# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Dalgarno, Scott' _publ_contact_author_email S.J.Dalgarno@hw.ac.uk _publ_section_title ; Calixarene supported enneanuclear Cu(II) clusters ; loop_ _publ_author_name G.Karotsis S.Kennedy S.Dalgarno E.Brechin # Attachment '1.CIF.txt' data_GK2553 _database_code_depnum_ccdc_archive 'CCDC 766939' #TrackingRef '1.CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common GK2553 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C162 H237 Cl4 Cu10 O31 S12' _chemical_formula_weight 3842.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 34.3956(13) _cell_length_b 20.5605(7) _cell_length_c 28.6345(18) _cell_angle_alpha 90.00 _cell_angle_beta 115.4880(10) _cell_angle_gamma 90.00 _cell_volume 18279.2(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7917 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 23.08 _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.396 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8028 _exptl_absorpt_coefficient_mu 1.399 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6790 _exptl_absorpt_correction_T_max 0.8176 _exptl_absorpt_process_details Bruker-SADABS _exptl_special_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _diffrn_ambient_temperature 100(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 Nonius X8 Apex II CCD Diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54201 _diffrn_reflns_av_R_equivalents 0.0687 _diffrn_reflns_av_sigmaI/netI 0.0720 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 23.43 _reflns_number_total 13098 _reflns_number_gt 8883 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 2001)' _computing_publication_material 'local program' _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.Numerous restraints were applied to the model due to extensive disorder in co-crystallised solvent molecules, and in one ligated solvent position on a Cu centre. Due to this disorder, some atoms have been refined isotropically. Residual electron density is assocaited with badly disordered solvent molecules and maximum shifts are associated with H-torsion angle changes on a disordered solvent molecule. Although numerous restraints have been applied, the disorder has been restricted to solvent molecules and has been modelled appropriately. The difference in calculated and reported formulae is due to disorder that could not be modelled appropriately, and where the formula contains the entire molecule(s). ; _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^)+(0.0928P)^2^+121.1491P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13098 _refine_ls_number_parameters 1099 _refine_ls_number_restraints 213 _refine_ls_R_factor_all 0.1013 _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.1834 _refine_ls_wR_factor_gt 0.1595 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.084 _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 0.08833(3) 0.07310(4) 0.30112(3) 0.0188(2) Uani 1 1 d . . . Cl1 Cl 0.05355(6) 0.13385(9) 0.36288(7) 0.0254(4) Uani 1 1 d . . . S1 S 0.16643(6) 0.07878(10) 0.40538(7) 0.0312(5) Uani 1 1 d . . . O1 O 0.06157(15) -0.0131(2) 0.29427(18) 0.0236(11) Uani 1 1 d . . . C1 C 0.1023(2) -0.1004(4) 0.2811(3) 0.0263(18) Uani 1 1 d . . . Cu2 Cu 0.0000 -0.01582(6) 0.2500 0.0204(3) Uani 1 2 d S . . Cl2 Cl 0.28228(9) 0.32358(14) 0.47997(9) 0.0681(8) Uani 1 1 d . . . O2 O -0.01188(15) -0.0134(2) 0.31083(18) 0.0255(12) Uani 1 1 d . . . C2 C 0.1261(2) -0.1569(4) 0.3003(3) 0.0319(19) Uani 1 1 d . . . H2 H 0.1387 -0.1773 0.2803 0.038 Uiso 1 1 calc R . . Cu3 Cu -0.03014(3) 0.07193(4) 0.32552(3) 0.0199(2) Uani 1 1 d . . . S3 S 0.06399(7) 0.28650(12) 0.42794(9) 0.0217(6) Uani 0.75 1 d PD A 1 O3 O -0.06635(15) 0.1483(2) 0.31916(17) 0.0216(11) Uani 1 1 d . . . C3 C 0.1324(2) -0.1850(4) 0.3472(3) 0.033(2) Uani 1 1 d . . . Cu4 Cu -0.07172(3) 0.20952(4) 0.26477(3) 0.0189(2) Uani 1 1 d . . . S4 S 0.1008(3) 0.2840(5) 0.4196(4) 0.054(3) Uani 0.25 1 d PD A 2 O4 O -0.02638(14) 0.2637(2) 0.31596(17) 0.0222(11) Uani 1 1 d . . . C4 C 0.1128(2) -0.1550(4) 0.3745(3) 0.0292(18) Uani 1 1 d . . . H4 H 0.1159 -0.1738 0.4062 0.035 Uiso 1 1 calc R . . Cu5 Cu 0.02990(3) 0.25642(4) 0.31378(3) 0.0177(2) Uani 1 1 d . . . S5 S 0.13355(9) 0.02929(12) 0.57442(9) 0.0540(7) Uani 1 1 d D . . O5 O 0.07503(15) 0.2683(2) 0.28994(18) 0.0244(12) Uani 1 1 d . . . C5 C 0.0884(2) -0.0978(4) 0.3573(3) 0.0244(17) Uani 1 1 d . . . Cu6 Cu 0.2500 0.2500 0.5000 0.0509(5) Uani 1 2 d S . . S6 S 0.0114(4) -0.2789(5) 0.2773(4) 0.038(2) Uiso 0.25 1 d P . . O6 O 0.11358(14) 0.1518(2) 0.28606(17) 0.0223(11) Uani 1 1 d . . . C6 C 0.0841(2) -0.0703(4) 0.3112(3) 0.0265(18) Uani 1 1 d . . . O91 O 0.0487(10) -0.2974(16) 0.2609(13) 0.060(8) Uiso 0.25 1 d P . . O7 O 0.14134(15) 0.0418(2) 0.35522(18) 0.0250(12) Uani 1 1 d . . . C7 C 0.1614(3) -0.2445(5) 0.3697(4) 0.049(2) Uani 1 1 d . . . S8 S -0.18744(13) 0.3403(2) 0.31236(17) 0.0736(11) Uani 0.75 1 d PDU B 1 O8 O 0.03567(15) 0.0963(3) 0.24240(17) 0.0303(13) Uani 1 1 d . . . C8 C 0.2039(3) -0.2213(6) 0.4146(5) 0.083(4) Uani 1 1 d . . . H8A H 0.2224 -0.2589 0.4305 0.124 Uiso 1 1 calc R . . H8B H 0.1974 -0.1989 0.4406 0.124 Uiso 1 1 calc R . . H8C H 0.2188 -0.1913 0.4012 0.124 Uiso 1 1 calc R . . S9 S -0.2121(4) 0.3290(6) 0.2534(5) 0.070(3) Uani 0.25 1 d PDU C 2 C9 C 0.1715(4) -0.2804(5) 0.3301(4) 0.073(3) Uani 1 1 d . . . H9A H 0.1888 -0.3190 0.3462 0.110 Uiso 1 1 calc R . . H9B H 0.1877 -0.2518 0.3175 0.110 Uiso 1 1 calc R . . H9C H 0.1446 -0.2937 0.3011 0.110 Uiso 1 1 calc R . . S10 S 0.09406(19) 0.5212(3) 0.3892(2) 0.1154(18) Uiso 0.75 1 d PDU D 1 O10 O 0.06090(15) 0.3071(2) 0.37562(17) 0.0264(12) Uani 1 1 d . A . C10 C 0.1397(4) -0.2934(5) 0.3911(5) 0.075(3) Uani 1 1 d . . . H10A H 0.1138 -0.3109 0.3627 0.112 Uiso 1 1 calc R . . H10B H 0.1317 -0.2717 0.4162 0.112 Uiso 1 1 calc R . . H10C H 0.1598 -0.3290 0.4083 0.112 Uiso 1 1 calc R . . O11 O 0.0000 0.2085(3) 0.2500 0.0288(17) Uani 1 2 d S . . C11 C 0.0652(2) -0.0694(4) 0.3874(3) 0.0254(17) Uani 1 1 d . . . H11A H 0.0617 -0.0219 0.3813 0.030 Uiso 1 1 calc R . . H11B H 0.0827 -0.0767 0.4249 0.030 Uiso 1 1 calc R . . O12 O 0.0985(3) 0.0153(6) 0.5249(4) 0.041(3) Uani 0.50 1 d PD E 2 C12 C 0.0211(2) -0.1011(4) 0.3705(3) 0.0254(17) Uani 1 1 d . . . O13 O 0.0840(3) 0.0077(6) 0.5605(4) 0.043(3) Uani 0.50 1 d PD E 1 C13 C 0.0165(2) -0.1597(3) 0.3911(3) 0.0243(17) Uani 1 1 d . . . H13 H 0.0414 -0.1794 0.4172 0.029 Uiso 1 1 calc R . . O14 O -0.2262(4) 0.2897(6) 0.2907(4) 0.144(3) Uani 0.75 1 d PDU B 1 C14 C -0.0228(2) -0.1912(4) 0.3756(3) 0.0282(18) Uani 1 1 d . . . C15 C -0.0583(2) -0.1608(4) 0.3374(3) 0.0297(19) Uani 1 1 d . . . H15 H -0.0857 -0.1812 0.3261 0.036 Uiso 1 1 calc R . . C16 C -0.0558(2) -0.1021(4) 0.3148(3) 0.0257(18) Uani 1 1 d . . . C17 C -0.0153(2) -0.0711(4) 0.3322(3) 0.0256(18) Uani 1 1 d . . . C18 C -0.0280(3) -0.2553(4) 0.3997(3) 0.034(2) Uani 1 1 d . . . C19 C 0.0148(3) -0.2847(4) 0.4362(3) 0.047(2) Uani 1 1 d . . . H19A H 0.0318 -0.2945 0.4171 0.071 Uiso 1 1 calc R . . H19B H 0.0097 -0.3248 0.4512 0.071 Uiso 1 1 calc R . . H19C H 0.0305 -0.2536 0.4640 0.071 Uiso 1 1 calc R . . C20 C -0.0518(4) -0.3052(5) 0.3569(4) 0.066(3) Uani 1 1 d . . . H20A H -0.0803 -0.2881 0.3339 0.099 Uiso 1 1 calc R . . H20B H -0.0552 -0.3459 0.3725 0.099 Uiso 1 1 calc R . . H20C H -0.0352 -0.3133 0.3370 0.099 Uiso 1 1 calc R . . C21 C -0.0548(3) -0.2427(5) 0.4307(4) 0.057(3) Uani 1 1 d . . . H21A H -0.0390 -0.2129 0.4594 0.086 Uiso 1 1 calc R . . H21B H -0.0598 -0.2839 0.4444 0.086 Uiso 1 1 calc R . . H21C H -0.0825 -0.2232 0.4078 0.086 Uiso 1 1 calc R . . C22 C -0.0962(2) -0.0741(4) 0.2704(3) 0.0303(19) Uani 1 1 d . . . H22A H -0.1218 -0.0847 0.2763 0.036 Uiso 1 1 calc R F . H22B H -0.0937 -0.0261 0.2702 0.036 Uiso 1 1 calc R . . C23 C -0.1500(2) 0.0870(3) 0.2752(3) 0.0272(18) Uani 1 1 d . . . H23A H -0.1256 0.0673 0.2706 0.033 Uiso 1 1 calc R . . H23B H -0.1684 0.0512 0.2775 0.033 Uiso 1 1 calc R . . C24 C -0.1327(2) 0.1257(3) 0.3254(3) 0.0243(18) Uani 1 1 d . . . C25 C -0.1568(2) 0.1328(4) 0.3533(3) 0.0268(18) Uani 1 1 d . . . H25 H -0.1841 0.1120 0.3406 0.032 Uiso 1 1 calc R . . C26 C -0.1434(2) 0.1688(3) 0.3987(3) 0.0238(17) Uani 1 1 d . . . C27 C -0.1033(2) 0.1990(3) 0.4152(3) 0.0230(17) Uani 1 1 d . . . H27 H -0.0933 0.2245 0.4459 0.028 Uiso 1 1 calc R . . C28 C -0.0774(2) 0.1939(3) 0.3896(3) 0.0191(16) Uani 1 1 d . . . C29 C -0.0920(2) 0.1558(3) 0.3443(3) 0.0226(17) Uani 1 1 d . . . C30 C -0.1684(2) 0.1741(4) 0.4317(3) 0.0297(18) Uani 1 1 d . . . C31 C -0.1427(3) 0.1402(5) 0.4832(3) 0.049(2) Uani 1 1 d . . . H31A H -0.1594 0.1404 0.5036 0.074 Uiso 1 1 calc R . . H31B H -0.1155 0.1633 0.5021 0.074 Uiso 1 1 calc R . . H31C H -0.1368 0.0953 0.4769 0.074 Uiso 1 1 calc R . . C32 C -0.2128(3) 0.1417(5) 0.4048(4) 0.048(2) Uani 1 1 d . . . H32A H -0.2298 0.1639 0.3720 0.072 Uiso 1 1 calc R . . H32B H -0.2278 0.1446 0.4271 0.072 Uiso 1 1 calc R . . H32C H -0.2093 0.0959 0.3981 0.072 Uiso 1 1 calc R . . C33 C -0.1751(3) 0.2455(4) 0.4423(4) 0.051(3) Uani 1 1 d . . . H33A H -0.1939 0.2668 0.4098 0.076 Uiso 1 1 calc R . . H33B H -0.1472 0.2678 0.4575 0.076 Uiso 1 1 calc R . . H33C H -0.1884 0.2474 0.4665 0.076 Uiso 1 1 calc R . . C34 C -0.0352(2) 0.2310(3) 0.4079(3) 0.0222(17) Uani 1 1 d . . . H34A H -0.0219 0.2338 0.4461 0.027 Uiso 1 1 calc R F . H34B H -0.0152 0.2071 0.3975 0.027 Uiso 1 1 calc R . . C35 C -0.0419(2) 0.2987(3) 0.3855(3) 0.0228(17) Uani 1 1 d . . . C36 C -0.0554(2) 0.3488(4) 0.4085(3) 0.0305(19) Uani 1 1 d . . . H36 H -0.0585 0.3393 0.4392 0.037 Uiso 1 1 calc R F . C37 C -0.0644(3) 0.4112(4) 0.3888(3) 0.038(2) Uani 1 1 d . . . C38 C -0.0601(3) 0.4221(4) 0.3426(3) 0.041(2) Uani 1 1 d . . . H38 H -0.0655 0.4646 0.3281 0.049 Uiso 1 1 calc R F . C39 C -0.0483(2) 0.3741(4) 0.3174(3) 0.0292(19) Uani 1 1 d . . . C40 C -0.0388(2) 0.3117(4) 0.3390(3) 0.0243(17) Uani 1 1 d . . . C41 C -0.0778(4) 0.4660(5) 0.4143(5) 0.077(3) Uani 1 1 d U . . C42 C -0.1166(5) 0.5006(7) 0.3775(6) 0.130(6) Uani 1 1 d U . . H42A H -0.1422 0.4742 0.3708 0.195 Uiso 1 1 calc R . . H42B H -0.1143 0.5081 0.3450 0.195 Uiso 1 1 calc R . . H42C H -0.1191 0.5425 0.3924 0.195 Uiso 1 1 calc R . . C43 C -0.0425(6) 0.5201(5) 0.4281(5) 0.115(5) Uani 1 1 d U . . H43A H -0.0511 0.5582 0.4419 0.173 Uiso 1 1 calc R . . H43B H -0.0393 0.5324 0.3969 0.173 Uiso 1 1 calc R . . H43C H -0.0150 0.5034 0.4542 0.173 Uiso 1 1 calc R . . C44 C -0.0824(5) 0.4449(5) 0.4607(5) 0.086(4) Uani 1 1 d U . . H44A H -0.0885 0.4827 0.4773 0.128 Uiso 1 1 calc R . . H44B H -0.0556 0.4243 0.4849 0.128 Uiso 1 1 calc R . . H44C H -0.1061 0.4136 0.4508 0.128 Uiso 1 1 calc R . . C45 C 0.0481(2) 0.3893(4) 0.2347(3) 0.033(2) Uani 1 1 d . . . H45A H 0.0266 0.3614 0.2394 0.040 Uiso 1 1 calc R . . H45B H 0.0396 0.4352 0.2350 0.040 Uiso 1 1 calc R . . C46 C 0.0926(2) 0.3778(4) 0.2793(3) 0.0298(19) Uani 1 1 d . . . C47 C 0.1225(3) 0.4272(4) 0.2934(3) 0.038(2) Uani 1 1 d . . . H47 H 0.1142 0.4677 0.2759 0.045 Uiso 1 1 calc R . . C48 C 0.1651(3) 0.4204(4) 0.3325(3) 0.037(2) Uani 1 1 d . . . C49 C 0.1753(3) 0.3590(4) 0.3564(3) 0.035(2) Uani 1 1 d . . . H49 H 0.2035 0.3520 0.3828 0.042 Uiso 1 1 calc R . . C50 C 0.1461(2) 0.3084(4) 0.3430(3) 0.0264(18) Uani 1 1 d . . . C51 C 0.1039(2) 0.3179(4) 0.3038(3) 0.0239(17) Uani 1 1 d . . . C52 C 0.1985(3) 0.4753(5) 0.3489(5) 0.066(3) Uani 1 1 d U . . C53 C 0.2045(5) 0.4985(7) 0.4014(6) 0.120(5) Uani 1 1 d U . . H53A H 0.2212 0.5390 0.4100 0.181 Uiso 1 1 calc R . . H53B H 0.2199 0.4653 0.4273 0.181 Uiso 1 1 calc R . . H53C H 0.1762 0.5063 0.4010 0.181 Uiso 1 1 calc R . . C54 C 0.1847(4) 0.5329(6) 0.3113(6) 0.113(5) Uani 1 1 d U . . H54A H 0.1578 0.5512 0.3094 0.169 Uiso 1 1 calc R . . H54B H 0.1804 0.5181 0.2768 0.169 Uiso 1 1 calc R . . H54C H 0.2072 0.5664 0.3235 0.169 Uiso 1 1 calc R . . C55 C 0.2412(3) 0.4510(5) 0.3521(5) 0.080(4) Uani 1 1 d U . . H55A H 0.2612 0.4875 0.3592 0.120 Uiso 1 1 calc R . . H55B H 0.2366 0.4307 0.3191 0.120 Uiso 1 1 calc R . . H55C H 0.2533 0.4189 0.3799 0.120 Uiso 1 1 calc R . . C56 C 0.1597(2) 0.2421(3) 0.3674(3) 0.0256(18) Uani 1 1 d . . . H56A H 0.1341 0.2184 0.3657 0.031 Uiso 1 1 calc R F . H56B H 0.1800 0.2473 0.4043 0.031 Uiso 1 1 calc R . . C57 C 0.1811(2) 0.2027(4) 0.3403(3) 0.0229(17) Uani 1 1 d . . . C58 C 0.2248(2) 0.2089(4) 0.3542(3) 0.0275(18) Uani 1 1 d . . . H58 H 0.2413 0.2367 0.3823 0.033 Uiso 1 1 calc R F . C59 C 0.2459(2) 0.1763(4) 0.3289(3) 0.0292(18) Uani 1 1 d . . . C60 C 0.2206(2) 0.1363(4) 0.2873(3) 0.0308(19) Uani 1 1 d . . . H60 H 0.2339 0.1134 0.2692 0.037 Uiso 1 1 calc R F . C61 C 0.1761(2) 0.1291(3) 0.2714(3) 0.0258(18) Uani 1 1 d . . . C62 C 0.1566(2) 0.1611(3) 0.2991(3) 0.0246(17) Uani 1 1 d . . . C63 C 0.2951(3) 0.1819(5) 0.3491(3) 0.047(2) Uani 1 1 d . . . C64 C 0.3089(3) 0.2531(5) 0.3576(5) 0.079(4) Uani 1 1 d . . . H64A H 0.2960 0.2764 0.3246 0.118 Uiso 1 1 calc R . . H64B H 0.3404 0.2558 0.3719 0.118 Uiso 1 1 calc R . . H64C H 0.2992 0.2728 0.3819 0.118 Uiso 1 1 calc R . . C65 C 0.3107(3) 0.1484(6) 0.3120(4) 0.062(3) Uani 1 1 d . . . H65A H 0.3009 0.1031 0.3068 0.093 Uiso 1 1 calc R . . H65B H 0.3422 0.1496 0.3271 0.093 Uiso 1 1 calc R . . H65C H 0.2988 0.1712 0.2787 0.093 Uiso 1 1 calc R . . C66 C 0.3167(3) 0.1471(6) 0.4009(3) 0.071(4) Uani 1 1 d . . . H66A H 0.3058 0.1648 0.4248 0.106 Uiso 1 1 calc R . . H66B H 0.3479 0.1535 0.4154 0.106 Uiso 1 1 calc R . . H66C H 0.3102 0.1005 0.3959 0.106 Uiso 1 1 calc R . . C67 C 0.2212(3) 0.0609(5) 0.4194(3) 0.046(2) Uani 1 1 d . . . H67A H 0.2250 0.0137 0.4190 0.070 Uiso 1 1 calc R . . H67B H 0.2402 0.0780 0.4537 0.070 Uiso 1 1 calc R . . H67C H 0.2286 0.0812 0.3933 0.070 Uiso 1 1 calc R . . C68 C 0.1611(3) 0.0274(5) 0.4526(3) 0.048(2) Uani 1 1 d . . . H68A H 0.1316 0.0301 0.4493 0.072 Uiso 1 1 calc R . . H68B H 0.1812 0.0416 0.4873 0.072 Uiso 1 1 calc R . . H68C H 0.1675 -0.0176 0.4471 0.072 Uiso 1 1 calc R . . S2 S 0.0085(3) 0.0338(5) 0.4397(3) 0.0445(15) Uani 0.50 1 d PDU F -2 O9 O -0.02781(16) 0.0454(2) 0.39184(19) 0.042(3) Uani 0.50 1 d PU F -2 C69 C 0.0042(10) -0.0369(17) 0.4712(13) 0.092(5) Uani 0.50 1 d PDU F 1 H69A H 0.0305 -0.0407 0.5035 0.110 Uiso 0.50 1 calc PR F 1 H69B H 0.0027 -0.0730 0.4482 0.110 Uiso 0.50 1 calc PR