# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_e1723a _database_code_depnum_ccdc_archive 'CCDC 895668' #TrackingRef 'web_deposit_cif_file_0_SylvieFERLAY_1344596913.2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C64 H68 N4 O4 S4),3(C H4 O)' _chemical_formula_sum 'C131 H148 N8 O11 S8' _chemical_formula_weight 2267.05 _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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.5022(14) _cell_length_b 19.9845(12) _cell_length_c 28.2241(18) _cell_angle_alpha 90.00 _cell_angle_beta 107.0190(10) _cell_angle_gamma 90.00 _cell_volume 12136.4(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3286 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 25.53 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.241 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4824 _exptl_absorpt_coefficient_mu 0.210 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9773 _exptl_absorpt_correction_T_max 0.9896 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 31654 _diffrn_reflns_av_R_equivalents 0.0571 _diffrn_reflns_av_sigmaI/netI 0.0983 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 27.54 _reflns_number_total 13979 _reflns_number_gt 7739 _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. ; _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^)+(0.1001P)^2^+22.5416P] 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 13979 _refine_ls_number_parameters 723 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.1519 _refine_ls_R_factor_gt 0.0786 _refine_ls_wR_factor_ref 0.2243 _refine_ls_wR_factor_gt 0.1872 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _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 S1 S 0.23304(4) 0.72118(5) 0.16046(4) 0.0360(3) Uani 1 1 d . . . C1 C 0.29910(17) 0.67678(19) 0.19674(15) 0.0308(9) Uani 1 1 d . . . C2 C 0.33123(17) 0.63058(19) 0.17710(15) 0.0295(9) Uani 1 1 d . . . C3 C 0.38500(16) 0.60200(19) 0.20792(16) 0.0300(9) Uani 1 1 d . . . C4 C 0.40911(17) 0.62417(19) 0.25616(15) 0.0312(9) Uani 1 1 d . . . H4 H 0.4469 0.6053 0.2762 0.037 Uiso 1 1 calc R . . C5 C 0.37972(17) 0.67343(19) 0.27637(16) 0.0317(9) Uani 1 1 d . A . C6 C 0.32257(17) 0.6971(2) 0.24614(15) 0.0327(9) Uani 1 1 d . . . H6 H 0.2993 0.7275 0.2595 0.039 Uiso 1 1 calc R . . C7 C 0.4078(2) 0.7013(2) 0.32865(18) 0.0487(8) Uani 1 1 d D . . C8 C 0.3655(4) 0.6983(4) 0.3586(3) 0.0487(8) Uani 0.609(7) 1 d P A 2 H8A H 0.3829 0.7238 0.3892 0.073 Uiso 0.609(7) 1 calc PR A 2 H8B H 0.3596 0.6516 0.3667 0.073 Uiso 0.609(7) 1 calc PR A 2 H8C H 0.3254 0.7176 0.3401 0.073 Uiso 0.609(7) 1 calc PR A 2 C9 C 0.4204(4) 0.7802(4) 0.3227(3) 0.0487(8) Uani 0.609(7) 1 d P A 2 H9A H 0.3806 0.8033 0.3089 0.073 Uiso 0.609(7) 1 calc PR A 2 H9B H 0.4462 0.7859 0.3004 0.073 Uiso 0.609(7) 1 calc PR A 2 H9C H 0.4419 0.7992 0.3553 0.073 Uiso 0.609(7) 1 calc PR A 2 C10 C 0.4721(4) 0.6725(4) 0.3533(3) 0.0487(8) Uani 0.609(7) 1 d P A 2 H10A H 0.4879 0.6901 0.3871 0.073 Uiso 0.609(7) 1 calc PR A 2 H10B H 0.5004 0.6851 0.3342 0.073 Uiso 0.609(7) 1 calc PR A 2 H10C H 0.4694 0.6236 0.3545 0.073 Uiso 0.609(7) 1 calc PR A 2 C8A C 0.4421(6) 0.6443(5) 0.3657(4) 0.0487(8) Uani 0.391(7) 1 d PD A 1 H8A1 H 0.4538 0.6614 0.3997 0.073 Uiso 0.391(7) 1 calc PR A 1 H8A2 H 0.4795 0.6302 0.3573 0.073 Uiso 0.391(7) 1 calc PR A 1 H8A3 H 0.4142 0.6059 0.3629 0.073 Uiso 0.391(7) 1 calc PR A 1 C9A C 0.3526(5) 0.7232(7) 0.3519(5) 0.0487(8) Uani 0.391(7) 1 d PD A 1 H9A1 H 0.3225 0.6866 0.3476 0.073 Uiso 0.391(7) 1 calc PR A 1 H9A2 H 0.3318 0.7632 0.3348 0.073 Uiso 0.391(7) 1 calc PR A 1 H9A3 H 0.3703 0.7329 0.3872 0.073 Uiso 0.391(7) 1 calc PR A 1 C10A C 0.4452(6) 0.7609(6) 0.3267(5) 0.0487(8) Uani 0.391(7) 1 d PD A 1 H10D H 0.4235 0.7884 0.2982 0.073 Uiso 0.391(7) 1 calc PR A 1 H10E H 0.4856 0.7471 0.3235 0.073 Uiso 0.391(7) 1 calc PR A 1 H10F H 0.4514 0.7869 0.3573 0.073 Uiso 0.391(7) 1 calc PR A 1 O1 O 0.31223(15) 0.61465(15) 0.12711(12) 0.0462(7) Uani 1 1 d . . . C11 C 0.3369(2) 0.6643(2) 0.10092(17) 0.0462(7) Uani 1 1 d . . . H11A H 0.3810 0.6731 0.1191 0.055 Uiso 1 1 calc R . . H11B H 0.3135 0.7067 0.0993 0.055 Uiso 1 1 calc R . . C12 C 0.3321(2) 0.6412(3) 0.05001(18) 0.0499(12) Uani 1 1 d . . . C13 C 0.3689(3) 0.5929(3) 0.0432(2) 0.0713(17) Uani 1 1 d . . . H13 H 0.3965 0.5704 0.0706 0.086 Uiso 1 1 calc R . . C14 C 0.3660(4) 0.5767(4) -0.0041(3) 0.099(2) Uani 1 1 d . . . H14 H 0.3906 0.5412 -0.0104 0.119 Uiso 1 1 calc R . . C15 C 0.3273(4) 0.6119(4) -0.0428(2) 0.087(2) Uani 1 1 d . . . H15 H 0.3258 0.6018 -0.0761 0.104 Uiso 1 1 calc R . . C16 C 0.2916(4) 0.6609(4) -0.0329(3) 0.103(3) Uani 1 1 d . . . H16 H 0.2644 0.6847 -0.0597 0.124 Uiso 1 1 calc R . . N1 N 0.2931(3) 0.6772(3) 0.0133(2) 0.0889(19) Uani 1 1 d . . . S2 S 0.42855(4) 0.54250(5) 0.18501(4) 0.0317(2) Uani 1 1 d . . . C17 C 0.38008(16) 0.47061(19) 0.16907(14) 0.0266(8) Uani 1 1 d . . . C18 C 0.34736(16) 0.44306(19) 0.19895(15) 0.0270(8) Uani 1 1 d . . . C19 C 0.31322(16) 0.38486(19) 0.18343(16) 0.0295(9) Uani 1 1 d . . . C20 C 0.31606(18) 0.3527(2) 0.14034(16) 0.0334(9) Uani 1 1 d . . . H20 H 0.2930 0.3126 0.1305 0.040 Uiso 1 1 calc R . . C21 C 0.35113(18) 0.3770(2) 0.11148(16) 0.0333(9) Uani 1 1 d . B . C22 C 0.38151(17) 0.4376(2) 0.12583(15) 0.0308(9) Uani 1 1 d . . . H22 H 0.4039 0.4571 0.1056 0.037 Uiso 1 1 calc R . . C23 C 0.3560(2) 0.3397(2) 0.06518(17) 0.0415(11) Uani 1 1 d D . . C24 C 0.4232(5) 0.3206(7) 0.0751(5) 0.0810(16) Uani 0.525(5) 1 d PD B 1 H24A H 0.4275 0.2897 0.0494 0.121 Uiso 0.525(5) 1 calc PR B 1 H24B H 0.4379 0.2988 0.1076 0.121 Uiso 0.525(5) 1 calc PR B 1 H24C H 0.4480 0.3609 0.0750 0.121 Uiso 0.525(5) 1 calc PR B 1 C25 C 0.3173(6) 0.2751(6) 0.0575(4) 0.0810(16) Uani 0.525(5) 1 d PD B 1 H25A H 0.2730 0.2863 0.0458 0.121 Uiso 0.525(5) 1 calc PR B 1 H25B H 0.3261 0.2508 0.0889 0.121 Uiso 0.525(5) 1 calc PR B 1 H25C H 0.3282 0.2470 0.0328 0.121 Uiso 0.525(5) 1 calc PR B 1 C26 C 0.3348(7) 0.3845(6) 0.0208(4) 0.0810(16) Uani 0.525(5) 1 d PD B 1 H26A H 0.3615 0.4242 0.0258 0.121 Uiso 0.525(5) 1 calc PR B 1 H26B H 0.2917 0.3982 0.0164 0.121 Uiso 0.525(5) 1 calc PR B 1 H26C H 0.3375 0.3604 -0.0087 0.121 Uiso 0.525(5) 1 calc PR B 1 C24A C 0.2936(6) 0.3386(8) 0.0248(5) 0.0810(16) Uani 0.475(5) 1 d PD B 2 H24D H 0.2808 0.3846 0.0145 0.121 Uiso 0.475(5) 1 calc PR B 2 H24E H 0.2622 0.3176 0.0377 0.121 Uiso 0.475(5) 1 calc PR B 2 H24F H 0.2977 0.3131 -0.0037 0.121 Uiso 0.475(5) 1 calc PR B 2 C25A C 0.3763(8) 0.2660(6) 0.0769(5) 0.0810(16) Uani 0.475(5) 1 d PD B 2 H25D H 0.3491 0.2445 0.0939 0.121 Uiso 0.475(5) 1 calc PR B 2 H25E H 0.4193 0.2646 0.0982 0.121 Uiso 0.475(5) 1 calc PR B 2 H25F H 0.3732 0.2421 0.0459 0.121 Uiso 0.475(5) 1 calc PR B 2 C26A C 0.4063(7) 0.3682(7) 0.0420(5) 0.0810(16) Uani 0.475(5) 1 d PD B 2 H26D H 0.4175 0.3338 0.0215 0.121 Uiso 0.475(5) 1 calc PR B 2 H26E H 0.4433 0.3814 0.0686 0.121 Uiso 0.475(5) 1 calc PR B 2 H26F H 0.3894 0.4073 0.0215 0.121 Uiso 0.475(5) 1 calc PR B 2 O2 O 0.34633(12) 0.47215(13) 0.24311(10) 0.0317(6) Uani 1 1 d . . . C27 C 0.4042(2) 0.4662(2) 0.28302(16) 0.0391(10) Uani 1 1 d . . . H27A H 0.4035 0.4979 0.3098 0.047 Uiso 1 1 calc R . . H27B H 0.4393 0.4785 0.2704 0.047 Uiso 1 1 calc R . . C28 C 0.41427(18) 0.3965(2) 0.30396(16) 0.0359(10) Uani 1 1 d . . . N2 N 0.43656(19) 0.3467(3) 0.27877(19) 0.0676(13) Uani 1 1 d . . . C29 C 0.4441(2) 0.2822(3) 0.2990(2) 0.0520(13) Uani 1 1 d . . . H29 H 0.4586 0.2469 0.2828 0.062 Uiso 1 1 calc R . . C30 C 0.4303(2) 0.2709(3) 0.3423(2) 0.0511(13) Uani 1 1 d . . . H30 H 0.4352 0.2277 0.3569 0.061 Uiso 1 1 calc R . . C31 C 0.4092(2) 0.3235(3) 0.36405(19) 0.0537(13) Uani 1 1 d . . . H31 H 0.3994 0.3153 0.3941 0.064 Uiso 1 1 calc R . . C32 C 0.4017(2) 0.3848(2) 0.34589(15) 0.0321(9) Uani 1 1 d . . . H32 H 0.3875 0.4196 0.3627 0.038 Uiso 1 1 calc RD . . S3 S 0.27479(5) 0.34258(5) 0.22116(4) 0.0356(3) Uani 1 1 d . . . C33 C 0.21311(16) 0.39366(18) 0.22728(15) 0.0266(8) Uani 1 1 d . . . C34 C 0.17611(16) 0.43503(19) 0.19045(14) 0.0269(8) Uani 1 1 d . . . C35 C 0.12414(17) 0.46505(19) 0.19843(14) 0.0280(8) Uani 1 1 d . . . C36 C 0.10821(17) 0.4530(2) 0.24165(15) 0.0321(9) Uani 1 1 d . . . H36 H 0.0727 0.4744 0.2464 0.038 Uiso 1 1 calc R . . C37 C 0.14334(18) 0.4102(2) 0.27812(15) 0.0310(9) Uani 1 1 d . . . C38 C 0.19629(17) 0.38249(19) 0.27040(15) 0.0296(9) Uani 1 1 d . . . H38 H 0.2221 0.3548 0.2955 0.035 Uiso 1 1 calc R . . C39 C 0.1235(2) 0.3939(2) 0.32399(16) 0.0400(10) Uani 1 1 d . . . C40 C 0.1801(3) 0.3837(3) 0.36941(18) 0.0613(16) Uani 1 1 d . . . H40A H 0.2066 0.4235 0.3744 0.092 Uiso 1 1 calc R . . H40B H 0.2037 0.3446 0.3641 0.092 Uiso 1 1 calc R . . H40C H 0.1661 0.3763 0.3988 0.092 Uiso 1 1 calc R . . C41 C 0.0908(4) 0.3261(4) 0.3153(2) 0.0613(16) Uani 1 1 d . . . H41A H 0.0879 0.3083 0.3469 0.092 Uiso 1 1 calc R . . H41B H 0.1146 0.2950 0.3010 0.092 Uiso 1 1 calc R . . H41C H 0.0490 0.3314 0.2924 0.092 Uiso 1 1 calc R . . C42 C 0.0845(4) 0.4477(4) 0.3362(3) 0.0613(16) Uani 1 1 d . . . H42A H 0.1021 0.4915 0.3322 0.092 Uiso 1 1 calc R . . H42B H 0.0838 0.4425 0.3706 0.092 Uiso 1 1 calc R . . H42C H 0.0421 0.4445 0.3139 0.092 Uiso 1 1 calc R . . O3 O 0.19147(11) 0.44768(13) 0.14758(10) 0.0294(6) Uani 1 1 d . . . C43 C 0.16156(19) 0.4048(2) 0.10724(15) 0.0380(10) Uani 1 1 d . . . H43A H 0.1169 0.4007 0.1046 0.046 Uiso 1 1 calc R . . H43B H 0.1803 0.3596 0.1129 0.046 Uiso 1 1 calc R . . C44 C 0.16904(19) 0.4337(2) 0.06017(16) 0.0381(10) Uani 1 1 d . . . N3 N 0.1390(2) 0.3991(2) 0.02013(15) 0.0583(12) Uani 1 1 d . . . C45 C 0.1421(3) 0.4228(4) -0.0237(2) 0.0720(18) Uani 1 1 d . . . H45 H 0.1202 0.3995 -0.0530 0.086 Uiso 1 1 calc R . . C46 C 0.1750(3) 0.4788(3) -0.0286(2) 0.0640(16) Uani 1 1 d . . . H46 H 0.1759 0.4939 -0.0603 0.077 Uiso 1 1 calc R . . C47 C 0.2064(3) 0.5123(3) 0.0134(2) 0.0559(14) Uani 1 1 d . . . H47 H 0.2301 0.5509 0.0111 0.067 Uiso 1 1 calc R . . C48 C 0.2040(2) 0.4902(2) 0.05926(17) 0.0423(11) Uani 1 1 d . . . H48 H 0.2256 0.5130 0.0889 0.051 Uiso 1 1 calc R . . S4 S 0.06817(4) 0.51089(6) 0.15246(4) 0.0353(3) Uani 1 1 d . . . C49 C 0.10608(16) 0.57197(18) 0.12629(14) 0.0254(8) Uani 1 1 d . . . C50 C 0.15745(16) 0.60955(18) 0.15252(14) 0.0250(8) Uani 1 1 d . . . C51 C 0.17749(16) 0.66134(18) 0.12822(14) 0.0256(8) Uani 1 1 d . . . C52 C 0.14664(16) 0.67555(19) 0.07877(14) 0.0275(8) Uani 1 1 d . . . H52 H 0.1615 0.7108 0.0627 0.033 Uiso 1 1 calc R . . C53 C 0.09464(16) 0.63938(19) 0.05238(14) 0.0258(8) Uani 1 1 d . . . C54 C 0.07553(16) 0.58746(19) 0.07701(14) 0.0260(8) Uani 1 1 d . . . H54 H 0.0405 0.5616 0.0597 0.031 Uiso 1 1 calc R . . C55 C 0.05812(19) 0.6576(2) -0.00144(14) 0.0351(10) Uani 1 1 d . . . C56 C 0.0262(3) 0.5965(3) -0.03019(18) 0.0600(15) Uani 1 1 d . . . H56A H 0.0088 0.6082 -0.0652 0.090 Uiso 1 1 calc R . . H56B H -0.0072 0.5817 -0.0169 0.090 Uiso 1 1 calc R . . H56C H 0.0566 0.5604 -0.0269 0.090 Uiso 1 1 calc R . . C57 C 0.0083(3) 0.7079(3) 0.0007(2) 0.078(2) Uani 1 1 d . . . H57A H -0.0184 0.7169 -0.0330 0.118 Uiso 1 1 calc R . . H57B H 0.0280 0.7496 0.0157 0.118 Uiso 1 1 calc R . . H57C H -0.0169 0.6896 0.0207 0.118 Uiso 1 1 calc R . . C58 C 0.1016(3) 0.6862(4) -0.02870(18) 0.087(2) Uani 1 1 d . . . H58A H 0.0790 0.6915 -0.0639 0.131 Uiso 1 1 calc R . . H58B H 0.1366 0.6556 -0.0252 0.131 Uiso 1 1 calc R . . H58C H 0.1171 0.7298 -0.0146 0.131 Uiso 1 1 calc R . . O4 O 0.18893(11) 0.59377(13) 0.20068(9) 0.0290(6) Uani 1 1 d . . . C59 C 0.16781(19) 0.6273(2) 0.23752(15) 0.0366(10) Uani 1 1 d . . . H59A H 0.1232 0.6177 0.2323 0.044 Uiso 1 1 calc R . . H59B H 0.1729 0.6762 0.2350 0.044 Uiso 1 1 calc R . . C60 C 0.20510(17) 0.6032(2) 0.28771(14) 0.0298(9) Uani 1 1 d . . . N4 N 0.19089(17) 0.63190(19) 0.32563(13) 0.0400(9) Uani 1 1 d . . . C61 C 0.2222(2) 0.6119(2) 0.37167(17) 0.0474(12) Uani 1 1 d . . . H61 H 0.2135 0.6330 0.3990 0.057 Uiso 1 1 calc R . . C62 C 0.2664(2) 0.5618(2) 0.38080(17) 0.0463(12) Uani 1 1 d . . . H62 H 0.2869 0.5481 0.4138 0.056 Uiso 1 1 calc R . . C63 C 0.2799(2) 0.5323(2) 0.34171(17) 0.0420(11) Uani 1 1 d . . . H63 H 0.3099 0.4975 0.3472 0.050 Uiso 1 1 calc R . . C64 C 0.24992(18) 0.5532(2) 0.29422(15) 0.0332(9) Uani 1 1 d . . . H64 H 0.2596 0.5340 0.2666 0.040 Uiso 1 1 calc R . . C65 C 0.0419(3) 0.6357(3) 0.3224(3) 0.102(3) Uani 1 1 d . . . H65A H 0.0483 0.6384 0.3582 0.153 Uiso 1 1 calc R . . H65B H 0.0596 0.5938 0.3146 0.153 Uiso 1 1 calc R . . H65C H -0.0027 0.6369 0.3051 0.153 Uiso 1 1 calc R . . O5 O 0.07097(19) 0.6896(2) 0.3073(2) 0.0842(14) Uani 1 1 d . . . H5 H 0.1097 0.6850 0.3182 0.126 Uiso 1 1 calc R . . C66 C 0.4802(3) 0.5124(3) 0.4321(2) 0.068(3) Uani 0.50 1 d P . . H66A H 0.4977 0.4911 0.4645 0.102 Uiso 0.50 1 calc PR . . H66B H 0.4844 0.5611 0.4358 0.102 Uiso 0.50 1 calc PR . . H66C H 0.5026 0.4969 0.4092 0.102 Uiso 0.50 1 calc PR . . O6 O 0.4186(3) 0.4960(3) 0.4138(2) 0.0522(17) Uani 0.50 1 d PR . . H6C H 0.4117 0.4603 0.4270 0.078 Uiso 0.50 1 calc PRD . . _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 S1 0.0256(5) 0.0240(5) 0.0461(6) -0.0005(5) -0.0088(4) -0.0022(4) C1 0.0220(18) 0.0228(19) 0.040(2) 0.0026(18) -0.0029(17) -0.0008(15) C2 0.0237(18) 0.027(2) 0.033(2) -0.0007(18) 0.0009(16) -0.0097(15) C3 0.0204(18) 0.025(2) 0.043(2) -0.0038(18) 0.0075(17) -0.0061(15) C4 0.0194(18) 0.027(2) 0.040(2) -0.0015(18) -0.0013(16) -0.0025(15) C5 0.0223(18) 0.026(2) 0.040(2) -0.0067(18) -0.0019(17) 0.0001(15) C6 0.0245(19) 0.027(2) 0.039(2) -0.0088(19) -0.0016(17) -0.0013(15) C7 0.0417(18) 0.046(2) 0.0457(17) -0.0129(16) -0.0064(14) 0.0070(14) C8 0.0417(18) 0.046(2) 0.0457(17) -0.0129(16) -0.0064(14) 0.0070(14) C9 0.0417(18) 0.046(2) 0.0457(17) -0.0129(16) -0.0064(14) 0.0070(14) C10 0.0417(18) 0.046(2) 0.0457(17) -0.0129(16) -0.0064(14) 0.0070(14) C8A 0.0417(18) 0.046(2) 0.0457(17) -0.0129(16) -0.0064(14) 0.0070(14) C9A 0.0417(18) 0.046(2) 0.0457(17) -0.0129(16) -0.0064(14) 0.0070(14) C10A 0.0417(18) 0.046(2) 0.0457(17) -0.0129(16) -0.0064(14) 0.0070(14) O1 0.0558(16) 0.0406(15) 0.0431(16) 0.0030(13) 0.0158(13) -0.0112(12) C11 0.0558(16) 0.0406(15) 0.0431(16) 0.0030(13) 0.0158(13) -0.0112(12) C12 0.057(3) 0.046(3) 0.042(3) 0.008(2) 0.008(2) -0.013(2) C13 0.102(5) 0.065(4) 0.050(3) 0.005(3) 0.028(3) 0.018(4) C14 0.121(6) 0.092(6) 0.091(6) -0.007(5) 0.043(5) 0.005(5) C15 0.131(7) 0.092(5) 0.043(4) 0.002(4) 0.034(4) -0.035(5) C16 0.138(8) 0.083(6) 0.068(5) 0.012(4) -0.004(5) -0.049(5) N1 0.083(4) 0.078(4) 0.082(4) 0.024(3) -0.012(3) -0.036(3) S2 0.0209(4) 0.0311(5) 0.0443(6) -0.0057(5) 0.0114(4) -0.0064(4) C17 0.0170(17) 0.028(2) 0.032(2) -0.0013(17) 0.0033(15) -0.0024(14) C18 0.0204(17) 0.027(2) 0.033(2) 0.0001(17) 0.0079(16) 0.0035(14) C19 0.0159(17) 0.027(2) 0.045(2) 0.0036(19) 0.0090(16) 0.0010(14) C20 0.028(2) 0.026(2) 0.045(3) -0.0068(19) 0.0087(18) -0.0053(16) C21 0.0255(19) 0.033(2) 0.040(2) -0.0075(19) 0.0072(17) -0.0012(16) C22 0.0261(19) 0.035(2) 0.034(2) 0.0002(19) 0.0126(17) -0.0008(16) C23 0.041(2) 0.043(3) 0.041(3) -0.015(2) 0.011(2) -0.003(2) C24 0.103(4) 0.083(4) 0.063(3) -0.030(3) 0.033(3) 0.011(3) C25 0.103(4) 0.083(4) 0.063(3) -0.030(3) 0.033(3) 0.011(3) C26 0.103(4) 0.083(4) 0.063(3) -0.030(3) 0.033(3) 