14I C14E H14J 106.8 . . ? O3E C15E N2E 118(3) . . ? O3E C15E C14E 128(3) . . ? N2E C15E C14E 113(2) . . ? O5E C16E O4E 125.1(15) . . ? O5E C16E C13E 116.7(15) . . ? O4E C16E C13E 118.2(15) . . ? C15E N2E H2E1 120.0 . . ? C15E N2E H2E2 120.0 . . ? H2E1 N2E H2E2 120.0 . . ? C15E O3E Cu2 138.0(19) . . ? C16E O4E Cu3 114.5(10) . . ? C16E O5E Cu4 129.9(11) . . ? O1F C1F N1F 117.7(13) . . ? O1F C1F C2F 125.8(13) . . ? N1F C1F C2F 116.5(12) . . ? C3F C2F C6F 122.3(13) . . ? C3F C2F C1F 122.8(13) . . ? C6F C2F C1F 114.7(13) . . ? C4F C3F C2F 120.0(13) . . ? C4F C3F C9F 117.1(12) . . ? C2F C3F C9F 122.7(13) . . ? C3F C4F C12F 124.1(13) . . ? C3F C4F C5F 124.1(13) . . ? C12F C4F C5F 111.7(13) . . ? O2F C5F N1F 113.4(13) . . ? O2F C5F C4F 131.6(14) . . ? N1F C5F C4F 114.7(12) . . ? C2F C6F C7F 115.6(13) . . ? C2F C6F H6F 122.2 . . ? C7F C6F H6F 122.2 . . ? C8F C7F C6F 120.2(14) . . ? C8F C7F H7F 119.9 . . ? C6F C7F H7F 119.9 . . ? C9F C8F C7F 125.2(15) . . ? C9F C8F H8F 117.4 . . ? C7F C8F H8F 117.4 . . ? C8F C9F C10F 131.5(15) . . ? C8F C9F C3F 113.3(13) . . ? C10F C9F C3F 115.1(13) . . ? C11F C10F C9F 128.4(16) . . ? C11F C10F H10F 115.8 . . ? C9F C10F H10F 115.8 . . ? C10F C11F C12F 117.6(15) . . ? C10F C11F H11F 121.2 . . ? C12F C11F H11F 121.2 . . ? C4F C12F C11F 116.9(14) . . ? C4F C12F H12F 121.5 . . ? C11F C12F H12F 121.5 . . ? C16F C13F N1F 116.0(15) . . ? C16F C13F C14F 119.1(15) . . ? N1F C13F C14F 106.8(15) . . ? C16F C13F H13F 104.4 . . ? N1F C13F H13F 104.4 . . ? C14F C13F H13F 104.4 . . ? C1F N1F C5F 121.8(12) . . ? C1F N1F C13F 116.5(12) . . ? C5F N1F C13F 121.7(12) . . ? C15F C14F C13F 108.9(14) . . ? C15F C14F H14K 109.9 . . ? C13F C14F H14K 109.9 . . ? C15F C14F H14L 109.9 . . ? C13F C14F H14L 109.9 . . ? H14K C14F H14L 108.3 . . ? O3F C15F N2F 116.4(17) . . ? O3F C15F C14F 124.2(17) . . ? N2F C15F C14F 118.3(17) . . ? O5F C16F O4F 119.1(15) . . ? O5F C16F C13F 121.4(15) . . ? O4F C16F C13F 119.4(15) . . ? C15F N2F H2F1 120.0 . . ? C15F N2F H2F2 120.0 . . ? H2F1 N2F H2F2 120.0 . . ? C16F O4F Cu3 127.9(10) . . ? C16F O5F Cu4 122.6(11) . . ? O1H C1H N1H 119.4(12) . . ? O1H C1H C2H 122.8(12) . . ? N1H C1H C2H 117.6(12) . . ? C3H C2H C6H 123.3(13) . . ? C3H C2H C1H 120.9(12) . . ? C6H C2H C1H 115.6(12) . . ? C4H C3H C2H 121.0(12) . . ? C4H C3H C9H 118.4(12) . . ? C2H C3H C9H 120.7(12) . . ? C3H C4H C12H 122.7(13) . . ? C3H C4H C5H 123.8(12) . . ? C12H C4H C5H 112.6(12) . . ? O2H C5H C4H 132.5(14) . . ? O2H