F 1 H69C H -0.0210 -0.0384 0.4789 0.110 Uiso 0.50 1 calc PR F 1 O70 O 0.0510(4) 0.1178(6) 0.4693(4) 0.049(3) Uani 0.50 1 d P G 3 C71 C 0.0651(3) 0.3630(5) 0.4589(4) 0.031(3) Uani 0.75 1 d PD A 1 H71A H 0.0365 0.3830 0.4430 0.037 Uiso 0.75 1 calc PR A 1 H71B H 0.0861 0.3919 0.4549 0.037 Uiso 0.75 1 calc PR A 1 H71C H 0.0734 0.3557 0.4958 0.037 Uiso 0.75 1 calc PR A 1 C72 C 0.1190(3) 0.2619(5) 0.4640(4) 0.032(3) Uani 0.75 1 d PDU A 1 H72A H 0.1235 0.2197 0.4512 0.039 Uiso 0.75 1 calc PR A 1 H72B H 0.1253 0.2582 0.5007 0.039 Uiso 0.75 1 calc PR A 1 H72C H 0.1380 0.2943 0.4597 0.039 Uiso 0.75 1 calc PR A 1 C73 C 0.1261(14) 0.3626(15) 0.4462(17) 0.12(2) Uani 0.25 1 d PD A 2 H73A H 0.1367 0.3825 0.4228 0.141 Uiso 0.25 1 calc PR A 2 H73B H 0.1502 0.3558 0.4801 0.141 Uiso 0.25 1 calc PR A 2 H73C H 0.1049 0.3915 0.4498 0.141 Uiso 0.25 1 calc PR A 2 C74 C -0.2131(5) 0.4035(6) 0.2677(5) 0.066(4) Uani 0.75 1 d PDU B 1 H74A H -0.2313 0.4287 0.2794 0.079 Uiso 0.75 1 calc PR B 1 H74B H -0.2308 0.3846 0.2336 0.079 Uiso 0.75 1 calc PR B 1 H74C H -0.1912 0.4320 0.2651 0.079 Uiso 0.75 1 calc PR B 1 C75 C -0.1578(5) 0.3043(13) 0.2792(5) 0.037(4) Uani 0.75 1 d PDU B 1 H75A H -0.1430 0.2649 0.2976 0.045 Uiso 0.75 1 calc PR B 1 H75B H -0.1365 0.3356 0.2786 0.045 Uiso 0.75 1 calc PR B 1 H75C H -0.1779 0.2931 0.2437 0.045 Uiso 0.75 1 calc PR B 1 O78 O 0.0139(7) 0.5529(12) 0.3473(9) 0.062(7) Uiso 0.25 1 d PDU H 2 S10A S 0.0465(5) 0.5170(7) 0.3919(6) 0.095(4) Uiso 0.25 1 d PDU H 2 C80 C 0.0623(6) 0.5884(9) 0.3915(8) 0.112(6) Uiso 0.75 1 d PDU D 1 H80A H 0.0812 0.6231 0.4126 0.134 Uiso 0.75 1 calc PR D 1 H80B H 0.0430 0.5745 0.4066 0.134 Uiso 0.75 1 calc PR D 1 H80C H 0.0452 0.6046 0.3563 0.134 Uiso 0.75 1 calc PR D 1 C81 C 0.0515(5) 0.4693(8) 0.3501(6) 0.073(5) Uiso 0.75 1 d PDU D 1 H81A H 0.0634 0.4284 0.3444 0.088 Uiso 0.75 1 calc PR D 1 H81B H 0.0346 0.4904 0.3167 0.088 Uiso 0.75 1 calc PR D 1 H81C H 0.0329 0.4604 0.3674 0.088 Uiso 0.75 1 calc PR D 1 O82 O 0.1154(5) 0.4875(8) 0.4439(6) 0.152(6) Uiso 0.75 1 d PDU D 1 C86 C 0.1212(6) 0.0332(9) 0.6272(6) 0.043(5) Uani 0.50 1 d PD E 2 H86A H 0.1095 -0.0087 0.6314 0.051 Uiso 0.50 1 calc PR E 2 H86B H 0.0997 0.0675 0.6214 0.051 Uiso 0.50 1 calc PR E 2 H86C H 0.1473 0.0431 0.6585 0.051 Uiso 0.50 1 calc PR E 2 C87 C 0.1483(6) 0.0682(9) 0.6360(5) 0.048(5) Uani 0.50 1 d PD E 1 H87A H 0.1574 0.0351 0.6633 0.057 Uiso 0.50 1 calc PR E 1 H87B H 0.1234 0.0920 0.6356 0.057 Uiso 0.50 1 calc PR E 1 H87C H 0.1720 0.0986 0.6427 0.057 Uiso 0.50 1 calc PR E 1 C88 C 0.1534(7) 0.1099(7) 0.5761(9) 0.054(5) Uani 0.50 1 d PD E 2 H88A H 0.1619 0.1155 0.5479 0.065 Uiso 0.50 1 calc PR E 2 H88B H 0.1783 0.1171 0.6093 0.065 Uiso 0.50 1 calc PR E 2 H88C H 0.1307 0.1413 0.5722 0.065 Uiso 0.50 1 calc PR E 2 C89 C 0.1196(7) 0.1062(8) 0.5381(7) 0.053(5) Uani 0.50 1 d PD E 1 H89A H 0.1100 0.0973 0.5012 0.064 Uiso 0.50 1 calc PR E 1 H89B H 0.1449 0.1347 0.5504 0.064 Uiso 0.50 1 calc PR E 1 H89C H 0.0963 0.1277 0.5433 0.064 Uiso 0.50 1 calc PR E 1 C91 C 0.040(2) -0.317(3) 0.278(3) 0.075(16) Uiso 0.25 1 d P . . C72A C 0.0856(14) 0.262(2) 0.4702(13) 0.070(10) Uani 0.25 1 d PDU A 2 H72D H 0.0709 0.2196 0.4622 0.084 Uiso 0.25 1 calc PR A 2 H72E H 0.0661 0.2949 0.4729 0.084 Uiso 0.25 1 calc PR A 2 H72F H 0.1114 0.2589 0.5031 0.084 Uiso 0.25 1 calc PR A 2 C74A C -0.2018(17) 0.3998(17) 0.2956(17) 0.066(4) Uani 0.25 1 d PDU C 2 H74D H -0.2289 0.4230 0.2873 0.079 Uiso 0.25 1 calc PR C 2 H74E H -0.1814 0.4289 0.2904 0.079 Uiso 0.25 1 calc PR C 2 H74F H -0.1896 0.3856 0.3317 0.079 Uiso 0.25 1 calc PR C 2 C75A C -0.1567(13) 0.303(5) 0.2928(19) 0.045(8) Uani 0.25 1 d PDU C 2 H75D H -0.1526 0.2589 0.2825 0.055 Uiso 0.25 1 calc PR C 2 H75E H -0.1512 0.3026 0.3294 0.055 Uiso 0.25 1 calc PR C 2 H75F H -0.1368 0.3329 0.2878 0.055 Uiso 0.25 1 calc PR C 2 S7 S 0.0182(5) -0.2771(6) 0.2482(5) 0.064(3) Uiso 0.25 1 d P . . C80A C 0.0930(11) 0.572(2) 0.4232(18) 0.100(12) Uiso 0.25 1 d PDU H 2 H80D H 0.0855 0.6066 0.4416 0.120 Uiso 0.25 1 calc PR H 2 H80E H 0.1003 0.5915 0.3968 0.120 Uiso 0.25 1 calc PR H 2 H80F H 0.1177 0.5475 0.4478 0.120 Uiso 0.25 1 calc PR H 2 C81A C 0.0709(15) 0.463(2) 0.3602(19) 0.087(12) Uiso 0.25 1 d PDU H 2 H81D H 0.0506 0.4279 0.3418 0.104 Uiso 0.25 1 calc PR H 2 H81E H 0.0975 0.4438 0.3864 0.104 Uiso 0.25 1 calc PR H 2 H81F H 0.0776 0.4879 0.3354 0.104 Uiso 0.25 1 calc PR H 2 C90 C 0.0000 -0.1966(9) 0.2500 0.088(5) Uiso 1 2 d S . . C150 C 0.0045(13) 0.0298(19) 0.4440(10) 0.0445(15) Uani 0.50 1 d PDU F 1 H15A H 0.0033 0.0648 0.4670 0.053 Uiso 0.50 1 calc PR F 1 H15B H 0.0330 0.0332 0.4433 0.053 Uiso 0.50 1 calc PR F 1 C70 C -0.0004(8) 0.0885(8) 0.4845(6) 0.066(7) Uani 0.50 1 d PD F -2 H70A H 0.0079 0.1328 0.4801 0.079 Uiso 0.50 1 calc PR F -2 H70B H 0.0170 0.0741 0.5202 0.079 Uiso 0.50 1 calc PR F -2 H70C H -0.0310 0.0878 0.4774 0.079 Uiso 0.50 1 calc PR F -2 C69A C -0.0124(9) -0.0386(15) 0.4591(13) 0.092(5) Uani 0.50 1 d PDU F -2 H69D H -0.0102 -0.0764 0.4395 0.110 Uiso 0.50 1 calc PR F -2 H69E H -0.0427 -0.0315 0.4518 0.110 Uiso 0.50 1 calc PR F -2 H69F H 0.0044 -0.0464 0.4962 0.110 Uiso 0.50 1 calc PR F -2 C91A C 0.0295(19) -0.327(3) 0.247(2) 0.077(16) Uiso 0.25 1 d P . . O92 O 0.0279(14) -0.316(2) 0.2978(16) 0.099(13) Uiso 0.25 1 d P . . O93 O -0.2928(3) 0.4344(4) 0.2566(4) 0.099(3) Uiso 1 1 d U . . C151 C -0.2858(4) 0.4546(6) 0.3090(4) 0.085(5) Uiso 0.50 1 d PDU I 1 H15C H -0.2948 0.4188 0.3253 0.102 Uiso 0.50 1 calc PR I 1 H15D H -0.3043 0.4927 0.3063 0.102 Uiso 0.50 1 calc PR I 1 C152 C -0.2389(8) 0.472(2) 0.3438(14) 0.174(11) Uiso 0.50 1 d PDU I 1 H15E H -0.2363 0.4855 0.3779 0.209 Uiso 0.50 1 calc PR I 1 H15F H -0.2299 0.5082 0.3282 0.209 Uiso 0.50 1 calc PR I 1 H15G H -0.2205 0.4344 0.3476 0.209 Uiso 0.50 1 calc PR I 1 C154 C -0.2737(13) 0.4039(17) 0.3509(13) 0.180(11) Uiso 0.50 1 d PDU I 2 H15H H -0.2699 0.4246 0.3834 0.215 Uiso 0.50 1 calc PR I 2 H15I H -0.2467 0.3828 0.3555 0.215 Uiso 0.50 1 calc PR I 2 H15J H -0.2966 0.3712 0.3411 0.215 Uiso 0.50 1 calc PR I 2 C153 C -0.2858(4) 0.4546(6) 0.3090(4) 0.050(3) Uiso 0.50 1 d PDU I 2 H15K H -0.3126 0.4760 0.3061 0.060 Uiso 0.50 1 calc PR I 2 H15L H -0.2629 0.4881 0.3208 0.060 Uiso 0.50 1 calc PR I 2 O9A O -0.02781(16) 0.0454(2) 0.39184(19) 0.021(2) Uani 0.50 1 d PDU F 1 O14A O -0.2262(4) 0.2897(6) 0.2907(4) 0.144(3) Uani 0.25 1 d PDU C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0139(5) 0.0184(5) 0.0182(5) 0.0007(4) 0.0012(4) 0.0003(4) Cl1 0.0224(10) 0.0251(10) 0.0205(9) 0.0004(8) 0.0015(8) 0.0023(8) S1 0.0240(11) 0.0349(12) 0.0260(10) 0.0044(9) 0.0025(9) -0.0025(9) O1 0.021(3) 0.019(3) 0.024(3) 0.002(2) 0.003(2) -0.006(2) C1 0.009(4) 0.033(5) 0.029(4) -0.006(4) 0.001(3) -0.009(3) Cu2 0.0208(7) 0.0166(7) 0.0193(6) 0.000 0.0043(5) 0.000 Cl2 0.0670(18) 0.083(2) 0.0353(13) -0.0040(13) 0.0040(12) -0.0334(16) O2 0.027(3) 0.022(3) 0.023(3) 0.007(2) 0.007(2) 0.011(2) C2 0.019(4) 0.033(5) 0.040(5) -0.012(4) 0.009(4) -0.007(4) Cu3 0.0191(5) 0.0208(5) 0.0168(5) 0.0035(4) 0.0050(4) 0.0044(4) S3 0.0155(13) 0.0291(14) 0.0152(12) -0.0033(10) 0.0017(10) -0.0022(11) O3 0.025(3) 0.018(3) 0.017(2) 0.001(2) 0.004(2) 0.001(2) C3 0.022(4) 0.030(5) 0.040(5) -0.001(4) 0.006(4) -0.001(4) Cu4 0.0140(5) 0.0229(5) 0.0152(4) 0.0004(4) 0.0018(4) 0.0036(4) S4 0.046(6) 0.066(7) 0.040(6) -0.010(5) 0.008(5) -0.009(5) O4 0.016(3) 0.027(3) 0.020(3) 0.000(2) 0.005(2) 0.001(2) C4 0.021(4) 0.026(4) 0.039(5) 0.005(4) 0.012(4) -0.001(4) Cu5 0.0132(4) 0.0198(5) 0.0151(4) -0.0028(4) 0.0014(4) -0.0017(4) S5 0.0690(18) 0.0440(15) 0.0490(15) -0.0039(12) 0.0253(14) -0.0126(13) O5 0.016(3) 0.033(3) 0.022(3) -0.007(2) 0.007(2) -0.004(2) C5 0.019(4) 0.022(4) 0.025(4) -0.001(3) 0.003(3) -0.006(3) Cu6 0.0423(10) 0.0652(12) 0.0280(8) -0.0041(8) -0.0010(7) -0.0150(8) O6 0.018(3) 0.019(3) 0.017(2) 0.001(2) -0.004(2) -0.006(2) C6 0.020(4) 0.020(4) 0.031(4) -0.003(4) 0.003(4) -0.005(3) O7 0.017(3) 0.024(3) 0.025(3) 0.001(2) 0.000(2) 0.002(2) C7 0.032(5) 0.049(6) 0.056(6) -0.001(5) 0.011(5) 0.014(5) S8 0.065(2) 0.074(3) 0.095(3) -0.005(2) 0.047(2) 0.009(2) O8 0.022(3) 0.049(3) 0.013(3) -0.003(2) 0.001(2) 0.012(3) C8 0.052(7) 0.080(9) 0.091(9) -0.009(7) 0.007(6) 0.037(7) S9 0.060(5) 0.070(6) 0.086(6) 0.023(5) 0.038(5) 0.014(5) C9 0.084(8) 0.054(7) 0.087(8) 0.002(6) 0.042(7) 0.027(6) O10 0.022(3) 0.032(3) 0.017(3) -0.007(2) 0.000(2) -0.004(2) C10 0.085(8) 0.039(6) 0.107(9) 0.030(6) 0.046(8) 0.031(6) O11 0.034(4) 0.024(4) 0.012(3) 0.000 -0.006(3) 0.000 C11 0.023(4) 0.026(4) 0.019(4) 0.003(3) 0.001(3) 0.004(3) O12 0.034(7) 0.048(7) 0.036(7) 0.006(6) 0.010(6) 0.009(6) C12 0.025(4) 0.024(4) 0.024(4) 0.000(3) 0.008(4) 0.003(3) O13 0.031(7) 0.048(8) 0.045(7) 0.013(6) 0.010(6) -0.002(6) C13 0.024(4) 0.019(4) 0.023(4) 0.005(3) 0.004(3) 0.006(3) O14 0.130(7) 0.149(7) 0.138(7) 0.013(6) 0.045(6) 0.004(6) C14 0.027(5) 0.030(4) 0.032(4) 0.006(4) 0.017(4) 0.009(4) C15 0.020(4) 0.037(5) 0.031(4) 0.000(4) 0.010(4) 0.002(4) C16 0.021(4) 0.034(5) 0.024(4) 0.004(4) 0.011(3) 0.014(4) C17 0.031(5) 0.025(4) 0.020(4) -0.001(3) 0.011(4) 0.006(4) C18 0.031(5) 0.033(5) 0.036(5) 0.009(4) 0.013(4) 0.000(4) C19 0.047(6) 0.043(6) 0.051(6) 0.022(5) 0.020(5) 0.001(5) C20 0.077(8) 0.039(6) 0.064(7) 0.001(5) 0.014(6) -0.018(6) C21 0.048(6) 0.076(7) 0.054(6) 0.024(5) 0.027(5) 0.005(5) C22 0.020(4) 0.040(5) 0.030(4) 0.010(4) 0.009(4) 0.010(4) C23 0.029(4) 0.018(4) 0.025(4) 0.004(3) 0.002(4) 0.003(3) C24 0.024(4) 0.017(4) 0.020(4) 0.004(3) -0.002(3) 0.009(3) C25 0.021(4) 0.024(4) 0.028(4) 0.001(3) 0.003(4) -0.003(3) C26 0.016(4) 0.023(4) 0.027(4) 0.009(3) 0.004(3) 0.007(3) C27 0.020(4) 0.026(4) 0.018(4) -0.001(3) 0.003(3) 0.005(3) C28 0.013(4) 0.019(4) 0.020(4) 0.004(3) 0.002(3) 0.004(3) C29 0.022(4) 0.016(4) 0.023(4) 0.006(3) 0.003(3) 0.006(3) C30 0.021(4) 0.026(5) 0.040(5) -0.003(4) 0.012(4) -0.002(3) C31 0.041(5) 0.075(7) 0.034(5) 0.009(5) 0.018(4) 0.003(5) C32 0.032(5) 0.051(6) 0.058(6) -0.005(5) 0.016(5) -0.007(4) C33 0.041(6) 0.052(6) 0.064(6) -0.013(5) 0.027(5) -0.007(5) C34 0.016(4) 0.036(5) 0.014(4) -0.007(3) 0.006(3) 0.004(3) C35 0.014(4) 0.025(4) 0.022(4) -0.004(3) 0.000(3) 0.002(3) C36 0.026(4) 0.036(5) 0.032(4) -0.006(4) 0.015(4) -0.001(4) C37 0.033(5) 0.026(5) 0.048(5) -0.003(4) 0.012(4) 0.005(4) C38 0.041(5) 0.029(5) 0.047(5) -0.002(4) 0.014(5) -0.007(4) C39 0.021(4) 0.030(5) 0.029(4) -0.001(4) 0.004(4) -0.009(4) C40 0.013(4) 0.027(5) 0.027(4) -0.007(3) 0.004(3) -0.005(3) C41 0.128(9) 0.040(6) 0.082(7) -0.004(5) 0.064(7) 0.021(6) C42 0.146(12) 0.111(10) 0.135(11) 0.007(9) 0.064(10) 0.093(9) C43 0.228(14) 0.033(6) 0.108(9) -0.019(6) 0.095(10) -0.010(8) C44 0.144(10) 0.047(6) 0.109(9) -0.007(6) 0.096(8) 0.025(7) C45 0.024(4) 0.035(5) 0.034(5) -0.005(4) 0.006(4) 0.004(4) C46 0.030(5) 0.027(5) 0.024(4) -0.005(4) 0.005(4) 0.001(4) C47 0.032(5) 0.027(5) 0.045(5) 0.004(4) 0.008(4) 0.004(4) C48 0.024(5) 0.028(5) 0.054(6) -0.006(4) 0.011(4) -0.004(4) C49 0.019(4) 0.038(5) 0.040(5) -0.009(4) 0.004(4) -0.005(4) C50 0.023(4) 0.029(4) 0.024(4) -0.009(3) 0.007(4) -0.003(4) C51 0.019(4) 0.033(5) 0.021(4) -0.007(3) 0.010(3) -0.004(4) C52 0.042(5) 0.042(6) 0.113(8) -0.028(6) 0.032(6) -0.018(5) C53 0.116(10) 0.115(10) 0.130(11) -0.069(9) 0.053(9) -0.075(9) C54 0.077(8) 0.043(7) 0.173(12) 0.016(8) 0.010(9) -0.021(6) C55 0.039(6) 0.050(6) 0.146(10) 0.002(7) 0.034(7) -0.010(5) C56 0.016(4) 0.031(4) 0.019(4) -0.004(3) -0.002(3) -0.009(3) C57 0.022(4) 0.025(4) 0.015(4) 0.004(3) 0.002(3) -0.006(3) C58 0.024(4) 0.026(4) 0.022(4) 0.001(3) 0.000(3) -0.003(4) C59 0.017(4) 0.034(5) 0.030(4) -0.001(4) 0.003(4) -0.004(4) C60 0.024(5) 0.028(5) 0.031(4) 0.000(4) 0.003(4) 0.002(4) C61 0.029(5) 0.015(4) 0.021(4) 0.007(3) 0.000(4) 0.000(3) C62 0.023(4) 0.022(4) 0.018(4) 0.006(3) -0.002(3) -0.004(3) C63 0.023(5) 0.062(7) 0.050(6) -0.012(5) 0.011(4) -0.003(4) C64 0.036(6) 0.085(9) 0.118(10) -0.042(8) 0.036(7) -0.025(6) C65 0.031(5) 0.098(9) 0.054(6) -0.013(6) 0.016(5) 0.001(6) C66 0.024(5) 0.131(11) 0.041(6) -0.033(6) -0.001(4) 0.014(6) C67 0.023(5) 0.052(6) 0.049(6) 0.010(5) 0.002(4) 0.010(4) C68 0.043(6) 0.060(6) 0.033(5) 0.006(4) 0.009(4) -0.018(5) S2 0.047(3) 0.044(2) 0.044(2) 0.0066(18) 0.021(2) 0.0000(19) O9 0.050(5) 0.041(5) 0.033(5) 0.009(5) 0.015(5) 0.007(5) C69 0.088(11) 0.084(8) 0.075(10) 0.015(8) 0.008(9) 0.001(9) O70 0.036(7) 0.069(9) 0.034(7) 0.004(6) 0.007(6) -0.008(6) C71 0.033(6) 0.036(6) 0.019(5) -0.014(5) 0.008(5) -0.002(5) C72 0.027(6) 0.046(7) 0.015(5) 0.002(5) 0.002(5) 0.007(5) C73 0.04(3) 0.22(7) 0.06(3) 0.04(4) -0.01(2) -0.04(4) C74 0.060(8) 0.041(6) 0.109(9) 0.022(7) 0.048(8) 0.028(6) C75 0.037(7) 0.043(7) 0.037(9) 0.004(9) 0.021(6) 0.015(6) C86 0.046(12) 0.033(11) 0.045(11) -0.002(9) 0.015(10) 0.009(9) C87 0.028(10) 0.061(14) 0.047(11) 0.029(10) 0.010(9) 0.011(10) C88 0.050(13) 0.038(12) 0.081(16) -0.001(11) 0.034(12) -0.006(10) C89 0.063(14) 0.057(13) 0.051(12) -0.007(10) 0.034(12) -0.022(11) C72A 0.054(17) 0.076(18) 0.057(17) -0.006(16) 0.002(16) 0.005(17) C74A 0.060(8) 0.041(6) 0.109(9) 0.022(7) 0.048(8) 0.028(6) C75A 0.054(13) 0.054(13) 0.049(14) -0.003(15) 0.041(11) 0.018(12) C150 0.047(3) 0.044(2) 0.044(2) 0.0066(18) 0.021(2) 0.0000(19) C70 0.12(2) 0.030(11) 0.023(9) -0.009(8) 0.011(11) 0.012(12) C69A 0.088(11) 0.084(8) 0.075(10) 0.015(8) 0.008(9) 0.001(9) O9A 0.021(3) 0.021(3) 0.021(4) 0.000(4) 0.009(4) 0.000(4) O14A 0.130(7) 0.149(7) 0.138(7) 0.013(6) 0.045(6) 0.004(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O7 1.926(5) . ? Cu1 O8 1.927(5) . ? Cu1 O1 1.968(5) . ? Cu1 O6 1.971(5) . ? S1 O7 1.523(5) . ? S1 C68 1.787(8) . ? S1 C67 1.788(8) . ? O1 C6 1.375(8) . ? O1 Cu2 1.945(5) . ? C1 C2 1.392(11) . ? C1 C6 1.408(11) . ? C1 C22 1.498(10) 2 ? Cu2 O1 1.945(5) 2 ? Cu2 O2 1.953(5) . ? Cu2 O2 1.953(5) 2 ? Cl2 Cu6 2.097(3) . ? O2 C17 1.363(9) . ? O2 Cu3 1.968(5) . ? C2 C3 1.391(11) . ? Cu3 O8 1.937(5) 2 ? Cu3 O9 1.944(5) . ? Cu3 O3 1.964(5) . ? S3 O10 1.516(5) . ? S3 C72 1.793(9) . ? S3 C71 1.798(9) . ? O3 C29 1.365(8) . ? O3 Cu4 1.948(5) . ? C3 C4 1.380(11) . ? C3 C7 1.533(11) . ? Cu4 O5 1.943(5) 2 ? Cu4 O6 1.948(4) 2 ? Cu4 O4 1.963(5) . ? S4 O10 1.485(11) . ? S4 C72A 1.80(2) . ? S4 C73 1.84(2) . ? O4 C40 1.355(9) . ? O4 Cu5 1.969(5) . ? C4 C5 1.404(10) . ? Cu5 O10 1.933(4) . ? Cu5 O11 