0.011(3) C24A 0.103(4) 0.083(4) 0.063(3) -0.030(3) 0.033(3) 0.011(3) C25A 0.103(4) 0.083(4) 0.063(3) -0.030(3) 0.033(3) 0.011(3) C26A 0.103(4) 0.083(4) 0.063(3) -0.030(3) 0.033(3) 0.011(3) O2 0.0306(14) 0.0323(15) 0.0345(15) -0.0052(13) 0.0129(12) -0.0022(11) C27 0.039(2) 0.039(2) 0.036(2) -0.004(2) 0.0061(19) -0.0077(19) C28 0.0251(19) 0.036(2) 0.042(3) -0.006(2) 0.0019(18) 0.0009(17) N2 0.040(2) 0.077(3) 0.081(3) 0.002(3) 0.010(2) 0.012(2) C29 0.045(3) 0.045(3) 0.063(3) -0.001(3) 0.011(2) 0.017(2) C30 0.040(3) 0.044(3) 0.065(3) 0.012(3) 0.009(2) 0.005(2) C31 0.059(3) 0.058(3) 0.047(3) 0.002(3) 0.021(3) -0.001(3) C32 0.049(2) 0.025(2) 0.025(2) -0.0025(18) 0.0154(18) 0.0014(17) S3 0.0268(5) 0.0278(5) 0.0569(7) 0.0083(5) 0.0197(5) 0.0010(4) C33 0.0192(17) 0.0238(19) 0.037(2) -0.0001(17) 0.0080(16) -0.0047(14) C34 0.0227(18) 0.029(2) 0.030(2) -0.0048(17) 0.0092(16) -0.0100(15) C35 0.0242(18) 0.026(2) 0.031(2) 0.0057(17) 0.0029(16) -0.0015(15) C36 0.0249(19) 0.033(2) 0.039(2) 0.0020(19) 0.0119(17) 0.0001(16) C37 0.032(2) 0.029(2) 0.033(2) 0.0026(18) 0.0111(17) -0.0007(16) C38 0.028(2) 0.025(2) 0.035(2) 0.0062(18) 0.0070(17) 0.0000(16) C39 0.040(2) 0.047(3) 0.036(2) 0.009(2) 0.016(2) 0.004(2) C40 0.067(4) 0.081(4) 0.040(3) 0.003(3) 0.022(3) 0.001(3) C41 0.067(4) 0.081(4) 0.040(3) 0.003(3) 0.022(3) 0.001(3) C42 0.067(4) 0.081(4) 0.040(3) 0.003(3) 0.022(3) 0.001(3) O3 0.0258(13) 0.0342(15) 0.0287(14) -0.0003(12) 0.0086(11) -0.0080(11) C43 0.032(2) 0.048(3) 0.034(2) -0.002(2) 0.0087(18) -0.0095(19) C44 0.030(2) 0.052(3) 0.033(2) -0.004(2) 0.0110(18) -0.0018(19) N3 0.056(3) 0.082(3) 0.039(2) -0.014(2) 0.017(2) -0.017(2) C45 0.075(4) 0.106(5) 0.038(3) -0.012(3) 0.020(3) -0.004(4) C46 0.083(4) 0.076(4) 0.043(3) 0.010(3) 0.033(3) 0.015(3) C47 0.072(4) 0.049(3) 0.059(3) 0.010(3) 0.038(3) 0.005(3) C48 0.045(3) 0.046(3) 0.041(3) 0.004(2) 0.021(2) 0.000(2) S4 0.0193(4) 0.0410(6) 0.0425(6) 0.0138(5) 0.0042(4) -0.0032(4) C49 0.0231(18) 0.0238(19) 0.029(2) 0.0009(17) 0.0065(15) 0.0012(15) C50 0.0215(17) 0.0264(19) 0.024(2) -0.0002(16) 0.0025(15) 0.0027(14) C51 0.0191(17) 0.0224(19) 0.031(2) -0.0039(17) 0.0009(15) -0.0027(14) C52 0.0237(18) 0.027(2) 0.031(2) 0.0030(17) 0.0076(16) -0.0011(15) C53 0.0231(18) 0.029(2) 0.025(2) 0.0001(17) 0.0061(15) 0.0030(15) C54 0.0179(17) 0.031(2) 0.028(2) -0.0022(17) 0.0048(15) -0.0029(15) C55 0.037(2) 0.042(2) 0.021(2) -0.0003(19) 0.0010(17) 0.0004(19) C56 0.062(3) 0.068(4) 0.033(3) -0.007(3) -0.013(2) -0.008(3) C57 0.100(5) 0.078(4) 0.039(3) 0.005(3) -0.009(3) 0.052(4) C58 0.077(4) 0.151(7) 0.026(3) 0.024(3) 0.003(3) -0.051(4) O4 0.0279(13) 0.0304(15) 0.0245(14) 0.0003(12) 0.0012(11) 0.0029(11) C59 0.034(2) 0.042(2) 0.030(2) -0.004(2) 0.0042(18) 0.0086(18) C60 0.0256(19) 0.034(2) 0.027(2) -0.0031(18) 0.0035(16) -0.0039(16) N4 0.041(2) 0.046(2) 0.033(2) -0.0013(18) 0.0106(16) 0.0052(17) C61 0.054(3) 0.057(3) 0.032(2) -0.001(2) 0.012(2) 0.006(2) C62 0.043(3) 0.058(3) 0.030(2) 0.007(2) -0.001(2) 0.000(2) C63 0.035(2) 0.044(3) 0.041(3) 0.005(2) 0.002(2) 0.0005(19) C64 0.030(2) 0.036(2) 0.030(2) -0.0002(19) 0.0028(17) -0.0019(17) C65 0.074(4) 0.069(4) 0.172(8) 0.050(5) 0.051(5) 0.019(4) O5 0.058(2) 0.071(3) 0.129(4) 0.033(3) 0.036(3) 0.025(2) C66 0.046(6) 0.087(9) 0.063(7) 0.007(7) 0.003(5) 0.000(6) O6 0.044(4) 0.066(5) 0.051(4) -0.003(4) 0.021(3) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C1 1.776(4) . ? S1 C51 1.776(4) . ? C1 C2 1.385(6) . ? C1 C6 1.399(6) . ? C2 O1 1.386(5) . ? C2 C3 1.389(5) . ? C3 C4 1.383(6) . ? C3 S2 1.778(4) . ? C4 C5 1.397(5) . ? C4 H4 0.9500 . ? C5 C6 1.401(5) . ? C5 C7 1.530(6) . ? C6 H6 0.9500 . ? C7 C8 1.447(11) . ? C7 C10A 1.467(10) . ? C7 C10 1.524(8) . ? C7 C8A 1.586(10) . ? C7 C9 1.619(10) . ? C7 C9A 1.624(11) . ? 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 . ? C8A H8A1 0.9800 . ? C8A H8A2 0.9800 . ? C8A H8A3 0.9800 . ? C9A H9A1 0.9800 . ? C9A H9A2 0.9800 . ? C9A H9A3 0.9800 . ? C10A H10D 0.9800 . ? C10A H10E 0.9800 . ? C10A H10F 0.9800 . ? O1 C11 1.442(5) . ? C11 C12 1.483(7) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.321(8) . ? C12 N1 1.353(7) . ? C13 C14 1.357(9) . ? C13 H13 0.9500 . ? C14 C15 1.375(10) . ? C14 H14 0.9500 . ? C15 C16 1.348(11) . ? C15 H15 0.9500 . ? C16 N1 1.336(10) . ? C16 H16 0.9500 . ? S2 C17 1.780(4) . ? C17 C18 1.386(5) . ? C17 C22 1.396(5) . ? C18 O2 1.382(5) . ? C18 C19 1.392(5) . ? C19 C20 1.393(6) . ? C19 S3 1.770(4) . ? C20 C21 1.378(6) . ? C20 H20 0.9500 . ? C21 C22 1.391(5) . ? C21 C23 1.536(6) . ? C22 H22 0.9500 . ? C23 C26 1.498(11) . ? C23 C24 1.504(11) . ? C23 C24A 1.528(12) . ? C23 C25 1.536(11) . ? C23 C25A 1.550(12) . ? C23 C26A 1.571(12) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C24A H24D 0.9800 . ? C24A H24E 0.9800 . ? C24A H24F 0.9800 . ? C25A H25D 0.9800 . ? C25A H25E 0.9800 . ? C25A H25F 0.9800 . ? C26A H26D 0.9800 . ? C26A H26E 0.9800 . ? C26A H26F 0.9800 . ? O2 C27 1.456(5) . ? C27 C28 1.503(6) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C32 1.316(6) . ? C28 N2 1.399(6) . ? N2 C29 1.399(7) . ? C29 C30 1.365(7) . ? C29 H29 0.9500 . ? C30 C31 1.371(7) . ? C30 H30 0.9500 . ? C31 C32 1.319(6) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? S3 C33 1.772(4) . ? C33 C38 1.394(5) . ? C33 C34 1.397(5) . ? C34 O3 1.376(4) . ? C34 C35 1.390(5) . ? C35 C36 1.389(5) . ? C35 S4 1.775(4) . ? C36 C37 1.394(5) . ? C36 H36 0.9500 . ? C37 C38 1.388(5) . ? C37 C39 1.523(6) . ? C38 H38 0.9500 . ? C39 C42 1.490(7) . ? C39 C41 1.528(8) . ? C39 C40 1.534(7) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? O3 C43 1.427(5) . ? C43 C44 1.503(6) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 N3 1.329(6) . ? C44 C48 1.382(6) . ? N3 C45 1.347(7) . ? C45 C46 1.371(8) . ? C45 H45 0.9500 . ? C46 C47 1.364(8) . ? C46 H46 0.9500 . ? C47 C48 1.383(6) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? S4 C49 1.770(4) . ? C49 C54 1.394(5) . ? C49 C50 1.395(5) . ? C50 O4 1.373(4) . ? C50 C51 1.388(5) . ? C51 C52 1.394(5) . ? C52 C53 1.391(5) . ? C52 H52 0.9500 . ? C53 C54 1.386(5) . ? C53 C55 1.545(5) . ? C54 H54 0.9500 . ? C55 C57 1.520(7) . ? C55 C58 1.521(7) . ? C55 C56 1.524(6) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? O4 C59 1.430(5) . ? C59 C60 1.499(5) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 N4 1.333(5) . ? C60 C64 1.392(5) . ? N4 C61 1.345(6) . ? C61 C62 1.381(7) . ? C61 H61 0.9500 . ? C62 C63 1.361(7) . ? C62 H62 0.9500 . ? C63 C64 1.377(6) . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? C65 O5 1.391(7) . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? O5 H5 0.8400 . ? C66 O6 1.3704 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? O6 H6C 0.8400 . ? _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 C1 S1 C51 107.68(18) . . ? C2 C1 C6 120.2(3) . . ? C2 C1 S1 123.3(3) . . ? C6 C1 S1 116.0(3) . . ? C1 C2 O1 121.3(4) . . ? C1 C2 C3 119.0(4) . . ? O1 C2 C3 119.7(4) . . ? C4 C3 C2 120.2(4) . . ? C4 C3 S2 118.2(3) . . ? C2 C3 S2 121.2(3) . . ? C3 C4 C5 122.1(4) . . ? C3 C4 H4 118.9 . . ? C5 C4 H4 118.9 . . ? C4 C5 C6 116.7(4) . . ? C4 C5 C7 122.6(3) . . ? C6 C5 C7 120.7(4) . . ? C1 C6 C5 121.4(4) . . ? C1 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? C8 C7 C10A 122.4(7) . . ? C8 C7 C10 114.6(6) . . ? C10A C7 C10 81.1(6) . . ? C8 C7 C5 113.1(5) . . ? C10A C7 C5 109.8(6) . . ? C10 C7 C5 111.8(4) . . ? C10A C7 C8A 115.7(7) . . ? C5 C7 C8A 111.0(5) . . ? C8 C7 C9 105.4(5) . . ? C10 C7 C9 104.1(5) . . ? C5 C7 C9 106.9(5) . . ? C8A C7 C9 134.6(6) . . ? C10A C7 C9A 108.1(7) . . ? C10 C7 C9A 130.8(7) . . ? C5 C7 C9A 109.8(6) . . ? C8A C7 C9A 102.1(7) . . ? C9 C7 C9A 87.5(6) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 C8A H8A1 109.5 . . ? C7 C8A H8A2 109.5 . . ? C7 C8A H8A3 109.5 . . ? C7 C9A H9A1 109.5 . . ? C7 C9A H9A2 109.5 . . ? C7 C9A H9A3 109.5 . . ? C7 C10A H10D 109.5 . . ? C7 C10A H10E 109.5 . . ? C7 C10A H10F 109.5 . . ? C2 O1 C11 108.3(3) . . ? O1 C11 C12 110.6(4) . . ? O1 C11 H11A 109.5 . . ? C12 C11 H11A 109.5 . . ? O1 C11 H11B 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? C13 C12 N1 124.9(6) . . ? C13 C12 C11 119.8(5) . . ? N1 C12 C11 114.9(5) . . ? C12 C13 C14 117.7(6) . . ? C12 C13 H13 121.2 . . ? C14 C13 H13 121.2 . . ? C13 C14 C15 119.9(7) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C16 C15 C14 118.9(7) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? N1 C16 C15 122.3(8) . . ? N1 C16 H16 118.8 . . ? C15 C16 H16 118.8 . . ? C16 N1 C12 116.3(7) . . ? C3 S2 C17 105.63(17) . . ? C18 C17 C22 119.8(3) . . ? C18 C17 S2 124.2(3) . . ? C22 C17 S2 115.7(3) . . ? O2 C18 C17 122.3(3) . . ? O2 C18 C19 118.8(3) . . ? C17 C18 C19 118.9(4) . . ? C18 C19 C20 119.9(4) . . ? C18 C19 S3 122.1(3) . . ? C20 C19 S3 117.4(3) . . ? C21 C20 C19 122.3(4) . . ? C21 C20 H20 118.9 . . ? C19 C20 H20 118.9 . . ? C20 C21 C22 116.9(4) . . ? C20 C21 C23 121.8(4) . . ? C22 C21 C23 121.3(4) . . ? C21 C22 C17 122.0(4) . . ? C21 C22 H22 119.0 . . ? C17 C22 H22 119.0 . . ? C26 C23 C24 111.3(8) . . ? C24 C23 C24A 142.2(7) . . ? C26 C23 C25 110.8(8) . . ? C24 C23 C25 108.0(8) . . ? C26 C23 C21 109.7(5) . . ? C24 C23 C21 106.4(5) . . ? C24A C23 C21 111.3(5) . . ? C25 C23 C21 110.5(5) . . ? C26 C23 C25A 138.4(7) . . ? C24A C23 C25A 107.1(8) . . ? C21 C23 C25A 111.8(6) . . ? C24A C23 C26A 108.2(8) . . ? C25 C23 C26A 133.9(7) . . ? C21 C23 C26A 114.7(5) . . ? C25A C23 C26A 103.3(8) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? C23 C24A H24D 109.5 . . ? C23 C24A H24E 109.5 . . ? H24D C24A H24E 109.5 . . ? C23 C24A H24F 109.5 . . ? H24D C24A H24F 109.5 . . ? H24E C24A H24F 109.5 . . ? C23 C25A H25D 109.5 . . ? C23 C25A H25E 109.5 . . ? H25D C25A H25E 109.5 . . ? C23 C25A H25F 109.5 . . ? H25D C25A H25F 109.5 . . ? H25E C25A H25F 109.5 . . ? C23 C26A H26D 109.5 . . ? C23 C26A H26E 109.5 . . ? H26D C26A H26E 109.5 . . ? C23 C26A H26F 109.5 . . ? H26D C26A H26F 109.5 . . ? H26E C26A H26F 109.5 . . ? C18 O2 C27 114.6(3) . . ? O2 C27 C28 112.3(3) . . ? O2 C27 H27A 109.2 . . ? C28 C27 H27A 109.2 . . ? O2 C27 H27B 109.2 . . ? C28 C27 H27B 109.2 . . ? H27A C27 H27B 107.9 . . ? C32 C28 N2 122.2(4) . . ? C32 C28 C27 118.2(4) . . ? N2 C28 C27 119.6(4) . . ? C29 N2 C28 117.8(5) . . ? C30 C29 N2 119.1(5) . . ? C30 C29 H29 120.5 . . ? N2 C29 H29 120.5 . . ? C29 C30 C31 118.2(5) . . ? C29 C30 H30 120.9 . . ? C31 C30 H30 120.9 . . ? C32 C31 C30 124.0(5) . . ? C32 C31 H31 118.0 . . ? C30 C31 H31 118.0 . . ? C28 C32 C31 118.6(4) . . ? C28 C32 H32 120.7 . . ? C31 C32 H32 120.7 . . ? C19 S3 C33 108.55(17) . . ? C38 C33 C34 119.3(3) . . ? C38 C33 S3 114.4(3) . . ? C34 C33 S3 125.6(3) . . ? O3 C34 C35 120.2(3) . . ? O3 C34 C33 121.0(3) . . ? C35 C34 C33 118.8(3) . . ? C36 C35 C34 120.9(3) . . ? C36 C35 S4 114.9(3) . . ? C34 C35 S4 123.7(3) . . ? C35 C36 C37 121.2(4) . . ? C35 C36 H36 119.4 . . ? C37 C36 H36 119.4 . . ? C38 C37 C36 117.2(4) . . ? C38 C37 C39 121.9(4) . . ? C36 C37 C39 121.0(4) . . ? C37 C38 C33 122.6(4) . . ? C37 C38 H38 118.7 . . ? C33 C38 H38 118.7 . . ? C42 C39 C37 112.5(4) . . ? C42 C39 C41 112.9(6) . . ? C37 C39 C41 107.4(4) . . ? C42 C39 C40 107.7(5) . . ? C37 C39 C40 111.1(4) . . ? C41 C39 C40 105.0(5) . . ? 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 . . ? C34 O3 C43 114.2(3) . . ? O3 C43 C44 109.0(3) . . ? O3 C43 H43A 109.9 . . ? C44 C43 H43A 109.9 . . ? O3 C43 H43B 109.9 . . ? C44 C43 H43B 109.9 . . ? H43A C43 H43B 108.3 . . ? N3 C44 C48 124.1(4) . . ? N3 C44 C43 113.0(4) . . ? C48 C44 C43 122.9(4) . . ? C44 N3 C45 116.6(5) . . ? N3 C45 C46 123.7(5) . . ? N3 C45 H45 118.2 . . ? C46 C45 H45 118.2 . . ? C47 C46 C45 118.1(5) . . ? C47 C46 H46 120.9 . . ? C45 C46 H46 120.9 . . ? C46 C47 C48 120.3(5) . . ? C46 C47 H47 119.8 . . ? C48 C47 H47 119.8 . . ? C44 C48 C47 117.2(5) . . ? C44 C48 H48 121.4 . . ? C47 C48 H48 121.4 . . ? C49 S4 C35 109.59(17) . . ? C54 C49 C50 120.0(3) . . ? C54 C49 S4 114.3(3) . . ? C50 C49 S4 125.1(3) . . ? O4 C50 C51 120.8(3) . . ? O4 C50 C49 120.6(3) . . ? C51 C50 C49 118.5(3) . . ? C50 C51 C52 120.5(3) . . ? C50 C51 S1 122.1(3) . . ? C52 C51 S1 116.5(3) . . ? C53 C52 C51 121.6(3) . . ? C53 C52 H52 119.2 . . ? C51 C52 H52 119.2 . . ? C54 C53 C52 117.2(3) . . ? C54 C53 C55 121.1(3) . . ? C52 C53 C55 121.7(3) . . ? C53 C54 C49 122.1(3) . . ? C53 C54 H54 118.9 . . ? C49 C54 H54 118.9 . . ? C57 C55 C58 111.3(5) . . ? C57 C55 C56 108.2(4) . . ? C58 C55 C56 107.7(4) . . ? C57 C55 C53 107.7(3) . . ? C58 C55 C53 110.5(4) . . ? C56 C55 C53 111.5(4) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C55 C57 H57A 109.5 . . ? C55 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C55 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C55 C58 H58A 109.5 . . ? C55 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C55 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C50 O4 C59 115.3(3) . . ? O4 C59 C60 108.9(3) . . ? O4 C59 H59A 109.9 . . ? C60 C59 H59A 109.9 . . ? O4 C59 H59B 109.9 . . ? C60 C59 H59B 109.9 . . ? H59A C59 H59B 108.3 . . ? N4 C60 C64 122.5(4) . . ? N4 C60 C59 114.9(3) . . ? C64 C60 C59 122.6(4) . . ? C60 N4 C61 117.8(4) . . ? N4 C61 C62 122.7(4) . . ? N4 C61 H61 118.6 . . ? C62 C61 H61 118.6 . . ? C63 C62 C61 118.8(4) . . ? C63 C62 H62 120.6 . . ? C61 C62 H62 120.6 . . ? C62 C63 C64 119.7(4) . . ? C62 C63 H63 120.1 . . ? C64 C63 H63 120.1 . . ? C63 C64 C60 118.4(4) . . ? C63 C64 H64 120.8 . . ? C60 C64 H64 120.8 . . ? O5 C65 H65A 109.5 . . ? O5 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? O5 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C65 O5 H5 109.5 . . ? O6 C66 H66A 109.5 . . ? O6 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? O6 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C66 O6 H6C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.047 _refine_diff_density_min -0.663 _refine_diff_density_rms 0.075 data_e2350a _database_code_depnum_ccdc_archive 'CCDC 895669' #TrackingRef 'web_deposit_cif_file_1_SylvieFERLAY_1344596913.2-AgBF4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H34 Ag B F4 N2 O2 S2, H2 O' _chemical_formula_sum 'C32 H36 Ag B F4 N2 O3 S2' _chemical_formula_weight 755.43 _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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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 Tetragonal _symmetry_space_group_name_H-M I-42d _symmetry_space_group_name_Hall 'I-4 2bw' _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y, -z+3/4' 'x+1/2, -y, -z+3/4' '-y+1/2, -x, z+3/4' 'y+1/2, x, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' '-x+1, y+1/2, -z+5/4' 'x+1, -y+1/2, -z+5/4' '-y+1, -x+1/2, z+5/4' 'y+1, x+1/2, z+5/4' _cell_length_a 23.2001(5) _cell_length_b 23.2001(5) _cell_length_c 14.3622(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7730.4(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8283 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 22.69 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3088 _exptl_absorpt_coefficient_mu 0.679 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9540 _exptl_absorpt_correction_T_max 0.9668 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 43137 _diffrn_reflns_av_R_equivalents 