C5H N1H 111.6(12) . . ? C4H C5H N1H 115.6(11) . . ? C2H C6H C7H 117.2(13) . . ? C2H C6H H6H 121.4 . . ? C7H C6H H6H 121.4 . . ? C8H C7H C6H 115.9(14) . . ? C8H C7H H7H 122.1 . . ? C6H C7H H7H 122.1 . . ? C9H C8H C7H 128.5(16) . . ? C9H C8H H8H 115.8 . . ? C7H C8H H8H 115.8 . . ? C8H C9H C10H 131.5(16) . . ? C8H C9H C3H 114.1(14) . . ? C10H C9H C3H 114.4(14) . . ? C11H C10H C9H 128.8(17) . . ? C11H C10H H10H 115.6 . . ? C9H C10H H10H 115.6 . . ? C10H C11H C12H 117.6(15) . . ? C10H C11H H11H 121.2 . . ? C12H C11H H11H 121.2 . . ? C4H C12H C11H 117.7(14) . . ? C4H C12H H12H 121.2 . . ? C11H C12H H12H 121.2 . . ? N1H C13H C14H 113.3(14) . . ? N1H C13H C16H 108.8(13) . . ? C14H C13H C16H 112.5(14) . . ? N1H C13H H13H 107.3 . . ? C14H C13H H13H 107.3 . . ? C16H C13H H13H 107.3 . . ? C1H N1H C5H 120.7(11) . . ? C1H N1H C13H 118.3(12) . . ? C5H N1H C13H 121.0(11) . . ? C15H C14H C13H 108.0(14) . . ? C15H C14H H14M 110.1 . . ? C13H C14H H14M 110.1 . . ? C15H C14H H14N 110.1 . . ? C13H C14H H14N 110.1 . . ? H14M C14H H14N 108.4 . . ? O3H C15H N2H 124(3) . . ? O3H C15H C14H 126(2) . . ? N2H C15H C14H 110(2) . . ? C15H N2H H2H1 120.0 . . ? C15H N2H H2H2 120.0 . . ? H2H1 N2H H2H2 120.0 . . ? O5H C16H O4H 130.8(17) . . ? O5H C16H C13H 117.8(16) . . ? O4H C16H C13H 111.5(15) . . ? C16H O4H Cu3 116.1(11) . . ? C16H O5H Cu4 123.3(11) . . ? C21I N3I C25I 120.0 . . ? C21I N3I Cu1 121.0(14) . . ? C25I N3I Cu1 119.0(14) . . ? N3I C21I C22I 120.0 . . ? N3I C21I H21I 120.0 . . ? C22I C21I H21I 120.0 . . ? C21I C22I C23I 120.0 . . ? C21I C22I H22I 120.0 . . ? C23I C22I H22I 120.0 . . ? C24I C23I C22I 120.0 . . ? C24I C23I H23I 120.0 . . ? C22I C23I H23I 120.0 . . ? C25I C24I C23I 120.0 . . ? C25I C24I H24I 120.0 . . ? C23I C24I H24I 120.0 . . ? C24I C25I N3I 120.0 . . ? C24I C25I H25I 120.0 . . ? N3I C25I H25I 120.0 . . ? C21J N3J C25J 120.0 . . ? C21J N3J Cu1 118.7(14) . . ? C25J N3J Cu1 120.0(14) . . ? N3J C21J C22J 120.0 . . ? N3J C21J H21J 120.0 . . ? C22J C21J H21J 120.0 . . ? C23J C22J C21J 120.0 . . ? C23J C22J H22J 120.0 . . ? C21J C22J H22J 120.0 . . ? C24J C23J C22J 120.0 . . ? C24J C23J H23J 120.0 . . ? C22J C23J H23J 120.0 . . ? C23J C24J C25J 120.0 . . ? C23J C24J H24J 120.0 . . ? C25J C24J H24J 120.0 . . ? C24J C25J N3J 120.0 . . ? C24J C25J H25J 120.0 . . ? N3J C25J H25J 120.0 . . ? C31 O36 Cu3 119.2(18) . . ? C31 O37 C32 111.5(17) . . ? O36 C31 O37 119(2) . . ? O36 C31 C34 140(2) . . ? O37 C31 C34 