# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_publication_text _publ_contact_author 'Xiong Li' _publ_contact_author_email 'lxwhu2008@hotmail.com' loop_ _publ_author_name 'Xiong Li' 'Shu-Ling Gong' 'Wei-Ping Yang' 'Yuan-Yin Chen' 'Xiang-Gao Meng' _journal_name_full 'Dalton Transactions' data_CCDC-740901 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,3-alternate-5,11,17,23-Tetra-tert-butyl-25,27-[1,2- bis(oxyethoxy)benzene]-2,8,14,20-tetra-thiacalix[4]arene ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H62 Cl4 O6 S4' _chemical_formula_weight 1053.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.0598(11) _cell_length_b 14.4713(11) _cell_length_c 16.9810(13) _cell_angle_alpha 76.995(2) _cell_angle_beta 69.653(2) _cell_angle_gamma 87.282(2) _cell_volume 3154.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 7530 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 26.25 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.109 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1108 _exptl_absorpt_coefficient_mu 0.360 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30649 _diffrn_reflns_av_R_equivalents 0.0785 _diffrn_reflns_av_sigmaI/netI 0.0716 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11058 _reflns_number_gt 7274 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. During the refinement, some tert-butyl groups were found to be seriously disordered. Commands ¡®SIMU¡¯and ¡®DFIX¡¯ were used to refine them to arrive at more appropriate values. During the refinement, the non-coordinated solvent molecules are severely disordered which could not be modeled by discrete atoms in the complexes. Correspondingly, the contribution of the solvent to the diffraction pattern was subtracted using SQUEEZE procedure of the PLATON. ; _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^)+(0.1697P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11058 _refine_ls_number_parameters 669 _refine_ls_number_restraints 1418 _refine_ls_R_factor_all 0.1084 _refine_ls_R_factor_gt 0.0823 _refine_ls_wR_factor_ref 0.2623 _refine_ls_wR_factor_gt 0.2395 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.121 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9919(3) 0.7461(3) 0.5191(3) 0.0504(10) Uani 1 1 d U . . C2 C 0.9522(3) 0.8359(3) 0.5155(3) 0.0472(9) Uani 1 1 d U . . C3 C 0.9090(4) 0.8660(4) 0.5913(3) 0.0617(11) Uani 1 1 d U . . H3 H 0.8814 0.9257 0.5904 0.074 Uiso 1 1 calc R . . C4 C 0.9065(4) 0.8071(4) 0.6699(4) 0.0728(13) Uani 1 1 d U . . H4 H 0.8778 0.8276 0.7210 0.087 Uiso 1 1 calc R . . C5 C 0.9462(4) 0.7198(4) 0.6705(4) 0.0757(14) Uani 1 1 d U . . H5 H 0.9448 0.6807 0.7226 0.091 Uiso 1 1 calc R . . C6 C 0.9880(4) 0.6885(4) 0.5968(3) 0.0617(11) Uani 1 1 d U . . H6 H 1.0141 0.6281 0.5987 0.074 Uiso 1 1 calc R . . C7 C 1.0081(3) 0.6283(3) 0.4365(3) 0.0493(10) Uani 1 1 d U . . H7A H 1.0271 0.5797 0.4774 0.059 Uiso 1 1 calc R . . H7B H 1.0441 0.6181 0.3792 0.059 Uiso 1 1 calc R . . C8 C 0.8980(3) 0.6210(3) 0.4553(3) 0.0495(10) Uani 1 1 d U . . H8A H 0.8625 0.6153 0.5165 0.059 Uiso 1 1 calc R . . H8B H 0.8763 0.6782 0.4246 0.059 Uiso 1 1 calc R . . C9 C 0.8141(3) 0.5566(3) 0.3782(3) 0.0386(9) Uani 1 1 d U . . C10 C 0.7100(3) 0.5714(3) 0.4099(3) 0.0395(8) Uani 1 1 d U . . C11 C 0.6533(3) 0.5813(3) 0.3570(3) 0.0455(9) Uani 1 1 d U . . H11 H 0.5837 0.5879 0.3806 0.055 Uiso 1 1 calc R . . C12 C 0.6955(4) 0.5818(3) 0.2699(3) 0.0509(10) Uani 1 1 d U A . C13 C 0.7999(3) 0.5674(3) 0.2391(3) 0.0499(10) Uani 1 1 d U . . H13 H 0.8310 0.5646 0.1816 0.060 Uiso 1 1 calc R . . C14 C 0.8584(3) 0.5571(3) 0.2909(3) 0.0415(9) Uani 1 1 d U . . C15 C 0.6324(4) 0.5931(4) 0.2124(3) 0.0675(13) Uani 1 1 d U . . C16 C 0.6931(9) 0.6035(11) 0.1191(7) 0.088(3) Uani 0.580(6) 1 d PU A 1 H16A H 0.7431 0.6541 0.1013 0.132 Uiso 0.580(6) 1 calc PR A 1 H16B H 0.6490 0.6178 0.0860 0.132 Uiso 0.580(6) 1 calc PR A 1 H16C H 0.7264 0.5454 0.1100 0.132 Uiso 0.580(6) 1 calc PR A 1 C17 C 0.5671(10) 0.5004(10) 0.2365(8) 0.090(3) Uani 0.580(6) 1 d PU A 1 H17A H 0.6108 0.4473 0.2310 0.136 Uiso 0.580(6) 1 calc PR A 1 H17B H 0.5292 0.5049 0.1985 0.136 Uiso 0.580(6) 1 calc PR A 1 H17C H 0.5211 0.4916 0.2948 0.136 Uiso 0.580(6) 1 calc PR A 1 C18 C 0.5596(10) 0.6793(10) 0.2296(8) 0.094(3) Uani 0.580(6) 1 d PU A 1 H18A H 0.5160 0.6662 0.2889 0.141 Uiso 0.580(6) 1 calc PR A 1 H18B H 0.5192 0.6876 0.1933 0.141 Uiso 0.580(6) 1 calc PR A 1 H18C H 0.5997 0.7362 0.2170 0.141 Uiso 0.580(6) 1 calc PR A 1 C16' C 0.6895(13) 0.6715(15) 0.1306(11) 0.093(4) Uani 0.420(6) 1 d PU A 2 H16D H 0.7568 0.6822 0.1295 0.139 Uiso 0.420(6) 1 calc PR A 2 H16E H 0.6533 0.7294 0.1326 0.139 Uiso 0.420(6) 1 calc PR A 2 H16F H 0.6932 0.6510 0.0797 0.139 Uiso 0.420(6) 1 calc PR A 2 C17' C 0.6220(15) 0.5059(14) 0.1900(13) 0.094(3) Uani 0.420(6) 1 d PU A 2 H17D H 0.6821 0.4965 0.1440 0.141 Uiso 0.420(6) 1 calc PR A 2 H17E H 0.5643 0.5079 0.1718 0.141 Uiso 0.420(6) 1 calc PR A 2 H17F H 0.6125 0.4545 0.2393 0.141 Uiso 0.420(6) 1 calc PR A 2 C18' C 0.5205(12) 0.6201(14) 0.2576(11) 0.087(3) Uani 0.420(6) 1 d PU A 2 H18D H 0.4992 0.5917 0.3181 0.131 Uiso 0.420(6) 1 calc PR A 2 H18E H 0.4768 0.5973 0.2330 0.131 Uiso 0.420(6) 1 calc PR A 2 H18F H 0.5169 0.6878 0.2495 0.131 Uiso 0.420(6) 1 calc PR A 2 C19 C 1.0130(3) 0.6537(3) 0.1583(3) 0.0441(9) Uani 1 1 d U . . C20 C 0.9986(3) 0.7432(3) 0.1780(3) 0.0427(9) Uani 1 1 d U . . C21 C 1.0108(3) 0.8230(3) 0.1099(2) 0.0388(8) Uani 1 1 d U . . C22 C 1.0370(4) 0.8122(3) 0.0269(3) 0.0515(10) Uani 1 1 d U . . H22 H 1.0442 0.8662 -0.0168 0.062 Uiso 1 1 calc R . . C23 C 1.0535(4) 0.7240(3) 0.0050(3) 0.0540(11) Uani 1 1 d U A . C24 C 1.0396(4) 0.6459(3) 0.0737(3) 0.0529(10) Uani 1 1 d U . . H24 H 1.0486 0.5857 0.0620 0.063 Uiso 1 1 calc R . . C25 C 1.0810(5) 0.7132(4) -0.0872(3) 0.0784(15) Uani 1 1 d U . . C26 C 1.0132(12) 0.7783(10) -0.1302(8) 0.096(3) Uani 0.580(6) 1 d PU A 1 H26A H 1.0298 0.7717 -0.1885 0.145 Uiso 0.580(6) 1 calc PR A 1 H26B H 1.0248 0.8432 -0.1302 0.145 Uiso 0.580(6) 1 calc PR A 1 H26C H 0.9430 0.7603 -0.0985 0.145 Uiso 0.580(6) 1 calc PR A 1 C27 C 1.1840(11) 0.7654(9) -0.1394(7) 0.106(3) Uani 0.580(6) 1 d PU A 1 H27A H 1.2376 0.7240 -0.1335 0.159 Uiso 0.580(6) 1 calc PR A 1 H27B H 1.1881 0.8207 -0.1182 0.159 Uiso 0.580(6) 1 calc PR A 1 H27C H 1.1905 0.7841 -0.1990 0.159 Uiso 0.580(6) 1 calc PR A 1 C28 C 1.0741(13) 0.6197(8) -0.0989(7) 0.092(3) Uani 0.580(6) 1 d PU A 1 H28A H 1.0073 0.5928 -0.0653 0.138 Uiso 0.580(6) 1 calc PR A 1 H28B H 1.1234 0.5812 -0.0806 0.138 Uiso 0.580(6) 1 calc PR A 1 H28C H 1.0870 0.6220 -0.1587 0.138 Uiso 0.580(6) 1 calc PR A 1 C29 C 0.8630(3) 0.9477(3) 0.1712(3) 0.0402(9) Uani 1 1 d U . . C30 C 0.8107(3) 0.9453(3) 0.2579(2) 0.0366(8) Uani 1 1 d U . . C31 C 0.7069(3) 0.9603(3) 0.2856(3) 0.0393(8) Uani 1 1 d U . . C32 C 0.6575(3) 0.9751(3) 0.2271(3) 0.0519(10) Uani 1 1 d U . . H32 H 0.5883 0.9856 0.2458 0.062 Uiso 1 1 calc R . . C33 C 0.7083(4) 0.9749(3) 0.1400(3) 0.0553(11) Uani 1 1 d U . . C34 C 0.8107(3) 0.9624(3) 0.1142(3) 0.0476(9) Uani 1 1 d U . . H34 H 0.8463 0.9637 0.0564 0.057 Uiso 1 1 calc R . . C35 C 0.6506(4) 0.9944(4) 0.0753(4) 0.0738(14) Uani 1 1 d U . . C36 C 0.5443(6) 0.9564(7) 0.1153(5) 0.130(3) Uani 1 1 d U . . H36A H 0.5081 0.9870 0.1612 0.195 Uiso 1 1 calc R . . H36B H 0.5440 0.8893 0.1379 0.195 Uiso 1 1 calc R . . H36C H 0.5121 0.9682 0.0727 0.195 Uiso 1 1 calc R . . C37 C 0.6685(8) 1.0932(7) 0.0309(6) 0.147(3) Uani 1 1 d U . . H37A H 0.6472 1.1036 -0.0183 0.221 Uiso 1 1 calc R . . H37B H 0.7395 1.1094 0.0122 0.221 Uiso 1 1 calc R . . H37C H 0.6305 1.1322 0.0692 0.221 Uiso 1 1 calc R . . C38 C 0.6985(7) 0.9400(7) 0.0037(5) 0.135(3) Uani 1 1 d U . . H38A H 0.7151 0.8777 0.0284 0.202 Uiso 1 1 calc R . . H38B H 0.7591 0.9735 -0.0374 0.202 Uiso 1 1 calc R . . H38C H 0.6513 0.9348 -0.0246 0.202 Uiso 1 1 calc R . . C39 C 0.5775(3) 0.8510(3) 0.4402(3) 0.0382(8) Uani 1 1 d U . . C40 C 0.6318(3) 0.7716(3) 0.4594(3) 0.0410(9) Uani 1 1 d U . . C41 C 0.5790(3) 0.6843(3) 0.4996(3) 0.0416(9) Uani 1 1 d U . . C42 C 0.4754(3) 0.6791(3) 0.5200(3) 0.0415(9) Uani 1 1 d U . . H42 H 0.4414 0.6207 0.5470 0.050 Uiso 1 1 calc R . . C43 C 0.4193(3) 0.7580(3) 0.5016(3) 0.0430(9) Uani 1 1 d U . . C44 C 0.4726(3) 0.8432(3) 0.4618(3) 0.0405(9) Uani 1 1 d U . . H44 H 0.4375 0.8973 0.4490 0.049 Uiso 1 1 calc R . . C45 C 0.3047(3) 0.7468(3) 0.5245(3) 0.0489(10) Uani 1 1 d U . . C46 C 0.2850(4) 0.6825(4) 0.4717(4) 0.0638(13) Uani 1 1 d U . . H46A H 0.2132 0.6744 0.4857 0.096 Uiso 1 1 calc R . . H46B H 0.3135 0.6218 0.4847 0.096 Uiso 1 1 calc R . . H46C H 0.3158 0.7106 0.4115 0.096 Uiso 1 1 calc R . . C47 C 0.2568(4) 0.8409(4) 0.5037(4) 0.0767(16) Uani 1 1 d U . . H47A H 0.2661 0.8819 0.5380 0.115 Uiso 1 1 calc R . . H47B H 0.1856 0.8305 0.5164 0.115 Uiso 1 1 calc R . . H47C H 0.2885 0.8698 0.4438 0.115 Uiso 1 1 calc R . . C48 C 0.2564(4) 0.7007(5) 0.6211(4) 0.0846(17) Uani 1 1 d U . . H48A H 0.2765 0.7367 0.6542 0.127 Uiso 1 1 calc R . . H48B H 0.2790 0.6370 0.6321 0.127 Uiso 1 1 calc R . . H48C H 0.1839 0.6997 0.6374 0.127 Uiso 1 1 calc R . . C49 C 0.9008(3) 0.9972(3) 0.3396(3) 0.0408(9) Uani 1 1 d U . . H49A H 0.8614 1.0534 0.3330 0.049 Uiso 1 1 calc R . . H49B H 0.9705 1.0126 0.3017 0.049 Uiso 1 1 calc R . . C50 C 0.8963(3) 0.9663(3) 0.4302(3) 0.0467(10) Uani 1 1 d U . . H50A H 0.9198 1.0176 0.4478 0.056 Uiso 1 1 calc R . . H50B H 0.8269 0.9488 0.4679 0.056 Uiso 1 1 calc R . . C51 C 0.1887(7) 0.8564(8) 0.2703(7) 0.144(3) Uani 1 1 d . . . H51A H 0.1337 0.8570 0.2481 0.173 Uiso 1 1 calc R . . H51B H 0.1616 0.8294 0.3318 0.173 Uiso 1 1 calc R . . C52 C 0.5494(7) 0.8196(6) 0.6612(5) 0.143(3) Uani 1 1 d DU . . H52A H 0.5206 0.8396 0.6160 0.172 Uiso 1 1 calc R . . H52B H 0.5952 0.7693 0.6453 0.172 Uiso 1 1 calc R . . C26' C 1.1620(16) 0.6487(13) -0.1105(10) 0.107(4) Uani 0.420(6) 1 d PU A 2 H26D H 1.2216 0.6716 -0.1047 0.160 Uiso 0.420(6) 1 calc PR A 2 H26E H 1.1765 0.6446 -0.1692 0.160 Uiso 0.420(6) 1 calc PR A 2 H26F H 1.1419 0.5871 -0.0733 0.160 Uiso 0.420(6) 1 calc PR A 2 C27' C 1.0902(16) 0.7976(11) -0.1529(9) 0.084(4) Uani 0.420(6) 1 d PU A 2 H27D H 1.1515 0.8323 -0.1633 0.126 Uiso 0.420(6) 1 calc PR A 2 H27E H 1.0330 0.8363 -0.1344 0.126 Uiso 0.420(6) 1 calc PR A 2 H27F H 1.0924 0.7807 -0.2050 0.126 Uiso 0.420(6) 1 calc PR A 2 C28' C 0.9876(15) 0.6506(13) -0.0850(10) 0.096(4) Uani 0.420(6) 1 d PU A 2 H28D H 1.0078 0.6239 -0.1350 0.144 Uiso 0.420(6) 1 calc PR A 2 H28E H 0.9308 0.6902 -0.0844 0.144 Uiso 0.420(6) 1 calc PR A 2 H28F H 0.9687 0.6004 -0.0340 0.144 Uiso 0.420(6) 1 calc PR A 2 Cl1 Cl 0.2271(4) 0.9654(3) 0.2554(3) 0.242(2) Uani 1 1 d . . . Cl2 Cl 0.2783(6) 0.7854(4) 0.2240(4) 0.311(3) Uani 1 1 d . . . Cl3 Cl 0.6184(3) 0.9074(3) 0.6563(3) 0.2239(18) Uani 1 1 d D . . Cl4 Cl 0.4598(6) 0.7727(5) 0.7448(4) 0.359(4) Uani 1 1 d D . . O1 O 1.0363(2) 0.7199(2) 0.4417(2) 0.0530(8) Uani 1 1 d . . . O2 O 0.8725(2) 0.53948(19) 0.42967(18) 0.0453(7) Uani 1 1 d . . . O3 O 0.9716(2) 0.7496(2) 0.26080(18) 0.0528(8) Uani 1 1 d . . . H3A H 0.9657 0.8055 0.2636 0.079 Uiso 1 1 calc R . . O4 O 0.85999(19) 0.92046(17) 0.31746(16) 0.0372(6) Uani 1 1 d . . . O5 O 0.73283(19) 0.77465(19) 0.4424(2) 0.0499(8) Uani 1 1 d . . . H5A H 0.7551 0.8293 0.4200 0.075 Uiso 1 1 calc R . . O6 O 0.9595(2) 0.8867(2) 0.43620(19) 0.0537(8) Uani 1 1 d . . . S1 S 0.99293(8) 0.55045(7) 0.24300(7) 0.0483(3) Uani 1 1 d . . . S2 S 0.99793(8) 0.93751(7) 0.13328(7) 0.0427(3) Uani 1 1 d . . . S3 S 0.63974(8) 0.96490(7) 0.39561(7) 0.0423(3) Uani 1 1 d . . . S4 S 0.64799(8) 0.57976(7) 0.51922(6) 0.0427(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0428(19) 0.055(2) 0.060(2) -0.0046(19) -0.0295(18) -0.0052(17) C2 0.049(2) 0.049(2) 0.052(2) -0.0084(18) -0.0288(17) -0.0010(17) C3 0.072(3) 0.063(3) 0.056(2) -0.010(2) -0.031(2) 0.000(2) C4 0.084(3) 0.083(3) 0.055(3) -0.017(2) -0.026(2) -0.005(3) C5 0.079(3) 0.079(3) 0.065(3) 0.006(3) -0.033(2) -0.005(3) C6 0.061(2) 0.063(3) 0.062(2) -0.002(2) -0.030(2) 0.002(2) C7 0.046(2) 0.041(2) 0.062(2) -0.0049(19) -0.0239(19) 0.0038(17) C8 0.050(2) 0.049(2) 0.054(2) -0.0149(18) -0.0210(18) 0.0037(18) C9 0.0436(19) 0.0255(17) 0.045(2) -0.0014(15) -0.0172(16) -0.0012(15) C10 0.0457(19) 0.0331(18) 0.0387(18) -0.0071(15) -0.0138(16) -0.0012(15) C11 0.0409(18) 0.047(2) 0.048(2) -0.0069(17) -0.0168(16) 0.0039(16) C12 0.059(2) 0.045(2) 0.053(2) -0.0096(18) -0.0250(18) 0.0023(18) C13 0.054(2) 0.048(2) 0.045(2) -0.0092(17) -0.0148(17) 0.0013(17) C14 0.0447(19) 0.0332(18) 0.0443(19) -0.0054(15) -0.0145(16) 0.0023(15) C15 0.069(3) 0.085(3) 0.060(3) -0.016(2) -0.037(2) 0.011(2) C16 0.090(5) 0.115(6) 0.069(5) -0.011(5) -0.047(4) 0.010(5) C17 0.088(6) 0.117(6) 0.072(5) -0.007(5) -0.040(4) -0.022(5) C18 0.090(6) 0.112(6) 0.083(5) -0.005(5) -0.047(5) 0.031(5) C16' 0.087(6) 0.112(7) 0.076(6) 0.008(6) -0.044(5) 0.014(6) C17' 0.090(6) 0.114(7) 0.085(6) -0.019(6) -0.041(5) 0.003(6) C18' 0.077(6) 0.116(7) 0.072(6) 0.003(6) -0.046(5) 0.011(6) C19 0.044(2) 0.039(2) 0.041(2) -0.0034(16) -0.0078(16) 0.0025(16) C20 0.046(2) 0.0388(19) 0.0370(19) -0.0058(16) -0.0083(16) 0.0028(16) C21 0.0422(19) 0.0334(18) 0.0391(19) -0.0069(15) -0.0126(15) 0.0004(15) C22 0.062(2) 0.042(2) 0.042(2) -0.0044(17) -0.0099(18) -0.0002(18) C23 0.071(2) 0.043(2) 0.042(2) -0.0116(17) -0.0112(19) -0.0039(19) C24 0.066(2) 0.040(2) 0.045(2) -0.0124(17) -0.0080(18) 0.0011(18) C25 0.119(4) 0.059(3) 0.044(2) -0.016(2) -0.009(3) -0.001(3) C26 0.125(6) 0.101(6) 0.064(5) -0.018(5) -0.034(5) 0.007(6) C27 0.127(6) 0.107(6) 0.060(5) -0.030(5) 0.008(5) -0.005(5) C28 0.135(6) 0.076(5) 0.055(5) -0.025(4) -0.013(5) -0.004(5) C29 0.0471(19) 0.0303(18) 0.0413(19) -0.0058(15) -0.0139(16) -0.0010(15) C30 0.0412(18) 0.0299(17) 0.0397(18) -0.0043(15) -0.0170(15) -0.0013(15) C31 0.0394(18) 0.0314(18) 0.0436(19) -0.0021(15) -0.0140(15) -0.0001(15) C32 0.048(2) 0.054(2) 0.053(2) -0.0011(18) -0.0221(18) -0.0016(18) C33 0.057(2) 0.061(2) 0.049(2) -0.0020(19) -0.0251(19) -0.006(2) C34 0.055(2) 0.048(2) 0.039(2) -0.0036(17) -0.0181(17) -0.0026(18) C35 0.074(3) 0.094(3) 0.058(3) -0.001(3) -0.038(2) -0.004(3) C36 0.099(4) 0.192(6) 0.107(5) 0.001(5) -0.065(4) -0.018(5) C37 0.163(6) 0.148(6) 0.135(6) 0.031(5) -0.098(5) -0.001(5) C38 0.141(5) 0.190(7) 0.100(5) -0.034(5) -0.075(4) 0.014(5) C39 0.0367(18) 0.0363(18) 0.0387(18) -0.0086(15) -0.0095(15) 0.0031(15) C40 0.0405(19) 0.0407(19) 0.0402(19) -0.0076(16) -0.0126(15) -0.0008(16) C41 0.0427(19) 0.0395(19) 0.0384(19) -0.0048(16) -0.0112(16) 0.0008(16) C42 0.0416(18) 0.0368(19) 0.0410(19) -0.0084(16) -0.0077(16) -0.0017(16) C43 0.0417(19) 0.044(2) 0.045(2) -0.0150(17) -0.0134(16) 0.0017(17) C44 0.0400(18) 0.0401(19) 0.0397(19) -0.0084(16) -0.0124(15) 0.0047(16) C45 0.036(2) 0.046(2) 0.062(3) -0.0152(19) -0.0121(18) 0.0015(17) C46 0.054(3) 0.055(3) 0.088(3) -0.017(3) -0.030(2) 0.004(2) C47 0.043(3) 0.064(3) 0.128(5) -0.036(3) -0.027(3) 0.006(2) C48 0.043(3) 0.117(4) 0.073(3) -0.018(3) 0.005(2) -0.005(3) C49 0.046(2) 0.0302(19) 0.050(2) -0.0090(16) -0.0205(17) 0.0019(16) C50 0.051(2) 0.045(2) 0.052(2) -0.0173(18) -0.0246(18) 0.0027(18) C51 0.119(7) 0.164(9) 0.133(8) -0.019(7) -0.029(6) -0.017(7) C52 0.161(5) 0.127(5) 0.105(4) -0.020(4) -0.001(4) -0.008(5) C26' 0.126(7) 0.100(6) 0.061(6) -0.008(6) 0.000(6) 0.021(6) C27' 0.117(7) 0.070(6) 0.044(5) -0.008(5) -0.003(6) 0.004(6) C28' 0.125(7) 0.095(6) 0.064(6) -0.019(5) -0.026(6) -0.007(6) Cl1 0.271(5) 0.207(4) 0.201(4) -0.062(3) -0.002(3) -0.065(3) Cl2 0.372(8) 0.259(5) 0.215(5) -0.046(4) -0.008(5) 0.084(5) Cl3 0.144(3) 0.192(3) 0.281(5) 0.006(3) -0.042(3) -0.005(2) Cl4 0.451(10) 0.284(6) 0.301(7) -0.016(5) -0.082(6) -0.200(7) O1 0.0486(17) 0.0448(17) 0.0571(19) -0.0083(14) -0.0093(14) -0.0015(14) O2 0.0491(16) 0.0384(15) 0.0486(17) -0.0006(13) -0.0231(14) 0.0036(12) O3 0.078(2) 0.0400(16) 0.0359(16) -0.0055(13) -0.0158(15) 0.0043(15) O4 0.0421(14) 0.0304(14) 0.0382(15) -0.0038(11) -0.0150(12) 0.0006(11) O5 0.0319(14) 0.0389(16) 0.069(2) 0.0063(14) -0.0163(14) 0.0000(12) O6 0.0626(19) 0.0521(19) 0.0461(18) -0.0109(14) -0.0197(15) 0.0128(15) S1 0.0467(6) 0.0384(6) 0.0472(6) -0.0004(5) -0.0074(5) 0.0093(5) S2 0.0425(6) 0.0351(6) 0.0433(6) -0.0079(4) -0.0058(4) -0.0036(4) S3 0.0410(6) 0.0335(6) 0.0461(6) -0.0086(4) -0.0072(4) -0.0002(4) S4 0.0431(6) 0.0371(6) 0.0383(6) 0.0016(4) -0.0086(4) 0.0028(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.376(5) . ? C1 C6 1.378(7) . ? C1 C2 1.387(6) . ? C2 O6 1.353(5) . ? C2 C3 1.378(7) . ? C3 C4 1.402(7) . ? C3 H3 0.9300 . ? C4 C5 1.356(8) . ? C4 H4 0.9300 . ? C5 C6 1.355(8) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 O1 1.431(5) . ? C7 C8 1.472(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O2 1.445(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O2 1.372(5) . ? C9 C14 1.394(6) . ? C9 C10 1.396(5) . ? C10 C11 1.376(6) . ? C10 S4 1.786(4) . ? C11 C12 1.387(6) . ? C11 H11 0.9300 . ? C12 C13 1.399(6) . ? C12 C15 1.512(7) . ? C13 C14 1.379(6) . ? C13 H13 0.9300 . ? C14 S1 1.788(4) . ? C15 C17' 1.425(19) . ? C15 C16 1.491(12) . ? C15 C17 1.555(13) . ? C15 C18' 1.567(17) . ? C15 C16' 1.569(18) . ? C15 C18 1.588(13) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C16' H16D 0.9600 . ? C16' H16E 0.9600 . ? C16' H16F 0.9600 . ? C17' H17D 0.9600 . ? C17' H17E 0.9600 . ? C17' H17F 0.9600 . ? C18' H18D 0.9600 . ? C18' H18E 0.9600 . ? C18' H18F 0.9600 . ? C19 C24 1.383(6) . ? C19 C20 1.399(6) . ? C19 S1 1.781(4) . ? C20 O3 1.346(5) . ? C20 C21 1.407(6) . ? C21 C22 1.372(6) . ? C21 S2 1.776(4) . ? C22 C23 1.396(6) . ? C22 H22 0.9300 . ? C23 C24 1.394(6) . ? C23 C25 1.520(7) . ? C24 H24 0.9300 . ? C25 C28 1.424(12) . ? C25 C27' 1.432(15) . ? C25 C26' 1.441(18) . ? C25 C27 1.537(14) . ? C25 C26 1.556(14) . ? C25 C28' 1.615(18) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C34 1.383(6) . ? C29 C30 1.392(5) . ? C29 S2 1.789(4) . ? C30 O4 1.390(5) . ? C30 C31 1.392(5) . ? C31 C32 1.373(6) . ? C31 S3 1.791(4) . ? C32 C33 1.401(6) . ? C32 H32 0.9300 . ? C33 C34 1.368(6) . ? C33 C35 1.550(7) . ? C34 H34 0.9300 . ? C35 C37 1.447(10) . ? C35 C36 1.484(9) . ? C35 C38 1.537(10) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C40 1.390(6) . ? C39 C44 1.394(5) . ? C39 S3 1.780(4) . ? C40 O5 1.348(4) . ? C40 C41 1.401(5) . ? C41 C42 1.377(6) . ? C41 S4 1.788(4) . ? C42 C43 1.396(6) . ? C42 H42 0.9300 . ? C43 C44 1.378(6) . ? C43 C45 1.529(6) . ? C44 H44 0.9300 . ? C45 C47 1.513(7) . ? C45 C46 1.523(7) . ? C45 C48 1.541(7) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 O4 1.451(4) . ? C49 C50 1.483(6) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 O6 1.428(5) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 Cl1 1.629(10) . ? C51 Cl2 1.677(11) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 Cl4 1.570(7) . ? C52 Cl3 1.606(8) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C26' H26D 0.9600 . ? C26' H26E 0.9600 . ? C26' H26F 0.9600 . ? C27' H27D 0.9600 . ? C27' H27E 0.9600 . ? C27' H27F 0.9600 . ? C28' H28D 0.9600 . ? C28' H28E 0.9600 . ? C28' H28F 0.9600 . ? O3 H3A 0.8200 . ? O5 H5A 0.8200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C6 122.9(4) . . ? O1 C1 C2 116.5(4) . . ? C6 C1 C2 120.6(5) . . ? O6 C2 C3 125.6(4) . . ? O6 C2 C1 116.0(4) . . ? C3 C2 C1 118.4(4) . . ? C2 C3 C4 120.4(5) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 119.2(5) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C6 C5 C4 121.3(5) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C5 C6 C1 120.0(5) . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? O1 C7 C8 110.5(4) . . ? O1 C7 H7A 109.6 . . ? C8 C7 H7A 109.6 . . ? O1 C7 H7B 109.6 . . ? C8 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? O2 C8 C7 110.6(4) . . ? O2 C8 H8A 109.5 . . ? C7 C8 H8A 109.5 . . ? O2 C8 H8B 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? O2 C9 C14 119.6(3) . . ? O2 C9 C10 122.9(4) . . ? C14 C9 C10 117.6(4) . . ? C11 C10 C9 120.6(4) . . ? C11 C10 S4 118.5(3) . . ? C9 C10 S4 120.9(3) . . ? C10 C11 C12 122.9(4) . . ? C10 C11 H11 118.6 . . ? C12 C11 H11 118.6 . . ? C11 C12 C13 115.7(4) . . ? C11 C12 C15 122.3(4) . . ? C13 C12 C15 121.9(4) . . ? C14 C13 C12 122.4(4) . . ? C14 C13 H13 118.8 . . ? C12 C13 H13 118.8 . . ? C13 C14 C9 120.6(4) . . ? C13 C14 S1 118.9(3) . . ? C9 C14 S1 120.4(3) . . ? C17' C15 C16 72.5(10) . . ? C17' C15 C12 111.1(8) . . ? C16 C15 C12 114.1(6) . . ? C17' C15 C17 34.1(8) . . ? C16 C15 C17 104.4(8) . . ? C12 C15 C17 108.3(6) . . ? C17' C15 C18' 104.1(11) . . ? C16 C15 C18' 130.4(8) . . ? C12 C15 C18' 112.9(7) . . ? C17 C15 C18' 74.5(9) . . ? C17' C15 C16' 111.4(12) . . ? C16 C15 C16' 39.7(7) . . ? C12 C15 C16' 105.7(7) . . ? C17 C15 C16' 139.2(9) . . ? C18' C15 C16' 111.7(10) . . ? C17' C15 C18 133.3(10) . . ? C16 C15 C18 112.1(8) . . ? C12 C15 C18 108.5(6) . . ? C17 C15 C18 109.3(8) . . ? C18' C15 C18 35.8(7) . . ? C16' C15 C18 79.8(9) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? C15 C16' H16D 109.5 . . ? C15 C16' H16E 109.5 . . ? H16D C16' H16E 109.5 . . ? C15 C16' H16F 109.5 . . ? H16D C16' H16F 109.5 . . ? H16E C16' H16F 109.5 . . ? C15 C17' H17D 109.5 . . ? C15 C17' H17E 109.5 . . ? H17D C17' H17E 109.5 . . ? C15 C17' H17F 109.5 . . ? H17D C17' H17F 109.5 . . ? H17E C17' H17F 109.5 . . ? C15 C18' H18D 109.5 . . ? C15 C18' H18E 109.5 . . ? H18D C18' H18E 109.5 . . ? C15 C18' H18F 109.5 . . ? H18D C18' H18F 109.5 . . ? H18E C18' H18F 109.5 . . ? C24 C19 C20 119.8(4) . . ? C24 C19 S1 120.7(3) . . ? C20 C19 S1 119.5(3) . . ? O3 C20 C19 119.2(4) . . ? O3 C20 C21 122.8(4) . . ? C19 C20 C21 118.0(4) . . ? C22 C21 C20 120.3(4) . . ? C22 C21 S2 121.0(3) . . ? C20 C21 S2 118.6(3) . . ? C21 C22 C23 123.0(4) . . ? C21 C22 H22 118.5 . . ? C23 C22 H22 118.5 . . ? C24 C23 C22 115.6(4) . . ? C24 C23 C25 122.1(4) . . ? C22 C23 C25 122.3(4) . . ? C19 C24 C23 123.2(4) . . ? C19 C24 H24 118.4 . . ? C23 C24 H24 118.4 . . ? C28 C25 C27' 124.1(9) . . ? C28 C25 C26' 52.1(9) . . ? C27' C25 C26' 113.5(10) . . ? C28 C25 C23 116.6(6) . . ? C27' C25 C23 117.8(7) . . ? C26' C25 C23 112.8(9) . . ? C28 C25 C27 114.8(8) . . ? C27' C25 C27 58.5(9) . . ? C26' C25 C27 67.7(10) . . ? C23 C25 C27 107.2(6) . . ? C28 C25 C26 108.7(9) . . ? C27' C25 C26 40.6(8) . . ? C26' C25 C26 138.3(9) . . ? C23 C25 C26 108.9(6) . . ? C27 C25 C26 99.1(8) . . ? C28 C25 C28' 47.5(8) . . ? C27' C25 C28' 106.4(12) . . ? C26' C25 C28' 99.6(12) . . ? C23 C25 C28' 104.2(7) . . ? C27 C25 C28' 148.6(8) . . ? C26 C25 C28' 70.7(9) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? C34 C29 C30 119.6(4) . . ? C34 C29 S2 120.4(3) . . ? C30 C29 S2 120.0(3) . . ? O4 C30 C31 120.1(3) . . ? O4 C30 C29 120.2(3) . . ? C31 C30 C29 119.5(4) . . ? C32 C31 C30 119.3(4) . . ? C32 C31 S3 120.5(3) . . ? C30 C31 S3 120.2(3) . . ? C31 C32 C33 122.1(4) . . ? C31 C32 H32 119.0 . . ? C33 C32 H32 119.0 . . ? C34 C33 C32 117.4(4) . . ? C34 C33 C35 121.9(4) . . ? C32 C33 C35 120.6(4) . . ? C33 C34 C29 122.1(4) . . ? C33 C34 H34 118.9 . . ? C29 C34 H34 118.9 . . ? C37 C35 C36 118.3(7) . . ? C37 C35 C38 104.1(7) . . ? C36 C35 C38 103.7(6) . . ? C37 C35 C33 108.0(5) . . ? C36 C35 C33 112.2(5) . . ? C38 C35 C33 109.8(5) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 C44 120.1(4) . . ? C40 C39 S3 120.3(3) . . ? C44 C39 S3 119.4(3) . . ? O5 C40 C39 123.2(3) . . ? O5 C40 C41 118.2(4) . . ? C39 C40 C41 118.6(4) . . ? C42 C41 C40 119.8(4) . . ? C42 C41 S4 120.7(3) . . ? C40 C41 S4 119.5(3) . . ? C41 C42 C43 122.6(4) . . ? C41 C42 H42 118.7 . . ? C43 C42 H42 118.7 . . ? C44 C43 C42 116.8(4) . . ? C44 C43 C45 123.3(4) . . ? C42 C43 C45 119.9(4) . . ? C43 C44 C39 122.1(4) . . ? C43 C44 H44 118.9 . . ? C39 C44 H44 118.9 . . ? C47 C45 C46 108.0(4) . . ? C47 C45 C43 112.0(4) . . ? C46 C45 C43 108.5(4) . . ? C47 C45 C48 110.0(4) . . ? C46 C45 C48 109.4(4) . . ? C43 C45 C48 108.9(4) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O4 C49 C50 108.3(3) . . ? O4 C49 H49A 110.0 . . ? C50 C49 H49A 110.0 . . ? O4 C49 H49B 110.0 . . ? C50 C49 H49B 110.0 . . ? H49A C49 H49B 108.4 . . ? O6 C50 C49 108.3(3) . . ? O6 C50 H50A 110.0 . . ? C49 C50 H50A 110.0 . . ? O6 C50 H50B 110.0 . . ? C49 C50 H50B 110.0 . . ? H50A C50 H50B 108.4 . . ? Cl1 C51 Cl2 115.0(6) . . ? Cl1 C51 H51A 108.5 . . ? Cl2 C51 H51A 108.5 . . ? Cl1 C51 H51B 108.5 . . ? Cl2 C51 H51B 108.5 . . ? H51A C51 H51B 107.5 . . ? Cl4 C52 Cl3 123.1(6) . . ? Cl4 C52 H52A 106.6 . . ? Cl3 C52 H52A 106.6 . . ? Cl4 C52 H52B 106.6 . . ? Cl3 C52 H52B 106.6 . . ? H52A C52 H52B 106.5 . . ? C25 C26' H26D 109.5 . . ? C25 C26' H26E 109.5 . . ? H26D C26' H26E 109.5 . . ? C25 C26' H26F 109.5 . . ? H26D C26' H26F 109.5 . . ? H26E C26' H26F 109.5 . . ? C25 C27' H27D 109.5 . . ? C25 C27' H27E 109.5 . . ? H27D C27' H27E 109.5 . . ? C25 C27' H27F 109.5 . . ? H27D C27' H27F 109.5 . . ? H27E C27' H27F 109.5 . . ? C25 C28' H28D 109.5 . . ? C25 C28' H28E 109.5 . . ? H28D C28' H28E 109.5 . . ? C25 C28' H28F 109.5 . . ? H28D C28' H28F 109.5 . . ? H28E C28' H28F 109.5 . . ? C1 O1 C7 117.3(3) . . ? C9 O2 C8 115.9(3) . . ? C20 O3 H3A 109.5 . . ? C30 O4 C49 117.2(3) . . ? C40 O5 H5A 109.5 . . ? C2 O6 C50 118.2(3) . . ? C19 S1 C14 97.64(19) . . ? C21 S2 C29 101.70(18) . . ? C39 S3 C31 102.74(17) . . ? C10 S4 C41 97.92(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 O6 1.6(5) . . . . ? C6 C1 C2 O6 -179.7(4) . . . . ? O1 C1 C2 C3 -178.6(4) . . . . ? C6 C1 C2 C3 0.0(6) . . . . ? O6 C2 C3 C4 -179.6(4) . . . . ? C1 C2 C3 C4 0.6(7) . . . . ? C2 C3 C4 C5 -0.5(8) . . . . ? C3 C4 C5 C6 -0.2(8) . . . . ? C4 C5 C6 C1 0.9(8) . . . . ? O1 C1 C6 C5 177.8(4) . . . . ? C2 C1 C6 C5 -0.8(7) . . . . ? O1 C7 C8 O2 165.8(4) . . . . ? O2 C9 C10 C11 -175.1(3) . . . . ? C14 C9 C10 C11 3.2(6) . . . . ? O2 C9 C10 S4 5.8(5) . . . . ? C14 C9 C10 S4 -175.9(3) . . . . ? C9 C10 C11 C12 -3.1(6) . . . . ? S4 C10 C11 C12 175.9(3) . . . . ? C10 C11 C12 C13 2.7(6) . . . . ? C10 C11 C12 C15 -179.7(4) . . . . ? C11 C12 C13 C14 -2.5(6) . . . . ? C15 C12 C13 C14 179.9(4) . . . . ? C12 C13 C14 C9 2.9(6) . . . . ? C12 C13 C14 S1 -174.0(3) . . . . ? O2 C9 C14 C13 175.3(3) . . . . ? C10 C9 C14 C13 -3.0(6) . . . . ? O2 C9 C14 S1 -7.8(5) . . . . ? C10 C9 C14 S1 173.8(3) . . . . ? C11 C12 C15 C17' -107.4(10) . . . . ? C13 C12 C15 C17' 70.1(11) . . . . ? C11 C12 C15 C16 173.0(7) . . . . ? C13 C12 C15 C16 -9.6(9) . . . . ? C11 C12 C15 C17 -71.2(8) . . . . ? C13 C12 C15 C17 106.2(8) . . . . ? C11 C12 C15 C18' 9.2(10) . . . . ? C13 C12 C15 C18' -173.4(9) . . . . ? C11 C12 C15 C16' 131.6(9) . . . . ? C13 C12 C15 C16' -51.0(10) . . . . ? C11 C12 C15 C18 47.3(8) . . . . ? C13 C12 C15 C18 -135.3(7) . . . . ? C24 C19 C20 O3 179.2(4) . . . . ? S1 C19 C20 O3 1.1(5) . . . . ? C24 C19 C20 C21 0.9(6) . . . . ? S1 C19 C20 C21 -177.3(3) . . . . ? O3 C20 C21 C22 -179.0(4) . . . . ? C19 C20 C21 C22 -0.7(6) . . . . ? O3 C20 C21 S2 4.2(5) . . . . ? C19 C20 C21 S2 -177.5(3) . . . . ? C20 C21 C22 C23 -0.3(7) . . . . ? S2 C21 C22 C23 176.3(4) . . . . ? C21 C22 C23 C24 1.2(7) . . . . ? C21 C22 C23 C25 179.0(5) . . . . ? C20 C19 C24 C23 0.1(7) . . . . ? S1 C19 C24 C23 178.2(4) . . . . ? C22 C23 C24 C19 -1.1(7) . . . . ? C25 C23 C24 C19 -178.9(5) . . . . ? C24 C23 C25 C28 11.0(11) . . . . ? C22 C23 C25 C28 -166.7(9) . . . . ? C24 C23 C25 C27' 177.9(11) . . . . ? C22 C23 C25 C27' 0.2(13) . . . . ? C24 C23 C25 C26' -46.8(12) . . . . ? C22 C23 C25 C26' 135.6(11) . . . . ? C24 C23 C25 C27 -119.3(8) . . . . ? C22 C23 C25 C27 63.1(9) . . . . ? C24 C23 C25 C26 134.4(8) . . . . ? C22 C23 C25 C26 -43.2(9) . . . . ? C24 C23 C25 C28' 60.3(10) . . . . ? C22 C23 C25 C28' -117.4(9) . . . . ? C34 C29 C30 O4 173.0(3) . . . . ? S2 C29 C30 O4 -9.9(5) . . . . ? C34 C29 C30 C31 -1.8(6) . . . . ? S2 C29 C30 C31 175.3(3) . . . . ? O4 C30 C31 C32 -173.3(3) . . . . ? C29 C30 C31 C32 1.5(6) . . . . ? O4 C30 C31 S3 9.1(5) . . . . ? C29 C30 C31 S3 -176.1(3) . . . . ? C30 C31 C32 C33 0.5(6) . . . . ? S3 C31 C32 C33 178.1(3) . . . . ? C31 C32 C33 C34 -2.1(7) . . . . ? C31 C32 C33 C35 -178.4(4) . . . . ? C32 C33 C34 C29 1.8(7) . . . . ? C35 C33 C34 C29 178.0(4) . . . . ? C30 C29 C34 C33 0.2(6) . . . . ? S2 C29 C34 C33 -176.9(3) . . . . ? C34 C33 C35 C37 -78.2(7) . . . . ? C32 C33 C35 C37 97.9(7) . . . . ? C34 C33 C35 C36 149.5(6) . . . . ? C32 C33 C35 C36 -34.3(8) . . . . ? C34 C33 C35 C38 34.8(8) . . . . ? C32 C33 C35 C38 -149.1(6) . . . . ? C44 C39 C40 O5 -178.1(4) . . . . ? S3 C39 C40 O5 -3.1(5) . . . . ? C44 C39 C40 C41 0.9(6) . . . . ? S3 C39 C40 C41 175.9(3) . . . . ? O5 C40 C41 C42 178.3(4) . . . . ? C39 C40 C41 C42 -0.8(6) . . . . ? O5 C40 C41 S4 -4.6(5) . . . . ? C39 C40 C41 S4 176.3(3) . . . . ? C40 C41 C42 C43 0.5(6) . . . . ? S4 C41 C42 C43 -176.6(3) . . . . ? C41 C42 C43 C44 -0.3(6) . . . . ? C41 C42 C43 C45 178.8(4) . . . . ? C42 C43 C44 C39 0.4(6) . . . . ? C45 C43 C44 C39 -178.7(4) . . . . ? C40 C39 C44 C43 -0.7(6) . . . . ? S3 C39 C44 C43 -175.7(3) . . . . ? C44 C43 C45 C47 -3.9(6) . . . . ? C42 C43 C45 C47 177.2(4) . . . . ? C44 C43 C45 C46 115.2(5) . . . . ? C42 C43 C45 C46 -63.8(5) . . . . ? C44 C43 C45 C48 -125.8(5) . . . . ? C42 C43 C45 C48 55.2(5) . . . . ? O4 C49 C50 O6 62.7(4) . . . . ? C6 C1 O1 C7 49.2(5) . . . . ? C2 C1 O1 C7 -132.2(4) . . . . ? C8 C7 O1 C1 59.2(5) . . . . ? C14 C9 O2 C8 105.8(4) . . . . ? C10 C9 O2 C8 -75.9(5) . . . . ? C7 C8 O2 C9 -128.6(4) . . . . ? C31 C30 O4 C49 -89.6(4) . . . . ? C29 C30 O4 C49 95.6(4) . . . . ? C50 C49 O4 C30 148.6(3) . . . . ? C3 C2 O6 C50 -17.2(6) . . . . ? C1 C2 O6 C50 162.6(4) . . . . ? C49 C50 O6 C2 -167.9(3) . . . . ? C24 C19 S1 C14 -109.6(4) . . . . ? C20 C19 S1 C14 68.5(4) . . . . ? C13 C14 S1 C19 51.1(4) . . . . ? C9 C14 S1 C19 -125.8(3) . . . . ? C22 C21 S2 C29 101.6(4) . . . . ? C20 C21 S2 C29 -81.6(3) . . . . ? C34 C29 S2 C21 -73.4(4) . . . . ? C30 C29 S2 C21 109.6(3) . . . . ? C40 C39 S3 C31 76.2(4) . . . . ? C44 C39 S3 C31 -108.8(3) . . . . ? C32 C31 S3 C39 80.3(4) . . . . ? C30 C31 S3 C39 -102.2(3) . . . . ? C11 C10 S4 C41 -46.8(4) . . . . ? C9 C10 S4 C41 132.2(3) . . . . ? C42 C41 S4 C10 108.4(3) . . . . ? C40 C41 S4 C10 -68.7(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C51 H51B O1 0.97 2.40 3.232(10) 143.8 1_455 O3 H3A S2 0.82 2.50 3.018(3) 122.6 . O3 H3A O4 0.82 2.31 3.026(4) 146.8 . O5 H5A S3 0.82 2.54 3.053(3) 121.8 . O5 H5A O4 0.82 2.08 2.802(4) 147.3 . C8 H8B O5 0.97 2.37 3.167(5) 139.2 . _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.942 _refine_diff_density_min -1.067 _refine_diff_density_rms 0.085 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.500 0.500 0.000 578.4 119.0 2 0.414 0.875 0.302 11.0 -0.1 3 0.586 0.125 0.699 11.0 -0.2 _platon_squeeze_details ; During the refinement,the non-coordinated solvent molecules are severely disordered and could not be modeled by discrete atoms in the complexes. Correspondingly, the contribution of the solvent to the diffraction pattern was subtracted using SQUEEZE procedure of PLATON (Spek, 2003), resultig in very large accessible void in the structure. The result indicated that the solvent-accessible void in the unit cell has one volume of ca. 578.4\%A^3^, and this residual electron-density count amounted to 119.0 electrons, corresponding to nearly two molecules of methanol and two molecules of dichloromethane. ; # start Validation Reply Form _vrf_PLAT606_CCDC-740901 ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: The non-coordinated solvent molecules are severely disordered which could not be modeled by discrete atoms in the complexes. Correspondingly, the contribution of the solvent to the diffraction pattern was subtracted using SQUEEZE procedure of the PLATON, resultig in very large accessible void in the structure. ; # end Validation Reply Form #===END data_publication_text _publ_contact_author 'Xiong Li' _publ_contact_author_email 'lxwhu2008@hotmail.com' loop_ _publ_author_name 'Xiong Li' 'Shu-Ling Gong' 'Wei-Ping Yang' 'Yuan-Yin Chen' 'Xiang-Gao Meng' _journal_name_full 'Dalton Transactions' data_CCDC-740900 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,3-alternate-5,11,17,23-Tetra-tert-butyl-25,27-[1,3- bis(oxyethoxy)benzene]-2,8,14,20-tetra-thiacalix[4]arene ; _chemical_name_common ; 1,3-alternate-thiacalix[4]-m-benzocrown-4 ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H58 O6 S4' _chemical_formula_weight 883.20 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.1148(7) _cell_length_b 22.5558(9) _cell_length_c 25.0673(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9676.9(7) _cell_formula_units_Z 8 _cell_measurement_temperature 292(2) _cell_measurement_reflns_used 7939 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 22.66 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.212 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3760 _exptl_absorpt_coefficient_mu 0.243 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 292(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 77082 _diffrn_reflns_av_R_equivalents 0.0849 _diffrn_reflns_av_sigmaI/netI 0.0455 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8525 _reflns_number_gt 6445 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. During the refinement, some tert-butyl groups were found to be seriously disordered. Commands ¡®DFIX¡¯, ¡®SADI¡¯and ¡®ISOR¡¯ were used to refine them to arrive at more appropriate values. ; _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^)+(0.0568P)^2^+7.1222P] 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 8525 _refine_ls_number_parameters 673 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.1027 _refine_ls_R_factor_gt 0.0762 _refine_ls_wR_factor_ref 0.1598 _refine_ls_wR_factor_gt 0.1493 _refine_ls_goodness_of_fit_ref 1.173 _refine_ls_restrained_S_all 1.214 _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 C1 C 0.78253(19) 0.24018(15) 0.61441(15) 0.0360(8) Uani 1 1 d . . . C2 C 0.78976(19) 0.23489(16) 0.55925(15) 0.0389(9) Uani 1 1 d . . . C3 C 0.8347(2) 0.18952(17) 0.53873(15) 0.0427(9) Uani 1 1 d . . . H3 H 0.8400 0.1865 0.5019 0.051 Uiso 1 1 calc R . . C4 C 0.8724(2) 0.14814(17) 0.57074(16) 0.0453(10) Uani 1 1 d . A . C5 C 0.8630(2) 0.15440(17) 0.62565(16) 0.0450(10) Uani 1 1 d . . . H5 H 0.8874 0.1274 0.6482 0.054 Uiso 1 1 calc R . . C6 C 0.81859(19) 0.19937(16) 0.64775(14) 0.0381(9) Uani 1 1 d . . . C7 C 0.9264(2) 0.10084(18) 0.54711(18) 0.0594(12) Uani 1 1 d D . . C8 C 0.8826(7) 0.0685(6) 0.5010(5) 0.090(5) Uani 0.508(14) 1 d PD A 1 H8A H 0.8359 0.0505 0.5147 0.135 Uiso 0.508(14) 1 calc PR A 1 H8B H 0.9158 0.0384 0.4862 0.135 Uiso 0.508(14) 1 calc PR A 1 H8C H 0.8692 0.0966 0.4738 0.135 Uiso 0.508(14) 1 calc PR A 1 C9 C 1.0005(6) 0.1264(5) 0.5256(7) 0.091(5) Uani 0.508(14) 1 d PD A 1 H9A H 0.9884 0.1569 0.5002 0.136 Uiso 0.508(14) 1 calc PR A 1 H9B H 1.0303 0.0958 0.5085 0.136 Uiso 0.508(14) 1 calc PR A 1 H9C H 1.0304 0.1431 0.5544 0.136 Uiso 0.508(14) 1 calc PR A 1 C10 C 0.9445(8) 0.0522(4) 0.5885(5) 0.082(4) Uani 0.508(14) 1 d PD A 1 H10A H 0.9799 0.0676 0.6149 0.122 Uiso 0.508(14) 1 calc PR A 1 H10B H 0.9681 0.0189 0.5710 0.122 Uiso 0.508(14) 1 calc PR A 1 H10C H 0.8970 0.0399 0.6055 0.122 Uiso 0.508(14) 1 calc PR A 1 C8' C 0.9089(9) 0.0392(4) 0.5654(5) 0.096(5) Uani 0.492(14) 1 d PRD A 2 H8D H 0.9001 0.0392 0.6033 0.145 Uiso 0.492(14) 1 d PR A 2 H8E H 0.9523 0.0138 0.5572 0.145 Uiso 0.492(14) 1 d PR A 2 H8F H 0.8630 0.0249 0.5475 0.145 Uiso 0.492(14) 1 d PR A 2 C9' C 0.9293(10) 0.1042(7) 0.4861(3) 0.095(5) Uani 0.492(14) 1 d PD A 2 H9D H 0.8784 0.0959 0.4718 0.143 Uiso 0.492(14) 1 calc PR A 2 H9E H 0.9660 0.0757 0.4729 0.143 Uiso 0.492(14) 1 calc PR A 2 H9F H 0.9452 0.1433 0.4754 0.143 Uiso 0.492(14) 1 calc PR A 2 C10' C 1.0099(5) 0.1182(6) 0.5665(6) 0.079(4) Uani 0.492(14) 1 d PD A 2 H10D H 1.0209 0.1584 0.5563 0.118 Uiso 0.492(14) 1 calc PR A 2 H10E H 1.0477 0.0922 0.5506 0.118 Uiso 0.492(14) 1 calc PR A 2 H10F H 1.0126 0.1148 0.6046 0.118 Uiso 0.492(14) 1 calc PR A 2 C11 C 0.74684(19) 0.15976(16) 0.74422(14) 0.0384(8) Uani 1 1 d . . . C12 C 0.66795(19) 0.16539(15) 0.73131(13) 0.0347(8) Uani 1 1 d . . . C13 C 0.61476(19) 0.12658(16) 0.75644(14) 0.0372(8) Uani 1 1 d . . . C14 C 0.6406(2) 0.08766(16) 0.79546(14) 0.0381(8) Uani 1 1 d . . . H14 H 0.6047 0.0626 0.8118 0.046 Uiso 1 1 calc R . . C15 C 0.7188(2) 0.08501(17) 0.81102(14) 0.0416(9) Uani 1 1 d . B . C16 C 0.7710(2) 0.12059(17) 0.78352(15) 0.0433(9) Uani 1 1 d . . . H16 H 0.8239 0.1181 0.7917 0.052 Uiso 1 1 calc R . . C17 C 0.7450(2) 0.04793(19) 0.85883(17) 0.0568(11) Uani 1 1 d D . . C18 C 0.8257(6) 0.0215(8) 0.8496(8) 0.071(4) Uani 0.62(3) 1 d PD B 1 H18A H 0.8230 -0.0071 0.8213 0.107 Uiso 0.62(3) 1 calc PR B 1 H18B H 0.8433 0.0025 0.8817 0.107 Uiso 0.62(3) 1 calc PR B 1 H18C H 0.8615 0.0524 0.8400 0.107 Uiso 0.62(3) 1 calc PR B 1 C19 C 0.7543(12) 0.0940(5) 0.9053(4) 0.088(5) Uani 0.62(3) 1 d PD B 1 H19A H 0.7925 0.1232 0.8956 0.131 Uiso 0.62(3) 1 calc PR B 1 H19B H 0.7710 0.0738 0.9371 0.131 Uiso 0.62(3) 1 calc PR B 1 H19C H 0.7051 0.1131 0.9118 0.131 Uiso 0.62(3) 1 calc PR B 1 C20 C 0.6874(7) 0.0016(7) 0.8761(6) 0.084(5) Uani 0.62(3) 1 d PD B 1 H20A H 0.6389 0.0203 0.8855 0.127 Uiso 0.62(3) 1 calc PR B 1 H20B H 0.7077 -0.0193 0.9065 0.127 Uiso 0.62(3) 1 calc PR B 1 H20C H 0.6788 -0.0258 0.8474 0.127 Uiso 0.62(3) 1 calc PR B 1 C18' C 0.7144(17) -0.0161(5) 0.8465(13) 0.102(8) Uani 0.38(3) 1 d PD B 2 H18D H 0.6592 -0.0147 0.8398 0.152 Uiso 0.38(3) 1 calc PR B 2 H18E H 0.7245 -0.0414 0.8765 0.152 Uiso 0.38(3) 1 calc PR B 2 H18F H 0.7407 -0.0314 0.8156 0.152 Uiso 0.38(3) 1 calc PR B 2 C19' C 0.7069(16) 0.0678(13) 0.9104(5) 0.098(8) Uani 0.38(3) 1 d PD B 2 H19D H 0.7236 0.1073 0.9188 0.147 Uiso 0.38(3) 1 calc PR B 2 H19E H 0.7217 0.0414 0.9387 0.147 Uiso 0.38(3) 1 calc PR B 2 H19F H 0.6511 0.0671 0.9063 0.147 Uiso 0.38(3) 1 calc PR B 2 C20' C 0.8330(5) 0.0423(12) 0.8661(13) 0.067(6) Uani 0.38(3) 1 d PD B 2 H20D H 0.8567 0.0316 0.8328 0.100 Uiso 0.38(3) 1 calc PR B 2 H20E H 0.8440 0.0123 0.8922 0.100 Uiso 0.38(3) 1 calc PR B 2 H20F H 0.8539 0.0796 0.8780 0.100 Uiso 0.38(3) 1 calc PR B 2 C21 C 0.51662(19) 0.11975(15) 0.67178(14) 0.0359(8) Uani 1 1 d . . . C22 C 0.47538(18) 0.15714(15) 0.63783(15) 0.0356(8) Uani 1 1 d . . . C23 C 0.48740(19) 0.15190(16) 0.58334(15) 0.0375(9) Uani 1 1 d . . . C24 C 0.5350(2) 0.10773(16) 0.56298(15) 0.0401(9) Uani 1 1 d . . . H24 H 0.5405 0.1041 0.5262 0.048 Uiso 1 1 calc R . . C25 C 0.5745(2) 0.06884(16) 0.59619(16) 0.0425(9) Uani 1 1 d . C . C26 C 0.5641(2) 0.07592(15) 0.65066(15) 0.0400(9) Uani 1 1 d . . . H26 H 0.5900 0.0504 0.6738 0.048 Uiso 1 1 calc R . . C27 C 0.6278(3) 0.02005(18) 0.57426(17) 0.0622(12) Uani 1 1 d D . . C28 C 0.7048(5) 0.0194(6) 0.6056(5) 0.076(3) Uani 0.71(2) 1 d PD C 1 H28A H 0.7308 0.0568 0.6014 0.114 Uiso 0.71(2) 1 calc PR C 1 H28B H 0.7377 -0.0118 0.5923 0.114 Uiso 0.71(2) 1 calc PR C 1 H28C H 0.6940 0.0127 0.6427 0.114 Uiso 0.71(2) 1 calc PR C 1 C29 C 0.5857(5) -0.0400(3) 0.5852(7) 0.090(4) Uani 0.71(2) 1 d PD C 1 H29A H 0.5791 -0.0452 0.6230 0.135 Uiso 0.71(2) 1 calc PR C 1 H29B H 0.6166 -0.0720 0.5713 0.135 Uiso 0.71(2) 1 calc PR C 1 H29C H 0.5355 -0.0399 0.5682 0.135 Uiso 0.71(2) 1 calc PR C 1 C30 C 0.6434(10) 0.0257(7) 0.5151(3) 0.107(5) Uani 0.71(2) 1 d PD C 1 H30A H 0.6712 0.0619 0.5083 0.160 Uiso 0.71(2) 1 calc PR C 1 H30B H 0.5947 0.0261 0.4962 0.160 Uiso 0.71(2) 1 calc PR C 1 H30C H 0.6744 -0.0073 0.5034 0.160 Uiso 0.71(2) 1 calc PR C 1 C28' C 0.6810(14) 0.0515(11) 0.5319(10) 0.077(7) Uani 0.29(2) 1 d PD C 2 H28D H 0.6487 0.0708 0.5058 0.115 Uiso 0.29(2) 1 calc PR C 2 H28E H 0.7134 0.0226 0.5147 0.115 Uiso 0.29(2) 1 calc PR C 2 H28F H 0.7132 0.0804 0.5493 0.115 Uiso 0.29(2) 1 calc PR C 2 C29' C 0.5815(14) -0.0277(12) 0.5439(16) 0.105(11) Uani 0.29(2) 1 d PD C 2 H29D H 0.5404 -0.0426 0.5663 0.158 Uiso 0.29(2) 1 calc PR C 2 H29E H 0.6158 -0.0596 0.5343 0.158 Uiso 0.29(2) 1 calc PR C 2 H29F H 0.5592 -0.0107 0.5122 0.158 Uiso 0.29(2) 1 calc PR C 2 C30' C 0.6828(17) -0.0100(15) 0.6142(10) 0.091(9) Uani 0.29(2) 1 d PD C 2 H30D H 0.7032 0.0192 0.6384 0.136 Uiso 0.29(2) 1 calc PR C 2 H30E H 0.7251 -0.0285 0.5954 0.136 Uiso 0.29(2) 1 calc PR C 2 H30F H 0.6545 -0.0394 0.6340 0.136 Uiso 0.29(2) 1 calc PR C 2 C31 C 0.5307(2) 0.21992(15) 0.50036(15) 0.0390(9) Uani 1 1 d . . . C32 C 0.59617(19) 0.24684(16) 0.52287(14) 0.0371(8) Uani 1 1 d . . . C33 C 0.66267(19) 0.25400(16) 0.49089(15) 0.0388(9) Uani 1 1 d . . . C34 C 0.6606(2) 0.23738(17) 0.43779(15) 0.0439(9) Uani 1 1 d . . . H34 H 0.7052 0.2427 0.4172 0.053 Uiso 1 1 calc R . . C35 C 0.5950(2) 0.21314(16) 0.41404(15) 0.0436(9) Uani 1 1 d . D . C36 C 0.5309(2) 0.20421(16) 0.44702(15) 0.0424(9) Uani 1 1 d . . . H36 H 0.4863 0.1870 0.4327 0.051 Uiso 1 1 calc R . . C37 C 0.5928(3) 0.19500(19) 0.35500(17) 0.0601(12) Uani 1 1 d D . . C38 C 0.5692(16) 0.1310(5) 0.3494(7) 0.115(7) Uani 0.54(3) 1 d PD D 1 H38A H 0.5989 0.1072 0.3738 0.173 Uiso 0.54(3) 1 calc PR D 1 H38B H 0.5791 0.1180 0.3135 0.173 Uiso 0.54(3) 1 calc PR D 1 H38C H 0.5145 0.1270 0.3572 0.173 Uiso 0.54(3) 1 calc PR D 1 C39 C 0.6715(7) 0.2049(11) 0.3274(6) 0.093(5) Uani 0.54(3) 1 d PD D 1 H39A H 0.7100 0.1791 0.3428 0.140 Uiso 0.54(3) 1 calc PR D 1 H39B H 0.6875 0.2454 0.3322 0.140 Uiso 0.54(3) 1 calc PR D 1 H39C H 0.6665 0.1966 0.2900 0.140 Uiso 0.54(3) 1 calc PR D 1 C40 C 0.5328(11) 0.2351(10) 0.3278(5) 0.100(6) Uani 0.54(3) 1 d PD D 1 H40A H 0.5296 0.2252 0.2906 0.151 Uiso 0.54(3) 1 calc PR D 1 H40B H 0.5484 0.2758 0.3316 0.151 Uiso 0.54(3) 1 calc PR D 1 H40C H 0.4826 0.2295 0.3441 0.151 Uiso 0.54(3) 1 calc PR D 1 C38' C 0.5102(6) 0.1924(14) 0.3322(7) 0.101(7) Uani 0.46(3) 1 d PD D 2 H38D H 0.5126 0.1824 0.2950 0.151 Uiso 0.46(3) 1 calc PR D 2 H38E H 0.4855 0.2303 0.3363 0.151 Uiso 0.46(3) 1 calc PR D 2 H38F H 0.4805 0.1628 0.3509 0.151 Uiso 0.46(3) 1 calc PR D 2 C39' C 0.6420(15) 0.2364(10) 0.3213(7) 0.099(7) Uani 0.46(3) 1 d PD D 2 H39D H 0.6952 0.2352 0.3334 0.148 Uiso 0.46(3) 1 calc PR D 2 H39E H 0.6223 0.2761 0.3245 0.148 Uiso 0.46(3) 1 calc PR D 2 H39F H 0.6397 0.2242 0.2846 0.148 Uiso 0.46(3) 1 calc PR D 2 C40' C 0.6277(18) 0.1325(7) 0.3523(7) 0.105(7) Uani 0.46(3) 1 d PD D 2 H40D H 0.6004 0.1070 0.3767 0.158 Uiso 0.46(3) 1 calc PR D 2 H40E H 0.6820 0.1340 0.3619 0.158 Uiso 0.46(3) 1 calc PR D 2 H40F H 0.6225 0.1173 0.3167 0.158 Uiso 0.46(3) 1 calc PR D 2 C41 C 0.7788(2) 0.33844(18) 0.64808(19) 0.0602(12) Uani 1 1 d . . . H41A H 0.7945 0.3578 0.6152 0.072 Uiso 1 1 calc R . . H41B H 0.8254 0.3292 0.6685 0.072 Uiso 1 1 calc R . . C42 C 0.7269(3) 0.3783(2) 0.6794(2) 0.0671(13) Uani 1 1 d . . . H42A H 0.7065 0.3572 0.7101 0.080 Uiso 1 1 calc R . . H42B H 0.7563 0.4122 0.6920 0.080 Uiso 1 1 calc R . . C43 C 0.5965(3) 0.41162(19) 0.67429(18) 0.0610(12) Uani 1 1 d . . . C44 C 0.5940(4) 0.4583(2) 0.7097(2) 0.0786(15) Uani 1 1 d . . . H44 H 0.6375 0.4822 0.7155 0.094 Uiso 1 1 calc R . . C45 C 0.5247(4) 0.4683(2) 0.7362(2) 0.0900(18) Uani 1 1 d . . . H45 H 0.5214 0.5000 0.7599 0.108 Uiso 1 1 calc R . . C46 C 0.4609(4) 0.4332(2) 0.7286(2) 0.0809(16) Uani 1 1 d . . . H46 H 0.4151 0.4406 0.7474 0.097 Uiso 1 1 calc R . . C47 C 0.4642(3) 0.3865(2) 0.6928(2) 0.0693(14) Uani 1 1 d . . . C48 C 0.5329(3) 0.37636(19) 0.66480(19) 0.0648(13) Uani 1 1 d . . . H48 H 0.5357 0.3459 0.6398 0.078 Uiso 1 1 calc R . . C49 C 0.4013(3) 0.3015(2) 0.6552(2) 0.0711(14) Uani 1 1 d . . . H49A H 0.4206 0.3134 0.6204 0.085 Uiso 1 1 calc R . . H49B H 0.3487 0.2865 0.6505 0.085 Uiso 1 1 calc R . . C50 C 0.4523(2) 0.25240(17) 0.67642(17) 0.0500(10) Uani 1 1 d . . . H50A H 0.5057 0.2577 0.6644 0.060 Uiso 1 1 calc R . . H50B H 0.4520 0.2527 0.7151 0.060 Uiso 1 1 calc R . . O1 O 0.73607(13) 0.28452(10) 0.63620(10) 0.0430(6) Uani 1 1 d . . . O2 O 0.42191(13) 0.19750(11) 0.65701(10) 0.0437(6) Uani 1 1 d . . . O3 O 0.63965(14) 0.20610(11) 0.69714(10) 0.0469(7) Uani 1 1 d . . . H3A H 0.6757 0.2264 0.6857 0.070 Uiso 1 1 calc R . . O4 O 0.59324(14) 0.26454(12) 0.57420(10) 0.0500(7) Uani 1 1 d . . . H4 H 0.6351 0.2796 0.5825 0.075 Uiso 1 1 calc R . . O5 O 0.6641(2) 0.39764(13) 0.64648(12) 0.0676(9) Uani 1 1 d . . . O6 O 0.3987(2) 0.35233(16) 0.68906(16) 0.0881(11) Uani 1 1 d . . . S1 S 0.74720(5) 0.28994(4) 0.51654(4) 0.0469(3) Uani 1 1 d . . . S2 S 0.81677(6) 0.21080(5) 0.71859(4) 0.0501(3) Uani 1 1 d . . . S3 S 0.51331(5) 0.13171(5) 0.74196(4) 0.0427(3) Uani 1 1 d . . . S4 S 0.44568(5) 0.20578(5) 0.53946(4) 0.0476(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0257(17) 0.039(2) 0.044(2) 0.0046(17) 0.0038(16) -0.0064(15) C2 0.0270(18) 0.046(2) 0.043(2) 0.0115(18) -0.0006(16) -0.0066(16) C3 0.0323(19) 0.057(2) 0.038(2) 0.0038(19) 0.0022(16) -0.0027(18) C4 0.037(2) 0.049(2) 0.050(3) 0.0044(19) 0.0021(18) -0.0030(17) C5 0.0317(19) 0.052(2) 0.051(3) 0.018(2) -0.0059(18) -0.0014(17) C6 0.0274(18) 0.049(2) 0.038(2) 0.0078(17) -0.0006(15) -0.0120(16) C7 0.051(3) 0.057(3) 0.070(3) 0.004(2) 0.007(2) 0.012(2) C8 0.086(9) 0.089(9) 0.095(10) -0.034(8) 0.004(7) 0.005(7) C9 0.075(8) 0.082(8) 0.116(14) -0.001(9) 0.042(9) -0.003(6) C10 0.099(12) 0.061(7) 0.085(9) -0.006(7) 0.004(7) 0.019(6) C8' 0.097(12) 0.069(8) 0.123(15) -0.002(8) 0.029(9) -0.008(7) C9' 0.103(12) 0.098(11) 0.085(9) -0.015(7) 0.018(8) 0.040(9) C10' 0.051(6) 0.092(9) 0.093(10) -0.001(8) 0.020(6) 0.023(6) C11 0.0316(18) 0.052(2) 0.032(2) 0.0022(17) -0.0005(16) -0.0088(16) C12 0.0357(19) 0.043(2) 0.0256(19) 0.0006(16) -0.0006(15) -0.0025(16) C13 0.0301(18) 0.050(2) 0.032(2) 0.0030(17) -0.0006(15) -0.0029(16) C14 0.038(2) 0.044(2) 0.033(2) 0.0059(17) 0.0022(16) -0.0063(16) C15 0.041(2) 0.049(2) 0.035(2) 0.0018(18) -0.0050(17) -0.0018(17) C16 0.0331(19) 0.059(2) 0.038(2) -0.0002(19) -0.0043(16) -0.0047(18) C17 0.051(2) 0.071(3) 0.049(3) 0.019(2) -0.008(2) 0.003(2) C18 0.071(6) 0.061(10) 0.082(12) 0.015(6) -0.016(5) 0.010(6) C19 0.117(12) 0.100(8) 0.046(6) 0.014(5) -0.017(6) 0.007(7) C20 0.078(7) 0.102(9) 0.073(9) 0.061(8) -0.016(6) -0.021(6) C18' 0.096(16) 0.104(14) 0.10(2) 0.040(12) -0.021(13) -0.007(11) C19' 0.100(16) 0.12(2) 0.071(11) 0.030(11) 0.009(10) 0.014(15) C20' 0.067(9) 0.066(16) 0.067(16) 0.014(10) -0.022(8) -0.008(8) C21 0.0284(18) 0.039(2) 0.040(2) 0.0117(16) -0.0034(16) -0.0074(15) C22 0.0203(16) 0.040(2) 0.046(2) 0.0041(17) 0.0002(16) -0.0041(15) C23 0.0274(17) 0.044(2) 0.042(2) 0.0136(17) -0.0037(16) -0.0043(15) C24 0.040(2) 0.045(2) 0.035(2) 0.0039(17) -0.0012(17) -0.0021(17) C25 0.037(2) 0.038(2) 0.053(3) 0.0043(18) -0.0007(18) -0.0053(16) C26 0.037(2) 0.038(2) 0.045(2) 0.0147(17) -0.0051(17) -0.0032(16) C27 0.070(3) 0.050(3) 0.067(3) -0.004(2) -0.001(3) 0.018(2) C28 0.055(5) 0.072(7) 0.101(7) 0.006(6) 0.011(5) 0.026(4) C29 0.096(6) 0.057(5) 0.117(10) -0.016(5) -0.008(7) 0.009(4) C30 0.139(12) 0.112(10) 0.069(6) -0.019(6) 0.016(6) 0.059(9) C28' 0.077(15) 0.075(15) 0.078(17) -0.005(11) 0.008(12) 0.019(11) C29' 0.111(18) 0.094(18) 0.11(3) -0.028(19) 0.003(18) 0.004(15) C30' 0.093(18) 0.08(2) 0.096(18) 0.001(15) 0.006(15) 0.010(15) C31 0.0335(19) 0.044(2) 0.039(2) 0.0152(17) -0.0004(16) 0.0053(16) C32 0.0317(18) 0.044(2) 0.035(2) 0.0133(17) 0.0015(16) 0.0030(16) C33 0.0331(19) 0.044(2) 0.039(2) 0.0156(17) 0.0010(16) 0.0036(16) C34 0.040(2) 0.052(2) 0.039(2) 0.0154(18) 0.0058(18) 0.0051(18) C35 0.052(2) 0.039(2) 0.040(2) 0.0121(17) -0.0017(19) 0.0073(18) C36 0.045(2) 0.042(2) 0.041(2) 0.0133(18) -0.0063(18) 0.0008(17) C37 0.069(3) 0.070(3) 0.041(3) 0.000(2) 0.003(2) 0.000(2) C38 0.141(18) 0.110(11) 0.095(10) -0.037(8) 0.015(12) -0.023(11) C39 0.101(9) 0.122(15) 0.057(8) -0.014(8) 0.015(7) -0.003(8) C40 0.112(12) 0.131(14) 0.059(7) 0.013(9) -0.022(7) 0.020(11) C38' 0.104(11) 0.12(2) 0.077(10) -0.017(11) -0.015(8) 0.002(10) C39' 0.132(17) 0.099(14) 0.066(10) 0.012(10) 0.012(11) -0.026(11) C40' 0.129(17) 0.097(12) 0.089(11) -0.029(9) -0.002(13) 0.022(11) C41 0.056(3) 0.051(3) 0.073(3) -0.005(2) 0.007(2) -0.022(2) C42 0.075(3) 0.050(3) 0.076(3) -0.010(2) 0.007(3) -0.012(2) C43 0.085(3) 0.037(2) 0.061(3) 0.011(2) 0.013(3) 0.015(2) C44 0.105(4) 0.051(3) 0.080(4) -0.004(3) 0.003(3) 0.011(3) C45 0.121(5) 0.056(3) 0.093(4) -0.014(3) 0.000(4) 0.040(3) C46 0.095(4) 0.067(3) 0.081(4) -0.002(3) 0.014(3) 0.045(3) C47 0.078(3) 0.048(3) 0.082(4) 0.009(3) 0.012(3) 0.030(3) C48 0.085(4) 0.038(2) 0.071(3) 0.003(2) 0.017(3) 0.014(2) C49 0.053(3) 0.063(3) 0.097(4) 0.008(3) 0.002(3) 0.015(2) C50 0.041(2) 0.053(2) 0.056(3) 0.008(2) 0.0073(19) 0.0056(19) O1 0.0368(14) 0.0408(15) 0.0514(16) 0.0017(12) 0.0063(12) -0.0082(11) O2 0.0267(12) 0.0527(16) 0.0518(16) 0.0095(13) 0.0053(11) 0.0026(11) O3 0.0354(13) 0.0573(16) 0.0479(16) 0.0210(13) -0.0002(12) -0.0062(12) O4 0.0368(14) 0.0751(19) 0.0379(16) -0.0004(14) 0.0043(12) -0.0035(13) O5 0.085(2) 0.0548(18) 0.063(2) 0.0107(16) 0.0121(18) 0.0019(17) O6 0.070(2) 0.068(2) 0.127(3) -0.006(2) 0.026(2) 0.0245(19) S1 0.0364(5) 0.0522(6) 0.0523(6) 0.0222(5) 0.0001(4) -0.0065(4) S2 0.0411(5) 0.0723(7) 0.0368(6) 0.0052(5) -0.0052(4) -0.0236(5) S3 0.0289(5) 0.0612(6) 0.0382(5) 0.0124(5) 0.0041(4) -0.0022(4) S4 0.0272(5) 0.0666(7) 0.0490(6) 0.0222(5) -0.0022(4) 0.0049(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.388(5) . ? C1 O1 1.390(4) . ? C1 C2 1.393(5) . ? C2 C3 1.380(5) . ? C2 S1 1.794(4) . ? C3 C4 1.390(5) . ? C3 H3 0.9300 . ? C4 C5 1.393(5) . ? C4 C7 1.530(6) . ? C5 C6 1.383(5) . ? C5 H5 0.9300 . ? C6 S2 1.794(4) . ? C7 C9 1.494(7) . ? C7 C8' 1.496(6) . ? C7 C9' 1.531(7) . ? C7 C10 1.542(7) . ? C7 C8 1.559(7) . ? C7 C10' 1.560(7) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C10 H8D 0.8946 . ? C8' H8D 0.9600 . ? C8' H8E 0.9606 . ? C8' H8F 0.9598 . ? C9' H9D 0.9600 . ? C9' H9E 0.9600 . ? C9' H9F 0.9600 . ? C10' H10D 0.9600 . ? C10' H10E 0.9600 . ? C10' H10F 0.9600 . ? C11 C16 1.386(5) . ? C11 C12 1.394(5) . ? C11 S2 1.781(3) . ? C12 O3 1.346(4) . ? C12 C13 1.411(5) . ? C13 C14 1.387(5) . ? C13 S3 1.778(3) . ? C14 C15 1.395(5) . ? C14 H14 0.9300 . ? C15 C16 1.385(5) . ? C15 C17 1.529(5) . ? C16 H16 0.9300 . ? C17 C20 1.500(7) . ? C17 C19' 1.515(8) . ? C17 C18 1.521(7) . ? C17 C20' 1.523(8) . ? C17 C18' 1.567(8) . ? C17 C19 1.570(7) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C18' H18D 0.9600 . ? C18' H18E 0.9600 . ? C18' H18F 0.9600 . ? C19' H19D 0.9600 . ? C19' H19E 0.9600 . ? C19' H19F 0.9600 . ? C20' H20D 0.9600 . ? C20' H20E 0.9600 . ? C20' H20F 0.9600 . ? C21 C26 1.385(5) . ? C21 C22 1.391(5) . ? C21 S3 1.781(4) . ? C22 O2 1.377(4) . ? C22 C23 1.386(5) . ? C23 C24 1.384(5) . ? C23 S4 1.788(3) . ? C24 C25 1.386(5) . ? C24 H24 0.9300 . ? C25 C26 1.386(5) . ? C25 C27 1.531(5) . ? C26 H26 0.9300 . ? C27 C30 1.511(7) . ? C27 C30' 1.532(9) . ? C27 C28 1.534(6) . ? C27 C29' 1.539(9) . ? C27 C29 1.560(7) . ? C27 C28' 1.568(8) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C28' H28D 0.9600 . ? C28' H28E 0.9600 . ? C28' H28F 0.9600 . ? C29' H29D 0.9600 . ? C29' H29E 0.9600 . ? C29' H29F 0.9600 . ? C30' H30D 0.9600 . ? C30' H30E 0.9600 . ? C30' H30F 0.9600 . ? C31 C36 1.383(5) . ? C31 C32 1.394(5) . ? C31 S4 1.783(4) . ? C32 O4 1.348(4) . ? C32 C33 1.401(5) . ? C33 C34 1.383(5) . ? C33 S1 1.779(4) . ? C34 C35 1.384(5) . ? C34 H34 0.9300 . ? C35 C36 1.388(5) . ? C35 C37 1.536(6) . ? C36 H36 0.9300 . ? C37 C38 1.505(7) . ? C37 C39' 1.515(8) . ? C37 C38' 1.526(8) . ? C37 C40 1.529(7) . ? C37 C39 1.531(7) . ? C37 C40' 1.532(8) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C38' H38D 0.9600 . ? C38' H38E 0.9600 . ? C38' H38F 0.9600 . ? C39' H39D 0.9600 . ? C39' H39E 0.9600 . ? C39' H39F 0.9600 . ? C40' H40D 0.9600 . ? C40' H40E 0.9600 . ? C40' H40F 0.9600 . ? C41 O1 1.450(4) . ? C41 C42 1.487(6) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 O5 1.423(6) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C48 1.370(6) . ? C43 C44 1.378(6) . ? C43 O5 1.387(5) . ? C44 C45 1.378(7) . ? C44 H44 0.9300 . ? C45 C46 1.363(8) . ? C45 H45 0.9300 . ? C46 C47 1.384(7) . ? C46 H46 0.9300 . ? C47 O6 1.363(6) . ? C47 C48 1.389(6) . ? C48 H48 0.9300 . ? C49 O6 1.428(6) . ? C49 C50 1.507(6) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 O2 1.429(5) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? O3 H3A 0.8200 . ? O4 H4 0.8200 . ? 