1.935(4) . ? Cu5 O5 1.962(5) . ? S5 O12 1.439(10) . ? S5 O13 1.635(10) . ? S5 C86 1.740(14) . ? S5 C88 1.784(14) . ? S5 C87 1.799(15) . ? S5 C89 1.840(14) . ? O5 C51 1.359(8) . ? O5 Cu4 1.943(5) 2 ? C5 C6 1.384(10) . ? C5 C11 1.522(10) . ? Cu6 Cl2 2.097(3) 7_556 ? S6 S7 0.955(12) . ? S6 S7 0.965(13) 2 ? S6 O92 0.97(4) . ? S6 C91 1.25(6) . ? S6 S6 1.41(2) 2 ? S6 O91 1.59(3) . ? S6 C91A 1.61(6) . ? S6 C91A 1.62(6) 2 ? S6 C90 1.83(2) . ? S6 O91 1.92(3) 2 ? S6 C91 1.96(6) 2 ? S6 O92 2.13(4) 2 ? O6 C62 1.374(8) . ? O6 Cu4 1.948(4) 2 ? O91 C91 0.78(7) . ? O91 C91A 0.87(6) . ? O91 S7 1.04(3) . ? O91 O92 1.56(5) . ? O91 S6 1.92(3) 2 ? C7 C9 1.514(13) . ? C7 C10 1.530(14) . ? C7 C8 1.550(14) . ? S8 O14 1.591(11) . ? S8 C74 1.769(7) . ? S8 C75 1.822(7) . ? O8 Cu3 1.937(5) 2 ? S9 C74A 1.826(8) . ? S9 C75A 1.828(8) . ? S10 O82 1.575(13) . ? S10 C81 1.767(13) . ? S10 C80 1.780(15) . ? O11 Cu5 1.935(4) 2 ? C11 C12 1.525(10) . ? C12 C13 1.382(10) . ? C12 C17 1.403(10) . ? C13 C14 1.390(10) . ? C14 C15 1.389(10) . ? C14 C18 1.533(11) . ? C15 C16 1.388(11) . ? C16 C17 1.415(11) . ? C16 C22 1.535(10) . ? C18 C19 1.516(11) . ? C18 C20 1.537(12) . ? C18 C21 1.552(12) . ? C22 C1 1.498(10) 2 ? C23 C61 1.520(10) 2 ? C23 C24 1.523(10) . ? C24 C25 1.385(10) . ? C24 C29 1.408(10) . ? C25 C26 1.390(10) . ? C26 C27 1.397(10) . ? C26 C30 1.531(10) . ? C27 C28 1.381(10) . ? C28 C29 1.410(10) . ? C28 C34 1.519(10) . ? C30 C31 1.522(11) . ? C30 C33 1.536(11) . ? C30 C32 1.537(11) . ? C34 C35 1.507(10) . ? C35 C36 1.404(10) . ? C35 C40 1.407(10) . ? C36 C37 1.381(11) . ? C37 C38 1.412(12) . ? C37 C41 1.518(13) . ? C38 C39 1.384(11) . ? C39 C40 1.400(11) . ? C39 C45 1.525(11) 2 ? C41 C44 1.469(15) . ? C41 C42 1.480(17) . ? C41 C43 1.565(18) . ? C45 C39 1.525(11) 2 ? C45 C46 1.533(10) . ? C46 C47 1.377(11) . ? C46 C51 1.387(10) . ? C47 C48 1.416(11) . ? C48 C49 1.406(11) . ? C48 C52 1.535(12) . ? C49 C50 1.380(10) . ? C50 C51 1.417(10) . ? C50 C56 1.511(10) . ? C52 C53 1.505(17) . ? C52 C55 1.515(14) . ? C52 C54 1.532(16) . ? C56 C57 1.514(10) . ? C57 C58 1.387(10) . ? C57 C62 1.406(10) . ? C58 C59 1.399(11) . ? C59 C60 1.399(10) . ? C59 C63 1.540(11) . ? C60 C61 1.405(10) . ? C61 C62 1.403(11) . ? C61 C23 1.520(10) 2 ? C63 C66 1.523(14) . ? C63 C64 1.525(14) . ? C63 C65 1.540(12) . ? S2 O9 1.422(9) . ? S2 C70 1.830(10) . ? S2 C69A 1.841(10) . ? C69 C150 1.580(19) . ? O78 S10A 1.484(17) . ? S10A C80A 1.847(19) . ? S10A C81A 1.853(19) . ? C91 C91A 0.82(7) . ? C91 O92 0.84(7) . ? C91 S7 1.19(6) . ? C91 S6 1.96(6) 2 ? C91 S7 1.99(6) 2 ? S7 S6 0.965(13) 2 ? S7 C91A 1.11(5) . ? S7 S7 1.30(3) 2 ? S7 O92 1.53(5) . ? S7 O92 1.75(4) 2 ? S7 C90 1.78(2) . ? S7 C91 1.99(6) 2 ? S7 C91A 1.99(5) 2 ? C90 S7 1.78(2) 2 ? C90 S6 1.83(2) 2 ? C91A O92 1.49(7) . ? C91A S6 1.62(6) 2 ? C91A O92 1.85(7) 2 ? C91A S7 1.99(5) 2 ? O92 S7 1.75(4) 2 ? O92 C91A 1.85(7) 2 ? O92 S6 2.13(4) 2 ? O93 C151 1.474(13) . ? C151 C152 1.532(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Cu1 O8 173.6(2) . . ? O7 Cu1 O1 91.1(2) . . ? O8 Cu1 O1 85.0(2) . . ? O7 Cu1 O6 95.5(2) . . ? O8 Cu1 O6 86.7(2) . . ? O1 Cu1 O6 161.7(2) . . ? O7 S1 C68 102.6(4) . . ? O7 S1 C67 102.9(4) . . ? C68 S1 C67 98.7(4) . . ? C6 O1 Cu2 119.7(4) . . ? C6 O1 Cu1 124.5(4) . . ? Cu2 O1 Cu1 115.0(2) . . ? C2 C1 C6 117.9(7) . . ? C2 C1 C22 119.9(7) . 2 ? C6 C1 C22 122.1(7) . 2 ? O1 Cu2 O1 176.7(3) 2 . ? O1 Cu2 O2 89.6(2) 2 . ? O1 Cu2 O2 90.3(2) . . ? O1 Cu2 O2 90.3(2) 2 2 ? O1 Cu2 O2 89.6(2) . 2 ? O2 Cu2 O2 177.0(3) . 2 ? C17 O2 Cu2 117.9(4) . . ? C17 O2 Cu3 125.7(4) . . ? Cu2 O2 Cu3 115.0(2) . . ? C3 C2 C1 123.2(8) . . ? O8 Cu3 O9 176.8(2) 2 . ? O8 Cu3 O3 85.1(2) 2 . ? O9 Cu3 O3 94.2(2) . . ? O8 Cu3 O2 85.3(2) 2 . ? O9 Cu3 O2 94.3(2) . . ? O3 Cu3 O2 160.18(19) . . ? O10 S3 C72 104.8(4) . . ? O10 S3 C71 102.7(4) . . ? C72 S3 C71 99.8(5) . . ? C29 O3 Cu4 119.2(4) . . ? C29 O3 Cu3 124.6(4) . . ? Cu4 O3 Cu3 115.4(2) . . ? C4 C3 C2 116.8(7) . . ? C4 C3 C7 120.5(7) . . ? C2 C3 C7 122.6(8) . . ? O5 Cu4 O6 90.5(2) 2 2 ? O5 Cu4 O3 177.3(2) 2 . ? O6 Cu4 O3 89.40(19) 2 . ? O5 Cu4 O4 90.1(2) 2 . ? O6 Cu4 O4 176.0(2) 2 . ? O3 Cu4 O4 89.89(19) . . ? O10 S4 C72A 106.4(15) . . ? O10 S4 C73 99.8(15) . . ? C72A S4 C73 98(2) . . ? C40 O4 Cu4 117.5(4) . . ? C40 O4 Cu5 126.3(4) . . ? Cu4 O4 Cu5 114.2(2) . . ? C3 C4 C5 122.6(7) . . ? O10 Cu5 O11 177.1(2) . . ? O10 Cu5 O5 92.5(2) . . ? O11 Cu5 O5 85.04(14) . . ? O10 Cu5 O4 95.3(2) . . ? O11 Cu5 O4 86.46(14) . . ? O5 Cu5 O4 159.6(2) . . ? O12 S5 O13 50.5(6) . . ? O12 S5 C86 116.8(8) . . ? O13 S5 C86 66.7(8) . . ? O12 S5 C88 111.1(9) . . ? O13 S5 C88 127.2(8) . . ? C86 S5 C88 99.6(9) . . ? O12 S5 C87 144.8(8) . . ? O13 S5 C87 100.6(8) . . ? C86 S5 C87 36.7(7) . . ? C88 S5 C87 67.5(9) . . ? O12 S5 C89 73.1(8) . . ? O13 S5 C89 96.0(8) . . ? C86 S5 C89 110.4(8) . . ? C88 S5 C89 38.8(8) . . ? C87 S5 C89 93.9(8) . . ? C51 O5 Cu4 119.0(4) . 2 ? C51 O5 Cu5 125.4(4) . . ? Cu4 O5 Cu5 115.0(2) 2 . ? C6 C5 C4 118.8(7) . . ? C6 C5 C11 121.0(7) . . ? C4 C5 C11 120.1(7) . . ? Cl2 Cu6 Cl2 180.00(17) 7_556 . ? S7 S6 S7 85.0(19) . 2 ? S7 S6 O92 105(3) . . ? S7 S6 O92 130(3) 2 . ? S7 S6 C91 63(4) . . ? S7 S6 C91 127(3) 2 . ? O92 S6 C91 42(3) . . ? S7 S6 S6 42.9(11) . 2 ? S7 S6 S6 42.3(10) 2 2 ? O92 S6 S6 125(3) . 2 ? C91 S6 S6 94(3) . 2 ? S7 S6 O91 39.0(15) . . ? S7 S6 O91 121(2) 2 . ? O92 S6 O91 70(3) . . ? C91 S6 O91 29(3) . . ? S6 S6 O91 79.0(15) 2 . ? S7 S6 C91A 43(2) . . ? S7 S6 C91A 98(2) 2 . ? O92 S6 C91A 66(3) . . ? C91 S6 C91A 30(3) . . ? S6 S6 C91A 64(2) 2 . ? O91 S6 C91A 31(2) . . ? S7 S6 C91A 98(2) . 2 ? S7 S6 C91A 42(2) 2 2 ? O92 S6 C91A 87(3) . 2 ? C91 S6 C91A 99(3) . 2 ? S6 S6 C91A 64(2) 2 2 ? O91 S6 C91A 113(3) . 2 ? C91A S6 C91A 81(4) . 2 ? S7 S6 C90 71.4(11) . . ? S7 S6 C90 71.3(11) 2 . ? O92 S6 C90 159(3) . . ? C91 S6 C90 127(4) . . ? S6 S6 C90 67.3(4) 2 . ? O91 S6 C90 98.5(14) . . ? C91A S6 C90 114(2) . . ? C91A S6 C90 113(2) 2 . ? S7 S6 O91 96.8(17) . 2 ? S7 S6 O91 17.8(14) 2 2 ? O92 S6 O91 113(3) . 2 ? C91 S6 O91 122(3) . 2 ? S6 S6 O91 54.5(12) 2 2 ? O91 S6 O91 126.5(15) . 2 ? C91A S6 O91 98(2) . 2 ? C91A S6 O91 27(2) 2 2 ? C90 S6 O91 87.6(11) . 2 ? S7 S6 C91 78(2) . 2 ? S7 S6 C91 27(2) 2 2 ? O92 S6 C91 105(3) . 2 ? C91 S6 C91 101(4) . 2 ? S6 S6 C91 40(2) 2 2 ? O91 S6 C91 103(2) . 2 ? C91A S6 C91 75(3) . 2 ? C91A S6 C91 24(2) 2 2 ? C90 S6 C91 94.1(19) . 2 ? O91 S6 C91 23(2) 2 2 ? S7 S6 O92 54.6(16) . 2 ? S7 S6 O92 40.8(16) 2 2 ? O92 S6 O92 107(3) . 2 ? C91 S6 O92 87(3) . 2 ? S6 S6 O92 22.1(12) 2 2 ? O91 S6 O92 81.9(17) . 2 ? C91A S6 O92 57(2) . 2 ? C91A S6 O92 45(2) 2 2 ? C90 S6 O92 88.3(11) . 2 ? O91 S6 O92 45.0(15) 2 2 ? C91 S6 O92 23.3(19) 2 2 ? C62 O6 Cu4 118.8(4) . 2 ? C62 O6 Cu1 125.3(4) . . ? Cu4 O6 Cu1 114.2(2) 2 . ? O1 C6 C5 120.0(7) . . ? O1 C6 C1 119.4(7) . . ? C5 C6 C1 120.6(7) . . ? C91 O91 C91A 59(5) . . ? C91 O91 S7 80(5) . . ? C91A O91 S7 71(4) . . ? C91 O91 O92 17(6) . . ? C91A O91 O92 70(5) . . ? S7 O91 O92 69(2) . . ? C91 O91 S6 51(5) . . ? C91A O91 S6 75(4) . . ? S7 O91 S6 35.4(14) . . ? O92 O91 S6 36.0(16) . . ? C91 O91 S6 81(5) . 2 ? C91A O91 S6 57(4) . 2 ? S7 O91 S6 16.5(13) . 2 ? O92 O91 S6 75(2) . 2 ? S6 O91 S6 46.4(12) . 2 ? S1 O7 Cu1 123.2(3) . . ? C9 C7 C10 106.8(9) . . ? C9 C7 C3 113.1(8) . . ? C10 C7 C3 110.7(7) . . ? C9 C7 C8 109.4(9) . . ? C10 C7 C8 108.5(9) . . ? C3 C7 C8 108.3(8) . . ? O14 S8 C74 97.2(7) . . ? O14 S8 C75 95.3(10) . . ? C74 S8 C75 97.9(9) . . ? Cu1 O8 Cu3 117.5(2) . 2 ? C74A S9 C75A 88(3) . . ? O82 S10 C81 105.7(9) . . ? O82 S10 C80 109.7(10) . . ? C81 S10 C80 97.9(9) . . ? S4 O10 S3 55.0(4) . . ? S4 O10 Cu5 123.2(5) . . ? S3 O10 Cu5 122.1(3) . . ? Cu5 O11 Cu5 118.8(4) . 2 ? C5 C11 C12 110.3(6) . . ? C13 C12 C17 119.3(7) . . ? C13 C12 C11 121.2(7) . . ? C17 C12 C11 119.5(7) . . ? C12 C13 C14 123.1(7) . . ? C15 C14 C13 116.5(7) . . ? C15 C14 C18 120.6(7) . . ? C13 C14 C18 122.8(7) . . ? C16 C15 C14 123.3(7) . . ? C15 C16 C17 118.4(7) . . ? C15 C16 C22 119.8(7) . . ? C17 C16 C22 121.7(7) . . ? O2 C17 C12 120.8(7) . . ? O2 C17 C16 119.8(6) . . ? C12 C17 C16 119.4(7) . . ? C19 C18 C14 112.8(7) . . ? C19 C18 C20 108.1(7) . . ? C14 C18 C20 109.8(7) . . ? C19 C18 C21 108.2(7) . . ? C14 C18 C21 109.0(7) . . ? C20 C18 C21 108.9(8) . . ? C1 C22 C16 111.9(6) 2 . ? C61 C23 C24 112.0(6) 2 . ? C25 C24 C29 118.4(7) . . ? C25 C24 C23 120.7(7) . . ? C29 C24 C23 120.9(7) . . ? C24 C25 C26 123.8(7) . . ? C25 C26 C27 115.7(7) . . ? C25 C26 C30 124.6(6) . . ? C27 C26 C30 119.6(6) . . ? C28 C27 C26 123.7(7) . . ? C27 C28 C29 118.4(6) . . ? C27 C28 C34 121.2(6) . . ? C29 C28 C34 120.3(6) . . ? O3 C29 C24 120.6(6) . . ? O3 C29 C28 119.5(6) . . ? C24 C29 C28 119.9(7) . . ? C31 C30 C26 108.7(6) . . ? C31 C30 C33 108.6(7) . . ? C26 C30 C33 111.3(6) . . ? C31 C30 C32 108.9(7) . . ? C26 C30 C32 111.1(6) . . ? C33 C30 C32 108.2(7) . . ? C35 C34 C28 111.7(6) . . ? C36 C35 C40 118.6(7) . . ? C36 C35 C34 119.9(7) . . ? C40 C35 C34 121.2(6) . . ? C37 C36 C35 123.5(7) . . ? C36 C37 C38 115.7(8) . . ? C36 C37 C41 123.7(8) . . ? C38 C37 C41 120.6(8) . . ? C39 C38 C37 123.3(8) . . ? C38 C39 C40 119.2(7) . . ? C38 C39 C45 119.3(7) . 2 ? C40 C39 C45 121.5(7) . 2 ? O4 C40 C39 120.9(7) . . ? O4 C40 C35 119.4(7) . . ? C39 C40 C35 119.7(7) . . ? C44 C41 C42 111.8(12) . . ? C44 C41 C37 112.8(9) . . ? C42 C41 C37 112.4(10) . . ? C44 C41 C43 110.8(10) . . ? C42 C41 C43 101.7(11) . . ? C37 C41 C43 106.7(10) . . ? C39 C45 C46 111.1(6) 2 . ? C47 C46 C51 119.7(7) . . ? C47 C46 C45 118.8(7) . . ? C51 C46 C45 121.4(7) . . ? C46 C47 C48 123.1(7) . . ? C49 C48 C47 115.5(7) . . ? C49 C48 C52 121.0(8) . . ? C47 C48 C52 123.5(8) . . ? C50 C49 C48 122.8(7) . . ? C49 C50 C51 119.4(7) . . ? C49 C50 C56 120.6(7) . . ? C51 C50 C56 119.9(6) . . ? O5 C51 C46 120.5(6) . . ? O5 C51 C50 119.9(7) . . ? C46 C51 C50 119.5(7) . . ? C53 C52 C55 109.4(11) . . ? C53 C52 C54 109.0(11) . . ? C55 C52 C54 107.3(10) . . ? C53 C52 C48 107.4(9) . . ? C55 C52 C48 110.7(8) . . ? C54 C52 C48 113.0(9) . . ? C50 C56 C57 111.5(6) . . ? C58 C57 C62 118.8(7) . . ? C58 C57 C56 120.7(6) . . ? C62 C57 C56 120.5(6) . . ? C57 C58 C59 123.2(7) . . ? C60 C59 C58 116.9(7) . . ? C60 C59 C63 123.0(7) . . ? C58 C59 C63 120.0(7) . . ? C59 C60 C61 121.9(7) . . ? C62 C61 C60 119.2(7) . . ? C62 C61 C23 121.3(7) . 2 ? C60 C61 C23 119.5(7) . 2 ? O6 C62 C61 120.2(6) . . ? O6 C62 C57 119.9(7) . . ? C61 C62 C57 119.9(7) . . ? C66 C63 C64 107.9(9) . . ? C66 C63 C65 107.0(8) . . ? C64 C63 C65 111.3(9) . . ? C66 C63 C59 109.0(8) . . ? C64 C63 C59 110.4(8) . . ? C65 C63 C59 111.0(7) . . ? O9 S2 C70 103.3(8) . . ? O9 S2 C69A 97.5(11) . . ? C70 S2 C69A 94.5(17) . . ? S2 O9 Cu3 129.6(5) . . ? O78 S10A C80A 106.7(18) . . ? O78 S10A C81A 102.1(18) . . ? C80A S10A C81A 97.3(17) . . ? O91 C91 C91A 65(8) . . ? O91 C91 O92 147(10) . . ? C91A C91 O92 128(10) . . ? O91 C91 S7 60(5) . . ? C91A C91 S7 64(6) . . ? O92 C91 S7 97(7) . . ? O91 C91 S6 100(6) . . ? C91A C91 S6 100(7) . . ? O92 C91 S6 51(5) . . ? S7 C91 S6 46(2) . . ? O91 C91 S6 75(5) . 2 ? C91A C91 S6 54(6) . 2 ? O92 C91 S6 90(6) . 2 ? S7 C91 S6 22.0(17) . 2 ? S6 C91 S6 46(2) . 2 ? O91 C91 S7 98(6) . 2 ? C91A C91 S7 78(6) . 2 ? O92 C91 S7 62(5) . 2 ? S7 C91 S7 39(2) . 2 ? S6 C91 S7 22.9(14) . 2 ? S6 C91 S7 28.0(9) 2 2 ? S6 S7 S6 94.8(19) . 2 ? S6 S7 O91 106(3) . . ? S6 S7 O91 146(3) 2 . ? S6 S7 C91A 102(3) . . ? S6 S7 C91A 102(4) 2 . ? O91 S7 C91A 47(3) . . ? S6 S7 C91 71(4) . . ? S6 S7 C91 131(4) 2 . ? O91 S7 C91 41(3) . . ? C91A S7 C91 42(3) . . ? S6 S7 S7 47.8(11) . 2 ? S6 S7 S7 47.2(11) 2 2 ? O91 S7 S7 147(2) . 2 ? C91A S7 S7 111(3) . 2 ? C91 S7 S7 106(4) . 2 ? S6 S7 O92 37.8(18) . . ? S6 S7 O92 115(2) 2 . ? O91 S7 O92 72(3) . . ? C91A S7 O92 67(4) . . ? C91 S7 O92 33(3) . . ? S7 S7 O92 76(2) 2 . ? S6 S7 O92 99(2) . 2 ? S6 S7 O92 25.3(15) 2 2 ? O91 S7 O92 122(3) . 2 ? C91A S7 O92 77(3) . 2 ? C91 S7 O92 108(3) . 2 ? S7 S7 O92 58.0(18) 2 2 ? O92 S7 O92 103(2) . 2 ? S6 S7 C90 78.0(11) . . ? S6 S7 C90 77.7(11) 2 . ? O91 S7 C90 133(2) . . ? C91A S7 C90 180(4) . . ? C91 S7 C90 138(4) . . ? S7 S7 C90 68.6(5) 2 . ? O92 S7 C90 113(2) . . ? O92 S7 C90 103.1(16) 2 . ? S6 S7 C91 74(2) . 2 ? S6 S7 C91 30(2) 2 2 ? O91 S7 C91 132(3) . 2 ? C91A S7 C91 85(3) . 2 ? C91 S7 C91 102(5) . 2 ? S7 S7 C91 35(2) 2 2 ? O92 S7 C91 85(2) . 2 ? O92 S7 C91 25(2) 2 2 ? C90 S7 C91 95(2) . 2 ? S6 S7 C91A 54(2) . 2 ? S6 S7 C91A 53(2) 2 2 ? O91 S7 C91A 120(3) . 2 ? C91A S7 C91A 80(5) . 2 ? C91 S7 C91A 83(4) . 2 ? S7 S7 C91A 31.3(17) 2 2 ? O92 S7 C91A 62(2) . 2 ? O92 S7 C91A 47(2) 2 2 ? C90 S7 C91A 99.9(18) . 2 ? C91 S7 C91A 24(2) 2 2 ? S7 C90 S7 42.8(10) 2 . ? S7 C90 S6 30.6(5) 2 2 ? S7 C90 S6 31.0(5) . 2 ? S7 C90 S6 31.0(5) 2 . ? S7 C90 S6 30.6(5) . . ? S6 C90 S6 45.4(8) 2 . ? C91 C91A O91 55(6) . . ? C91 C91A S7 74(6) . . ? O91 C91A S7 62(4) . . ? C91 C91A O92 26(6) . . ? O91 C91A O92 78(5) . . ? S7 C91A O92 70(4) . . ? C91 C91A S6 50(6) . . ? O91 C91A S6 73(4) . . ? S7 C91A S6 35.6(19) . . ? O92 C91A S6 36(2) . . ? C91 C91A S6 102(7) . 2 ? O91 C91A S6 96(5) . 2 ? S7 C91A S6 36(2) . 2 ? O92 C91A S6 86(3) . 2 ? S6 C91A S6 52.1(19) . 2 ? C91 C91A O92 124(7) . 2 ? O91 C91A O92 127(6) . 2 ? S7 C91A O92 67(3) . 2 ? O92 C91A O92 101(4) . 2 ? S6 C91A O92 76(3) . 2 ? S6 C91A O92 31.7(16) 2 2 ? C91 C91A S7 78(6) . 2 ? O91 C91A S7 95(5) . 2 ? S7 C91A S7 37(2) . 2 ? O92 C91A S7 58(3) . 2 ? S6 C91A S7 28.7(11) . 2 ? S6 C91A S7 28.4(10) 2 2 ? O92 C91A S7 46.9(19) 2 2 ? C91 O92 S6 87(6) . . ? C91 O92 C91A 26(6) . . ? S6 O92 C91A 78(3) . . ? C91 O92 S7 50(5) . . ? S6 O92 S7 37.0(18) . . ? C91A O92 S7 43(2) . . ? C91 O92 O91 16(5) . . ? S6 O92 O91 74(3) . . ? C91A O92 O91 33(2) . . ? S7 O92 O91 39.3(15) . . ? C91 O92 S7 93(6) . 2 ? S6 O92 S7 25.1(15) . 2 ? C91A O92 S7 75(3) . 2 ? S7 O92 S7 45.9(16) . 2 ? O91 O92 S7 85(2) . 2 ? C91 O92 C91A 102(6) . 2 ? S6 O92 C91A 61(3) . 2 ? C91A O92 C91A 77(4) . 2 ? S7 O92 C91A 71(2) . 2 ? O91 O92 C91A 103(3) . 2 ? S7 O92 C91A 35.7(19) 2 2 ? C91 O92 S6 67(5) . 2 ? S6 O92 S6 33.1(18) . 2 ? C91A O92 S6 49(2) . 2 ? S7 O92 S6 24.3(9) . 2 ? O91 O92 S6 60.4(18) . 