99.0(19) . . ? O37 C32 C33 108.2(17) . . ? O37 C32 H32A 110.1 . . ? C33 C32 H32A 110.1 . . ? O37 C32 H32B 110.1 . . ? C33 C32 H32B 110.1 . . ? H32A C32 H32B 108.4 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O38 C34 C35 113(2) . . ? O38 C34 C31 98.3(19) . . ? C35 C34 C31 122(2) . . ? O38 C34 H34 107.6 . . ? C35 C34 H34 107.6 . . ? C31 C34 H34 107.6 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4C Cu1 Cu2 O5B -92.0(5) . . . . ? O4A Cu1 Cu2 O5B 90.0(5) . . . . ? O4B Cu1 Cu2 O5B -0.4(4) . . . . ? O4D Cu1 Cu2 O5B 177.5(5) . . . . ? O4C Cu1 Cu2 O5D 89.5(5) . . . . ? O4A Cu1 Cu2 O5D -88.5(5) . . . . ? O4B Cu1 Cu2 O5D -178.9(5) . . . . ? O4D Cu1 Cu2 O5D -1.1(5) . . . . ? O4C Cu1 Cu2 O5C 1.4(5) . . . . ? O4A Cu1 Cu2 O5C -176.6(5) . . . . ? O4B Cu1 Cu2 O5C 93.0(4) . . . . ? O4D Cu1 Cu2 O5C -89.1(5) . . . . ? O4C Cu1 Cu2 O5A 177.7(5) . . . . ? O4A Cu1 Cu2 O5A -0.3(5) . . . . ? O4B Cu1 Cu2 O5A -90.7(5) . . . . ? O4D Cu1 Cu2 O5A 87.2(5) . . . . ? O4G Cu3 Cu4 O5H 85.5(4) . . . . ? O4F Cu3 Cu4 O5H -179.3(4) . . . . ? O4H Cu3 Cu4 O5H -4.2(4) . . . . ? O4E Cu3 Cu4 O5H -89.9(4) . . . . ? O4G Cu3 Cu4 O5F -98.3(4) . . . . ? O4F Cu3 Cu4 O5F -3.1(4) . . . . ? O4H Cu3 Cu4 O5F 171.9(4) . . . . ? O4E Cu3 Cu4 O5F 86.3(4) . . . . ? O4G Cu3 Cu4 O5E 176.7(5) . . . . ? O4F Cu3 Cu4 O5E -88.1(4) . . . . ? O4H Cu3 Cu4 O5E 86.9(4) . . . . ? O4E Cu3 Cu4 O5E 1.3(5) . . . . ? O36 Cu3 Cu4 O5E -114(2) . . . . ? O4G Cu3 Cu4 O5G -3.7(4) . . . . ? O4F Cu3 Cu4 O5G 91.6(4) . . . . ? O4H Cu3 Cu4 O5G -93.4(4) . . . . ? O4E Cu3 Cu4 O5G -179.0(4) . . . . ? O1G C1G C2G C3G 179.8(19) . . . . ? N1G C1G C2G C3G 8(3) . . . . ? O1G C1G C2G C6G -10(3) . . . . ? N1G C1G C2G C6G 178.4(16) . . . . ? C6G C2G C3G C4G -179.0(19) . . . . ? C1G C2G C3G C9G 170.6(17) . . . . ? C9G C3G C4G C5G -177.9(19) . . . . ? C12G C4G C5G N1G -175.9(16) . . . . ? C1G C2G C6G C7G -173.3(15) . . . . ? C4G C3G C9G C8G -175.8(19) . . . . ? C5G C4G C12G C11G 176.8(17) . . . . ? C2G C1G N1G C13G 176.7(15) . . . . ? O1G C1G N1G C5G -171.2(16) . . . . ? C14G C13G N1G C1G -78.7(18) . . . . ? C16G C13G N1G C5G -136.4(17) . . . . ? C14G C13G N1G C5G 97.2(17) . . . . ? O2G C5G N1G C1G 179.0(16) . . . . ? C4G C5G N1G C13G 176.8(15) . . . . ? N1G C13G C14G C15G -160.6(16) . . . . ? C13G C14G C15G N2G -148.5(19) . . . . ? N1G C13G C16G O5G -134.3(18) . . . . ? C14G C13G C16G O4G 171.4(14) . . . . ? C13G C16G O4G Cu3 -170.1(10) . . . . ? O4F Cu3 O4G C16G -83.8(13) . . . . ? O4H Cu3 