0.0585 _diffrn_reflns_av_sigmaI/netI 0.0494 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 30.10 _reflns_number_total 5685 _reflns_number_gt 3695 _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(7) _refine_ls_number_reflns 5685 _refine_ls_number_parameters 202 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1358 _refine_ls_R_factor_gt 0.0931 _refine_ls_wR_factor_ref 0.3056 _refine_ls_wR_factor_gt 0.2705 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.132 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _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 1.03802(4) 0.7500 1.1250 0.0620(3) Uani 1 2 d S . . S1 S 1.06221(7) 0.84306(7) 0.99835(13) 0.0406(4) Uani 1 1 d . . . C1 C 0.9997(3) 0.8704(3) 0.9400(5) 0.0377(13) Uani 1 1 d . . . C2 C 0.9525(3) 0.8895(3) 0.9927(5) 0.0400(14) Uani 1 1 d . . . C3 C 0.9052(3) 0.9123(3) 0.9416(5) 0.0419(14) Uani 1 1 d . . . C4 C 0.9058(3) 0.9130(3) 0.8459(5) 0.0447(15) Uani 1 1 d . . . H4 H 0.8742 0.9294 0.8132 0.054 Uiso 1 1 calc R . . C5 C 0.9520(3) 0.8900(3) 0.7957(5) 0.0438(15) Uani 1 1 d . . . C6 C 0.9989(3) 0.8712(3) 0.8443(5) 0.0461(15) Uani 1 1 d . . . H6 H 1.0318 0.8582 0.8111 0.055 Uiso 1 1 calc R . . O1 O 0.9526(2) 0.8846(2) 1.0868(4) 0.0425(11) Uani 1 1 d . . . C7 C 0.9216(4) 0.8357(3) 1.1191(6) 0.0523(17) Uani 1 1 d . . . H7A H 0.9321 0.8016 1.0813 0.063 Uiso 1 1 calc R . . H7B H 0.8797 0.8425 1.1117 0.063 Uiso 1 1 calc R . . C8 C 0.9961(4) 0.7159(3) 0.9230(6) 0.055(2) Uani 1 1 d . . . H8 H 1.0307 0.7359 0.9084 0.067 Uiso 1 1 calc R . . N1 N 0.9842(3) 0.7051(3) 1.0123(5) 0.0474(14) Uani 1 1 d . . . C9 C 0.9348(3) 0.6760(3) 1.0304(6) 0.0471(16) Uani 1 1 d . . . C10 C 0.8972(5) 0.6575(5) 0.9600(8) 0.073(3) Uani 1 1 d . . . H10 H 0.8632 0.6363 0.9733 0.087 Uiso 1 1 calc R . . C11 C 0.9129(6) 0.6723(5) 0.8685(9) 0.082(3) Uani 1 1 d . . . H11 H 0.8879 0.6620 0.8188 0.098 Uiso 1 1 calc R . . C12 C 0.9597(6) 0.6992(4) 0.8499(7) 0.074(3) Uani 1 1 d . . . H12 H 0.9697 0.7078 0.7872 0.088 Uiso 1 1 calc R . . C13 C 0.9482(4) 0.8873(4) 0.6886(6) 0.057(2) Uani 1 1 d . . . C14 C 0.9228(11) 0.8270(6) 0.6613(11) 0.132(7) Uani 1 1 d . . . H14A H 0.9251 0.8010 0.7149 0.198 Uiso 1 1 calc R . . H14B H 0.9451 0.8108 0.6095 0.198 Uiso 1 1 calc R . . H14C H 0.8825 0.8315 0.6424 0.198 Uiso 1 1 calc R . . C15 C 0.9050(9) 0.9261(7) 0.6478(9) 0.138(8) Uani 1 1 d . . . H15A H 0.8667 0.9159 0.6712 0.207 Uiso 1 1 calc R . . H15B H 0.9056 0.9223 0.5798 0.207 Uiso 1 1 calc R . . H15C H 0.9140 0.9660 0.6650 0.207 Uiso 1 1 calc R . . C16 C 1.0072(5) 0.8839(12) 0.6435(8) 0.137(8) Uani 1 1 d . . . H16A H 1.0339 0.9096 0.6762 0.205 Uiso 1 1 calc R . . H16B H 1.0043 0.8956 0.5781 0.205 Uiso 1 1 calc R . . H16C H 1.0215 0.8442 0.6470 0.205 Uiso 1 1 calc R . . B1 B 1.1871(9) 0.7557(8) 1.0658(13) 0.110 Uiso 0.50 1 d PD . . F1 F 1.1860(7) 0.7541(7) 0.9646(8) 0.110 Uiso 0.50 1 d PD . . F2 F 1.2090(7) 0.8152(6) 1.0942(11) 0.110 Uiso 0.50 1 d PD . . F3 F 1.1379(5) 0.7500 1.1250 0.110 Uiso 1 2 d SD . . F4 F 1.2234(6) 0.7049(6) 1.0906(11) 0.110 Uiso 0.50 1 d PD . . O2 O 0.1016(11) 0.7693(6) 0.7837(16) 0.137(10) Uani 0.50 1 d P . . _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 0.0628(6) 0.0732(6) 0.0499(4) -0.0185(4) 0.000 0.000 S1 0.0360(7) 0.0323(7) 0.0535(9) -0.0092(7) 0.0013(7) 0.0022(6) C1 0.033(3) 0.030(3) 0.050(3) -0.005(3) 0.002(3) -0.002(2) C2 0.041(3) 0.028(3) 0.051(4) -0.012(3) 0.000(3) 0.002(2) C3 0.038(3) 0.035(3) 0.052(4) 0.003(3) 0.008(3) -0.001(3) C4 0.039(3) 0.039(3) 0.056(4) -0.009(3) -0.002(3) -0.001(3) C5 0.042(3) 0.044(3) 0.045(4) -0.011(3) 0.000(3) -0.002(3) C6 0.041(3) 0.044(4) 0.053(4) -0.015(3) 0.004(3) -0.005(3) O1 0.042(2) 0.036(2) 0.049(3) 0.0013(19) 0.006(2) -0.0012(18) C7 0.059(4) 0.036(3) 0.063(4) 0.011(3) -0.019(4) 0.005(3) C8 0.078(6) 0.043(4) 0.046(4) -0.004(3) 0.015(4) -0.010(4) N1 0.060(4) 0.031(3) 0.051(3) 0.008(2) -0.008(3) -0.007(2) C9 0.050(4) 0.035(3) 0.056(4) 0.006(3) -0.001(3) -0.004(3) C10 0.072(6) 0.064(5) 0.082(7) 0.005(5) -0.024(5) -0.011(5) C11 0.111(9) 0.072(6) 0.063(6) 0.003(6) -0.015(7) -0.021(6) C12 0.114(8) 0.054(5) 0.054(5) 0.004(4) -0.004(5) -0.008(5) C13 0.051(4) 0.073(5) 0.047(4) -0.014(4) 0.004(3) 0.011(4) C14 0.23(2) 0.082(9) 0.085(9) -0.029(8) 0.018(12) -0.033(11) C15 0.22(2) 0.123(12) 0.067(8) -0.014(7) -0.021(10) 0.102(13) C16 0.065(7) 0.29(3) 0.056(6) 0.003(11) 0.003(5) 0.008(10) O2 0.20(2) 0.041(7) 0.173(19) -0.015(9) 0.147(18) -0.011(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. ; _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 N1 2.294(7) 14_466 ? Ag1 N1 2.294(7) . ? Ag1 F3 2.317(11) . ? Ag1 S1 2.8784(18) . ? Ag1 S1 2.8785(18) 14_466 ? S1 C3 1.781(7) 4_757 ? S1 C1 1.791(7) . ? C1 C6 1.374(10) . ? C1 C2 1.403(9) . ? C2 O1 1.356(9) . ? C2 C3 1.423(10) . ? C3 C4 1.374(11) . ? C3 S1 1.781(7) 3_577 ? C4 C5 1.398(10) . ? C4 H4 0.9500 . ? C5 C6 1.364(11) . ? C5 C13 1.542(11) . ? C6 H6 0.9500 . ? O1 C7 1.423(9) . ? C7 C9 1.499(11) 14_466 ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N1 1.336(10) . ? C8 C12 1.402(14) . ? C8 H8 0.9500 . ? N1 C9 1.356(10) . ? C9 C10 1.403(13) . ? C9 C7 1.499(11) 14_466 ? C10 C11 1.405(16) . ? C10 H10 0.9500 . ? C11 C12 1.281(17) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C15 1.468(16) . ? C13 C16 1.516(15) . ? C13 C14 1.568(19) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? B1 F3 1.430(17) . ? B1 F1 1.453(17) . ? B1 F4 1.493(17) . ? B1 F2 1.526(17) . ? B1 B1 1.72(4) 14_466 ? B1 F4 1.83(2) 14_466 ? F2 F4 1.099(19) 14_466 ? F3 B1 1.430(17) 14_466 ? F4 F2 1.099(19) 14_466 ? F4 B1 1.83(2) 14_466 ? _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 N1 Ag1 N1 114.1(4) 14_466 . ? N1 Ag1 F3 122.95(18) 14_466 . ? N1 Ag1 F3 122.95(18) . . ? N1 Ag1 S1 102.20(15) 14_466 . ? N1 Ag1 S1 90.05(15) . . ? F3 Ag1 S1 78.75(4) . . ? N1 Ag1 S1 90.05(15) 14_466 14_466 ? N1 Ag1 S1 102.19(15) . 14_466 ? F3 Ag1 S1 78.75(4) . 14_466 ? S1 Ag1 S1 157.51(7) . 14_466 ? C3 S1 C1 102.0(3) 4_757 . ? C3 S1 Ag1 111.5(3) 4_757 . ? C1 S1 Ag1 113.8(2) . . ? C6 C1 C2 121.6(7) . . ? C6 C1 S1 119.0(5) . . ? C2 C1 S1 119.4(5) . . ? O1 C2 C1 120.7(6) . . ? O1 C2 C3 123.1(6) . . ? C1 C2 C3 116.2(6) . . ? C4 C3 C2 120.8(7) . . ? C4 C3 S1 119.3(6) . 3_577 ? C2 C3 S1 119.9(5) . 3_577 ? C3 C4 C5 121.3(7) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C6 C5 C4 118.0(7) . . ? C6 C5 C13 122.9(7) . . ? C4 C5 C13 119.1(7) . . ? C5 C6 C1 121.9(7) . . ? C5 C6 H6 119.1 . . ? C1 C6 H6 119.1 . . ? C2 O1 C7 113.0(6) . . ? O1 C7 C9 110.8(6) . 14_466 ? O1 C7 H7A 109.5 . . ? C9 C7 H7A 109.5 14_466 . ? O1 C7 H7B 109.5 . . ? C9 C7 H7B 109.5 14_466 . ? H7A C7 H7B 108.1 . . ? N1 C8 C12 122.8(8) . . ? N1 C8 H8 118.6 . . ? C12 C8 H8 118.6 . . ? C8 N1 C9 117.0(7) . . ? C8 N1 Ag1 118.6(5) . . ? C9 N1 Ag1 123.4(5) . . ? N1 C9 C10 122.6(8) . . ? N1 C9 C7 116.6(7) . 14_466 ? C10 C9 C7 120.8(8) . 14_466 ? C9 C10 C11 116.0(10) . . ? C9 C10 H10 122.0 . . ? C11 C10 H10 122.0 . . ? C12 C11 C10 122.3(11) . . ? C12 C11 H11 118.9 . . ? C10 C11 H11 118.9 . . ? C11 C12 C8 119.3(10) . . ? C11 C12 H12 120.4 . . ? C8 C12 H12 120.4 . . ? C15 C13 C16 118.5(13) . . ? C15 C13 C5 114.4(8) . . ? C16 C13 C5 112.1(7) . . ? C15 C13 C14 101.0(12) . . ? C16 C13 C14 100.7(14) . . ? C5 C13 C14 107.9(9) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? F3 B1 F1 125.3(16) . . ? F3 B1 F4 103.6(12) . . ? F1 B1 F4 103.2(13) . . ? F3 B1 F2 101.0(12) . . ? F1 B1 F2 107.2(13) . . ? F4 B1 F2 117.6(15) . . ? F1 B1 B1 170(2) . 14_466 ? F2 B1 B1 82.8(14) . 14_466 ? F3 B1 F4 88.7(10) . 14_466 ? F1 B1 F4 139.0(14) . 14_466 ? F4 B1 F4 87.7(14) . 14_466 ?? F4 F2 B1 86.9(14) 14_466 . ? B1 F3 Ag1 143.0(8) 14_466 . ? B1 F3 Ag1 143.0(8) . . ? F2 F4 B1 111.5(14) 14_466 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.10 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.298 _refine_diff_density_min -0.865 _refine_diff_density_rms 0.237 data_e2261b _database_code_depnum_ccdc_archive 'CCDC 895670' #TrackingRef 'web_deposit_cif_file_2_SylvieFERLAY_1344596913.2-AgPF6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H36 Ag N2 O3 S2, F6 P' _chemical_formula_sum 'C32 H36 Ag F6 N2 O3 P S2' _chemical_formula_weight 813.59 _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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I-42d _symmetry_space_group_name_Hall 'I -4 2bw' _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y, -z+3/4' 'x+1/2, -y, -z+3/4' '-y+1/2, -x, z+3/4' 'y+1/2, x, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' '-x+1, y+1/2, -z+5/4' 'x+1, -y+1/2, -z+5/4' '-y+1, -x+1/2, z+5/4' 'y+1, x+1/2, z+5/4' _cell_length_a 23.7715(9) _cell_length_b 23.7715(9) _cell_length_c 14.1007(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7968.1(5) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7034 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 20.99 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.356 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3312 _exptl_absorpt_coefficient_mu 0.710 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9389 _exptl_absorpt_correction_T_max 0.9586 _exptl_absorpt_process_details sadabs _exptl_special_details ; Owing to large disorder of the solvent present in the cavities of this structure, the SQUEEZE command has been applied. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 37022 _diffrn_reflns_av_R_equivalents 0.0677 _diffrn_reflns_av_sigmaI/netI 0.0541 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 30.14 _reflns_number_total 5599 _reflns_number_gt 3891 _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. ; _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^)+(0.1950P)^2^+0.6068P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(10) _refine_ls_number_reflns 5599 _refine_ls_number_parameters 219 _refine_ls_number_restraints 51 _refine_ls_R_factor_all 0.1194 _refine_ls_R_factor_gt 0.0957 _refine_ls_wR_factor_ref 0.3051 _refine_ls_wR_factor_gt 0.2846 _refine_ls_goodness_of_fit_ref 1.153 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.016 _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 Ag2 Ag 1.04852(7) 0.23302(7) 1.10694(15) 0.0631(6) Uani 0.50 1 d P . 1 S1 S 1.06955(8) 0.14891(8) 0.98959(17) 0.0416(5) Uani 1 1 d . . 1 C1 C 1.0064(3) 0.1251(3) 0.9380(6) 0.0380(16) Uani 1 1 d . . 1 C2 C 0.9592(3) 0.1104(3) 0.9924(6) 0.0374(15) Uani 1 1 d . . 1 C3 C 1.0910(3) 0.0887(3) 1.0544(6) 0.0386(16) Uani 1 1 d . . 1 C4 C 1.0888(4) 0.0908(4) 1.1543(7) 0.0434(18) Uani 1 1 d . . 1 H4 H 1.0747 0.1236 1.1845 0.052 Uiso 1 1 calc R . 1 C5 C 1.0035(4) 0.1226(4) 0.8379(6) 0.0420(17) Uani 1 1 d . . 1 H5 H 1.0360 0.1319 0.8018 0.050 Uiso 1 1 calc R . 1 C6 C 0.9543(4) 0.1068(4) 0.7904(7) 0.0467(19) Uani 1 1 d . . 1 O1 O 0.9609(2) 0.1166(2) 1.0878(4) 0.0382(12) Uani 1 1 d . . 1 C7 C 0.9368(6) 0.1687(4) 1.1171(8) 0.062(3) Uani 1 1 d . . 1 H7A H 0.8956 0.1676 1.1079 0.074 Uiso 1 1 calc R . 1 H7B H 0.9521 0.1996 1.0777 0.074 Uiso 1 1 calc R . 1 C8 C 0.9500(5) 0.1796(4) 1.2199(7) 0.050(2) Uani 1 1 d . . 1 N1 N 0.9975(4) 0.2077(3) 1.2402(6) 0.0492(18) Uani 1 1 d . . 1 C9 C 1.0100(5) 0.2189(4) 1.3301(9) 0.062(3) Uani 1 1 d . . 1 H9 H 1.0450 0.2365 1.3437 0.074 Uiso 1 1 calc R . 1 C10 C 0.9748(8) 0.2062(6) 1.4039(9) 0.081(4) Uani 1 1 d . . 1 H10 H 0.9841 0.2169 1.4669 0.097 Uiso 1 1 calc R . 1 C11 C 0.9252(7) 0.1773(8) 1.3846(11) 0.086(4) Uani 1 1 d . . 1 H11 H 0.9011 0.1659 1.4348 0.104 Uiso 1 1 calc R . 1 C12 C 0.9111(6) 0.1652(6) 1.2899(10) 0.071(3) Uani 1 1 d . . 1 H12 H 0.8763 0.1478 1.2742 0.085 Uiso 1 1 calc R . 1 C13 C 0.9493(5) 0.1119(7) 0.6831(9) 0.080(4) Uani 1 1 d DU . 1 C14 C 0.9335(13) 0.1749(9) 0.6628(16) 0.088(7) Uani 0.58(5) 1 d PD . 1 H14A H 0.9137 0.1905 0.7177 0.132 Uiso 0.58(5) 1 calc PR . 1 H14B H 0.9090 0.1768 0.6069 0.132 Uiso 0.58(5) 1 calc PR . 1 H14C H 0.9678 0.1966 0.6510 0.132 Uiso 0.58(5) 1 calc PR . 1 C15 C 0.9008(11) 0.0763(12) 0.6427(18) 0.088(7) Uani 0.58(5) 1 d PD . 1 H15A H 0.9094 0.0363 0.6508 0.132 Uiso 0.58(5) 1 calc PR . 1 H15B H 0.8961 0.0847 0.5751 0.132 Uiso 0.58(5) 1 calc PR . 1 H15C H 0.8659 0.0854 0.6765 0.132 Uiso 0.58(5) 1 calc PR . 1 C16 C 1.0056(9) 0.0973(13) 0.6363(18) 0.088(7) Uani 0.58(5) 1 d PD . 1 H16A H 1.0338 0.1254 0.6541 0.132 Uiso 0.58(5) 1 calc PR . 1 H16B H 1.0010 0.0970 0.5673 0.132 Uiso 0.58(5) 1 calc PR . 1 H16C H 1.0179 0.0600 0.6578 0.132 Uiso 0.58(5) 1 calc PR . 1 C14A C 1.0024(14) 0.127(2) 0.628(3) 0.127(14) Uani 0.42(5) 1 d PDU . 2 H14D H 1.0289 0.1460 0.6709 0.190 Uiso 0.42(5) 1 calc PR . 2 H14E H 0.9927 0.1521 0.5757 0.190 Uiso 0.42(5) 1 calc PR . 2 H14F H 1.0197 0.0927 0.6034 0.190 Uiso 0.42(5) 1 calc PR . 2 C15A C 0.927(2) 0.0522(14) 0.656(3) 0.127(14) Uani 0.42(5) 1 d PDU . 2 H15D H 0.9185 0.0511 0.5884 0.190 Uiso 0.42(5) 1 calc PR . 2 H15E H 0.8933 0.0438 0.6929 0.190 Uiso 0.42(5) 1 calc PR . 2 H15F H 0.9563 0.0241 0.6706 0.190 Uiso 0.42(5) 1 calc PR . 2 C16A C 0.9021(17) 0.1556(19) 0.661(3) 0.127(14) Uani 0.42(5) 1 d PDU . 2 H16D H 0.8742 0.1551 0.7123 0.190 Uiso 0.42(5) 1 calc PR . 2 H16E H 0.8838 0.1458 0.6011 0.190 Uiso 0.42(5) 1 calc PR . 2 H16F H 0.9186 0.1933 0.6563 0.190 Uiso 0.42(5) 1 calc PR . 