2 ? S7 O92 S6 26.3(8) 2 2 ? C91A O92 S6 47(2) 2 2 ? O93 C151 C152 113.2(18) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 23.43 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.442 _refine_diff_density_min -1.221 _refine_diff_density_rms 0.123 # Attachment '2.CIF.txt' data_GK2583 _database_code_depnum_ccdc_archive 'CCDC 766940' #TrackingRef '2.CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common GK2583 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C157 H219 Cu9 N3 O36.75 S11' _chemical_formula_weight 3660.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.649(16) _cell_length_b 20.57(3) _cell_length_c 34.42(4) _cell_angle_alpha 89.20(3) _cell_angle_beta 86.79(4) _cell_angle_gamma 77.90(2) _cell_volume 8743(19) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8213 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 21.98 _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.391 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3826 _exptl_absorpt_coefficient_mu 1.273 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7848 _exptl_absorpt_correction_T_max 0.8832 _exptl_absorpt_process_details Bruker-SADABS _exptl_special_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _diffrn_ambient_temperature 100(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 Nonius X8 Apex II CCD Diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 105039 _diffrn_reflns_av_R_equivalents 0.1035 _diffrn_reflns_av_sigmaI/netI 0.1193 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 23.24 _reflns_number_total 24377 _reflns_number_gt 14643 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 2001)' _computing_publication_material 'local program' _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.Numerous restraints were applied to the model due to extensive disorder in tert-butyl groups of the calixarene molecules, co-crystallised solvent molecules, and in disordered non-coordinated nitrate anion. Due to this disorder, some atoms have been refined isotropically. Residual electron density is assocaited with the disordered nitrate anion in one position. The difference in calculated and reported formulae is due to disorder that could not be modelled appropriately, and where the formula contains the entire molecule(s). Due to the poorly diffracting nature/crystal quality, this has resulted in a higher Rint value than desired. Given the disorder around one of the coordinated nitrate anions, we have checked for lower symmetry, with no suggestion of this requirement. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0808P)^2^+24.8503P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 24377 _refine_ls_number_parameters 2058 _refine_ls_number_restraints 331 _refine_ls_R_factor_all 0.1325 _refine_ls_R_factor_gt 0.0664 _refine_ls_wR_factor_ref 0.1801 _refine_ls_wR_factor_gt 0.1507 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.027 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 1.02504(7) 0.22340(5) 0.17203(3) 0.0217(2) Uani 1 1 d . . . S1 S 1.41140(18) 0.05727(12) 0.24009(7) 0.0433(7) Uani 1 1 d . . . O1 O 0.8936(4) 0.2925(2) 0.16513(14) 0.0190(12) Uani 1 1 d . . . C1 C 0.8702(6) 0.3177(4) 0.0969(2) 0.022(2) Uani 1 1 d . G . Cu2 Cu 1.00871(7) 0.45125(4) 0.24953(3) 0.0175(2) Uani 1 1 d . . . S2 S 0.70634(18) 0.16112(13) 0.28950(8) 0.0471(7) Uani 1 1 d . . . O2 O 0.9390(4) 0.1658(2) 0.19953(15) 0.0243(13) Uani 1 1 d . G . C2 C 0.8174(6) 0.3105(4) 0.0626(2) 0.028(2) Uani 1 1 d . . . H2 H 0.8372 0.3315 0.0394 0.033 Uiso 1 1 calc R . . Cu3 Cu 1.07327(7) 0.21725(5) 0.32913(3) 0.0240(3) Uani 1 1 d . . . S3 S 1.30714(18) 0.41662(12) 0.12614(7) 0.0376(6) Uani 1 1 d . . . O3 O 1.1564(4) 0.1580(2) 0.18298(15) 0.0244(13) Uani 1 1 d . G . C3 C 0.7357(6) 0.2729(4) 0.0618(2) 0.025(2) Uani 1 1 d . . . Cu4 Cu 1.18216(7) 0.15633(5) 0.23898(3) 0.0238(3) Uani 1 1 d . . . S4 S 0.62855(17) 0.43350(11) 0.19492(7) 0.0316(6) Uani 1 1 d . . . O4 O 1.1146(4) 0.2820(2) 0.14785(15) 0.0209(13) Uani 1 1 d . G . C4 C 0.7094(6) 0.2432(4) 0.0967(3) 0.027(2) Uani 1 1 d . . . H4 H 0.6546 0.2179 0.0969 0.032 Uiso 1 1 calc R . . Cu5 Cu 0.92686(7) 0.17965(5) 0.25588(3) 0.0239(3) Uani 1 1 d . . . S5 S 1.4234(3) 0.35046(17) 0.31342(11) 0.0482(9) Uani 0.75 1 d P A 1 O5 O 0.9208(4) 0.4502(2) 0.29810(14) 0.0192(12) Uani 1 1 d . . . C5 C 0.7597(6) 0.2487(4) 0.1315(2) 0.0213(19) Uani 1 1 d . . . Cu6 Cu 1.12278(7) 0.36570(4) 0.17431(3) 0.0201(2) Uani 1 1 d . . . S6 S 1.3711(6) 0.3748(4) 0.3488(2) 0.0123(17) Uani 0.25 1 d P A 2 O6 O 0.8773(4) 0.4623(2) 0.21920(14) 0.0194(12) Uani 1 1 d . . . C6 C 0.8408(6) 0.2865(4) 0.1314(2) 0.0204(19) Uani 1 1 d . . . Cu7 Cu 0.87298(7) 0.37625(4) 0.19436(3) 0.0197(2) Uani 1 1 d . . . S7 S 0.73730(18) 0.41150(12) 0.39268(7) 0.0366(6) Uani 1 1 d . . . O7 O 1.0939(4) 0.4529(2) 0.20067(14) 0.0182(12) Uani 1 1 d . . . C7 C 0.7328(6) 0.2088(4) 0.1667(2) 0.024(2) Uani 1 1 d . . . H7A H 0.6543 0.2089 0.1682 0.029 Uiso 1 1 calc R . . H7B H 0.7501 0.2295 0.1907 0.029 Uiso 1 1 calc R . . Cu8 Cu 1.18248(7) 0.34481(5) 0.30655(3) 0.0244(3) Uani 1 1 d . A . S500 S 0.3816(7) 0.4136(4) 0.4506(2) 0.102(2) Uiso 0.50 1 d PDU B 1 O8 O 1.1415(4) 0.4329(2) 0.27967(14) 0.0209(12) Uani 1 1 d . A . N3 N 1.0713(10) 0.5476(6) 0.0235(3) 0.028(3) Uiso 0.50 1 d PDU . . O42 O 1.0482(17) 0.5034(10) 0.0031(6) 0.145(7) Uiso 0.50 1 d PDU . . C8 C 0.7975(6) 0.1371(4) 0.1637(3) 0.030(2) Uani 1 1 d . G . Cu9 Cu 0.92826(7) 0.36799(4) 0.32958(3) 0.0203(2) Uani 1 1 d . . . S504 S 0.3723(5) 0.4713(3) 0.45986(17) 0.0635(16) Uiso 0.50 1 d PDU C 2 O9 O 1.1893(4) 0.2640(2) 0.33953(14) 0.0226(13) Uani 1 1 d . . . C9 C 0.7604(7) 0.0897(4) 0.1415(2) 0.032(2) Uani 1 1 d . . . H9 H 0.6906 0.1011 0.1313 0.038 Uiso 1 1 calc R . . S10 S 0.9380(11) 0.7284(5) 0.2635(4) 0.061(3) Uani 0.25 1 d P D 2 O10 O 1.1739(4) 0.1509(2) 0.29651(15) 0.0243(13) Uani 1 1 d . G . C10 C 0.8256(7) 0.0253(4) 0.1340(2) 0.031(2) Uani 1 1 d . J . S11 S 1.0271(3) 0.71642(17) 0.24737(10) 0.0396(8) Uani 0.75 1 d P D 1 O11 O 0.9507(4) 0.1791(2) 0.31224(15) 0.0237(13) Uani 1 1 d . G . C11 C 0.9261(6) 0.0105(4) 0.1502(3) 0.032(2) Uani 1 1 d . . . H11 H 0.9700 -0.0326 0.1458 0.038 Uiso 1 1 calc R . . S12 S 1.0070(2) 0.06224(15) 0.04942(10) 0.0337(8) Uani 0.75 1 d P E 2 O12 O 0.9716(4) 0.2853(2) 0.35871(15) 0.0278(14) Uani 1 1 d . G . C12 C 0.9665(7) 0.0552(4) 0.1727(2) 0.029(2) Uani 1 1 d . G . S13 S 1.0031(8) 0.1113(6) 0.0247(3) 0.052(3) Uani 0.25 1 d P E 1 O13 O 1.0485(4) 0.2227(2) 0.24429(15) 0.0222(13) Uani 1 1 d . G . C13 C 0.9005(6) 0.1194(4) 0.1788(2) 0.026(2) Uani 1 1 d . . . O14 O 1.0168(4) 0.3475(2) 0.21405(14) 0.0198(12) Uani 1 1 d . . . C14 C 1.0788(6) 0.0356(4) 0.1884(3) 0.032(2) Uani 1 1 d . . . H14A H 1.0813 0.0620 0.2120 0.038 Uiso 1 1 calc R G . H14B H 1.0922 -0.0119 0.1961 0.038 Uiso 1 1 calc R . . S15 S 0.7825(9) 0.9203(5) 0.2326(4) 0.040(3) Uiso 0.25 1 d PU F 3 O15 O 1.0458(4) 0.3255(2) 0.29257(15) 0.0212(13) Uani 1 1 d . . . C15 C 1.1685(6) 0.0461(4) 0.1593(2) 0.026(2) Uani 1 1 d . G . S16 S 0.7741(7) 0.9128(5) 0.2513(3) 0.072(3) Uiso 0.50 1 d PU F 1 O16 O 1.3299(9) 0.2078(6) 0.2346(4) 0.040(3) Uani 0.50 1 d PU G 2 N2 N 0.7463(6) 0.3276(4) 0.2773(2) 0.0333(18) Uani 1 1 d . . . C16 C 1.2192(6) -0.0053(4) 0.1345(2) 0.029(2) Uani 1 1 d . . . H16 H 1.1991 -0.0472 0.1372 0.034 Uiso 1 1 calc R G . S17 S 0.7658(11) 0.9181(7) 0.2675(4) 0.055(3) Uiso 0.25 1 d PU F 2 O17 O 1.2572(9) 0.2628(6) 0.2458(3) 0.024(3) Uani 0.50 1 d PU G 1 N1 N 1.3215(6) 0.2714(4) 0.2196(2) 0.0310(16) Uani 1 1 d U . . C17 C 1.2994(6) 0.0025(4) 0.1056(2) 0.026(2) Uani 1 1 d . G . S18 S 1.3970(5) 0.4624(3) -0.0582(2) 0.0766(18) Uani 0.50 1 d PU H 1 O18 O 1.2434(11) 0.3079(7) 0.2314(4) 0.052(3) Uani 0.50 1 d PU G 2 C18 C 1.3272(6) 0.0656(4) 0.1034(2) 0.023(2) Uani 1 1 d . . . H18 H 1.3808 0.0728 0.0843 0.028 Uiso 1 1 calc R G . S19 S 1.3448(3) 0.52844(17) -0.05196(11) 0.0152(9) Uani 0.50 1 d PU H 2 O19 O 1.2967(7) 0.3269(4) 0.1970(3) 0.013(2) Uani 0.50 1 d PU G 1 C19 C 1.2793(6) 0.1172(4) 0.1281(2) 0.022(2) Uani 1 1 d . G . O20 O 1.3970(12) 0.2743(8) 0.1987(4) 0.047(3) Uani 0.50 1 d PU G 2 C20 C 1.2002(6) 0.1078(4) 0.1567(2) 0.023(2) Uani 1 1 d . . . O21 O 1.4092(9) 0.2329(6) 0.2117(4) 0.031(3) Uani 0.50 1 d PU G 1 C21 C 1.3086(6) 0.1858(4) 0.1234(2) 0.023(2) Uani 1 1 d . . . H21A H 1.3013 0.2080 0.1491 0.027 Uiso 1 1 calc R G . H21B H 1.3849 0.1804 0.1134 0.027 Uiso 1 1 calc R . . O22 O 0.7570(4) 0.3547(3) 0.30975(18) 0.0322(14) Uani 1 1 d . . . C22 C 1.2342(6) 0.2286(4) 0.0953(2) 0.0212(19) Uani 1 1 d . G . O23 O 0.8264(4) 0.3074(3) 0.25522(17) 0.0320(14) Uani 1 1 d . . . C23 C 1.2587(6) 0.2221(4) 0.0550(2) 0.024(2) Uani 1 1 d . . . H23 H 1.3226 0.1916 0.0463 0.028 Uiso 1 1 calc R G . O24 O 0.6536(5) 0.3226(4) 0.2684(2) 0.062(2) Uani 1 1 d . . . C24 C 1.1942(6) 0.2580(4) 0.0274(2) 0.0213(19) Uani 1 1 d . G . O25 O 1.2915(5) 0.0760(3) 0.23114(19) 0.0520(19) Uani 1 1 d . G . C25 C 1.0983(6) 0.3015(4) 0.0417(2) 0.022(2) Uani 1 1 d . . . H25 H 1.0513 0.3261 0.0236 0.026 Uiso 1 1 calc R G . O26 O 0.8047(4) 0.1369(3) 0.26124(18) 0.0402(16) Uani 1 1 d . G . C26 C 1.0707(6) 0.3094(4) 0.0812(2) 0.0209(19) Uani 1 1 d . G . O27 O 1.1972(4) 0.3951(3) 0.12886(16) 0.0380(16) Uani 1 1 d . G . C27 C 1.1391(6) 0.2727(4) 0.1086(2) 0.0221(19) Uani 1 1 d . . . O28 O 0.7358(4) 0.4115(3) 0.17173(16) 0.0306(14) Uani 1 1 d . G . C28 C 0.9624(6) 0.3549(4) 0.0940(2) 0.024(2) Uani 1 1 d . . . H28A H 0.9690 0.3745 0.1196 0.028 Uiso 1 1 calc R G . H28B H 0.9453 0.3918 0.0750 0.028 Uiso 1 1 calc R . . O29 O 1.3129(6) 0.3634(4) 0.3262(3) 0.084(3) Uani 1 1 d . . . C29 C 0.6855(6) 0.2636(4) 0.0225(2) 0.032(2) Uani 1 1 d . . . O30 O 0.8488(4) 0.4165(3) 0.37436(15) 0.0273(13) Uani 1 1 d . . . C30 C 0.6276(7) 0.3305(5) 0.0065(3) 0.045(3) Uani 1 1 d . . . H30A H 0.5932 0.3233 -0.0175 0.067 Uiso 1 1 calc R . . H30B H 0.6803 0.3586 0.0008 0.067 Uiso 1 1 calc R . . H30C H 0.5723 0.3524 0.0258 0.067 Uiso 1 1 calc R . . C502 C 0.275(2) 0.4735(13) 0.4290(8) 0.114(9) Uiso 0.50 1 d PDU B 1 H50A H 0.2347 0.4503 0.4122 0.137 Uiso 0.50 1 calc PR B 1 H50B H 0.3066 0.5056 0.4135 0.137 Uiso 0.50 1 calc PR B 1 H50C H 0.2254 0.4969 0.4496 0.137 Uiso 0.50 1 calc PR B 1 C31 C 0.6046(7) 0.2170(5) 0.0270(3) 0.047(3) Uani 1 1 d . . . H31A H 0.5489 0.2342 0.0474 0.070 Uiso 1 1 calc R . . H31B H 0.6431 0.1724 0.0342 0.070 Uiso 1 1 calc R . . H31C H 0.5704 0.2149 0.0023 0.070 Uiso 1 1 calc R . . O505 O 0.4784(13) 0.4524(8) 0.4400(5) 0.077(4) Uiso 0.50 1 d PU C 2 C32 C 0.7768(6) 0.2326(4) -0.0070(2) 0.033(2) Uani 1 1 d . . . H32A H 0.8130 0.1889 0.0024 0.050 Uiso 1 1 calc R . . H32B H 0.8292 0.2615 -0.0101 0.050 Uiso 1 1 calc R . . H32C H 0.7465 0.2277 -0.0321 0.050 Uiso 1 1 calc R . . O33 O 0.9961(6) 0.7670(3) 0.2779(3) 0.078(3) Uani 1 1 d . . . C33 C 0.7816(8) -0.0266(5) 0.1104(3) 0.047(3) Uani 1 1 d . . . O454 O 1.087(2) 0.4332(9) 0.5243(7) 0.105(9) Uiso 0.25 1 d PDU I -2 C34 C 0.7106(8) 0.0063(6) 0.0789(4) 0.081(4) Uani 1 1 d . J . H34A H 0.6909 -0.0279 0.0628 0.121 Uiso 1 1 calc R . . H34B H 0.7500 0.0337 0.0625 0.121 Uiso 1 1 calc R . . H34C H 0.6448 0.0343 0.0907 0.121 Uiso 1 1 calc R . . O35 O 0.9088(5) 0.0726(3) 0.0248(2) 0.068(2) Uani 1 1 d . . . C35 C 0.7478(18) -0.0764(10) 0.1402(7) 0.070(7) Uani 0.50 1 d P J 2 H35A H 0.6853 -0.0538 0.1565 0.084 Uiso 0.50 1 calc PR J 2 H35B H 0.8083 -0.0940 0.1566 0.084 Uiso 0.50 1 calc PR J 2 H35C H 0.7282 -0.1131 0.1263 0.084 Uiso 0.50 1 calc PR J 2 O36 O 1.1121(6) 0.8640(4) 0.2885(2) 0.077(2) Uiso 1 1 d . . . C36 C 0.8743(8) -0.0775(5) 0.0919(3) 0.070(4) Uani 1 1 d . J . H36A H 0.8453 -0.1108 0.0782 0.105 Uiso 1 1 calc R . . H36B H 0.9208 -0.0994 0.1122 0.105 Uiso 1 1 calc R . . H36C H 0.9168 -0.0553 0.0734 0.105 Uiso 1 1 calc R . . C37 C 1.3561(7) -0.0572(4) 0.0805(3) 0.034(2) Uani 1 1 d . . . O38 O 1.1356(14) 0.5850(9) 0.0313(6) 0.116(6) Uiso 0.50 1 d PDU . . C38 C 1.2708(9) -0.0916(5) 0.0630(3) 0.068(4) Uani 1 1 d . G . H38A H 1.3080 -0.1292 0.0468 0.102 Uiso 1 1 calc R . . H38B H 1.2231 -0.0595 0.0470 0.102 Uiso 1 1 calc R . . H38C H 1.2275 -0.1075 0.0841 0.102 Uiso 1 1 calc R . . O39 O 0.9846(14) 0.5539(11) 0.0452(6) 0.132(7) Uiso 0.50 1 d PDU . . C39 C 1.4293(10) -0.1068(5) 0.1062(3) 0.083(4) Uani 1 1 d . G . H39A H 1.4857 -0.0861 0.1158 0.124 Uiso 1 1 calc R . . H39B H 1.4631 -0.1463 0.0909 0.124 Uiso 1 1 calc R . . H39C H 1.3859 -0.1199 0.1283 0.124 Uiso 1 1 calc R . . C40 C 1.4247(7) -0.0358(5) 0.0459(3) 0.042(3) Uani 1 1 d . G . H40A H 1.4814 -0.0155 0.0558 0.064 Uiso 1 1 calc R . . H40B H 1.3780 -0.0034 0.0298 0.064 Uiso 1 1 calc R . . H40C H 1.4581 -0.0748 0.0302 0.064 Uiso 1 1 calc R . . C41 C 1.2254(6) 0.2545(4) -0.0173(2) 0.029(2) Uani 1 1 d . . . C42 C 1.2746(8) 0.3146(5) -0.0277(3) 0.047(3) Uani 1 1 d . G . H42A H 1.2231 0.3554 -0.0199 0.071 Uiso 1 1 calc R . . H42B H 1.2908 0.3155 -0.0559 0.071 Uiso 1 1 calc R . . H42C H 1.3416 0.3115 -0.0142 0.071 Uiso 1 1 calc R . . C43 C 1.1251(7) 0.2575(4) -0.0417(2) 0.034(2) Uani 1 1 d . G . H43A H 1.0763 0.3011 -0.0383 0.052 Uiso 1 1 calc R . . H43B H 1.0871 0.2226 -0.0329 0.052 Uiso 1 1 calc R . . H43C H 1.1486 0.2508 -0.0692 0.052 Uiso 1 1 calc R . . C44 C 1.3091(7) 0.1904(4) -0.0277(2) 0.034(2) Uani 1 1 d . G . H44A H 1.3231 0.1879 -0.0560 0.051 Uiso 1 1 calc R . . H44B H 1.2807 0.1517 -0.0186 0.051 Uiso 1 1 calc R . . H44C H 1.3766 0.1908 -0.0152 0.051 Uiso 1 1 calc R . . C45 C 0.9428(6) 0.5343(4) 0.3433(2) 0.026(2) Uani 1 1 d . G . C46 C 0.9005(7) 0.5952(4) 0.3615(3) 0.038(2) Uani 1 1 d . . . H46 H 0.9409 0.6104 0.3806 0.045 Uiso 1 1 calc R . . C47 C 0.7997(7) 0.6349(4) 0.3524(3) 0.041(3) Uani 1 1 d . K . C48 C 0.7428(6) 0.6111(4) 0.3244(3) 0.035(2) Uani 1 1 d . . . H48 H 0.6753 0.6373 0.3176 0.042 Uiso 1 1 calc R . . C49 C 0.7814(6) 0.5492(4) 0.3056(2) 0.025(2) Uani 1 1 d . . . C50 C 0.8822(6) 0.5110(4) 0.3152(2) 0.0209(19) Uani 1 1 d . . . C51 C 0.7145(6) 0.5262(4) 0.2752(2) 0.025(2) Uani 1 1 d . . . H51A H 0.7334 0.4771 0.2735 0.029 Uiso 1 1 calc R . . H51B H 0.6367 0.5395 0.2833 0.029 Uiso 1 1 calc R . . C52 C 0.7342(6) 0.5556(4) 0.2356(2) 0.0205(19) Uani 1 1 d . G . C53 C 0.6726(6) 0.6186(4) 0.2249(3) 0.028(2) Uani 1 1 d . . . H53 H 0.6152 0.6397 0.2423 0.034 Uiso 1 1 calc R . . C54 C 0.6913(7) 0.6506(4) 0.1907(3) 0.032(2) Uani 1 1 d . L . C55 C 0.7775(6) 0.6189(4) 0.1660(2) 0.026(2) Uani 1 1 d . . . H55 H 0.7929 0.6401 0.1423 0.031 Uiso 1 1 calc R . . C56 C 0.8419(6) 0.5569(4) 0.1748(2) 0.0210(19) Uani 