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 C6 C1 O1 119.7(3) . . ? C6 C1 C2 120.1(3) . . ? O1 C1 C2 120.2(3) . . ? C3 C2 C1 118.9(3) . . ? C3 C2 S1 121.1(3) . . ? C1 C2 S1 119.8(3) . . ? C2 C3 C4 122.8(4) . . ? C2 C3 H3 118.6 . . ? C4 C3 H3 118.6 . . ? C3 C4 C5 116.6(4) . . ? C3 C4 C7 121.7(4) . . ? C5 C4 C7 121.5(3) . . ? C6 C5 C4 122.3(3) . . ? C6 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? C5 C6 C1 119.3(3) . . ? C5 C6 S2 120.8(3) . . ? C1 C6 S2 119.5(3) . . ? C9 C7 C8' 129.8(8) . . ? C9 C7 C4 112.5(6) . . ? C8' C7 C4 114.1(7) . . ? C8' C7 C9' 111.1(8) . . ? C4 C7 C9' 111.8(5) . . ? C9 C7 C10 110.3(8) . . ? C4 C7 C10 110.9(6) . . ? C9' C7 C10 134.5(7) . . ? C9 C7 C8 108.8(8) . . ? C8' C7 C8 72.3(7) . . ? C4 C7 C8 108.9(5) . . ? C10 C7 C8 105.2(6) . . ? C8' C7 C10' 108.8(7) . . ? C4 C7 C10' 104.9(5) . . ? C9' C7 C10' 105.6(7) . . ? C8 C7 C10' 142.1(7) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? C7 C10 H8D 109.8 . . ? C7 C10 H8E 95.6 . . ? H8D C10 H8E 97.5 . . ? C7 C8' H8D 109.5 . . ? C7 C8' H8E 109.5 . . ? H8D C8' H8E 109.5 . . ? C7 C8' H8F 109.5 . . ? H8D C8' H8F 109.6 . . ? H8E C8' H8F 109.4 . . ? C7 C9' H9D 109.5 . . ? C7 C9' H9E 109.5 . . ? H9D C9' H9E 109.5 . . ? C7 C9' H9F 109.5 . . ? H9D C9' H9F 109.5 . . ? H9E C9' H9F 109.5 . . ? C7 C10' H10D 109.5 . . ? C7 C10' H10E 109.5 . . ? H10D C10' H10E 109.5 . . ? C7 C10' H10F 109.5 . . ? H10D C10' H10F 109.5 . . ? H10E C10' H10F 109.5 . . ? C16 C11 C12 120.8(3) . . ? C16 C11 S2 117.9(3) . . ? C12 C11 S2 120.5(3) . . ? O3 C12 C11 124.0(3) . . ? O3 C12 C13 118.4(3) . . ? C11 C12 C13 117.7(3) . . ? C14 C13 C12 120.1(3) . . ? C14 C13 S3 119.8(3) . . ? C12 C13 S3 119.9(3) . . ? C13 C14 C15 122.0(3) . . ? C13 C14 H14 119.0 . . ? C15 C14 H14 119.0 . . ? C16 C15 C14 117.1(3) . . ? C16 C15 C17 121.2(3) . . ? C14 C15 C17 121.6(3) . . ? C15 C16 C11 122.0(3) . . ? C15 C16 H16 119.0 . . ? C11 C16 H16 119.0 . . ? C20 C17 C18 111.5(9) . . ? C19' C17 C18 129.5(10) . . ? C20 C17 C20' 123.9(13) . . ? C19' C17 C20' 110.4(12) . . ? C20 C17 C15 114.5(5) . . ? C19' C17 C15 112.4(8) . . ? C18 C17 C15 111.2(8) . . ? C20' C17 C15 115.4(13) . . ? C19' C17 C18' 107.2(11) . . ? C20' C17 C18' 106.2(12) . . ? C15 C17 C18' 104.5(9) . . ? C20 C17 C19 108.2(7) . . ? C18 C17 C19 106.3(7) . . ? C20' C17 C19 82.3(9) . . ? C15 C17 C19 104.5(5) . . ? C18' C17 C19 142.2(10) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? C17 C18' H18D 109.5 . . ? C17 C18' H18E 109.5 . . ? H18D C18' H18E 109.5 . . ? C17 C18' H18F 109.5 . . ? H18D C18' H18F 109.5 . . ? H18E C18' H18F 109.5 . . ? C17 C19' H19D 109.5 . . ? C17 C19' H19E 109.5 . . ? H19D C19' H19E 109.5 . . ? C17 C19' H19F 109.5 . . ? H19D C19' H19F 109.5 . . ? H19E C19' H19F 109.5 . . ? C17 C20' H20D 109.5 . . ? C17 C20' H20E 109.5 . . ? H20D C20' H20E 109.5 . . ? C17 C20' H20F 109.5 . . ? H20D C20' H20F 109.5 . . ? H20E C20' H20F 109.5 . . ? C26 C21 C22 119.8(3) . . ? C26 C21 S3 120.3(3) . . ? C22 C21 S3 119.8(3) . . ? O2 C22 C23 119.9(3) . . ? O2 C22 C21 121.6(3) . . ? C23 C22 C21 118.4(3) . . ? C24 C23 C22 120.8(3) . . ? C24 C23 S4 119.8(3) . . ? C22 C23 S4 119.3(3) . . ? C23 C24 C25 121.4(4) . . ? C23 C24 H24 119.3 . . ? C25 C24 H24 119.3 . . ? C24 C25 C26 117.1(3) . . ? C24 C25 C27 122.0(4) . . ? C26 C25 C27 120.9(3) . . ? C21 C26 C25 122.3(3) . . ? C21 C26 H26 118.9 . . ? C25 C26 H26 118.9 . . ? C30 C27 C25 113.4(5) . . ? C30 C27 C30' 124.7(13) . . ? C25 C27 C30' 116.6(13) . . ? C30 C27 C28 110.6(7) . . ? C25 C27 C28 109.5(5) . . ? C25 C27 C29' 112.0(10) . . ? C30' C27 C29' 109.3(14) . . ? C28 C27 C29' 133.5(12) . . ? C30 C27 C29 109.1(6) . . ? C25 C27 C29 106.6(5) . . ? C30' C27 C29 77.5(13) . . ? C28 C27 C29 107.3(5) . . ? C25 C27 C28' 105.3(9) . . ? C30' C27 C28' 106.7(14) . . ? C29' C27 C28' 106.3(13) . . ? C29 C27 C28' 141.4(10) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? C27 C28' H28D 109.5 . . ? C27 C28' H28E 109.5 . . ? H28D C28' H28E 109.5 . . ? C27 C28' H28F 109.5 . . ? H28D C28' H28F 109.5 . . ? H28E C28' H28F 109.5 . . ? C27 C29' H29D 109.5 . . ? C27 C29' H29E 109.5 . . ? H29D C29' H29E 109.5 . . ? C27 C29' H29F 109.5 . . ? H29D C29' H29F 109.5 . . ? H29E C29' H29F 109.5 . . ? C27 C30' H30D 109.5 . . ? C27 C30' H30E 109.5 . . ? H30D C30' H30E 109.5 . . ? C27 C30' H30F 109.5 . . ? H30D C30' H30F 109.5 . . ? H30E C30' H30F 109.5 . . ? C36 C31 C32 120.0(3) . . ? C36 C31 S4 119.2(3) . . ? C32 C31 S4 120.8(3) . . ? O4 C32 C31 119.0(3) . . ? O4 C32 C33 122.8(3) . . ? C31 C32 C33 118.1(3) . . ? C34 C33 C32 119.9(3) . . ? C34 C33 S1 119.5(3) . . ? C32 C33 S1 120.4(3) . . ? C33 C34 C35 122.8(3) . . ? C33 C34 H34 118.6 . . ? C35 C34 H34 118.6 . . ? C34 C35 C36 116.3(4) . . ? C34 C35 C37 122.7(4) . . ? C36 C35 C37 121.0(4) . . ? C31 C36 C35 122.7(4) . . ? C31 C36 H36 118.6 . . ? C35 C36 H36 118.6 . . ? C38 C37 C39' 133.5(11) . . ? C39' C37 C38' 109.2(10) . . ? C38 C37 C40 110.2(9) . . ? C38 C37 C39 109.5(9) . . ? C38' C37 C39 130.7(9) . . ? C40 C37 C39 107.7(8) . . ? C39' C37 C40' 109.0(10) . . ? C38' C37 C40' 108.0(9) . . ? C40 C37 C40' 141.9(9) . . ? C39 C37 C40' 76.8(9) . . ? C38 C37 C35 110.6(7) . . ? C39' C37 C35 111.1(9) . . ? C38' C37 C35 113.2(7) . . ? C40 C37 C35 106.8(6) . . ? C39 C37 C35 112.0(7) . . ? C40' C37 C35 106.1(7) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? C37 C38' H38D 109.5 . . ? C37 C38' H38E 109.5 . . ? H38D C38' H38E 109.5 . . ? C37 C38' H38F 109.5 . . ? H38D C38' H38F 109.5 . . ? H38E C38' H38F 109.5 . . ? C37 C39' H39D 109.5 . . ? C37 C39' H39E 109.5 . . ? H39D C39' H39E 109.5 . . ? C37 C39' H39F 109.5 . . ? H39D C39' H39F 109.5 . . ? H39E C39' H39F 109.5 . . ? C37 C40' H40D 109.5 . . ? C37 C40' H40E 109.5 . . ? H40D C40' H40E 109.5 . . ? C37 C40' H40F 109.5 . . ? H40D C40' H40F 109.5 . . ? H40E C40' H40F 109.5 . . ? O1 C41 C42 108.3(3) . . ? O1 C41 H41A 110.0 . . ? C42 C41 H41A 110.0 . . ? O1 C41 H41B 110.0 . . ? C42 C41 H41B 110.0 . . ? H41A C41 H41B 108.4 . . ? O5 C42 C41 109.3(4) . . ? O5 C42 H42A 109.8 . . ? C41 C42 H42A 109.8 . . ? O5 C42 H42B 109.8 . . ? C41 C42 H42B 109.8 . . ? H42A C42 H42B 108.3 . . ? C48 C43 C44 122.0(5) . . ? C48 C43 O5 116.3(4) . . ? C44 C43 O5 121.6(5) . . ? C45 C44 C43 117.6(5) . . ? C45 C44 H44 121.2 . . ? C43 C44 H44 121.2 . . ? C46 C45 C44 121.7(5) . . ? C46 C45 H45 119.1 . . ? C44 C45 H45 119.1 . . ? C45 C46 C47 120.1(5) . . ? C45 C46 H46 119.9 . . ? C47 C46 H46 119.9 . . ? O6 C47 C46 116.2(5) . . ? O6 C47 C48 124.7(5) . . ? C46 C47 C48 119.1(5) . . ? C43 C48 C47 119.4(5) . . ? C43 C48 H48 120.3 . . ? C47 C48 H48 120.3 . . ? O6 C49 C50 113.5(4) . . ? O6 C49 H49A 108.9 . . ? C50 C49 H49A 108.9 . . ? O6 C49 H49B 108.9 . . ? C50 C49 H49B 108.9 . . ? H49A C49 H49B 107.7 . . ? O2 C50 C49 107.8(3) . . ? O2 C50 H50A 110.1 . . ? C49 C50 H50A 110.1 . . ? O2 C50 H50B 110.1 . . ? C49 C50 H50B 110.1 . . ? H50A C50 H50B 108.5 . . ? C1 O1 C41 113.3(3) . . ? C22 O2 C50 116.7(3) . . ? C12 O3 H3A 109.5 . . ? C32 O4 H4 109.5 . . ? C43 O5 C42 114.1(3) . . ? C47 O6 C49 118.0(4) . . ? C33 S1 C2 103.33(16) . . ? C11 S2 C6 106.01(16) . . ? C13 S3 C21 99.25(16) . . ? C31 S4 C23 97.69(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -1.6(5) . . . . ? O1 C1 C2 C3 -178.4(3) . . . . ? C6 C1 C2 S1 -176.8(2) . . . . ? O1 C1 C2 S1 6.4(4) . . . . ? C1 C2 C3 C4 0.9(5) . . . . ? S1 C2 C3 C4 176.1(3) . . . . ? C2 C3 C4 C5 -0.1(5) . . . . ? C2 C3 C4 C7 -175.8(3) . . . . ? C3 C4 C5 C6 -0.1(5) . . . . ? C7 C4 C5 C6 175.6(3) . . . . ? C4 C5 C6 C1 -0.6(5) . . . . ? C4 C5 C6 S2 -173.0(3) . . . . ? O1 C1 C6 C5 178.2(3) . . . . ? C2 C1 C6 C5 1.4(5) . . . . ? O1 C1 C6 S2 -9.3(4) . . . . ? C2 C1 C6 S2 174.0(3) . . . . ? C3 C4 C7 C9 69.6(9) . . . . ? C5 C4 C7 C9 -105.9(9) . . . . ? C3 C4 C7 C8' -129.5(6) . . . . ? C5 C4 C7 C8' 55.0(7) . . . . ? C3 C4 C7 C9' -2.5(9) . . . . ? C5 C4 C7 C9' -177.9(8) . . . . ? C3 C4 C7 C10 -166.4(6) . . . . ? C5 C4 C7 C10 18.2(7) . . . . ? C3 C4 C7 C8 -51.0(8) . . . . ? C5 C4 C7 C8 133.5(8) . . . . ? C3 C4 C7 C10' 111.5(7) . . . . ? C5 C4 C7 C10' -63.9(8) . . . . ? C16 C11 C12 O3 173.8(3) . . . . ? S2 C11 C12 O3 4.1(5) . . . . ? C16 C11 C12 C13 -5.1(5) . . . . ? S2 C11 C12 C13 -174.8(3) . . . . ? O3 C12 C13 C14 -174.1(3) . . . . ? C11 C12 C13 C14 4.8(5) . . . . ? O3 C12 C13 S3 0.8(5) . . . . ? C11 C12 C13 S3 179.7(3) . . . . ? C12 C13 C14 C15 -0.4(6) . . . . ? S3 C13 C14 C15 -175.3(3) . . . . ? C13 C14 C15 C16 -3.8(6) . . . . ? C13 C14 C15 C17 172.0(4) . . . . ? C14 C15 C16 C11 3.5(6) . . . . ? C17 C15 C16 C11 -172.2(4) . . . . ? C12 C11 C16 C15 0.9(6) . . . . ? S2 C11 C16 C15 170.9(3) . . . . ? C16 C15 C17 C20 -166.4(10) . . . . ? C14 C15 C17 C20 18.1(11) . . . . ? C16 C15 C17 C19' 115.0(15) . . . . ? C14 C15 C17 C19' -60.6(15) . . . . ? C16 C15 C17 C18 -38.8(9) . . . . ? C14 C15 C17 C18 145.6(8) . . . . ? C16 C15 C17 C20' -12.8(13) . . . . ? C14 C15 C17 C20' 171.6(12) . . . . ? C16 C15 C17 C18' -129.0(14) . . . . ? C14 C15 C17 C18' 55.4(14) . . . . ? C16 C15 C17 C19 75.4(9) . . . . ? C14 C15 C17 C19 -100.2(9) . . . . ? C26 C21 C22 O2 173.7(3) . . . . ? S3 C21 C22 O2 -10.6(4) . . . . ? C26 C21 C22 C23 -4.4(5) . . . . ? S3 C21 C22 C23 171.3(2) . . . . ? O2 C22 C23 C24 -173.5(3) . . . . ? C21 C22 C23 C24 4.6(5) . . . . ? O2 C22 C23 S4 10.4(4) . . . . ? C21 C22 C23 S4 -171.5(2) . . . . ? C22 C23 C24 C25 -2.6(5) . . . . ? S4 C23 C24 C25 173.5(3) . . . . ? C23 C24 C25 C26 0.3(5) . . . . ? C23 C24 C25 C27 -179.6(3) . . . . ? C22 C21 C26 C25 2.2(5) . . . . ? S3 C21 C26 C25 -173.5(3) . . . . ? C24 C25 C26 C21 -0.1(5) . . . . ? C27 C25 C26 C21 179.7(3) . . . . ? C24 C25 C27 C30 10.1(10) . . . . ? C26 C25 C27 C30 -169.8(9) . . . . ? C24 C25 C27 C30' 165.8(17) . . . . ? C26 C25 C27 C30' -14.0(17) . . . . ? C24 C25 C27 C28 134.1(6) . . . . ? C26 C25 C27 C28 -45.7(7) . . . . ? C24 C25 C27 C29' -67.3(19) . . . . ? C26 C25 C27 C29' 112.9(19) . . . . ? C24 C25 C27 C29 -110.0(7) . . . . ? C26 C25 C27 C29 70.1(7) . . . . ? C24 C25 C27 C28' 47.8(14) . . . . ? C26 C25 C27 C28' -132.0(13) . . . . ? C36 C31 C32 O4 176.6(3) . . . . ? S4 C31 C32 O4 -2.9(5) . . . . ? C36 C31 C32 C33 -3.7(5) . . . . ? S4 C31 C32 C33 176.7(3) . . . . ? O4 C32 C33 C34 -177.0(3) . . . . ? C31 C32 C33 C34 3.4(5) . . . . ? O4 C32 C33 S1 -2.2(5) . . . . ? C31 C32 C33 S1 178.2(3) . . . . ? C32 C33 C34 C35 -0.4(5) . . . . ? S1 C33 C34 C35 -175.2(3) . . . . ? C33 C34 C35 C36 -2.1(5) . . . . ? C33 C34 C35 C37 179.7(3) . . . . ? C32 C31 C36 C35 1.2(5) . . . . ? S4 C31 C36 C35 -179.3(3) . . . . ? C34 C35 C36 C31 1.8(5) . . . . ? C37 C35 C36 C31 180.0(3) . . . . ? C34 C35 C37 C38 124.6(12) . . . . ? C36 C35 C37 C38 -53.5(13) . . . . ? C34 C35 C37 C39' -34.3(14) . . . . ? C36 C35 C37 C39' 147.6(14) . . . . ? C34 C35 C37 C38' -157.6(13) . . . . ? C36 C35 C37 C38' 24.3(14) . . . . ? C34 C35 C37 C40 -115.5(11) . . . . ? C36 C35 C37 C40 66.4(11) . . . . ? C34 C35 C37 C39 2.1(12) . . . . ? C36 C35 C37 C39 -176.0(11) . . . . ? C34 C35 C37 C40' 84.1(13) . . . . ? C36 C35 C37 C40' -94.0(13) . . . . ? O1 C41 C42 O5 -67.3(5) . . . . ? C48 C43 C44 C45 0.7(7) . . . . ? O5 C43 C44 C45 -179.0(4) . . . . ? C43 C44 C45 C46 0.9(8) . . . . ? C44 C45 C46 C47 -1.0(8) . . . . ? C45 C46 C47 O6 177.8(5) . . . . ? C45 C46 C47 C48 -0.4(8) . . . . ? C44 C43 C48 C47 -2.1(7) . . . . ? O5 C43 C48 C47 177.5(4) . . . . ? O6 C47 C48 C43 -176.1(4) . . . . ? C46 C47 C48 C43 2.0(7) . . . . ? O6 C49 C50 O2 151.2(4) . . . . ? C6 C1 O1 C41 90.9(4) . . . . ? C2 C1 O1 C41 -92.3(4) . . . . ? C42 C41 O1 C1 -170.4(4) . . . . ? C23 C22 O2 C50 -99.8(4) . . . . ? C21 C22 O2 C50 82.2(4) . . . . ? C49 C50 O2 C22 135.8(3) . . . . ? C48 C43 O5 C42 -114.7(4) . . . . ? C44 C43 O5 C42 65.0(5) . . . . ? C41 C42 O5 C43 152.7(4) . . . . ? C46 C47 O6 C49 -176.1(4) . . . . ? C48 C47 O6 C49 2.0(7) . . . . ? C50 C49 O6 C47 70.4(5) . . . . ? C34 C33 S1 C2 -109.6(3) . . . . ? C32 C33 S1 C2 75.6(3) . . . . ? C3 C2 S1 C33 80.4(3) . . . . ? C1 C2 S1 C33 -104.5(3) . . . . ? C16 C11 S2 C6 124.2(3) . . . . ? C12 C11 S2 C6 -65.8(3) . . . . ? C5 C6 S2 C11 -83.0(3) . . . . ? C1 C6 S2 C11 104.6(3) . . . . ? C14 C13 S3 C21 -126.6(3) . . . . ? C12 C13 S3 C21 58.5(3) . . . . ? C26 C21 S3 C13 43.0(3) . . . . ? C22 C21 S3 C13 -132.6(3) . . . . ? C36 C31 S4 C23 114.2(3) . . . . ? C32 C31 S4 C23 -66.3(3) . . . . ? C24 C23 S4 C31 -43.8(3) . . . . ? C22 C23 S4 C31 132.3(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4 O1 0.82 2.19 2.931(4) 150.0 . O4 H4 S1 0.82 2.54 3.059(3) 122.1 . O3 H3A O1 0.82 2.08 2.861(3) 159.1 . O3 H3A S2 0.82 2.58 3.081(3) 121.1 . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.338 _refine_diff_density_min -0.252 _refine_diff_density_rms 0.053 #===END data_publication_text _publ_contact_author 'Xiong Li' _publ_contact_author_email 'lxwhu2008@hotmail.com' loop_ _publ_author_name 'Xiong Li' 'Shu-Ling Gong' 'Wei-Ping Yang' 'Yuan-Yin Chen' 'Xiang-Gao Meng' _journal_name_full 'Dalton Transactions' data_CCDC-740899 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,3-alternate-5,11,17,23-Tetra-tert-butyl-25,27-[1,2- bis(oxyethoxy)benzene]-2,8,14,20 -tetra-thiacalix[4]arene silver picrate complex ; _chemical_name_common ; 1,3-alternate-thiacalix[4]-o-benzocrown-4 silver picrate complex ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C116 H124 Ag2 Cl12 N6 O26 S8' _chemical_formula_weight 2915.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 '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 13.9789(13) _cell_length_b 19.0304(18) _cell_length_c 26.184(3) _cell_angle_alpha 74.579(2) _cell_angle_beta 75.176(2) _cell_angle_gamma 77.048(2) _cell_volume 6399.5(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9133 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 25.16 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.513 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2992 _exptl_absorpt_coefficient_mu 0.759 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8630 _exptl_absorpt_correction_T_max 0.9280 _exptl_absorpt_process_details 'SADABS, Sheldrick,1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 96956 _diffrn_reflns_av_R_equivalents 0.0415 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 26.01 _reflns_number_total 24360 _reflns_number_gt 19351 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. During the refinement, some tert-butyl groups were found to be seriously disordered. Commands ¡®DFIX¡¯, ¡®SADI¡¯and ¡®ISOR¡¯ were used to refine them to arrive at more appropriate values. ; _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^)+(0.0533P)^2^+41.0570P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 24360 _refine_ls_number_parameters 1556 _refine_ls_number_restraints 61 _refine_ls_R_factor_all 0.0848 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.1627 _refine_ls_wR_factor_gt 0.1383 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.003 _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 Ag1 Ag 0.77550(3) 0.17612(2) 0.326733(15) 0.02002(10) Uani 1 1 d . . . Ag2 Ag 1.22509(3) 0.33456(2) 0.163822(15) 0.02123(10) Uani 1 1 d . . . C1 C 0.8269(4) 0.4384(3) 0.45532(19) 0.0192(10) Uani 1 1 d . . . C2 C 0.7239(4) 0.4614(3) 0.47074(19) 0.0198(10) Uani 1 1 d . . . C3 C 0.6859(4) 0.5334(3) 0.4774(2) 0.0224(11) Uani 1 1 d . . . H3 H 0.6154 0.5481 0.4876 0.027 Uiso 1 1 calc R . . C4 C 0.7490(4) 0.5841(3) 0.4695(2) 0.0237(11) Uani 1 1 d . A . C5 C 0.8513(4) 0.5608(3) 0.4542(2) 0.0208(11) Uani 1 1 d . . . H5 H 0.8956 0.5948 0.4482 0.025 Uiso 1 1 calc R . . C6 C 0.8912(4) 0.4895(3) 0.44720(19) 0.0216(11) Uani 1 1 d . . . C7 C 0.7063(4) 0.6624(3) 0.4776(2) 0.0342(14) Uani 1 1 d D . . C8 C 0.6287(8) 0.6962(8) 0.4405(5) 0.0568(12) Uani 0.544(7) 1 d PD A 1 H8A H 0.5820 0.6619 0.4467 0.085 Uiso 0.544(7) 1 calc PR A 1 H8B H 0.6640 0.7049 0.4025 0.085 Uiso 0.544(7) 1 calc PR A 1 H8C H 0.5912 0.7432 0.4491 0.085 Uiso 0.544(7) 1 calc PR A 1 C9 C 0.6560(9) 0.6665(7) 0.5327(3) 0.0568(12) Uani 0.544(7) 1 d PD A 1 H9A H 0.7037 0.6454 0.5567 0.085 Uiso 0.544(7) 1 calc PR A 1 H9B H 0.6003 0.6385 0.5443 0.085 Uiso 0.544(7) 1 calc PR A 1 H9C H 0.6300 0.7183 0.5345 0.085 Uiso 0.544(7) 1 calc PR A 1 C10 C 0.7869(8) 0.7119(7) 0.4571(5) 0.0568(12) Uani 0.544(7) 1 d PDU A 1 H10A H 0.7571 0.7619 0.4624 0.085 Uiso 0.544(7) 1 calc PR A 1 H10B H 0.8146 0.7139 0.4185 0.085 Uiso 0.544(7) 1 calc PR A 1 H10C H 0.8408 0.6917 0.4774 0.085 Uiso 0.544(7) 1 calc PR A 1 C11 C 1.0648(3) 0.4043(3) 0.3418(2) 0.0169(10) Uani 1 1 d . . . C12 C 1.0569(3) 0.4663(3) 0.36246(19) 0.0167(10) Uani 1 1 d . . . C13 C 1.0789(4) 0.5326(3) 0.3277(2) 0.0194(10) Uani 1 1 d . . . H13 H 1.0722 0.5744 0.3425 0.023 Uiso 1 1 calc R . . C14 C 1.1103(4) 0.5394(3) 0.2722(2) 0.0223(11) Uani 1 1 d . . . C15 C 1.1194(4) 0.4767(3) 0.2520(2) 0.0202(10) Uani 1 1 d . . . H15 H 1.1427 0.4793 0.2142 0.024 Uiso 1 1 calc R . . C16 C 1.0953(3) 0.4109(3) 0.28593(19) 0.0166(10) Uani 1 1 d . . . C17 C 1.1323(4) 0.6114(3) 0.2321(2) 0.0262(12) Uani 1 1 d . . . C18 C 1.0523(6) 0.6401(4) 0.1983(3) 0.0479(18) Uani 1 1 d . . . H18A H 0.9866 0.6504 0.2221 0.072 Uiso 1 1 calc R . . H18B H 1.0510 0.6027 0.1791 0.072 Uiso 1 1 calc R . . H18C H 1.0676 0.6855 0.1720 0.072 Uiso 1 1 calc R . . C19 C 1.2353(5) 0.5972(3) 0.1947(3) 0.0424(16) Uani 1 1 d . . . H19A H 1.2513 0.6439 0.1705 0.064 Uiso 1 1 calc R . . H19B H 1.2340 0.5625 0.1732 0.064 Uiso 1 1 calc R . . H19C H 1.2865 0.5760 0.2166 0.064 Uiso 1 1 calc R . . C20 C 1.1344(5) 0.6710(3) 0.2611(3) 0.0363(14) Uani 1 1 d . . . H20A H 1.0688 0.6818 0.2848 0.054 Uiso 1 1 calc R . . H20B H 1.1496 0.7161 0.2342 0.054 Uiso 1 1 calc R . . H20C H 1.1861 0.6533 0.2829 0.054 Uiso 1 1 calc R . . C21 C 0.8967(3) 0.3343(3) 0.27124(18) 0.0137(9) Uani 1 1 d . C . C22 C 0.9802(3) 0.3630(3) 0.23579(19) 0.0162(10) Uani 1 1 d . . . C23 C 0.9705(4) 0.4116(3) 0.18754(19) 0.0181(10) Uani 1 1 d . . . H23 H 1.0283 0.4298 0.1645 0.022 Uiso 1 1 calc R . . C24 C 0.8791(4) 0.4355(3) 0.17095(19) 0.0173(10) Uani 1 1 d . . . C25 C 0.7985(4) 0.4038(3) 0.2042(2) 0.0187(10) Uani 1 1 d . C . H25 H 0.7357 0.4170 0.1935 0.022 Uiso 1 1 calc R . . C26 C 0.8063(3) 0.3533(3) 0.25294(19) 0.0157(10) Uani 1 1 d . . . C27 C 0.8717(4) 0.4932(3) 0.1175(2) 0.0255(12) Uani 1 1 d . . . C28 C 0.9157(5) 0.5604(4) 0.1164(3) 0.0479(7) Uani 1 1 d . . . H28A H 0.9108 0.5968 0.0823 0.072 Uiso 1 1 calc R . . H28B H 0.9862 0.5449 0.1191 0.072 Uiso 1 1 calc R . . H28C H 0.8780 0.5826 0.1470 0.072 Uiso 1 1 calc R . . C29 C 0.7646(5) 0.5185(4) 0.1098(3) 0.0479(7) Uani 1 1 d . . . H29A H 0.7631 0.5572 0.0766 0.072 Uiso 1 1 calc R . . H29B H 0.7234 0.5382 0.1409 0.072 Uiso 1 1 calc R . . H29C H 0.7381 0.4765 0.1070 0.072 Uiso 1 1 calc R . . C30 C 0.9329(5) 0.4584(4) 0.0703(3) 0.0479(7) Uani 1 1 d . . . H30A H 0.9075 0.4138 0.0716 0.072 Uiso 1 1 calc R . . H30B H 1.0036 0.4452 0.0731 0.072 Uiso 1 1 calc R . . H30C H 0.9268 0.4938 0.0360 0.072 Uiso 1 1 calc R . . C31 C 0.6617(3) 0.3595(3) 0.38599(19) 0.0160(10) Uani 1 1 d . C . C32 C 0.6383(4) 0.3721(3) 0.3353(2) 0.0176(10) Uani 1 1 d . . . C33 C 0.5665(4) 0.4311(3) 0.3182(2) 0.0207(11) Uani 1 1 d . C . H33 H 0.5506 0.4372 0.2839 0.025 Uiso 1 1 calc R . . C34 C 0.5177(4) 0.4811(3) 0.3502(2) 0.0248(11) Uani 1 1 d . . . C35 C 0.5426(4) 0.4694(3) 0.4006(2) 0.0240(11) Uani 1 1 d . C . H35 H 0.5097 0.5029 0.4234 0.029 Uiso 1 1 calc R . . C36 C 0.6141(4) 0.4104(3) 0.4185(2) 0.0201(10) Uani 1 1 d . . . C37 C 0.4339(5) 0.5439(3) 0.3333(3) 0.0339(13) Uani 1 1 d . C . C38 C 0.4525(5) 0.5737(4) 0.2723(3) 0.0479(7) Uani 1 1 d . . . H38A H 0.4462 0.5361 0.2546 0.072 Uiso 1 1 calc R C . H38B H 0.5203 0.5861 0.2593 0.072 Uiso 1 1 calc R . . H38C H 0.4031 0.6182 0.2637 0.072 Uiso 1 1 calc R . . C39 C 0.3355(5) 0.5145(4) 0.3527(3) 0.0479(7) Uani 1 1 d . . . H39A H 0.3376 0.4759 0.3339 0.072 Uiso 1 1 calc R C . H39B H 0.2802 0.5549 0.3450 0.072 Uiso 1 1 calc R . . H39C H 0.3252 0.4938 0.3918 0.072 Uiso 1 1 calc R . . C40 C 0.4261(5) 0.6097(4) 0.3579(3) 0.0479(7) Uani 1 1 d . . . H40A H 0.3754 0.6501 0.3443 0.072 Uiso 1 1 calc R C . H40B H 0.4912 0.6263 0.3478 0.072 Uiso 1 1 calc R . . H40C H 0.4068 0.5949 0.3974 0.072 Uiso 1 1 calc R . . C41 C 1.1087(4) 0.2755(3) 0.3829(2) 0.0267(12) Uani 1 1 d . . . H41A H 1.1767 0.2886 0.3732 0.032 Uiso 1 1 calc R . . H41B H 1.1057 0.2449 0.3583 0.032 Uiso 1 1 calc R . . C42 C 1.0880(4) 0.2329(3) 0.4406(2) 0.0251(12) Uani 1 1 d . . . H42A H 1.1463 0.1936 0.4470 0.030 Uiso 1 1 calc R . . H42B H 1.0796 0.2665 0.4651 0.030 Uiso 1 1 calc R . . C43 C 1.0115(4) 0.1305(3) 0.44278(19) 0.0207(11) Uani 1 1 d . . . C44 C 0.9361(4) 0.1156(3) 0.42306(19) 0.0201(10) Uani 1 1 d . . . C45 C 0.9432(4) 0.0466(3) 0.4127(2) 0.0248(11) Uani 1 1 d . . . H45 H 0.8916 0.0367 0.3994 0.030 Uiso 1 1 calc R . . C46 C 1.0252(4) -0.0081(3) 0.4217(2) 0.0277(12) Uani 1 1 d . . . H46 H 1.0311 -0.0546 0.4133 0.033 Uiso 1 1 calc R . . C47 C 1.0983(4) 0.0057(3) 0.4431(2) 0.0266(12) Uani 1 1 d . . . H47 H 1.1536 -0.0320 0.4504 0.032 Uiso 1 1 calc R . . C48 C 1.0908(4) 0.0744(3) 0.4538(2) 0.0252(12) Uani 1 1 d . . . H48 H 1.1407 0.0832 0.4689 0.030 Uiso 1 1 calc R . . C49 C 0.7853(4) 0.1885(3) 0.45846(19) 0.0215(11) Uani 1 1 d . . . H49A H 0.8175 0.2132 0.4767 0.026 Uiso 1 1 calc R . . H49B H 0.7638 0.1437 0.4844 0.026 Uiso 1 1 calc R . . C50 C 0.6971(4) 0.2394(3) 0.4398(2) 0.0190(10) Uani 1 1 d . C . H50A H 0.6635 0.2142 0.4225 0.023 Uiso 1 1 calc R . . H50B H 0.6481 0.2557 0.4708 0.023 Uiso 1 1 calc R . . C51 C 1.3246(4) -0.0331(3) 0.15641(19) 0.0167(10) Uani 