2 O2 O 1.1525(11) 0.2299(11) 1.151(2) 0.114(9) Uani 0.50 1 d P . . P1 P 0.6119(3) 0.7500 0.1250 0.146(4) Uani 1 2 d SD . . F1 F 0.6097(6) 0.7155(6) 0.2294(8) 0.156 Uani 0.50 1 d PD . . F2 F 0.6105(6) 0.6886(5) 0.0656(11) 0.156 Uani 0.50 1 d PD . . F3 F 0.6811(3) 0.7500 0.1250 0.156 Uani 1 2 d SD . . F4 F 0.6105(6) 0.8114(5) 0.1844(11) 0.156 Uani 0.50 1 d PD . . F5 F 0.5398(4) 0.7500 0.1250 0.156 Uani 1 2 d SD . . F6 F 0.6097(6) 0.7845(6) 0.0206(8) 0.156 Uani 0.50 1 d PD . . _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 Ag2 0.0479(7) 0.0749(13) 0.0664(13) 0.0355(10) 0.0044(7) 0.0041(6) S1 0.0381(9) 0.0395(9) 0.0472(12) 0.0109(8) -0.0009(8) -0.0004(7) C1 0.034(3) 0.035(3) 0.045(5) 0.003(3) 0.005(3) 0.003(3) C2 0.041(4) 0.032(3) 0.039(4) 0.004(3) 0.002(3) -0.003(3) C3 0.035(4) 0.040(4) 0.041(4) 0.005(3) 0.002(3) 0.002(3) C4 0.050(4) 0.039(4) 0.040(5) 0.005(3) 0.002(3) 0.004(3) C5 0.043(4) 0.044(4) 0.039(5) 0.006(3) 0.003(3) -0.003(3) C6 0.049(4) 0.051(5) 0.040(5) 0.005(3) 0.004(4) -0.015(4) O1 0.044(3) 0.031(2) 0.040(3) -0.001(2) 0.005(2) 0.000(2) C7 0.097(8) 0.038(4) 0.050(6) -0.008(4) -0.004(5) 0.016(5) C8 0.067(5) 0.038(4) 0.045(5) -0.007(3) 0.004(4) -0.010(4) N1 0.061(4) 0.044(4) 0.042(4) 0.009(3) 0.013(4) -0.001(3) C9 0.070(7) 0.046(5) 0.069(8) 0.009(5) -0.011(5) -0.018(5) C10 0.136(13) 0.069(7) 0.038(6) -0.010(5) 0.011(7) -0.015(8) C11 0.089(10) 0.116(12) 0.055(8) 0.000(8) 0.028(7) -0.009(8) C12 0.069(7) 0.082(8) 0.063(7) 0.006(6) 0.016(6) -0.004(6) C13 0.071(7) 0.119(11) 0.050(7) 0.005(7) 0.008(6) -0.019(8) C14 0.109(13) 0.114(14) 0.041(8) 0.004(7) -0.004(7) -0.035(10) C15 0.109(13) 0.114(14) 0.041(8) 0.004(7) -0.004(7) -0.035(10) C16 0.109(13) 0.114(14) 0.041(8) 0.004(7) -0.004(7) -0.035(10) C14A 0.104(19) 0.21(3) 0.069(15) 0.05(2) -0.001(13) -0.05(2) C15A 0.104(19) 0.21(3) 0.069(15) 0.05(2) -0.001(13) -0.05(2) C16A 0.104(19) 0.21(3) 0.069(15) 0.05(2) -0.001(13) -0.05(2) O2 0.100(15) 0.107(19) 0.13(2) -0.017(15) -0.019(14) -0.062(13) P1 0.101(5) 0.071(4) 0.267(13) 0.030(6) 0.000 0.000 F1 0.097 0.071 0.300 0.039 0.000 0.000 F2 0.097 0.071 0.300 0.039 0.000 0.000 F3 0.097 0.071 0.300 0.039 0.000 0.000 F4 0.097 0.071 0.300 0.039 0.000 0.000 F5 0.097 0.071 0.300 0.039 0.000 0.000 F6 0.097 0.071 0.300 0.039 0.000 0.000 _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. ; _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag2 Ag2 0.954(4) 14_456 ? Ag2 N1 2.310(8) 14_456 ? Ag2 N1 2.316(8) . ? Ag2 O2 2.55(3) . ? Ag2 S1 2.643(3) . ? S1 C1 1.762(9) . ? S1 C3 1.772(8) . ? C1 C2 1.403(11) . ? C1 C5 1.414(13) . ? C2 O1 1.355(10) . ? C2 C3 1.395(12) 4_647 ? C3 C2 1.395(12) 3_667 ? C3 C4 1.411(13) . ? C4 C6 1.393(12) 3_667 ? C4 H4 0.9500 . ? C5 C6 1.399(13) . ? C5 H5 0.9500 . ? C6 C4 1.393(12) 4_647 ? C6 C13 1.523(15) . ? O1 C7 1.425(11) . ? C7 C8 1.506(15) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N1 1.342(14) . ? C8 C12 1.396(16) . ? N1 C9 1.329(16) . ? N1 Ag2 2.310(8) 14_456 ? C9 C10 1.369(19) . ? C9 H9 0.9500 . ? C10 C11 1.39(2) . ? C10 H10 0.9500 . ? C11 C12 1.41(2) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14A 1.52(2) . ? C13 C16 1.53(2) . ? C13 C15 1.539(19) . ? C13 C15A 1.56(2) . ? C13 C16A 1.56(2) . ? C13 C14 1.57(2) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C14A H14D 0.9800 . ? C14A H14E 0.9800 . ? C14A H14F 0.9800 . ? C15A H15D 0.9800 . ? C15A H15E 0.9800 . ? C15A H15F 0.9800 . ? O2 O2 1.20(5) 14_456 ? P1 F3 1.646(9) . ? P1 F4 1.682(9) . ? P1 F2 1.682(9) . ? P1 F2 1.682(9) 14_464 ? P1 F4 1.682(9) 14_464 ? P1 F6 1.685(9) 14_464 ? P1 F6 1.685(9) . ? P1 F1 1.685(9) . ? P1 F1 1.685(9) 14_464 ? P1 F5 1.713(9) . ? F1 F6 0.00(4) 14_464 ? F2 F4 0.00(3) 14_464 ? F4 F2 0.00(4) 14_464 ? F6 F1 0.00(3) 14_464 ? _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 Ag2 Ag2 N1 78.5(3) 14_456 14_456 ? Ag2 Ag2 N1 77.7(3) 14_456 . ? N1 Ag2 N1 111.4(5) 14_456 . ? Ag2 Ag2 O2 83.9(6) 14_456 . ? N1 Ag2 O2 132.2(6) 14_456 . ? N1 Ag2 O2 107.6(7) . . ? Ag2 Ag2 S1 166.86(15) 14_456 . ? N1 Ag2 S1 100.9(2) 14_456 . ? N1 Ag2 S1 114.2(2) . . ? O2 Ag2 S1 87.0(7) . . ? C1 S1 C3 101.5(4) . . ? C1 S1 Ag2 109.9(3) . . ? C3 S1 Ag2 110.0(3) . . ? C2 C1 C5 119.8(8) . . ? C2 C1 S1 122.4(7) . . ? C5 C1 S1 117.8(6) . . ? O1 C2 C3 122.0(7) . 4_647 ? O1 C2 C1 119.5(7) . . ? C3 C2 C1 118.5(8) 4_647 . ? C2 C3 C4 120.9(7) 3_667 . ? C2 C3 S1 120.7(6) 3_667 . ? C4 C3 S1 118.4(6) . . ? C6 C4 C3 121.3(8) 3_667 . ? C6 C4 H4 119.3 3_667 . ? C3 C4 H4 119.3 . . ? C6 C5 C1 121.9(8) . . ? C6 C5 H5 119.0 . . ? C1 C5 H5 119.0 . . ? C4 C6 C5 117.3(8) 4_647 . ? C4 C6 C13 121.4(9) 4_647 . ? C5 C6 C13 121.3(8) . . ? C2 O1 C7 111.8(7) . . ? O1 C7 C8 110.1(8) . . ? O1 C7 H7A 109.6 . . ? C8 C7 H7A 109.6 . . ? O1 C7 H7B 109.6 . . ? C8 C7 H7B 109.6 . . ? H7A C7 H7B 108.2 . . ? N1 C8 C12 121.9(10) . . ? N1 C8 C7 117.7(10) . . ? C12 C8 C7 120.0(11) . . ? C9 N1 C8 119.5(9) . . ? C9 N1 Ag2 109.0(7) . 14_456 ? C8 N1 Ag2 128.3(7) . 14_456 ? C9 N1 Ag2 127.1(7) . . ? C8 N1 Ag2 113.4(7) . . ? N1 C9 C10 122.9(11) . . ? N1 C9 H9 118.5 . . ? C10 C9 H9 118.5 . . ? C9 C10 C11 118.5(12) . . ? C9 C10 H10 120.7 . . ? C11 C10 H10 120.8 . . ? C10 C11 C12 119.3(12) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C8 C12 C11 117.6(13) . . ? C8 C12 H12 121.2 . . ? C11 C12 H12 121.2 . . ? C14A C13 C6 117(2) . . ? C6 C13 C16 110.0(14) . . ? C14A C13 C15 124(2) . . ? C6 C13 C15 112.4(12) . . ? C16 C13 C15 111.7(15) . . ? C14A C13 C15A 112(2) . . ? C6 C13 C15A 101.2(19) . . ? C14A C13 C16A 109.9(18) . . ? C6 C13 C16A 107.8(19) . . ? C16 C13 C16A 134.0(19) . . ? C15A C13 C16A 108.4(18) . . ? C6 C13 C14 106.0(13) . . ? C16 C13 C14 110.4(14) . . ? C15 C13 C14 106.1(15) . . ? C15A C13 C14 138(2) . . ? H14D C14A H14E 109.5 . . ? H14D C14A H14F 109.5 . . ? H14E C14A H14F 109.5 . . ? H15D C15A H15E 109.5 . . ? H15D C15A H15F 109.5 . . ? H15E C15A H15F 109.5 . . ? F3 P1 F4 91.1(5) . . ? F3 P1 F2 91.1(5) . . ? F4 P1 F2 177.8(7) . . ? F3 P1 F2 91.1(5) . 14_464 ? F2 P1 F2 177.8(10) . 14_464 ? F3 P1 F4 91.1(5) . 14_464 ? F4 P1 F4 177.8(10) . 14_464 ? F2 P1 F4 177.8(7) 14_464 14_464 ? F3 P1 F6 91.7(5) . 14_464 ? F4 P1 F6 89.2(7) . 14_464 ? F2 P1 F6 90.7(7) . 14_464 ? F2 P1 F6 89.2(7) 14_464 14_464 ? F4 P1 F6 90.7(7) 14_464 14_464 ? F2 P1 F6 90.7(7) 14_464 . ? F4 P1 F6 89.2(7) 14_464 . ? F6 P1 F6 176.6(10) 14_464 . ? F2 P1 F1 89.2(7) 14_464 . ? F4 P1 F1 90.7(7) 14_464 . ? F3 P1 F1 91.7(5) . 14_464 ? F4 P1 F1 90.7(7) . 14_464 ? F2 P1 F1 89.2(7) . 14_464 ? F2 P1 F1 90.7(7) 14_464 14_464 ? F4 P1 F1 89.2(7) 14_464 14_464 ? F6 P1 F1 176.6(7) 14_464 14_464 ? F1 P1 F1 176.6(10) . 14_464 ? F2 P1 F5 88.9(5) 14_464 . ? F4 P1 F5 88.9(5) 14_464 . ? F6 P1 F5 88.3(5) 14_464 . ? F1 P1 F5 88.3(5) 14_464 . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 30.14 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 1.273 _refine_diff_density_min -1.565 _refine_diff_density_rms 0.151 _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 0.250 0.750 -0.070 347.0 -3.5 2 0.250 0.250 0.042 346.9 -4.2 3 0.500 0.500 0.000 6.5 0.3 4 0.750 0.250 -0.053 346.9 -3.5 5 0.750 0.750 0.018 346.9 -4.2 6 0.000 0.000 0.104 12.1 -0.6 7 0.000 0.500 0.146 11.8 -1.0 8 0.500 0.000 0.250 6.5 0.5 9 0.000 0.500 0.357 12.0 -0.6 10 0.500 0.500 0.396 11.8 -0.7 11 0.000 0.000 0.500 6.5 0.3 12 0.500 0.500 0.607 12.0 -0.6 13 0.500 0.000 0.646 11.8 -1.0 14 0.000 0.500 0.750 6.5 0.5 15 0.500 0.000 0.857 12.0 -0.6 16 0.000 0.000 0.893 11.8 -0.7 _platon_squeeze_details ; ; data_e2342a _database_code_depnum_ccdc_archive 'CCDC 895671' #TrackingRef 'web_deposit_cif_file_3_SylvieFERLAY_1344596913.2-AgSbF6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H36 Ag N2 O3 S2, F6 Sb' _chemical_formula_sum 'C32 H36 Ag F6 N2 O3 S2 Sb' _chemical_formula_weight 904.37 _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' F F 0.0171 0.0103 '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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I-42d _symmetry_space_group_name_Hall 'I-4 2bw' _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y, -z+3/4' 'x+1/2, -y, -z+3/4' '-y+1/2, -x, z+3/4' 'y+1/2, x, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' '-x+1, y+1/2, -z+5/4' 'x+1, -y+1/2, -z+5/4' '-y+1, -x+1/2, z+5/4' 'y+1, x+1/2, z+5/4' _cell_length_a 24.1812(17) _cell_length_b 24.1812(17) _cell_length_c 13.9842(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8177.0(10) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2950 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 18.53 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3600 _exptl_absorpt_coefficient_mu 1.299 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9261 _exptl_absorpt_correction_T_max 0.9499 _exptl_absorpt_process_details sadabs _exptl_special_details ; Owing to large disorder of the solvent present in the cavities of this structure, the SQUEEZE command has been applied. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 32754 _diffrn_reflns_av_R_equivalents 0.1184 _diffrn_reflns_av_sigmaI/netI 0.0810 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 30.12 _reflns_number_total 5763 _reflns_number_gt 2903 _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.7244P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.11(11) _refine_ls_number_reflns 5763 _refine_ls_number_parameters 160 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.2252 _refine_ls_R_factor_gt 0.1316 _refine_ls_wR_factor_ref 0.3868 _refine_ls_wR_factor_gt 0.3527 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _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 1.05044(12) 0.7500 1.1250 0.044(8) Uani 1 2 d S . . S1 S 1.07199(14) 0.85495(15) 0.9834(3) 0.0452(8) Uani 1 1 d . . . C1 C 1.0077(2) 0.8764(3) 0.9349(6) 0.034(3) Uani 1 1 d G . . C2 C 0.9618(3) 0.8905(4) 0.9896(4) 0.041(3) Uani 1 1 d G . . C3 C 0.9136(3) 0.9086(4) 0.9453(5) 0.043(3) Uani 1 1 d G . . C4 C 0.9113(3) 0.9126(5) 0.8462(5) 0.069(6) Uani 1 1 d G . . H4 H 0.8784 0.9249 0.8160 0.082 Uiso 1 1 calc R . . C5 C 0.9572(4) 0.8985(5) 0.7915(4) 0.051(4) Uani 1 1 d G . . C6 C 1.0053(3) 0.8804(4) 0.8358(5) 0.051(3) Uani 1 1 d G . . H6 H 1.0367 0.8707 0.7983 0.061 Uiso 1 1 calc R . . O1 O 0.9667(3) 0.8829(3) 1.0872(6) 0.0337(18) Uani 1 1 d . . . C7 C 0.9463(11) 0.8329(6) 1.1112(13) 0.078(6) Uani 1 1 d . . . H7A H 0.9658 0.8041 1.0740 0.094 Uiso 1 1 calc R . . H7B H 0.9067 0.8314 1.0937 0.094 Uiso 1 1 calc R . . C8 C 0.9525(5) 0.8202(5) 1.2192(7) 0.074(6) Uani 1 1 d G . . N1 N 1.0016(4) 0.7929(4) 1.2399(8) 0.052(3) Uani 1 1 d G . . C9 C 1.0141(5) 0.7786(5) 1.3337(9) 0.088(8) Uani 1 1 d G . . H9 H 1.0477 0.7600 1.3479 0.106 Uiso 1 1 calc R . . C10 C 0.9775(7) 0.7916(6) 1.4069(7) 0.101(9) Uani 1 1 d G . . H10 H 0.9860 0.7819 1.4710 0.122 Uiso 1 1 calc R . . C11 C 0.9283(7) 0.8189(7) 1.3862(9) 0.074(6) Uani 1 1 d G . . H11 H 0.9032 0.8278 1.4362 0.133 Uiso 1 1 calc R . . C12 C 0.9158(5) 0.8332(7) 1.2924(10) 0.074(6) Uani 1 1 d G . . H12 H 0.8822 0.8518 1.2783 0.133 Uiso 1 1 calc R . . C13 C 0.9484(5) 0.8953(7) 0.6705(13) 0.085(6) Uani 1 1 d D . . C14 C 0.9092(5) 0.8484(5) 0.6451(12) 0.085(6) Uani 1 1 d D . . H14A H 0.9112 0.8411 0.5763 0.117 Uiso 1 1 calc R . . H14B H 0.8713 0.8589 0.6622 0.117 Uiso 1 1 calc R . . H14C H 0.9197 0.8151 0.6805 0.117 Uiso 1 1 calc R . . C15 C 1.0052(5) 0.8906(6) 0.6238(13) 0.085(6) Uani 1 1 d D . . H15A H 1.0266 0.8615 0.6557 0.117 Uiso 1 1 calc R . . H15B H 1.0247 0.9259 0.6297 0.117 Uiso 1 1 calc R . . H15C H 1.0008 0.8813 0.5560 0.117 Uiso 1 1 calc R . . C16 C 0.9209(6) 0.9519(5) 0.6521(12) 0.085(6) Uani 1 1 d D . . H16A H 0.8838 0.9462 0.6253 0.117 Uiso 1 1 calc R . . H16B H 0.9434 0.9731 0.6068 0.117 Uiso 1 1 calc R . . H16C H 0.9179 0.9723 0.7124 0.117 Uiso 1 1 calc R . . O2 O 1.1508(7) 0.7500 1.1250 0.142(14) Uani 1 2 d S . . H2 H 1.1624 0.7816 1.1104 0.213 Uiso 1 1 calc R . . Sb1 Sb 0.2500 0.38500(9) 0.8750 0.0797(7) Uani 1 2 d SD . . F1 F 0.2500 0.3056(8) 0.8750 0.27(3) Uiso 1 2 d SD . . F2 F 0.2068(6) 0.3925(7) 0.9854(10) 0.103(4) Uiso 1 1 d D . . F3 F 0.2500 0.4656(8) 0.8750 0.205(16) Uiso 1 2 d SD . . F4 F 0.3159(7) 0.3819(10) 0.9483(15) 0.140(6) Uiso 1 1 d D . . _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 0.0428(13) 0.050(17) 0.048(8) -0.005(11) 0.000 0.000 S1 0.0448(17) 0.0498(18) 0.0411(19) -0.0068(15) 0.0021(14) -0.0008(14) C1 0.032(5) 0.031(5) 0.037(7) 0.001(5) 0.002(5) -0.009(5) C2 0.023(5) 0.035(6) 0.065(9) 0.031(6) -0.006(5) 0.004(4) C3 0.062(8) 0.038(6) 0.031(7) 0.000(5) -0.014(6) 0.004(6) C4 0.032(6) 0.136(18) 0.038(9) -0.023(9) 0.007(6) 0.000(9) C5 0.057(8) 0.073(10) 0.024(7) -0.006(6) 0.002(6) 0.019(7) C6 0.076(10) 0.044(7) 0.034(8) -0.006(6) -0.001(7) 0.002(7) O1 0.037(4) 0.035(4) 0.030(4) -0.002(3) 0.002(3) -0.023(4) C7 0.15(2) 0.041(8) 0.042(9) -0.028(7) -0.007(11) -0.022(10) C8 0.126(18) 0.041(8) 0.056(11) 0.003(7) 0.026(11) -0.007(10) N1 0.041(6) 0.037(6) 0.078(9) -0.023(6) 0.005(6) -0.002(5) C9 0.094(14) 0.033(7) 0.14(2) -0.043(10) -0.056(14) 0.024(9) C10 0.11(2) 0.111(19) 0.079(15) -0.040(15) 0.024(14) -0.031(16) C11 0.126(18) 0.041(8) 0.056(11) 0.003(7) 0.026(11) -0.007(10) C12 0.126(18) 0.041(8) 0.056(11) 0.003(7) 0.026(11) -0.007(10) C13 0.045(7) 0.144(17) 0.066(12) 0.011(12) -0.003(8) 0.052 C14 0.045(7) 0.144(17) 0.066(12) 0.011(12) -0.003(8) 0.052 C15 0.045(7) 0.144(17) 0.066(12) 0.011(12) -0.003(8) 0.052 C16 0.045(7) 0.144(17) 0.066(12) 0.011(12) -0.003(8) 0.052 O2 0.024(7) 0.19(3) 0.21(3) 0.11(3) 0.000 0.000 Sb1 0.0653(11) 0.0786(13) 0.0953(16) 0.000 0.0098(10) 0.000 _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. ; _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 N1 2.247(8) . ? Ag1 N1 2.247(17) 14_466 ? Ag1 O2 2.426(18) . ? S1 C1 1.775(7) . ? S1 C3 1.797(17) 4_757 ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C2 O1 1.382(10) . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C3 S1 1.797(7) 3_577 ? C4 C5 1.3900 . ? C4 H4 0.9500 . ? C5 C6 1.3900 . ? C5 C13 1.706(19) . ? C6 H6 0.9500 . ? O1 C7 1.349(19) . ? C7 C8 1.55(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N1 1.3900 . ? C8 C12 1.3900 . ? N1 C9 1.3900 . ? C9 C10 1.3900 . ? C9 H9 0.9500 . ? C10 C11 1.3900 . ? C10 H10 0.9500 . ? C11 C12 1.3900 . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.519(16) . ? C13 C15 1.525(15) . ? C13 C16 1.543(15) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? O2 H2 0.8400 . ? Sb1 F2 1.872(12) 5_556 ? Sb1 F2 1.872(12) . ? Sb1 F4 1.896(15) 5_556 ? Sb1 F4 1.897(15) . ? Sb1 F1 1.92(2) . ? Sb1 F3 1.949(19) . ? _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 N1 Ag1 N1 116.6(11) . 14_466 ? N1 Ag1 O2 121.7(3) . . ? N1 Ag1 O2 121.7(8) 14_466 . ? C1 S1 C3 102.2(8) . 4_757 ? C2 C1 C6 120.0 . . ? C2 C1 S1 124.1(5) . . ? C6 C1 S1 115.9(5) . . ? O1 C2 C3 123.6(6) . . ? O1 C2 C1 116.3(6) . . ? C3 C2 C1 120.0 . . ? C2 C3 C4 120.0 . . ? C2 C3 S1 119.8(4) . 3_577 ? C4 C3 S1 120.2(4) . 3_577 ? C5 C4 C3 120.0 . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.0 . . ? C4 C5 C13 117.3(7) . . ? C6 C5 C13 122.1(7) . . ? C5 C6 C1 120.0 . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? C7 O1 C2 109.4(10) . . ? O1 C7 C8 112.7(12) . . ? O1 C7 H7A 109.1 . . ? C8 C7 H7A 109.1 . . ? O1 C7 H7B 109.1 . . ? C8 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? N1 C8 C12 120.0 . . ? N1 C8 C7 112.3(12) . . ? C12 C8 C7 127.7(12) . . ? C9 N1 C8 120.0 . . ? C9 N1 Ag1 116.5(6) . . ? C8 N1 Ag1 121.3(6) . . ? N1 C9 C10 120.0 . . ? N1 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C11 C10 C9 120.0 . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.0 . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C11 C12 C8 120.0 . . ? C11 C12 H12 120.0 . . ? C8 C12 H12 120.0 . . ? C14 C13 C15 114.0(13) . . ? C14 C13 C16 110.7(11) . . ? C15 C13 C16 112.5(12) . . ? C14 C13 C5 110.1(13) . . ? C15 C13 C5 108.4(11) . . ? C16 C13 C5 100.3(12) . . ? F2 Sb1 F2 168.9(10) 5_556 . ? F2 Sb1 F4 91.5(9) 5_556 5_556 ? F2 Sb1 F4 88.9(9) . 5_556 ? F2 Sb1 F4 88.9(9) 5_556 . ? F2 Sb1 F4 91.5(9) . . ? F4 Sb1 F4 175.4(14) 5_556 . ? F2 Sb1 F1 95.5(5) 5_556 . ? F2 Sb1 F1 95.5(5) . . ? F4 Sb1 F1 87.7(7) 5_556 . ? F4 Sb1 F1 87.7(7) . . ? F2 Sb1 F3 84.5(5) 5_556 . ? F2 Sb1 F3 84.5(5) . . ? F4 Sb1 F3 92.3(7) 5_556 . ? F4 Sb1 F3 92.3(7) . . ? F1 Sb1 F3 180.000(4) . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 30.12 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 2.894 _refine_diff_density_min -1.680 _refine_diff_density_rms 0.277 _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 0.250 0.250 -0.067 370.8 -26.4 2 0.250 0.750 0.054 370.8 -26.6 3 0.500 0.500 0.000 11.5 -1.3 4 0.750 0.750 -0.064 370.8 -26.4 5 0.750 0.250 0.027 370.8 -26.6 6 0.000 0.000 0.097 11.2 -2.1 7 0.000 0.500 0.153 10.9 -2.2 8 0.500 0.000 0.250 11.5 -0.5 9 0.000 0.500 0.351 11.0 -2.5 10 0.500 0.500 0.403 10.9 -1.7 11 0.000 0.000 0.500 11.5 -1.3 12 0.500 0.500 0.601 11.0 -2.1 13 0.500 0.000 0.653 10.9 -2.2 14 0.000 0.500 0.750 11.5 -0.5 15 0.500 0.000 0.851 11.0 -2.5 16 0.000 0.000 0.899 10.7 -1.7 _platon_squeeze_details ; ; data_e1911a _database_code_depnum_ccdc_archive 'CCDC 895672' #TrackingRef 'web_deposit_cif_file_4_SylvieFERLAY_1344596913.3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H68 N4 O4 S4' _chemical_formula_sum 'C64 H68 N4 O4 S4' _chemical_formula_weight 1085.46 _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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/a _symmetry_space_group_name_Hall '-I 4ad' _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 19.446(2) _cell_length_b 19.446(2) _cell_length_c 15.0141(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5677.6(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2111 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 27.39 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.270 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2304 _exptl_absorpt_coefficient_mu 0.219 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9763 _exptl_absorpt_correction_T_max 0.9805 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 6235 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0420 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 27.26 _reflns_number_total 3047 _reflns_number_gt 2623 _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. ; _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^)+(0.0312P)^2^+21.6136P] 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 3047 _refine_ls_number_parameters 169 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0779 _refine_ls_R_factor_gt 0.0669 _refine_ls_wR_factor_ref 0.1449 _refine_ls_wR_factor_gt 0.1387 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _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 S1 S 0.20096(4) 0.26635(4) 0.12924(5) 0.02574(19) Uani 1 1 d . . . C1 C 0.15162(13) 0.20322(13) 0.07292(17) 0.0213(5) Uani 1 1 d . . . C2 C 0.10521(14) 0.16088(14) 0.11698(16) 0.0215(5) Uani 1 1 d . . . C3 C 0.07237(14) 0.10907(14) 0.06933(17) 0.0215(5) Uani 1 1 d . . . C4 C 0.08970(14) 0.09735(14) -0.01967(17) 0.0244(6) Uani 1 1 d . . . H4 H 0.0670 0.0617 -0.0514 0.029 Uiso 1 1 calc R . . C5 C 0.13950(14) 0.13659(14) -0.06337(17) 0.0229(5) Uani 1 1 d . . . C6 C 0.16821(14) 0.19097(14) -0.01659(17) 0.0232(5) Uani 1 1 d . . . H6 H 0.1998 0.2206 -0.0458 0.028 Uiso 1 1 calc R . . O1 O 0.09306(10) 0.16975(10) 0.20700(11) 0.0250(4) Uani 1 1 d . . . C7 C 0.13682(18) 0.12621(18) 0.25963(19) 0.0377(8) Uani 1 1 d . . . H7A H 0.1855 0.1352 0.2445 0.045 Uiso 1 1 calc R . . H7B H 0.1268 0.0774 0.2463 0.045 Uiso 1 1 calc R . . C8 C 0.12519(18) 0.13984(17) 0.35691(19) 0.0365(8) Uani 1 1 d . . . C9 C 0.1725(2) 0.1156(2) 0.4183(2) 0.0548(11) Uani 1 1 d . . . H9 H 0.2111 0.0906 0.3969 0.066 Uiso 1 1 calc R . . C10 C 0.1668(5) 0.1255(3) 0.5049(3) 0.0548(11) Uani 1 1 d . . . H10 H 0.1998 0.1069 0.5450 0.066 Uiso 1 1 calc R . . C11 C 0.1155(5) 0.1608(3) 0.5338(3) 0.0548(11) Uani 1 1 d . . . H11 H 0.1135 0.1697 0.5959 0.066 Uiso 1 1 calc R . . N2 N 0.0599(3) 0.1885(2) 0.4786(3) 0.0548(11) Uani 1 1 d . . . C12 C 0.0699(2) 0.1761(2) 0.3890(2) 0.0492(10) Uani 1 1 d . . . H12 H 0.0371 0.1934 0.3477 0.059 Uiso 1 1 calc R . . C13 C 0.16172(16) 0.11695(15) -0.15838(17) 0.0271(6) Uani 1 1 d . . . C14 C 0.20976(18) 0.17034(18) -0.19912(19) 0.0381(8) Uani 1 1 d . . . H14A H 0.1864 0.2149 -0.2015 0.057 Uiso 1 1 calc R . . H14B H 0.2225 0.1561 -0.2595 0.057 Uiso 1 1 calc R . . H14C H 0.2513 0.1743 -0.1625 0.057 Uiso 1 1 calc R . . C15 C 0.09867(18) 0.10963(18) -0.21901(19) 0.0378(7) Uani 1 1 d . . . H15A H 0.0757 0.1543 -0.2247 0.057 Uiso 1 1 calc R . . H15B H 0.0667 0.0762 -0.1931 0.057 Uiso 1 1 calc R . . H15C H 0.1133 0.0937 -0.2780 0.057 Uiso 1 1 calc R . . C16 C 0.19937(18) 0.04758(17) -0.15339(19) 0.0370(7) Uani 1 1 d . . . H16A H 0.2153 0.0345 -0.2130 0.055 Uiso 1 1 calc R . . H16B H 0.1679 0.0123 -0.1307 0.055 Uiso 1 1 calc R . . H16C H 0.2389 0.0516 -0.1133 0.055 Uiso 1 1 calc R . . _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 S1 0.0212(4) 0.0270(4) 0.0290(3) -0.0100(3) -0.0018(3) 0.0001(3) C1 0.0210(13) 0.0204(13) 0.0223(12) -0.0044(10) 0.0000(10) 0.0013(10) C2 0.0239(13) 0.0239(13) 0.0168(11) -0.0045(10) 0.0034(10) 0.0029(10) C3 0.0221(13) 0.0217(13) 0.0208(12) -0.0021(10) 0.0053(10) 0.0005(10) C4 0.0285(15) 0.0237(14) 0.0210(12) -0.0042(10) 0.0009(11) -0.0011(11) C5 0.0243(14) 0.0243(14) 0.0201(12) -0.0035(10) 0.0011(10) 0.0027(10) C6 0.0249(14) 0.0231(14) 0.0215(12) 0.0007(10) 0.0050(10) -0.0012(10) O1 0.0301(11) 0.0290(11) 0.0159(8) -0.0035(7) 0.0040(8) 0.0039(8) C7 0.0424(19) 0.048(2) 0.0229(14) -0.0012(13) -0.0021(13) 0.0084(15) C8 0.053(2) 0.0360(17) 0.0204(13) 0.0004(12) -0.0011(13) -0.0205(15) C9 0.080(3) 0.046(2) 0.0389(19) 0.0132(16) -0.0166(19) -0.021(2) C10 0.080(3) 0.046(2) 0.0389(19) 0.0132(16) -0.0166(19) -0.021(2) C11 0.080(3) 0.046(2) 0.0389(19) 0.0132(16) -0.0166(19) -0.021(2) N2 0.080(3) 0.046(2) 0.0389(19) 0.0132(16) -0.0166(19) -0.021(2) C12 0.072(3) 0.048(2) 0.0276(16) -0.0086(15) 0.0129(17) -0.0130(19) C13 0.0341(16) 0.0308(15) 0.0165(11) -0.0030(10) 0.0059(11) 0.0005(12) C14 0.0442(19) 0.046(2) 0.0238(14) -0.0015(13) 0.0126(13) -0.0045(15) C15 0.047(2) 0.047(2) 0.0199(13) -0.0026(13) -0.0026(13) -0.0019(15) C16 0.050(2) 0.0381(18) 0.0228(13) -0.0064(12) 0.0077(13) 0.0087(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C1 1.773(3) . ? S1 C3 1.774(3) 12_666 ? C1 C2 1.389(4) . ? C1 C6 1.403(3) . ? C2 O1 1.383(3) . ? C2 C3 1.391(4) . ? C3 C4 1.397(3) . ? C3 S1 1.774(3) 15 ? C4 C5 1.397(4) . ? C4 H4 0.9500 . ? C5 C6 1.387(4) . ? C5 C13 1.539(3) . ? C6 H6 0.9500 . ? O1 C7 1.437(4) . ? C7 C8 1.501(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C12 1.373(5) . ? C8 C9 1.385(5) . ? C9 C10 1.320(6) . ? C9 H9 0.9500 . ? C10 C11 1.287(11) . ? C10 H10 0.9500 . ? C11 N2 1.464(9) . ? C11 H11 0.9500 . ? N2 C12 1.382(5) . ? C12 H12 0.9500 . ? C13 C14 1.525(4) . ? C13 C15 1.534(4) . ? C13 C16 1.537(4) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? _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 C1 S1 C3 106.07(12) . 12_666 ? C2 C1 C6 120.3(2) . . ? C2 C1 S1 122.34(19) . . ? C6 C1 S1 116.8(2) . . ? O1 C2 C1 120.2(2) . . ? O1 C2 C3 121.0(2) . . ? C1 C2 C3 118.9(2) . . ? C2 C3 C4 120.0(2) . . ? C2 C3 S1 122.33(19) . 15 ? C4 C3 S1 117.2(2) . 15 ? C3 C4 C5 121.8(2) . . ? C3 C4 H4 119.1 . . ? C5 C4 H4 119.1 . . ? C6 C5 C4 117.2(2) . . ? C6 C5 C13 123.1(2) . . ? C4 C5 C13 119.6(2) . . ? C5 C6 C1 121.5(2) . . ? C5 C6 H6 119.3 . . ? C1 C6 H6 119.3 . . ? C2 O1 C7 111.3(2) . . ? O1 C7 C8 110.0(3) . . ? O1 C7 H7A 109.7 . . ? C8 C7 H7A 109.7 . . ? O1 C7 H7B 109.7 . . ? C8 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? C12 C8 C9 117.5(3) . . ? C12 C8 C7 123.3(3) . . ? C9 C8 C7 119.1(3) . . ? C10 C9 C8 123.4(6) . . ? C10 C9 H9 118.3 . . ? C8 C9 H9 118.3 . . ? C9 C10 C11 118.3(7) . . ? C9 C10 H10 120.8 . . ? C11 C10 H10 120.8 . . ? C10 C11 N2 125.4(5) . . ? C10 C11 H11 117.3 . . ? N2 C11 H11 117.3 . . ? C12 N2 C11 112.5(5) . . ? C8 C12 N2 122.8(4) . . ? C8 C12 H12 118.6 . . ? N2 C12 H12 118.6 . . ? C14 C13 C15 108.4(2) . . ? C14 C13 C16 109.0(3) . . ? C15 C13 C16 109.2(3) . . ? C14 C13 C5 112.0(2) . . ? C15 C13 C5 110.4(2) . . ? C16 C13 C5 107.8(2) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.26 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.688 _refine_diff_density_min -0.621 _refine_diff_density_rms 0.060 data_e2344a _database_code_depnum_ccdc_archive 'CCDC 895673' #TrackingRef 'web_deposit_cif_file_5_SylvieFERLAY_1344596913.3-AgBF4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C129 H140 Ag4 N8 O9 S8, 4(B F4), 7(C H Cl3), 2(H2 0)' _chemical_formula_sum 'C136 H151 Ag4 B4 Cl21 F16 N8 O11 S8' _chemical_formula_weight 3853.30 _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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 22.6083(13) _cell_length_b 28.6805(14) _cell_length_c 27.2831(13) _cell_angle_alpha 90.00 _cell_angle_beta 100.757(2) _cell_angle_gamma 90.00 _cell_volume 17380.0(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9887 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 24.03 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7792 _exptl_absorpt_coefficient_mu 0.933 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9291 _exptl_absorpt_correction_T_max 0.9548 _exptl_absorpt_process_details sadabs _exptl_special_details ; Owing to large disorder of the solvent present in the cavities of this structure, the SQUEEZE command has been applied. Some constraints and EADP fonctions were applied because of the flopiness of some tertiobutyls groups and chloroform The hydrogen of the water molecule were not found but they were introduced in the molecular formula ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 199983 _diffrn_reflns_av_R_equivalents 0.0992 _diffrn_reflns_av_sigmaI/netI 0.1416 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 30.10 _reflns_number_total 50328 _reflns_number_gt 19590 _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. ; _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^)+(0.1904P)^2^+0.4118P] 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 50328 _refine_ls_number_parameters 1959 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.2355 _refine_ls_R_factor_gt 0.1203 _refine_ls_wR_factor_ref 0.3059 _refine_ls_wR_factor_gt 0.2682 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.025 _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 0.20917(3) 0.07951(3) -0.04355(2) 0.0523(2) Uani 1 1 d . . 1 Ag2 Ag 0.31652(3) 0.06387(3) 0.54824(2) 0.0496(2) Uani 1 1 d . . 1 Ag3 Ag 0.19480(3) -0.21133(3) 0.46851(2) 0.0546(2) Uani 1 1 d . . 1 Ag4 Ag 0.31653(4) -0.17627(3) 1.04875(2) 0.0568(2) Uani 1 1 d . . 1 S1 S 0.06388(8) 0.12777(7) 0.20210(7) 0.0356(4) Uani 1 1 d . . 1 C1 C 0.1037(3) 0.0858(2) 0.2424(2) 0.0257(14) Uani 1 1 d . . 1 C2 C 0.1563(3) 0.0653(2) 0.2332(2) 0.0269(15) Uani 1 1 d . . 1 C3 C 0.1800(3) 0.0268(3) 0.2614(3) 0.0303(16) Uani 1 1 d . . 1 C4 C 0.1508(3) 0.0095(2) 0.2989(3) 0.0309(16) Uani 1 1 d . . 1 H4 H 0.1682 -0.0159 0.3190 0.037 Uiso 1 1 calc R . 1 C5 C 0.0980(3) 0.0284(3) 0.3073(3) 0.0298(15) Uani 1 1 d . . 1 C6 C 0.0759(3) 0.0670(2) 0.2797(2) 0.0274(15) Uani 1 1 d . . 1 H6 H 0.0403 0.0813 0.2862 0.033 Uiso 1 1 calc R . 1 O1 O 0.1864(2) 0.08360(17) 0.19820(16) 0.0300(11) Uani 1 1 d . . 1 C7 C 0.1711(4) 0.0636(3) 0.1500(3) 0.0376(18) Uani 1 1 d . . 1 H7A H 0.1279 0.0687 0.1364 0.045 Uiso 1 1 calc R . 1 H7B H 0.1788 0.0296 0.1519 0.045 Uiso 1 1 calc R . 1 C8 C 0.2088(3) 0.0861(3) 0.1167(2) 0.0302(16) Uani 1 1 d . . 1 C9 C 0.1978(4) 0.0764(3) 0.0668(3) 0.0397(19) Uani 1 1 d . . 1 H9 H 0.1660 0.0555 0.0543 0.048 Uiso 1 1 calc R . 1 N1 N 0.2298(3) 0.0950(3) 0.0343(2) 0.0437(17) Uani 1 1 d . . 1 C10 C 0.2748(4) 0.1241(3) 0.0525(3) 0.0401(19) Uani 1 1 d . . 1 H10 H 0.2976 0.1377 0.0302 0.048 Uiso 1 1 calc R . 1 C11 C 0.2887(4) 0.1349(3) 0.1015(3) 0.0412(19) Uani 1 1 d . . 1 H11 H 0.3215 0.1551 0.1133 0.049 Uiso 1 1 calc R . 1 C12 C 0.2556(3) 0.1167(3) 0.1346(3) 0.0351(17) Uani 1 1 d . . 1 H12 H 0.2646 0.1249 0.1689 0.042 Uiso 1 1 calc R . 1 C13 C 0.0622(4) 0.0079(3) 0.3458(3) 0.0409(19) Uani 1 1 d . . 1 C14 C 0.0529(6) 0.0489(5) 0.3842(4) 0.094(4) Uani 1 1 d . . 1 H14A H 0.0919 0.0634 0.3976 0.141 Uiso 1 1 calc R . 1 H14B H 0.0357 0.0358 0.4116 0.141 Uiso 1 1 calc R . 1 H14C H 0.0255 0.0725 0.3666 0.141 Uiso 1 1 calc R . 1 C15 C 0.0955(6) -0.0304(7) 0.3764(6) 0.160(9) Uani 1 1 d . . 1 H15A H 0.0889 -0.0280 0.4108 0.241 Uiso 1 1 calc R . 1 H15B H 0.1386 -0.0277 0.3760 0.241 Uiso 1 1 calc R . 1 H15C H 0.0807 -0.0606 0.3624 0.241 Uiso 1 1 calc R . 1 C16 C -0.0002(5) -0.0027(6) 0.3218(5) 0.106(5) Uani 1 1 d . . 1 H16A H -0.0005 -0.0291 0.2990 0.160 Uiso 1 1 calc R . 1 H16B H -0.0180 0.0246 0.3031 0.160 Uiso 1 1 calc R . 1 H16C H -0.0237 -0.0106 0.3474 0.160 Uiso 1 1 calc R . 1 S2 S 0.24049(9) -0.00774(7) 0.24909(8) 0.0392(5) Uani 1 1 d . . 1 C17 C 0.2973(3) 0.0300(2) 0.2344(3) 0.0280(15) Uani 1 1 d . . 1 C18 C 0.3207(3) 0.0659(2) 0.2642(2) 0.0286(15) Uani 1 1 d . . 1 C19 C 0.3721(3) 0.0894(2) 0.2544(2) 0.0269(15) Uani 1 1 d . . 1 C20 C 0.3972(3) 0.0743(3) 0.2142(3) 0.0327(16) Uani 1 1 d . . 1 H20 H 0.4314 0.0902 0.2069 0.039 Uiso 1 1 calc R . 1 C21 C 0.3743(3) 0.0374(2) 0.1849(2) 0.0279(15) Uani 1 1 d . . 1 C22 C 0.3241(3) 0.0155(3) 0.1954(3) 0.0332(16) Uani 1 1 d . . 1 H22 H 0.3075 -0.0102 0.1755 0.040 Uiso 1 1 calc R . 1 O2 O 0.2939(2) 0.08152(17) 0.30327(17) 0.0316(11) Uani 1 1 d . . 1 C23 C 0.3145(4) 0.0571(3) 0.3496(2) 0.0370(18) Uani 1 1 d . . 1 H23A H 0.3581 0.0625 0.3612 0.044 Uiso 1 1 calc R . 1 H23B H 0.3077 0.0232 0.3449 0.044 Uiso 1 1 calc R . 1 C24 C 0.2800(3) 0.0752(2) 0.3873(3) 0.0318(16) Uani 1 1 d . . 1 C25 C 0.3006(4) 0.0637(3) 0.4362(3) 0.0381(18) Uani 1 1 d . . 1 H25 H 0.3361 0.0453 0.4441 0.046 Uiso 1 1 calc R . 1 N2 N 0.2735(3) 0.0769(2) 0.4737(2) 0.0409(16) Uani 1 1 d . . 1 C26 C 0.2228(4) 0.1005(3) 0.4625(3) 0.047(2) Uani 1 1 d . . 1 H26 H 0.2022 0.1089 0.4885 0.056 Uiso 1 1 calc R . 1 C27 C 0.1982(4) 0.1137(3) 0.4135(3) 0.044(2) Uani 1 1 d . . 1 H27 H 0.1613 0.1304 0.4063 0.052 Uiso 1 1 calc R . 1 C28 C 0.2288(4) 0.1017(3) 0.3754(3) 0.0399(19) Uani 1 1 d . . 1 H28 H 0.2146 0.1117 0.3420 0.048 Uiso 1 1 calc R . 1 C29 C 0.4031(3) 0.0192(3) 0.1414(3) 0.0390(19) Uani 1 1 d . . 1 C30 C 0.4324(7) 0.0592(4) 0.1164(5) 0.107(6) Uani 1 1 d . . 1 H30A H 0.4733 0.0647 0.1348 0.160 Uiso 1 1 calc R . 1 H30B H 0.4084 0.0876 0.1165 0.160 Uiso 1 1 calc R . 1 H30C H 0.4340 0.0505 0.0819 0.160 Uiso 1 1 calc R . 1 C31 C 0.4479(8) -0.0157(6) 0.1614(5) 0.149(9) Uani 1 1 d . . 1 H31A H 0.4287 -0.0407 0.1773 0.224 Uiso 1 1 calc R . 1 H31B H 0.4796 -0.0012 0.1861 0.224 Uiso 1 1 calc R . 1 H31C H 0.4656 -0.0288 0.1342 0.224 Uiso 1 1 calc R . 1 C32 C 0.3598(5) 0.0003(5) 0.0999(4) 0.093(4) Uani 1 1 d . . 1 H32A H 0.3304 0.0245 0.0868 0.139 Uiso 1 1 calc R . 1 H32B H 0.3389 -0.0263 0.1114 0.139 Uiso 1 1 calc R . 1 H32C H 0.3809 -0.0099 0.0735 0.139 Uiso 1 1 calc R . 1 S3 S 0.41416(8) 0.13028(7) 0.29577(6) 0.0312(4) Uani 1 1 d . . 1 C33 C 0.3623(3) 0.1686(2) 0.3160(2) 0.0268(15) Uani 1 1 d . . 1 C34 C 0.3233(3) 0.1962(3) 0.2835(2) 0.0303(16) Uani 1 1 d . . 1 C35 C 0.2842(3) 0.2268(2) 0.3019(3) 0.0309(16) Uani 1 1 d . . 1 C36 C 0.2912(3) 0.2341(3) 0.3532(3) 0.0334(16) Uani 1 1 d . . 1 H36 H 0.2664 0.2563 0.3655 0.040 Uiso 1 1 calc R . 1 C37 C 0.3343(3) 0.2092(3) 0.3870(3) 0.0333(16) Uani 1 1 d . . 1 C38 C 0.3672(3) 0.1753(3) 0.3673(2) 0.0303(16) Uani 1 1 d . . 1 H38 H 0.3939 0.1560 0.3896 0.036 Uiso 1 1 calc R . 1 O3 O 0.3258(2) 0.19605(18) 0.23259(16) 0.0336(12) Uani 1 1 d . . 1 C39 C 0.3683(4) 0.2330(3) 0.2259(3) 0.0411(19) Uani 1 1 d . . 1 H39A H 0.4054 0.2302 0.2515 0.049 Uiso 1 1 calc R . 1 H39B H 0.3501 0.2640 0.2294 0.049 Uiso 1 1 calc R . 1 C40 C 0.3827(3) 0.2282(3) 0.1755(3) 0.0370(17) Uani 1 1 d . . 1 C41 C 0.3493(4) 0.2529(3) 0.1359(3) 0.042(2) Uani 1 1 d . . 1 H41 H 0.3188 0.2736 0.1424 0.051 Uiso 1 1 calc R . 1 N3 N 0.3587(3) 0.2486(2) 0.0883(2) 0.0462(17) Uani 1 1 d . . 1 C42 C 0.4044(4) 0.2225(3) 0.0809(3) 0.047(2) Uani 1 1 d . . 1 H42 H 0.4128 0.2208 0.0481 0.057 Uiso 1 1 calc R . 1 C43 C 0.4399(4) 0.1979(3) 0.1174(3) 0.055(2) Uani 1 1 d . . 1 H43 H 0.4720 0.1795 0.1100 0.066 Uiso 1 1 calc R . 