1 1 d . G . C57 C 0.8188(6) 0.5241(4) 0.2094(2) 0.0205(19) Uani 1 1 d . . . C58 C 0.9409(6) 0.5278(4) 0.1480(2) 0.0208(19) Uani 1 1 d . . . H58A H 0.9529 0.4787 0.1488 0.025 Uiso 1 1 calc R G . H58B H 0.9258 0.5422 0.1209 0.025 Uiso 1 1 calc R . . C59 C 1.0435(6) 0.5489(4) 0.1592(2) 0.0182(18) Uani 1 1 d . G . C60 C 1.0679(6) 0.6075(4) 0.1432(2) 0.023(2) Uani 1 1 d . . . H60 H 1.0201 0.6326 0.1256 0.028 Uiso 1 1 calc R G . C61 C 1.1613(6) 0.6305(4) 0.1526(2) 0.0221(19) Uani 1 1 d . G . C62 C 1.2287(6) 0.5908(4) 0.1786(2) 0.024(2) Uani 1 1 d . . . H62 H 1.2926 0.6044 0.1852 0.028 Uiso 1 1 calc R G . C63 C 1.2072(6) 0.5328(4) 0.1951(2) 0.0189(18) Uani 1 1 d . G . C64 C 1.1138(6) 0.5115(4) 0.1850(2) 0.0176(18) Uani 1 1 d . . . C65 C 1.2798(6) 0.4926(3) 0.2251(2) 0.0176(18) Uani 1 1 d . . . H65A H 1.2756 0.4452 0.2234 0.021 Uiso 1 1 calc R G . H65B H 1.3559 0.4958 0.2188 0.021 Uiso 1 1 calc R . . C66 C 1.2471(6) 0.5171(4) 0.2665(2) 0.0191(19) Uani 1 1 d . G . C67 C 1.2862(6) 0.5725(4) 0.2793(2) 0.023(2) Uani 1 1 d . . . H67 H 1.3322 0.5920 0.2621 0.027 Uiso 1 1 calc R G . C68 C 1.2588(6) 0.5992(4) 0.3164(2) 0.024(2) Uani 1 1 d . G . C69 C 1.1869(6) 0.5705(4) 0.3401(2) 0.024(2) Uani 1 1 d . . . H69 H 1.1669 0.5880 0.3654 0.029 Uiso 1 1 calc R G . C70 C 1.1438(6) 0.5179(4) 0.3282(2) 0.023(2) Uani 1 1 d . G . C71 C 1.1780(6) 0.4882(3) 0.2912(2) 0.0183(19) Uani 1 1 d . . . C72 C 1.0537(6) 0.4951(4) 0.3535(2) 0.026(2) Uani 1 1 d . . . H72A H 1.0577 0.4471 0.3493 0.031 Uiso 1 1 calc R G . H72B H 1.0646 0.5016 0.3813 0.031 Uiso 1 1 calc R . . C73 C 0.7505(7) 0.7023(5) 0.3723(3) 0.064(4) Uani 1 1 d D . . C74 C 0.745(2) 0.7595(12) 0.3433(7) 0.076(8) Uiso 0.50 1 d PD K 1 H74A H 0.7308 0.8018 0.3573 0.113 Uiso 0.50 1 calc PR K 1 H74B H 0.6856 0.7593 0.3260 0.113 Uiso 0.50 1 calc PR K 1 H74C H 0.8132 0.7542 0.3278 0.113 Uiso 0.50 1 calc PR K 1 C75 C 0.8217(13) 0.7161(9) 0.4060(5) 0.035(5) Uiso 0.50 1 d PD K 1 H75A H 0.8951 0.7166 0.3954 0.052 Uiso 0.50 1 calc PR K 1 H75B H 0.8249 0.6811 0.4258 0.052 Uiso 0.50 1 calc PR K 1 H75C H 0.7896 0.7593 0.4179 0.052 Uiso 0.50 1 calc PR K 1 C76 C 0.6450(8) 0.6996(5) 0.3936(3) 0.063(3) Uiso 1 1 d D K . H76A H 0.6569 0.6648 0.4137 0.094 Uiso 1 1 calc R . . H76B H 0.5942 0.6895 0.3753 0.094 Uiso 1 1 calc R . . H76C H 0.6148 0.7426 0.4060 0.094 Uiso 1 1 calc R . . C77 C 0.5005(15) 0.7088(15) 0.1780(10) 0.043(6) Uiso 0.33 1 d PDU L 3 H77A H 0.4839 0.6835 0.2011 0.052 Uiso 0.33 1 calc PR L 3 H77B H 0.4897 0.6852 0.1545 0.052 Uiso 0.33 1 calc PR L 3 H77C H 0.4525 0.7529 0.1785 0.052 Uiso 0.33 1 calc PR L 3 C78 C 0.663(3) 0.7532(19) 0.1451(9) 0.037(7) Uiso 0.33 1 d PDU L 3 H78A H 0.7383 0.7536 0.1497 0.045 Uiso 0.33 1 calc PR L 3 H78B H 0.6209 0.7991 0.1441 0.045 Uiso 0.33 1 calc PR L 3 H78C H 0.6590 0.7311 0.1203 0.045 Uiso 0.33 1 calc PR L 3 C79 C 0.605(2) 0.7642(13) 0.2156(7) 0.038(6) Uiso 0.33 1 d PDU L 3 H79A H 0.6759 0.7741 0.2200 0.045 Uiso 0.33 1 calc PR L 3 H79B H 0.5801 0.7416 0.2385 0.045 Uiso 0.33 1 calc PR L 3 H79C H 0.5530 0.8057 0.2110 0.045 Uiso 0.33 1 calc PR L 3 C80 C 0.6157(6) 0.7162(4) 0.1778(2) 0.041(2) Uani 1 1 d DU . . C81 C 1.1926(7) 0.6922(4) 0.1330(3) 0.034(2) Uani 1 1 d . . . C82 C 1.1018(7) 0.7334(5) 0.1095(3) 0.048(3) Uani 1 1 d . G . H82A H 1.0872 0.7067 0.0879 0.071 Uiso 1 1 calc R . . H82B H 1.1244 0.7733 0.0992 0.071 Uiso 1 1 calc R . . H82C H 1.0360 0.7464 0.1264 0.071 Uiso 1 1 calc R . . C83 C 1.2934(7) 0.6680(5) 0.1046(3) 0.045(3) Uani 1 1 d . G . H83A H 1.3501 0.6385 0.1186 0.067 Uiso 1 1 calc R . . H83B H 1.3209 0.7065 0.0946 0.067 Uiso 1 1 calc R . . H83C H 1.2727 0.6439 0.0829 0.067 Uiso 1 1 calc R . . C84 C 1.2212(8) 0.7380(5) 0.1639(3) 0.048(3) Uani 1 1 d . G . H84A H 1.1582 0.7527 0.1820 0.072 Uiso 1 1 calc R . . H84B H 1.2416 0.7768 0.1512 0.072 Uiso 1 1 calc R . . H84C H 1.2819 0.7137 0.1783 0.072 Uiso 1 1 calc R . . C85 C 1.3060(6) 0.6568(4) 0.3312(3) 0.029(2) Uani 1 1 d . . . C86 C 1.3780(9) 0.6831(5) 0.3008(3) 0.057(3) Uani 1 1 d . G . H86A H 1.4417 0.6482 0.2939 0.086 Uiso 1 1 calc R . . H86B H 1.4012 0.7216 0.3112 0.086 Uiso 1 1 calc R . . H86C H 1.3375 0.6964 0.2775 0.086 Uiso 1 1 calc R . . C87 C 1.3766(8) 0.6313(5) 0.3663(3) 0.050(3) Uani 1 1 d . G . H87A H 1.3312 0.6166 0.3872 0.075 Uiso 1 1 calc R . . H87B H 1.4081 0.6673 0.3758 0.075 Uiso 1 1 calc R . . H87C H 1.4347 0.5939 0.3578 0.075 Uiso 1 1 calc R . . C88 C 1.2136(7) 0.7140(4) 0.3455(3) 0.042(3) Uani 1 1 d . G . H88A H 1.1664 0.7292 0.3241 0.063 Uiso 1 1 calc R . . H88B H 1.2440 0.7509 0.3543 0.063 Uiso 1 1 calc R . . H88C H 1.1714 0.6984 0.3670 0.063 Uiso 1 1 calc R . . C89 C 1.2137(6) 0.2769(4) 0.4085(2) 0.026(2) Uani 1 1 d . G . C90 C 1.2736(7) 0.2550(4) 0.4412(3) 0.035(2) Uani 1 1 d . . . H90 H 1.2509 0.2757 0.4656 0.042 Uiso 1 1 calc R . . C91 C 1.3672(7) 0.2025(4) 0.4387(3) 0.032(2) Uani 1 1 d . M . C92 C 1.3969(6) 0.1743(4) 0.4023(2) 0.027(2) Uani 1 1 d . . . H92 H 1.4598 0.1398 0.3999 0.032 Uiso 1 1 calc R . . C93 C 1.3405(6) 0.1933(4) 0.3692(2) 0.026(2) Uani 1 1 d . . . C94 C 1.2473(6) 0.2458(4) 0.3725(2) 0.024(2) Uani 1 1 d . . . C95 C 1.3729(6) 0.1552(4) 0.3314(2) 0.026(2) Uani 1 1 d . . . H95A H 1.4528 0.1424 0.3283 0.031 Uiso 1 1 calc R . . H95B H 1.3466 0.1841 0.3092 0.031 Uiso 1 1 calc R . . C96 C 1.3250(6) 0.0925(4) 0.3312(2) 0.026(2) Uani 1 1 d . G . C97 C 1.3776(7) 0.0341(4) 0.3498(3) 0.033(2) Uani 1 1 d . . . H97 H 1.4450 0.0334 0.3608 0.040 Uiso 1 1 calc R . . C98 C 1.3335(7) -0.0231(4) 0.3524(3) 0.045(3) Uani 1 1 d . . . C99 C 1.2325(7) -0.0186(4) 0.3358(3) 0.046(3) Uani 1 1 d . . . H99 H 1.2001 -0.0563 0.3373 0.055 Uiso 1 1 calc R . . C100 C 1.1780(6) 0.0387(4) 0.3174(3) 0.031(2) Uani 1 1 d . G . C101 C 1.2251(6) 0.0939(4) 0.3153(2) 0.027(2) Uani 1 1 d . . . C102 C 1.0656(6) 0.0400(4) 0.3021(3) 0.034(2) Uani 1 1 d . . . H10A H 1.0545 0.0702 0.2794 0.041 Uiso 1 1 calc R G . H10B H 1.0622 -0.0051 0.2934 0.041 Uiso 1 1 calc R . . C103 C 0.9755(7) 0.0632(4) 0.3333(3) 0.035(2) Uani 1 1 d . G . C104 C 0.9483(7) 0.0164(5) 0.3591(3) 0.051(3) Uani 1 1 d . . . H104 H 0.9825 -0.0290 0.3554 0.061 Uiso 1 1 calc R G . C105 C 0.8717(8) 0.0335(5) 0.3905(4) 0.063(4) Uani 1 1 d . G . C106 C 0.8236(8) 0.1022(5) 0.3949(3) 0.054(3) Uani 1 1 d . . . H106 H 0.7726 0.1159 0.4161 0.065 Uiso 1 1 calc R G . C107 C 0.8491(6) 0.1494(4) 0.3694(3) 0.038(2) Uani 1 1 d . G . C108 C 0.9250(6) 0.1320(4) 0.3378(3) 0.031(2) Uani 1 1 d . . . C109 C 0.7977(7) 0.2226(4) 0.3786(3) 0.039(2) Uani 1 1 d . . . H10C H 0.7987 0.2495 0.3546 0.047 Uiso 1 1 calc R G . H10D H 0.7212 0.2262 0.3879 0.047 Uiso 1 1 calc R . . C110 C 0.8582(7) 0.2501(4) 0.4096(3) 0.037(2) Uani 1 1 d . G . C111 C 0.8331(7) 0.2434(5) 0.4492(3) 0.046(3) Uani 1 1 d . . . H111 H 0.7720 0.2254 0.4571 0.056 Uiso 1 1 calc R G . C112 C 0.8946(8) 0.2622(5) 0.4778(3) 0.054(3) Uani 1 1 d D G . C113 C 0.9830(8) 0.2908(5) 0.4652(3) 0.049(3) Uani 1 1 d . . . H113 H 1.0249 0.3049 0.4842 0.059 Uiso 1 1 calc R G . C114 C 1.0115(6) 0.2991(4) 0.4256(2) 0.031(2) Uani 1 1 d . G . C115 C 0.9473(7) 0.2783(4) 0.3976(3) 0.032(2) Uani 1 1 d . . . C116 C 1.1086(6) 0.3290(4) 0.4132(2) 0.029(2) Uani 1 1 d . . . H11A H 1.1169 0.3619 0.4329 0.035 Uiso 1 1 calc R G . H11B H 1.0948 0.3528 0.3882 0.035 Uiso 1 1 calc R . . C117 C 1.4317(8) 0.1791(5) 0.4751(3) 0.050(3) Uani 1 1 d DU . . C118 C 1.462(3) 0.2430(11) 0.4939(9) 0.060(6) Uani 0.33 1 d PDU M 2 H11C H 1.5088 0.2620 0.4754 0.072 Uiso 0.33 1 calc PR M 2 H11D H 1.4997 0.2300 0.5178 0.072 Uiso 0.33 1 calc PR M 2 H11E H 1.3954 0.2762 0.5001 0.072 Uiso 0.33 1 calc PR M 2 C119 C 1.5453(11) 0.1904(9) 0.4679(5) 0.064(4) Uani 0.67 1 d PDU M 1 H11F H 1.5753 0.1714 0.4427 0.077 Uiso 0.67 1 calc PR M 1 H11G H 1.5906 0.1689 0.4886 0.077 Uiso 0.67 1 calc PR M 1 H11H H 1.5438 0.2382 0.4678 0.077 Uiso 0.67 1 calc PR M 1 C120 C 1.5377(19) 0.1279(15) 0.4689(8) 0.052(6) Uani 0.33 1 d PDU M 2 H12A H 1.5831 0.1432 0.4482 0.062 Uiso 0.33 1 calc PR M 2 H12B H 1.5219 0.0852 0.4614 0.062 Uiso 0.33 1 calc PR M 2 H12C H 1.5760 0.1222 0.4931 0.062 Uiso 0.33 1 calc PR M 2 C121 C 1.4420(14) 0.1013(6) 0.4791(4) 0.063(4) Uani 0.67 1 d PDU M 1 H12D H 1.4788 0.0794 0.4554 0.075 Uiso 0.67 1 calc PR M 1 H12E H 1.3696 0.0913 0.4826 0.075 Uiso 0.67 1 calc PR M 1 H12F H 1.4839 0.0849 0.5016 0.075 Uiso 0.67 1 calc PR M 1 C122 C 1.360(2) 0.1560(17) 0.5071(8) 0.057(6) Uani 0.33 1 d PDU M 2 H12G H 1.2925 0.1891 0.5108 0.069 Uiso 0.33 1 calc PR M 2 H12H H 1.3980 0.1504 0.5314 0.069 Uiso 0.33 1 calc PR M 2 H12I H 1.3440 0.1134 0.4998 0.069 Uiso 0.33 1 calc PR M 2 C123 C 1.3749(15) 0.2057(10) 0.5124(4) 0.072(5) Uani 0.67 1 d PDU M 1 H12J H 1.3021 0.1962 0.5142 0.086 Uiso 0.67 1 calc PR M 1 H12K H 1.3696 0.2539 0.5133 0.086 Uiso 0.67 1 calc PR M 1 H12L H 1.4157 0.1846 0.5342 0.086 Uiso 0.67 1 calc PR M 1 C124 C 1.3904(9) -0.0877(5) 0.3723(5) 0.085(4) Uani 1 1 d U . . C125 C 1.4964(9) -0.0808(5) 0.3889(4) 0.073(4) Uani 1 1 d U . . H19 H 1.4816 -0.0478 0.4098 0.109 Uiso 1 1 calc R . . H20 H 1.5431 -0.0664 0.3683 0.109 Uiso 1 1 calc R . . H21 H 1.5328 -0.1238 0.3993 0.109 Uiso 1 1 calc R . . O126 O 1.4547(6) 0.5258(4) -0.0737(2) 0.081(3) Uani 1 1 d . . . C126 C 1.4133(13) -0.1436(6) 0.3430(5) 0.140(6) Uani 1 1 d U . . H22 H 1.4734 -0.1380 0.3249 0.210 Uiso 1 1 calc R . . H24 H 1.3486 -0.1429 0.3285 0.210 Uiso 1 1 calc R . . H26 H 1.4327 -0.1863 0.3567 0.210 Uiso 1 1 calc R . . C127 C 1.3174(12) -0.1083(8) 0.4046(6) 0.154(6) Uani 1 1 d U . . H27 H 1.3508 -0.1524 0.4143 0.231 Uiso 1 1 calc R . . H28 H 1.2471 -0.1097 0.3944 0.231 Uiso 1 1 calc R . . H29 H 1.3071 -0.0761 0.4259 0.231 Uiso 1 1 calc R . . C128 C 0.8476(12) -0.0170(7) 0.4230(4) 0.101(4) Uiso 1 1 d DU . . C150 C 0.8496(14) 0.1694(8) 0.5248(5) 0.040(5) Uiso 0.50 1 d PD G 2 H15A H 0.7953 0.1605 0.5075 0.048 Uiso 0.50 1 calc PR G 2 H15B H 0.8267 0.1619 0.5519 0.048 Uiso 0.50 1 calc PR G 2 H15C H 0.9194 0.1396 0.5183 0.048 Uiso 0.50 1 calc PR G 2 C151 C 0.8611(11) 0.2410(8) 0.5198(4) 0.031(5) Uiso 0.50 1 d PD G 2 C152 C 0.8686(13) 0.2744(9) 0.5230(4) 0.044(5) Uiso 0.50 1 d PD G 1 C155 C 0.7521(13) 0.2928(10) 0.5301(6) 0.039(5) Uiso 0.50 1 d PD G 2 H15D H 0.7641 0.3381 0.5262 0.047 Uiso 0.50 1 calc PR G 2 H15E H 0.7286 0.2869 0.5573 0.047 Uiso 0.50 1 calc PR G 2 H15F H 0.6961 0.2855 0.5130 0.047 Uiso 0.50 1 calc PR G 2 C156 C 0.858(2) 0.3447(10) 0.5419(7) 0.081(8) Uiso 0.50 1 d PD G 1 H15G H 0.9251 0.3608 0.5359 0.097 Uiso 0.50 1 calc PR G 1 H15H H 0.8471 0.3411 0.5702 0.097 Uiso 0.50 1 calc PR G 1 H15I H 0.7969 0.3758 0.5316 0.097 Uiso 0.50 1 calc PR G 1 C157 C 0.7615(17) 0.2557(14) 0.5348(8) 0.079(8) Uiso 0.50 1 d PD G 1 H15J H 0.7038 0.2829 0.5202 0.095 Uiso 0.50 1 calc PR G 1 H15K H 0.7454 0.2635 0.5628 0.095 Uiso 0.50 1 calc PR G 1 H15L H 0.7662 0.2086 0.5291 0.095 Uiso 0.50 1 calc PR G 1 C158 C 0.9566(17) 0.2322(12) 0.5460(7) 0.054(8) Uiso 0.50 1 d PD G 1 H15M H 1.0264 0.2436 0.5384 0.065 Uiso 0.50 1 calc PR G 1 H15N H 0.9604 0.1851 0.5406 0.065 Uiso 0.50 1 calc PR G 1 H15O H 0.9400 0.2407 0.5739 0.065 Uiso 0.50 1 calc PR G 1 C160 C 0.9464(16) 0.2594(12) 0.5460(6) 0.046(7) Uiso 0.50 1 d PD G 2 H16A H 0.9503 0.3060 0.5416 0.055 Uiso 0.50 1 calc PR G 2 H16B H 1.0174 0.2309 0.5395 0.055 Uiso 0.50 1 calc PR G 2 H16C H 0.9254 0.2529 0.5734 0.055 Uiso 0.50 1 calc PR G 2 C180 C 1.4299(8) -0.0302(5) 0.2448(4) 0.076(4) Uani 1 1 d . . . H18A H 1.3940 -0.0411 0.2693 0.114 Uiso 1 1 calc R . . H18B H 1.5075 -0.0500 0.2448 0.114 Uiso 1 1 calc R . . H18C H 1.3985 -0.0480 0.2229 0.114 Uiso 1 1 calc R . . C181 C 1.4808(8) 0.0621(6) 0.1947(3) 0.059(3) Uani 1 1 d . . . H18D H 1.4506 0.0381 0.1752 0.088 Uiso 1 1 calc R . . H18E H 1.5578 0.0421 0.1968 0.088 Uiso 1 1 calc R . . H18F H 1.4729 0.1088 0.1869 0.088 Uiso 1 1 calc R . . C182 C 0.6797(8) 0.0854(5) 0.3116(4) 0.080(4) Uani 1 1 d . . . H18G H 0.6727 0.0541 0.2912 0.119 Uiso 1 1 calc R . . H18H H 0.6124 0.0957 0.3279 0.119 Uiso 1 1 calc R . . H18I H 0.7398 0.0655 0.3277 0.119 Uiso 1 1 calc R . . C183 C 0.5957(8) 0.1788(6) 0.2577(3) 0.063(3) Uani 1 1 d . . . H18J H 0.5963 0.2209 0.2440 0.095 Uiso 1 1 calc R . . H18K H 0.5271 0.1824 0.2730 0.095 Uiso 1 1 calc R . . H18L H 0.6033 0.1429 0.2387 0.095 Uiso 1 1 calc R . . C184 C 1.3944(8) 0.3525(5) 0.0975(3) 0.053(3) Uani 1 1 d . . . H18M H 1.4139 0.3122 0.1133 0.079 Uiso 1 1 calc R . . H18N H 1.4602 0.3676 0.0886 0.079 Uiso 1 1 calc R . . H18O H 1.3566 0.3426 0.0749 0.079 Uiso 1 1 calc R . . C185 C 1.2879(8) 0.4813(5) 0.0907(3) 0.050(3) Uani 1 1 d . . . H18P H 1.2613 0.4654 0.0671 0.074 Uiso 1 1 calc R . . H18Q H 1.3570 0.4945 0.0842 0.074 Uiso 1 1 calc R . . H18R H 1.2349 0.5197 0.1011 0.074 Uiso 1 1 calc R . . C186 C 0.5569(7) 0.3716(4) 0.1843(3) 0.043(3) Uani 1 1 d . . . H18S H 0.5523 0.3689 0.1560 0.065 Uiso 1 1 calc R . . H18T H 0.4838 0.3829 0.1967 0.065 Uiso 1 1 calc R . . H18U H 0.5949 0.3286 0.1942 0.065 Uiso 1 1 calc R . . C187 C 0.5580(7) 0.5010(4) 0.1659(3) 0.043(3) Uani 1 1 d . . . H18V H 0.5987 0.5366 0.1643 0.064 Uiso 1 1 calc R . . H18W H 0.4857 0.5180 0.1780 0.064 Uiso 1 1 calc R . . H18Z H 0.5514 0.4849 0.1397 0.064 Uiso 1 1 calc R . . C188 C 0.7484(8) 0.4235(6) 0.4428(3) 0.062(3) Uani 1 1 d . . . H1 H 0.7959 0.3844 0.4536 0.092 Uiso 1 1 calc R . . H3 H 0.6765 0.4300 0.4561 0.092 Uiso 1 1 calc R . . H5 H 0.7790 0.4628 0.4465 0.092 Uiso 1 1 calc R . . C189 C 0.6532(7) 0.4898(5) 0.3823(3) 0.055(3) Uani 1 1 d . . . H6 H 0.6905 0.5254 0.3882 0.082 Uiso 1 1 calc R . . H7 H 0.5853 0.4953 0.3982 0.082 Uiso 1 1 calc R . . H8 H 0.6376 0.4919 0.3547 0.082 Uiso 1 1 calc R . . C190 C 1.4988(9) 0.3138(6) 0.3545(4) 0.092(5) Uani 0.75 1 d P A 1 H19A H 1.4910 0.2677 0.3579 0.110 Uiso 0.75 1 calc PR A 1 H19B H 1.4705 0.3391 0.3781 0.110 Uiso 0.75 1 calc PR A 1 H19C H 1.5755 0.3149 0.3497 0.110 Uiso 0.75 1 calc PR A 1 C191 C 1.4610(9) 0.4298(6) 0.3187(5) 0.117(7) Uani 0.75 1 d P A 1 H19D H 1.4283 0.4604 0.2985 0.141 Uiso 0.75 1 calc PR A 1 H19E H 1.5400 0.4238 0.3160 0.141 Uiso 0.75 1 calc PR A 1 H19F H 1.4351 0.4482 0.3444 0.141 Uiso 0.75 1 calc PR A 1 O501 O 0.4854(14) 0.4108(8) 0.4280(5) 0.087(5) Uiso 0.50 1 d PU B 1 C302 C 0.9914(8) 0.6415(4) 0.2626(3) 0.042(2) Uani 0.75 1 d P D 1 H30D H 1.0395 0.6206 0.2826 0.051 Uiso 0.75 1 calc PR D 1 H30E H 0.9984 0.6115 0.2403 0.051 