1 1 d . . . C52 C 1.3799(4) -0.0285(3) 0.1032(2) 0.0199(10) Uani 1 1 d . . . C53 C 1.3873(4) -0.0832(3) 0.0760(2) 0.0218(11) Uani 1 1 d . . . H53 H 1.4236 -0.0780 0.0395 0.026 Uiso 1 1 calc R . . C54 C 1.3429(4) -0.1456(3) 0.1004(2) 0.0215(11) Uani 1 1 d . . . C55 C 1.2922(4) -0.1517(3) 0.1541(2) 0.0206(11) Uani 1 1 d . . . H55 H 1.2632 -0.1947 0.1721 0.025 Uiso 1 1 calc R . . C56 C 1.2821(3) -0.0979(3) 0.18248(19) 0.0171(10) Uani 1 1 d . . . C57 C 1.3514(4) -0.2081(3) 0.0718(2) 0.0302(13) Uani 1 1 d . . . C58 C 1.3990(5) -0.1884(4) 0.0115(2) 0.0417(17) Uani 1 1 d . . . H58A H 1.3617 -0.1418 -0.0056 0.063 Uiso 1 1 calc R . . H58B H 1.3968 -0.2278 -0.0056 0.063 Uiso 1 1 calc R . . H58C H 1.4689 -0.1830 0.0072 0.063 Uiso 1 1 calc R . . C59 C 1.4163(5) -0.2764(3) 0.0992(3) 0.0391(15) Uani 1 1 d . . . H59A H 1.4856 -0.2676 0.0912 0.059 Uiso 1 1 calc R . . H59B H 1.4145 -0.3191 0.0855 0.059 Uiso 1 1 calc R . . H59C H 1.3904 -0.2860 0.1385 0.059 Uiso 1 1 calc R . . C60 C 1.2471(5) -0.2247(3) 0.0765(2) 0.0356(14) Uani 1 1 d . . . H60A H 1.2144 -0.2377 0.1148 0.053 Uiso 1 1 calc R . . H60B H 1.2533 -0.2662 0.0596 0.053 Uiso 1 1 calc R . . H60C H 1.2067 -0.1809 0.0581 0.053 Uiso 1 1 calc R . . C61 C 1.0858(4) 0.0070(3) 0.26997(19) 0.0167(10) Uani 1 1 d . C . C62 C 1.1088(4) -0.0645(3) 0.26101(19) 0.0186(10) Uani 1 1 d . . . C63 C 1.0319(4) -0.0995(3) 0.2596(2) 0.0204(10) Uani 1 1 d . . . H63 H 1.0486 -0.1486 0.2543 0.024 Uiso 1 1 calc R . . C64 C 0.9324(4) -0.0655(3) 0.2657(2) 0.0231(11) Uani 1 1 d . . . C65 C 0.9114(4) 0.0069(3) 0.2729(2) 0.0212(11) Uani 1 1 d . C . H65 H 0.8440 0.0322 0.2769 0.025 Uiso 1 1 calc R . . C66 C 0.9856(4) 0.0425(3) 0.27438(19) 0.0162(10) Uani 1 1 d . . . C67 C 0.8458(4) -0.1034(3) 0.2665(3) 0.0302(13) Uani 1 1 d . . . C68 C 0.8847(5) -0.1777(4) 0.2502(4) 0.0501(19) Uani 1 1 d . . . H68A H 0.9289 -0.1703 0.2142 0.075 Uiso 1 1 calc R . . H68B H 0.8279 -0.1993 0.2493 0.075 Uiso 1 1 calc R . . H68C H 0.9223 -0.2112 0.2765 0.075 Uiso 1 1 calc R . . C69 C 0.7812(5) -0.0547(4) 0.2266(3) 0.0436(17) Uani 1 1 d . . . H69A H 0.7508 -0.0081 0.2379 0.065 Uiso 1 1 calc R . . H69B H 0.7282 -0.0806 0.2263 0.065 Uiso 1 1 calc R . . H69C H 0.8234 -0.0444 0.1902 0.065 Uiso 1 1 calc R . . C70 C 0.7819(5) -0.1158(4) 0.3241(3) 0.0457(17) Uani 1 1 d . . . H70A H 0.8238 -0.1463 0.3494 0.069 Uiso 1 1 calc R . . H70B H 0.7270 -0.1411 0.3258 0.069 Uiso 1 1 calc R . . H70C H 0.7541 -0.0680 0.3340 0.069 Uiso 1 1 calc R . . C71 C 1.0556(4) 0.2095(3) 0.18268(19) 0.0172(10) Uani 1 1 d . C . C72 C 0.9668(4) 0.1816(3) 0.21068(19) 0.0178(10) Uani 1 1 d . . . C73 C 0.8906(4) 0.1878(3) 0.1838(2) 0.0205(10) Uani 1 1 d . C . H73 H 0.8321 0.1674 0.2032 0.025 Uiso 1 1 calc R . . C74 C 0.8967(4) 0.2229(3) 0.1295(2) 0.0244(11) Uani 1 1 d . . . C75 C 0.9821(4) 0.2546(3) 0.1032(2) 0.0219(11) Uani 1 1 d . C . H75 H 0.9877 0.2807 0.0665 0.026 Uiso 1 1 calc R . . C76 C 1.0592(4) 0.2490(3) 0.12943(19) 0.0176(10) Uani 1 1 d . . . C77 C 0.8144(4) 0.2249(3) 0.1005(2) 0.0336(14) Uani 1 1 d DU B . C78 C 0.7152(7) 0.2087(6) 0.1368(4) 0.0568(12) Uani 0.627(8) 1 d PD B 1 H78A H 0.6666 0.2131 0.1145 0.085 Uiso 0.627(8) 1 calc PR B 1 H78B H 0.6902 0.2440 0.1603 0.085 Uiso 0.627(8) 1 calc PR B 1 H78C H 0.7245 0.1583 0.1590 0.085 Uiso 0.627(8) 1 calc PR B 1 C79 C 0.8525(8) 0.1625(5) 0.0680(5) 0.0568(12) Uani 0.627(8) 1 d PD B 1 H79A H 0.8653 0.1147 0.0931 0.085 Uiso 0.627(8) 1 calc PR B 1 H79B H 0.9146 0.1723 0.0418 0.085 Uiso 0.627(8) 1 calc PR B 1 H79C H 0.8014 0.1614 0.0488 0.085 Uiso 0.627(8) 1 calc PR B 1 C80 C 0.7956(9) 0.2958(5) 0.0580(4) 0.0568(12) Uani 0.627(8) 1 d PD B 1 H80A H 0.8573 0.3020 0.0305 0.085 Uiso 0.627(8) 1 calc PR B 1 H80B H 0.7748 0.3380 0.0754 0.085 Uiso 0.627(8) 1 calc PR B 1 H80C H 0.7425 0.2929 0.0408 0.085 Uiso 0.627(8) 1 calc PR B 1 C81 C 1.3097(4) 0.1713(3) 0.07706(19) 0.0169(10) Uani 1 1 d . C . C82 C 1.2386(4) 0.2278(3) 0.05598(19) 0.0169(10) Uani 1 1 d . . . C83 C 1.2214(4) 0.2327(3) 0.0052(2) 0.0196(10) Uani 1 1 d . C . H83 H 1.1747 0.2729 -0.0092 0.024 Uiso 1 1 calc R . . C84 C 1.2710(4) 0.1802(3) -0.0255(2) 0.0241(11) Uani 1 1 d . . . C85 C 1.3382(4) 0.1223(3) -0.0029(2) 0.0228(11) Uani 1 1 d . C . H85 H 1.3710 0.0845 -0.0220 0.027 Uiso 1 1 calc R . . C86 C 1.3588(4) 0.1181(3) 0.04747(19) 0.0166(10) Uani 1 1 d . . . C87 C 1.2504(5) 0.1892(3) -0.0822(2) 0.0342(14) Uani 1 1 d . C . C88 C 1.3033(6) 0.1223(4) -0.1065(3) 0.0513(19) Uani 1 1 d . . . H88A H 1.2862 0.1286 -0.1417 0.077 Uiso 1 1 calc R C . H88B H 1.2815 0.0773 -0.0820 0.077 Uiso 1 1 calc R . . H88C H 1.3761 0.1180 -0.1114 0.077 Uiso 1 1 calc R . . C89 C 1.2900(6) 0.2582(4) -0.1192(2) 0.0504(19) Uani 1 1 d . . . H89A H 1.2561 0.3015 -0.1042 0.076 Uiso 1 1 calc R C . H89B H 1.2769 0.2651 -0.1554 0.076 Uiso 1 1 calc R . . H89C H 1.3625 0.2520 -0.1217 0.076 Uiso 1 1 calc R . . C90 C 1.1367(5) 0.1989(4) -0.0790(3) 0.0473(17) Uani 1 1 d . . . H90A H 1.1025 0.2427 -0.0646 0.071 Uiso 1 1 calc R C . H90B H 1.1109 0.1551 -0.0550 0.071 Uiso 1 1 calc R . . H90C H 1.1245 0.2051 -0.1153 0.071 Uiso 1 1 calc R . . C91 C 1.2267(4) 0.0133(3) 0.30540(19) 0.0177(10) Uani 1 1 d . C . H91A H 1.2898 -0.0069 0.2827 0.021 Uiso 1 1 calc R . . H91B H 1.2022 -0.0280 0.3344 0.021 Uiso 1 1 calc R . . C92 C 1.2452(4) 0.0706(3) 0.3298(2) 0.0217(11) Uani 1 1 d . . . H92A H 1.1807 0.0967 0.3473 0.026 Uiso 1 1 calc R . . H92B H 1.2861 0.0469 0.3575 0.026 Uiso 1 1 calc R . . C93 C 1.3317(4) 0.1732(3) 0.3023(2) 0.0200(10) Uani 1 1 d . . . C94 C 1.3587(4) 0.2335(3) 0.2611(2) 0.0187(10) Uani 1 1 d . . . C95 C 1.3944(5) 0.2882(3) 0.2722(2) 0.0331(13) Uani 1 1 d . . . H95 H 1.4116 0.3294 0.2440 0.040 Uiso 1 1 calc R . . C96 C 1.4054(5) 0.2838(4) 0.3239(2) 0.0379(15) Uani 1 1 d . . . H96 H 1.4294 0.3221 0.3314 0.045 Uiso 1 1 calc R . . C97 C 1.3815(4) 0.2237(3) 0.3647(2) 0.0294(12) Uani 1 1 d . . . H97 H 1.3915 0.2198 0.4000 0.035 Uiso 1 1 calc R . . C98 C 1.3430(4) 0.1689(3) 0.3545(2) 0.0245(11) Uani 1 1 d . . . H98 H 1.3244 0.1285 0.3830 0.029 Uiso 1 1 calc R . . C99 C 1.4281(4) 0.1929(3) 0.1802(2) 0.0231(11) Uani 1 1 d . . . H99A H 1.4307 0.1404 0.1995 0.028 Uiso 1 1 calc R . . H99B H 1.4928 0.2077 0.1779 0.028 Uiso 1 1 calc R . . C100 C 1.4107(4) 0.2026(3) 0.12406(19) 0.0205(11) Uani 1 1 d . C . H10D H 1.3943 0.2558 0.1076 0.025 Uiso 1 1 calc R . . H10E H 1.4723 0.1813 0.1009 0.025 Uiso 1 1 calc R . . C101 C 0.6374(4) 0.0412(3) 0.3903(2) 0.0215(11) Uani 1 1 d . . . C102 C 0.5808(4) 0.0442(3) 0.3501(2) 0.0213(11) Uani 1 1 d . C . C103 C 0.5140(4) -0.0025(3) 0.3568(2) 0.0233(11) Uani 1 1 d . . . H103 H 0.4790 0.0021 0.3291 0.028 Uiso 1 1 calc R C . C104 C 0.4984(4) -0.0562(3) 0.4041(2) 0.0226(11) Uani 1 1 d . C . C105 C 0.5507(4) -0.0642(3) 0.4444(2) 0.0248(11) Uani 1 1 d . . . H105 H 0.5420 -0.1026 0.4760 0.030 Uiso 1 1 calc R C . C106 C 0.6145(4) -0.0165(3) 0.4382(2) 0.0236(11) Uani 1 1 d . C . C107 C 1.3750(4) 0.4637(3) 0.1125(2) 0.0209(11) Uani 1 1 d . . . C108 C 1.3309(4) 0.5091(3) 0.0677(2) 0.0197(10) Uani 1 1 d . . . C109 C 1.3772(4) 0.5610(3) 0.0271(2) 0.0199(10) Uani 1 1 d . . . H109 H 1.3454 0.5886 -0.0018 0.024 Uiso 1 1 calc R . . C110 C 1.4703(4) 0.5722(3) 0.0289(2) 0.0196(10) Uani 1 1 d . . . C111 C 1.5180(4) 0.5329(3) 0.0707(2) 0.0253(12) Uani 1 1 d . . . H111 H 1.5814 0.5418 0.0720 0.030 Uiso 1 1 calc R . . C112 C 1.4718(4) 0.4814(3) 0.1098(2) 0.0247(12) Uani 1 1 d . D . C113 C 0.2424(7) 0.4250(5) 0.6881(4) 0.074(3) Uani 1 1 d . . . H113 H 0.3008 0.4316 0.6569 0.088 Uiso 1 1 calc R . . C114 C 0.5212(5) 0.1684(4) 0.7232(3) 0.0403(15) Uani 1 1 d . . . H114 H 0.5910 0.1612 0.7010 0.048 Uiso 1 1 calc R . . C115 C 0.8904(5) 0.2560(4) 0.5704(3) 0.0387(15) Uani 1 1 d . . . H115 H 0.9077 0.2601 0.5303 0.046 Uiso 1 1 calc R . . C116 C 0.8831(5) 1.0158(3) 0.9151(3) 0.0379(14) Uani 1 1 d . . . H116 H 0.8237 1.0478 0.9014 0.045 Uiso 1 1 calc R . . Cl1 Cl 0.1776(3) 0.35950(13) 0.68099(12) 0.1012(10) Uani 1 1 d . . . Cl2 Cl 0.16275(16) 0.50824(11) 0.68846(10) 0.0627(6) Uani 1 1 d . . . Cl3 Cl 0.2858(3) 0.3952(2) 0.74896(16) 0.1335(14) Uani 1 1 d . . . Cl4 Cl 0.49247(13) 0.08172(10) 0.75897(8) 0.0512(4) Uani 1 1 d . . . Cl5 Cl 0.43872(18) 0.21165(12) 0.67904(10) 0.0724(7) Uani 1 1 d . . . Cl6 Cl 0.51715(15) 0.22428(11) 0.76738(8) 0.0549(5) Uani 1 1 d . . . Cl7 Cl 0.78329(16) 0.21457(15) 0.59657(8) 0.0708(6) Uani 1 1 d . . . Cl8 Cl 0.99207(18) 0.20110(12) 0.59698(11) 0.0715(6) Uani 1 1 d . . . Cl9 Cl 0.8718(2) 0.34509(11) 0.58173(9) 0.0732(7) Uani 1 1 d . . . Cl10 Cl 0.90439(18) 0.93347(14) 0.89409(13) 0.0863(8) Uani 1 1 d . . . Cl11 Cl 0.9831(2) 1.06309(16) 0.88859(11) 0.0892(8) Uani 1 1 d . . . Cl12 Cl 0.8543(2) 1.00190(16) 0.98517(9) 0.0923(9) Uani 1 1 d . . . N7 N 0.5972(3) 0.0950(3) 0.29734(19) 0.0276(10) Uani 1 1 d . . . N8 N 0.4282(3) -0.1050(3) 0.4114(2) 0.0280(10) Uani 1 1 d . . . N9 N 0.6662(4) -0.0280(3) 0.48278(19) 0.0311(11) Uani 1 1 d . . . N10 N 1.2325(3) 0.5005(3) 0.06348(19) 0.0285(11) Uani 1 1 d . . . N11 N 1.5191(4) 0.6262(3) -0.01390(19) 0.0277(10) Uani 1 1 d . . . N12 N 1.5231(4) 0.4391(3) 0.1531(2) 0.0420(14) Uani 1 1 d D . . O1 O 0.8595(3) 0.3682(2) 0.44984(15) 0.0257(8) Uani 1 1 d D . . H1A H 0.917(2) 0.364(4) 0.432(2) 0.038 Uiso 1 1 d D . . O2 O 0.9103(3) 0.28913(19) 0.31884(13) 0.0187(7) Uani 1 1 d D . . H2A H 0.860(3) 0.289(3) 0.3431(17) 0.028 Uiso 1 1 d D . . O3 O 1.0348(2) 0.34163(18) 0.37685(13) 0.0186(7) Uani 1 1 d . . . O4 O 0.9993(3) 0.1998(2) 0.45339(15) 0.0245(8) Uani 1 1 d . . . O5 O 0.7346(2) 0.30207(18) 0.40120(13) 0.0171(7) Uani 1 1 d . . . O6 O 0.8543(2) 0.16884(18) 0.41140(13) 0.0189(7) Uani 1 1 d . . . O7 O 1.3114(3) 0.01893(19) 0.18463(14) 0.0221(8) Uani 1 1 d D . . H7A H 1.333(4) 0.056(2) 0.164(2) 0.033 Uiso 1 1 d D . . O8 O 1.1347(3) 0.2011(2) 0.20557(14) 0.0203(7) Uani 1 1 d D . . H8G H 1.135(5) 0.168(2) 0.2331(14) 0.030 Uiso 1 1 d D . . O9 O 1.1529(2) 0.04743(19) 0.27289(14) 0.0194(7) Uani 1 1 d . . . O10 O 1.2970(3) 0.1214(2) 0.28736(14) 0.0243(8) Uani 1 1 d . . . O11 O 1.3287(3) 0.16564(19) 0.12728(13) 0.0188(7) Uani 1 1 d . . . O12 O 1.3471(3) 0.23838(19) 0.20917(13) 0.0206(7) Uani 1 1 d . . . O13 O 0.7012(3) 0.0802(2) 0.38572(15) 0.0297(9) Uani 1 1 d . C . O15 O 0.5624(4) 0.0877(3) 0.26202(18) 0.0487(12) Uani 1 1 d . C . O16 O 0.3756(3) -0.0923(2) 0.37745(19) 0.0390(10) Uani 1 1 d . C . O17 O 0.4248(3) -0.1577(2) 0.45039(17) 0.0381(10) Uani 1 1 d . C . O18 O 0.6892(4) -0.0920(3) 0.5072(2) 0.0566(14) Uani 1 1 d . C . O19 O 0.6819(3) 0.0251(3) 0.49450(17) 0.0404(11) Uani 1 1 d . C . O20 O 1.3396(3) 0.4129(2) 0.14886(14) 0.0275(8) Uani 1 1 d . . . O21 O 1.1754(3) 0.4760(2) 0.10517(17) 0.0359(10) Uani 1 1 d . . . O22 O 1.2121(4) 0.5177(3) 0.0189(2) 0.0641(17) Uani 1 1 d . . . O23 O 1.4743(3) 0.6609(2) -0.05051(16) 0.0344(10) Uani 1 1 d . . . O24 O 1.6024(3) 0.6355(2) -0.01233(18) 0.0383(10) Uani 1 1 d . . . O14 O 0.626(2) 0.1537(13) 0.2950(11) 0.048(7) Uani 0.59(6) 1 d P C 1 O25 O 1.6049(8) 0.3996(6) 0.1392(4) 0.068(3) Uani 0.574(13) 1 d PD D 1 O26 O 1.4846(8) 0.4419(6) 0.1979(4) 0.068(3) Uani 0.574(13) 1 d PD D 1 S1 S 1.02403(9) 0.46088(7) 0.43412(5) 0.0212(3) Uani 1 1 d . . . S2 S 1.09909(9) 0.33534(6) 0.25580(5) 0.0153(2) Uani 1 1 d . . . S3 S 0.70003(9) 0.31107(7) 0.28985(5) 0.0165(2) Uani 1 1 d . C . S4 S 0.63889(9) 0.39865(7) 0.48443(5) 0.0210(3) Uani 1 1 d . C . S5 S 1.23192(9) -0.11811(6) 0.25340(5) 0.0170(2) Uani 1 1 d . . . S6 S 0.95655(9) 0.13680(7) 0.28064(5) 0.0169(2) Uani 1 1 d . C . S7 S 1.16269(9) 0.29544(7) 0.09275(5) 0.0177(2) Uani 1 1 d . C . S8 S 1.45042(9) 0.04464(7) 0.07310(5) 0.0194(3) Uani 1 1 d . C . O14' O 0.675(3) 0.123(2) 0.2819(5) 0.034(8) Uani 0.41(6) 1 d P C 2 O25' O 1.5477(10) 0.4753(7) 0.1795(5) 0.057(4) Uani 0.426(13) 1 d PDU D 2 O26' O 1.5380(12) 0.3735(6) 0.1635(6) 0.075(6) Uani 0.426(13) 1 d PD D 2 C9' C 0.7536(10) 0.6735(10) 0.5222(6) 0.0568(12) Uani 0.456(7) 1 d PD A 2 H9'1 H 0.7406 0.7260 0.5229 0.085 Uiso 0.456(7) 1 calc PR A 2 H9'2 H 0.8262 0.6562 0.5142 0.085 Uiso 0.456(7) 1 calc PR A 2 H9'3 H 0.7238 0.6451 0.5576 0.085 Uiso 0.456(7) 1 calc PR A 2 C8' C 0.5919(6) 0.6792(9) 0.5007(6) 0.0568(12) Uani 0.456(7) 1 d PD A 2 H8'1 H 0.5750 0.6458 0.5360 0.085 Uiso 0.456(7) 1 calc PR A 2 H8'2 H 0.5552 0.6720 0.4757 0.085 Uiso 0.456(7) 1 calc PR A 2 H8'3 H 0.5734 0.7305 0.5048 0.085 Uiso 0.456(7) 1 calc PR A 2 C10' C 0.7341(11) 0.7252(7) 0.4346(5) 0.0568(12) Uani 0.456(7) 1 d PDU A 2 H10F H 0.7068 0.7710 0.4476 0.085 Uiso 0.456(7) 1 calc PR A 2 H10G H 0.7069 0.7270 0.4033 0.085 Uiso 0.456(7) 1 calc PR A 2 H10H H 0.8075 0.7199 0.4241 0.085 Uiso 0.456(7) 1 calc PR A 2 C78' C 0.7931(14) 0.1494(6) 0.1051(8) 0.0568(12) Uani 0.373(8) 1 d PDU B 2 H78D H 0.7369 0.1538 0.0878 0.085 Uiso 0.373(8) 1 calc PR B 2 H78E H 0.7757 0.1249 0.1434 0.085 Uiso 0.373(8) 1 calc PR B 2 H78F H 0.8528 0.1200 0.0871 0.085 Uiso 0.373(8) 1 calc PR B 2 C79' C 0.7181(11) 0.2685(9) 0.1301(7) 0.0568(12) Uani 0.373(8) 1 d PD B 2 H79D H 0.6633 0.2748 0.1114 0.085 Uiso 0.373(8) 1 calc PR B 2 H79E H 0.7308 0.3172 0.1300 0.085 Uiso 0.373(8) 1 calc PR B 2 H79F H 0.6995 0.2411 0.1676 0.085 Uiso 0.373(8) 1 calc PR B 2 C80' C 0.8321(14) 0.2663(9) 0.0419(4) 0.0568(12) Uani 0.373(8) 1 d PD B 2 H80D H 0.8930 0.2411 0.0214 0.085 Uiso 0.373(8) 1 calc PR B 2 H80E H 0.8402 0.3169 0.0397 0.085 Uiso 0.373(8) 1 calc PR B 2 H80F H 0.7746 0.2676 0.0265 0.085 Uiso 0.373(8) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01901(19) 0.0188(2) 0.0209(2) -0.00333(15) -0.00033(15) -0.00600(15) Ag2 0.01846(19) 0.0216(2) 0.0229(2) -0.00368(15) -0.00262(15) -0.00539(15) C1 0.025(3) 0.018(3) 0.015(2) -0.0070(19) -0.002(2) -0.004(2) C2 0.025(3) 0.022(3) 0.014(2) -0.0034(19) -0.004(2) -0.010(2) C3 0.020(3) 0.029(3) 0.021(3) -0.008(2) -0.006(2) -0.005(2) C4 0.029(3) 0.020(3) 0.026(3) -0.006(2) -0.010(2) -0.006(2) C5 0.026(3) 0.021(3) 0.020(3) -0.006(2) -0.008(2) -0.006(2) C6 0.021(3) 0.030(3) 0.014(2) -0.002(2) -0.006(2) -0.005(2) C7 0.031(3) 0.023(3) 0.048(4) -0.012(3) -0.005(3) -0.002(2) C8 0.052(2) 0.055(3) 0.070(3) -0.017(2) -0.024(2) -0.006(2) C9 0.052(2) 0.055(3) 0.070(3) -0.017(2) -0.024(2) -0.006(2) C10 0.052(2) 0.055(3) 0.070(3) -0.017(2) -0.024(2) -0.006(2) C11 0.010(2) 0.017(2) 0.024(3) -0.0045(19) -0.0037(19) -0.0013(19) C12 0.012(2) 0.020(3) 0.019(2) -0.0066(19) -0.0020(18) -0.0021(19) C13 0.019(2) 0.017(3) 0.025(3) -0.008(2) -0.006(2) -0.003(2) C14 0.019(3) 0.019(3) 0.028(3) -0.003(2) -0.004(2) -0.004(2) C15 0.017(2) 0.023(3) 0.020(3) -0.002(2) -0.006(2) -0.002(2) C16 0.014(2) 0.017(2) 0.020(2) -0.0067(19) -0.0009(19) -0.0060(19) C17 0.031(3) 0.022(3) 0.028(3) -0.003(2) -0.008(2) -0.011(2) C18 0.067(5) 0.029(3) 0.050(4) 0.012(3) -0.033(4) -0.014(3) C19 0.051(4) 0.025(3) 0.043(4) -0.006(3) 0.013(3) -0.018(3) C20 0.052(4) 0.018(3) 0.038(3) 0.001(2) -0.006(3) -0.017(3) C21 0.015(2) 0.014(2) 0.013(2) -0.0051(18) -0.0007(18) -0.0046(19) C22 0.013(2) 0.017(2) 0.019(2) -0.0039(19) -0.0049(19) -0.0028(19) C23 0.017(2) 0.020(3) 0.017(2) -0.0039(19) 0.0004(19) -0.007(2) C24 0.016(2) 0.016(2) 0.019(2) -0.0051(19) -0.0019(19) -0.0008(19) C25 0.019(2) 0.019(3) 0.020(2) -0.003(2) -0.006(2) -0.006(2) C26 0.015(2) 0.012(2) 0.020(2) -0.0085(18) 0.0009(19) -0.0004(19) C27 0.020(3) 0.032(3) 0.020(3) 0.007(2) -0.006(2) -0.007(2) C28 0.0451(16) 0.0421(16) 0.0489(17) 0.0010(13) -0.0177(13) 0.0036(13) C29 0.0451(16) 0.0421(16) 0.0489(17) 0.0010(13) -0.0177(13) 0.0036(13) C30 0.0451(16) 0.0421(16) 0.0489(17) 0.0010(13) -0.0177(13) 0.0036(13) C31 0.011(2) 0.016(2) 0.018(2) -0.0017(19) 0.0014(18) -0.0050(19) C32 0.016(2) 0.014(2) 0.024(3) -0.0050(19) -0.0014(19) -0.0057(19) C33 0.022(3) 0.018(3) 0.023(3) -0.002(2) -0.005(2) -0.008(2) C34 0.019(3) 0.022(3) 0.032(3) -0.008(2) -0.005(2) -0.001(2) C35 0.020(3) 0.023(3) 0.028(3) -0.009(2) 0.001(2) -0.003(2) C36 0.017(2) 0.023(3) 0.019(2) -0.003(2) -0.0004(19) -0.007(2) C37 0.035(3) 0.026(3) 0.039(3) -0.008(3) -0.012(3) 0.005(3) C38 0.0451(16) 0.0421(16) 0.0489(17) 0.0010(13) -0.0177(13) 0.0036(13) C39 0.0451(16) 0.0421(16) 0.0489(17) 0.0010(13) -0.0177(13) 0.0036(13) C40 0.0451(16) 0.0421(16) 0.0489(17) 0.0010(13) -0.0177(13) 0.0036(13) C41 0.023(3) 0.020(3) 0.027(3) 0.005(2) 0.001(2) -0.001(2) C42 0.029(3) 0.022(3) 0.027(3) 0.002(2) -0.013(2) -0.010(2) C43 0.023(3) 0.022(3) 0.012(2) 0.0035(19) 0.0004(19) -0.008(2) C44 0.022(3) 0.017(3) 0.016(2) 0.0010(19) 0.001(2) -0.004(2) C45 0.032(3) 0.021(3) 0.020(3) -0.001(2) -0.002(2) -0.008(2) C46 0.034(3) 0.020(3) 0.020(3) -0.002(2) 0.005(2) -0.003(2) C47 0.026(3) 0.021(3) 0.021(3) 0.002(2) 0.004(2) 0.002(2) C48 0.018(3) 0.033(3) 0.019(3) 0.001(2) -0.002(2) -0.005(2) C49 0.024(3) 0.020(3) 0.015(2) -0.0015(19) 0.000(2) -0.001(2) C50 0.018(2) 0.018(3) 0.019(2) -0.0019(19) -0.0008(19) -0.004(2) C51 0.022(2) 0.010(2) 0.019(2) -0.0053(18) -0.007(2) 0.0021(19) C52 0.017(2) 0.022(3) 0.019(2) -0.002(2) -0.0023(19) -0.004(2) C53 0.022(3) 0.022(3) 0.019(3) -0.006(2) 0.002(2) -0.006(2) C54 0.021(3) 0.023(3) 0.021(3) -0.009(2) 0.000(2) -0.005(2) C55 0.020(3) 0.013(2) 0.026(3) -0.004(2) 0.001(2) -0.006(2) C56 0.015(2) 0.016(2) 0.018(2) -0.0029(19) 0.0001(19) -0.0024(19) C57 0.038(3) 0.028(3) 0.027(3) -0.010(2) 0.002(2) -0.016(3) C58 0.059(4) 0.040(4) 0.029(3) -0.023(3) 0.016(3) -0.025(3) C59 0.046(4) 0.027(3) 0.045(4) -0.017(3) -0.003(3) -0.004(3) C60 0.046(4) 0.032(3) 0.034(3) -0.011(3) -0.001(3) -0.020(3) C61 0.019(2) 0.016(2) 0.014(2) -0.0011(18) -0.0014(19) -0.007(2) C62 0.019(2) 0.019(3) 0.016(2) -0.0059(19) 0.0000(19) -0.002(2) C63 0.023(3) 0.014(2) 0.024(3) -0.006(2) 0.000(2) -0.006(2) C64 0.023(3) 0.023(3) 0.025(3) -0.004(2) -0.002(2) -0.012(2) C65 0.018(2) 0.020(3) 0.025(3) -0.005(2) -0.003(2) -0.003(2) C66 0.019(2) 0.012(2) 0.015(2) -0.0014(18) -0.0015(19) -0.0018(19) C67 0.018(3) 0.019(3) 0.059(4) -0.015(3) -0.006(3) -0.008(2) C68 0.030(3) 0.030(4) 0.101(6) -0.030(4) -0.014(4) -0.007(3) C69 0.027(3) 0.047(4) 0.071(5) -0.030(4) -0.021(3) -0.003(3) C70 0.027(3) 0.046(4) 0.061(5) -0.012(3) 0.007(3) -0.018(3) C71 0.019(2) 0.018(3) 0.018(2) -0.0062(19) -0.0029(19) -0.008(2) C72 0.020(2) 0.014(2) 0.018(2) -0.0043(19) -0.0024(19) -0.001(2) C73 0.017(2) 0.019(3) 0.024(3) -0.003(2) -0.004(2) -0.005(2) C74 0.025(3) 0.025(3) 0.027(3) -0.006(2) -0.009(2) -0.006(2) C75 0.024(3) 0.022(3) 0.017(2) 0.000(2) -0.004(2) -0.004(2) C76 0.018(2) 0.012(2) 0.020(2) -0.0030(19) 0.0010(19) -0.0027(19) C77 0.027(3) 0.041(3) 0.035(3) -0.001(3) -0.016(2) -0.007(3) C78 0.052(2) 0.055(3) 0.070(3) -0.017(2) -0.024(2) -0.006(2) C79 0.052(2) 0.055(3) 0.070(3) -0.017(2) -0.024(2) -0.006(2) C80 0.052(2) 0.055(3) 0.070(3) -0.017(2) -0.024(2) -0.006(2) C81 0.020(2) 0.015(2) 0.015(2) -0.0026(18) 0.0016(19) -0.008(2) C82 0.017(2) 0.014(2) 0.019(2) -0.0029(19) -0.0006(19) -0.0057(19) C83 0.024(3) 0.013(2) 0.020(3) -0.0020(19) -0.005(2) -0.001(2) C84 0.027(3) 0.028(3) 0.018(3) -0.006(2) -0.003(2) -0.006(2) C85 0.025(3) 0.021(3) 0.021(3) -0.007(2) 0.003(2) -0.008(2) C86 0.019(2) 0.014(2) 0.015(2) 0.0002(18) -0.0015(19) -0.0075(19) C87 0.044(4) 0.035(3) 0.023(3) -0.007(2) -0.011(3) -0.003(3) C88 0.085(6) 0.047(4) 0.026(3) -0.018(3) -0.022(3) 0.005(4) C89 0.073(5) 0.052(4) 0.017(3) 0.000(3) -0.005(3) -0.005(4) C90 0.051(4) 0.060(5) 0.041(4) -0.020(3) -0.022(3) -0.003(4) C91 0.017(2) 0.017(2) 0.016(2) -0.0026(19) -0.0006(19) -0.0006(19) C92 0.022(3) 0.022(3) 0.021(3) -0.006(2) 0.001(2) -0.008(2) C93 0.017(2) 0.024(3) 0.020(3) -0.007(2) -0.004(2) -0.003(2) C94 0.018(2) 0.018(3) 0.019(2) -0.0055(19) -0.0023(19) 0.000(2) C95 0.045(4) 0.028(3) 0.029(3) -0.004(2) -0.005(3) -0.019(3) C96 0.048(4) 0.041(4) 0.035(3) -0.014(3) -0.007(3) -0.023(3) C97 0.032(3) 0.035(3) 0.026(3) -0.014(2) -0.012(2) -0.001(3) C98 0.027(3) 0.022(3) 0.025(3) -0.005(2) -0.007(2) -0.002(2) C99 0.019(3) 0.032(3) 0.020(3) -0.007(2) -0.003(2) -0.008(2) C100 0.018(2) 0.026(3) 0.016(2) -0.003(2) 0.0008(19) -0.008(2) C101 0.017(2) 0.021(3) 0.022(3) -0.003(2) 0.000(2) -0.003(2) C102 0.020(3) 0.021(3) 0.020(3) 0.004(2) -0.001(2) -0.010(2) C103 0.018(3) 0.025(3) 0.030(3) -0.006(2) -0.007(2) -0.007(2) C104 0.015(2) 0.019(3) 0.032(3) -0.001(2) -0.003(2) -0.008(2) C105 0.024(3) 0.019(3) 0.028(3) 0.000(2) -0.001(2) -0.006(2) C106 0.024(3) 0.028(3) 0.019(3) -0.001(2) -0.007(2) -0.006(2) C107 0.019(2) 0.020(3) 0.024(3) -0.008(2) -0.005(2) -0.002(2) C108 0.018(2) 0.020(3) 0.022(3) -0.002(2) -0.003(2) -0.008(2) C109 0.026(3) 0.015(2) 0.019(2) -0.0048(19) -0.004(2) -0.003(2) C110 0.021(3) 0.013(2) 0.022(3) -0.008(2) 0.005(2) -0.004(2) C111 0.025(3) 0.026(3) 0.031(3) -0.007(2) -0.006(2) -0.014(2) C112 0.024(3) 0.030(3) 0.025(3) 0.000(2) -0.012(2) -0.012(2) C113 0.064(5) 0.048(5) 0.067(6) 0.008(4) 0.021(4) 0.011(4) C114 0.032(3) 0.043(4) 0.051(4) -0.012(3) -0.017(3) -0.007(3) C115 0.051(4) 0.036(4) 0.030(3) -0.006(3) -0.007(3) -0.011(3) C116 0.035(3) 0.032(3) 0.050(4) -0.012(3) -0.016(3) 0.000(3) Cl1 0.174(3) 0.0435(13) 0.0879(18) -0.0208(12) -0.0256(19) -0.0160(16) Cl2 0.0681(13) 0.0441(11) 0.0912(15) -0.0304(10) -0.0423(12) 0.0076(9) Cl3 0.112(3) 0.139(3) 0.135(3) 0.031(2) -0.082(2) -0.001(2) Cl4 0.0400(9) 0.0440(10) 0.0663(12) -0.0117(8) -0.0064(8) -0.0063(8) Cl5 0.0765(14) 0.0583(13) 0.0999(17) -0.0120(12) -0.0643(14) -0.0003(11) Cl6 0.0557(11) 0.0522(11) 0.0642(12) -0.0253(9) -0.0224(9) 0.0020(9) Cl7 0.0591(12) 0.1104(19) 0.0418(10) -0.0119(11) 0.0079(9) -0.0395(13) Cl8 0.0738(14) 0.0481(12) 0.1036(18) -0.0127(11) -0.0492(13) -0.0025(10) Cl9 0.131(2) 0.0409(11) 0.0557(12) -0.0187(9) -0.0409(13) 0.0043(12) Cl10 0.0626(14) 0.0658(15) 0.148(2) -0.0612(16) -0.0321(15) 0.0112(11) Cl11 0.0769(16) 0.0911(18) 0.0951(19) -0.0169(15) 0.0159(14) -0.0483(14) Cl12 0.133(2) 0.0951(19) 0.0466(12) 0.0059(12) -0.0128(14) -0.0478(18) N7 0.026(2) 0.026(3) 0.029(3) 0.0088(19) -0.010(2) -0.012(2) N8 0.022(2) 0.024(2) 0.037(3) -0.003(2) -0.005(2) -0.008(2) N9 0.032(3) 0.041(3) 0.022(2) 0.001(2) -0.008(2) -0.018(2) N10 0.022(2) 0.031(3) 0.031(3) 0.000(2) -0.010(2) -0.006(2) N11 0.031(3) 0.023(2) 0.027(2) -0.005(2) 0.005(2) -0.013(2) N12 0.036(3) 0.051(4) 0.040(3) 0.008(3) -0.014(3) -0.024(3) O1 0.0218(19) 0.028(2) 0.028(2) -0.0108(16) 0.0019(16) -0.0065(17) O2 0.0201(18) 0.0162(17) 0.0158(17) 0.0022(14) -0.0010(14) -0.0054(14) O3 0.0172(17) 0.0150(17) 0.0222(18) -0.0012(14) -0.0032(14) -0.0043(14) O4 0.0223(19) 0.024(2) 0.026(2) -0.0069(15) -0.0010(15) -0.0055(15) O5 0.0148(16) 0.0191(18) 0.0159(17) -0.0006(13) -0.0023(13) -0.0045(14) O6 0.0192(17) 0.0169(18) 0.0170(17) -0.0020(13) -0.0041(14) 0.0028(14) O7 0.034(2) 0.0136(18) 0.0171(18) -0.0030(14) 0.0028(15) -0.0094(16) O8 0.0199(18) 0.0228(19) 0.0167(18) 0.0029(14) -0.0047(14) -0.0083(15) O9 0.0174(17) 0.0179(18) 0.0232(18) -0.0004(14) -0.0062(14) -0.0064(14) O10 0.034(2) 0.025(2) 0.0170(18) -0.0069(15) 0.0011(15) -0.0170(17) O11 0.0216(18) 0.0226(19) 0.0130(16) -0.0035(14) -0.0014(14) -0.0087(15) O12 0.0229(18) 0.0219(19) 0.0155(17) -0.0035(14) -0.0025(14) -0.0036(15) O13 0.030(2) 0.031(2) 0.029(2) 0.0042(17) -0.0080(17) -0.0187(18) O15 0.057(3) 0.059(3) 0.033(2) 0.011(2) -0.022(2) -0.029(3) O16 0.030(2) 0.039(3) 0.054(3) 0.000(2) -0.020(2) -0.0149(19) O17 0.042(2) 0.033(2) 0.037(2) 0.0064(19) -0.0074(19) -0.021(2) O18 0.075(4) 0.050(3) 0.052(3) 0.019(2) -0.040(3) -0.028(3) O19 0.046(3) 0.053(3) 0.031(2) -0.013(2) -0.008(2) -0.022(2) O20 0.029(2) 0.031(2) 0.0221(19) 0.0050(16) -0.0069(16) -0.0160(17) O21 0.0177(19) 0.042(3) 0.038(2) 0.0097(19) -0.0013(17) -0.0114(18) O22 0.052(3) 0.104(5) 0.042(3) 0.018(3) -0.031(2) -0.042(3) O23 0.041(2) 0.029(2) 0.028(2) 0.0044(17) -0.0024(18) -0.0146(19) O24 0.029(2) 0.033(2) 0.051(3) -0.003(2) -0.0001(19) -0.0180(19) O14 0.052(12) 0.036(8) 0.058(9) 0.028(7) -0.035(10) -0.029(9) O25 0.085(6) 0.062(5) 0.062(5) 0.006(4) -0.039(4) -0.019(5) O26 0.085(6) 0.062(5) 0.062(5) 0.006(4) -0.039(4) -0.019(5) S1 0.0204(6) 0.0279(7) 0.0186(6) -0.0077(5) -0.0058(5) -0.0057(5) S2 0.0149(6) 0.0141(6) 0.0164(6) -0.0029(4) -0.0025(4) -0.0031(5) S3 0.0160(6) 0.0163(6) 0.0181(6) -0.0038(5) -0.0021(5) -0.0063(5) S4 0.0211(6) 0.0244(7) 0.0191(6) -0.0062(5) -0.0010(5) -0.0087(5) S5 0.0164(6) 0.0139(6) 0.0166(6) -0.0005(4) 0.0001(4) -0.0022(5) S6 0.0177(6) 0.0143(6) 0.0174(6) -0.0040(4) -0.0005(5) -0.0032(5) S7 0.0205(6) 0.0139(6) 0.0169(6) -0.0019(4) -0.0016(5) -0.0039(5) S8 0.0184(6) 0.0170(6) 0.0197(6) -0.0025(5) 0.0013(5) -0.0047(5) O14' 0.039(14) 0.046(14) 0.023(6) 0.002(6) -0.007(6) -0.032(12) O25' 0.060(7) 0.085(8) 0.036(6) -0.013(5) -0.025(5) -0.015(6) O26' 0.075(11) 0.045(8) 0.096(12) 0.038(8) -0.053(9) -0.011(7) C9' 0.052(2) 0.055(3) 0.070(3) -0.017(2) -0.024(2) -0.006(2) C8' 0.052(2) 0.055(3) 0.070(3) -0.017(2) -0.024(2) -0.006(2) C10' 0.052(2) 0.055(3) 0.070(3) -0.017(2) -0.024(2) -0.006(2) C78' 0.052(2) 0.055(3) 0.070(3) -0.017(2) -0.024(2) -0.006(2) C79' 0.052(2) 0.055(3) 0.070(3) -0.017(2) -0.024(2) -0.006(2) C80' 0.052(2) 0.055(3) 0.070(3) -0.017(2) -0.024(2) -0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 O13 2.308(4) . ? Ag1 O14' 2.540(12) . ? Ag1 S6 2.5476(12) . ? Ag1 S3 2.5747(13) . ? Ag1 O14 2.587(10) . ? Ag2 O20 2.318(4) . ? Ag2 O12 2.480(3) . ? Ag2 S7 2.5762(13) . ? Ag2 S2 2.5960(12) . ? C1 O1 1.345(6) . ? C1 C2 1.394(7) . ? C1 C6 1.408(7) . ? C2 C3 1.394(7) . ? C2 S4 1.776(5) . ? C3 C4 1.391(7) . ? C3 H3 0.9500 . ? C4 C5 1.385(7) . ? C4 C7 1.525(7) . ? C5 C6 1.388(7) . ? C5 H5 0.9500 . ? C6 S1 1.784(5) . ? C7 C9 1.448(7) . ? C7 C10' 1.455(8) . ? C7 C10 1.532(8) . ? C7 C8' 1.549(8) . ? C7 C9' 1.561(9) . ? C7 C8 1.558(8) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 O3 1.374(6) . ? C11 C12 1.395(7) . ? C11 C16 1.395(7) . ? C12 C13 1.390(7) . ? C12 S1 1.794(5) . ? C13 C14 1.388(7) . ? C13 H13 0.9500 . ? C14 C15 1.396(7) . ? C14 C17 1.527(7) . ? C15 C16 1.385(7) . ? C15 H15 0.9500 . ? C16 S2 1.800(5) . ? C17 C18 1.520(8) . ? C17 C19 1.533(8) . ? C17 C20 1.534(8) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 O2 1.345(6) . ? C21 C26 1.403(7) . ? C21 C22 1.409(6) . ? C22 C23 1.371(7) . ? C22 S2 1.794(5) . ? C23 C24 1.396(7) . ? C23 H23 0.9500 . ? C24 C25 1.384(7) . ? C24 C27 1.543(7) . ? C25 C26 1.391(7) . ? C25 H25 0.9500 . ? C26 S3 1.782(5) . ? C27 C29 1.514(8) . ? C27 C28 1.528(9) . ? C27 C30 1.529(9) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 O5 1.367(6) . ? C31 C32 1.394(7) . ? C31 C36 1.401(7) . ? C32 C33 1.388(7) . ? C32 S3 1.808(5) . ? C33 C34 1.383(7) . ? C33 H33 0.9500 . ? C34 C35 1.400(8) . ? C34 C37 1.533(8) . ? C35 C36 1.391(7) . ? C35 H35 0.9500 . ? C36 S4 1.794(5) . ? C37 C40 1.525(9) . ? C37 C39 1.515(9) . ? C37 C38 1.521(9) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 O3 1.439(6) . ? C41 C42 1.502(7) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 O4 1.440(6) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C48 1.385(7) . ? C43 C44 1.396(7) . ? C43 O4 1.384(6) . ? C44 C45 1.385(7) . ? C44 O6 1.386(6) . ? C45 C46 1.388(8) . ? C45 H45 0.9500 . ? C46 C47 1.383(8) . ? C46 H46 0.9500 . ? C47 C48 1.385(8) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 O6 1.437(6) . ? C49 C50 1.489(7) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 O5 1.444(6) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 O7 1.341(6) . ? C51 C52 1.399(7) . ? C51 C56 1.419(7) . ? C52 C53 1.385(7) . ? C52 S8 1.778(5) . ? C53 C54 1.388(7) . ? C53 H53 0.9500 . ? C54 C55 1.390(7) . ? C54 C57 1.535(7) . ? C55 C56 1.380(7) . ? C55 H55 0.9500 . ? C56 S5 1.778(5) . ? C57 C60 1.527(8) . ? C57 C59 1.527(9) . ? C57 C58 1.528(8) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 O9 1.366(6) . ? C61 C62 1.395(7) . ? C61 C66 1.402(7) . ? C62 C63 1.398(7) . ? C62 S5 1.786(5) . ? C63 C64 1.384(7) . ? C63 H63 0.9500 . ? C64 C65 1.396(7) . ? C64 C67 1.535(7) . ? C65 C66 1.373(7) . ? C65 H65 0.9500 . ? C66 S6 1.792(5) . ? C67 C68 1.530(8) . ? C67 C70 1.531(9) . ? C67 C69 1.534(9) . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 O8 1.347(6) . ? C71 C76 1.392(7) . ? C71 C72 1.408(7) . ? C72 C73 1.389(7) . ? C72 S6 1.787(5) . ? C73 C74 1.391(7) . ? C73 H73 0.9500 . ? C74 C75 1.395(7) . ? C74 C77 1.521(7) . ? C75 C76 1.390(7) . ? C75 H75 0.9500 . ? C76 S7 1.791(5) . ? C77 C78' 1.501(8) . ? C77 C78 1.511(7) . ? C77 C80' 1.511(9) . ? C77 C80 1.521(7) . ? C77 C79 1.561(8) . ? C77 C79' 1.552(8) . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 O11 1.379(6) . ? C81 C82 1.390(7) . ? C81 C86 1.390(7) . ? C82 C83 1.387(7) . ? C82 S7 1.799(5) . ? C83 C84 1.399(7) . ? C83 H83 0.9500 . ? C84 C85 1.386(8) . ? C84 C87 1.541(7) . ? C85 C86 1.398(7) . ? C85 H85 0.9500 . ? C86 S8 1.784(5) . ? C87 C88 1.530(9) . ? C87 C89 1.531(9) . ? C87 C90 1.541(9) . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? C89 H89A 0.9800 . ? C89 H89B 0.9800 . ? C89 H89C 0.9800 . ? C90 H90A 0.9800 . ? C90 H90B 0.9800 . ? C90 H90C 0.9800 . ? C91 O9 1.438(6) . ? C91 C92 1.498(7) . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? C92 O10 1.423(6) . ? C92 H92A 0.9900 . ? C92 H92B 0.9900 . ? C93 O10 1.370(6) . ? C93 C94 1.397(7) . ? C93 C98 1.394(7) . ? C94 C95 1.373(7) . ? C94 O12 1.387(6) . ? C95 C96 1.381(8) . ? C95 H95 0.9500 . ? C96 C97 1.378(9) . ? C96 H96 0.9500 . ? C97 C98 1.386(8) . ? C97 H97 0.9500 . ? C98 H98 0.9500 . ? C99 O12 1.441(6) . ? C99 C100 1.507(7) . ? C99 H99A 0.9900 . ? C99 H99B 0.9900 . ? C100 O11 1.447(6) . ? C100 H10D 0.9900 . ? C100 H10E 0.9900 . ? C101 O13 1.247(6) . ? C101 C106 1.450(7) . ? C101 C102 1.452(7) . ? C102 C103 1.378(7) . ? C102 N7 1.457(6) . ? C103 C104 1.385(7) . ? C103 H103 0.9500 . ? C104 C105 1.388(8) . ? C104 N8 1.443(6) . ? C105 C106 1.363(7) . ? C105 H105 0.9500 . ? C106 N9 1.469(7) . ? C107 O20 1.253(6) . ? C107 C108 1.448(7) . ? C107 C112 1.447(7) . ? C108 C109 1.378(7) . ? C108 N10 1.455(6) . ? C109 C110 1.381(7) . ? C109 H109 0.9500 . ? C110 C111 1.384(8) . ? C110 N11 1.445(6) . ? C111 C112 1.356(7) . ? C111 H111 0.9500 . ? C112 N12 1.455(7) . ? C113 Cl2 1.721(8) . ? C113 Cl1 1.767(11) . ? C113 Cl3 1.758(10) . ? C113 H113 1.0000 . ? C114 Cl4 1.743(7) . ? C114 Cl6 1.752(7) . ? C114 Cl5 1.759(7) . ? C114 H114 1.0000 . ? C115 Cl9 1.750(7) . ? C115 Cl7 1.747(7) . ? C115 Cl8 1.747(7) . ? C115 H115 1.0000 . ? C116 Cl11 1.727(7) . ? C116 Cl10 1.735(7) . ? C116 Cl12 1.734(7) . ? C116 H116 1.0000 . ? N7 O15 1.200(6) . ? N7 O14' 1.251(18) . ? N7 O14 1.254(16) . ? N8 O17 1.225(6) . ? N8 O16 1.237(6) . ? N9 O19 1.209(6) . ? N9 O18 1.230(7) . ? N10 O22 1.215(6) . ? N10 O21 1.223(6) . ? N11 O24 1.228(6) . ? N11 O23 1.238(6) . ? N12 O26 1.171(9) . ? N12 O26' 1.186(10) . ? N12 O25' 1.247(10) . ? N12 O25 1.245(10) . ? O1 H1A 0.82(4) . ? O2 H2A 0.82(4) . ? O7 H7A 0.83(5) . ? O8 H8G 0.82(4) . ? C9' H9'1 0.9800 . ? C9' H9'2 0.9800 . ? C9' H9'3 0.9800 . ? C8' H8'1 0.9800 . ? C8' H8'2 0.9800 . ? C8' H8'3 0.9800 . ? C10' H10F 0.9800 . ? C10' H10G 0.9800 . ? C10' H10H 0.9800 . ? C78' H78D 0.9800 . ? C78' H78E 0.9800 . ? C78' H78F 0.9800 . ? C79' H79D 0.9800 . ? C79' H79E 0.9800 . ? C79' H79F 0.9800 . ? C80' H80D 0.9800 . ? C80' H80E 0.9800 . ? C80' H80F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O13 Ag1 O14' 67.9(4) . . ? O13 Ag1 S6 113.96(11) . . ? O14' Ag1 S6 103.2(9) . . ? O13 Ag1 S3 130.86(10) . . ? O14' Ag1 S3 93.7(9) . . ? S6 Ag1 S3 114.54(4) . . ? O13 Ag1 O14 68.0(2) . . ? O14' Ag1 O14 19.2(3) . . ? S6 Ag1 O14 121.4(9) . . ? S3 Ag1 O14 80.6(5) . . ? O20 Ag2 O12 85.76(12) . . ? O20 Ag2 S7 127.91(9) . . ? O12 Ag2 S7 114.67(9) . . ? O20 Ag2 S2 111.52(10) . . ? O12 Ag2 S2 90.84(8) . . ? S7 Ag2 S2 115.21(4) . . ? O1 C1 C2 118.1(4) . . ? O1 C1 C6 123.6(5) . . ? C2 C1 C6 118.3(5) . . ? C1 C2 C3 120.5(5) . . ? C1 C2 S4 120.7(4) . . ? C3 C2 S4 118.8(4) . . ? C4 C3 C2 121.5(5) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C5 C4 C3 117.6(5) . . ? C5 C4 C7 121.6(5) . . ? C3 C4 C7 120.7(5) . . ? C4 C5 C6 122.2(5) . . ? C4 C5 H5 118.9 . . ? C6 C5 H5 118.9 . . ? C5 C6 C1 119.9(5) . . ? C5 C6 S1 119.5(4) . . ? C1 C6 S1 120.3(4) . . ? C9 C7 C10' 124.9(8) . . ? C9 C7 C4 114.5(7) . . ? C10' C7 C4 119.5(7) . . ? C9 C7 C10 110.0(6) . . ? C10' C7 C10 39.3(7) . . ? C4 C7 C10 111.3(7) . . ? C9 C7 C8' 52.1(7) . . ? C10' C7 C8' 108.2(7) . . ? C4 C7 C8' 116.7(7) . . ? C10 C7 C8' 131.8(8) . . ? C9 C7 C9' 53.2(7) . . ? C10' C7 C9' 99.5(10) . . ? C4 C7 C9' 106.9(7) . . ? C10 C7 C9' 64.7(8) . . ? C8' C7 C9' 103.3(7) . . ? C9 C7 C8 108.3(6) . . ? C10' C7 C8 66.1(8) . . ? C4 C7 C8 107.0(6) . . ? C10 C7 C8 105.3(6) . . ? C8' C7 C8 57.5(7) . . ? C9' C7 C8 146.0(9) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? O3 C11 C12 118.5(4) . . ? O3 C11 C16 123.0(4) . . ? C12 C11 C16 118.3(4) . . ? C11 C12 C13 120.3(4) . . ? C11 C12 S1 120.8(4) . . ? C13 C12 S1 118.9(4) . . ? C14 C13 C12 121.8(5) . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C13 C14 C15 117.5(5) . . ? C13 C14 C17 123.9(5) . . ? C15 C14 C17 118.5(5) . . ? C16 C15 C14 121.3(5) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C15 C16 C11 120.8(4) . . ? C15 C16 S2 118.2(4) . . ? C11 C16 S2 120.9(4) . . ? C18 C17 C14 109.7(5) . . ? C18 C17 C19 109.4(5) . . ? C14 C17 C19 109.4(5) . . ? C18 C17 C20 108.7(5) . . ? C14 C17 C20 111.7(5) . . ? C19 C17 C20 107.9(5) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O2 C21 C26 125.2(4) . . ? O2 C21 C22 117.8(4) . . ? C26 C21 C22 116.9(4) . . ? C23 C22 C21 120.7(4) . . ? C23 C22 S2 120.9(4) . . ? C21 C22 S2 118.4(4) . . ? C22 C23 C24 122.7(4) . . ? C22 C23 H23 118.7 . . ? C24 C23 H23 118.7 . . ? C25 C24 C23 116.5(4) . . ? C25 C24 C27 123.2(4) . . ? C23 C24 C27 120.3(4) . . ? C24 C25 C26 122.2(5) . . ? C24 C25 H25 118.9 . . ? C26 C25 H25 118.9 . . ? C25 C26 C21 120.7(4) . . ? C25 C26 S3 118.0(4) . . ? C21 C26 S3 121.2(4) . . ? C29 C27 C28 109.0(5) . . ? C29 C27 C30 108.4(5) . . ? C28 C27 C30 108.7(5) . . ? C29 C27 C24 112.3(5) . . ? C28 C27 C24 109.8(5) . . ? C30 C27 C24 108.6(5) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O5 C31 C32 120.1(4) . . ? O5 C31 C36 121.6(4) . . ? C32 C31 C36 118.1(4) . . ? C33 C32 C31 121.4(5) . . ? C33 C32 S3 117.7(4) . . ? C31 C32 S3 120.8(4) . . ? C34 C33 C32 121.1(5) . . ? C34 C33 H33 119.4 . . ? C32 C33 H33 119.4 . . ? C33 C34 C35 117.5(5) . . ? C33 C34 C37 121.7(5) . . ? C35 C34 C37 120.7(5) . . ? C36 C35 C34 122.2(5) . . ? C36 C35 H35 118.9 . . ? C34 C35 H35 118.9 . . ? C35 C36 C31 119.7(5) . . ? C35 C36 S4 119.0(4) . . ? C31 C36 S4 121.3(4) . . ? C40 C37 C39 109.2(6) . . ? C40 C37 C38 105.9(5) . . ? C39 C37 C38 109.9(6) . . ? C40 C37 C34 111.5(5) . . ? C39 C37 C34 108.2(5) . . ? C38 C37 C34 112.0(5) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O3 C41 C42 108.9(4) . . ? O3 C41 H41A 109.9 . . ? C42 C41 H41A 109.9 . . ? O3 C41 H41B 109.9 . . ? C42 C41 H41B 109.9 . . ? H41A C41 H41B 108.3 . . ? O4 C42 C41 112.0(4) . . ? O4 C42 H42A 109.2 . . ? C41 C42 H42A 109.2 . . ? O4 C42 H42B 109.2 . . ? C41 C42 H42B 109.2 . . ? H42A C42 H42B 107.9 . . ? C48 C43 C44 118.8(5) . . ? C48 C43 O4 123.6(5) . . ? C44 C43 O4 117.5(4) . . ? C45 C44 O6 117.9(5) . . ? C45 C44 C43 120.1(5) . . ? O6 C44 C43 122.0(5) . . ? C44 C45 C46 120.5(5) . . ? C44 C45 H45 119.7 . . ? C46 C45 H45 119.7 . . ? C47 C46 C45 119.5(5) . . ? C47 C46 H46 120.2 . . ? C45 C46 H46 120.2 . . ? C46 C47 C48 120.0(5) . . ? C46 C47 H47 120.0 . . ? C48 C47 H47 120.0 . . ? C43 C48 C47 121.0(5) . . ? C43 C48 H48 119.5 . . ? C47 C48 H48 119.5 . . ? O6 C49 C50 107.3(4) . . ? O6 C49 H49A 110.3 . . ? C50 C49 H49A 110.3 . . ? O6 C49 H49B 110.3 . . ? C50 C49 H49B 110.3 . . ? H49A C49 H49B 108.5 . . ? O5 C50 C49 107.0(4) . . ? O5 C50 H50A 110.3 . . ? C49 C50 H50A 110.3 . . ? O5 C50 H50B 110.3 . . ? C49 C50 H50B 110.3 . . ? H50A C50 H50B 108.6 . . ? O7 C51 C52 124.2(4) . . ? O7 C51 C56 118.1(4) . . ? C52 C51 C56 117.7(4) . . ? C53 C52 C51 120.9(5) . . ? C53 C52 S8 120.0(4) . . ? C51 C52 S8 118.9(4) . . ? C52 C53 C54 121.8(5) . . ? C52 C53 H53 119.1 . . ? C54 C53 H53 119.1 . . ? C53 C54 C55 117.1(5) . . ? C53 C54 C57 123.2(4) . . ? C55 C54 C57 119.6(5) . . ? C56 C55 C54 122.8(5) . . ? C56 C55 H55 118.6 . . ? C54 C55 H55 118.6 . . ? C55 C56 C51 119.5(4) . . ? C55 C56 S5 118.3(4) . . ? C51 C56 S5 121.5(4) . . ? C60 C57 C59 110.2(5) . . ? C60 C57 C58 107.4(5) . . ? C59 C57 C58 109.0(5) . . ? C60 C57 C54 110.0(5) . . ? C59 C57 C54 107.8(5) . . ? C58 C57 C54 112.4(4) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C57 C59 H59A 109.5 . . ? C57 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C57 C60 H60A 109.5 . . ? C57 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C57 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? O9 C61 C62 126.0(4) . . ? O9 C61 C66 116.3(4) . . ? C62 C61 C66 117.7(4) . . ? C61 C62 C63 119.7(5) . . ? C61 C62 S5 124.3(4) . . ? C63 C62 S5 115.9(4) . . ? C64 C63 C62 122.7(5) . . ? C64 C63 H63 118.7 . . ? C62 C63 H63 118.7 . . ? C63 C64 C65 116.8(5) . . ? C63 C64 C67 123.9(5) . . ? C65 C64 C67 119.3(5) . . ? C66 C65 C64 121.7(5) . . ? C66 C65 H65 119.2 . . ? C64 C65 H65 119.2 . . ? C65 C66 C61 121.4(4) . . ? C65 C66 S6 120.3(4) . . ? C61 C66 S6 118.2(4) . . ? C68 C67 C64 111.4(5) . . ? C68 C67 C70 109.3(5) . . ? C64 C67 C70 108.0(5) . . ? C68 C67 C69 107.7(5) . . ? C64 C67 C69 110.4(5) . . ? C70 C67 C69 109.9(5) . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C67 C69 H69A 109.5 . . ? C67 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C67 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C67 C70 H70A 109.5 . . ? C67 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C67 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? O8 C71 C76 119.5(4) . . ? O8 C71 C72 123.0(4) . . ? C76 C71 C72 117.4(4) . . ? C73 C72 C71 120.2(4) . . ? C73 C72 S6 121.4(4) . . ? C71 C72 S6 118.4(4) . . ? C74 C73 C72 122.4(5) . . ? C74 C73 H73 118.8 . . ? C72 C73 H73 118.8 . . ? C73 C74 C75 116.7(5) . . ? C73 C74 C77 121.0(5) . . ? C75 C74 C77 122.3(5) . . ? C76 C75 C74 121.7(5) . . ? C76 C75 H75 119.1 . . ? C74 C75 H75 119.1 . . ? C75 C76 C71 121.2(4) . . ? C75 C76 S7 117.9(4) . . ? C71 C76 S7 121.0(4) . . ? C78' C77 C78 65.2(8) . . ? C78' C77 C80' 110.3(7) . . ? C78 C77 C80' 127.1(9) . . ? C78' C77 C74 112.6(8) . . ? C78 C77 C74 115.5(6) . . ? C80' C77 C74 114.1(8) . . ? C78' C77 C80 129.6(9) . . ? C78 C77 C80 109.0(6) . . ? C80' C77 C80 30.6(7) . . ? C74 C77 C80 114.1(6) . . ? C78' C77 C79 42.7(7) . . ? C78 C77 C79 105.9(6) . . ? C80' C77 C79 76.0(8) . . ? C74 C77 C79 106.5(6) . . ? C80 C77 C79 105.0(6) . . ? C78' C77 C79' 107.3(7) . . ? C78 C77 C79' 42.6(7) . . ? C80' C77 C79' 106.4(7) . . ? C74 C77 C79' 105.7(8) . . ? C80 C77 C79' 77.3(8) . . ? C79 C77 C79' 143.1(8) . . ? C77 C78 H78A 109.5 . . ? C77 C78 H78B 109.5 . . ? C77 C78 H78C 109.5 . . ? C77 C79 H79A 109.5 . . ? C77 C79 H79B 109.5 . . ? C77 C79 H79C 109.5 . . ? C77 C80 H80A 109.5 . . ? C77 C80 H80B 109.5 . . ? C77 C80 H80C 109.5 . . ? O11 C81 C82 121.4(4) . . ? O11 C81 C86 120.0(4) . . ? C82 C81 C86 118.6(4) . . ? C81 C82 C83 120.3(4) . . ? C81 C82 S7 122.8(4) . . ? C83 C82 S7 116.8(4) . . ? C82 C83 C84 121.8(5) . . ? C82 C83 H83 119.1 . . ? C84 C83 H83 119.1 . . ? C85 C84 C83 117.2(5) . . ? C85 C84 C87 123.2(5) . . ? C83 C84 C87 119.6(5) . . ? C84 C85 C86 121.5(5) . . ? C84 C85 H85 119.2 . . ? C86 C85 H85 119.2 . . ? C81 C86 C85 120.4(5) . . ? C81 C86 S8 120.0(4) . . ? C85 C86 S8 119.5(4) . . ? C88 C87 C89 108.7(5) . . ? C88 C87 C84 111.5(5) . . ? C89 C87 C84 108.3(5) . . ? C88 C87 C90 108.9(6) . . ? C89 C87 C90 109.2(6) . . ? C84 C87 C90 110.1(5) . . ? C87 C88 H88A 109.5 . . ? C87 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C87 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C87 C89 H89A 109.5 . . ? C87 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? C87 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? C87 C90 H90A 109.5 . . ? C87 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? C87 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? O9 C91 C92 108.3(4) . . ? O9 C91 H91A 110.0 . . ? C92 C91 H91A 110.0 . . ? O9 C91 H91B 110.0 . . ? C92 C91 H91B 110.0 . . ? H91A C91 H91B 108.4 . . ? O10 C92 C91 107.9(4) . . ? O10 C92 H92A 110.1 . . ? C91 C92 H92A 110.1 . . ? O10 C92 H92B 110.1 . . ? C91 C92 H92B 110.1 . . ? H92A C92 H92B 108.4 . . ? O10 C93 C94 116.0(4) . . ? O10 C93 C98 124.9(5) . . ? C94 C93 C98 119.1(5) . . ? C95 C94 O12 120.3(5) . . ? C95 C94 C93 120.3(5) . . ? O12 C94 C93 119.4(4) . . ? C94 C95 C96 120.4(5) . . ? C94 C95 H95 119.8 . . ? C96 C95 H95 119.8 . . ? C97 C96 C95 119.9(5) . . ? C97 C96 H96 120.0 . . ? C95 C96 H96 120.0 . . ? C96 C97 C98 120.3(5) . . ? C96 C97 H97 119.8 . . ? C98 C97 H97 119.8 . . ? C97 C98 C93 119.9(5) . . ? C97 C98 H98 120.0 . . ? C93 C98 H98 120.0 . . ? O12 C99 C100 108.7(4) . . ? O12 C99 H99A 109.9 . . ? C100 C99 H99A 109.9 . . ? O12 C99 H99B 109.9 . . ? C100 C99 H99B 109.9 . . ? H99A C99 H99B 108.3 . . ? O11 C100 C99 109.3(4) . . ? O11 C100 H10D 109.8 . . ? C99 C100 H10D 109.8 . . ? O11 C100 H10E 109.8 . . ? C99 C100 H10E 109.8 . . ? H10D C100 H10E 108.3 . . ? O13 C101 C106 121.4(5) . . ? O13 C101 C102 126.7(5) . . ? C106 C101 C102 111.8(4) . . ? C103 C102 C101 123.9(5) . . ? C103 C102 N7 115.1(5) . . ? C101 C102 N7 120.8(4) . . ? C102 C103 C104 119.5(5) . . ? C102 C103 H103 120.3 . . ? C104 C103 H103 120.3 . . ? C105 C104 C103 120.6(5) . . ? C105 C104 N8 119.7(5) . . ? C103 C104 N8 119.7(5) . . ? C106 C105 C104 119.6(5) . . ? C106 C105 H105 120.2 . . ? C104 C105 H105 120.2 . . ? C105 C106 C101 124.5(5) . . ? C105 C106 N9 116.4(5) . . ? C101 C106 N9 119.1(5) . . ? O20 C107 C108 127.0(5) . . ? O20 C107 C112 121.6(5) . . ? C108 C107 C112 111.3(4) . . ? C109 C108 C107 123.8(5) . . ? C109 C108 N10 116.3(5) . . ? C107 C108 N10 119.8(4) . . ? C110 C109 C108 119.2(5) . . ? C110 C109 H109 120.4 . . ? C108 C109 H109 120.4 . . ? C109 C110 C111 121.5(5) . . ? C109 C110 N11 119.2(5) . . ? C111 C110 N11 119.4(5) . . ? C112 C111 C110 118.3(5) . . ? C112 C111 H111 120.8 . . ? C110 C111 H111 120.8 . . ? C111 C112 C107 125.8(5) . . ? C111 C112 N12 118.1(5) . . ? C107 C112 N12 116.1(5) . . ? Cl2 C113 Cl1 109.4(5) . . ? Cl2 C113 Cl3 109.0(5) . . ? Cl1 C113 Cl3 110.6(5) . . ? Cl2 C113 H113 109.3 . . ? Cl1 C113 H113 109.3 . . ? Cl3 C113 H113 109.3 . . ? Cl4 C114 Cl6 111.1(4) . . ? Cl4 C114 Cl5 110.4(3) . . ? Cl6 C114 Cl5 110.5(4) . . ? Cl4 C114 H114 108.2 . . ? Cl6 C114 H114 108.2 . . ? Cl5 C114 H114 108.2 . . ? Cl9 C115 Cl7 112.7(4) . . ? Cl9 C115 Cl8 109.9(4) . . ? Cl7 C115 Cl8 110.7(4) . . ? Cl9 C115 H115 107.8 . . ? Cl7 C115 H115 107.8 . . ? Cl8 C115 H115 107.8 . . ? Cl11 C116 Cl10 112.3(4) . . ? Cl11 C116 Cl12 110.0(4) . . ? Cl10 C116 Cl12 111.9(4) . . ? Cl11 C116 H116 107.5 . . ? Cl10 C116 H116 107.5 . . ? Cl12 C116 H116 107.5 . . ? O15 N7 O14' 115.7(7) . . ? O15 N7 O14 121.8(7) . . ? O14' N7 O14 39.9(6) . . ? O15 N7 C102 119.1(4) . . ? O14' N7 C102 118.9(11) . . ? O14 N7 C102 117.0(10) . . ? O17 N8 O16 123.3(5) . . ? O17 N8 C104 118.3(5) . . ? O16 N8 C104 118.3(4) . . ? O19 N9 O18 123.4(5) . . ? O19 N9 C106 119.2(5) . . ? O18 N9 C106 117.4(5) . . ? O22 N10 O21 123.9(5) . . ? O22 N10 C108 118.3(5) . . ? O21 N10 C108 117.9(4) . . ? O24 N11 O23 123.3(4) . . ? O24 N11 C110 118.8(5) . . ? O23 N11 C110 117.9(4) . . ? O26 N12 O26' 92.7(10) . . ? O26 N12 O25' 55.8(8) . . ? O26' N12 O25' 121.9(9) . . ? O26 N12 O25 124.4(8) . . ? O26' N12 O25 55.0(8) . . ? O25' N12 O25 100.8(9) . . ? O26 N12 C112 119.2(7) . . ? O26' N12 C112 121.5(8) . . ? O25' N12 C112 116.6(7) . . ? O25 N12 C112 116.3(7) . . ? C1 O1 H1A 111(5) . . ? C21 O2 H2A 114(4) . . ? C11 O3 C41 117.8(4) . . ? C43 O4 C42 116.9(4) . . ? C31 O5 C50 114.5(3) . . ? C44 O6 C49 113.9(4) . . ? C51 O7 H7A 109(4) . . ? C71 O8 H8G 115(4) . . ? C61 O9 C91 119.2(4) . . ? C93 O10 C92 116.8(4) . . ? C81 O11 C100 112.4(3) . . ? C94 O12 C99 112.2(4) . . ? C94 O12 Ag2 123.7(3) . . ? C99 O12 Ag2 122.6(3) . . ? C101 O13 Ag1 141.6(4) . . ? C107 O20 Ag2 139.2(3) . . ? N7 O14 Ag1 131.0(13) . . ? C6 S1 C12 103.7(2) . . ? C22 S2 C16 99.4(2) . . ? C22 S2 Ag2 102.48(16) . . ? C16 S2 Ag2 115.11(16) . . ? C26 S3 C32 101.6(2) . . ? C26 S3 Ag1 104.15(16) . . ? C32 S3 Ag1 120.70(17) . . ? C2 S4 C36 101.2(2) . . ? C56 S5 C62 104.7(2) . . ? C72 S6 C66 99.2(2) . . ? C72 S6 Ag1 106.03(17) . . ? C66 S6 Ag1 114.06(16) . . ? C76 S7 C82 100.7(2) . . ? C76 S7 Ag2 105.95(17) . . ? C82 S7 Ag2 121.73(17) . . ? C52 S8 C86 102.2(2) . . ? N7 O14' Ag1 135.1(12) . . ? C7 C9' H9'1 109.5 . . ? C7 C9' H9'2 109.5 . . ? H9'1 C9' H9'2 109.5 . . ? C7 C9' H9'3 109.5 . . ? H9'1 C9' H9'3 109.5 . . ? H9'2 C9' H9'3 109.5 . . ? C7 C8' H8'1 109.5 . . ? C7 C8' H8'2 109.5 . . ? H8'1 C8' H8'2 109.5 . . ? C7 C8' H8'3 109.5 . . ? H8'1 C8' H8'3 109.5 . . ? H8'2 C8' H8'3 109.5 . . ? C7 C10' H10F 109.5 . . ? C7 C10' H10G 109.5 . . ? H10F C10' H10G 109.5 . . ? C7 C10' H10H 109.5 . . ? H10F C10' H10H 109.5 . . ? H10G C10' H10H 109.5 . . ? C77 C78' H78D 109.5 . . ? C77 C78' H78E 109.5 . . ? H78D C78' H78E 109.5 . . ? C77 C78' H78F 109.5 . . ? H78D C78' H78F 109.5 . . ? H78E C78' H78F 109.5 . . ? C77 C79' H79D 109.5 . . ? C77 C79' H79E 109.5 . . ? H79D C79' H79E 109.5 . . ? C77 C79' H79F 109.5 . . ? H79D C79' H79F 109.5 . . ? H79E C79' H79F 109.5 . . ? C77 C80' H80D 109.5 . . ? C77 C80' H80E 109.5 . . ? H80D C80' H80E 109.5 . . ? C77 C80' H80F 109.5 . . ? H80D C80' H80F 109.5 . . ? H80E C80' H80F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 179.5(4) . . . . ? C6 C1 C2 C3 0.5(7) . . . . ? O1 C1 C2 S4 1.7(6) . . . . ? C6 C1 C2 S4 -177.3(4) . . . . ? C1 C2 C3 C4 -0.6(8) . . . . ? S4 C2 C3 C4 177.3(4) . . . . ? C2 C3 C4 C5 0.6(8) . . . . ? C2 C3 C4 C7 -179.3(5) . . . . ? C3 C4 C5 C6 -0.5(8) . . . . ? C7 C4 C5 C6 179.3(5) . . . . ? C4 C5 C6 C1 0.5(8) . . . . ? C4 C5 C6 S1 -173.7(4) . . . . ? O1 C1 C6 C5 -179.4(5) . . . . ? C2 C1 C6 C5 -0.5(7) . . . . ? O1 C1 C6 S1 -5.2(7) . . . . ? C2 C1 C6 S1 173.7(4) . . . . ? C5 C4 C7 C9 -115.4(7) . . . . ? C3 C4 C7 C9 64.4(8) . . . . ? C5 C4 C7 C10' 53.1(10) . . . . ? C3 C4 C7 C10' -127.1(9) . . . . ? C5 C4 C7 C10 10.2(8) . . . . ? C3 C4 C7 C10 -170.0(6) . . . . ? C5 C4 C7 C8' -173.6(7) . . . . ? C3 C4 C7 C8' 6.2(9) . . . . ? C5 C4 C7 C9' -58.7(9) . . . . ? C3 C4 C7 C9' 121.1(8) . . . . ? C5 C4 C7 C8 124.7(7) . . . . ? C3 C4 C7 C8 -55.5(7) . . . . ? O3 C11 C12 C13 -174.8(4) . . . . ? C16 C11 C12 C13 0.2(7) . . . . ? O3 C11 C12 S1 8.1(6) . . . . ? C16 C11 C12 S1 -177.0(4) . . . . ? C11 C12 C13 C14 -0.8(7) . . . . ? S1 C12 C13 C14 176.3(4) . . . . ? C12 C13 C14 C15 -0.2(7) . . . . ? C12 C13 C14 C17 178.1(5) . . . . ? C13 C14 C15 C16 1.9(7) . . . . ? C17 C14 C15 C16 -176.5(5) . . . . ? C14 C15 C16 C11 -2.6(7) . . . . ? C14 C15 C16 S2 174.7(4) . . . . ? O3 C11 C16 C15 176.3(4) . . . . ? C12 C11 C16 C15 1.5(7) . . . . ? O3 C11 C16 S2 -1.0(6) . . . . ? C12 C11 C16 S2 -175.7(4) . . . . ? C13 C14 C17 C18 -110.2(6) . . . . ? C15 C14 C17 C18 68.1(7) . . . . ? C13 C14 C17 C19 129.8(6) . . . . ? C15 C14 C17 C19 -51.9(7) . . . . ? C13 C14 C17 C20 10.4(7) . . . . ? C15 C14 C17 C20 -171.3(5) . . . . ? O2 C21 C22 C23 -177.5(4) . . . . ? C26 C21 C22 C23 4.8(7) . . . . ? O2 C21 C22 S2 1.6(6) . . . . ? C26 C21 C22 S2 -176.1(3) . . . . ? C21 C22 C23 C24 0.3(8) . . . . ? S2 C22 C23 C24 -178.8(4) . . . . ? C22 C23 C24 C25 -4.1(7) . . . . ? C22 C23 C24 C27 177.0(5) . . . . ? C23 C24 C25 C26 2.8(7) . . . . ? C27 C24 C25 C26 -178.4(5) . . . . ? C24 C25 C26 C21 2.3(7) . . . . ? C24 C25 C26 S3 -175.4(4) . . . . ? O2 C21 C26 C25 176.4(4) . . . . ? C22 C21 C26 C25 -6.0(7) . . . . ? O2 C21 C26 S3 -6.0(7) . . . . ? C22 C21 C26 S3 171.6(3) . . . . ? C25 C24 C27 C29 7.9(8) . . . . ? C23 C24 C27 C29 -173.4(5) . . . . ? C25 C24 C27 C28 129.3(5) . . . . ? C23 C24 C27 C28 -51.9(7) . . . . ? C25 C24 C27 C30 -111.9(6) . . . . ? C23 C24 C27 C30 66.8(6) . . . . ? O5 C31 C32 C33 -178.3(4) . . . . ? C36 C31 C32 C33 -3.0(7) . . . . ? O5 C31 C32 S3 2.3(6) . . . . ? C36 C31 C32 S3 177.6(4) . . . . ? C31 C32 C33 C34 2.1(7) . . . . ? S3 C32 C33 C34 -178.5(4) . . . . ? C32 C33 C34 C35 -0.7(8) . . . . ? C32 C33 C34 C37 -176.3(5) . . . . ? C33 C34 C35 C36 0.5(8) . . . . ? C37 C34 C35 C36 176.2(5) . . . . ? C34 C35 C36 C31 -1.5(8) . . . . ? C34 C35 C36 S4 -178.5(4) . . . . ? O5 C31 C36 C35 178.0(4) . . . . ? C32 C31 C36 C35 2.7(7) . . . . ? O5 C31 C36 S4 -5.2(6) . . . . ? C32 C31 C36 S4 179.6(3) . . . . ? C33 C34 C37 C40 -153.2(5) . . . . ? C35 C34 C37 C40 31.3(8) . . . . ? C33 C34 C37 C39 86.6(7) . . . . ? C35 C34 C37 C39 -88.9(7) . . . . ? C33 C34 C37 C38 -34.7(8) . . . . ? C35 C34 C37 C38 149.8(6) . . . . ? O3 C41 C42 O4 71.2(6) . . . . ? C48 C43 C44 C45 -2.6(7) . . . . ? O4 C43 C44 C45 -178.7(4) . . . . ? C48 C43 C44 O6 179.7(4) . . . . ? O4 C43 C44 O6 3.6(7) . . . . ? O6 C44 C45 C46 177.7(4) . . . . ? C43 C44 C45 C46 -0.1(7) . . . . ? C44 C45 C46 C47 2.4(7) . . . . ? C45 C46 C47 C48 -1.9(7) . . . . ? C44 C43 C48 C47 3.1(7) . . . . ? O4 C43 C48 C47 179.0(4) . . . . ? C46 C47 C48 C43 -0.9(8) . . . . ? O6 C49 C50 O5 -58.4(5) . . . . ? O7 C51 C52 C53 -177.6(5) . . . . ? C56 C51 C52 C53 4.1(7) . . . . ? O7 C51 C52 S8 8.1(7) . . . . ? C56 C51 C52 S8 -170.2(4) . . . . ? C51 C52 C53 C54 -1.9(8) . . . . ? S8 C52 C53 C54 