O4G C16G 83.5(13) . . . . ? O36 Cu3 O4G C16G -172.9(14) . . . . ? Cu4 Cu3 O4G C16G -2.8(13) . . . . ? C13G C16G O5G Cu4 166.1(12) . . . . ? O5H Cu4 O5G C16G -71.4(13) . . . . ? O5F Cu4 O5G C16G 99.1(14) . . . . ? O3Z Cu4 O5G C16G -175.7(15) . . . . ? O3A Cu4 O5G C16G -165.5(15) . . . . ? Cu3 Cu4 O5G C16G 11.9(13) . . . . ? O1A C1A C2A C3A 179.7(19) . . . . ? N1A C1A C2A C3A -0.4(13) . . . . ? N1A C1A C2A C6A 178.5(18) . . . . ? C1A C2A C3A C4A -1.0(15) . . . . ? C1A C2A C3A C9A 178.3(14) . . . . ? C2A C3A C4A C12A 179.1(19) . . . . ? C1A C2A C6A C7A 176.8(16) . . . . ? C2A C3A C9A C10A -178.6(16) . . . . ? O2A C5A N1A C1A 176.9(19) . . . . ? C4A C5A N1A C13A 172.7(19) . . . . ? C2A C1A N1A C13A -170.0(13) . . . . ? O4B Cu1 O4A C16A 72.8(15) . . . . ? O4D Cu1 O4A C16A -83.1(15) . . . . ? N3J Cu1 O4A C16A 169.9(17) . . . . ? N3I Cu1 O4A C16A 168.8(17) . . . . ? Cu2 Cu1 O4A C16A -5.9(14) . . . . ? O5B Cu2 O5A C16A -80.0(17) . . . . ? O5D Cu2 O5A C16A 95.5(18) . . . . ? O3E Cu2 O5A C16A -170.7(17) . . . . ? Cu1 Cu2 O5A C16A 7.4(17) . . . . ? Cu2 O5A C16A C13A 170.1(12) . . . . ? Cu1 O4A C16A C13A -171.3(11) . . . . ? O5A C16A C13A N1A -152.1(17) . . . . ? O4A C16A C13A C14A 147.0(19) . . . . ? N1B C1B C2B C6B 172.7(19) . . . . ? C1B C2B C3B C9B -179.0(18) . . . . ? C9B C3B C4B C5B 178.0(19) . . . . ? C12B C4B C5B N1B -171.2(17) . . . . ? C1B C2B C6B C7B 178.2(18) . . . . ? C5B C4B C12B C11B 179.7(17) . . . . ? O1B C1B N1B C5B -174.2(18) . . . . ? C2B C1B N1B C13B -172.8(17) . . . . ? O2B C5B N1B C1B -177.1(18) . . . . ? C4B C5B N1B C13B 173.1(17) . . . . ? C16B C13B N1B C5B -141.9(18) . . . . ? N1B C13B C14B C15B -165.1(16) . . . . ? N1B C13B C16B O5B -139.2(17) . . . . ? C14B C13B C16B O4B 175.7(14) . . . . ? C13B C16B O4B Cu1 175.6(12) . . . . ? O4C Cu1 O4B C16B 84.1(13) . . . . ? O4A Cu1 O4B C16B -90.8(13) . . . . ? N3J Cu1 O4B C16B 170.7(15) . . . . ? N3I Cu1 O4B C16B -179.7(14) . . . . ? Cu2 Cu1 O4B C16B -2.6(12) . . . . ? C13B C16B O5B Cu2 -175.3(13) . . . . ? O5C Cu2 O5B C16B -76.1(14) . . . . ? O5A Cu2 O5B C16B 82.6(14) . . . . ? O3E Cu2 O5B C16B 178.5(14) . . . . ? Cu1 Cu2 O5B C16B 3.7(13) . . . . ? N1C C13C C14C C15C -52(3) . . . . ? C16C C13C C14C C15C -175.0(18) . . . . ? C13C C14C C15C O3C -44(3) . . . . ? C13C C14C C15C N2C 133(2) . . . . ? N1C C13C C16C O5C -158.0(16) . . . . ? C14C C13C C16C O4C 145.5(16) . . . . ? C13C C16C O4C Cu1 -171.8(12) . . . . ? O4B Cu1 O4C C16C -83.3(13) . . . . ? O4D