Uiso 0.75 1 calc PR D 1 H30F H 0.9163 0.6507 0.2733 0.051 Uiso 0.75 1 calc PR D 1 C303 C 0.9246(10) 0.7380(5) 0.2123(3) 0.069(3) Uani 0.75 1 d P D 1 H30G H 0.9305 0.7803 0.1998 0.083 Uiso 0.75 1 calc PR D 1 H30H H 0.8528 0.7423 0.2255 0.083 Uiso 0.75 1 calc PR D 1 H30I H 0.9350 0.7031 0.1925 0.083 Uiso 0.75 1 calc PR D 1 C304 C 0.9940(7) 0.1389(5) 0.0760(3) 0.044(3) Uani 0.75 1 d P E 2 H30J H 0.9332 0.1432 0.0954 0.053 Uiso 0.75 1 calc PR E 2 H30K H 0.9808 0.1765 0.0579 0.053 Uiso 0.75 1 calc PR E 2 H30L H 1.0609 0.1385 0.0891 0.053 Uiso 0.75 1 calc PR E 2 C305 C 1.1183(9) 0.0718(6) 0.0191(4) 0.079(4) Uani 0.75 1 d P E 2 H30M H 1.1391 0.0336 0.0015 0.095 Uiso 0.75 1 calc PR E 2 H30N H 1.1792 0.0745 0.0349 0.095 Uiso 0.75 1 calc PR E 2 H30O H 1.0991 0.1127 0.0037 0.095 Uiso 0.75 1 calc PR E 2 O456 O 0.990(3) 0.5060(12) 0.4777(7) 0.086(10) Uiso 0.25 1 d PDU N -2 O308 O 0.815(3) 0.9108(18) 0.3148(11) 0.087(10) Uiso 0.25 1 d PU F 2 C309 C 0.8790(10) 0.9592(6) 0.2483(4) 0.074(4) Uiso 1 1 d . . . C310 C 0.681(2) 0.9723(15) 0.2313(10) 0.010(6) Uiso 0.25 1 d PU F 3 C311 C 0.666(3) 0.9654(17) 0.2685(11) 0.025(7) Uiso 0.25 1 d PU F 2 C312 C 0.6710(16) 0.9686(10) 0.2487(7) 0.032(5) Uiso 0.50 1 d PU F 1 C313 C 1.2663(7) 0.4937(5) -0.0800(3) 0.058(3) Uani 0.50 1 d P H 1 H31D H 1.2770 0.4930 -0.1085 0.070 Uiso 0.50 1 calc PR H 1 H31E H 1.2367 0.5393 -0.0713 0.070 Uiso 0.50 1 calc PR H 1 H31F H 1.2156 0.4653 -0.0720 0.070 Uiso 0.50 1 calc PR H 1 C314 C 1.3770(10) 0.4642(6) -0.0147(3) 0.076(4) Uani 0.50 1 d P H 1 H31G H 1.4454 0.4477 -0.0023 0.091 Uiso 0.50 1 calc PR H 1 H31H H 1.3256 0.4361 -0.0071 0.091 Uiso 0.50 1 calc PR H 1 H31I H 1.3469 0.5100 -0.0064 0.091 Uiso 0.50 1 calc PR H 1 C315 C 1.1893(10) 0.8627(6) 0.2567(3) 0.079(4) Uiso 1 1 d . . . H31J H 1.2165 0.9039 0.2563 0.118 Uiso 1 1 calc R . . H31K H 1.1549 0.8586 0.2323 0.118 Uiso 1 1 calc R . . H31L H 1.2496 0.8247 0.2596 0.118 Uiso 1 1 calc R . . O316 O 1.1059(14) 0.1398(9) 0.3922(5) 0.216(7) Uiso 1 1 d U O . C317 C 1.1262(11) 0.1063(7) 0.4245(4) 0.091(4) Uiso 1 1 d U . . C318 C 1.087(3) 0.1131(19) 0.4632(10) 0.050(8) Uiso 0.33 1 d PU O 2 C74A C 0.695(3) 0.7525(15) 0.3390(8) 0.100(11) Uiso 0.50 1 d PD K 2 H74D H 0.6709 0.7973 0.3499 0.150 Uiso 0.50 1 calc PR K 2 H74E H 0.6323 0.7371 0.3299 0.150 Uiso 0.50 1 calc PR K 2 H74F H 0.7475 0.7535 0.3172 0.150 Uiso 0.50 1 calc PR K 2 C75A C 0.8313(14) 0.7404(9) 0.3836(6) 0.043(5) Uiso 0.50 1 d PD K 2 H75D H 0.7941 0.7851 0.3919 0.065 Uiso 0.50 1 calc PR K 2 H75E H 0.8817 0.7436 0.3613 0.065 Uiso 0.50 1 calc PR K 2 H75F H 0.8716 0.7176 0.4051 0.065 Uiso 0.50 1 calc PR K 2 C77A C 0.526(2) 0.6984(17) 0.1536(10) 0.039(7) Uiso 0.33 1 d PDU L 1 H77D H 0.5599 0.6719 0.1311 0.047 Uiso 0.33 1 calc PR L 1 H77E H 0.4793 0.7393 0.1448 0.047 Uiso 0.33 1 calc PR L 1 H77F H 0.4834 0.6728 0.1698 0.047 Uiso 0.33 1 calc PR L 1 C78A C 0.680(3) 0.7574(19) 0.1519(11) 0.025(7) Uiso 0.33 1 d PDU L 1 H78D H 0.7155 0.7305 0.1297 0.031 Uiso 0.33 1 calc PR L 1 H78E H 0.7350 0.7712 0.1670 0.031 Uiso 0.33 1 calc PR L 1 H78F H 0.6307 0.7969 0.1423 0.031 Uiso 0.33 1 calc PR L 1 C79A C 0.558(3) 0.7568(15) 0.2123(8) 0.039(7) Uiso 0.33 1 d PDU L 1 H79D H 0.5174 0.7298 0.2283 0.047 Uiso 0.33 1 calc PR L 1 H79E H 0.5088 0.7963 0.2029 0.047 Uiso 0.33 1 calc PR L 1 H79F H 0.6122 0.7706 0.2280 0.047 Uiso 0.33 1 calc PR L 1 C77B C 0.553(2) 0.6962(14) 0.1413(7) 0.026(6) Uiso 0.33 1 d PDU L 2 H77G H 0.6064 0.6780 0.1204 0.031 Uiso 0.33 1 calc PR L 2 H77H H 0.5040 0.7359 0.1319 0.031 Uiso 0.33 1 calc PR L 2 H77I H 0.5117 0.6628 0.1497 0.031 Uiso 0.33 1 calc PR L 2 C78B C 0.673(3) 0.7706(14) 0.1622(10) 0.035(7) Uiso 0.33 1 d PDU L 2 H78G H 0.7327 0.7510 0.1439 0.042 Uiso 0.33 1 calc PR L 2 H78H H 0.7006 0.7911 0.1838 0.042 Uiso 0.33 1 calc PR L 2 H78I H 0.6210 0.8044 0.1487 0.042 Uiso 0.33 1 calc PR L 2 C79B C 0.5214(19) 0.7426(15) 0.2063(7) 0.035(6) Uiso 0.33 1 d PDU L 2 H79G H 0.4875 0.7061 0.2154 0.041 Uiso 0.33 1 calc PR L 2 H79H H 0.4681 0.7763 0.1934 0.041 Uiso 0.33 1 calc PR L 2 H79I H 0.5475 0.7627 0.2286 0.041 Uiso 0.33 1 calc PR L 2 C404 C 0.9940(7) 0.1389(5) 0.0760(3) 0.044(3) Uani 0.25 1 d P E 1 H40D H 0.9212 0.1651 0.0824 0.053 Uiso 0.25 1 calc PR E 1 H40E H 1.0475 0.1662 0.0795 0.053 Uiso 0.25 1 calc PR E 1 H40F H 1.0084 0.0999 0.0931 0.053 Uiso 0.25 1 calc PR E 1 C405 C 1.1183(9) 0.0718(6) 0.0191(4) 0.079(4) Uani 0.25 1 d P E 1 H40G H 1.1309 0.0549 -0.0076 0.095 Uiso 0.25 1 calc PR E 1 H40H H 1.1296 0.0344 0.0374 0.095 Uiso 0.25 1 calc PR E 1 H40I H 1.1690 0.1006 0.0238 0.095 Uiso 0.25 1 calc PR E 1 C403 C 0.9246(10) 0.7380(5) 0.2123(3) 0.069(3) Uani 0.25 1 d P D 2 H40J H 0.8950 0.7848 0.2062 0.083 Uiso 0.25 1 calc PR D 2 H40K H 0.8757 0.7105 0.2037 0.083 Uiso 0.25 1 calc PR D 2 H40L H 0.9958 0.7239 0.1987 0.083 Uiso 0.25 1 calc PR D 2 C402 C 0.9914(8) 0.6415(4) 0.2626(3) 0.042(2) Uani 0.25 1 d P D 2 H40M H 1.0053 0.6254 0.2891 0.051 Uiso 0.25 1 calc PR D 2 H40N H 1.0592 0.6323 0.2465 0.051 Uiso 0.25 1 calc PR D 2 H40O H 0.9391 0.6188 0.2516 0.051 Uiso 0.25 1 calc PR D 2 C291 C 1.4610(9) 0.4298(6) 0.3187(5) 0.117(7) Uani 0.25 1 d P A 2 H29A H 1.4142 0.4710 0.3100 0.141 Uiso 0.25 1 calc PR A 2 H29B H 1.4975 0.4047 0.2960 0.141 Uiso 0.25 1 calc PR A 2 H29C H 1.5153 0.4405 0.3354 0.141 Uiso 0.25 1 calc PR A 2 C290 C 1.4988(9) 0.3138(6) 0.3545(4) 0.092(5) Uani 0.25 1 d P A 2 H29D H 1.4840 0.2757 0.3696 0.110 Uiso 0.25 1 calc PR A 2 H29E H 1.5491 0.3346 0.3681 0.110 Uiso 0.25 1 calc PR A 2 H29F H 1.5311 0.2988 0.3288 0.110 Uiso 0.25 1 calc PR A 2 C413 C 1.2663(7) 0.4937(5) -0.0800(3) 0.058(3) Uani 0.50 1 d P H 2 H41A H 1.2424 0.5236 -0.1017 0.070 Uiso 0.50 1 calc PR H 2 H41B H 1.2029 0.4860 -0.0644 0.070 Uiso 0.50 1 calc PR H 2 H41C H 1.3080 0.4512 -0.0903 0.070 Uiso 0.50 1 calc PR H 2 C414 C 1.3770(10) 0.4642(6) -0.0147(3) 0.076(4) Uani 0.50 1 d P H 2 H41D H 1.4226 0.4784 0.0042 0.091 Uiso 0.50 1 calc PR H 2 H41E H 1.4158 0.4227 -0.0270 0.091 Uiso 0.50 1 calc PR H 2 H41F H 1.3098 0.4570 -0.0014 0.091 Uiso 0.50 1 calc PR H 2 C131 C 0.8811(15) -0.0872(8) 0.4088(5) 0.166(7) Uiso 1 1 d DU G . H13A H 0.9603 -0.1007 0.4077 0.199 Uiso 1 1 calc R . . H13B H 0.8550 -0.0902 0.3827 0.199 Uiso 1 1 calc R . . H13C H 0.8499 -0.1166 0.4266 0.199 Uiso 1 1 calc R . . C132 C 0.7274(15) -0.0172(11) 0.4203(7) 0.207(9) Uiso 1 1 d DU G . H13D H 0.6840 0.0261 0.4286 0.248 Uiso 1 1 calc R . . H13E H 0.7082 -0.0520 0.4373 0.248 Uiso 1 1 calc R . . H13F H 0.7129 -0.0258 0.3934 0.248 Uiso 1 1 calc R . . C130 C 0.950(2) -0.0324(15) 0.4485(8) 0.114(9) Uiso 0.50 1 d PDU G 2 H13G H 0.9536 0.0072 0.4635 0.137 Uiso 0.50 1 calc PR G 2 H13H H 1.0158 -0.0448 0.4315 0.137 Uiso 0.50 1 calc PR G 2 H13I H 0.9444 -0.0692 0.4664 0.137 Uiso 0.50 1 calc PR G 2 C129 C 0.823(2) 0.0126(14) 0.4633(6) 0.100(8) Uiso 0.50 1 d PDU G 1 H12M H 0.8030 0.0611 0.4613 0.120 Uiso 0.50 1 calc PR G 1 H12N H 0.8875 0.0001 0.4786 0.120 Uiso 0.50 1 calc PR G 1 H12O H 0.7632 -0.0043 0.4762 0.120 Uiso 0.50 1 calc PR G 1 O455 O 1.002(4) 0.4262(11) 0.5349(7) 0.129(10) Uiso 0.25 1 d PDU P -2 N453 N 1.0017(11) 0.4658(6) 0.5062(4) 0.039(4) Uiso 0.50 1 d PDU . -2 C319 C 1.139(2) 0.0757(15) 0.4636(8) 0.042(7) Uiso 0.33 1 d PU O 1 C320 C 1.119(3) 0.1335(17) 0.4669(10) 0.052(8) Uiso 0.33 1 d PU O 3 O312 O 0.776(2) 0.8885(12) 0.2952(7) 0.137(7) Uiso 0.50 1 d PU F 1 O458 O 0.913(2) 0.4506(17) 0.5228(10) 0.113(10) Uiso 0.25 1 d PDU Q -2 O457 O 1.1061(18) 0.4536(14) 0.5082(10) 0.114(10) Uiso 0.25 1 d PDU R -2 C507 C 0.280(2) 0.4540(14) 0.4237(7) 0.099(8) Uiso 0.50 1 d PDU C 2 H50D H 0.2809 0.4840 0.4015 0.118 Uiso 0.50 1 calc PR C 2 H50E H 0.2059 0.4608 0.4356 0.118 Uiso 0.50 1 calc PR C 2 H50F H 0.3027 0.4078 0.4149 0.118 Uiso 0.50 1 calc PR C 2 C503 C 0.371(2) 0.4998(9) 0.4665(8) 0.100(8) Uiso 0.50 1 d PDU B 1 H50G H 0.4289 0.5015 0.4840 0.120 Uiso 0.50 1 calc PR B 1 H50H H 0.3006 0.5158 0.4802 0.120 Uiso 0.50 1 calc PR B 1 H50I H 0.3784 0.5280 0.4437 0.120 Uiso 0.50 1 calc PR B 1 C506 C 0.368(2) 0.4154(12) 0.4990(7) 0.105(9) Uiso 0.50 1 d PDU C 2 H50J H 0.4158 0.4240 0.5189 0.126 Uiso 0.50 1 calc PR C 2 H50K H 0.3923 0.3697 0.4896 0.126 Uiso 0.50 1 calc PR C 2 H50L H 0.2938 0.4215 0.5103 0.126 Uiso 0.50 1 calc PR C 2 C35A C 0.6903(18) -0.0514(11) 0.1334(7) 0.076(8) Uani 0.50 1 d P J 1 H35D H 0.6367 -0.0132 0.1438 0.091 Uiso 0.50 1 calc PR J 1 H35E H 0.7204 -0.0797 0.1550 0.091 Uiso 0.50 1 calc PR J 1 H35F H 0.6555 -0.0771 0.1162 0.091 Uiso 0.50 1 calc PR J 1 O459 O 0.998(2) 0.4792(14) 0.4682(6) 0.050(6) Uiso 0.25 1 d PDU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0177(5) 0.0169(5) 0.0291(6) -0.0078(5) 0.0028(4) -0.0013(4) S1 0.0262(13) 0.0444(15) 0.0517(17) -0.0140(13) -0.0073(11) 0.0118(11) O1 0.018(3) 0.017(3) 0.020(3) -0.008(2) 0.002(2) 0.001(2) C1 0.016(4) 0.018(5) 0.031(6) -0.011(4) 0.002(4) 0.001(3) Cu2 0.0169(5) 0.0139(5) 0.0205(6) -0.0017(4) 0.0004(4) -0.0008(4) S2 0.0268(13) 0.0500(16) 0.0599(18) 0.0229(14) 0.0089(12) -0.0022(11) O2 0.024(3) 0.020(3) 0.030(3) -0.009(3) 0.005(3) -0.006(2) C2 0.029(5) 0.020(5) 0.028(5) -0.004(4) 0.010(4) 0.006(4) Cu3 0.0210(5) 0.0183(6) 0.0302(6) 0.0001(5) 0.0026(4) 0.0004(4) S3 0.0328(13) 0.0404(15) 0.0427(15) -0.0232(12) 0.0205(11) -0.0194(11) O3 0.022(3) 0.019(3) 0.029(3) -0.008(3) -0.001(3) 0.003(2) C3 0.018(4) 0.029(5) 0.028(5) -0.009(4) -0.003(4) -0.003(4) Cu4 0.0183(5) 0.0200(6) 0.0308(6) -0.0061(5) 0.0012(4) 0.0010(4) S4 0.0266(12) 0.0297(13) 0.0349(14) -0.0004(11) 0.0024(10) 0.0010(10) O4 0.019(3) 0.015(3) 0.028(4) -0.009(3) 0.004(2) -0.003(2) C4 0.017(4) 0.022(5) 0.043(6) -0.011(4) 0.003(4) -0.005(4) Cu5 0.0193(5) 0.0185(6) 0.0332(6) -0.0017(5) 0.0032(5) -0.0034(4) S5 0.0292(19) 0.049(2) 0.066(3) -0.0062(19) -0.0023(17) -0.0075(16) O5 0.019(3) 0.012(3) 0.023(3) -0.005(2) 0.003(2) 0.004(2) C5 0.018(4) 0.019(5) 0.025(5) -0.013(4) 0.000(4) 0.000(4) Cu6 0.0164(5) 0.0178(5) 0.0250(6) -0.0080(5) 0.0026(4) -0.0018(4) S6 0.005(4) 0.026(5) 0.005(4) 0.003(4) 0.002(3) -0.003(3) O6 0.011(3) 0.017(3) 0.027(3) -0.001(2) 0.001(2) 0.005(2) C6 0.020(4) 0.015(4) 0.022(5) -0.009(4) 0.002(4) 0.005(4) Cu7 0.0167(5) 0.0160(5) 0.0247(6) -0.0068(4) -0.0018(4) 0.0010(4) S7 0.0293(13) 0.0432(15) 0.0341(14) 0.0015(12) 0.0074(11) -0.0027(11) O7 0.016(3) 0.016(3) 0.022(3) -0.005(2) 0.002(2) -0.002(2) C7 0.020(4) 0.021(5) 0.033(5) -0.012(4) -0.001(4) -0.007(4) Cu8 0.0198(5) 0.0221(6) 0.0319(6) 0.0065(5) -0.0053(5) -0.0048(4) O8 0.023(3) 0.016(3) 0.024(3) 0.000(2) -0.004(2) -0.002(2) C8 0.028(5) 0.025(5) 0.037(6) -0.010(4) 0.006(4) -0.007(4) Cu9 0.0200(5) 0.0164(5) 0.0227(6) -0.0006(4) 0.0026(4) -0.0003(4) O9 0.025(3) 0.022(3) 0.020(3) 0.002(2) -0.003(2) -0.002(2) C9 0.034(5) 0.029(5) 0.036(6) -0.010(4) 0.002(4) -0.017(4) S10 0.084(9) 0.026(6) 0.070(9) -0.017(6) 0.012(7) -0.009(6) O10 0.022(3) 0.019(3) 0.029(3) 0.002(3) 0.000(2) 0.002(2) C10 0.034(5) 0.029(5) 0.033(6) -0.008(4) 0.009(4) -0.013(4) S11 0.036(2) 0.043(2) 0.043(2) 0.0033(17) -0.0023(17) -0.0142(16) O11 0.023(3) 0.018(3) 0.027(3) 0.006(3) 0.004(2) 0.000(2) C11 0.025(5) 0.017(5) 0.052(6) -0.007(4) 0.008(4) -0.002(4) S12 0.0320(17) 0.0218(17) 0.048(2) -0.0036(16) -0.0040(15) -0.0068(13) O12 0.030(3) 0.022(3) 0.027(3) 0.009(3) 0.006(3) 0.002(3) C12 0.035(5) 0.013(5) 0.038(6) 0.001(4) 0.013(4) -0.004(4) S13 0.048(7) 0.054(7) 0.051(7) -0.007(6) 0.004(5) -0.002(5) O13 0.018(3) 0.016(3) 0.031(3) -0.004(3) 0.005(2) 0.000(2) C13 0.027(5) 0.022(5) 0.032(5) -0.002(4) 0.004(4) -0.012(4) O14 0.015(3) 0.023(3) 0.020(3) -0.006(2) 0.002(2) -0.001(2) C14 0.027(5) 0.019(5) 0.048(6) -0.005(4) 0.007(4) -0.003(4) O15 0.015(3) 0.016(3) 0.030(3) -0.008(2) 0.005(2) 0.002(2) C15 0.023(5) 0.023(5) 0.033(5) -0.009(4) -0.003(4) -0.003(4) O16 0.034(6) 0.030(6) 0.056(6) 0.008(5) -0.002(5) -0.008(5) N2 0.034(5) 0.031(5) 0.035(5) 0.006(4) -0.005(4) -0.007(4) C16 0.025(5) 0.022(5) 0.039(6) -0.007(4) -0.009(4) -0.002(4) O17 0.027(6) 0.010(6) 0.033(7) 0.003(5) 0.008(5) 0.000(5) N1 0.023(4) 0.029(4) 0.040(4) -0.001(3) -0.002(3) -0.003(3) C17 0.027(5) 0.019(5) 0.031(5) -0.005(4) -0.007(4) -0.002(4) S18 0.063(4) 0.076(4) 0.092(5) 0.000(4) -0.005(3) -0.017(3) O18 0.043(7) 0.042(8) 0.062(8) -0.011(7) 0.003(7) 0.008(7) C18 0.017(4) 0.024(5) 0.025(5) -0.007(4) 0.000(4) 0.004(4) S19 0.0113(18) 0.0040(19) 0.032(2) -0.0041(17) -0.0019(17) -0.0043(15) O19 0.010(4) 0.009(5) 0.021(5) 0.001(4) 0.003(4) -0.003(4) C19 0.017(4) 0.016(5) 0.030(5) -0.008(4) -0.005(4) 0.007(3) O20 0.041(7) 0.048(8) 0.052(8) -0.001(7) 0.012(6) -0.017(7) C20 0.018(4) 0.016(5) 0.033(5) -0.005(4) -0.005(4) 0.000(4) O21 0.021(6) 0.021(6) 0.044(7) 0.014(6) -0.002(5) 0.014(6) C21 0.012(4) 0.023(5) 0.031(5) -0.014(4) 0.010(4) -0.002(3) O22 0.026(3) 0.029(3) 0.040(4) -0.006(3) 0.005(3) -0.006(3) C22 0.027(5) 0.014(4) 0.024(5) -0.006(4) 0.001(4) -0.008(4) O23 0.020(3) 0.028(3) 0.046(4) -0.004(3) 0.006(3) -0.001(3) C23 0.016(4) 0.016(5) 0.037(6) -0.005(4) 0.005(4) 0.001(3) O24 0.025(4) 0.109(6) 0.057(5) -0.013(4) -0.009(3) -0.022(4) C24 0.022(4) 0.015(4) 0.028(5) -0.007(4) 0.005(4) -0.008(4) O25 0.033(4) 0.055(4) 0.057(5) -0.033(4) -0.017(3) 0.021(3) C25 0.017(4) 0.014(4) 0.034(6) -0.009(4) 0.000(4) 0.001(3) O26 0.028(3) 0.041(4) 0.052(4) -0.003(3) 0.008(3) -0.010(3) C26 0.018(4) 0.019(5) 0.025(5) -0.011(4) 0.013(4) -0.006(3) O27 0.033(3) 0.050(4) 0.036(4) -0.021(3) 0.020(3) -0.023(3) C27 0.018(4) 0.021(5) 0.025(5) -0.009(4) 0.007(4) 0.000(4) O28 0.023(3) 0.024(3) 0.040(4) -0.008(3) -0.006(3) 0.006(2) C28 0.023(4) 0.026(5) 0.021(5) -0.013(4) 0.006(4) -0.004(4) O29 0.042(5) 0.079(6) 0.146(8) 0.071(5) -0.056(5) -0.041(4) C29 0.027(5) 0.039(6) 0.031(5) -0.016(4) -0.006(4) -0.004(4) O30 0.025(3) 0.026(3) 0.027(3) -0.001(3) 0.005(3) 0.001(2) C30 0.033(5) 0.063(7) 0.031(6) -0.007(5) -0.008(4) 0.011(5) C31 0.035(6) 0.073(7) 0.036(6) -0.016(5) -0.009(5) -0.019(5) C32 0.025(5) 0.042(6) 0.033(6) -0.012(5) -0.001(4) -0.005(4) O33 0.081(6) 0.033(4) 0.125(7) -0.013(5) -0.045(5) -0.011(4) C33 0.050(6) 0.027(6) 0.068(8) -0.027(5) 0.000(6) -0.010(5) C34 0.043(7) 0.071(8) 0.125(11) -0.064(8) -0.028(7) 0.003(6) O35 0.049(4) 0.043(4) 0.115(7) -0.022(4) -0.035(4) -0.005(3) C35 0.080(17) 0.033(13) 0.11(2) -0.021(13) -0.031(15) -0.031(12) C36 0.060(7) 0.047(7) 0.100(10) -0.050(7) -0.024(7) 0.002(6) C37 