172.4(4) . . . . ? C52 C53 C54 C55 -1.2(8) . . . . ? C52 C53 C54 C57 -178.7(5) . . . . ? C53 C54 C55 C56 2.1(8) . . . . ? C57 C54 C55 C56 179.6(5) . . . . ? C54 C55 C56 C51 0.2(8) . . . . ? C54 C55 C56 S5 -170.9(4) . . . . ? O7 C51 C56 C55 178.3(4) . . . . ? C52 C51 C56 C55 -3.3(7) . . . . ? O7 C51 C56 S5 -10.8(6) . . . . ? C52 C51 C56 S5 167.6(4) . . . . ? C53 C54 C57 C60 -128.6(6) . . . . ? C55 C54 C57 C60 54.0(7) . . . . ? C53 C54 C57 C59 111.2(6) . . . . ? C55 C54 C57 C59 -66.2(6) . . . . ? C53 C54 C57 C58 -9.0(8) . . . . ? C55 C54 C57 C58 173.5(5) . . . . ? O9 C61 C62 C63 179.3(4) . . . . ? C66 C61 C62 C63 -3.4(7) . . . . ? O9 C61 C62 S5 1.8(7) . . . . ? C66 C61 C62 S5 179.2(4) . . . . ? C61 C62 C63 C64 1.4(8) . . . . ? S5 C62 C63 C64 179.1(4) . . . . ? C62 C63 C64 C65 0.6(8) . . . . ? C62 C63 C64 C67 -177.7(5) . . . . ? C63 C64 C65 C66 -0.6(8) . . . . ? C67 C64 C65 C66 177.8(5) . . . . ? C64 C65 C66 C61 -1.5(8) . . . . ? C64 C65 C66 S6 177.2(4) . . . . ? O9 C61 C66 C65 -178.9(4) . . . . ? C62 C61 C66 C65 3.5(7) . . . . ? O9 C61 C66 S6 2.4(6) . . . . ? C62 C61 C66 S6 -175.3(4) . . . . ? C63 C64 C67 C68 -9.7(8) . . . . ? C65 C64 C67 C68 172.1(6) . . . . ? C63 C64 C67 C70 110.4(6) . . . . ? C65 C64 C67 C70 -67.8(7) . . . . ? C63 C64 C67 C69 -129.4(6) . . . . ? C65 C64 C67 C69 52.4(7) . . . . ? O8 C71 C72 C73 -175.8(5) . . . . ? C76 C71 C72 C73 6.0(7) . . . . ? O8 C71 C72 S6 3.0(7) . . . . ? C76 C71 C72 S6 -175.2(4) . . . . ? C71 C72 C73 C74 -1.8(8) . . . . ? S6 C72 C73 C74 179.5(4) . . . . ? C72 C73 C74 C75 -2.5(8) . . . . ? C72 C73 C74 C77 176.5(5) . . . . ? C73 C74 C75 C76 2.4(8) . . . . ? C77 C74 C75 C76 -176.6(5) . . . . ? C74 C75 C76 C71 2.0(8) . . . . ? C74 C75 C76 S7 -177.2(4) . . . . ? O8 C71 C76 C75 175.6(4) . . . . ? C72 C71 C76 C75 -6.1(7) . . . . ? O8 C71 C76 S7 -5.3(7) . . . . ? C72 C71 C76 S7 173.0(4) . . . . ? C73 C74 C77 C78' -54.2(10) . . . . ? C75 C74 C77 C78' 124.7(9) . . . . ? C73 C74 C77 C78 18.1(8) . . . . ? C75 C74 C77 C78 -163.0(6) . . . . ? C73 C74 C77 C80' 179.1(9) . . . . ? C75 C74 C77 C80' -2.0(10) . . . . ? C73 C74 C77 C80 145.5(7) . . . . ? C75 C74 C77 C80 -35.6(8) . . . . ? C73 C74 C77 C79 -99.2(7) . . . . ? C75 C74 C77 C79 79.7(7) . . . . ? C73 C74 C77 C79' 62.6(9) . . . . ? C75 C74 C77 C79' -118.5(8) . . . . ? O11 C81 C82 C83 179.4(4) . . . . ? C86 C81 C82 C83 -3.4(7) . . . . ? O11 C81 C82 S7 -2.4(6) . . . . ? C86 C81 C82 S7 174.8(4) . . . . ? C81 C82 C83 C84 2.7(7) . . . . ? S7 C82 C83 C84 -175.5(4) . . . . ? C82 C83 C84 C85 0.3(8) . . . . ? C82 C83 C84 C87 -178.9(5) . . . . ? C83 C84 C85 C86 -2.6(8) . . . . ? C87 C84 C85 C86 176.5(5) . . . . ? O11 C81 C86 C85 178.3(4) . . . . ? C82 C81 C86 C85 1.1(7) . . . . ? O11 C81 C86 S8 -2.7(6) . . . . ? C82 C81 C86 S8 -179.9(3) . . . . ? C84 C85 C86 C81 1.9(7) . . . . ? C84 C85 C86 S8 -177.0(4) . . . . ? C85 C84 C87 C88 6.8(8) . . . . ? C83 C84 C87 C88 -174.1(6) . . . . ? C85 C84 C87 C89 -112.8(6) . . . . ? C83 C84 C87 C89 66.3(7) . . . . ? C85 C84 C87 C90 127.8(6) . . . . ? C83 C84 C87 C90 -53.1(7) . . . . ? O9 C91 C92 O10 -70.1(5) . . . . ? O10 C93 C94 C95 -179.9(5) . . . . ? C98 C93 C94 C95 -0.9(8) . . . . ? O10 C93 C94 O12 1.4(7) . . . . ? C98 C93 C94 O12 -179.6(4) . . . . ? O12 C94 C95 C96 179.6(5) . . . . ? C93 C94 C95 C96 0.9(9) . . . . ? C94 C95 C96 C97 0.7(10) . . . . ? C95 C96 C97 C98 -2.3(10) . . . . ? C96 C97 C98 C93 2.3(9) . . . . ? O10 C93 C98 C97 178.2(5) . . . . ? C94 C93 C98 C97 -0.6(8) . . . . ? O12 C99 C100 O11 -72.4(5) . . . . ? O13 C101 C102 C103 177.3(5) . . . . ? C106 C101 C102 C103 -0.5(8) . . . . ? O13 C101 C102 N7 1.9(8) . . . . ? C106 C101 C102 N7 -175.9(5) . . . . ? C101 C102 C103 C104 0.0(8) . . . . ? N7 C102 C103 C104 175.6(5) . . . . ? C102 C103 C104 C105 -1.2(8) . . . . ? C102 C103 C104 N8 179.7(5) . . . . ? C103 C104 C105 C106 3.0(8) . . . . ? N8 C104 C105 C106 -177.9(5) . . . . ? C104 C105 C106 C101 -3.7(8) . . . . ? C104 C105 C106 N9 179.4(5) . . . . ? O13 C101 C106 C105 -175.5(5) . . . . ? C102 C101 C106 C105 2.4(8) . . . . ? O13 C101 C106 N9 1.4(8) . . . . ? C102 C101 C106 N9 179.2(5) . . . . ? O20 C107 C108 C109 -175.7(5) . . . . ? C112 C107 C108 C109 1.7(7) . . . . ? O20 C107 C108 N10 3.5(8) . . . . ? C112 C107 C108 N10 -179.1(5) . . . . ? C107 C108 C109 C110 -1.3(8) . . . . ? N10 C108 C109 C110 179.5(4) . . . . ? C108 C109 C110 C111 -0.4(8) . . . . ? C108 C109 C110 N11 179.5(4) . . . . ? C109 C110 C111 C112 1.4(8) . . . . ? N11 C110 C111 C112 -178.5(5) . . . . ? C110 C111 C112 C107 -0.8(9) . . . . ? C110 C111 C112 N12 178.7(5) . . . . ? O20 C107 C112 C111 176.9(5) . . . . ? C108 C107 C112 C111 -0.7(8) . . . . ? O20 C107 C112 N12 -2.6(8) . . . . ? C108 C107 C112 N12 179.8(5) . . . . ? C103 C102 N7 O15 -8.3(8) . . . . ? C101 C102 N7 O15 167.5(5) . . . . ? C103 C102 N7 O14' -159(2) . . . . ? C101 C102 N7 O14' 17(2) . . . . ? C103 C102 N7 O14 155.4(19) . . . . ? C101 C102 N7 O14 -29(2) . . . . ? C105 C104 N8 O17 -8.1(8) . . . . ? C103 C104 N8 O17 171.1(5) . . . . ? C105 C104 N8 O16 173.0(5) . . . . ? C103 C104 N8 O16 -7.8(8) . . . . ? C105 C106 N9 O19 -144.1(5) . . . . ? C101 C106 N9 O19 38.8(7) . . . . ? C105 C106 N9 O18 34.1(8) . . . . ? C101 C106 N9 O18 -143.0(6) . . . . ? C109 C108 N10 O22 24.8(8) . . . . ? C107 C108 N10 O22 -154.4(6) . . . . ? C109 C108 N10 O21 -155.5(5) . . . . ? C107 C108 N10 O21 25.2(7) . . . . ? C109 C110 N11 O24 -179.3(5) . . . . ? C111 C110 N11 O24 0.6(7) . . . . ? C109 C110 N11 O23 0.7(7) . . . . ? C111 C110 N11 O23 -179.4(5) . . . . ? C111 C112 N12 O26 120.3(9) . . . . ? C107 C112 N12 O26 -60.2(10) . . . . ? C111 C112 N12 O26' -125.8(12) . . . . ? C107 C112 N12 O26' 53.8(13) . . . . ? C111 C112 N12 O25' 56.3(10) . . . . ? C107 C112 N12 O25' -124.1(9) . . . . ? C111 C112 N12 O25 -62.4(9) . . . . ? C107 C112 N12 O25 117.2(8) . . . . ? C12 C11 O3 C41 -118.9(5) . . . . ? C16 C11 O3 C41 66.3(6) . . . . ? C42 C41 O3 C11 144.7(4) . . . . ? C48 C43 O4 C42 41.9(6) . . . . ? C44 C43 O4 C42 -142.2(4) . . . . ? C41 C42 O4 C43 87.3(5) . . . . ? C32 C31 O5 C50 -104.5(5) . . . . ? C36 C31 O5 C50 80.4(5) . . . . ? C49 C50 O5 C31 -170.7(4) . . . . ? C45 C44 O6 C49 112.2(5) . . . . ? C43 C44 O6 C49 -70.0(6) . . . . ? C50 C49 O6 C44 -173.9(4) . . . . ? C62 C61 O9 C91 -46.7(6) . . . . ? C66 C61 O9 C91 135.9(4) . . . . ? C92 C91 O9 C61 -145.7(4) . . . . ? C94 C93 O10 C92 -164.1(4) . . . . ? C98 C93 O10 C92 17.0(7) . . . . ? C91 C92 O10 C93 -172.4(4) . . . . ? C82 C81 O11 C100 -93.1(5) . . . . ? C86 C81 O11 C100 89.7(5) . . . . ? C99 C100 O11 C81 -179.1(4) . . . . ? C95 C94 O12 C99 100.9(6) . . . . ? C93 C94 O12 C99 -80.4(5) . . . . ? C95 C94 O12 Ag2 -65.7(6) . . . . ? C93 C94 O12 Ag2 113.0(4) . . . . ? C100 C99 O12 C94 -178.9(4) . . . . ? C100 C99 O12 Ag2 -12.1(5) . . . . ? O20 Ag2 O12 C94 77.7(3) . . . . ? S7 Ag2 O12 C94 -152.2(3) . . . . ? S2 Ag2 O12 C94 -33.8(3) . . . . ? O20 Ag2 O12 C99 -87.5(3) . . . . ? S7 Ag2 O12 C99 42.5(3) . . . . ? S2 Ag2 O12 C99 160.9(3) . . . . ? C106 C101 O13 Ag1 180.0(4) . . . . ? C102 C101 O13 Ag1 2.4(10) . . . . ? O14' Ag1 O13 C101 -12.3(13) . . . . ? S6 Ag1 O13 C101 -107.4(6) . . . . ? S3 Ag1 O13 C101 62.8(6) . . . . ? O14 Ag1 O13 C101 8.4(11) . . . . ? C108 C107 O20 Ag2 20.7(9) . . . . ? C112 C107 O20 Ag2 -156.4(4) . . . . ? O12 Ag2 O20 C107 140.5(5) . . . . ? S7 Ag2 O20 C107 22.2(6) . . . . ? S2 Ag2 O20 C107 -130.3(5) . . . . ? O15 N7 O14 Ag1 -144.1(15) . . . . ? O14' N7 O14 Ag1 -51.1(14) . . . . ? C102 N7 O14 Ag1 53(3) . . . . ? O13 Ag1 O14 N7 -37(3) . . . . ? O14' Ag1 O14 N7 48.4(18) . . . . ? S6 Ag1 O14 N7 68(3) . . . . ? S3 Ag1 O14 N7 -179(3) . . . . ? C5 C6 S1 C12 -101.6(4) . . . . ? C1 C6 S1 C12 84.2(4) . . . . ? C11 C12 S1 C6 -94.0(4) . . . . ? C13 C12 S1 C6 88.8(4) . . . . ? C23 C22 S2 C16 84.6(4) . . . . ? C21 C22 S2 C16 -94.4(4) . . . . ? C23 C22 S2 Ag2 -33.9(4) . . . . ? C21 C22 S2 Ag2 147.0(3) . . . . ? C15 C16 S2 C22 -80.3(4) . . . . ? C11 C16 S2 C22 97.0(4) . . . . ? C15 C16 S2 Ag2 28.4(4) . . . . ? C11 C16 S2 Ag2 -154.3(3) . . . . ? O20 Ag2 S2 C22 122.27(19) . . . . ? O12 Ag2 S2 C22 -151.96(18) . . . . ? S7 Ag2 S2 C22 -34.03(17) . . . . ? O20 Ag2 S2 C16 15.5(2) . . . . ? O12 Ag2 S2 C16 101.2(2) . . . . ? S7 Ag2 S2 C16 -140.84(18) . . . . ? C25 C26 S3 C32 -93.3(4) . . . . ? C21 C26 S3 C32 89.0(4) . . . . ? C25 C26 S3 Ag1 140.6(4) . . . . ? C21 C26 S3 Ag1 -37.1(4) . . . . ? C33 C32 S3 C26 91.0(4) . . . . ? C31 C32 S3 C26 -89.5(4) . . . . ? C33 C32 S3 Ag1 -154.7(3) . . . . ? C31 C32 S3 Ag1 24.8(4) . . . . ? O13 Ag1 S3 C26 173.6(2) . . . . ? O14' Ag1 S3 C26 -122.6(6) . . . . ? S6 Ag1 S3 C26 -16.30(17) . . . . ? O14 Ag1 S3 C26 -136.7(8) . . . . ? O13 Ag1 S3 C32 60.6(2) . . . . ? O14' Ag1 S3 C32 124.4(6) . . . . ? S6 Ag1 S3 C32 -129.29(18) . . . . ? O14 Ag1 S3 C32 110.3(8) . . . . ? C1 C2 S4 C36 -89.2(4) . . . . ? C3 C2 S4 C36 92.9(4) . . . . ? C35 C36 S4 C2 -82.4(4) . . . . ? C31 C36 S4 C2 100.7(4) . . . . ? C55 C56 S5 C62 -107.5(4) . . . . ? C51 C56 S5 C62 81.5(4) . . . . ? C61 C62 S5 C56 -91.5(4) . . . . ? C63 C62 S5 C56 91.0(4) . . . . ? C73 C72 S6 C66 78.5(4) . . . . ? C71 C72 S6 C66 -100.2(4) . . . . ? C73 C72 S6 Ag1 -39.9(4) . . . . ? C71 C72 S6 Ag1 141.3(4) . . . . ? C65 C66 S6 C72 -86.5(4) . . . . ? C61 C66 S6 C72 92.2(4) . . . . ? C65 C66 S6 Ag1 25.8(5) . . . . ? C61 C66 S6 Ag1 -155.5(3) . . . . ? O13 Ag1 S6 C72 134.7(2) . . . . ? O14' Ag1 S6 C72 63.2(7) . . . . ? S3 Ag1 S6 C72 -37.19(18) . . . . ? O14 Ag1 S6 C72 56.7(3) . . . . ? O13 Ag1 S6 C66 26.6(2) . . . . ? O14' Ag1 S6 C66 -44.8(7) . . . . ? S3 Ag1 S6 C66 -145.25(17) . . . . ? O14 Ag1 S6 C66 -51.3(3) . . . . ? C75 C76 S7 C82 -84.2(4) . . . . ? C71 C76 S7 C82 96.7(4) . . . . ? C75 C76 S7 Ag2 148.2(4) . . . . ? C71 C76 S7 Ag2 -31.0(4) . . . . ? C81 C82 S7 C76 -87.8(4) . . . . ? C83 C82 S7 C76 90.5(4) . . . . ? C81 C82 S7 Ag2 28.7(5) . . . . ? C83 C82 S7 Ag2 -153.0(3) . . . . ? O20 Ag2 S7 C76 -169.5(2) . . . . ? O12 Ag2 S7 C76 85.73(19) . . . . ? S2 Ag2 S7 C76 -17.81(17) . . . . ? O20 Ag2 S7 C82 76.6(2) . . . . ? O12 Ag2 S7 C82 -28.1(2) . . . . ? S2 Ag2 S7 C82 -131.68(18) . . . . ? C53 C52 S8 C86 100.5(4) . . . . ? C51 C52 S8 C86 -85.2(4) . . . . ? C81 C86 S8 C52 97.6(4) . . . . ? C85 C86 S8 C52 -83.4(4) . . . . ? O15 N7 O14' Ag1 167(3) . . . . ? O14 N7 O14' Ag1 58(2) . . . . ? C102 N7 O14' Ag1 -41(5) . . . . ? O13 Ag1 O14' N7 33(4) . . . . ? S6 Ag1 O14' N7 144(4) . . . . ? S3 Ag1 O14' N7 -100(4) . . . . ? O14 Ag1 O14' N7 -53(3) . . . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.380 _refine_diff_density_min -1.617 _refine_diff_density_rms 0.127 #===END data_publication_text _publ_contact_author 'Xiong Li' _publ_contact_author_email 'lxwhu2008@hotmail.com' loop_ _publ_author_name 'Xiong Li' 'Shu-Ling Gong' 'Wei-Ping Yang' 'Yuan-Yin Chen' 'Xiang-Gao Meng' _journal_name_full 'Dalton Transactions' data_CCDC-740898 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,3-alternate-5,11,17,23-Tetra-tert-butyl-25,27-[1,3- bis(oxyethoxy)benzene]-2,8,14,20 -tetra-thiacalix[4]arene silver picrate complex ; _chemical_name_common ; 1,3-alternate-thiacalix[4]-m-benzocrown-4 silver picrate complex ; _chemical_melting_point ? _chemical_formula_moiety 'C112 H120 Ag2 N6 O26 S8, 2(C H2 Cl2)' _chemical_formula_sum 'C114 H124 Ag2 Cl4 N6 O26 S8' _chemical_formula_weight 2608.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.1544(7) _cell_length_b 23.6949(12) _cell_length_c 39.290(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.955(1) _cell_angle_gamma 90.00 _cell_volume 12217.2(11) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 5400 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 19.05 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.418 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5392 _exptl_absorpt_coefficient_mu 0.617 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8866 _exptl_absorpt_correction_T_max 0.9409 _exptl_absorpt_process_details 'SADABS, Sheldrick,1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 116563 _diffrn_reflns_av_R_equivalents 0.0936 _diffrn_reflns_av_sigmaI/netI 0.0744 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.00 _reflns_number_total 21478 _reflns_number_gt 13583 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Commands ¡®DFIX¡¯, ¡®SADI¡¯ and ¡®ISOR¡¯ were used in the refinement.. During the refinement, some tert-butyl groups were found to be seriously disordered. We attempt to refine them using command ¡®PART¡¯, but the final model gave very unstable thermal factors. So we only refined them by restraining the C-C distances with command ¡®DFIX¡¯ and some thermal factors were restrained using command ¡®ISOR¡¯. The nitro O6 and O7 atoms were disordered over two sites with the final occupancies of 0.54(1):0.46(1) for the two components. Although some higher factors, i.e. R1 and wR2, were resulted in the final refinement, the current structure was more chemically reasonable than the earlier model. The structure contains several solvent accessible voids of ca.40.00 \%A^3^ in the unit cell, the residual electron-density count in each void is less than 1 electron. Therefore, there is no solvent molecule accommodated in the voids. ; _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^)+(0.1502P)^2^+40.1752P] 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 21478 _refine_ls_number_parameters 1488 _refine_ls_number_restraints 49 _refine_ls_R_factor_all 0.1564 _refine_ls_R_factor_gt 0.1063 _refine_ls_wR_factor_ref 0.2919 _refine_ls_wR_factor_gt 0.2631 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.042 _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 Ag1 Ag 0.39711(7) 0.52707(4) 0.66867(2) 0.0750(3) Uani 1 1 d . . . Ag2 Ag 0.31575(6) 0.32459(3) 0.526921(15) 0.0619(3) Uani 1 1 d . . . C1 C 0.6315(9) 0.5770(5) 0.6781(3) 0.074(3) Uani 1 1 d . . . C2 C 0.6589(8) 0.5697(4) 0.6441(3) 0.070(3) Uani 1 1 d . . . C3 C 0.7571(9) 0.5772(4) 0.6344(3) 0.074(3) Uani 1 1 d . . . H3 H 0.7724 0.5730 0.6118 0.089 Uiso 1 1 calc R . . C4 C 0.8326(9) 0.5913(5) 0.6597(3) 0.086(3) Uani 1 1 d . . . C5 C 0.8118(11) 0.5974(5) 0.6926(3) 0.092(4) Uani 1 1 d . . . H5 H 0.8632 0.6072 0.7090 0.111 Uiso 1 1 calc R . . C6 C 0.7168(10) 0.5893(6) 0.7014(3) 0.089(4) Uani 1 1 d D A . C7 C 0.4026(9) 0.5477(6) 0.7516(3) 0.080(3) Uani 1 1 d . . . C8 C 0.3975(9) 0.6083(5) 0.7496(3) 0.082(3) Uani 1 1 d . . . C9 C 0.4238(10) 0.6430(7) 0.7762(4) 0.102(4) Uani 1 1 d . . . H9 H 0.4220 0.6820 0.7737 0.123 Uiso 1 1 calc R . . C10 C 0.4527(10) 0.6188(8) 0.8065(4) 0.101(4) Uani 1 1 d . . . C11 C 0.4559(10) 0.5626(8) 0.8112(4) 0.097(4) Uani 1 1 d . . . H11 H 0.4720 0.5477 0.8328 0.117 Uiso 1 1 calc R . . C12 C 0.4360(9) 0.5288(7) 0.7850(3) 0.089(4) Uani 1 1 d . . . C13 C 0.0696(7) 0.4562(3) 0.6367(2) 0.048(2) Uani 1 1 d . . . C14 C 0.1550(7) 0.4745(4) 0.6557(2) 0.052(2) Uani 1 1 d . . . C15 C 0.1516(8) 0.4884(4) 0.6905(2) 0.065(3) Uani 1 1 d . . . H15 H 0.2101 0.5017 0.7025 0.078 Uiso 1 1 calc R . . C16 C 0.0628(8) 0.4825(4) 0.7072(2) 0.066(3) Uani 1 1 d . . . C17 C -0.0243(8) 0.4645(4) 0.6866(2) 0.064(3) Uani 1 1 d . . . H17 H -0.0861 0.4615 0.6966 0.076 Uiso 1 1 calc R . . C18 C -0.0214(7) 0.4514(3) 0.6529(2) 0.052(2) Uani 1 1 d . . . C19 C 0.0625(8) 0.4938(5) 0.7455(3) 0.083(3) Uani 1 1 d D . . C20 C 0.1382(12) 0.4543(7) 0.7654(4) 0.159(7) Uani 1 1 d D . . H20A H 0.1487 0.4672 0.7885 0.238 Uiso 1 1 calc R . . H20B H 0.2020 0.4545 0.7549 0.238 Uiso 1 1 calc R . . H20C H 0.1112 0.4167 0.7651 0.238 Uiso 1 1 calc R . . C21 C 0.0982(12) 0.5550(5) 0.7523(4) 0.142(6) Uani 1 1 d D . . H21A H 0.0424 0.5804 0.7473 0.214 Uiso 1 1 calc R . . H21B H 0.1525 0.5638 0.7381 0.214 Uiso 1 1 calc R . . H21C H 0.1221 0.5588 0.7758 0.214 Uiso 1 1 calc R . . C22 C -0.0448(9) 0.4847(7) 0.7577(4) 0.143(6) Uani 1 1 d D . . H22A H -0.0512 0.5050 0.7786 0.215 Uiso 1 1 calc R . . H22B H -0.0555 0.4452 0.7615 0.215 Uiso 1 1 calc R . . H22C H -0.0947 0.4982 0.7406 0.215 Uiso 1 1 calc R . . C23 C 0.3088(6) 0.4037(3) 0.6399(2) 0.0428(19) Uani 1 1 d . . . C24 C 0.3303(5) 0.3723(3) 0.61110(17) 0.0335(16) Uani 1 1 d . . . C25 C 0.3431(5) 0.3150(3) 0.61512(16) 0.0333(16) Uani 1 1 d . . . C26 C 0.3385(7) 0.2897(4) 0.6464(2) 0.049(2) Uani 1 1 d . . . H26 H 0.3494 0.2510 0.6484 0.058 Uiso 1 1 calc R . . C27 C 0.3176(8) 0.3212(4) 0.6755(2) 0.061(3) Uani 1 1 d . . . C28 C 0.3047(8) 0.3780(4) 0.6714(2) 0.057(2) Uani 1 1 d . . . H28 H 0.2927 0.4000 0.6903 0.068 Uiso 1 1 calc R . . C29 C 0.3031(10) 0.2922(5) 0.7099(3) 0.086(4) Uani 1 1 d D . . C30 C 0.2178(13) 0.3236(8) 0.7274(5) 0.184(9) Uani 1 1 d D . . H30A H 0.1914 0.2996 0.7444 0.275 Uiso 1 1 calc R . . H30B H 0.1641 0.3334 0.7107 0.275 Uiso 1 1 calc R . . H30C H 0.2451 0.3573 0.7381 0.275 Uiso 1 1 calc R . . C31 C 0.4054(12) 0.2970(9) 0.7309(6) 0.205(10) Uani 1 1 d D . . H31A H 0.4023 0.2762 0.7517 0.308 Uiso 1 1 calc R . . H31B H 0.4194 0.3360 0.7360 0.308 Uiso 1 1 calc R . . H31C H 0.4586 0.2819 0.7180 0.308 Uiso 1 1 calc R . . C32 C 0.2699(13) 0.2306(5) 0.7052(4) 0.142(6) Uani 1 1 d D . . H32A H 0.3280 0.2078 0.7008 0.212 Uiso 1 1 calc R . . H32B H 0.2199 0.2278 0.6863 0.212 Uiso 1 1 calc R . . H32C H 0.2411 0.2175 0.7255 0.212 Uiso 1 1 calc R . . C33 C 0.2531(5) 0.2238(3) 0.58335(16) 0.0297(15) Uani 1 1 d . . . C34 C 0.1542(6) 0.2435(3) 0.57565(16) 0.0327(16) Uani 1 1 d . . . C35 C 0.0731(5) 0.2060(3) 0.57937(18) 0.0380(17) Uani 1 1 d . . . C36 C 0.0933(6) 0.1526(3) 0.5923(2) 0.0442(19) Uani 1 1 d . . . H36 H 0.0387 0.1284 0.5950 0.053 Uiso 1 1 calc R . . C37 C 0.1911(6) 0.1331(3) 0.6015(2) 0.0417(18) Uani 1 1 d . . . C38 C 0.2712(6) 0.1705(3) 0.59629(18) 0.0361(17) Uani 1 1 d . . . H38 H 0.3380 0.1590 0.6017 0.043 Uiso 1 1 calc R . . C39 C 0.2064(7) 0.0760(4) 0.6192(2) 0.059(2) Uani 1 1 d D . . C40 C 0.1549(11) 0.0768(6) 0.6533(3) 0.124(5) Uani 1 1 d D . . H40A H 0.1668 0.0414 0.6649 0.186 Uiso 1 1 calc R . . H40B H 0.0830 0.0825 0.6490 0.186 Uiso 1 1 calc R . . H40C H 0.1831 0.1069 0.6674 0.186 Uiso 1 1 calc R . . C41 C 0.1557(9) 0.0283(4) 0.5973(3) 0.091(4) Uani 1 1 d D . . H41A H 0.1766 0.0310 0.5744 0.136 Uiso 1 1 calc R . . H41B H 0.0830 0.0319 0.5970 0.136 Uiso 1 1 calc R . . H41C H 0.1761 -0.0076 0.6068 0.136 Uiso 1 1 calc R . . C42 C 0.3194(8) 0.0608(6) 0.6247(4) 0.140(6) Uani 1 1 d D . . H42A H 0.3556 0.0913 0.6361 0.210 Uiso 1 1 calc R . . H42B H 0.3467 0.0542 0.6030 0.210 Uiso 1 1 calc R . . H42C H 0.3268 0.0273 0.6384 0.210 Uiso 1 1 calc R . . C43 C -0.0845(5) 0.2660(3) 0.60490(19) 0.0388(18) Uani 1 1 d . . . C44 C -0.0912(5) 0.3255(3) 0.60239(19) 0.0388(18) Uani 1 1 d . . . C45 C -0.1200(6) 0.3557(4) 0.6303(2) 0.0448(19) Uani 1 1 d . . . C46 C -0.1392(7) 0.3273(4) 0.6601(2) 0.053(2) Uani 1 1 d . . . H46 H -0.1602 0.3479 0.6785 0.064 Uiso 1 1 calc R . . C47 C -0.1283(7) 0.2692(4) 0.6634(2) 0.057(2) Uani 1 1 d . . . C48 C -0.1031(6) 0.2397(4) 0.6351(2) 0.047(2) Uani 1 1 d . . . H48 H -0.0984 0.2006 0.6363 0.057 Uiso 1 1 calc R . . C49 C -0.1476(9) 0.2403(5) 0.6974(3) 0.091(4) Uani 1 1 d D . . C50 C -0.0538(14) 0.2476(12) 0.7224(7) 0.288(16) Uani 1 1 d D . . H50A H -0.0549 0.2845 0.7325 0.432 Uiso 1 1 calc R . . H50B H 0.0069 0.2435 0.7104 0.432 Uiso 1 1 calc R . . H50C H -0.0546 0.2195 0.7400 0.432 Uiso 1 1 calc R . . C51 C -0.2386(12) 0.2684(7) 0.7134(5) 0.156(7) Uani 1 1 d D . . H51A H -0.2278 0.2676 0.7378 0.234 Uiso 1 1 calc R . . H51B H -0.3000 0.2483 0.7065 0.234 Uiso 1 1 calc R . . H51C H -0.2445 0.3069 0.7058 0.234 Uiso 1 1 calc R . . C52 C -0.1767(13) 0.1779(5) 0.6917(4) 0.145(7) Uani 1 1 d D . . H52A H -0.1167 0.1564 0.6878 0.218 Uiso 1 1 calc R . . H52B H -0.2246 0.1748 0.6722 0.218 Uiso 1 1 calc R . . H52C H -0.2070 0.1636 0.7115 0.218 Uiso 1 1 calc R . . C53 C 0.4116(6) 0.4380(3) 0.5750(2) 0.0452(19) Uani 1 1 d . . . H53A H 0.4678 0.4206 0.5642 0.054 Uiso 1 1 calc R . . H53B H 0.4372 0.4518 0.5973 0.054 Uiso 1 1 calc R . . C54 C 0.3701(8) 0.4866(4) 0.5536(3) 0.063(3) Uani 1 1 d . . . H54A H 0.3068 0.4992 0.5623 0.076 Uiso 1 1 calc R . . H54B H 0.4181 0.5177 0.5558 0.076 Uiso 1 1 calc R . . C55 C 0.2520(8) 0.4642(4) 0.5059(2) 0.061(3) Uani 1 1 d . . . C56 C 0.2337(9) 0.4705(4) 0.4709(2) 0.068(3) Uani 1 1 d . . . H56 H 0.2862 0.4814 0.4576 0.081 Uiso 1 1 calc R . . C57 C 0.1407(9) 0.4607(4) 0.4563(2) 0.070(3) Uani 1 1 d . . . H57 H 0.1293 0.4656 0.4329 0.084 Uiso 1 1 calc R . . C58 C 0.0617(8) 0.4438(4) 0.4747(2) 0.060(2) Uani 1 1 d . . . H58 H -0.0022 0.4364 0.4640 0.073 Uiso 1 1 calc R . . C59 C 0.0793(8) 0.4377(4) 0.5099(2) 0.052(2) Uani 1 1 d . . . C60 C 0.1721(7) 0.4477(3) 0.5252(2) 0.051(2) Uani 1 1 d . . . H60 H 0.1830 0.4437 0.5487 0.061 Uiso 1 1 calc R . . C61 C -0.0734(7) 0.3883(5) 0.5187(2) 0.061(3) Uani 1 1 d . . . H61A H -0.0454 0.3559 0.5074 0.073 Uiso 1 1 calc R . . H61B H -0.1182 0.4084 0.5022 0.073 Uiso 1 1 calc R . . C62 C -0.1318(6) 0.3692(4) 0.5482(2) 0.056(2) Uani 1 1 d . . . H62A H -0.1730 0.3998 0.5561 0.067 Uiso 1 1 calc R . . H62B H -0.1762 0.3378 0.5415 0.067 Uiso 1 1 calc R . . C63 C 0.2110(5) 0.1975(3) 0.49363(17) 0.0330(16) Uani 1 1 d . . . C64 C 0.1471(6) 0.2413(3) 0.48244(18) 0.0379(17) Uani 1 1 d . . . C65 C 0.0432(6) 0.2340(4) 0.47627(18) 0.044(2) Uani 1 1 d . . . H65 H 0.0031 0.2645 0.4688 0.053 Uiso 1 1 calc R . . C66 C -0.0020(6) 0.1826(4) 0.4810(2) 0.048(2) Uani 1 1 d . . . C67 C 0.0607(6) 0.1376(4) 0.4921(2) 0.046(2) Uani 1 1 d . . . H67 H 0.0322 0.1022 0.4953 0.055 Uiso 1 1 calc R . . C68 C 0.1647(5) 0.1452(3) 0.49828(17) 0.0370(17) Uani 1 1 d . . . C69 C -0.1159(6) 0.1723(4) 0.4707(2) 0.070(3) Uani 1 1 d D . . C70 C -0.1797(7) 0.2260(4) 0.4756(3) 0.090(4) Uani 1 1 d D . . H70A H -0.2508 0.2167 0.4735 0.135 Uiso 1 1 calc R . . H70B H -0.1654 0.2533 0.4585 0.135 Uiso 1 1 calc R . . H70C H -0.1624 0.2416 0.4978 0.135 Uiso 1 1 calc R . . C71 C -0.1588(8) 0.1246(5) 0.4923(3) 0.109(5) Uani 1 1 d D . . H71A H -0.1437 0.1325 0.5160 0.163 Uiso 1 1 calc R . . H71B H -0.1281 0.0894 0.4866 0.163 Uiso 1 1 calc R . . H71C H -0.2313 0.1223 0.4876 0.163 Uiso 1 1 calc R . . C72 C -0.1214(9) 0.1575(7) 0.4323(2) 0.125(6) Uani 1 1 d D . . H72A H -0.0929 0.1207 0.4293 0.187 Uiso 1 1 calc R . . H72B H -0.0834 0.1849 0.4204 0.187 Uiso 1 1 calc R . . H72C H -0.1912 0.1579 0.4234 0.187 Uiso 1 1 calc R . . C73 C 0.2971(5) 0.0653(3) 0.47555(18) 0.0334(16) Uani 1 1 d . . . C74 C 0.3984(5) 0.0769(3) 0.47165(17) 0.0309(15) Uani 1 1 d . . . C75 C 0.4438(5) 0.0590(3) 0.44197(18) 0.0347(16) Uani 1 1 d . . . C76 C 0.3840(6) 0.0299(3) 0.41712(19) 0.0393(18) Uani 1 1 d . . . H76 H 0.4135 0.0182 0.3975 0.047 Uiso 1 1 calc R . . C77 C 0.2826(6) 0.0177(3) 0.4206(2) 0.0436(19) Uani 1 1 d . . . C78 C 0.2410(6) 0.0362(3) 0.45019(19) 0.0433(19) Uani 1 1 d . . . H78 H 0.1727 0.0287 0.4530 0.052 Uiso 1 1 calc R . . C79 C 0.2145(6) -0.0141(3) 0.3937(2) 0.064(3) Uani 1 1 d D . . C80 C 0.1233(8) 0.0241(4) 0.3820(3) 0.102(4) Uani 1 1 d D . . H80A H 0.0876 0.0350 0.4015 0.153 Uiso 1 1 calc R . . H80B H 0.0780 0.0038 0.3662 0.153 Uiso 1 1 calc R . . H80C H 0.1478 0.0572 0.3711 0.153 Uiso 1 1 calc R . . C81 C 0.1741(9) -0.0685(4) 0.4095(3) 0.088(4) Uani 1 1 d D . . H81A H 0.2299 -0.0938 0.4151 0.133 Uiso 1 1 calc R . . H81B H 0.1261 -0.0864 0.3935 0.133 Uiso 1 1 calc R . . H81C H 0.1412 -0.0594 0.4299 0.133 Uiso 1 1 calc R . . C82 C 0.2739(9) -0.0319(6) 0.3631(3) 0.112(5) Uani 1 1 d D . . H82A H 0.2966 0.0011 0.3517 0.168 Uiso 1 1 calc R . . H82B H 0.2304 -0.0538 0.3476 0.168 Uiso 1 1 calc R . . H82C H 0.3318 -0.0541 0.3710 0.168 Uiso 1 1 calc R . . C83 C 0.5910(5) 0.1256(3) 0.41118(18) 0.0342(16) Uani 1 1 d . . . C84 C 0.5719(5) 0.1799(3) 0.42203(18) 0.0348(16) Uani 1 1 d . . . C85 C 0.5938(6) 0.2245(3) 0.40055(18) 0.0372(17) Uani 1 1 d . . . C86 C 0.6339(6) 0.2148(3) 0.36953(19) 0.0428(19) Uani 1 1 d . . . H86 H 0.6456 0.2451 0.3553 0.051 Uiso 1 1 calc R . . C87 C 0.6573(6) 0.1600(4) 0.3592(2) 0.046(2) Uani 1 1 d . . . C88 C 0.6325(5) 0.1157(3) 0.38014(18) 0.0371(17) Uani 1 1 d . . . H88 H 0.6438 0.0788 0.3733 0.045 Uiso 1 1 calc R . . C89 C 0.7070(7) 0.1516(4) 0.32478(19) 0.067(3) Uani 1 1 d D . . C90 C 0.8052(9) 0.1869(6) 0.3249(3) 0.128(6) Uani 1 1 d D . . H90A H 0.8293 0.1874 0.3024 0.193 Uiso 1 1 calc R . . H90B H 0.8562 0.1706 0.3406 0.193 Uiso 1 1 calc R . . H90C H 0.7913 0.2248 0.3319 0.193 Uiso 1 1 calc R . . C91 C 0.7321(11) 0.0889(4) 0.3191(3) 0.109(5) Uani 1 1 d D . . H91A H 0.6700 0.0675 0.3170 0.163 Uiso 1 1 calc R . . H91B H 0.7744 0.0752 0.3382 0.163 Uiso 1 1 calc R . . H91C H 0.7674 0.0851 0.2987 0.163 Uiso 1 1 calc R . . C92 C 0.6319(9) 0.1716(5) 0.2957(2) 