1 C44 C 0.4290(4) 0.1999(3) 0.1666(3) 0.051(2) Uani 1 1 d . . 1 H44 H 0.4528 0.1825 0.1926 0.061 Uiso 1 1 calc R . 1 C45 C 0.3471(3) 0.2216(2) 0.4417(3) 0.0376(18) Uani 1 1 d D . 1 C46 C 0.3862(10) 0.1825(6) 0.4702(7) 0.060(2) Uani 0.411(10) 1 d PD . 1 H46A H 0.3608 0.1556 0.4740 0.090 Uiso 0.411(10) 1 calc PR . 1 H46B H 0.4054 0.1939 0.5032 0.090 Uiso 0.411(10) 1 calc PR . 1 H46C H 0.4173 0.1732 0.4514 0.090 Uiso 0.411(10) 1 calc PR . 1 C47 C 0.2877(7) 0.2262(8) 0.4603(7) 0.060(2) Uani 0.411(10) 1 d PD . 1 H47A H 0.2620 0.2491 0.4397 0.090 Uiso 0.411(10) 1 calc PR . 1 H47B H 0.2957 0.2367 0.4951 0.090 Uiso 0.411(10) 1 calc PR . 1 H47C H 0.2673 0.1960 0.4579 0.090 Uiso 0.411(10) 1 calc PR . 1 C48 C 0.3819(10) 0.2677(6) 0.4481(8) 0.060(2) Uani 0.411(10) 1 d PD . 1 H48A H 0.4212 0.2634 0.4384 0.090 Uiso 0.411(10) 1 calc PR . 1 H48B H 0.3879 0.2776 0.4830 0.090 Uiso 0.411(10) 1 calc PR . 1 H48C H 0.3591 0.2916 0.4269 0.090 Uiso 0.411(10) 1 calc PR . 1 C46A C 0.4130(6) 0.2402(6) 0.4558(5) 0.060(2) Uani 0.589(10) 1 d PD . 2 H46D H 0.4411 0.2139 0.4591 0.090 Uiso 0.589(10) 1 calc PR . 2 H46E H 0.4179 0.2572 0.4875 0.090 Uiso 0.589(10) 1 calc PR . 2 H46F H 0.4212 0.2613 0.4295 0.090 Uiso 0.589(10) 1 calc PR . 2 C47A C 0.3050(7) 0.2591(5) 0.4557(5) 0.060(2) Uani 0.589(10) 1 d PD . 2 H47D H 0.3085 0.2874 0.4364 0.090 Uiso 0.589(10) 1 calc PR . 2 H47E H 0.3162 0.2660 0.4914 0.090 Uiso 0.589(10) 1 calc PR . 2 H47F H 0.2634 0.2478 0.4483 0.090 Uiso 0.589(10) 1 calc PR . 2 C48A C 0.3415(8) 0.1774(4) 0.4722(5) 0.060(2) Uani 0.589(10) 1 d PD . 2 H48D H 0.3008 0.1646 0.4626 0.090 Uiso 0.589(10) 1 calc PR . 2 H48E H 0.3493 0.1851 0.5078 0.090 Uiso 0.589(10) 1 calc PR . 2 H48F H 0.3710 0.1543 0.4656 0.090 Uiso 0.589(10) 1 calc PR . 2 S4 S 0.23555(9) 0.26622(7) 0.26284(8) 0.0403(5) Uani 1 1 d . . . C49 C 0.1887(3) 0.2318(2) 0.2172(3) 0.0306(16) Uani 1 1 d . . . C50 C 0.1523(3) 0.1953(3) 0.2305(2) 0.0297(16) Uani 1 1 d . . . C51 C 0.1149(3) 0.1718(3) 0.1928(3) 0.0309(16) Uani 1 1 d . . . C52 C 0.1086(3) 0.1863(3) 0.1428(3) 0.0345(17) Uani 1 1 d . . . H52 H 0.0815 0.1703 0.1176 0.041 Uiso 1 1 calc R . . C53 C 0.1423(3) 0.2247(3) 0.1298(3) 0.0345(17) Uani 1 1 d . . . C54 C 0.1821(3) 0.2451(3) 0.1674(3) 0.0384(18) Uani 1 1 d . . . H54 H 0.2067 0.2696 0.1591 0.046 Uiso 1 1 calc R . . O4 O 0.1570(2) 0.18163(18) 0.27923(16) 0.0364(12) Uani 1 1 d . . . C55 C 0.1070(4) 0.1959(4) 0.3019(3) 0.054(2) Uani 1 1 d . . . H55A H 0.1071 0.1770 0.3324 0.065 Uiso 1 1 calc R . . H55B H 0.0689 0.1893 0.2785 0.065 Uiso 1 1 calc R . . C56 C 0.1089(4) 0.2460(3) 0.3154(3) 0.048(2) Uani 1 1 d . . . C57 C 0.1374(4) 0.2592(4) 0.3634(3) 0.053(2) Uani 1 1 d . . . H57 H 0.1535 0.2357 0.3867 0.064 Uiso 1 1 calc R . . N4 N 0.1425(4) 0.3031(3) 0.3772(2) 0.059(2) Uani 1 1 d . . . C58 C 0.1197(5) 0.3363(4) 0.3444(3) 0.068(3) Uani 1 1 d . . . H58 H 0.1225 0.3679 0.3547 0.082 Uiso 1 1 calc R . . C59 C 0.0924(5) 0.3257(4) 0.2962(4) 0.073(3) Uani 1 1 d . . . H59 H 0.0783 0.3498 0.2730 0.088 Uiso 1 1 calc R . . C60 C 0.0859(4) 0.2798(4) 0.2824(3) 0.063(3) Uani 1 1 d . . . H60 H 0.0655 0.2716 0.2499 0.076 Uiso 1 1 calc R . . C61 C 0.1323(3) 0.2407(3) 0.0745(3) 0.0398(19) Uani 1 1 d D . . C62 C 0.1638(12) 0.2057(7) 0.0486(6) 0.074(7) Uani 0.63(2) 1 d PD . 1 H62A H 0.1588 0.2137 0.0132 0.111 Uiso 0.63(2) 1 calc PR . 1 H62B H 0.1468 0.1747 0.0522 0.111 Uiso 0.63(2) 1 calc PR . 1 H62C H 0.2068 0.2056 0.0635 0.111 Uiso 0.63(2) 1 calc PR . 1 C63 C 0.0652(5) 0.2464(7) 0.0519(5) 0.074(7) Uani 0.63(2) 1 d PD . 1 H63A H 0.0603 0.2500 0.0157 0.111 Uiso 0.63(2) 1 calc PR . 1 H63B H 0.0495 0.2742 0.0661 0.111 Uiso 0.63(2) 1 calc PR . 1 H63C H 0.0431 0.2188 0.0596 0.111 Uiso 0.63(2) 1 calc PR . 1 C64 C 0.1625(8) 0.2904(5) 0.0728(6) 0.074(7) Uani 0.63(2) 1 d PD . 1 H64A H 0.1816 0.2924 0.0434 0.111 Uiso 0.63(2) 1 calc PR . 1 H64B H 0.1930 0.2949 0.1030 0.111 Uiso 0.63(2) 1 calc PR . 1 H64C H 0.1316 0.3147 0.0709 0.111 Uiso 0.63(2) 1 calc PR . 1 C62A C 0.0991(15) 0.2886(8) 0.0706(11) 0.103(17) Uani 0.37(2) 1 d PD . 2 H62D H 0.1035 0.3042 0.0395 0.155 Uiso 0.37(2) 1 calc PR . 2 H62E H 0.1166 0.3083 0.0990 0.155 Uiso 0.37(2) 1 calc PR . 2 H62F H 0.0563 0.2836 0.0708 0.155 Uiso 0.37(2) 1 calc PR . 2 C63A C 0.0885(13) 0.2062(10) 0.0397(7) 0.081(15) Uani 0.37(2) 1 d PD . 2 H63D H 0.0939 0.2099 0.0051 0.121 Uiso 0.37(2) 1 calc PR . 2 H63E H 0.0467 0.2134 0.0420 0.121 Uiso 0.37(2) 1 calc PR . 2 H63F H 0.0978 0.1740 0.0506 0.121 Uiso 0.37(2) 1 calc PR . 2 C64A C 0.1915(8) 0.2445(11) 0.0568(10) 0.066(10) Uani 0.37(2) 1 d PD . 2 H64D H 0.2193 0.2207 0.0734 0.098 Uiso 0.37(2) 1 calc PR . 2 H64E H 0.2088 0.2755 0.0649 0.098 Uiso 0.37(2) 1 calc PR . 2 H64F H 0.1848 0.2398 0.0206 0.098 Uiso 0.37(2) 1 calc PR . 2 S5 S 0.27688(9) 0.01322(6) 0.73259(7) 0.0355(4) Uani 1 1 d . . . C65 C 0.3214(3) -0.0214(3) 0.7799(3) 0.0329(16) Uani 1 1 d . . . C66 C 0.3560(3) -0.0587(2) 0.7679(2) 0.0246(14) Uani 1 1 d . . . C67 C 0.3918(3) -0.0820(2) 0.8069(2) 0.0275(15) Uani 1 1 d . . . C68 C 0.3952(3) -0.0665(2) 0.8555(2) 0.0290(15) Uani 1 1 d . . . H68 H 0.4204 -0.0830 0.8816 0.035 Uiso 1 1 calc R . . C69 C 0.3640(3) -0.0287(3) 0.8679(3) 0.0320(16) Uani 1 1 d . . . C70 C 0.3259(3) -0.0069(2) 0.8288(3) 0.0321(16) Uani 1 1 d . . . H70 H 0.3021 0.0187 0.8358 0.038 Uiso 1 1 calc R . . O5 O 0.3524(2) -0.07243(17) 0.71916(16) 0.0308(11) Uani 1 1 d . . . C71 C 0.4043(4) -0.0618(3) 0.6971(3) 0.0367(18) Uani 1 1 d . . . H71A H 0.4042 -0.0819 0.6677 0.044 Uiso 1 1 calc R . . H71B H 0.4416 -0.0682 0.7216 0.044 Uiso 1 1 calc R . . C72 C 0.4035(4) -0.0118(3) 0.6817(3) 0.0401(19) Uani 1 1 d . . . C73 C 0.3741(4) 0.0022(3) 0.6349(3) 0.0389(18) Uani 1 1 d . . . H73 H 0.3567 -0.0214 0.6123 0.047 Uiso 1 1 calc R . . N5 N 0.3683(3) 0.0451(2) 0.6196(2) 0.0417(16) Uani 1 1 d . . . C74 C 0.3944(4) 0.0791(3) 0.6506(3) 0.051(2) Uani 1 1 d . . . H74 H 0.3916 0.1104 0.6392 0.062 Uiso 1 1 calc R . . C75 C 0.4245(5) 0.0701(3) 0.6977(4) 0.060(3) Uani 1 1 d . . . H75 H 0.4416 0.0946 0.7192 0.072 Uiso 1 1 calc R . . C76 C 0.4293(4) 0.0239(4) 0.7131(4) 0.057(2) Uani 1 1 d . . . H76 H 0.4505 0.0165 0.7456 0.068 Uiso 1 1 calc R . . C77 C 0.3709(3) -0.0120(3) 0.9218(3) 0.0355(17) Uani 1 1 d . . . C78 C 0.4357(4) -0.0034(5) 0.9443(4) 0.089(4) Uani 1 1 d . . . H78A H 0.4504 0.0236 0.9281 0.133 Uiso 1 1 calc R . . H78B H 0.4596 -0.0310 0.9395 0.133 Uiso 1 1 calc R . . H78C H 0.4393 0.0028 0.9801 0.133 Uiso 1 1 calc R . . C79 C 0.3399(8) 0.0319(7) 0.9266(5) 0.089(4) Uani 1 1 d . . . H79A H 0.3080 0.0364 0.8973 0.133 Uiso 1 1 calc R . . H79B H 0.3687 0.0577 0.9290 0.133 Uiso 1 1 calc R . . H79C H 0.3222 0.0311 0.9567 0.133 Uiso 1 1 calc R . . C80 C 0.3502(11) -0.0500(6) 0.9519(5) 0.089(4) Uani 1 1 d . . . H80A H 0.3700 -0.0467 0.9869 0.133 Uiso 1 1 calc R . . H80B H 0.3605 -0.0803 0.9392 0.133 Uiso 1 1 calc R . . H80C H 0.3065 -0.0479 0.9494 0.133 Uiso 1 1 calc R . . S6 S 0.44024(8) -0.12878(6) 0.79770(6) 0.0279(4) Uani 1 1 d . . . C81 C 0.3965(3) -0.1698(2) 0.7574(2) 0.0222(13) Uani 1 1 d . . . C82 C 0.3432(3) -0.1883(2) 0.7683(2) 0.0227(14) Uani 1 1 d . . . C83 C 0.3160(3) -0.2249(2) 0.7405(3) 0.0275(15) Uani 1 1 d . . . C84 C 0.3412(3) -0.2429(2) 0.7015(3) 0.0305(16) Uani 1 1 d . . . H84 H 0.3217 -0.2681 0.6824 0.037 Uiso 1 1 calc R . . C85 C 0.3938(3) -0.2249(2) 0.6898(2) 0.0280(15) Uani 1 1 d . . . C86 C 0.4215(3) -0.1880(2) 0.7187(2) 0.0258(14) Uani 1 1 d . . . H86 H 0.4578 -0.1753 0.7119 0.031 Uiso 1 1 calc R . . O6 O 0.3177(2) -0.16858(17) 0.80589(17) 0.0302(11) Uani 1 1 d . . . C87 C 0.3348(4) -0.1900(3) 0.8541(3) 0.0404(19) Uani 1 1 d . . . H87A H 0.3784 -0.1855 0.8668 0.048 Uiso 1 1 calc R . . H87B H 0.3264 -0.2238 0.8519 0.048 Uiso 1 1 calc R . . C88 C 0.2990(4) -0.1673(3) 0.8881(3) 0.0354(17) Uani 1 1 d . . . C89 C 0.3143(4) -0.1783(3) 0.9382(3) 0.0395(18) Uani 1 1 d . . . H89 H 0.3480 -0.1980 0.9491 0.047 Uiso 1 1 calc R . . N6 N 0.2825(3) -0.1615(2) 0.9725(2) 0.0402(16) Uani 1 1 d . . . C90 C 0.2357(4) -0.1344(3) 0.9569(3) 0.046(2) Uani 1 1 d . . . H90 H 0.2135 -0.1227 0.9805 0.055 Uiso 1 1 calc R . . C91 C 0.2176(4) -0.1221(3) 0.9068(3) 0.046(2) Uani 1 1 d . . . H91 H 0.1834 -0.1028 0.8966 0.055 Uiso 1 1 calc R . . C92 C 0.2498(3) -0.1382(3) 0.8724(3) 0.0381(18) Uani 1 1 d . . . H92 H 0.2387 -0.1297 0.8383 0.046 Uiso 1 1 calc R . . C93 C 0.4209(4) -0.2462(3) 0.6471(3) 0.0413(19) Uani 1 1 d . . . C94 C 0.3738(7) -0.2434(9) 0.6001(4) 0.0413(19) Uani 1 1 d . . . H94A H 0.3390 -0.2624 0.6039 0.054 Uiso 1 1 calc R . . H94B H 0.3908 -0.2550 0.5719 0.054 Uiso 1 1 calc R . . H94C H 0.3612 -0.2109 0.5940 0.054 Uiso 1 1 calc R . . C95 C 0.4775(7) -0.2224(6) 0.6402(6) 0.0413(19) Uani 1 1 d . . . H95A H 0.4956 -0.2396 0.6157 0.054 Uiso 1 1 calc R . . H95B H 0.5057 -0.2214 0.6721 0.054 Uiso 1 1 calc R . . H95C H 0.4682 -0.1906 0.6282 0.054 Uiso 1 1 calc R . . C96 C 0.4299(9) -0.2983(5) 0.6581(7) 0.0413(19) Uani 1 1 d . . . H96A H 0.3953 -0.3105 0.6710 0.054 Uiso 1 1 calc R . . H96B H 0.4666 -0.3029 0.6831 0.054 Uiso 1 1 calc R . . H96C H 0.4336 -0.3148 0.6274 0.054 Uiso 1 1 calc R . . S7 S 0.25674(9) -0.25796(7) 0.75732(8) 0.0416(5) Uani 1 1 d . . . C97 C 0.2020(3) -0.2178(3) 0.7728(3) 0.0341(17) Uani 1 1 d . . . C98 C 0.1808(3) -0.1811(2) 0.7439(3) 0.0287(15) Uani 1 1 d . . . C99 C 0.1302(3) -0.1572(3) 0.7530(3) 0.0320(16) Uani 1 1 d . . . C100 C 0.1021(3) -0.1728(3) 0.7919(3) 0.0337(17) Uani 1 1 d . . . H100 H 0.0675 -0.1569 0.7983 0.040 Uiso 1 1 calc R . . C101 C 0.1241(3) -0.2113(3) 0.8216(3) 0.0363(18) Uani 1 1 d . . . C102 C 0.1734(3) -0.2324(3) 0.8115(3) 0.0341(17) Uani 1 1 d . . . H102 H 0.1895 -0.2582 0.8314 0.041 Uiso 1 1 calc R . . O7 O 0.2091(2) -0.16583(16) 0.70625(17) 0.0281(10) Uani 1 1 d . . . C103 C 0.1866(4) -0.1892(3) 0.6602(3) 0.0399(19) Uani 1 1 d . . . H10A H 0.1433 -0.1823 0.6491 0.048 Uiso 1 1 calc R . . H10B H 0.1915 -0.2233 0.6646 0.048 Uiso 1 1 calc R . . C104 C 0.2219(3) -0.1721(3) 0.6218(3) 0.0309(16) Uani 1 1 d . . . C105 C 0.2067(4) -0.1912(3) 0.5748(3) 0.0380(18) Uani 1 1 d . . . H105 H 0.1763 -0.2144 0.5689 0.046 Uiso 1 1 calc R . . N7 N 0.2334(4) -0.1780(3) 0.5370(2) 0.0484(18) Uani 1 1 d . . . C106 C 0.2769(4) -0.1470(3) 0.5447(3) 0.0411(19) Uani 1 1 d . . . H106 H 0.2963 -0.1384 0.5180 0.049 Uiso 1 1 calc R . . C107 C 0.2950(4) -0.1265(3) 0.5914(3) 0.046(2) Uani 1 1 d . . . H107 H 0.3269 -0.1044 0.5967 0.055 Uiso 1 1 calc R . . C108 C 0.2665(4) -0.1385(3) 0.6298(3) 0.0385(18) Uani 1 1 d . . . H108 H 0.2773 -0.1239 0.6615 0.046 Uiso 1 1 calc R . . C109 C 0.0890(4) -0.2293(3) 0.8615(3) 0.048(2) Uani 1 1 d . . . C110 C 0.0291(4) -0.2477(4) 0.8336(4) 0.071(3) Uani 1 1 d . . . H11A H 0.0363 -0.2709 0.8089 0.107 Uiso 1 1 calc R . . H11B H 0.0053 -0.2219 0.8166 0.107 Uiso 1 1 calc R . . H11C H 0.0071 -0.2623 0.8573 0.107 Uiso 1 1 calc R . . C111 C 0.1239(6) -0.2653(5) 0.8940(5) 0.111(6) Uani 1 1 d . . . H11D H 0.1349 -0.2906 0.8734 0.167 Uiso 1 1 calc R . . H11E H 0.0992 -0.2777 0.9170 0.167 Uiso 1 1 calc R . . H11F H 0.1605 -0.2512 0.9133 0.167 Uiso 1 1 calc R . . C112 C 0.0735(4) -0.1885(4) 0.8937(3) 0.067(3) Uani 1 1 d . . . H11G H 0.0537 -0.2006 0.9201 0.101 Uiso 1 1 calc R . . H11H H 0.0465 -0.1667 0.8727 0.101 Uiso 1 1 calc R . . H11I H 0.1106 -0.1722 0.9088 0.101 Uiso 1 1 calc R . . S8 S 0.08849(8) -0.11624(7) 0.71180(7) 0.0346(4) Uani 1 1 d . . . C113 C 0.1401(3) -0.0785(3) 0.6892(2) 0.0284(15) Uani 1 1 d . . . C114 C 0.1837(3) -0.0528(2) 0.7201(2) 0.0270(15) Uani 1 1 d . . . C115 C 0.2204(3) -0.0236(2) 0.6988(2) 0.0265(14) Uani 1 1 d . . . C116 C 0.2098(3) -0.0171(2) 0.6470(3) 0.0314(16) Uani 1 1 d . . . H116 H 0.2359 0.0026 0.6328 0.038 Uiso 1 1 calc R . . C117 C 0.1617(3) -0.0391(3) 0.6157(2) 0.0300(15) Uani 1 1 d . . . C118 C 0.1286(3) -0.0712(2) 0.6380(2) 0.0268(15) Uani 1 1 d . . . H118 H 0.0976 -0.0885 0.6177 0.032 Uiso 1 1 calc R . . O8 O 0.1925(2) -0.05661(18) 0.77162(17) 0.0354(12) Uani 1 1 d . . . C119 C 0.1454(4) -0.0368(3) 0.7943(3) 0.049(2) Uani 1 1 d . . . H11J H 0.1414 -0.0555 0.8240 0.059 Uiso 1 1 calc R . . H11K H 0.1068 -0.0388 0.7703 0.059 Uiso 1 1 calc R . . C120 C 0.1567(4) 0.0123(3) 0.8094(3) 0.0416(19) Uani 1 1 d . . . C121 C 0.1748(4) 0.0233(3) 0.8609(3) 0.043(2) Uani 1 1 d . . . H121 H 0.1786 -0.0016 0.8842 0.051 Uiso 1 1 calc R . . N8 N 0.1867(3) 0.0654(3) 0.8780(2) 0.0469(18) Uani 1 1 d . . . C122 C 0.1841(5) 0.1009(3) 0.8437(3) 0.054(2) Uani 1 1 d . . . H122 H 0.1949 0.1315 0.8555 0.065 Uiso 1 1 calc R . . C123 C 0.1666(5) 0.0944(4) 0.7932(3) 0.063(3) Uani 1 1 d . . . H123 H 0.1644 0.1197 0.7705 0.075 Uiso 1 1 calc R . . C124 C 0.1521(5) 0.0490(3) 0.7765(3) 0.059(3) Uani 1 1 d . . . H124 H 0.1389 0.0434 0.7419 0.071 Uiso 1 1 calc R . . C125 C 0.1449(3) -0.0288(3) 0.5598(3) 0.0348(17) Uani 1 1 d . . . C126 C 0.0935(6) 0.0026(5) 0.5502(4) 0.103(5) Uani 1 1 d . . . H12A H 0.1050 0.0329 0.5658 0.154 Uiso 1 1 calc R . . H12B H 0.0604 -0.0106 0.5643 0.154 Uiso 1 1 calc R . . H12C H 0.0806 0.0067 0.5142 0.154 Uiso 1 1 calc R . . C127 C 0.1970(5) -0.0053(5) 0.5403(3) 0.086(4) Uani 1 1 d . . . H12D H 0.1997 0.0275 0.5505 0.129 Uiso 1 1 calc R . . H12E H 0.1898 -0.0072 0.5038 0.129 Uiso 1 1 calc R . . H12F H 0.2348 -0.0212 0.5541 0.129 Uiso 1 1 calc R . . C128 C 0.1317(8) -0.0727(4) 0.5301(3) 0.112(6) Uani 1 1 d . . . H12G H 0.1252 -0.0653 0.4945 0.169 Uiso 1 1 calc R . . H12H H 0.0955 -0.0874 0.5380 0.169 Uiso 1 1 calc R . . H12I H 0.1659 -0.0941 0.5385 0.169 Uiso 1 1 calc R . . B1 B 0.3230(6) 0.9434(4) 0.4535(5) 0.058(3) Uani 1 1 d . . . F1 F 0.3369(3) 0.9567(3) 0.5019(3) 0.093(2) Uani 1 1 d . . . F2 F 0.2676(3) 0.9600(3) 0.4326(4) 0.126(3) Uani 1 1 d . . . F3 F 0.3652(4) 0.9639(2) 0.4287(3) 0.096(2) Uani 1 1 d . . . F4 F 0.3278(4) 0.8971(2) 0.4471(3) 0.093(2) Uani 1 1 d . . . B2 B 0.3462(5) 0.7019(4) 0.9671(4) 0.055(3) Uani 1 1 d . . . F5 F 0.3862(3) 0.7247(2) 0.9429(2) 0.0773(18) Uani 1 1 d . . . F6 F 0.2887(3) 0.7116(2) 0.9454(3) 0.095(2) Uani 1 1 d . . . F7 F 0.3556(3) 0.7203(3) 1.0161(2) 0.104(3) Uani 1 1 d . . . F8 F 0.3570(4) 0.6563(2) 0.9680(3) 0.100(2) Uani 1 1 d . . . B3 B 0.3133(5) 0.1837(4) 0.9288(4) 0.056(3) Uiso 1 1 d D . . F9 F 0.2659(7) 0.2026(5) 0.8861(5) 0.095(5) Uiso 0.487(14) 1 d PD A 1 F10 F 0.3049(7) 0.2074(4) 0.9757(4) 0.090(5) Uiso 0.487(14) 1 d PD A 1 F11 F 0.3042(5) 0.1345(3) 0.9343(4) 0.055(4) Uiso 0.487(14) 1 d PD A 1 F12 F 0.3744(7) 0.1953(8) 0.9182(8) 0.178(11) Uiso 0.487(14) 1 d PD A 1 F9A F 0.3417(7) 0.2061(4) 0.9679(5) 0.076(4) Uiso 0.513(14) 1 d P A 2 F10A F 0.3015(7) 0.2045(4) 0.8847(5) 0.076(4) Uiso 0.513(14) 1 d P A 2 F11A F 0.2709(11) 0.1566(8) 0.9348(8) 0.151(8) Uiso 0.513(14) 1 d P A 2 F12A F 0.3581(11) 0.1520(9) 0.9229(9) 0.169(9) Uiso 0.513(14) 1 d P A 2 B4 B 0.1501(6) 0.9702(5) 0.9908(5) 0.102 Uiso 1 1 d D . . F13 F 0.1564(12) 0.9452(8) 1.0331(7) 0.260(14) Uiso 0.597(16) 1 d PD B 1 F14 F 0.2023(6) 0.9840(5) 0.9777(6) 0.130(6) Uiso 0.597(16) 1 d PD B 1 F15 F 0.1107(8) 1.0090(5) 0.9867(7) 0.171(8) Uiso 0.597(16) 1 d PD B 1 F16 F 0.1223(7) 0.9434(6) 0.9458(6) 0.158(8) Uiso 0.597(16) 1 d PD B 1 F13A F 0.2136(7) 0.9658(8) 1.0187(9) 0.145(10) Uiso 0.403(16) 1 d PD B 2 F14A F 0.1200(10) 0.9777(8) 1.0350(7) 0.149(11) Uiso 0.403(16) 1 d