Cu1 O4C C16C 72.5(13) . . . . ? N3J Cu1 O4C C16C 179.8(15) . . . . ? N3I Cu1 O4C C16C -179.4(15) . . . . ? Cu2 Cu1 O4C C16C -4.6(12) . . . . ? C13C C16C O5C Cu2 173.4(13) . . . . ? O5B Cu2 O5C C16C 88.3(14) . . . . ? O5D Cu2 O5C C16C -86.6(14) . . . . ? O3E Cu2 O5C C16C 179.9(13) . . . . ? Cu1 Cu2 O5C C16C 1.5(13) . . . . ? C1D C2D C3D C9D 179.0(18) . . . . ? C2D C1D N1D C13D -172.7(16) . . . . ? C4D C5D N1D C13D 173.1(18) . . . . ? C14D C13D C16D O4D 166.9(15) . . . . ? C13D C16D O4D Cu1 177.5(10) . . . . ? O4C Cu1 O4D C16D -86.3(14) . . . . ? O4A Cu1 O4D C16D 89.5(14) . . . . ? N3J Cu1 O4D C16D -172.6(15) . . . . ? N3I Cu1 O4D C16D 177.4(15) . . . . ? Cu2 Cu1 O4D C16D 0.6(13) . . . . ? C13D C16D O5D Cu2 -178.3(15) . . . . ? O5C Cu2 O5D C16D 82.4(17) . . . . ? O5A Cu2 O5D C16D -76.6(17) . . . . ? O3E Cu2 O5D C16D -172.4(17) . . . . ? Cu1 Cu2 O5D C16D 2.3(17) . . . . ? O1E C1E C2E C3E 177.5(13) . . . . ? N1E C1E C2E C3E 1.3(10) . . . . ? O1E C1E C2E C6E -0.9(15) . . . . ? N1E C1E C2E C6E -177.1(14) . . . . ? C6E C2E C3E C4E 177.0(16) . . . . ? C1E C2E C3E C4E -1.2(12) . . . . ? C6E C2E C3E C9E -4.5(15) . . . . ? C1E C2E C3E C9E 177.3(11) . . . . ? C2E C3E C4E C12E 177.0(14) . . . . ? C9E C3E C4E C5E -172.3(16) . . . . ? C3E C4E C5E O2E -176.9(19) . . . . ? C12E C4E C5E N1E 177.9(14) . . . . ? C1E C2E C6E C7E -177.4(14) . . . . ? C4E C3E C9E C8E -174.4(16) . . . . ? C2E C3E C9E C10E 175.7(12) . . . . ? C5E C4E C12E C11E 177.3(15) . . . . ? O1E C1E N1E C5E 177.6(13) . . . . ? C2E C1E N1E C5E -5.9(17) . . . . ? C2E C1E N1E C13E 176.0(10) . . . . ? O2E C5E N1E C1E 179.0(14) . . . . ? C4E C5E N1E C13E -172.3(15) . . . . ? C14E C13E N1E C1E -77.1(18) . . . . ? C16E C13E N1E C1E 55.7(19) . . . . ? C14E C13E N1E C5E 104.8(19) . . . . ? C16E C13E N1E C5E -122.3(17) . . . . ? N1E C13E C14E C15E -151.8(17) . . . . ? N1E C13E C16E O5E -152.4(14) . . . . ? C14E C13E C16E O4E 156.8(16) . . . . ? C14E C15E O3E Cu2 164.3(15) . . . . ? C13E C16E O4E Cu3 -178.5(11) . . . . ? O4F Cu3 O4E C16E 79.8(11) . . . . ? O4H Cu3 O4E C16E -88.0(11) . . . . ? O36 Cu3 O4E C16E 168.6(11) . . . . ? Cu4 Cu3 O4E C16E -1.9(11) . . . . ? C13E C16E O5E Cu4 -179.8(10) . . . . ? O5H Cu4 O5E C16E 82.0(14) . . . . ? O5F Cu4 O5E C16E -89.7(14) . . . . ? O3Z Cu4 O5E C16E -173.4(15) . . . . ? O3A Cu4 O5E C16E 176.2(15) . . . . ? Cu3 Cu4 O5E C16E -1.2(13) . . . . ? N1F C1F C2F C6F -171.7(18) . . . . ? C1F C2F C3F C9F -177.9(19) . . . . ? C2F C3F C4F