0.096(4) Uani 1 1 d D . . H92A H 0.6678 0.1779 0.2756 0.145 Uiso 1 1 calc R . . H92B H 0.6004 0.2061 0.3023 0.145 Uiso 1 1 calc R . . H92C H 0.5805 0.1433 0.2912 0.145 Uiso 1 1 calc R . . C93 C 0.4301(6) 0.2900(3) 0.41256(18) 0.0372(17) Uani 1 1 d . . . C94 C 0.3781(6) 0.3057(3) 0.44138(18) 0.0373(17) Uani 1 1 d . . . C95 C 0.2746(6) 0.2957(3) 0.43976(17) 0.0369(17) Uani 1 1 d . . . C96 C 0.2240(6) 0.2700(3) 0.41183(18) 0.0436(19) Uani 1 1 d . . . H96 H 0.1543 0.2636 0.4120 0.052 Uiso 1 1 calc R . . C97 C 0.2751(7) 0.2536(4) 0.38357(19) 0.049(2) Uani 1 1 d . . . C98 C 0.3774(7) 0.2659(3) 0.38485(19) 0.048(2) Uani 1 1 d . . . H98 H 0.4131 0.2575 0.3659 0.058 Uiso 1 1 calc R . . C99 C 0.2254(7) 0.2208(4) 0.3542(2) 0.070(3) Uani 1 1 d D . . C100 C 0.1116(9) 0.2085(8) 0.3585(4) 0.154(7) Uani 1 1 d D . . H10A H 0.1047 0.1904 0.3801 0.231 Uiso 1 1 calc R . . H10B H 0.0854 0.1841 0.3405 0.231 Uiso 1 1 calc R . . H10C H 0.0741 0.2432 0.3577 0.231 Uiso 1 1 calc R . . C101 C 0.2832(11) 0.1651(5) 0.3507(4) 0.129(6) Uani 1 1 d D . . H10D H 0.3492 0.1727 0.3426 0.194 Uiso 1 1 calc R . . H10E H 0.2456 0.1410 0.3347 0.194 Uiso 1 1 calc R . . H10F H 0.2912 0.1468 0.3725 0.194 Uiso 1 1 calc R . . C102 C 0.2338(13) 0.2546(6) 0.3209(3) 0.142(6) Uani 1 1 d D . . H10G H 0.1920 0.2878 0.3213 0.213 Uiso 1 1 calc R . . H10H H 0.2111 0.2316 0.3017 0.213 Uiso 1 1 calc R . . H10I H 0.3034 0.2654 0.3188 0.213 Uiso 1 1 calc R . . C103 C 0.5085(6) 0.0823(3) 0.52290(19) 0.0408(18) Uani 1 1 d . . . H10J H 0.5683 0.0636 0.5150 0.049 Uiso 1 1 calc R . . H10K H 0.4656 0.0541 0.5326 0.049 Uiso 1 1 calc R . . C104 C 0.5393(6) 0.1263(3) 0.5489(2) 0.046(2) Uani 1 1 d . . . H10L H 0.4795 0.1447 0.5569 0.055 Uiso 1 1 calc R . . H10M H 0.5771 0.1092 0.5684 0.055 Uiso 1 1 calc R . . C105 C 0.6099(5) 0.2191(3) 0.54887(18) 0.0385(18) Uani 1 1 d . . . C106 C 0.6352(6) 0.2241(4) 0.5834(2) 0.051(2) Uani 1 1 d . . . H106 H 0.6491 0.1924 0.5969 0.062 Uiso 1 1 calc R . . C107 C 0.6391(7) 0.2777(4) 0.5975(2) 0.056(2) Uani 1 1 d . . . H107 H 0.6562 0.2820 0.6207 0.067 Uiso 1 1 calc R . . C108 C 0.6184(6) 0.3241(4) 0.5779(2) 0.046(2) Uani 1 1 d . . . H108 H 0.6213 0.3598 0.5878 0.056 Uiso 1 1 calc R . . C109 C 0.5928(6) 0.3185(3) 0.54314(18) 0.0395(18) Uani 1 1 d . . . C110 C 0.5874(6) 0.2650(3) 0.52866(19) 0.0407(18) Uani 1 1 d . . . H110 H 0.5686 0.2605 0.5056 0.049 Uiso 1 1 calc R . . C111 C 0.5851(7) 0.3714(4) 0.4908(2) 0.050(2) Uani 1 1 d . . . H11A H 0.6213 0.3383 0.4836 0.060 Uiso 1 1 calc R . . H11B H 0.6271 0.4042 0.4868 0.060 Uiso 1 1 calc R . . C112 C 0.4861(7) 0.3766(3) 0.4694(2) 0.045(2) Uani 1 1 d . . . H11C H 0.4471 0.4079 0.4775 0.054 Uiso 1 1 calc R . . H11D H 0.4999 0.3842 0.4459 0.054 Uiso 1 1 calc R . . C113 C 0.1895(13) 0.6316(8) 0.6141(4) 0.135(6) Uani 1 1 d . . . H11E H 0.2568 0.6358 0.6256 0.162 Uiso 1 1 calc R . . H11F H 0.1512 0.6056 0.6274 0.162 Uiso 1 1 calc R . . C114 C 0.5846(12) 0.4224(8) 0.7033(5) 0.144(7) Uani 1 1 d . . . H11G H 0.5403 0.4528 0.7097 0.173 Uiso 1 1 calc R . . H11H H 0.5597 0.3876 0.7127 0.173 Uiso 1 1 calc R . . Cl1 Cl 0.2008(4) 0.6046(3) 0.57538(18) 0.178(2) Uani 1 1 d . . . Cl2 Cl 0.1292(7) 0.6965(3) 0.6127(2) 0.239(4) Uani 1 1 d . . . Cl3 Cl 0.5794(4) 0.4171(3) 0.65947(14) 0.188(3) Uani 1 1 d . . . Cl4 Cl 0.7058(4) 0.4350(3) 0.72025(11) 0.1527(18) Uani 1 1 d . . . N1 N 0.5852(8) 0.5547(4) 0.6172(2) 0.076(2) Uani 1 1 d . . . N2 N 0.9352(10) 0.5990(6) 0.6499(4) 0.112(4) Uani 1 1 d . . . N3 N 0.7035(16) 0.5935(9) 0.7387(5) 0.137(6) Uani 1 1 d D . . N4 N 0.3606(12) 0.6326(6) 0.7169(4) 0.116(4) Uani 1 1 d . . . N5 N 0.4721(15) 0.6583(10) 0.8368(6) 0.146(6) Uani 1 1 d . . . N6 N 0.4441(13) 0.4690(9) 0.7902(5) 0.139(6) Uani 1 1 d . . . O1 O 0.5424(7) 0.5688(4) 0.6879(2) 0.102(3) Uani 1 1 d . . . O2 O 0.4959(7) 0.5692(4) 0.6188(2) 0.101(3) Uani 1 1 d . . . O3 O 0.6120(7) 0.5277(5) 0.5936(2) 0.117(3) Uani 1 1 d . . . O4 O 0.9544(8) 0.5888(6) 0.6201(3) 0.144(4) Uani 1 1 d . . . O5 O 1.0012(9) 0.6132(5) 0.6704(3) 0.132(4) Uani 1 1 d . . . O6 O 0.639(2) 0.5666(13) 0.7525(7) 0.153(9) Uani 0.54 1 d PD A 1 O7 O 0.767(4) 0.6199(14) 0.7558(12) 0.156(12) Uani 0.54 1 d PD A 1 O6' O 0.632(3) 0.6253(16) 0.7426(9) 0.164(11) Uani 0.46 1 d P A 2 O7' O 0.765(5) 0.582(3) 0.7622(17) 0.20(2) Uani 0.46 1 d P A 2 O8 O 0.3803(7) 0.5137(3) 0.72752(19) 0.087(2) Uani 1 1 d . . . O9 O 0.3085(9) 0.6123(5) 0.6959(3) 0.122(4) Uani 1 1 d . . . O10 O 0.4069(15) 0.6795(8) 0.7111(4) 0.202(7) Uani 1 1 d . . . O11 O 0.4633(13) 0.7077(8) 0.8318(4) 0.173(6) Uani 1 1 d . . . O12 O 0.4831(12) 0.6364(8) 0.8646(4) 0.174(6) Uani 1 1 d . . . O13 O 0.4471(14) 0.4517(8) 0.8197(5) 0.211(7) Uani 1 1 d . . . O14 O 0.4522(17) 0.4343(9) 0.7677(6) 0.225(8) Uani 1 1 d . . . O15 O 0.0812(5) 0.4415(3) 0.60391(15) 0.0635(17) Uani 1 1 d . . . H15A H 0.0311 0.4237 0.5964 0.095 Uiso 1 1 calc R . . O16 O 0.1410(4) 0.2973(2) 0.56442(13) 0.0392(12) Uani 1 1 d . . . H16 H 0.0850 0.3003 0.5540 0.059 Uiso 1 1 calc R . . O17 O -0.0574(4) 0.3524(2) 0.57412(13) 0.0423(12) Uani 1 1 d . . . O18 O 0.0048(5) 0.4235(3) 0.53127(15) 0.0592(16) Uani 1 1 d . . . O19 O 0.3321(4) 0.3963(2) 0.57917(12) 0.0414(12) Uani 1 1 d . . . O20 O 0.3522(5) 0.4734(3) 0.51908(16) 0.074(2) Uani 1 1 d . . . O21 O 0.5359(4) 0.1929(2) 0.45265(13) 0.0432(13) Uani 1 1 d . . . H21 H 0.5395 0.1650 0.4650 0.065 Uiso 1 1 calc R . . O22 O 0.3116(3) 0.2071(2) 0.49923(13) 0.0361(11) Uani 1 1 d . . . H22 H 0.3395 0.1789 0.5075 0.054 Uiso 1 1 calc R . . O23 O 0.4536(4) 0.11077(19) 0.49505(12) 0.0350(11) Uani 1 1 d . . . O24 O 0.6009(4) 0.1660(2) 0.53316(13) 0.0427(13) Uani 1 1 d . . . O25 O 0.4276(4) 0.3252(2) 0.47098(12) 0.0389(12) Uani 1 1 d . . . O26 O 0.5711(6) 0.3672(2) 0.52589(14) 0.0649(18) Uani 1 1 d . . . S1 S 0.27233(18) 0.47671(9) 0.63496(6) 0.0515(6) Uani 1 1 d . . . S2 S 0.36147(14) 0.26888(8) 0.57970(5) 0.0356(4) Uani 1 1 d . . . S3 S -0.05412(15) 0.22671(9) 0.56806(5) 0.0457(5) Uani 1 1 d . . . S4 S -0.13349(18) 0.43027(10) 0.62826(6) 0.0555(6) Uani 1 1 d . . . S5 S 0.19861(15) 0.31082(8) 0.47533(5) 0.0417(5) Uani 1 1 d . . . S6 S 0.24181(16) 0.08701(9) 0.51389(5) 0.0435(5) Uani 1 1 d . . . S7 S 0.57789(14) 0.06674(8) 0.43904(5) 0.0416(5) Uani 1 1 d . . . S8 S 0.56657(16) 0.29513(8) 0.41297(5) 0.0462(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0816(6) 0.0766(6) 0.0676(5) -0.0187(4) 0.0102(4) -0.0141(4) Ag2 0.0887(6) 0.0646(5) 0.0324(3) 0.0019(3) 0.0046(3) -0.0316(4) C1 0.075(7) 0.070(7) 0.079(7) -0.012(6) 0.028(6) -0.013(6) C2 0.060(6) 0.065(7) 0.086(7) 0.007(6) 0.016(6) -0.008(5) C3 0.087(8) 0.066(7) 0.073(7) 0.000(5) 0.024(6) -0.001(6) C4 0.076(8) 0.088(9) 0.097(9) -0.008(7) 0.026(7) -0.029(7) C5 0.100(10) 0.091(9) 0.088(9) -0.017(7) 0.015(7) -0.020(7) C6 0.094(9) 0.106(10) 0.068(7) -0.020(7) 0.024(7) -0.030(7) C7 0.078(8) 0.099(9) 0.066(7) -0.021(6) 0.022(6) -0.012(7) C8 0.094(9) 0.089(9) 0.062(7) -0.032(6) 0.010(6) 0.015(7) C9 0.101(10) 0.109(11) 0.098(10) -0.033(9) 0.017(8) 0.000(8) C10 0.080(9) 0.136(14) 0.086(10) -0.036(10) 0.008(7) -0.006(9) C11 0.074(8) 0.132(13) 0.086(9) -0.010(9) 0.011(7) 0.011(9) C12 0.079(8) 0.135(13) 0.053(7) -0.006(8) 0.009(6) 0.014(8) C13 0.059(6) 0.036(4) 0.052(5) -0.011(4) 0.022(4) -0.004(4) C14 0.064(6) 0.044(5) 0.052(5) -0.009(4) 0.027(4) -0.004(4) C15 0.068(6) 0.072(7) 0.057(5) -0.026(5) 0.022(5) -0.015(5) C16 0.076(7) 0.074(7) 0.051(5) -0.023(5) 0.029(5) -0.012(5) C17 0.069(6) 0.064(6) 0.063(6) -0.012(5) 0.039(5) -0.005(5) C18 0.071(6) 0.031(4) 0.055(5) -0.016(4) 0.019(4) -0.003(4) C19 0.080(8) 0.097(9) 0.075(7) -0.022(7) 0.025(6) -0.004(7) C20 0.168(18) 0.179(19) 0.131(15) -0.005(14) 0.020(13) 0.010(15) C21 0.158(16) 0.143(15) 0.128(13) -0.039(11) 0.025(11) -0.021(12) C22 0.143(15) 0.173(17) 0.117(12) -0.027(12) 0.037(11) -0.009(13) C23 0.045(5) 0.036(4) 0.049(5) -0.001(4) 0.014(4) -0.009(4) C24 0.033(4) 0.032(4) 0.036(4) 0.002(3) 0.012(3) -0.007(3) C25 0.037(4) 0.038(4) 0.027(3) -0.002(3) 0.010(3) -0.004(3) C26 0.064(6) 0.039(5) 0.044(5) 0.008(4) 0.006(4) -0.008(4) C27 0.094(7) 0.050(6) 0.040(5) 0.004(4) 0.015(5) -0.008(5) C28 0.085(7) 0.052(6) 0.035(4) -0.008(4) 0.011(4) -0.013(5) C29 0.126(11) 0.080(8) 0.053(6) 0.013(6) 0.017(7) 0.002(8) C30 0.20(2) 0.19(2) 0.166(19) 0.024(16) 0.051(17) 0.013(17) C31 0.22(3) 0.21(3) 0.19(2) 0.033(19) 0.01(2) -0.02(2) C32 0.168(17) 0.136(15) 0.122(13) 0.035(11) 0.023(11) -0.024(12) C33 0.035(4) 0.026(4) 0.030(3) -0.005(3) 0.012(3) -0.002(3) C34 0.046(4) 0.029(4) 0.024(3) 0.001(3) 0.013(3) -0.004(3) C35 0.034(4) 0.044(5) 0.036(4) -0.006(3) 0.004(3) 0.000(3) C36 0.047(5) 0.032(4) 0.055(5) -0.007(4) 0.016(4) -0.009(4) C37 0.052(5) 0.025(4) 0.049(4) -0.005(3) 0.010(4) -0.005(4) C38 0.040(4) 0.029(4) 0.039(4) -0.005(3) 0.006(3) 0.004(3) C39 0.064(6) 0.048(5) 0.064(6) 0.008(4) 0.008(5) -0.004(5) C40 0.162(15) 0.110(12) 0.100(10) 0.023(9) 0.015(10) 0.012(10) C41 0.114(10) 0.061(7) 0.099(9) 0.012(6) 0.014(7) -0.011(7) C42 0.141(15) 0.103(12) 0.175(17) 0.039(11) -0.004(12) 0.006(10) C43 0.028(4) 0.045(5) 0.044(4) -0.003(4) 0.006(3) -0.007(3) C44 0.028(4) 0.045(5) 0.045(4) 0.000(4) 0.008(3) -0.006(3) C45 0.040(4) 0.050(5) 0.045(4) -0.006(4) 0.008(4) 0.000(4) C46 0.057(5) 0.060(6) 0.045(5) -0.006(4) 0.019(4) -0.008(4) C47 0.061(6) 0.058(6) 0.054(5) 0.008(4) 0.016(4) -0.011(5) C48 0.043(5) 0.044(5) 0.055(5) 0.002(4) 0.009(4) -0.004(4) C49 0.103(10) 0.100(10) 0.070(7) 0.017(7) 0.013(7) -0.010(8) C50 0.29(4) 0.30(4) 0.27(4) 0.02(3) 0.01(3) -0.02(3) C51 0.178(18) 0.157(17) 0.142(15) 0.006(12) 0.067(14) 0.005(14) C52 0.169(17) 0.127(14) 0.143(15) 0.035(11) 0.042(13) -0.019(12) C53 0.048(5) 0.042(5) 0.047(4) 0.003(4) 0.017(4) -0.008(4) C54 0.070(6) 0.043(5) 0.079(7) 0.011(5) 0.027(5) -0.016(5) C55 0.079(7) 0.052(6) 0.054(5) 0.026(4) 0.028(5) 0.022(5) C56 0.080(8) 0.072(7) 0.055(6) 0.024(5) 0.038(5) 0.021(6) C57 0.088(8) 0.080(7) 0.044(5) 0.021(5) 0.026(5) 0.030(6) C58 0.069(6) 0.057(6) 0.057(6) 0.011(4) 0.016(5) 0.019(5) C59 0.071(6) 0.043(5) 0.047(5) 0.018(4) 0.023(5) 0.022(4) C60 0.066(6) 0.044(5) 0.045(5) 0.018(4) 0.021(4) 0.018(4) C61 0.055(6) 0.093(8) 0.034(4) 0.009(5) 0.006(4) 0.006(5) C62 0.040(5) 0.073(6) 0.054(5) 0.013(4) 0.004(4) 0.010(4) C63 0.024(4) 0.047(5) 0.029(3) -0.006(3) 0.006(3) 0.003(3) C64 0.033(4) 0.043(5) 0.037(4) -0.003(3) 0.004(3) 0.000(3) C65 0.032(4) 0.067(6) 0.032(4) -0.004(4) -0.003(3) 0.015(4) C66 0.030(4) 0.077(6) 0.038(4) -0.011(4) 0.001(3) -0.008(4) C67 0.036(4) 0.058(5) 0.046(4) -0.009(4) 0.014(4) -0.011(4) C68 0.034(4) 0.047(5) 0.031(4) -0.001(3) 0.009(3) -0.005(3) C69 0.029(5) 0.120(9) 0.059(6) -0.024(6) -0.003(4) -0.005(5) C70 0.040(6) 0.142(12) 0.087(8) -0.015(8) -0.008(5) 0.009(6) C71 0.036(6) 0.152(13) 0.138(12) 0.007(10) 0.004(6) -0.038(7) C72 0.054(7) 0.245(19) 0.073(8) -0.055(10) -0.013(6) -0.019(9) C73 0.036(4) 0.025(4) 0.041(4) 0.005(3) 0.013(3) -0.003(3) C74 0.035(4) 0.026(4) 0.032(4) 0.006(3) 0.000(3) 0.000(3) C75 0.036(4) 0.027(4) 0.041(4) 0.005(3) 0.008(3) 0.000(3) C76 0.046(5) 0.035(4) 0.038(4) 0.001(3) 0.008(3) -0.007(4) C77 0.048(5) 0.031(4) 0.051(5) 0.000(3) 0.000(4) -0.011(4) C78 0.034(4) 0.051(5) 0.046(4) -0.004(4) 0.007(3) -0.012(4) C79 0.068(6) 0.068(6) 0.054(5) -0.009(5) -0.009(5) -0.029(5) C80 0.106(10) 0.097(10) 0.096(9) 0.010(7) -0.044(8) -0.037(8) C81 0.102(9) 0.059(7) 0.103(9) -0.017(6) 0.002(7) -0.044(6) C82 0.117(10) 0.166(14) 0.057(6) -0.051(8) 0.025(7) -0.074(10) C83 0.021(4) 0.045(5) 0.037(4) 0.005(3) 0.006(3) -0.005(3) C84 0.033(4) 0.037(4) 0.036(4) -0.003(3) 0.011(3) -0.007(3) C85 0.037(4) 0.040(4) 0.036(4) 0.001(3) 0.008(3) -0.001(3) C86 0.042(4) 0.048(5) 0.040(4) 0.004(4) 0.012(3) -0.006(4) C87 0.038(4) 0.057(5) 0.043(4) -0.009(4) 0.009(3) 0.007(4) C88 0.032(4) 0.039(4) 0.040(4) 0.002(3) 0.003(3) 0.007(3) C89 0.101(8) 0.070(7) 0.034(4) 0.000(4) 0.026(5) 0.005(6) C90 0.119(11) 0.171(15) 0.106(10) -0.034(10) 0.080(9) -0.053(11) C91 0.180(14) 0.093(9) 0.061(7) 0.003(6) 0.066(8) 0.045(9) C92 0.144(12) 0.099(9) 0.048(6) -0.006(6) 0.018(7) 0.024(8) C93 0.052(5) 0.027(4) 0.035(4) 0.008(3) 0.016(3) 0.001(3) C94 0.049(5) 0.028(4) 0.035(4) 0.006(3) 0.003(3) 0.004(3) C95 0.048(5) 0.036(4) 0.027(4) 0.000(3) 0.008(3) 0.013(4) C96 0.041(4) 0.054(5) 0.036(4) 0.002(4) 0.001(3) 0.009(4) C97 0.064(6) 0.049(5) 0.032(4) 0.003(4) -0.001(4) 0.002(4) C98 0.067(6) 0.051(5) 0.029(4) -0.001(4) 0.018(4) 0.011(4) C99 0.065(7) 0.098(8) 0.046(5) -0.018(5) -0.003(5) 0.007(6) C100 0.146(16) 0.174(18) 0.140(15) -0.050(13) 0.000(12) -0.012(14) C101 0.129(13) 0.124(13) 0.132(13) -0.039(10) -0.007(10) -0.002(10) C102 0.171(17) 0.150(15) 0.102(11) 0.000(11) -0.012(11) -0.007(13) C103 0.047(5) 0.032(4) 0.043(4) 0.016(3) -0.004(3) -0.004(3) C104 0.048(5) 0.046(5) 0.041(4) 0.016(4) -0.008(4) -0.003(4) C105 0.030(4) 0.049(5) 0.038(4) -0.012(4) 0.008(3) -0.007(3) C106 0.051(5) 0.059(6) 0.043(5) 0.005(4) -0.005(4) -0.002(4) C107 0.050(5) 0.077(7) 0.040(5) -0.007(5) -0.006(4) -0.008(5) C108 0.036(4) 0.055(5) 0.049(5) -0.009(4) 0.006(4) -0.003(4) C109 0.044(5) 0.042(5) 0.032(4) -0.002(3) 0.001(3) -0.004(4) C110 0.037(4) 0.047(5) 0.038(4) -0.004(4) 0.006(3) -0.003(4) C111 0.068(6) 0.038(5) 0.045(5) 0.002(4) 0.006(4) -0.015(4) C112 0.066(6) 0.028(4) 0.044(4) 0.000(3) 0.016(4) -0.003(4) C113 0.126(13) 0.163(17) 0.115(12) 0.038(12) 0.007(10) -0.041(12) C114 0.113(13) 0.143(15) 0.183(18) 0.041(13) 0.061(12) 0.022(11) Cl1 0.156(5) 0.164(5) 0.216(6) -0.050(4) 0.019(4) 0.022(4) Cl2 0.330(10) 0.119(4) 0.283(9) -0.018(5) 0.133(8) -0.005(5) Cl3 0.124(4) 0.306(8) 0.134(4) -0.040(5) -0.001(3) -0.007(4) Cl4 0.136(4) 0.215(6) 0.106(3) 0.014(3) 0.004(3) -0.020(4) N1 0.068(6) 0.094(7) 0.067(6) 0.000(5) 0.019(5) -0.015(5) N2 0.102(10) 0.122(10) 0.110(10) -0.013(8) 0.007(8) -0.020(8) N3 0.122(15) 0.144(16) 0.144(16) -0.023(14) 0.009(12) -0.011(16) N4 0.142(12) 0.092(10) 0.117(11) -0.009(8) 0.018(9) -0.001(9) N5 0.135(13) 0.162(17) 0.143(15) -0.007(16) 0.029(12) 0.027(14) N6 0.154(13) 0.156(17) 0.107(12) 0.021(11) 0.020(11) 0.044(12) O1 0.096(6) 0.115(7) 0.097(6) -0.037(5) 0.030(5) -0.028(5) O2 0.074(6) 0.134(8) 0.095(6) 0.030(5) 0.015(5) -0.003(5) O3 0.092(6) 0.192(11) 0.069(5) -0.012(6) 0.023(5) -0.032(6) O4 0.114(8) 0.182(12) 0.138(10) -0.024(9) 0.035(7) -0.020(8) O5 0.109(8) 0.162(10) 0.124(8) -0.004(7) 0.001(7) -0.039(7) O6 0.15(2) 0.17(3) 0.14(2) 0.006(17) 0.023(17) -0.01(2) O7 0.17(3) 0.16(3) 0.15(3) -0.01(3) 0.01(2) -0.01(3) O6' 0.17(3) 0.16(3) 0.16(3) -0.02(2) 0.01(2) 0.00(2) O7' 0.20(5) 0.20(5) 0.19(5) 0.00(4) 0.01(3) 0.01(5) O8 0.116(6) 0.083(5) 0.064(5) -0.015(4) 0.011(4) -0.015(5) O9 0.157(10) 0.119(8) 0.086(6) -0.026(6) -0.027(6) 0.023(7) O10 0.242(19) 0.166(14) 0.194(16) 0.000(12) -0.002(13) -0.001(13) O11 0.170(13) 0.184(14) 0.164(13) -0.061(13) 0.013(10) -0.026(13) O12 0.154(12) 0.215(17) 0.151(12) -0.038(12) 0.003(11) 0.039(11) O13 0.220(17) 0.216(17) 0.199(17) 0.032(14) 0.037(14) 0.044(13) O14 0.25(2) 0.21(2) 0.206(19) -0.003(15) -0.005(16) 0.015(15) O15 0.068(4) 0.073(5) 0.051(4) -0.019(3) 0.019(3) -0.007(3) O16 0.035(3) 0.033(3) 0.050(3) 0.007(2) 0.009(2) 0.003(2) O17 0.040(3) 0.047(3) 0.041(3) 0.007(2) 0.009(2) 0.001(2) O18 0.068(4) 0.062(4) 0.051(3) 0.008(3) 0.025(3) -0.002(3) O19 0.053(3) 0.035(3) 0.037(3) 0.004(2) 0.011(2) -0.004(2) O20 0.070(5) 0.102(6) 0.053(4) 0.024(4) 0.029(3) 0.001(4) O21 0.057(3) 0.034(3) 0.041(3) 0.005(2) 0.024(3) -0.004(3) O22 0.023(3) 0.034(3) 0.050(3) 0.000(2) 0.000(2) 0.001(2) O23 0.034(3) 0.030(3) 0.041(3) 0.000(2) 0.000(2) -0.003(2) O24 0.048(3) 0.038(3) 0.043(3) -0.006(2) 0.008(2) -0.010(2) O25 0.047(3) 0.039(3) 0.031(3) 0.001(2) 0.003(2) -0.009(2) O26 0.112(6) 0.046(4) 0.037(3) -0.005(3) 0.004(3) 0.010(3) S1 0.0645(14) 0.0359(11) 0.0573(13) -0.0057(9) 0.0277(11) -0.0047(10) S2 0.0327(10) 0.0347(10) 0.0406(10) -0.0034(8) 0.0101(8) -0.0018(8) S3 0.0354(11) 0.0538(13) 0.0477(11) -0.0124(10) 0.0004(9) -0.0013(9) S4 0.0546(14) 0.0450(13) 0.0679(14) -0.0056(11) 0.0111(11) 0.0059(10) S5 0.0444(11) 0.0408(11) 0.0410(10) -0.0008(8) 0.0107(9) 0.0112(9) S6 0.0481(12) 0.0442(12) 0.0402(10) 0.0047(9) 0.0167(9) -0.0003(9) S7 0.0335(10) 0.0381(11) 0.0543(12) 0.0085(9) 0.0115(9) 0.0044(8) S8 0.0531(12) 0.0343(11) 0.0540(12) -0.0015(9) 0.0240(10) -0.0102(9) _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 Ag1 O1 2.236(9) . ? Ag1 O8 2.359(7) . ? Ag1 S1 2.360(3) . ? Ag1 O9 2.600(10) . ? Ag1 O2 2.623(8) . ? Ag2 S5 2.482(2) . ? Ag2 S2 2.497(2) . ? Ag2 O19 2.661(5) . ? Ag2 O25 2.728(5) . ? C1 O1 1.274(12) . ? C1 C2 1.419(14) . ? C1 C6 1.428(16) . ? C2 C3 1.383(14) . ? C2 N1 1.427(14) . ? C3 C4 1.395(16) . ? C3 H3 0.9300 . ? C4 C5 1.347(16) . ? C4 N2 1.441(16) . ? C5 C6 1.333(16) . ? C5 H5 0.9300 . ? C6 N3 1.49(2) . ? C7 O8 1.260(13) . ? C7 C12 1.429(17) . ? C7 C8 1.440(17) . ? C8 C9 1.355(16) . ? C8 N4 1.462(18) . ? C9 C10 1.35(2) . ? C9 H9 0.9300 . ? C10 C11 1.34(2) . ? C10 N5 1.52(2) . ? C11 C12 1.316(18) . ? C11 H11 0.9300 . ? C12 N6 1.43(2) . ? C13 O15 1.352(9) . ? C13 C14 1.376(12) . ? C13 C18 1.400(11) . ? C14 C15 1.408(12) . ? C14 S1 1.795(8) . ? C15 C16 1.386(13) . ? C15 H15 0.9300 . ? C16 C17 1.421(14) . ? C16 C19 1.528(13) . ? C17 C18 1.363(12) . ? C17 H17 0.9300 . ? C18 S4 1.778(10) . ? C19 C22 1.537(9) . ? C19 C20 1.54(2) . ? C19 C21 1.541(9) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C28 1.385(11) . ? C23 C24 1.398(10) . ? C23 S1 1.803(8) . ? C24 C25 1.376(10) . ? C24 O19 1.379(8) . ? C25 C26 1.373(10) . ? C25 S2 1.799(7) . ? C26 C27 1.409(12) . ? C26 H26 0.9300 . ? C27 C28 1.364(12) . ? C27 C29 1.539(12) . ? C28 H28 0.9300 . ? C29 C32 1.532(9) . ? C29 C31 1.53(2) . ? C29 C30 1.55(2) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 C38 1.377(10) . ? C33 C34 1.396(10) . ? C33 S2 1.794(7) . ? C34 O16 1.357(8) . ? C34 C35 1.403(10) . ? C35 C36 1.384(11) . ? C35 S3 1.770(8) . ? C36 C37 1.391(11) . ? C36 H36 0.9300 . ? C37 C38 1.403(10) . ? C37 C39 1.528(11) . ? C38 H38 0.9300 . ? C39 C42 1.530(9) . ? C39 C40 1.542(8) . ? C39 C41 1.545(8) . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 C48 1.376(11) . ? C43 C44 1.416(11) . ? C43 S3 1.789(8) . ? C44 O17 1.381(9) . ? C44 C45 1.384(11) . ? C45 C46 1.390(11) . ? C45 S4 1.776(9) . ? C46 C47 1.389(12) . ? C46 H46 0.9300 . ? C47 C48 1.375(12) . ? C47 C49 1.538(13) . ? C48 H48 0.9300 . ? C49 C50 1.53(3) . ? C49 C52 1.539(9) . ? C49 C51 1.54(2) . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 O19 1.457(9) . ? C53 C54 1.509(12) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 O20 1.395(12) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 C56 1.388(13) . ? C55 C60 1.394(12) . ? C55 O20 1.399(12) . ? C56 C57 1.336(15) . ? C56 H56 0.9300 . ? C57 C58 1.365(13) . ? C57 H57 0.9300 . ? C58 C59 1.394(12) . ? C58 H58 0.9300 . ? C59 C60 1.346(13) . ? C59 O18 1.376(10) . ? C60 H60 0.9300 . ? C61 O18 1.389(11) . ? C61 C62 1.504(11) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 O17 1.421(9) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 O22 1.346(8) . ? C63 C64 1.387(10) . ? C63 C68 1.398(10) . ? C64 C65 1.383(11) . ? C64 S5 1.810(8) . ? C65 C66 1.373(12) . ? C65 H65 0.9300 . ? C66 C67 1.398(12) . ? C66 C69 1.545(11) . ? C67 C68 1.385(11) . ? C67 H67 0.9300 . ? C68 S6 1.795(8) . ? C69 C71 1.542(8) . ? C69 C72 1.544(8) . ? C69 C70 1.544(8) . ? C70 H70A 0.9600 . ? C70 H70B 0.9600 . ? C70 H70C 0.9600 . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C71 H71C 0.9600 . ? C72 H72A 0.9600 . ? C72 H72B 0.9600 . ? C72 H72C 0.9600 . ? C73 C74 1.380(10) . ? C73 C78 1.382(10) . ? C73 S6 1.793(7) . ? C74 O23 1.388(8) . ? C74 C75 1.411(10) . ? C75 C76 1.394(10) . ? C75 S7 1.785(7) . ? C76 C77 1.380(11) . ? C76 H76 0.9300 . ? C77 C78 1.390(11) . ? C77 C79 1.534(11) . ? C78 H78 0.9300 . ? C79 C82 1.537(8) . ? C79 C81 1.542(8) . ? C79 C80 1.547(8) . ? C80 H80A 0.9600 . ? C80 H80B 0.9600 . ? C80 H80C 0.9600 . ? C81 H81A 0.9600 . ? C81 H81B 0.9600 . ? C81 H81C 0.9600 . ? C82 H82A 0.9600 . ? C82 H82B 0.9600 . ? C82 H82C 0.9600 . ? C83 C84 1.384(10) . ? C83 C88 1.390(10) . ? C83 S7 1.788(7) . ? C84 O21 1.359(8) . ? C84 C85 1.396(10) . ? C85 C86 1.380(10) . ? C85 S8 1.786(8) . ? C86 C87 1.401(11) . ? C86 H86 0.9300 . ? C87 C88 1.386(11) . ? C87 C89 1.557(10) . ? C88 H88 0.9300 . ? C89 C92 1.532(8) . ? C89 C90 1.540(8) . ? C89 C91 1.540(8) . ? C90 H90A 0.9600 . ? C90 H90B 0.9600 . ? C90 H90C 0.9600 . ? C91 H91A 0.9600 . ? C91 H91B 0.9600 . ? C91 H91C 0.9600 . ? C92 H92A 0.9600 . ? C92 H92B 0.9600 . ? C92 H92C 0.9600 . ? C93 C98 1.373(11) . ? C93 C94 1.412(10) . ? C93 S8 1.799(8) . ? C94 O25 1.373(9) . ? C94 C95 1.379(11) . ? C95 C96 1.385(11) . ? C95 S5 1.809(7) . ? C96 C97 1.392(11) . ? C96 H96 0.9300 . ? C97 C98 1.375(12) . ? C97 C99 1.504(12) . ? C98 H98 0.9300 . ? C99 C101 1.535(9) . ? C99 C102 1.544(9) . ? C99 C100 1.546(9) . ? C100 H10A 0.9600 . ? C100 H10B 0.9600 . ? C100 H10C 0.9600 . ? C101 H10D 0.9600 . ? C101 H10E 0.9600 . ? C101 H10F 0.9600 . ? C102 H10G 0.9600 . ? C102 H10H 0.9600 . ? C102 H10I 0.9600 . ? C103 O23 1.437(8) . ? C103 C104 1.498(11) . ? C103 H10J 0.9700 . ? C103 H10K 0.9700 . ? C104 O24 1.412(9) . ? C104 H10L 0.9700 . ? C104 H10M 0.9700 . ? C105 C110 1.367(11) . ? C105 C106 1.381(11) . ? C105 O24 1.403(9) . ? C106 C107 1.383(12) . ? C106 H106 0.9300 . ? C107 C108 1.360(12) . ? C107 H107 0.9300 . ? C108 C109 1.391(11) . ? C108 H108 0.9300 . ? C109 O26 1.360(9) . ? C109 C110 1.388(11) . ? C110 H110 0.9300 . ? C111 O26 1.409(9) . ? C111 C112 1.505(12) . ? C111 H11A 0.9700 . ? C111 H11B 0.9700 . ? C112 O25 1.445(9) . ? C112 H11C 0.9700 . ? C112 H11D 0.9700 . ? C113 Cl1 1.668(18) . ? C113 Cl2 1.728(19) . ? C113 H11E 0.9700 . ? C113 H11F 0.9700 . ? C114 Cl4 1.712(18) . ? C114 Cl3 1.722(19) . ? C114 H11G 0.9700 . ? C114 H11H 0.9700 . ? N1 O3 1.200(12) . ? N1 O2 1.230(11) . ? N2 O5 1.194(14) . ? N2 O4 1.239(15) . ? N3 O7 1.21(5) . ? N3 O6 1.21(3) . ? N3 O7' 1.22(7) . ? N3 O6' 1.23(4) . ? N4 O9 1.141(15) . ? N4 O10 1.293(18) . ? N5 O11 1.19(2) . ? N5 O12 1.21(2) . ? N6 O14 1.22(2) . ? N6 O13 1.23(2) . ? O15 H15A 0.8200 . ? O16 H16 0.8200 . ? O21 H21 0.8200 . ? O22 H22 0.8200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ag1 O8 82.2(3) . . ? O1 Ag1 S1 163.3(2) . . ? O8 Ag1 S1 111.9(2) . . ? O1 Ag1 O9 85.1(4) . . ? O8 Ag1 O9 68.0(3) . . ? S1 Ag1 O9 108.0(3) . . ? O1 Ag1 O2 68.2(3) . . ? O8 Ag1 O2 150.3(3) . . ? S1 Ag1 O2 97.7(2) . . ? O9 Ag1 O2 105.7(3) . . ? S5 Ag2 S2 135.18(7) . . ? S5 Ag2 O19 136.59(13) . . ? S2 Ag2 O19 72.23(12) . . ? S5 Ag2 O25 71.43(11) . . ? S2 Ag2 O25 124.02(12) . . ? O19 Ag2 O25 126.79(15) . . ? O1 C1 C2 124.4(11) . . ? O1 C1 C6 122.5(10) . . ? C2 C1 C6 112.9(10) . . ? C3 C2 C1 123.0(11) . . ? C3 C2 N1 115.5(10) . . ? C1 C2 N1 121.5(9) . . ? C2 C3 C4 117.9(10) . . ? C2 C3 H3 121.0 . . ? C4 C3 H3 121.0 . . ? C5 C4 C3 121.8(11) . . ? C5 C4 N2 120.0(13) . . ? C3 C4 N2 118.2(12) . . ? C6 C5 C4 119.2(12) . . ? C6 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? C5 C6 C1 125.0(11) . . ? C5 C6 N3 114.9(14) . . ? C1 C6 N3 120.2(13) . . ? O8 C7 C12 122.0(13) . . ? O8 C7 C8 126.1(11) . . ? C12 C7 C8 111.8(11) . . ? C9 C8 C7 123.7(13) . . ? C9 C8 N4 119.5(14) . . ? C7 C8 N4 116.8(11) . . ? C10 C9 C8 117.6(15) . . ? C10 C9 H9 121.2 . . ? C8 C9 H9 121.2 . . ? C11 C10 C9 123.0(14) . . ? C11 C10 N5 120.0(17) . . ? C9 C10 N5 116.8(18) . . ? C12 C11 C10 119.6(15) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C11 C12 C7 124.1(15) . . ? C11 C12 N6 118.7(15) . . ? C7 C12 N6 117.2(14) . . ? O15 C13 C14 117.3(7) . . ? O15 C13 C18 124.6(8) . . ? C14 C13 C18 118.0(7) . . ? C13 C14 C15 121.5(8) . . ? C13 C14 S1 117.2(6) . . ? C15 C14 S1 121.3(7) . . ? C16 C15 C14 121.4(9) . . ? C16 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? C15 C16 C17 115.6(8) . . ? C15 C16 C19 120.6(9) . . ? C17 C16 C19 123.8(8) . . ? C18 C17 C16 123.1(8) . . ? C18 C17 H17 118.4 . . ? C16 C17 H17 118.4 . . ? C17 C18 C13 120.3(9) . . ? C17 C18 S4 121.0(7) . . ? C13 C18 S4 118.6(6) . . ? C16 C19 C22 110.4(10) . . ? C16 C19 C20 110.4(10) . . ? C22 C19 C20 109.4(10) . . ? C16 C19 C21 108.4(10) . . ? C22 C19 C21 110.7(9) . . ? C20 C19 C21 107.6(10) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C28 C23 C24 120.9(7) . . ? C28 C23 S1 119.4(6) . . ? C24 C23 S1 119.3(6) . . ? C25 C24 O19 120.1(6) . . ? C25 C24 C23 117.5(6) . . ? O19 C24 C23 122.3(6) . . ? C26 C25 C24 121.5(7) . . ? C26 C25 S2 116.3(6) . . ? C24 C25 S2 122.2(5) . . ? C25 C26 C27 121.2(8) . . ? C25 C26 H26 119.4 . . ? C27 C26 H26 119.4 . . ? C28 C27 C26 117.2(8) . . ? C28 C27 C29 121.5(8) . . ? C26 C27 C29 121.3(8) . . ? C27 C28 C23 121.8(8) . . ? C27 C28 H28 119.1 . . ? C23 C28 H28 119.1 . . ? C32 C29 C31 111.6(10) . . ? C32 C29 C27 111.8(9) . . ? C31 C29 C27 106.3(12) . . ? C32 C29 C30 107.6(10) . . ? C31 C29 C30 111.2(11) . . ? C27 C29 C30 108.3(11) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C38 C33 C34 121.4(6) . . ? C38 C33 S2 117.2(6) . . ? C34 C33 S2 121.2(5) . . ? O16 C34 C33 118.8(6) . . ? O16 C34 C35 123.2(7) . . ? C33 C34 C35 118.0(6) . . ? C36 C35 C34 119.3(7) . . ? C36 C35 S3 120.0(6) . . ? C34 C35 S3 120.7(6) . . ? C35 C36 C37 123.4(7) . . ? C35 C36 H36 118.3 . . ? C37 C36 H36 118.3 . . ? C36 C37 C38 116.3(7) . . ? C36 C37 C39 120.2(7) . . ? C38 C37 C39 123.3(7) . . ? C33 C38 C37 121.4(7) . . ? C33 C38 H38 119.3 . . ? C37 C38 H38 119.3 . . ? C37 C39 C42 111.6(8) . . ? C37 C39 C40 109.5(8) . . ? C42 C39 C40 111.2(9) . . ? C37 C39 C41 110.8(7) . . ? C42 C39 C41 106.4(8) . . ? C40 C39 C41 107.2(8) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C39 C42 H42A 109.5 . . ? C39 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C39 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C48 C43 C44 119.8(7) . . ? C48 C43 S3 121.7(6) . . ? C44 C43 S3 118.6(6) . . ? O17 C44 C45 121.3(7) . . ? O17 C44 C43 119.6(6) . . ? C45 C44 C43 118.7(7) . . ? C44 C45 C46 119.4(8) . . ? C44 C45 S4 120.8(6) . . ? C46 C45 S4 119.8(6) . . ? C47 C46 C45 122.4(8) . . ? C47 C46 H46 118.8 . . ? C45 C46 H46 118.8 . . ? C48 C47 C46 117.2(8) . . ? C48 C47 C49 122.7(9) . . ? C46 C47 C49 120.1(8) . . ? C47 C48 C43 122.3(8) . . ? C47 C48 H48 118.8 . . ? C43 C48 H48 118.8 . . ? C50 C49 C47 109.4(14) . . ? C50 C49 C52 112.6(12) . . ? C47 C49 C52 110.9(10) . . ? C50 C49 C51 107.6(11) . . ? C47 C49 C51 109.9(10) . . ? C52 C49 C51 106.4(10) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C49 C52 H52A 109.5 . . ? C49 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C49 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O19 C53 C54 110.2(7) . . ? O19 C53 H53A 109.6 . . ? C54 C53 H53A 109.6 . . ? O19 C53 H53B 109.6 . . ? C54 C53 H53B 109.6 . . ? H53A C53 H53B 108.1 . . ? O20 C54 C53 113.7(8) . . ? O20 C54 H54A 108.8 . . ? C53 C54 H54A 108.8 . . ? O20 C54 H54B 108.8 . . ? C53 C54 H54B 108.8 . . ? H54A C54 H54B 107.7 . . ? C56 C55 C60 118.9(10) . . ? C56 C55 O20 116.4(8) . . ? C60 C55 O20 124.7(8) . . ? C57 C56 C55 119.9(9) . . ? C57 C56 H56 120.1 . . ? C55 C56 H56 120.1 . . ? C56 C57 C58 122.2(9) . . ? C56 C57 H57 118.9 . . ? C58 C57 H57 118.9 . . ? C57 C58 C59 118.3(10) . . ? C57 C58 H58 120.9 . . ? C59 C58 H58 120.9 . . ? C60 C59 O18 115.6(7) . . ? C60 C59 C58 120.6(8) . . ? O18 C59 C58 123.7(9) . . ? C59 C60 C55 120.1(8) . . ? C59 C60 H60 120.0 . . ? C55 C60 H60 120.0 . . ? O18 C61 C62 108.1(7) . . ? O18 C61 H61A 110.1 . . ? C62 C61 H61A 110.1 . . ? O18 C61 H61B 110.1 . . ? C62 C61 H61B 110.1 . . ? H61A C61 H61B 108.4 . . ? O17 C62 C61 105.9(7) . . ? O17 C62 H62A 110.6 . . ? C61 C62 H62A 110.6 . . ? O17 C62 H62B 110.6 . . ? C61 C62 H62B 110.6 . . ? H62A C62 H62B 108.7 . . ? O22 C63 C64 119.4(7) . . ? O22 C63 C68 124.2(7) . . ? C64 C63 C68 116.4(6) . . ? C65 C64 C63 122.1(7) . . ? C65 C64 S5 117.6(6) . . ? C63 C64 S5 120.3(6) . . ? C66 C65 C64 121.3(8) . . ? C66 C65 H65 119.4 . . ? C64 C65 H65 119.4 . . ? C65 C66 C67 117.9(7) . . ? C65 C66 C69 121.7(8) . . ? C67 C66 C69 120.1(8) . . ? C68 C67 C66 120.6(8) . . ? C68 C67 H67 119.7 . . ? C66 C67 H67 119.7 . . ? C67 C68 C63 121.8(7) . . ? C67 C68 S6 119.2(6) . . ? C63 C68 S6 119.0(5) . . ? C71 C69 C72 112.2(9) . . ? C71 C69 C70 108.2(8) . . ? C72 C69 C70 108.6(8) . . ? C71 C69 C66 110.9(7) . . ? C72 C69 C66 105.7(7) . . ? C70 C69 C66 111.2(7) . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C69 C71 H71A 109.5 . . ? C69 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C69 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C69 C72 H72A 109.5 . . ? C69 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C69 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C74 C73 C78 119.4(6) . . ? C74 C73 S6 119.1(5) . . ? C78 C73 S6 121.5(5) . . ? C73 C74 O23 120.5(6) . . ? C73 C74 C75 119.9(6) . . ? O23 C74 C75 119.3(6) . . ? C76 C75 C74 118.5(7) . . ? C76 C75 S7 121.2(5) . . ? C74 C75 S7 119.9(6) . . ? C77 C76 C75 122.5(7) . . ? C77 C76 H76 118.8 . . ? C75 C76 H76 118.8 . . ? C76 C77 C78 117.1(7) . . ? C76 C77 C79 123.8(7) . . ? C78 C77 C79 119.1(7) . . ? C73 C78 C77 122.6(7) . . ? C73 C78 H78 118.7 . . ? C77 C78 H78 118.7 . . ? C77 C79 C82 111.6(7) . . ? C77 C79 C81 109.6(7) . . ? C82 C79 C81 107.0(8) . . ? C77 C79 C80 108.8(7) . . ? C82 C79 C80 110.7(8) . . ? C81 C79 C80 109.1(8) . . ? C79 C80 H80A 109.5 . . ? C79 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C79 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C79 C81 H81A 109.5 . . ? C79 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C79 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C79 C82 H82A 109.5 . . ? C79 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C79 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C84 C83 C88 121.2(7) . . ? C84 C83 S7 120.6(5) . . ? C88 C83 S7 117.7(6) . . ? O21 C84 C83 124.4(6) . . ? O21 C84 C85 117.6(6) . . ? C83 C84 C85 118.0(6) . . ? C86 C85 C84 121.0(7) . . ? C86 C85 S8 119.6(6) . . ? C84 C85 S8 119.4(5) . . ? C85 C86 C87 120.9(7) . . ? C85 C86 H86 119.5 . . ? C87 C86 H86 119.5 . . ? C88 C87 C86 117.8(7) . . ? C88 C87 C89 123.2(7) . . ? C86 C87 C89 118.9(7) . . ? C87 C88 C83 120.9(7) . . ? C87 C88 H88 119.5 . . ? C83 C88 H88 119.5 . . ? C92 C89 C90 109.4(8) . . ? C92 C89 C91 108.9(8) . . ? C90 C89 C91 109.7(9) . . ? C92 C89 C87 108.7(7) . . ? C90 C89 C87 109.2(7) . . ? C91 C89 C87 110.9(7) . . ? C89 C90 H90A 109.5 . . ? C89 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? C89 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? C89 C91 H91A 109.5 . . ? C89 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C89 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? C89 C92 H92A 109.5 . . ? C89 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C89 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C98 C93 C94 120.0(7) . . ? C98 C93 S8 118.9(6) . . ? C94 C93 S8 120.8(6) . . ? O25 C94 C95 120.4(6) . . ? O25 C94 C93 122.7(7) . . ? C95 C94 C93 116.6(7) . . ? C94 C95 C96 122.1(7) . . ? C94 C95 S5 121.8(6) . . ? C96 C95 S5 116.0(6) . . ? C95 C96 C97 121.5(8) . . ? C95 C96 H96 119.2 . . ? C97 C96 H96 119.2 . . ? C98 C97 C96 115.9(7) . . ? C98 C97 C99 120.7(8) . . ? C96 C97 C99 123.3(8) . . ? C93 C98 C97 123.8(7) . . ? C93 C98 H98 118.1 . . ? C97 C98 H98 118.1 . . ? C97 C99 C101 108.7(8) . . ? C97 C99 C102 109.3(9) . . ? C101 C99 C102 107.8(9) . . ? C97 C99 C100 112.7(9) . . ? C101 C99 C100 109.7(9) . . ? C102 C99 C100 108.6(9) . . ? C99 C100 H10A 109.5 . . ? C99 C100 H10B 109.5 . . ? H10A C100 H10B 109.5 . . ? C99 C100 H10C 109.5 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? C99 C101 H10D 109.5 . . ? C99 C101 H10E 109.5 . . ? H10D C101 H10E 109.5 . . ? C99 C101 H10F 109.5 . . ? H10D C101 H10F 109.5 . . ? H10E C101 H10F 109.5 . . ? C99 C102 H10G 109.5 . . ? C99 C102 H10H 109.5 . . ? H10G C102 H10H 109.5 . . ? C99 C102 H10I 109.5 . . ? H10G C102 H10I 109.5 . . ? H10H C102 H10I 109.5 . . ? O23 C103 C104 106.9(6) . . ? O23 C103 H10J 110.3 . . ? C104 C103 H10J 110.3 . . ? O23 C103 H10K 110.3 . . ? C104 C103 H10K 110.3 . . ? H10J C103 H10K 108.6 . . ? O24 C104 C103 107.5(6) . . ? O24 C104 H10L 110.2 . . ? C103 C104 H10L 110.2 . . ? O24 C104 H10M 110.2 . . ? C103 C104 H10M 110.2 . . ? H10L C104 H10M 108.5 . . ? C110 C105 C106 122.1(8) . . ? C110 C105 O24 116.7(6) . . ? C106 C105 O24 121.1(7) . . ? C105 C106 C107 118.0(8) . . ? C105 C106 H106 121.0 . . ? C107 C106 H106 121.0 . . ? C108 C107 C106 121.2(8) . . ? C108 C107 H107 119.4 . . ? C106 C107 H107 119.4 . . ? C107 C108 C109 120.1(8) . . ? C107 C108 H108 119.9 . . ? C109 C108 H108 119.9 . . ? O26 C109 C110 124.6(7) . . ? O26 C109 C108 115.8(7) . . ? C110 C109 C108 119.6(7) . . ? C105 C110 C109 119.0(7) . . ? C105 C110 H110 120.5 . . ? C109 C110 H110 120.5 . . ? O26 C111 C112 112.7(7) . . ? O26 C111 H11A 109.0 . . ? C112 C111 H11A 109.0 . . ? O26 C111 H11B 109.0 . . ? C112 C111 H11B 109.0 . . ? H11A C111 H11B 107.8 . . ? O25 C112 C111 110.5(6) . . ? O25 C112 H11C 109.6 . . ? C111 C112 H11C 109.6 . . ? O25 C112 H11D 109.6 . . ? C111 C112 H11D 109.6 . . ? H11C C112 H11D 108.1 . . ? Cl1 C113 Cl2 112.4(10) . . ? Cl1 C113 H11E 109.1 . . ? Cl2 C113 H11E 109.1 . . ? Cl1 C113 H11F 109.1 . . ? Cl2 C113 H11F 109.1 . . ? H11E C113 H11F 107.9 . . ? Cl4 C114 Cl3 111.9(9) . . ? Cl4 C114 H11G 109.2 . . ? Cl3 C114 H11G 109.2 . . ? Cl4 C114 H11H 109.2 . . ? Cl3 C114 H11H 109.2 . . ? H11G C114 H11H 107.9 . . ? O3 N1 O2 121.3(10) . . ? O3 N1 C2 118.9(10) . . ? O2 N1 C2 119.8(10) . . ? O5 N2 O4 120.6(14) . . ? O5 N2 C4 120.3(14) . . ? O4 N2 C4 119.0(13) . . ? O7 N3 O6 120(3) . . ? O7 N3 O7' 45(3) . . ? O6 N3 O7' 89(4) . . ? O7 N3 O6' 97(3) . . ? O6 N3 O6' 73(2) . . ? O7' N3 O6' 121(4) . . ? O7 N3 C6 117(3) . . ? O6 N3 C6 123(2) . . ? O7' N3 C6 128(4) . . ? O6' N3 C6 108(2) . . ? O9 N4 O10 120.2(17) . . ? O9 N4 C8 128.0(15) . . ? O10 N4 C8 111.1(16) . . ? O11 N5 O12 125(2) . . ? O11 N5 C10 118(2) . . ? O12 N5 C10 117(2) . . ? O14 N6 O13 118(2) . . ? O14 N6 C12 124.9(18) . . ? O13 N6 C12 117.5(19) . . ? C1 O1 Ag1 138.4(7) . . ? N1 O2 Ag1 117.0(7) . . ? C7 O8 Ag1 128.0(8) . . ? N4 O9 Ag1 111.1(10) . . ? C13 O15 H15A 109.5 . . ? C34 O16 H16 109.5 . . ? C44 O17 C62 117.5(6) . . ? C59 O18 C61 118.0(7) . . ? C24 O19 C53 116.0(6) . . ? C24 O19 Ag2 115.7(4) . . ? C53 O19 Ag2 111.6(4) . . ? C54 O20 C55 119.1(7) . . ? C84 O21 H21 109.5 . . ? C63 O22 H22 109.5 . . ? C74 O23 C103 116.4(5) . . ? C105 O24 C104 115.9(6) . . ? C94 O25 C112 118.0(5) . . ? C94 O25 Ag2 115.5(4) . . ? C112 O25 Ag2 111.0(4) . . ? C109 O26 C111 120.8(6) . . ? C14 S1 C23 98.9(4) . . ? C14 S1 Ag1 110.3(3) . . ? C23 S1 Ag1 104.8(3) . . ? C33 S2 C25 98.6(3) . . ? C33 S2 Ag2 103.5(2) . . ? C25 S2 Ag2 106.5(2) . . ? C35 S3 C43 101.6(3) . . ? C45 S4 C18 100.3(4) . . ? C95 S5 C64 99.9(3) . . ? C95 S5 Ag2 108.2(3) . . ? C64 S5 Ag2 102.2(2) . . ? C73 S6 C68 100.7(3) . . ? C75 S7 C83 104.9(3) . . ? C85 S8 C93 98.8(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -177.8(11) . . . . ? C6 C1 C2 C3 -3.5(16) . . . . ? O1 C1 C2 N1 2.9(18) . . . . ? C6 C1 C2 N1 177.2(10) . . . . ? C1 C2 C3 C4 1.5(17) . . . . ? N1 C2 C3 C4 -179.2(10) . . . . ? C2 C3 C4 C5 0.2(19) . . . . ? C2 C3 C4 N2 179.8(11) . . . . ? C3 C4 C5 C6 1(2) . . . . ? N2 C4 C5 C6 -179.0(13) . . . . ? C4 C5 C6 C1 -3(2) . . . . ? C4 C5 C6 N3 176.2(13) . . . . ? O1 C1 C6 C5 178.9(13) . . . . ? C2 C1 C6 C5 4.5(19) . . . . ? O1 C1 C6 N3 0(2) . . . . ? C2 C1 C6 N3 -174.9(12) . . . . ? O8 C7 C8 C9 -179.1(12) . . . . ? C12 C7 C8 C9 1.4(17) . . . . ? O8 C7 C8 N4 1.7(18) . . . . ? C12 C7 C8 N4 -177.8(11) . . . . ? C7 C8 C9 C10 -2(2) . . . . ? N4 C8 C9 C10 176.7(13) . . . . ? C8 C9 C10 C11 0(2) . . . . ? C8 C9 C10 N5 -174.4(13) . . . . ? C9 C10 C11 C12 4(2) . . . . ? N5 C10 C11 C12 178.0(13) . . . . ? C10 C11 C12 C7 -5(2) . . . . ? C10 C11 C12 N6 177.4(14) . . . . ? O8 C7 C12 C11 -177.0(12) . . . . ? C8 C7 C12 C11 2.6(17) . . . . ? O8 C7 C12 N6 0.4(18) . . . . ? C8 C7 C12 N6 179.9(12) . . . . ? O15 C13 C14 C15 -177.2(8) . . . . ? C18 C13 C14 C15 -0.3(13) . . . . ? O15 C13 C14 S1 -0.1(11) . . . . ? C18 C13 C14 S1 176.8(6) . . . . ? C13 C14 C15 C16 2.0(15) . . . . ? S1 C14 C15 C16 -175.0(8) . . . . ? C14 C15 C16 C17 -2.9(15) . . . . ? C14 C15 C16 C19 175.7(9) . . . . ? C15 C16 C17 C18 2.5(15) . . . . ? C19 C16 C17 C18 -176.0(10) . . . . ? C16 C17 C18 C13 -1.0(15) . . . . ? C16 C17 C18 S4 -178.9(8) . . . . ? O15 C13 C18 C17 176.5(9) . . . . ? C14 C13 C18 C17 -0.1(13) . . . . ? O15 C13 C18 S4 -5.6(12) . . . . ? C14 C13 C18 S4 177.8(7) . . . . ? C15 C16 C19 C22 179.8(11) . . . . ? C17 C16 C19 C22 -1.7(15) . . . . ? C15 C16 C19 C20 -59.2(14) . . . . ? C17 C16 C19 C20 119.3(12) . . . . ? C15 C16 C19 C21 58.4(14) . . . . ? C17 C16 C19 C21 -123.1(12) . . . . ? C28 C23 C24 C25 2.4(12) . . . . ? S1 C23 C24 C25 -170.7(6) . . . . ? C28 C23 C24 O19 178.1(7) . . . . ? S1 C23 C24 O19 5.0(10) . . . . ? O19 C24 C25 C26 -177.9(7) . . . . ? C23 C24 C25 C26 -2.2(11) . . . . ? O19 C24 C25 S2 -0.5(10) . . . . ? C23 C24 C25 S2 175.2(6) . . . . ? C24 C25 C26 C27 1.8(13) . . . . ? S2 C25 C26 C27 -175.7(7) . . . . ? C25 C26 C27 C28 -1.5(14) . . . . ? C25 C26 C27 C29 174.5(9) . . . . ? C26 C27 C28 C23 1.8(15) . . . . ? C29 C27 C28 C23 -174.3(10) . . . . ? C24 C23 C28 C27 -2.3(14) . . . . ? S1 C23 C28 C27 170.8(8) . . . . ? C28 C27 C29 C32 152.1(11) . . . . ? C26 C27 C29 C32 -23.8(15) . . . . ? C28 C27 C29 C31 -85.9(14) . . . . ? C26 C27 C29 C31 98.2(13) . . . . ? C28 C27 C29 C30 33.7(15) . . . . ? C26 C27 C29 C30 -142.2(12) . . . . ? C38 C33 C34 O16 177.0(6) . . . . ? S2 C33 C34 O16 1.7(8) . . . . ? C38 C33 C34 C35 -4.1(10) . . . . ? S2 C33 C34 C35 -179.5(5) . . . . ? O16 C34 C35 C36 -177.4(6) . . . . ? C33 C34 C35 C36 3.8(10) . . . . ? O16 C34 C35 S3 2.0(9) . . . . ? C33 C34 C35 S3 -176.8(5) . . . . ? C34 C35 C36 C37 -1.1(11) . . . . ? S3 C35 C36 C37 179.5(6) . . . . ? C35 C36 C37 C38 -1.4(11) . . . . ? C35 C36 C37 C39 173.3(7) . . . . ? C34 C33 C38 C37 1.6(10) . . . . ? S2 C33 C38 C37 177.2(5) . . . . ? C36 C37 C38 C33 1.1(10) . . . . ? C39 C37 C38 C33 -173.4(7) . . . . ? C36 C37 C39 C42 175.7(9) . . . . ? C38 C37 C39 C42 -9.9(12) . . . . ? C36 C37 C39 C40 -60.7(11) . . . . ? C38 C37 C39 C40 113.6(9) . . . . ? C36 C37 C39 C41 57.3(10) . . . . ? C38 C37 C39 C41 -128.4(8) . . . . ? C48 C43 C44 O17 169.9(7) . . . . ? S3 C43 C44 O17 -11.2(9) . . . . ? C48 C43 C44 C45 -2.2(11) . . . . ? S3 C43 C44 C45 176.6(6) . . . . ? O17 C44 C45 C46 -170.6(7) . . . . ? C43 C44 C45 C46 1.5(12) . . . . ? O17 C44 C45 S4 9.9(10) . . . . ? C43 C44 C45 S4 -178.1(6) . . . . ? C44 C45 C46 C47 1.6(13) . . . . ? S4 C45 C46 C47 -178.9(7) . . . . ? C45 C46 C47 C48 -3.8(14) . . . . ? C45 C46 C47 C49 178.2(9) . . . . ? C46 C47 C48 C43 3.0(13) . . . . ? C49 C47 C48 C43 -179.1(9) . . . . ? C44 C43 C48 C47 0.0(12) . . . . ? S3 C43 C48 C47 -178.8(7) . . . . ? C48 C47 C49 C50 102.3(14) . . . . ? C46 C47 C49 C50 -79.7(14) . . . . ? C48 C47 C49 C52 -22.4(14) . . . . ? C46 C47 C49 C52 155.5(10) . . . . ? C48 C47 C49 C51 -139.7(11) . . . . ? C46 C47 C49 C51 38.2(14) . . . . ? O19 C53 C54 O20 -72.5(9) . . . . ? C60 C55 C56 C57 0.0(15) . . . . ? O20 C55 C56 C57 177.9(9) . . . . ? C55 C56 C57 C58 -1.0(16) . . . . ? C56 C57 C58 C59 1.3(15) . . . . ? C57 C58 C59 C60 -0.7(13) . . . . ? C57 C58 C59 O18 176.8(8) . . . . ? O18 C59 C60 C55 -177.9(7) . . . . ? C58 C59 C60 C55 -0.2(13) . . . . ? C56 C55 C60 C59 0.6(13) . . . . ? O20 C55 C60 C59 -177.2(8) . . . . ? O18 C61 C62 O17 -46.6(10) . . . . ? O22 C63 C64 C65 -179.9(6) . . . . ? C68 C63 C64 C65 0.2(10) . . . . ? O22 C63 C64 S5 0.1(9) . . . . ? C68 C63 C64 S5 -179.7(5) . . . . ? C63 C64 C65 C66 0.0(11) . . . . ? S5 C64 C65 C66 179.9(6) . . . . ? C64 C65 C66 C67 -0.4(11) . . . . ? C64 C65 C66 C69 -173.5(7) . . . . ? C65 C66 C67 C68 0.5(11) . . . . ? C69 C66 C67 C68 173.8(7) . . . . ? C66 C67 C68 C63 -0.3(11) . . . . ? C66 C67 C68 S6 177.9(6) . . . . ? O22 C63 C68 C67 -179.9(6) . . . . ? C64 C63 C68 C67 -0.1(10) . . . . ? O22 C63 C68 S6 1.9(9) . . . . ? C64 C63 C68 S6 -178.2(5) . . . . ? C65 C66 C69 C71 -154.0(8) . . . . ? C67 C66 C69 C71 33.0(11) . . . . ? C65 C66 C69 C72 84.2(10) . . . . ? C67 C66 C69 C72 -88.8(10) . . . . ? C65 C66 C69 C70 -33.5(10) . . . . ? C67 C66 C69 C70 153.5(8) . . . . ? C78 C73 C74 O23 173.5(6) . . . . ? S6 C73 C74 O23 -7.8(9) . . . . ? C78 C73 C74 C75 0.0(10) . . . . ? S6 C73 C74 C75 178.7(5) . . . . ? C73 C74 C75 C76 0.0(10) . . . . ? O23 C74 C75 C76 -173.6(6) . . . . ? C73 C74 C75 S7 -172.8(5) . . . . ? O23 C74 C75 S7 13.6(9) . . . . ? C74 C75 C76 C77 -0.2(11) . . . . ? S7 C75 C76 C77 172.5(6) . . . . ? C75 C76 C77 C78 0.4(12) . . . . ? C75 C76 C77 C79 179.8(7) . . . . ? C74 C73 C78 C77 0.2(12) . . . . ? S6 C73 C78 C77 -178.4(6) . . . . ? C76 C77 C78 C73 -0.4(12) . . . . ? C79 C77 C78 C73 -179.8(7) . . . . ? C76 C77 C79 C82 1.5(12) . . . . ? C78 C77 C79 C82 -179.2(9) . . . . ? C76 C77 C79 C81 119.9(9) . . . . ? C78 C77 C79 C81 -60.8(10) . . . . ? C76 C77 C79 C80 -121.0(9) . . . . ? C78 C77 C79 C80 58.4(10) . . . . ? C88 C83 C84 O21 -176.9(7) . . . . ? S7 C83 C84 O21 -4.8(10) . . . . ? C88 C83 C84 C85 1.2(11) . . . . ? S7 C83 C84 C85 173.3(6) . . . . ? O21 C84 C85 C86 177.8(7) . . . . ? C83 C84 C85 C86 -0.5(11) . . . . ? O21 C84 C85 S8 -3.7(10) . . . . ? C83 C84 C85 S8 178.0(5) . . . . ? C84 C85 C86 C87 -2.3(12) . . . . ? S8 C85 C86 C87 179.2(6) . . . . ? C85 C86 C87 C88 4.2(12) . . . . ? C85 C86 C87 C89 -177.2(7) . . . . ? C86 C87 C88 C83 -3.4(11) . . . . ? C89 C87 C88 C83 178.0(7) . . . . ? C84 C83 C88 C87 0.8(11) . . . . ? S7 C83 C88 C87 -171.5(6) . . . . ? C88 C87 C89 C92 115.0(9) . . . . ? C86 C87 C89 C92 -63.5(10) . . . . ? C88 C87 C89 C90 -125.7(10) . . . . ? C86 C87 C89 C90 55.8(11) . . . . ? C88 C87 C89 C91 -4.7(12) . . . . ? C86 C87 C89 C91 176.8(9) . . . . ? C98 C93 C94 O25 174.0(7) . . . . ? S8 C93 C94 O25 -0.4(10) . . . . ? C98 C93 C94 C95 -0.1(10) . . . . ? S8 C93 C94 C95 -174.6(5) . . . . ? O25 C94 C95 C96 -172.4(7) . . . . ? C93 C94 C95 C96 1.9(11) . . . . ? O25 C94 C95 S5 3.1(10) . . . . ? C93 C94 C95 S5 177.4(5) . . . . ? C94 C95 C96 C97 -1.0(12) . . . . ? S5 C95 C96 C97 -176.7(6) . . . . ? C95 C96 C97 C98 -1.7(12) . . . . ? C95 C96 C97 C99 174.1(8) . . . . ? C94 C93 C98 C97 -2.7(12) . . . . ? S8 C93 C98 C97 171.8(7) . . . . ? C96 C97 C98 C93 3.6(12) . . . . ? C99 C97 C98 C93 -172.3(8) . . . . ? C98 C97 C99 C101 54.8(12) . . . . ? C96 C97 C99 C101 -120.7(10) . . . . ? C98 C97 C99 C102 -62.5(12) . . . . ? C96 C97 C99 C102 121.9(10) . . . . ? C98 C97 C99 C100 176.7(10) . . . . ? C96 C97 C99 C100 1.1(13) . . . . ? O23 C103 C104 O24 -59.7(8) . . . . ? C110 C105 C106 C107 -1.1(12) . . . . ? O24 C105 C106 C107 -177.7(7) . . . . ? C105 C106 C107 C108 0.2(13) . . . . ? C106 C107 C108 C109 -0.1(13) . . . . ? C107 C108 C109 O26 178.5(8) . . . . ? C107 C108 C109 C110 0.8(12) . . . . ? C106 C105 C110 C109 1.9(11) . . . . ? O24 C105 C110 C109 178.6(6) . . . . ? O26 C109 C110 C105 -179.1(7) . . . . ? C108 C109 C110 C105 -1.7(11) . . . . ? O26 C111 C112 O25 -66.5(8) . . . . ? C3 C2 N1 O3 30.3(15) . . . . ? C1 C2 N1 O3 -150.3(11) . . . . ? C3 C2 N1 O2 -149.9(10) . . . . ? C1 C2 N1 O2 29.5(15) . . . . ? C5 C4 N2 O5 -3(2) . . . . ? C3 C4 N2 O5 177.0(13) . . . . ? C5 C4 N2 O4 174.3(14) . . . . ? C3 C4 N2 O4 -5(2) . . . . ? C5 C6 N3 O7 22(3) . . . . ? C1 C6 N3 O7 -158(2) . . . . ? C5 C6 N3 O6 -149(2) . . . . ? C1 C6 N3 O6 30(3) . . . . ? C5 C6 N3 O7' -31(5) . . . . ? C1 C6 N3 O7' 149(5) . . . . ? C5 C6 N3 O6' 130(3) . . . . ? C1 C6 N3 O6' -50(3) . . . . ? C9 C8 N4 O9 -154.2(16) . . . . ? C7 C8 N4 O9 25(2) . . . . ? C9 C8 N4 O10 35.6(19) . . . . ? C7 C8 N4 O10 -145.1(14) . . . . ? C11 C10 N5 O11 -176.1(18) . . . . ? C9 C10 N5 O11 -2(3) . . . . ? C11 C10 N5 O12 -5(3) . . . . ? C9 C10 N5 O12 169.4(17) . . . . ? C11 C12 N6 O14 -161(2) . . . . ? C7 C12 N6 O14 21(3) . . . . ? C11 C12 N6 O13 16(2) . . . . ? C7 C12 N6 O13 -161.8(17) . . . . ? C2 C1 O1 Ag1 15(2) . . . . ? C6 C1 O1 Ag1 -158.5(10) . . . . ? O8 Ag1 O1 C1 150.0(13) . . . . ? S1 Ag1 O1 C1 1(2) . . . . ? O9 Ag1 O1 C1 -141.6(13) . . . . ? O2 Ag1 O1 C1 -32.5(12) . . . . ? O3 N1 O2 Ag1 115.5(10) . . . . ? C2 N1 O2 Ag1 -64.3(12) . . . . ? O1 Ag1 O2 N1 53.8(8) . . . . ? O8 Ag1 O2 N1 58.7(12) . . . . ? S1 Ag1 O2 N1 -116.9(8) . . . . ? O9 Ag1 O2 N1 131.8(9) . . . . ? C12 C7 O8 Ag1 -149.1(9) . . . . ? C8 C7 O8 Ag1 31.4(17) . . . . ? O1 Ag1 O8 C7 39.6(10) . . . . ? S1 Ag1 O8 C7 -149.6(9) . . . . ? O9 Ag1 O8 C7 -48.2(10) . . . . ? O2 Ag1 O8 C7 35.1(13) . . . . ? O10 N4 O9 Ag1 103.2(16) . . . . ? C8 N4 O9 Ag1 -66.2(18) . . . . ? O1 Ag1 O9 N4 -22.8(12) . . . . ? O8 Ag1 O9 N4 60.7(11) . . . . ? S1 Ag1 O9 N4 167.7(11) . . . . ? O2 Ag1 O9 N4 -88.5(12) . . . . ? C45 C44 O17 C62 -87.7(9) . . . . ? C43 C44 O17 C62 100.3(9) . . . . ? C61 C62 O17 C44 -171.1(7) . . . . ? C60 C59 O18 C61 -150.0(8) . . . . ? C58 C59 O18 C61 32.4(12) . . . . ? C62 C61 O18 C59 168.3(7) . . . . ? C25 C24 O19 C53 -119.2(7) . . . . ? C23 C24 O19 C53 65.2(9) . . . . ? C25 C24 O19 Ag2 14.3(8) . . . . ? C23 C24 O19 Ag2 -161.2(6) . . . . ? C54 C53 O19 C24 -139.8(7) . . . . ? C54 C53 O19 Ag2 84.9(7) . . . . ? S5 Ag2 O19 C24 121.7(4) . . . . ? S2 Ag2 O19 C24 -16.5(4) . . . . ? O25 Ag2 O19 C24 -136.1(4) . . . . ? S5 Ag2 O19 C53 -102.8(5) . . . . ? S2 Ag2 O19 C53 119.0(5) . . . . ? O25 Ag2 O19 C53 -0.6(5) . . . . ? C53 C54 O20 C55 103.6(9) . . . . ? C56 C55 O20 C54 158.6(8) . . . . ? C60 C55 O20 C54 -23.6(13) . . . . ? C73 C74 O23 C103 92.6(8) . . . . ? C75 C74 O23 C103 -93.8(7) . . . . ? C104 C103 O23 C74 -165.9(6) . . . . ? C110 C105 O24 C104 -126.7(7) . . . . ? C106 C105 O24 C104 50.0(9) . . . . ? C103 C104 O24 C105 159.8(6) . . . . ? C95 C94 O25 C112 -124.6(7) . . . . ? C93 C94 O25 C112 61.5(9) . . . . ? C95 C94 O25 Ag2 10.0(8) . . . . ? C93 C94 O25 Ag2 -163.9(5) . . . . ? C111 C112 O25 C94 -138.9(7) . . . . ? C111 C112 O25 Ag2 84.6(6) . . . . ? S5 Ag2 O25 C94 -13.9(4) . . . . ? S2 Ag2 O25 C94 118.6(4) . . . . ? O19 Ag2 O25 C94 -148.8(4) . . . . ? S5 Ag2 O25 C112 123.7(5) . . . . ? S2 Ag2 O25 C112 -103.7(4) . . . . ? O19 Ag2 O25 C112 -11.1(5) . . . . ? C110 C109 O26 C111 -28.7(12) . . . . ? C108 C109 O26 C111 153.8(7) . . . . ? C112 C111 O26 C109 111.8(9) . . . . ? C13 C14 S1 C23 -82.6(7) . . . . ? C15 C14 S1 C23 94.5(8) . . . . ? C13 C14 S1 Ag1 167.9(6) . . . . ? C15 C14 S1 Ag1 -15.0(9) . . . . ? C28 C23 S1 C14 -47.3(8) . . . . ? C24 C23 S1 C14 125.8(7) . . . . ? C28 C23 S1 Ag1 66.5(7) . . . . ? C24 C23 S1 Ag1 -120.4(6) . . . . ? O1 Ag1 S1 C14 -179.5(10) . . . . ? O8 Ag1 S1 C14 34.2(4) . . . . ? O9 Ag1 S1 C14 -38.8(4) . . . . ? O2 Ag1 S1 C14 -148.2(4) . . . . ? O1 Ag1 S1 C23 75.0(10) . . . . ? O8 Ag1 S1 C23 -71.3(3) . . . . ? O9 Ag1 S1 C23 -144.3(4) . . . . ? O2 Ag1 S1 C23 106.3(3) . . . . ? C38 C33 S2 C25 -105.3(6) . . . . ? C34 C33 S2 C25 70.2(6) . . . . ? C38 C33 S2 Ag2 145.3(5) . . . . ? C34 C33 S2 Ag2 -39.1(5) . . . . ? C26 C25 S2 C33 57.0(7) . . . . ? C24 C25 S2 C33 -120.5(6) . . . . ? C26 C25 S2 Ag2 164.0(6) . . . . ? C24 C25 S2 Ag2 -13.6(7) . . . . ? S5 Ag2 S2 C33 -23.0(2) . . . . ? O19 Ag2 S2 C33 116.4(2) . . . . ? O25 Ag2 S2 C33 -120.7(2) . . . . ? S5 Ag2 S2 C25 -126.4(3) . . . . ? O19 Ag2 S2 C25 13.0(3) . . . . ? O25 Ag2 S2 C25 135.8(3) . . . . ? C36 C35 S3 C43 98.6(6) . . . . ? C34 C35 S3 C43 -80.9(6) . . . . ? C48 C43 S3 C35 -74.3(7) . . . . ? C44 C43 S3 C35 106.9(6) . . . . ? C44 C45 S4 C18 -105.3(7) . . . . ? C46 C45 S4 C18 75.1(7) . . . . ? C17 C18 S4 C45 -96.8(8) . . . . ? C13 C18 S4 C45 85.3(7) . . . . ? C94 C95 S5 C64 -121.5(6) . . . . ? C96 C95 S5 C64 54.2(6) . . . . ? C94 C95 S5 Ag2 -15.0(7) . . . . ? C96 C95 S5 Ag2 160.7(5) . . . . ? C65 C64 S5 C95 -113.8(6) . . . . ? C63 C64 S5 C95 66.1(6) . . . . ? C65 C64 S5 Ag2 135.0(5) . . . . ? C63 C64 S5 Ag2 -45.1(6) . . . . ? S2 Ag2 S5 C95 -107.5(3) . . . . ? O19 Ag2 S5 C95 136.8(3) . . . . ? O25 Ag2 S5 C95 12.4(3) . . . . ? S2 Ag2 S5 C64 -2.7(3) . . . . ? O19 Ag2 S5 C64 -118.4(3) . . . . ? O25 Ag2 S5 C64 117.3(3) . . . . ? C74 C73 S6 C68 106.7(6) . . . . ? C78 C73 S6 C68 -74.7(7) . . . . ? C67 C68 S6 C73 101.9(6) . . . . ? C63 C68 S6 C73 -79.9(6) . . . . ? C76 C75 S7 C83 82.9(6) . . . . ? C74 C75 S7 C83 -104.4(6) . . . . ? C84 C83 S7 C75 72.1(6) . . . . ? C88 C83 S7 C75 -115.6(6) . . . . ? C86 C85 S8 C93 113.9(7) . . . . ? C84 C85 S8 C93 -64.7(7) . . . . ? C98 C93 S8 C85 -47.9(7) . . . . ? C94 C93 S8 C85 126.5(6) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.370 _refine_diff_density_min -1.678 _refine_diff_density_rms 0.134 # start Validation Reply Form _vrf_PLAT220_CCDC-740898 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 9.67 Ratio RESPONSE: This is due to the disorder of some tert-butyl groups. ; _vrf_PLAT222_CCDC-740898 ; PROBLEM: Large Non-Solvent H Uiso(max)/Uso(min) ... 10.00 Rati RESPONSE: This is due to the disorder of some tert-butyl groups. ; _vrf_PLAT242_CCDC-740898 ; PROBLEM: Check Low Ueq as Compared to Neighbors for C29 RESPONSE: This is due to the disorder of some tert-butyl groups. ; _vrf_PLAT234_CCDC-740898 ; PROBLEM: Large Hirshfeld Difference C29 -- C31 .. 0.30 Ang. RESPONSE: This is due to the disorder of some tert-butyl groups. ; # end Validation Reply Form