PD B 2 F15A F 0.1423(11) 1.0034(7) 0.9613(7) 0.142(10) Uiso 0.403(16) 1 d PD B 2 F16A F 0.1339(10) 0.9230(6) 0.9806(10) 0.155(11) Uiso 0.403(16) 1 d PD B 2 C129 C 0.5056(6) 0.8501(4) 0.0272(5) 0.093(4) Uani 1 1 d . . . H129 H 0.5368 0.8374 0.0548 0.112 Uiso 1 1 calc R . . Cl1 Cl 0.4550(2) 0.88752(15) 0.05199(14) 0.1160(13) Uani 1 1 d . . . Cl2 Cl 0.5416(2) 0.88477(14) -0.01618(16) 0.1146(13) Uani 1 1 d . . . Cl3 Cl 0.47037(18) 0.80510(15) -0.0092(2) 0.1399(19) Uani 1 1 d . . . C130 C 0.9908(8) 0.9750(6) 0.1241(7) 0.156(18) Uani 0.50 1 d PD . . H130 H 0.9617 0.9873 0.0948 0.187 Uiso 0.50 1 calc PR . . Cl4 Cl 1.0622(3) 0.9672(3) 0.1097(4) 0.128(3) Uani 0.50 1 d PD . . Cl5 Cl 1.0005(4) 1.0127(3) 0.1721(4) 0.163(5) Uani 0.50 1 d PD . . Cl6 Cl 0.9661(3) 0.9228(2) 0.1449(5) 0.166(5) Uani 0.50 1 d PD . . C131 C 0.0975(8) 0.8677(6) 0.2122(7) 0.131(6) Uani 1 1 d . . . H131 H 0.0742 0.8933 0.1926 0.157 Uiso 1 1 calc R . . Cl7 Cl 0.0575(2) 0.8488(2) 0.25813(18) 0.1503(19) Uani 1 1 d . . . Cl8 Cl 0.1653(4) 0.8882(3) 0.2375(4) 0.287(6) Uani 1 1 d . . . Cl9 Cl 0.1066(2) 0.82362(15) 0.17203(16) 0.1195(13) Uani 1 1 d . . . C132 C 0.4796(6) 0.9281(5) 0.5202(5) 0.095(4) Uani 1 1 d . . . H132 H 0.4425 0.9456 0.5047 0.114 Uiso 1 1 calc R . . Cl10 Cl 0.4622(3) 0.8741(2) 0.5387(5) 0.339(7) Uani 1 1 d . . . Cl11 Cl 0.5172(4) 0.9564(4) 0.5709(4) 0.300(5) Uani 1 1 d . . . Cl12 Cl 0.5300(4) 0.9270(4) 0.4822(3) 0.318(7) Uani 1 1 d . . . C133 C 0.0023(9) 0.8008(6) 0.5639(7) 0.156(19) Uani 0.50 1 d PD . . H133 H -0.0353 0.7872 0.5438 0.187 Uiso 0.50 1 calc PR . . Cl13 Cl 0.0260(3) 0.7600(3) 0.6060(3) 0.110(2) Uani 0.50 1 d PD . . Cl14 Cl -0.0202(3) 0.8433(3) 0.5894(2) 0.102(2) Uani 0.50 1 d PD . . Cl15 Cl 0.0482(2) 0.80615(17) 0.5225(2) 0.0659(14) Uani 0.50 1 d PD . . C134 C 0.4435(6) 0.6688(4) 0.8627(5) 0.090(4) Uani 1 1 d . . . H134 H 0.4250 0.6802 0.8910 0.108 Uiso 1 1 calc R . . Cl16 Cl 0.4172(2) 0.61339(16) 0.84701(19) 0.1360(16) Uani 1 1 d . . . Cl17 Cl 0.5233(2) 0.66610(18) 0.8828(2) 0.1441(17) Uani 1 1 d . . . Cl18 Cl 0.4260(3) 0.70699(19) 0.81389(19) 0.168(2) Uani 1 1 d . . . C135 C 0.6067(6) 0.0941(4) 0.6622(5) 0.091(4) Uani 1 1 d . . . H135 H 0.6122 0.0836 0.6284 0.109 Uiso 1 1 calc R . . Cl19 Cl 0.59023(19) 0.04671(13) 0.69661(19) 0.1254(17) Uani 1 1 d . . . Cl20 Cl 0.54891(16) 0.13582(13) 0.65656(14) 0.0974(11) Uani 1 1 d . . . Cl21 Cl 0.67413(19) 0.12105(16) 0.69439(18) 0.1282(15) Uani 1 1 d . . . C136 C 0.3833(6) 0.1530(4) 0.8130(5) 0.087(4) Uani 1 1 d . . . H136 H 0.3714 0.1675 0.8430 0.105 Uiso 1 1 calc R . . Cl22 Cl 0.4062(2) 0.19625(17) 0.7785(2) 0.152(2) Uani 1 1 d . . . Cl23 Cl 0.4455(2) 0.11549(17) 0.83376(17) 0.1350(16) Uani 1 1 d . . . Cl24 Cl 0.32374(19) 0.12253(15) 0.78244(19) 0.1281(16) Uani 1 1 d . . . O9 O 0.0267(7) 0.1174(5) 0.4877(7) 0.096(6) Uani 0.50 1 d P . . O10 O 0.2734(4) 0.1341(3) 0.6014(4) 0.127(4) Uani 1 1 d . . . C138 C 0.2271(10) -0.1128(11) 1.1244(11) 0.150(5) Uani 1 1 d . . . H13A H 0.1848 -0.1121 1.1076 0.225 Uiso 1 1 calc R . . H13B H 0.2337 -0.0896 1.1513 0.225 Uiso 1 1 calc R . . H13C H 0.2371 -0.1439 1.1384 0.225 Uiso 1 1 calc R . . O11 O 0.2647(7) -0.1023(5) 1.0893(5) 0.150(5) Uani 1 1 d . . . H11L H 0.2607 -0.1231 1.0673 0.225 Uiso 1 1 calc R . . O12 O 0.2178(8) 0.8514(5) 0.4000(4) 0.092(6) Uani 0.50 1 d P . . _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 0.0601(4) 0.0738(5) 0.0240(3) -0.0104(3) 0.0105(3) 0.0121(4) Ag2 0.0630(4) 0.0566(4) 0.0303(3) 0.0140(3) 0.0117(3) 0.0029(3) Ag3 0.0629(5) 0.0674(5) 0.0341(3) -0.0210(3) 0.0107(3) -0.0129(4) Ag4 0.0750(5) 0.0711(5) 0.0254(3) 0.0115(3) 0.0126(3) -0.0129(4) S1 0.0296(9) 0.0426(11) 0.0327(9) 0.0147(9) 0.0012(7) 0.0004(8) C1 0.034(4) 0.025(4) 0.019(3) -0.005(3) 0.004(3) -0.001(3) C2 0.028(4) 0.030(4) 0.023(3) 0.000(3) 0.005(3) -0.008(3) C3 0.029(4) 0.034(4) 0.030(4) -0.004(3) 0.011(3) -0.004(3) C4 0.035(4) 0.026(4) 0.035(4) 0.002(3) 0.015(3) 0.003(3) C5 0.032(4) 0.031(4) 0.028(3) 0.007(3) 0.007(3) -0.001(3) C6 0.027(3) 0.028(4) 0.029(3) 0.000(3) 0.008(3) -0.004(3) O1 0.036(3) 0.034(3) 0.022(2) 0.002(2) 0.011(2) -0.008(2) C7 0.037(4) 0.049(5) 0.029(4) -0.008(4) 0.010(3) -0.021(4) C8 0.031(4) 0.038(4) 0.023(3) 0.001(3) 0.009(3) 0.004(3) C9 0.038(4) 0.050(5) 0.032(4) -0.012(4) 0.011(3) 0.002(4) N1 0.055(4) 0.061(5) 0.020(3) 0.003(3) 0.020(3) 0.012(4) C10 0.049(5) 0.044(5) 0.031(4) 0.003(4) 0.017(4) -0.001(4) C11 0.047(5) 0.045(5) 0.034(4) -0.001(4) 0.015(4) -0.010(4) C12 0.043(4) 0.039(4) 0.026(3) -0.007(3) 0.015(3) -0.009(4) C13 0.040(4) 0.038(5) 0.049(5) 0.013(4) 0.020(4) -0.003(4) C14 0.105(10) 0.128(11) 0.066(7) 0.022(8) 0.058(7) 0.017(9) C15 0.081(9) 0.27(2) 0.153(14) 0.171(15) 0.084(10) 0.076(12) C16 0.057(7) 0.171(14) 0.095(9) 0.070(10) 0.023(7) -0.008(8) S2 0.0363(10) 0.0236(10) 0.0641(13) -0.0024(9) 0.0259(9) 0.0010(8) C17 0.028(3) 0.020(4) 0.039(4) -0.001(3) 0.011(3) 0.002(3) C18 0.033(4) 0.033(4) 0.021(3) 0.001(3) 0.007(3) 0.012(3) C19 0.029(3) 0.030(4) 0.023(3) -0.001(3) 0.007(3) 0.005(3) C20 0.029(4) 0.037(4) 0.035(4) -0.008(3) 0.013(3) 0.001(3) C21 0.027(3) 0.031(4) 0.027(3) -0.003(3) 0.010(3) -0.001(3) C22 0.034(4) 0.035(4) 0.032(4) -0.008(3) 0.007(3) -0.002(3) O2 0.038(3) 0.034(3) 0.027(2) -0.002(2) 0.017(2) 0.007(2) C23 0.047(5) 0.043(5) 0.024(3) 0.007(3) 0.015(3) 0.016(4) C24 0.043(4) 0.021(4) 0.035(4) 0.000(3) 0.017(3) -0.002(3) C25 0.049(5) 0.037(4) 0.030(4) 0.004(3) 0.013(3) 0.005(4) N2 0.055(4) 0.038(4) 0.032(3) 0.007(3) 0.014(3) 0.009(3) C26 0.060(6) 0.056(5) 0.033(4) -0.008(4) 0.033(4) 0.000(4) C27 0.043(5) 0.059(6) 0.032(4) -0.010(4) 0.014(3) 0.002(4) C28 0.049(5) 0.047(5) 0.027(4) 0.001(4) 0.015(3) 0.011(4) C29 0.037(4) 0.043(5) 0.042(4) -0.019(4) 0.020(3) -0.002(4) C30 0.143(12) 0.101(9) 0.110(10) -0.052(8) 0.110(10) -0.052(9) C31 0.172(16) 0.214(18) 0.073(8) 0.028(10) 0.050(9) 0.159(15) C32 0.070(8) 0.161(13) 0.051(6) -0.046(7) 0.024(5) -0.020(8) S3 0.0283(9) 0.0388(11) 0.0260(8) -0.0101(8) 0.0036(7) 0.0008(8) C33 0.035(4) 0.018(3) 0.024(3) -0.001(3) -0.004(3) -0.004(3) C34 0.031(4) 0.037(4) 0.022(3) 0.000(3) 0.003(3) -0.007(3) C35 0.032(4) 0.025(4) 0.035(4) -0.003(3) 0.002(3) 0.000(3) C36 0.036(4) 0.033(4) 0.031(4) -0.003(3) 0.005(3) 0.003(3) C37 0.036(4) 0.041(4) 0.023(3) -0.003(3) 0.005(3) -0.001(3) C38 0.037(4) 0.034(4) 0.019(3) -0.003(3) 0.003(3) -0.001(3) O3 0.044(3) 0.038(3) 0.017(2) 0.001(2) -0.001(2) 0.003(2) C39 0.038(4) 0.053(5) 0.030(4) 0.000(4) 0.001(3) -0.002(4) C40 0.036(4) 0.035(4) 0.038(4) 0.006(4) 0.001(3) 0.000(3) C41 0.047(5) 0.057(5) 0.023(4) 0.010(4) 0.007(3) 0.004(4) N3 0.057(5) 0.049(4) 0.034(3) 0.009(3) 0.013(3) 0.003(4) C42 0.056(5) 0.057(6) 0.031(4) 0.008(4) 0.012(4) 0.011(4) C43 0.051(5) 0.061(6) 0.058(6) 0.011(5) 0.025(5) 0.014(5) C44 0.058(6) 0.054(6) 0.038(4) 0.011(4) -0.001(4) 0.009(5) C45 0.054(5) 0.034(4) 0.024(3) -0.010(3) 0.005(3) 0.008(4) C46 0.084(6) 0.069(6) 0.026(3) -0.010(4) 0.009(4) -0.003(5) C47 0.084(6) 0.069(6) 0.026(3) -0.010(4) 0.009(4) -0.003(5) C48 0.084(6) 0.069(6) 0.026(3) -0.010(4) 0.009(4) -0.003(5) C46A 0.084(6) 0.069(6) 0.026(3) -0.010(4) 0.009(4) -0.003(5) C47A 0.084(6) 0.069(6) 0.026(3) -0.010(4) 0.009(4) -0.003(5) C48A 0.084(6) 0.069(6) 0.026(3) -0.010(4) 0.009(4) -0.003(5) S4 0.0434(11) 0.0278(10) 0.0448(11) 0.0005(9) -0.0047(9) 0.0054(8) C49 0.036(4) 0.017(4) 0.037(4) 0.005(3) 0.004(3) 0.005(3) C50 0.035(4) 0.039(4) 0.015(3) 0.009(3) 0.003(3) 0.012(3) C51 0.030(4) 0.037(4) 0.026(3) 0.010(3) 0.007(3) 0.005(3) C52 0.031(4) 0.049(5) 0.024(3) 0.008(3) 0.004(3) 0.002(3) C53 0.037(4) 0.040(5) 0.027(4) 0.012(3) 0.009(3) 0.012(3) C54 0.036(4) 0.040(5) 0.038(4) 0.013(4) 0.004(3) -0.002(3) O4 0.044(3) 0.046(3) 0.015(2) 0.006(2) -0.005(2) 0.001(2) C55 0.050(5) 0.090(7) 0.024(4) 0.010(5) 0.013(4) 0.005(5) C56 0.056(5) 0.064(6) 0.028(4) -0.004(4) 0.015(4) 0.012(5) C57 0.059(6) 0.072(7) 0.030(4) -0.007(4) 0.012(4) 0.026(5) N4 0.083(6) 0.069(5) 0.025(3) -0.010(4) 0.013(4) 0.022(5) C58 0.088(8) 0.071(7) 0.041(5) -0.018(5) 0.000(5) 0.030(6) C59 0.092(8) 0.078(8) 0.050(6) 0.006(6) 0.012(6) 0.049(7) C60 0.058(6) 0.101(9) 0.027(4) -0.004(5) -0.003(4) 0.046(6) C61 0.044(5) 0.052(5) 0.025(4) 0.018(4) 0.010(3) 0.009(4) C62 0.083(15) 0.083(14) 0.051(9) 0.034(9) -0.002(9) -0.019(11) C63 0.083(15) 0.083(14) 0.051(9) 0.034(9) -0.002(9) -0.019(11) C64 0.083(15) 0.083(14) 0.051(9) 0.034(9) -0.002(9) -0.019(11) C62A 0.11(4) 0.14(4) 0.06(2) 0.05(2) 0.02(2) 0.04(3) C63A 0.12(3) 0.10(3) 0.014(10) 0.022(14) 0.004(14) -0.04(3) C64A 0.053(16) 0.10(3) 0.048(15) 0.036(18) 0.017(12) 0.027(17) S5 0.0360(10) 0.0243(10) 0.0406(10) 0.0000(8) -0.0076(8) 0.0005(8) C65 0.028(4) 0.035(4) 0.031(4) -0.005(3) -0.004(3) -0.001(3) C66 0.028(3) 0.021(3) 0.025(3) -0.005(3) 0.005(3) 0.004(3) C67 0.030(4) 0.033(4) 0.018(3) -0.006(3) 0.000(3) 0.000(3) C68 0.026(3) 0.035(4) 0.024(3) -0.008(3) 0.001(3) 0.005(3) C69 0.024(3) 0.039(4) 0.030(4) -0.016(3) -0.002(3) 0.003(3) C70 0.033(4) 0.025(4) 0.035(4) -0.009(3) -0.001(3) 0.003(3) O5 0.036(3) 0.035(3) 0.019(2) -0.001(2) -0.0007(19) 0.002(2) C71 0.045(4) 0.040(5) 0.025(3) 0.003(3) 0.006(3) 0.004(4) C72 0.040(4) 0.052(5) 0.028(4) -0.006(4) 0.006(3) -0.001(4) C73 0.045(5) 0.046(5) 0.024(3) -0.001(4) 0.003(3) 0.011(4) N5 0.044(4) 0.045(4) 0.035(3) 0.006(3) 0.006(3) 0.002(3) C74 0.058(6) 0.050(6) 0.043(5) 0.006(4) 0.004(4) -0.013(5) C75 0.065(6) 0.040(6) 0.071(7) -0.006(5) 0.001(5) -0.018(5) C76 0.041(5) 0.070(7) 0.054(5) -0.005(5) -0.008(4) -0.009(5) C77 0.034(4) 0.043(5) 0.028(4) -0.014(3) 0.001(3) 0.005(3) C78 0.037(5) 0.174(13) 0.053(6) -0.069(7) 0.003(4) -0.013(7) C79 0.037(5) 0.174(13) 0.053(6) -0.069(7) 0.003(4) -0.013(7) C80 0.037(5) 0.174(13) 0.053(6) -0.069(7) 0.003(4) -0.013(7) S6 0.0260(8) 0.0299(10) 0.0254(8) -0.0093(7) -0.0014(6) 0.0038(7) C81 0.028(3) 0.018(3) 0.021(3) 0.001(3) 0.005(3) 0.009(3) C82 0.031(3) 0.017(3) 0.021(3) 0.004(3) 0.006(3) 0.006(3) C83 0.030(4) 0.021(4) 0.033(4) 0.005(3) 0.012(3) 0.000(3) C84 0.033(4) 0.028(4) 0.030(4) -0.004(3) 0.007(3) -0.004(3) C85 0.030(4) 0.028(4) 0.027(3) -0.002(3) 0.010(3) 0.003(3) C86 0.030(4) 0.024(4) 0.024(3) -0.009(3) 0.005(3) 0.000(3) O6 0.038(3) 0.033(3) 0.023(2) 0.005(2) 0.016(2) 0.008(2) C87 0.045(5) 0.050(5) 0.027(4) 0.015(4) 0.011(3) 0.021(4) C88 0.044(4) 0.039(4) 0.024(3) 0.008(3) 0.009(3) -0.002(4) C89 0.045(5) 0.037(5) 0.036(4) 0.000(4) 0.006(4) 0.001(4) N6 0.048(4) 0.051(4) 0.024(3) 0.003(3) 0.014(3) 0.000(3) C90 0.054(5) 0.052(5) 0.038(4) 0.005(4) 0.024(4) 0.002(4) C91 0.041(5) 0.062(6) 0.035(4) -0.006(4) 0.008(3) 0.017(4) C92 0.039(4) 0.049(5) 0.026(3) 0.005(4) 0.006(3) 0.013(4) C93 0.050(5) 0.047(5) 0.028(4) -0.017(4) 0.010(3) -0.005(4) C94 0.050(5) 0.047(5) 0.028(4) -0.017(4) 0.010(3) -0.005(4) C95 0.050(5) 0.047(5) 0.028(4) -0.017(4) 0.010(3) -0.005(4) C96 0.050(5) 0.047(5) 0.028(4) -0.017(4) 0.010(3) -0.005(4) S7 0.0396(11) 0.0277(10) 0.0623(13) 0.0064(10) 0.0222(10) -0.0037(8) C97 0.030(4) 0.041(5) 0.034(4) 0.003(3) 0.013(3) -0.016(3) C98 0.031(4) 0.028(4) 0.027(3) 0.004(3) 0.005(3) -0.005(3) C99 0.028(4) 0.040(4) 0.027(3) 0.006(3) 0.005(3) -0.008(3) C100 0.025(4) 0.047(5) 0.029(4) 0.012(3) 0.006(3) -0.004(3) C101 0.021(3) 0.056(5) 0.032(4) 0.021(4) 0.003(3) 0.001(3) C102 0.029(4) 0.039(4) 0.035(4) 0.015(3) 0.007(3) 0.001(3) O7 0.027(2) 0.029(3) 0.030(2) 0.002(2) 0.011(2) -0.006(2) C103 0.044(5) 0.049(5) 0.029(4) 0.000(4) 0.014(3) -0.010(4) C104 0.032(4) 0.034(4) 0.028(3) -0.005(3) 0.009(3) -0.003(3) C105 0.050(5) 0.035(4) 0.031(4) -0.013(3) 0.013(3) -0.012(4) N7 0.069(5) 0.053(5) 0.026(3) -0.013(3) 0.015(3) -0.008(4) C106 0.058(5) 0.041(5) 0.031(4) -0.002(4) 0.022(4) -0.008(4) C107 0.056(5) 0.053(5) 0.032(4) -0.003(4) 0.020(4) -0.023(4) C108 0.047(5) 0.041(5) 0.028(4) -0.013(3) 0.008(3) -0.019(4) C109 0.050(5) 0.065(6) 0.030(4) 0.023(4) 0.011(4) 0.006(4) C110 0.042(5) 0.102(9) 0.079(7) 0.031(6) 0.036(5) -0.007(5) C111 0.105(10) 0.160(13) 0.087(9) 0.091(9) 0.064(8) 0.064(10) C112 0.046(5) 0.120(9) 0.041(5) -0.005(6) 0.023(4) -0.018(6) S8 0.0279(9) 0.0448(11) 0.0316(9) 0.0153(9) 0.0063(7) -0.0004(8) C113 0.024(3) 0.037(4) 0.023(3) 0.005(3) 0.001(3) 0.002(3) C114 0.025(3) 0.033(4) 0.021(3) 0.002(3) 0.001(3) 0.010(3) C115 0.028(3) 0.022(4) 0.028(3) 0.006(3) 0.001(3) 0.000(3) C116 0.034(4) 0.030(4) 0.030(4) 0.006(3) 0.005(3) -0.004(3) C117 0.035(4) 0.032(4) 0.025(3) 0.005(3) 0.009(3) -0.003(3) C118 0.026(3) 0.033(4) 0.020(3) 0.006(3) 0.001(3) -0.005(3) O8 0.042(3) 0.040(3) 0.020(2) 0.006(2) -0.003(2) 0.006(2) C119 0.053(5) 0.071(6) 0.026(4) -0.006(4) 0.014(4) 0.008(5) C120 0.051(5) 0.051(5) 0.023(3) 0.003(4) 0.008(3) 0.010(4) C121 0.046(5) 0.062(6) 0.021(3) -0.003(4) 0.009(3) 0.010(4) N8 0.054(4) 0.059(5) 0.028(3) -0.003(3) 0.009(3) 0.015(4) C122 0.078(7) 0.049(6) 0.039(5) -0.008(4) 0.018(4) 0.018(5) C123 0.094(8) 0.060(6) 0.032(4) 0.003(5) 0.007(5) 0.018(6) C124 0.095(8) 0.058(6) 0.024(4) 0.004(4) 0.009(4) 0.024(6) C125 0.036(4) 0.043(5) 0.024(3) 0.006(3) 0.003(3) -0.003(3) C126 0.115(10) 0.162(13) 0.036(5) 0.050(7) 0.026(6) 0.079(10) C127 0.067(7) 0.164(12) 0.031(5) 0.028(6) 0.022(5) -0.020(7) C128 0.213(18) 0.091(9) 0.022(5) -0.005(5) -0.008(7) -0.048(10) B1 0.068(8) 0.038(6) 0.073(8) -0.009(6) 0.029(6) -0.006(5) F1 0.105(6) 0.097(5) 0.082(5) -0.024(4) 0.031(4) 0.010(4) F2 0.071(5) 0.107(6) 0.190(9) -0.035(6) 0.005(5) 0.014(4) F3 0.128(6) 0.057(4) 0.128(6) 0.006(4) 0.085(5) -0.008(4) F4 0.143(7) 0.051(4) 0.098(5) 0.003(4) 0.057(5) -0.003(4) B2 0.052(7) 0.054(7) 0.061(7) -0.010(6) 0.014(5) -0.008(5) F5 0.085(4) 0.059(4) 0.101(5) 0.010(3) 0.052(4) -0.004(3) F6 0.057(4) 0.093(5) 0.128(6) -0.034(4) -0.002(4) -0.012(3) F7 0.086(5) 0.169(8) 0.060(4) -0.035(4) 0.022(4) 0.006(5) F8 0.119(6) 0.059(4) 0.133(6) 0.013(4) 0.052(5) -0.002(4) C129 0.075(8) 0.066(8) 0.124(11) 0.026(8) -0.023(8) -0.013(6) Cl1 0.139(3) 0.129(3) 0.090(2) -0.020(2) 0.046(2) -0.035(3) Cl2 0.132(3) 0.092(2) 0.128(3) -0.007(2) 0.046(3) 0.010(2) Cl3 0.080(2) 0.102(3) 0.226(5) -0.048(3) -0.003(3) -0.015(2) C130 0.047(14) 0.29(5) 0.12(2) 0.10(3) -0.005(15) -0.08(2) Cl4 0.082(4) 0.102(5) 0.225(9) -0.072(6) 0.094(6) -0.062(4) Cl5 0.162(8) 0.201(9) 0.154(7) -0.107(7) 0.103(7) -0.133(8) Cl6 0.042(3) 0.070(4) 0.395(16) 0.064(7) 0.064(6) -0.001(3) C131 0.140(15) 0.122(13) 0.139(14) -0.005(12) 0.049(12) -0.027(12) Cl7 0.118(4) 0.207(5) 0.136(4) -0.036(4) 0.050(3) -0.028(4) Cl8 0.207(7) 0.308(10) 0.387(12) -0.226(9) 0.156(8) -0.167(7) Cl9 0.136(4) 0.116(3) 0.110(3) -0.006(2) 0.034(3) -0.013(3) C132 0.061(7) 0.101(10) 0.115(11) 0.032(9) -0.006(7) 0.003(7) Cl10 0.147(6) 0.136(5) 0.70(2) 0.195(9) 0.004(9) -0.017(4) Cl11 0.160(6) 0.402(14) 0.285(10) -0.041(10) -0.099(7) 0.043(8) Cl12 0.238(8) 0.546(17) 0.194(7) 0.150(9) 0.096(6) 0.242(10) C133 0.042(13) 0.042(13) 0.35(5) 0.02(2) -0.06(2) 0.009(11) Cl13 0.080(5) 0.133(6) 0.102(5) 0.001(5) -0.026(4) -0.009(4) Cl14 0.082(4) 0.134(6) 0.093(4) -0.079(4) 0.028(3) -0.043(4) Cl15 0.049(3) 0.050(3) 0.105(4) -0.013(3) 0.031(3) -0.012(2) C134 0.117(11) 0.080(9) 0.074(8) -0.004(7) 0.024(7) 0.026(8) Cl16 0.128(4) 0.112(3) 0.166(4) -0.046(3) 0.022(3) -0.007(3) Cl17 0.125(4) 0.139(4) 0.154(4) 0.010(3) -0.011(3) -0.003(3) Cl18 0.222(6) 0.151(4) 0.139(4) 