C12F 177(2) . . . . ? C9F C3F C4F C5F 176.1(19) . . . . ? C3F C4F C5F O2F -173(2) . . . . ? C12F C4F C5F N1F -176.2(16) . . . . ? C1F C2F C6F C7F -179.9(17) . . . . ? C5F C4F C12F C11F -173.2(17) . . . . ? O1F C1F N1F C5F 178.6(18) . . . . ? C2F C1F N1F C13F 178.0(17) . . . . ? O2F C5F N1F C1F 174.6(18) . . . . ? C4F C5F N1F C13F -179.8(17) . . . . ? C16F C13F N1F C5F -124.1(18) . . . . ? C14F C13F N1F C5F 100.4(19) . . . . ? N1F C13F C14F C15F -160.3(13) . . . . ? C13F C14F C15F N2F -147.6(15) . . . . ? N1F C13F C16F O5F -146.1(15) . . . . ? C14F C13F C16F O4F 167.0(14) . . . . ? C13F C16F O4F Cu3 162.7(11) . . . . ? O4G Cu3 O4F C16F 91.9(12) . . . . ? O4E Cu3 O4F C16F -81.6(12) . . . . ? O36 Cu3 O4F C16F -174.9(13) . . . . ? Cu4 Cu3 O4F C16F 9.8(12) . . . . ? O4F C16F O5F Cu4 9.0(19) . . . . ? C13F C16F O5F Cu4 -167.7(12) . . . . ? O5E Cu4 O5F C16F 77.5(11) . . . . ? O5G Cu4 O5F C16F -86.9(12) . . . . ? O3Z Cu4 O5F C16F -177.8(13) . . . . ? O3A Cu4 O5F C16F 167.9(13) . . . . ? Cu3 Cu4 O5F C16F -1.9(11) . . . . ? O1H C1H C2H C3H -174.6(17) . . . . ? N1H C1H C2H C6H -174.0(16) . . . . ? C6H C2H C3H C4H 179.3(17) . . . . ? C1H C2H C3H C9H -176.1(17) . . . . ? C2H C3H C4H C12H -175.1(17) . . . . ? C9H C3H C4H C5H 173.8(17) . . . . ? C3H C4H C5H O2H 175.8(19) . . . . ? C12H C4H C5H N1H 172.5(15) . . . . ? C1H C2H C6H C7H -179.8(16) . . . . ? C4H C3H C9H C8H 178.7(18) . . . . ? C2H C3H C9H C10H 178.9(18) . . . . ? C5H C4H C12H C11H -173.6(17) . . . . ? O1H C1H N1H C5H 171.3(15) . . . . ? C2H C1H N1H C13H 174.2(15) . . . . ? O2H C5H N1H C1H -171.5(16) . . . . ? C4H C5H N1H C13H -176.1(15) . . . . ? C14H C13H N1H C5H 107.6(18) . . . . ? C16H C13H N1H C5H -126.5(16) . . . . ? C16H C13H C14H C15H 165.2(15) . . . . ? C13H C14H C15H O3H -61.3(15) . . . . ? C13H C14H C15H N2H 118.6(14) . . . . ? N1H C13H C16H O5H -127.2(15) . . . . ? N1H C13H C16H O4H 53.6(18) . . . . ? C14H C13H C16H O4H 179.9(15) . . . . ? C13H C16H O4H Cu3 177.2(9) . . . . ? O4G Cu3 O4H C16H -78.5(12) . . . . ? O4E Cu3 O4H C16H 95.9(12) . . . . ? O36 Cu3 O4H C16H -171.7(12) . . . . ? Cu4 Cu3 O4H C16H 4.4(11) . . . . ? C13H C16H O5H Cu4 177.2(9) . . . . ? O5E Cu4 O5H C16H -73.9(13) . . . . ? O5G Cu4 O5H C16H 90.7(13) . . . . ? O3Z Cu4 O5H C16H -178.4(13) . . . . ? O3A Cu4 O5H C16H -164.6(14) . . . . ? Cu3 Cu4 O5H C16H 5.4(12) . . . . ? O4C Cu1 N3I C21I 170.2(13) . . . . ? O4A Cu1 N3I C21I -11.4(14) . . . . ? O4B Cu1 N3I C21I 78.6(14) . . . . ? O4D