0.034(5) 0.030(5) 0.036(6) -0.013(5) 0.004(4) 0.000(4) C38 0.067(8) 0.070(8) 0.075(8) -0.052(7) 0.031(6) -0.036(6) C39 0.095(10) 0.061(8) 0.058(8) -0.006(6) 0.013(7) 0.057(7) C40 0.044(6) 0.041(6) 0.039(6) -0.021(5) 0.005(5) -0.001(5) C41 0.024(5) 0.030(5) 0.032(6) -0.004(4) 0.005(4) -0.006(4) C42 0.054(6) 0.052(7) 0.039(6) -0.007(5) 0.020(5) -0.022(5) C43 0.037(5) 0.035(5) 0.027(5) -0.009(4) 0.001(4) 0.002(4) C44 0.034(5) 0.041(6) 0.024(5) -0.011(4) 0.003(4) -0.003(4) C45 0.030(5) 0.022(5) 0.026(5) -0.004(4) 0.011(4) -0.006(4) C46 0.033(5) 0.043(6) 0.042(6) -0.018(5) 0.014(5) -0.023(5) C47 0.030(5) 0.028(5) 0.063(7) -0.022(5) 0.018(5) -0.009(4) C48 0.016(5) 0.028(5) 0.058(7) -0.010(5) 0.005(4) 0.004(4) C49 0.019(4) 0.024(5) 0.030(5) -0.004(4) 0.007(4) -0.004(4) C50 0.025(5) 0.021(5) 0.017(5) 0.004(4) 0.009(4) -0.008(4) C51 0.017(4) 0.012(4) 0.041(6) -0.004(4) 0.010(4) 0.004(3) C52 0.012(4) 0.020(5) 0.029(5) -0.002(4) 0.003(4) -0.003(3) C53 0.023(5) 0.017(5) 0.039(6) -0.001(4) 0.009(4) 0.004(4) C54 0.030(5) 0.017(5) 0.044(6) 0.012(5) 0.001(4) 0.002(4) C55 0.027(5) 0.020(5) 0.031(5) 0.015(4) -0.002(4) -0.006(4) C56 0.019(4) 0.023(5) 0.023(5) -0.005(4) 0.001(4) -0.009(4) C57 0.015(4) 0.020(5) 0.027(5) -0.001(4) 0.002(4) -0.008(3) C58 0.030(5) 0.018(4) 0.015(5) 0.004(4) -0.001(4) -0.006(4) C59 0.013(4) 0.024(5) 0.018(5) -0.009(4) 0.008(3) -0.006(3) C60 0.020(4) 0.022(5) 0.026(5) 0.002(4) -0.001(4) 0.000(4) C61 0.023(5) 0.019(5) 0.023(5) -0.002(4) 0.000(4) -0.003(4) C62 0.021(4) 0.030(5) 0.019(5) -0.005(4) 0.002(4) -0.004(4) C63 0.020(4) 0.020(5) 0.017(5) -0.003(4) 0.006(4) -0.006(4) C64 0.016(4) 0.017(4) 0.016(5) -0.007(4) 0.007(3) 0.002(3) C65 0.011(4) 0.010(4) 0.032(5) 0.002(4) 0.003(3) -0.003(3) C66 0.016(4) 0.015(4) 0.023(5) 0.000(4) 0.004(4) 0.003(3) C67 0.019(4) 0.013(4) 0.036(6) 0.001(4) -0.002(4) -0.001(3) C68 0.026(5) 0.014(4) 0.032(6) -0.001(4) -0.004(4) -0.003(4) C69 0.026(5) 0.022(5) 0.026(5) -0.006(4) -0.008(4) -0.002(4) C70 0.023(5) 0.029(5) 0.017(5) 0.002(4) -0.014(4) -0.004(4) C71 0.014(4) 0.012(4) 0.030(5) -0.001(4) -0.010(4) -0.001(3) C72 0.035(5) 0.026(5) 0.019(5) -0.008(4) 0.007(4) -0.014(4) C73 0.043(6) 0.051(7) 0.099(10) -0.052(7) 0.033(6) -0.015(5) C80 0.031(4) 0.033(4) 0.052(5) 0.017(4) 0.010(4) 0.006(4) C81 0.031(5) 0.032(5) 0.042(6) 0.017(5) -0.011(4) -0.008(4) C82 0.043(6) 0.042(6) 0.062(7) 0.022(5) -0.012(5) -0.019(5) C83 0.041(6) 0.062(7) 0.036(6) 0.017(5) -0.003(5) -0.022(5) C84 0.056(7) 0.035(6) 0.059(7) 0.006(5) -0.006(5) -0.020(5) C85 0.024(5) 0.025(5) 0.039(6) -0.009(4) 0.006(4) -0.009(4) C86 0.078(8) 0.038(6) 0.066(8) -0.025(6) 0.034(6) -0.042(6) C87 0.044(6) 0.053(7) 0.056(7) -0.017(6) -0.011(5) -0.015(5) C88 0.038(6) 0.029(5) 0.059(7) -0.016(5) 0.002(5) -0.007(4) C89 0.023(5) 0.026(5) 0.027(5) 0.000(4) 0.004(4) -0.002(4) C90 0.036(5) 0.039(6) 0.029(6) 0.001(5) -0.003(4) -0.004(4) C91 0.030(5) 0.029(5) 0.033(6) 0.012(4) -0.006(4) 0.002(4) C92 0.021(5) 0.029(5) 0.029(6) 0.003(4) 0.001(4) -0.006(4) C93 0.022(5) 0.030(5) 0.025(5) 0.007(4) 0.005(4) -0.006(4) C94 0.019(4) 0.020(5) 0.033(5) 0.007(4) -0.001(4) -0.006(4) C95 0.021(4) 0.025(5) 0.029(5) 0.005(4) 0.005(4) 0.001(4) C96 0.021(5) 0.018(5) 0.035(5) 0.000(4) 0.001(4) 0.006(4) C97 0.025(5) 0.029(5) 0.044(6) 0.004(5) -0.006(4) -0.002(4) C98 0.036(6) 0.030(6) 0.066(7) 0.016(5) 0.000(5) -0.004(4) C99 0.027(5) 0.030(6) 0.083(8) 0.007(5) -0.004(5) -0.007(4) C100 0.021(5) 0.019(5) 0.050(6) 0.001(4) 0.004(4) 0.003(4) C101 0.024(5) 0.018(5) 0.035(6) 0.003(4) 0.000(4) 0.004(4) C102 0.034(5) 0.020(5) 0.051(6) 0.004(4) -0.015(5) -0.008(4) C103 0.024(5) 0.029(5) 0.050(6) 0.014(5) -0.009(4) -0.003(4) C104 0.030(6) 0.030(6) 0.090(9) 0.024(6) 0.007(6) -0.005(4) C105 0.028(6) 0.055(7) 0.104(10) 0.051(7) 0.010(6) -0.009(5) C106 0.045(6) 0.039(6) 0.068(8) 0.035(6) 0.019(5) 0.007(5) C107 0.021(5) 0.033(6) 0.053(7) 0.021(5) 0.005(5) 0.003(4) C108 0.019(5) 0.027(5) 0.044(6) 0.001(4) -0.003(4) 0.001(4) C109 0.022(5) 0.047(6) 0.040(6) 0.016(5) 0.014(4) 0.006(4) C110 0.032(5) 0.041(6) 0.032(6) 0.018(5) 0.002(4) 0.005(4) C111 0.020(5) 0.070(7) 0.040(7) 0.032(6) 0.004(5) 0.006(5) C112 0.030(6) 0.086(8) 0.032(6) 0.029(6) 0.015(5) 0.010(5) C113 0.041(6) 0.061(7) 0.033(6) 0.010(5) 0.010(5) 0.015(5) C114 0.025(5) 0.037(6) 0.022(5) 0.003(4) 0.009(4) 0.012(4) C115 0.027(5) 0.028(5) 0.033(6) 0.016(4) 0.005(4) 0.008(4) C116 0.033(5) 0.034(5) 0.018(5) -0.006(4) 0.000(4) 0.001(4) C117 0.057(6) 0.054(6) 0.033(5) 0.011(5) -0.016(5) 0.003(5) C118 0.061(11) 0.066(12) 0.047(11) 0.001(10) -0.032(10) 0.007(10) C119 0.057(8) 0.073(9) 0.056(8) -0.003(8) -0.037(7) 0.007(8) C120 0.057(11) 0.061(11) 0.033(10) 0.009(11) -0.025(10) 0.002(11) C121 0.067(9) 0.068(9) 0.041(8) 0.009(7) -0.013(7) 0.014(8) C122 0.067(11) 0.062(12) 0.037(11) 0.012(11) -0.017(10) 0.004(11) C123 0.080(9) 0.075(10) 0.044(8) 0.013(8) -0.022(8) 0.025(9) C124 0.057(7) 0.032(6) 0.173(11) 0.048(7) -0.052(7) -0.012(5) C125 0.075(8) 0.029(6) 0.114(10) 0.017(6) -0.049(7) 0.000(5) O126 0.074(5) 0.122(7) 0.068(6) -0.027(5) 0.013(4) -0.072(5) C126 0.145(12) 0.034(7) 0.242(15) 0.005(9) -0.141(11) 0.013(8) C127 0.078(10) 0.131(12) 0.244(16) 0.135(11) -0.020(11) -0.008(9) C180 0.034(6) 0.036(7) 0.154(13) -0.009(7) -0.003(7) 0.004(5) C181 0.037(6) 0.085(9) 0.044(7) -0.016(6) -0.006(5) 0.010(6) C182 0.030(6) 0.067(8) 0.136(12) 0.069(8) -0.006(7) -0.002(5) C183 0.036(6) 0.077(8) 0.077(8) 0.034(7) -0.008(6) -0.013(6) C184 0.049(6) 0.054(7) 0.058(7) -0.036(6) 0.024(5) -0.021(5) C185 0.051(6) 0.050(7) 0.048(7) -0.006(5) 0.027(5) -0.017(5) C186 0.048(6) 0.023(5) 0.053(7) -0.005(5) 0.014(5) 0.001(4) C187 0.027(5) 0.043(6) 0.053(7) 0.014(5) 0.006(5) 0.001(4) C188 0.043(6) 0.095(9) 0.032(6) 0.009(6) 0.005(5) 0.016(6) C189 0.031(6) 0.060(7) 0.059(7) 0.022(6) 0.010(5) 0.017(5) C190 0.042(7) 0.083(9) 0.155(13) 0.082(9) -0.034(8) -0.021(6) C191 0.058(8) 0.058(8) 0.256(19) 0.099(10) -0.086(10) -0.041(6) C302 0.050(6) 0.022(5) 0.053(7) 0.002(5) 0.005(5) -0.005(4) C303 0.091(9) 0.050(7) 0.065(8) -0.003(6) -0.018(7) -0.009(6) C304 0.036(6) 0.048(6) 0.045(6) -0.020(5) 0.004(5) 0.000(5) C305 0.075(8) 0.085(9) 0.080(9) -0.056(8) 0.015(7) -0.024(7) C313 0.031(6) 0.076(8) 0.069(8) 0.020(6) -0.009(5) -0.013(5) C314 0.102(10) 0.076(9) 0.063(8) 0.037(7) -0.038(7) -0.041(7) C404 0.036(6) 0.048(6) 0.045(6) -0.020(5) 0.004(5) 0.000(5) C405 0.075(8) 0.085(9) 0.080(9) -0.056(8) 0.015(7) -0.024(7) C403 0.091(9) 0.050(7) 0.065(8) -0.003(6) -0.018(7) -0.009(6) C402 0.050(6) 0.022(5) 0.053(7) 0.002(5) 0.005(5) -0.005(4) C291 0.058(8) 0.058(8) 0.256(19) 0.099(10) -0.086(10) -0.041(6) C290 0.042(7) 0.083(9) 0.155(13) 0.082(9) -0.034(8) -0.021(6) C413 0.031(6) 0.076(8) 0.069(8) 0.020(6) -0.009(5) -0.013(5) C414 0.102(10) 0.076(9) 0.063(8) 0.037(7) -0.038(7) -0.041(7) C35A 0.088(17) 0.078(17) 0.080(17) -0.059(14) 0.057(14) -0.073(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O3 1.958(5) . ? Cu1 O4 1.967(5) . ? Cu1 O2 1.969(5) . ? Cu1 O1 1.972(5) . ? S1 O25 1.533(6) . ? S1 C181 1.759(10) . ? S1 C180 1.772(10) . ? O1 C6 1.391(9) . ? O1 Cu7 1.969(5) . ? C1 C6 1.411(11) . ? C1 C2 1.412(11) . ? C1 C28 1.521(11) . ? Cu2 O7 1.950(5) . ? Cu2 O5 1.958(5) . ? Cu2 O6 1.983(5) . ? Cu2 O8 1.990(5) . ? S2 O26 1.536(6) . ? S2 C183 1.799(10) . ? S2 C182 1.809(10) . ? O2 C13 1.382(9) . ? O2 Cu5 1.957(6) . ? C2 C3 1.416(11) . ? Cu3 O12 1.946(5) . ? Cu3 O9 1.966(5) . ? Cu3 O10 1.975(5) . ? Cu3 O11 1.996(5) . ? S3 O27 1.544(6) . ? S3 C185 1.782(10) . ? S3 C184 1.800(9) . ? O3 C20 1.386(9) . ? O3 Cu4 1.971(6) . ? C3 C4 1.393(11) . ? C3 C29 1.558(11) . ? Cu4 O25 1.931(6) . ? Cu4 O13 1.939(5) . ? Cu4 O10 1.980(6) . ? Cu4 O16 2.330(12) . ? S4 O28 1.521(6) . ? S4 C186 1.764(9) . ? S4 C187 1.805(8) . ? O4 C27 1.376(9) . ? O4 Cu6 1.983(5) . ? C4 C5 1.406(11) . ? Cu5 O26 1.931(6) . ? Cu5 O13 1.950(5) . ? Cu5 O11 1.979(6) . ? S5 O29 1.414(8) . ? S5 C191 1.807(11) . ? S5 C190 1.815(11) . ? O5 C50 1.372(8) . ? O5 Cu9 1.983(5) . ? C5 C6 1.410(11) . ? C5 C7 1.515(11) . ? Cu6 O27 1.935(6) . ? Cu6 O14 1.949(5) . ? Cu6 O7 1.978(5) . ? Cu6 O19 2.351(9) . ? S6 O29 1.158(10) . ? O6 C57 1.379(8) . ? O6 Cu7 1.989(5) . ? Cu7 O28 1.937(5) . ? Cu7 O14 1.948(5) . ? S7 O30 1.535(6) . ? S7 C188 1.762(10) . ? S7 C189 1.778(9) . ? O7 C64 1.377(8) . ? C7 C8 1.531(11) . ? Cu8 O29 1.930(7) . ? Cu8 O15 1.940(5) . ? Cu8 O9 1.989(5) . ? Cu8 O8 2.005(5) . ? S500 O501 1.479(17) . ? S500 C502 1.812(17) . ? S500 C503 1.839(17) . ? O8 C71 1.385(7) . ? N3 O42 1.248(10) . ? N3 O38 1.272(10) . ? N3 O39 1.276(10) . ? O42 O42 1.29(4) 2_765 ? C8 C13 1.404(11) . ? C8 C9 1.418(11) . ? Cu9 O12 1.955(5) . ? Cu9 O30 1.958(5) . ? Cu9 O15 1.967(5) . ? Cu9 O22 2.377(6) . ? S504 O505 1.452(16) . ? S504 C506 1.765(17) . ? S504 C507 1.843(16) . ? O9 C94 1.390(8) . ? C9 C10 1.424(11) . ? S10 O33 1.309(13) . ? O10 C101 1.385(8) . ? C10 C11 1.391(11) . ? C10 C33 1.558(12) . ? S11 O33 1.468(8) . ? S11 C302 1.759(9) . ? S11 C303 1.804(11) . ? O11 C108 1.376(9) . ? C11 C12 1.403(11) . ? S12 O35 1.519(7) . ? S12 C305 1.749(12) . ? S12 C304 1.806(9) . ? O12 C115 1.369(9) . ? C12 C13 1.418(11) . ? C12 C14 1.521(11) . ? S13 O35 1.566(13) . ? C14 C15 1.520(11) . ? S15 C310 1.49(3) . ? S15 C309 1.707(12) . ? C15 C16 1.391(11) . ? C15 C20 1.409(11) . ? S16 C312 1.55(2) . ? S16 O312 1.58(2) . ? S16 C309 1.787(12) . ? O16 N1 1.384(13) . ? N2 O23 1.235(8) . ? N2 O24 1.253(9) . ? N2 O22 1.281(9) . ? C16 C17 1.414(11) . ? S17 C311 1.42(3) . ? S17 O308 1.77(4) . ? S17 C309 1.895(14) . ? O17 N1 1.217(13) . ? N1 O18 1.165(14) . ? N1 O20 1.174(14) . ? N1 O21 1.238(13) . ? N1 O19 1.363(12) . ? C17 C18 1.413(11) . ? C17 C37 1.536(11) . ? S18 C314 1.502(12) . ? S18 O126 1.691(8) . ? S18 C313 1.843(9) . ? C18 C19 1.384(10) . ? S19 O126 1.532(7) . ? C19 C20 1.402(11) . ? C19 C21 1.537(11) . ? C21 C22 1.527(11) . ? C22 C27 1.404(10) . ? C22 C23 1.405(11) . ? C23 C24 1.389(11) . ? C24 C25 1.416(10) . ? C24 C41 1.563(11) . ? C25 C26 1.387(11) . ? C26 C27 1.417(11) . ? C26 C28 1.534(10) . ? C29 C30 1.527(12) . ? C29 C32 1.532(11) . ? C29 C31 1.542(12) . ? C33 C34 1.508(15) . ? C33 C36 1.516(13) . ? C33 C35A 1.534(18) . ? C33 C35 1.55(2) . ? O454 N453 1.329(18) . ? O36 C315 1.423(12) . ? C37 C39 1.535(13) . ? C37 C40 1.548(12) . ? C37 C38 1.560(13) . ? C41 C42 1.527(12) . ? C41 C44 1.541(8) . ? C41 C43 1.550(11) . ? C45 C46 1.396(11) . ? C45 C50 1.418(11) . ? C45 C72 1.521(11) . ? C46 C47 1.411(12) . ? C47 C48 1.386(12) . ? C47 C73 1.549(12) . ? C48 C49 1.416(11) . ? C49 C50 1.404(11) . ? C49 C51 1.522(11) . ? C51 C52 1.513(11) . ? C52 C57 1.412(10) . ? C52 C53 1.420(10) . ? C53 C54 1.372(11) . ? C54 C55 1.396(11) . ? C54 C80 1.557(11) . ? C55 C56 1.401(10) . ? C56 C57 1.406(11) . ? C56 C58 1.533(10) . ? C58 C59 1.523(10) . ? C59 C64 1.399(10) . ? C59 C60 1.404(11) . ? C60 C61 1.415(11) . ? C61 C62 1.403(11) . ? C61 C81 1.543(11) . ? C62 C63 1.386(11) . ? C63 C64 1.405(10) . ? C63 C65 1.536(10) . ? C65 C66 1.526(10) . ? C66 C71 1.399(11) . ? C66 C67 1.419(10) . ? C67 C68 1.394(11) . ? C68 C69 1.402(11) . ? C68 C85 1.539(11) . ? C69 C70 1.386(11) . ? C70 C71 1.426(11) . ? C70 C72 1.544(11) . ? C73 C75A 1.482(15) . ? C73 C76 1.499(11) . ? C73 C74 1.525(17) . ? C73 C75 1.572(15) . ? C73 C74A 1.620(18) . ? C77 C80 1.496(17) . ? C78 C80 1.515(18) . ? C79 C80 1.625(17) . ? C80 C79B 1.513(17) . ? C80 C79A 1.520(17) . ? C80 C78B 1.529(18) . ? C80 C78A 1.539(18) . ? C80 C77A 1.546(18) . ? C80 C77B 1.622(17) . ? C81 C84 1.538(12) . ? C81 C82 1.539(11) . ? C81 C83 1.561(12) . ? C85 C86 1.518(12) . ? C85 C88 1.539(11) . ? C85 C87 1.560(12) . ? C89 C94 1.406(11) . ? C89 C90 1.406(11) . ? C89 C116 1.526(11) . ? C90 C91 1.425(11) . ? C91 C92 1.387(11) . ? C91 C117 1.548(12) . ? C92 C93 1.386(11) . ? C93 C94 1.422(11) . ? C93 C95 1.520(11) . ? C95 C96 1.535(11) . ? C96 C101 1.399(11) . ? C96 C97 1.409(11) . ? C97 C98 1.402(12) . ? C98 C99 1.414(12) . ? C98 C124 1.544(13) . ? C99 C100 1.399(12) . ? C100 C101 1.388(11) . ? C100 C102 1.537(11) . ? C102 C103 1.525(12) . ? C103 C104 1.384(12) . ? C103 C108 1.432(11) . ? C104 C105 1.409(14) . ? C105 C106 1.424(14) . ? C105 C128 1.576(17) . ? C106 C107 1.377(12) . ? C107 C108 1.407(12) . ? C107 C109 1.541(12) . ? C109 C110 1.526(13) . ? C110 C111 1.395(12) . ? C110 C115 1.411(12) . ? C111 C112 1.393(14) . ? C112 C113 1.414(14) . ? C112 C151 1.565(14) . ? C112 C152 1.584(15) . ? C113 C114 1.407(12) . ? C114 C115 1.419(12) . ? C114 C116 1.523(12) . ? C117 C123 1.489(14) . ? C117 C119 1.509(14) . ? C117 C122 1.522(18) . ? C117 C120 1.528(17) . ? C117 C121 1.584(14) . ? C117 C118 1.598(18) . ? C124 C126 1.511(19) . ? C124 C127 1.518(19) . ? C124 C125 1.519(14) . ? C128 C131 1.499(15) . ? C128 C129 1.513(17) . ? C128 C132 1.530(16) . ? C128 C130 1.581(17) . ? C150 C151 1.517(16) . ? C151 C160 1.552(16) . ? C151 C155 1.581(16) . ? C152 C158 1.514(17) . ? C152 C157 1.518(17) . ? C152 C156 1.571(17) . ? O456 N453 1.268(18) . ? O316 C317 1.308(19) . ? C317 C318 1.39(4) . ? C317 C319 1.48(3) . ? C317 C320 1.56(4) . ? O455 N453 1.273(19) . ? N453 O457 1.297(19) . ? N453 O458 1.324(19) . ? N453 O459 1.334(18) . ? N453 O459 1.45(3) 2_766 ? O459 N453 1.45(3) 2_766 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Cu1 O4 89.8(2) . . ? O3 Cu1 O2 88.8(2) . . ? O4 Cu1 O2 176.3(2) . . ? O3 Cu1 O1 175.4(2) . . ? O4 Cu1 O1 90.2(2) . . ? O2 Cu1 O1 90.9(2) . . ? O25 S1 C181 104.3(3) . . ? O25 S1 C180 101.0(3) . . ? C181 S1 C180 99.7(6) . . ? C6 O1 Cu7 123.0(4) . . ? C6 O1 Cu1 114.7(4) . . ? Cu7 O1 Cu1 119.1(2) . . ? C6 C1 C2 119.0(7) . . ? C6 C1 C28 123.0(7) . . ? C2 C1 C28 117.9(7) . . ? O7 Cu2 O5 179.0(2) . . ? O7 Cu2 O6 88.5(2) . . ? O5 Cu2 O6 90.5(2) . . ? O7 Cu2 O8 91.6(2) . . ? O5 Cu2 O8 89.5(2) . . ? O6 Cu2 O8 175.7(2) . . ? O26 S2 C183 102.8(4) . . ? O26 S2 C182 103.9(4) . . ? C183 S2 C182 99.0(5) . . ? C13 O2 Cu5 127.7(5) . . ? C13 O2 Cu1 119.5(5) . . ? Cu5 O2 Cu1 112.6(2) . . ? C1 C2 C3 122.0(8) . . ? O12 Cu3 O9 88.9(2) . . ? O12 Cu3 O10 176.9(2) . . ? O9 Cu3 O10 91.5(2) . . ? O12 Cu3 O11 90.1(2) . . ? O9 Cu3 O11 171.7(2) . . ? O10 Cu3 O11 89.0(2) . . ? O27 S3 C185 103.2(3) . . ? O27 S3 C184 104.0(3) . . ? C185 S3 C184 99.0(5) . . ? C20 O3 Cu1 120.9(4) . . ? C20 O3 Cu4 125.5(4) . . ? Cu1 O3 Cu4 110.6(2) . . ? C4 C3 C2 116.7(7) . . ? C4 C3 C29 123.9(7) . . ? C2 C3 C29 119.3(8) . . ? O25 Cu4 O13 165.9(2) . . ? O25 Cu4 O3 89.5(2) . . ? O13 Cu4 O3 85.8(2) . . ? O25 Cu4 O10 95.7(2) . . ? O13 Cu4 O10 86.3(2) . . ? O3 Cu4 O10 166.8(2) . . ? O25 Cu4 O16 83.7(4) . . ? O13 Cu4 O16 110.0(3) . . ? O3 Cu4 O16 97.1(3) . . ? O10 Cu4 O16 95.5(3) . . ? O28 S4 C186 103.1(3) . . ? O28 S4 C187 102.8(3) . . ? C186 S4 C187 99.8(4) . . ? C27 O4 Cu1 115.3(4) . . ? C27 O4 Cu6 122.1(5) . . ? Cu1 O4 Cu6 119.5(3) . . ? C3 C4 C5 123.5(7) . . ? O26 Cu5 O13 173.7(2) . . ? O26 Cu5 O2 91.3(2) . . ? O13 Cu5 O2 82.5(2) . . ? O26 Cu5 O11 95.1(2) . . ? O13 Cu5 O11 91.2(2) . . ? O2 Cu5 O11 165.7(2) . . ? O29 S5 C191 103.4(5) . . ? O29 S5 C190 106.4(4) . . ? C191 S5 C190 93.3(6) . . ? C50 O5 Cu2 115.5(3) . . ? C50 O5 Cu9 119.7(3) . . ? Cu2 O5 Cu9 121.7(2) . . ? C4 C5 C6 118.4(8) . . ? C4 C5 C7 119.0(7) . . ? C6 C5 C7 122.3(7) . . ? O27 Cu6 O14 166.1(2) . . ? O27 Cu6 O7 94.8(2) . . ? O14 Cu6 O7 82.3(2) . . ? O27 Cu6 O4 91.1(2) . . ? O14 Cu6 O4 89.1(2) . . ? O7 Cu6 O4 166.7(2) . . ? O27 Cu6 O19 85.5(3) . . ? O14 Cu6 O19 108.3(3) . . ? O7 Cu6 O19 96.6(3) . . ? O4 Cu6 O19 95.7(3) . . ? C57 O6 Cu2 122.0(3) . . ? C57 O6 Cu7 126.5(3) . . ? Cu2 O6 Cu7 109.2(2) . . ? O1 C6 C5 120.3(7) . . ? O1 C6 C1 119.4(7) . . ? C5 C6 C1 120.3(7) . . ? O28 Cu7 O14 174.2(2) . . ? O28 Cu7 O1 92.3(2) . . ? O14 Cu7 O1 89.7(2) . . ? O28 Cu7 O6 93.1(2) . . ? O14 Cu7 O6 84.1(2) . . ? O1 Cu7 O6 169.8(2) . . ? O30 S7 C188 104.0(4) . . ? O30 S7 C189 104.0(3) . . ? C188 S7 C189 98.1(5) . . ? C64 O7 Cu2 121.6(3) . . ? C64 O7 Cu6 126.2(3) . . ? Cu2 O7 Cu6 111.4(2) . . ? C5 C7 C8 110.3(6) . . ? O29 Cu8 O15 173.8(3) . . ? O29 Cu8 O9 92.9(2) . . ? O15 Cu8 O9 83.3(2) . . ? O29 Cu8 O8 94.4(2) . . ? O15 Cu8 O8 88.5(2) . . ? O9 Cu8 O8 166.6(2) . . ? O501 S500 C502 110.0(11) . . ? O501 S500 C503 93.9(11) . . ? C502 S500 C503 65.6(10) . . ? C71 O8 Cu2 115.8(3) . . ? C71 O8 Cu8 121.9(3) . . ? Cu2 O8 Cu8 118.8(2) . . ? O42 N3 O38 150.0(19) . . ? O42 N3 O39 93.6(18) . . ? O38 N3 O39 116.4(18) . . ? N3 O42 O42 125(3) . 