Cu1 N3I C21I -98.0(14) . . . . ? O4C Cu1 N3I C25I -9.2(15) . . . . ? O4A Cu1 N3I C25I 169.2(15) . . . . ? O4B Cu1 N3I C25I -100.8(14) . . . . ? O4D Cu1 N3I C25I 82.5(15) . . . . ? O4C Cu1 N3J C21J 166.8(14) . . . . ? O4A Cu1 N3J C21J -14.8(14) . . . . ? O4B Cu1 N3J C21J 76.3(13) . . . . ? O4D Cu1 N3J C21J -104.4(13) . . . . ? O4C Cu1 N3J C25J -26.5(15) . . . . ? O4A Cu1 N3J C25J 151.8(14) . . . . ? O4B Cu1 N3J C25J -117.0(15) . . . . ? O4D Cu1 N3J C25J 62.3(16) . . . . ? O4G Cu3 O36 C31 117.8(19) . . . . ? O4F Cu3 O36 C31 23.8(19) . . . . ? O4H Cu3 O36 C31 -152.1(18) . . . . ? O4E Cu3 O36 C31 -65.7(19) . . . . ? C32 O37 C31 C34 -166.6(17) . . . . ? O37 C31 C34 O38 -173.5(17) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2A H2A1 O5E 0.88 2.30 3.03(3) 141.2 . N2A H2A1 O5F 0.88 2.62 3.18(3) 122.9 . N2A H2A2 O3B 0.88 2.33 3.16(3) 156.9 . N2Z H2Z1 O5H 0.88 2.45 3.12(3) 133.5 . N2Z H2Z2 O1D 0.88 2.22 2.94(3) 139.0 . N2B H2B1 O3F 0.88 2.15 2.99(2) 159.3 . N2E H2E1 O5D 0.88 2.16 2.91(2) 142.5 . N2E H2E2 O1H 0.88 2.05 2.85(2) 150.8 . N2F H2F1 O3B 0.88 1.99 2.86(2) 171.2 . N2H H2H2 O3D 0.88 2.12 2.88(3) 143.9 . N2G H2G1 O1C 0.88 2.18 2.99(2) 154.2 1_455 N2F H2F2 O3C 0.88 2.10 2.95(2) 164.3 1_455 N2C H2C1 O3Z 0.88 2.48 3.24(3) 145.1 1_655 N2C H2C2 O3G 0.88 2.22 3.09(2) 171.1 1_655 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 18.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.488 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.089 _vrf_THETM01_4 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: No diffraction observed at high angle due to extensive disorder and small crystal size. ; _vrf_PLAT023_4 ; PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6].. 18.00 Deg. RESPONSE: No diffraction observed at high angle due to extensive disorder and small crystal size. ; _vrf_PLAT201_4 ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 187 RESPONSE: Many atoms refined isotropically due to prevent physically unreasonable displacement parameters and a low data-to-parameter ratio. This is because of the moderate crystallinity and weak diffraction of the available crystals. ; _vrf_PLAT602_4 ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: Voids of volume 5877.7 cubic angstroms are present which are filled with disordered species. The disorder could not be successfully modeled. The Squeeze program was used to account for the diffusely scattering species in these regions. ; #===END