2_765 ? C13 C8 C9 118.7(8) . . ? C13 C8 C7 120.5(7) . . ? C9 C8 C7 120.3(8) . . ? O12 Cu9 O30 93.9(2) . . ? O12 Cu9 O15 83.2(2) . . ? O30 Cu9 O15 162.4(2) . . ? O12 Cu9 O5 166.8(2) . . ? O30 Cu9 O5 92.8(2) . . ? O15 Cu9 O5 87.0(2) . . ? O12 Cu9 O22 99.9(2) . . ? O30 Cu9 O22 86.4(2) . . ? O15 Cu9 O22 111.2(2) . . ? O5 Cu9 O22 91.9(2) . . ? O505 S504 C506 107.2(10) . . ? O505 S504 C507 103.5(9) . . ? C506 S504 C507 107.7(13) . . ? C94 O9 Cu3 117.8(3) . . ? C94 O9 Cu8 128.8(3) . . ? Cu3 O9 Cu8 111.9(2) . . ? C8 C9 C10 121.5(8) . . ? C101 O10 Cu3 116.3(3) . . ? C101 O10 Cu4 120.5(3) . . ? Cu3 O10 Cu4 122.3(2) . . ? C11 C10 C9 117.0(8) . . ? C11 C10 C33 122.5(8) . . ? C9 C10 C33 120.4(8) . . ? O33 S11 C302 110.5(4) . . ? O33 S11 C303 104.9(4) . . ? C302 S11 C303 96.0(5) . . ? C108 O11 Cu5 123.7(4) . . ? C108 O11 Cu3 112.6(3) . . ? Cu5 O11 Cu3 117.6(3) . . ? C10 C11 C12 123.9(8) . . ? O35 S12 C305 107.7(4) . . ? O35 S12 C304 105.3(3) . . ? C305 S12 C304 96.5(5) . . ? C115 O12 Cu3 122.1(3) . . ? C115 O12 Cu9 124.2(3) . . ? Cu3 O12 Cu9 113.1(3) . . ? C11 C12 C13 117.5(8) . . ? C11 C12 C14 120.5(7) . . ? C13 C12 C14 122.0(7) . . ? Cu4 O13 Cu5 110.0(3) . . ? O2 C13 C8 119.4(7) . . ? O2 C13 C12 119.3(7) . . ? C8 C13 C12 121.3(7) . . ? Cu7 O14 Cu6 108.3(3) . . ? C15 C14 C12 113.3(7) . . ? C310 S15 C309 106.1(12) . . ? Cu8 O15 Cu9 110.3(2) . . ? C16 C15 C20 119.5(8) . . ? C16 C15 C14 119.8(7) . . ? C20 C15 C14 120.7(7) . . ? C312 S16 O312 106.2(13) . . ? C312 S16 C309 101.8(9) . . ? O312 S16 C309 102.2(10) . . ? N1 O16 Cu4 121.6(7) . . ? O23 N2 O24 121.0(8) . . ? O23 N2 O22 120.0(7) . . ? O24 N2 O22 118.9(7) . . ? C15 C16 C17 122.4(8) . . ? C311 S17 O308 108.5(19) . . ? C311 S17 C309 109.5(15) . . ? O308 S17 C309 91.9(12) . . ? O18 N1 O20 136.8(14) . . ? O18 N1 O17 51.4(8) . . ? O20 N1 O17 168.2(12) . . ? O18 N1 O21 171.9(12) . . ? O20 N1 O21 46.0(8) . . ? O17 N1 O21 124.6(11) . . ? O18 N1 O19 67.7(10) . . ? O20 N1 O19 71.4(10) . . ? O17 N1 O19 118.6(9) . . ? O21 N1 O19 116.9(10) . . ? O18 N1 O16 112.6(12) . . ? O20 N1 O16 110.6(11) . . ? O17 N1 O16 61.9(8) . . ? O21 N1 O16 65.2(8) . . ? O19 N1 O16 163.3(8) . . ? C18 C17 C16 116.3(7) . . ? C18 C17 C37 123.8(8) . . ? C16 C17 C37 119.8(7) . . ? C314 S18 O126 110.8(5) . . ? C314 S18 C313 107.8(6) . . ? O126 S18 C313 95.8(4) . . ? C19 C18 C17 122.4(8) . . ? N1 O19 Cu6 122.5(6) . . ? C18 C19 C20 120.0(7) . . ? C18 C19 C21 120.4(7) . . ? C20 C19 C21 119.6(6) . . ? O3 C20 C19 120.4(7) . . ? O3 C20 C15 120.2(7) . . ? C19 C20 C15 119.4(7) . . ? C22 C21 C19 110.1(6) . . ? N2 O22 Cu9 122.1(5) . . ? C27 C22 C23 119.0(7) . . ? C27 C22 C21 121.5(7) . . ? C23 C22 C21 119.5(7) . . ? C24 C23 C22 123.3(7) . . ? C23 C24 C25 116.4(7) . . ? C23 C24 C41 123.3(7) . . ? C25 C24 C41 120.2(7) . . ? S1 O25 Cu4 132.8(4) . . ? C26 C25 C24 122.3(7) . . ? S2 O26 Cu5 123.2(4) . . ? C25 C26 C27 119.8(7) . . ? C25 C26 C28 118.7(7) . . ? C27 C26 C28 121.4(7) . . ? S3 O27 Cu6 128.3(4) . . ? O4 C27 C22 120.4(7) . . ? O4 C27 C26 120.3(6) . . ? C22 C27 C26 119.3(7) . . ? S4 O28 Cu7 124.6(3) . . ? C1 C28 C26 112.0(6) . . ? S6 O29 S5 65.1(5) . . ? S6 O29 Cu8 158.3(8) . . ? S5 O29 Cu8 135.1(7) . . ? C30 C29 C32 108.4(7) . . ? C30 C29 C31 109.0(7) . . ? C32 C29 C31 108.4(7) . . ? C30 C29 C3 110.8(7) . . ? C32 C29 C3 108.6(6) . . ? C31 C29 C3 111.5(7) . . ? S7 O30 Cu9 128.3(3) . . ? S10 O33 S11 51.1(6) . . ? C34 C33 C36 108.7(9) . . ? C34 C33 C35A 94.7(11) . . ? C36 C33 C35A 118.5(8) . . ? C34 C33 C35 123.6(11) . . ? C36 C33 C35 93.9(11) . . ? C35A C33 C35 31.7(11) . . ? C34 C33 C10 111.5(8) . . ? C36 C33 C10 110.6(8) . . ? C35A C33 C10 111.7(7) . . ? C35 C33 C10 106.9(10) . . ? S12 O35 S13 50.0(5) . . ? C39 C37 C17 108.6(7) . . ? C39 C37 C40 109.6(8) . . ? C17 C37 C40 111.7(7) . . ? C39 C37 C38 109.6(9) . . ? C17 C37 C38 110.3(7) . . ? C40 C37 C38 107.0(8) . . ? C42 C41 C44 109.2(6) . . ? C42 C41 C43 108.5(7) . . ? C44 C41 C43 108.7(6) . . ? C42 C41 C24 107.4(7) . . ? C44 C41 C24 111.2(6) . . ? C43 C41 C24 111.8(6) . . ? C46 C45 C50 119.1(7) . . ? C46 C45 C72 119.6(8) . . ? C50 C45 C72 121.3(7) . . ? C45 C46 C47 122.3(8) . . ? C48 C47 C46 117.3(8) . . ? C48 C47 C73 119.5(8) . . ? C46 C47 C73 123.2(9) . . ? C47 C48 C49 122.7(8) . . ? C50 C49 C48 118.6(7) . . ? C50 C49 C51 121.6(7) . . ? C48 C49 C51 119.8(7) . . ? O5 C50 C49 120.1(7) . . ? O5 C50 C45 119.8(6) . . ? C49 C50 C45 120.1(7) . . ? C52 C51 C49 111.7(6) . . ? C57 C52 C53 118.0(7) . . ? C57 C52 C51 121.4(7) . . ? C53 C52 C51 120.4(7) . . ? C54 C53 C52 123.6(7) . . ? C53 C54 C55 116.9(7) . . ? C53 C54 C80 122.5(7) . . ? C55 C54 C80 120.4(7) . . ? C54 C55 C56 122.5(8) . . ? C55 C56 C57 119.5(7) . . ? C55 C56 C58 119.6(7) . . ? C57 C56 C58 120.8(7) . . ? O6 C57 C56 122.3(6) . . ? O6 C57 C52 118.3(6) . . ? C56 C57 C52 119.4(7) . . ? C59 C58 C56 113.0(6) . . ? C64 C59 C60 119.2(7) . . ? C64 C59 C58 121.7(7) . . ? C60 C59 C58 119.1(7) . . ? C59 C60 C61 122.2(7) . . ? C62 C61 C60 116.0(7) . . ? C62 C61 C81 121.5(7) . . ? C60 C61 C81 122.4(7) . . ? C63 C62 C61 123.6(7) . . ? C62 C63 C64 118.8(7) . . ? C62 C63 C65 122.1(7) . . ? C64 C63 C65 119.0(7) . . ? O7 C64 C59 121.0(6) . . ? O7 C64 C63 118.8(6) . . ? C59 C64 C63 120.2(7) . . ? C66 C65 C63 112.2(6) . . ? C71 C66 C67 120.1(7) . . ? C71 C66 C65 122.2(7) . . ? C67 C66 C65 117.7(7) . . ? C68 C67 C66 121.8(7) . . ? C67 C68 C69 116.9(7) . . ? C67 C68 C85 122.0(7) . . ? C69 C68 C85 121.2(7) . . ? C70 C69 C68 123.1(8) . . ? C69 C70 C71 119.4(7) . . ? C69 C70 C72 120.2(7) . . ? C71 C70 C72 120.3(7) . . ? O8 C71 C66 121.0(6) . . ? O8 C71 C70 120.5(7) . . ? C66 C71 C70 118.5(7) . . ? C45 C72 C70 110.6(6) . . ? C75A C73 C76 126.9(11) . . ? C75A C73 C74 73.8(14) . . ? C76 C73 C74 114.4(14) . . ? C75A C73 C47 114.5(10) . . ? C76 C73 C47 110.5(8) . . ? C74 C73 C47 110.8(14) . . ? C75A C73 C75 35.3(9) . . ? C76 C73 C75 102.4(10) . . ? C74 C73 C75 107.4(14) . . ? C47 C73 C75 111.0(10) . . ? C75A C73 C74A 98.2(16) . . ? C76 C73 C74A 94.0(14) . . ? C74 C73 C74A 25.4(15) . . ? C47 C73 C74A 107.3(14) . . ? C75 C73 C74A 129.2(16) . . ? C77 C80 C79B 50.2(15) . . ? C77 C80 C78 120.3(19) . . ? C79B C80 C78 128(2) . . ? C77 C80 C79A 74.6(17) . . ? C79B C80 C79A 24.6(14) . . ? C78 C80 C79A 117(2) . . ? C77 C80 C78B 132.3(19) . . ? C79B C80 C78B 112.6(18) . . ? C78 C80 C78B 27.4(17) . . ? C79A C80 C78B 94.6(19) . . ? C77 C80 C78A 132(2) . . ? C79B C80 C78A 127(2) . . ? C78 C80 C78A 13(3) . . ? C79A C80 C78A 111(2) . . ? C78B C80 C78A 17(2) . . ? C77 C80 C77A 34.2(14) . . ? C79B C80 C77A 83.2(17) . . ? C78 C80 C77A 95(2) . . ? C79A C80 C77A 106.7(19) . . ? C78B C80 C77A 118(2) . . ? C78A C80 C77A 108(2) . . ? C77 C80 C54 111.2(13) . . ? C79B C80 C54 114.8(13) . . ? C78 C80 C54 114.9(16) . . ? C79A C80 C54 112.2(15) . . ? C78B C80 C54 115.7(15) . . ? C78A C80 C54 110.2(17) . . ? C77A C80 C54 108.6(14) . . ? C77 C80 C77B 53.0(16) . . ? C79B C80 C77B 101.1(16) . . ? C78 C80 C77B 79.2(18) . . ? C79A C80 C77B 123.5(17) . . ? C78B C80 C77B 104.9(18) . . ? C78A C80 C77B 92(2) . . ? C77A C80 C77B 18.9(16) . . ? C54 C80 C77B 105.7(12) . . ? C77 C80 C79 98.4(17) . . ? C79B C80 C79 48.3(15) . . ? C78 C80 C79 105(2) . . ? C79A C80 C79 23.7(14) . . ? C78B C80 C79 78.6(17) . . ? C78A C80 C79 95(2) . . ? C77A C80 C79 129.9(18) . . ? C54 C80 C79 103.7(12) . . ? C77B C80 C79 144.9(16) . . ? C84 C81 C82 107.8(8) . . ? C84 C81 C61 110.2(7) . . ? C82 C81 C61 113.2(7) . . ? C84 C81 C83 109.4(8) . . ? C82 C81 C83 108.2(7) . . ? C61 C81 C83 108.1(7) . . ? C86 C85 C88 109.3(7) . . ? C86 C85 C68 113.2(7) . . ? C88 C85 C68 109.8(7) . . ? C86 C85 C87 107.4(8) . . ? C88 C85 C87 108.5(7) . . ? C68 C85 C87 108.5(7) . . ? C94 C89 C90 118.8(7) . . ? C94 C89 C116 120.9(7) . . ? C90 C89 C116 120.0(7) . . ? C89 C90 C91 121.9(8) . . ? C92 C91 C90 116.5(7) . . ? C92 C91 C117 122.4(7) . . ? C90 C91 C117 121.0(8) . . ? C93 C92 C91 124.1(8) . . ? C92 C93 C94 118.2(8) . . ? C92 C93 C95 120.4(7) . . ? C94 C93 C95 121.3(7) . . ? O9 C94 C89 121.3(6) . . ? O9 C94 C93 118.3(7) . . ? C89 C94 C93 120.4(7) . . ? C93 C95 C96 110.8(7) . . ? C101 C96 C97 119.1(8) . . ? C101 C96 C95 120.8(7) . . ? C97 C96 C95 120.0(7) . . ? C98 C97 C96 122.1(8) . . ? C97 C98 C99 116.2(8) . . ? C97 C98 C124 122.8(9) . . ? C99 C98 C124 121.0(9) . . ? C100 C99 C98 123.2(8) . . ? C101 C100 C99 118.4(8) . . ? C101 C100 C102 122.2(7) . . ? C99 C100 C102 119.3(8) . . ? O10 C101 C100 119.7(7) . . ? O10 C101 C96 119.3(7) . . ? C100 C101 C96 121.0(7) . . ? C103 C102 C100 111.7(7) . . ? C104 C103 C108 120.3(9) . . ? C104 C103 C102 118.1(8) . . ? C108 C103 C102 121.6(8) . . ? C103 C104 C105 122.4(9) . . ? C104 C105 C106 116.6(9) . . ? C104 C105 C128 123.9(10) . . ? C106 C105 C128 119.1(10) . . ? C107 C106 C105 121.8(9) . . ? C106 C107 C108 121.4(8) . . ? C106 C107 C109 117.1(8) . . ? C108 C107 C109 121.3(8) . . ? O11 C108 C107 121.5(7) . . ? O11 C108 C103 120.9(7) . . ? C107 C108 C103 117.5(8) . . ? C110 C109 C107 111.4(7) . . ? C111 C110 C115 119.3(9) . . ? C111 C110 C109 121.8(9) . . ? C115 C110 C109 118.7(8) . . ? C112 C111 C110 122.4(9) . . ? C111 C112 C113 117.4(8) . . ? C111 C112 C151 113.2(10) . . ? C113 C112 C151 129.1(10) . . ? C111 C112 C152 130.9(10) . . ? C113 C112 C152 109.8(11) . . ? C151 C112 C152 26.6(7) . . ? C114 C113 C112 122.6(10) . . ? C113 C114 C115 117.9(8) . . ? C113 C114 C116 121.0(8) . . ? C115 C114 C116 121.1(7) . . ? O12 C115 C110 119.5(8) . . ? O12 C115 C114 120.1(7) . . ? C110 C115 C114 120.4(8) . . ? C114 C116 C89 112.8(7) . . ? C123 C117 C119 115.8(12) . . ? C123 C117 C122 42.7(13) . . ? C119 C117 C122 140.2(15) . . ? C123 C117 C120 128.6(13) . . ? C119 C117 C120 51.1(14) . . ? C122 C117 C120 110.1(19) . . ? C123 C117 C91 113.8(9) . . ? C119 C117 C91 108.5(9) . . ? C122 C117 C91 111.2(14) . . ? C120 C117 C91 117.3(12) . . ? C123 C117 C121 103.8(11) . . ? C119 C117 C121 106.5(10) . . ? C122 C117 C121 63.8(15) . . ? C120 C117 C121 55.6(14) . . ? C91 C117 C121 107.7(9) . . ? C123 C117 C118 61.0(15) . . ? C119 C117 C118 61.5(14) . . ? C122 C117 C118 102.8(19) . . ? C120 C117 C118 106.6(18) . . ? C91 C117 C118 107.6(12) . . ? C121 C117 C118 144.6(13) . . ? C126 C124 C127 106.3(12) . . ? C126 C124 C125 108.9(11) . . ? C127 C124 C125 109.2(13) . . ? C126 C124 C98 109.4(11) . . ? C127 C124 C98 110.9(10) . . ? C125 C124 C98 112.0(9) . . ? S19 O126 S18 51.0(3) . . ? C131 C128 C129 132.5(17) . . ? C131 C128 C132 92.3(14) . . ? C129 C128 C132 89.3(16) . . ? C131 C128 C105 110.9(13) . . ? C129 C128 C105 114.5(15) . . ? C132 C128 C105 104.5(13) . . ? C131 C128 C130 87.0(15) . . ? C129 C128 C130 67.9(16) . . ? C132 C128 C130 147.1(18) . . ? C105 C128 C130 106.4(15) . . ? C150 C151 C160 112.9(15) . . ? C150 C151 C112 116.2(13) . . ? C160 C151 C112 104.7(13) . . ? C150 C151 C155 112.9(14) . . ? C160 C151 C155 105.8(14) . . ? C112 C151 C155 103.2(11) . . ? C158 C152 C157 108.7(18) . . ? C158 C152 C156 101.5(17) . . ? C157 C152 C156 103.7(17) . . ? C158 C152 C112 110.3(14) . . ? C157 C152 C112 109.5(15) . . ? C156 C152 C112 122.2(15) . . ? S15 C309 S16 21.9(4) . . ? S15 C309 S17 38.8(6) . . ? S16 C309 S17 17.4(5) . . ? O316 C317 C318 136(2) . . ? O316 C317 C319 172.4(19) . . ? C318 C317 C319 36.4(16) . . ? O316 C317 C320 128.2(19) . . ? C318 C317 C320 24.9(17) . . ? C319 C317 C320 45.1(17) . . ? O456 N453 O455 174(3) . . ? O456 N453 O457 100(3) . . ? O455 N453 O457 86(3) . . ? O456 N453 O458 118(3) . . ? O455 N453 O458 57(2) . . ? O457 N453 O458 142(3) . . ? O456 N453 O454 134(2) . . ? O455 N453 O454 52(2) . . ? O457 N453 O454 33.1(18) . . ? O458 N453 O454 109(2) . . ? O456 N453 O459 27.9(16) . . ? O455 N453 O459 151.7(17) . . ? O457 N453 O459 98(2) . . ? O458 N453 O459 115(2) . . ? O454 N453 O459 126.3(17) . . ? O456 N453 O459 89.3(14) . 2_766 ? O455 N453 O459 91.2(14) . 2_766 ? O457 N453 O459 85.1(15) . 2_766 ? O458 N453 O459 95.0(17) . 2_766 ? O454 N453 O459 86.8(12) . 2_766 ? O459 N453 O459 117.0(16) . 2_766 ? N453 O459 N453 63.0(16) . 2_766 ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 23.24 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.368 _refine_diff_density_min -0.985 _refine_diff_density_rms 0.112