0.059(3) 0.053(4) 0.107(4) C135 0.112(11) 0.061(7) 0.121(11) 0.014(7) 0.076(9) 0.007(7) Cl19 0.112(3) 0.093(2) 0.193(4) 0.068(3) 0.086(3) 0.040(2) Cl20 0.091(2) 0.098(2) 0.105(2) 0.029(2) 0.0219(19) 0.0313(19) Cl21 0.096(3) 0.122(3) 0.155(4) -0.004(3) -0.003(3) 0.011(2) C136 0.102(10) 0.078(8) 0.084(8) 0.007(7) 0.025(7) 0.006(7) Cl22 0.136(4) 0.127(3) 0.216(5) 0.084(4) 0.092(4) 0.042(3) Cl23 0.120(3) 0.148(4) 0.124(3) 0.040(3) -0.009(3) 0.038(3) Cl24 0.099(3) 0.110(3) 0.164(4) -0.047(3) -0.005(3) 0.003(2) O9 0.068(10) 0.045(8) 0.163(17) -0.035(10) -0.012(10) 0.012(7) O10 0.109(7) 0.067(5) 0.166(9) -0.030(6) -0.077(7) 0.051(5) C138 0.162(11) 0.143(10) 0.154(11) -0.075(9) 0.055(9) -0.056(9) O11 0.162(11) 0.143(10) 0.154(11) -0.075(9) 0.055(9) -0.056(9) O12 0.161(15) 0.080(10) 0.036(6) -0.021(7) 0.019(8) -0.026(11) _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. ; _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 N1 2.135(6) . ? Ag1 N8 2.143(6) 1_554 ? Ag2 N2 2.116(6) . ? Ag2 N5 2.144(6) . ? Ag3 N3 2.118(7) 2_545 ? Ag3 N7 2.135(6) . ? Ag4 N6 2.121(6) . ? Ag4 N4 2.143(7) 2_546 ? S1 C51 1.761(7) . ? S1 C1 1.761(7) . ? C1 C2 1.391(9) . ? C1 C6 1.400(9) . ? C2 O1 1.376(7) . ? C2 C3 1.394(10) . ? C3 C4 1.408(9) . ? C3 S2 1.771(7) . ? C4 C5 1.367(10) . ? C5 C6 1.378(10) . ? C5 C13 1.556(10) . ? O1 C7 1.417(8) . ? C7 C8 1.500(9) . ? C8 C9 1.366(9) . ? C8 C12 1.393(10) . ? C9 N1 1.354(10) . ? N1 C10 1.338(11) . ? C10 C11 1.352(10) . ? C11 C12 1.377(10) . ? C13 C16 1.473(14) . ? C13 C15 1.494(14) . ? C13 C14 1.615(15) . ? S2 C17 1.781(7) . ? C17 C18 1.356(10) . ? C17 C22 1.383(9) . ? C18 O2 1.396(8) . ? C18 C19 1.412(10) . ? C19 C20 1.395(9) . ? C19 S3 1.774(7) . ? C20 C21 1.369(10) . ? C21 C22 1.375(10) . ? C21 C29 1.546(9) . ? O2 C23 1.445(8) . ? C23 C24 1.492(9) . ? C24 C25 1.369(10) . ? C24 C28 1.375(11) . ? C25 N2 1.342(9) . ? N2 C26 1.317(11) . ? C26 C27 1.402(11) . ? C27 C28 1.394(10) . ? C29 C31 1.455(14) . ? C29 C32 1.456(13) . ? C29 C30 1.547(13) . ? S3 C33 1.770(7) . ? C33 C34 1.378(10) . ? C33 C38 1.397(9) . ? C34 O3 1.399(8) . ? C34 C35 1.405(10) . ? C35 C36 1.395(10) . ? C35 S4 1.784(7) . ? C36 C37 1.403(10) . ? C37 C38 1.391(10) . ? C37 C45 1.510(9) . ? O3 C39 1.465(9) . ? C39 C40 1.476(10) . ? C40 C44 1.382(12) . ? C40 C41 1.392(10) . ? C41 N3 1.361(9) . ? N3 C42 1.323(11) . ? N3 Ag3 2.118(7) 2 ? C42 C43 1.355(12) . ? C43 C44 1.408(12) . ? C45 C47 1.526(14) . ? C45 C48A 1.532(12) . ? C45 C47A 1.530(12) . ? C45 C48 1.533(14) . ? C45 C46 1.545(14) . ? C45 C46A 1.562(13) . ? S4 C49 1.776(8) . ? C49 C54 1.394(10) . ? C49 C50 1.421(10) . ? C50 O4 1.370(7) . ? C50 C51 1.379(10) . ? C51 C52 1.405(9) . ? C52 C53 1.423(11) . ? C53 C54 1.363(11) . ? C53 C61 1.552(9) . ? O4 C55 1.446(10) . ? C55 C56 1.484(13) . ? C56 C60 1.357(13) . ? C56 C57 1.400(12) . ? C57 N4 1.312(12) . ? N4 C58 1.341(13) . ? N4 Ag4 2.144(7) 2_556 ? C58 C59 1.377(14) . ? C59 C60 1.371(15) . ? C61 C62 1.484(12) . ? C61 C64A 1.509(14) . ? C61 C63 1.535(12) . ? C61 C62A 1.561(15) . ? C61 C63A 1.583(15) . ? C61 C64 1.585(12) . ? S5 C115 1.776(7) . ? S5 C65 1.782(7) . ? C65 C70 1.383(10) . ? C65 C66 1.401(10) . ? C66 O5 1.374(8) . ? C66 C67 1.383(9) . ? C67 C68 1.387(9) . ? C67 S6 1.779(7) . ? C68 C69 1.371(9) . ? C69 C70 1.389(10) . ? C69 C77 1.524(9) . ? O5 C71 1.448(9) . ? C71 C72 1.492(11) . ? C72 C73 1.384(10) . ? C72 C76 1.391(12) . ? C73 N5 1.299(10) . ? N5 C74 1.352(11) . ? C74 C75 1.359(13) . ? C75 C76 1.389(13) . ? C77 C79 1.459(14) . ? C77 C80 1.491(16) . ? C77 C78 1.499(11) . ? S6 C81 1.778(7) . ? C81 C86 1.389(8) . ? C81 C82 1.399(9) . ? C82 C83 1.372(10) . ? C82 O6 1.387(7) . ? C83 C84 1.396(9) . ? C83 S7 1.770(7) . ? C84 C85 1.387(9) . ? C85 C86 1.396(9) . ? C85 C93 1.542(9) . ? O6 C87 1.438(8) . ? C87 C88 1.489(10) . ? C88 C89 1.381(10) . ? C88 C92 1.392(11) . ? C89 N6 1.370(10) . ? N6 C90 1.320(11) . ? C90 C91 1.396(11) . ? C91 C92 1.369(10) . ? C93 C95 1.493(14) . ? C93 C94 1.507(15) . ? C93 C96 1.530(16) . ? S7 C97 1.798(8) . ? C97 C98 1.349(10) . ? C97 C102 1.399(9) . ? C98 O7 1.378(8) . ? C98 C99 1.395(10) . ? C99 C100 1.408(9) . ? C99 S8 1.771(7) . ? C100 C101 1.405(10) . ? C101 C102 1.341(10) . ? C101 C109 1.549(10) . ? O7 C103 1.430(9) . ? C103 C104 1.513(10) . ? C104 C105 1.377(10) . ? C104 C108 1.382(10) . ? C105 N7 1.342(10) . ? N7 C106 1.315(10) . ? C106 C107 1.393(11) . ? C107 C108 1.372(10) . ? C109 C111 1.489(13) . ? C109 C110 1.520(13) . ? C109 C112 1.542(14) . ? S8 C113 1.784(7) . ? C113 C114 1.384(10) . ? C113 C118 1.387(9) . ? C114 C115 1.381(9) . ? C114 O8 1.387(8) . ? C115 C116 1.402(9) . ? C116 C117 1.402(10) . ? C117 C118 1.394(9) . ? C117 C125 1.532(9) . ? O8 C119 1.444(9) . ? C119 C120 1.477(12) . ? C120 C124 1.375(11) . ? C120 C121 1.422(10) . ? C121 N8 1.306(11) . ? N8 C122 1.378(11) . ? N8 Ag1 2.143(6) 1_556 ? C122 C123 1.372(12) . ? C123 C124 1.398(14) . ? C125 C126 1.453(13) . ? C125 C128 1.497(13) . ? C125 C127 1.536(12) . ? B1 F4 1.345(12) . ? B1 F1 1.352(14) . ? B1 F2 1.363(15) . ? B1 F3 1.400(13) . ? B2 F8 1.328(13) . ? B2 F6 1.355(13) . ? B2 F5 1.382(12) . ? B2 F7 1.414(13) . ? B3 F11A 1.27(2) . ? B3 F9A 1.308(16) . ? B3 F10A 1.325(16) . ? B3 F12A 1.39(2) . ? B3 F11 1.439(12) . ? B3 F10 1.494(13) . ? B3 F12 1.501(13) . ? B3 F9 1.526(13) . ? B4 F15A 1.237(14) . ? B4 F13 1.344(14) . ? B4 F14 1.353(14) . ? B4 F16A 1.417(15) . ? B4 F15 1.417(14) . ? B4 F16 1.487(14) . ? B4 F13A 1.499(15) . ? B4 F14A 1.508(15) . ? C129 Cl3 1.728(13) . ? C129 Cl1 1.790(15) . ? C129 Cl2 1.847(14) . ? C130 Cl5 1.682(17) . ? C130 Cl6 1.730(16) . ? C130 Cl4 1.745(16) . ? C131 Cl8 1.667(18) . ? C131 Cl9 1.710(17) . ? C131 Cl7 1.763(16) . ? C132 Cl12 1.678(15) . ? C132 Cl11 1.690(16) . ? C132 Cl10 1.697(14) . ? C133 Cl14 1.537(15) . ? C133 Cl13 1.657(15) . ? C133 Cl15 1.677(16) . ? C134 Cl18 1.713(13) . ? C134 Cl16 1.721(13) . ? C134 Cl17 1.787(15) . ? C135 Cl19 1.731(11) . ? C135 Cl20 1.758(12) . ? C135 Cl21 1.787(15) . ? C136 Cl24 1.689(14) . ? C136 Cl22 1.695(13) . ? C136 Cl23 1.778(13) . ? C138 O11 1.43(2) . ? _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 N1 Ag1 N8 178.4(3) . 1_554 ? N2 Ag2 N5 172.4(3) . . ? N3 Ag3 N7 165.4(3) 2_545 . ? N6 Ag4 N4 173.4(3) . 2_546 ? C51 S1 C1 107.9(3) . . ? C2 C1 C6 118.9(6) . . ? C2 C1 S1 122.0(5) . . ? C6 C1 S1 118.1(5) . . ? O1 C2 C1 121.0(6) . . ? O1 C2 C3 119.8(6) . . ? C1 C2 C3 119.2(6) . . ? C2 C3 C4 119.8(6) . . ? C2 C3 S2 124.6(5) . . ? C4 C3 S2 115.1(6) . . ? C5 C4 C3 121.5(7) . . ? C4 C5 C6 117.8(6) . . ? C4 C5 C13 122.8(6) . . ? C6 C5 C13 119.4(6) . . ? C5 C6 C1 122.6(6) . . ? C2 O1 C7 115.0(5) . . ? O1 C7 C8 108.7(6) . . ? C9 C8 C12 117.5(7) . . ? C9 C8 C7 119.9(7) . . ? C12 C8 C7 122.6(6) . . ? N1 C9 C8 123.7(8) . . ? C10 N1 C9 117.7(6) . . ? C10 N1 Ag1 120.5(5) . . ? C9 N1 Ag1 121.8(6) . . ? N1 C10 C11 121.9(7) . . ? C10 C11 C12 120.6(8) . . ? C11 C12 C8 118.6(7) . . ? C16 C13 C15 115.9(10) . . ? C16 C13 C5 110.7(7) . . ? C15 C13 C5 112.6(7) . . ? C16 C13 C14 102.0(9) . . ? C15 C13 C14 106.6(10) . . ? C5 C13 C14 108.0(7) . . ? C3 S2 C17 108.5(3) . . ? C18 C17 C22 120.7(6) . . ? C18 C17 S2 123.0(5) . . ? C22 C17 S2 115.3(5) . . ? C17 C18 O2 121.6(6) . . ? C17 C18 C19 119.6(6) . . ? O2 C18 C19 118.7(6) . . ? C20 C19 C18 118.0(6) . . ? C20 C19 S3 117.2(5) . . ? C18 C19 S3 123.9(5) . . ? C21 C20 C19 122.3(7) . . ? C20 C21 C22 118.0(6) . . ? C20 C21 C29 122.8(6) . . ? C22 C21 C29 119.2(6) . . ? C21 C22 C17 121.4(7) . . ? C18 O2 C23 113.5(5) . . ? O2 C23 C24 108.1(6) . . ? C25 C24 C28 118.8(7) . . ? C25 C24 C23 117.5(7) . . ? C28 C24 C23 123.7(7) . . ? N2 C25 C24 123.7(7) . . ? C26 N2 C25 118.0(7) . . ? C26 N2 Ag2 122.6(5) . . ? C25 N2 Ag2 119.3(5) . . ? N2 C26 C27 122.3(7) . . ? C28 C27 C26 118.7(8) . . ? C24 C28 C27 118.3(7) . . ? C31 C29 C32 110.9(11) . . ? C31 C29 C30 110.5(11) . . ? C32 C29 C30 102.2(9) . . ? C31 C29 C21 108.0(7) . . ? C32 C29 C21 113.9(7) . . ? C30 C29 C21 111.4(7) . . ? C33 S3 C19 107.5(3) . . ? C34 C33 C38 119.3(7) . . ? C34 C33 S3 122.4(5) . . ? C38 C33 S3 117.7(5) . . ? C33 C34 O3 120.0(6) . . ? C33 C34 C35 119.8(6) . . ? O3 C34 C35 120.1(6) . . ? C36 C35 C34 119.4(7) . . ? C36 C35 S4 116.6(5) . . ? C34 C35 S4 122.8(5) . . ? C35 C36 C37 121.2(7) . . ? C38 C37 C36 117.2(6) . . ? C38 C37 C45 121.9(7) . . ? C36 C37 C45 120.8(6) . . ? C37 C38 C33 122.3(7) . . ? C34 O3 C39 105.7(5) . . ? O3 C39 C40 108.1(6) . . ? C44 C40 C41 118.7(7) . . ? C44 C40 C39 121.8(7) . . ? C41 C40 C39 119.5(7) . . ? N3 C41 C40 122.4(8) . . ? C42 N3 C41 117.6(7) . . ? C42 N3 Ag3 123.5(5) . 2 ? C41 N3 Ag3 118.7(6) . 2 ? N3 C42 C43 123.7(8) . . ? C42 C43 C44 119.7(8) . . ? C40 C44 C43 117.8(8) . . ? C37 C45 C47 109.3(9) . . ? C37 C45 C48A 108.8(7) . . ? C37 C45 C47A 113.5(8) . . ? C48A C45 C47A 109.1(9) . . ? C37 C45 C48 108.3(9) . . ? C47 C45 C48 110.7(10) . . ? C48A C45 C48 138.1(11) . . ? C37 C45 C46 108.3(9) . . ? C47 C45 C46 110.7(10) . . ? C47A C45 C46 135.1(10) . . ? C48 C45 C46 109.6(11) . . ? C37 C45 C46A 108.7(7) . . ? C47 C45 C46A 138.3(10) . . ? C48A C45 C46A 108.7(9) . . ? C47A C45 C46A 107.9(9) . . ? C49 S4 C35 106.7(3) . . ? C54 C49 C50 119.3(7) . . ? C54 C49 S4 118.3(6) . . ? C50 C49 S4 122.0(5) . . ? O4 C50 C51 120.8(7) . . ? O4 C50 C49 120.9(6) . . ? C51 C50 C49 118.2(6) . . ? C50 C51 C52 121.2(7) . . ? C50 C51 S1 124.6(5) . . ? C52 C51 S1 113.6(6) . . ? C51 C52 C53 120.6(7) . . ? C54 C53 C52 116.9(6) . . ? C54 C53 C61 124.1(7) . . ? C52 C53 C61 119.0(7) . . ? C53 C54 C49 123.6(7) . . ? C50 O4 C55 114.1(6) . . ? O4 C55 C56 113.0(7) . . ? C60 C56 C57 118.7(9) . . ? C60 C56 C55 122.5(8) . . ? C57 C56 C55 118.7(8) . . ? N4 C57 C56 121.8(9) . . ? C57 N4 C58 119.1(8) . . ? C57 N4 Ag4 122.3(6) . 2_556 ? C58 N4 Ag4 118.6(7) . 2_556 ? N4 C58 C59 122.0(10) . . ? C60 C59 C58 118.6(10) . . ? C56 C60 C59 119.7(9) . . ? C62 C61 C63 114.1(11) . . ? C64A C61 C63 137.1(12) . . ? C62 C61 C53 105.4(8) . . ? C64A C61 C53 110.8(11) . . ? C63 C61 C53 112.1(7) . . ? C62 C61 C62A 146.3(13) . . ? C64A C61 C62A 111.0(12) . . ? C53 C61 C62A 107.9(12) . . ? C64A C61 C63A 110.3(12) . . ? C53 C61 C63A 111.0(9) . . ? C62A C61 C63A 105.7(12) . . ? C62 C61 C64 110.3(11) . . ? C63 C61 C64 106.9(9) . . ? C53 C61 C64 108.0(8) . . ? C63A C61 C64 140.2(11) . . ? C115 S5 C65 107.4(3) . . ? C70 C65 C66 120.7(7) . . ? C70 C65 S5 117.5(6) . . ? C66 C65 S5 121.5(5) . . ? O5 C66 C67 121.9(6) . . ? O5 C66 C65 120.5(6) . . ? C67 C66 C65 117.5(6) . . ? C66 C67 C68 120.1(6) . . ? C66 C67 S6 122.8(5) . . ? C68 C67 S6 116.8(5) . . ? C69 C68 C67 123.4(7) . . ? C68 C69 C70 116.1(6) . . ? C68 C69 C77 121.4(6) . . ? C70 C69 C77 122.5(6) . . ? C65 C70 C69 122.1(7) . . ? C66 O5 C71 115.7(5) . . ? O5 C71 C72 110.6(6) . . ? C73 C72 C76 115.3(8) . . ? C73 C72 C71 121.2(7) . . ? C76 C72 C71 123.4(7) . . ? N5 C73 C72 125.0(8) . . ? C73 N5 C74 118.3(7) . . ? C73 N5 Ag2 122.3(6) . . ? C74 N5 Ag2 119.3(6) . . ? N5 C74 C75 122.6(9) . . ? C74 C75 C76 117.6(9) . . ? C72 C76 C75 121.0(9) . . ? C79 C77 C80 112.0(14) . . ? C79 C77 C78 105.6(10) . . ? C80 C77 C78 106.1(12) . . ? C79 C77 C69 113.1(7) . . ? C80 C77 C69 108.4(7) . . ? C78 C77 C69 111.4(6) . . ? C81 S6 C67 107.5(3) . . ? C86 C81 C82 120.5(6) . . ? C86 C81 S6 117.4(5) . . ? C82 C81 S6 121.4(5) . . ? C83 C82 O6 121.0(6) . . ? C83 C82 C81 119.2(6) . . ? O6 C82 C81 119.7(6) . . ? C82 C83 C84 120.0(6) . . ? C82 C83 S7 123.3(5) . . ? C84 C83 S7 115.8(5) . . ? C85 C84 C83 121.8(7) . . ? C84 C85 C86 117.8(6) . . ? C84 C85 C93 120.3(6) . . ? C86 C85 C93 121.9(6) . . ? C81 C86 C85 120.8(6) . . ? C82 O6 C87 115.1(5) . . ? O6 C87 C88 107.4(6) . . ? C89 C88 C92 118.6(7) . . ? C89 C88 C87 116.8(7) . . ? C92 C88 C87 124.5(6) . . ? N6 C89 C88 122.0(7) . . ? C90 N6 C89 118.5(7) . . ? C90 N6 Ag4 123.8(5) . . ? C89 N6 Ag4 117.4(5) . . ? N6 C90 C91 122.4(7) . . ? C92 C91 C90 119.3(8) . . ? C91 C92 C88 119.2(7) . . ? C95 C93 C94 110.7(12) . . ? C95 C93 C96 112.7(12) . . ? C94 C93 C96 105.5(14) . . ? C95 C93 C85 112.6(7) . . ? C94 C93 C85 107.8(8) . . ? C96 C93 C85 107.2(7) . . ? C83 S7 C97 107.8(3) . . ? C98 C97 C102 120.7(7) . . ? C98 C97 S7 123.1(5) . . ? C102 C97 S7 115.0(6) . . ? C97 C98 O7 121.5(6) . . ? C97 C98 C99 119.5(6) . . ? O7 C98 C99 119.0(6) . . ? C98 C99 C100 118.6(7) . . ? C98 C99 S8 124.8(5) . . ? C100 C99 S8 115.3(6) . . ? C101 C100 C99 121.6(7) . . ? C102 C101 C100 117.0(6) . . ? C102 C101 C109 123.3(7) . . ? C100 C101 C109 119.6(7) . . ? C101 C102 C97 122.6(7) . . ? C98 O7 C103 111.6(5) . . ? O7 C103 C104 108.1(6) . . ? C105 C104 C108 118.2(7) . . ? C105 C104 C103 116.4(6) . . ? C108 C104 C103 125.4(6) . . ? N7 C105 C104 122.3(7) . . ? C106 N7 C105 119.8(7) . . ? C106 N7 Ag3 128.0(5) . . ? C105 N7 Ag3 112.2(5) . . ? N7 C106 C107 121.0(7) . . ? C108 C107 C106 119.5(7) . . ? C107 C108 C104 119.1(7) . . ? C111 C109 C110 112.3(10) . . ? C111 C109 C112 109.7(9) . . ? C110 C109 C112 105.9(8) . . ? C111 C109 C101 111.5(7) . . ? C110 C109 C101 106.9(6) . . ? C112 C109 C101 110.4(7) . . ? C99 S8 C113 108.5(3) . . ? C114 C113 C118 120.7(6) . . ? C114 C113 S8 123.3(5) . . ? C118 C113 S8 115.4(5) . . ? C115 C114 C113 118.8(6) . . ? C115 C114 O8 119.3(6) . . ? C113 C114 O8 121.8(6) . . ? C114 C115 C116 120.1(6) . . ? C114 C115 S5 125.0(5) . . ? C116 C115 S5 114.5(5) . . ? C117 C116 C115 121.4(6) . . ? C118 C117 C116 116.8(6) . . ? C118 C117 C125 120.6(6) . . ? C116 C117 C125 122.7(6) . . ? C113 C118 C117 121.6(6) . . ? C114 O8 C119 115.2(5) . . ? O8 C119 C120 113.1(7) . . ? C124 C120 C121 116.6(8) . . ? C124 C120 C119 124.0(7) . . ? C121 C120 C119 119.4(7) . . ? N8 C121 C120 124.1(8) . . ? C121 N8 C122 117.4(7) . . ? C121 N8 Ag1 121.8(6) . 1_556 ? C122 N8 Ag1 120.8(6) . 1_556 ? C123 C122 N8 123.3(9) . . ? C122 C123 C124 117.4(9) . . ? C120 C124 C123 121.0(8) . . ? C126 C125 C128 110.7(10) . . ? C126 C125 C117 109.9(7) . . ? C128 C125 C117 111.3(7) . . ? C126 C125 C127 107.8(9) . . ? C128 C125 C127 105.6(9) . . ? C117 C125 C127 111.4(6) . . ? F4 B1 F1 113.3(10) . . ? F4 B1 F2 112.3(10) . . ? F1 B1 F2 109.7(9) . . ? F4 B1 F3 105.9(9) . . ? F1 B1 F3 107.4(9) . . ? F2 B1 F3 107.9(10) . . ? F8 B2 F6 111.7(9) . . ? F8 B2 F5 109.8(9) . . ? F6 B2 F5 110.7(10) . . ? F8 B2 F7 110.9(10) . . ? F6 B2 F7 107.5(9) . . ? F5 B2 F7 106.0(9) . . ? F11A B3 F9A 117.7(14) . . ? F11A B3 F10A 111.4(14) . . ? F9A B3 F10A 120.3(11) . . ? F11A B3 F12A 101.5(16) . . ? F9A B3 F12A 99.1(14) . . ? F10A B3 F12A 102.5(14) . . ? F9A B3 F11 117.1(10) . . ? F10A B3 F11 121.9(10) . . ? F10A B3 F10 122.5(11) . . ? F12A B3 F10 127.4(14) . . ? F11 B3 F10 108.4(9) . . ? F11A B3 F12 154.9(16) . . ? F11 B3 F12 113.0(11) . . ? F10 B3 F12 109.4(11) . . ? F9A B3 F9 128.0(11) . . ? F12A B3 F9 124.4(14) . . ? F11 B3 F9 109.5(9) . . ? F10 B3 F9 108.0(10) . . ? F12 B3 F9 108.4(11) . . ? F15A B4 F13 161.6(17) . . ? F13 B4 F14 115.1(14) . . ? F15A B4 F16A 127.4(15) . . ? F14 B4 F16A 115.6(14) . . ? F13 B4 F15 116.9(14) . . ? F14 B4 F15 108.5(12) . . ? F16A B4 F15 126.9(15) . . ? F13 B4 F16 113.1(13) . . ? F14 B4 F16 100.9(11) . . ? F15 B4 F16 100.3(11) . . ? F15A B4 F13A 113.7(14) . . ? F16A B4 F13A 101.9(12) . . ? F15 B4 F13A 129.4(14) . . ? F16 B4 F13A 126.4(14) . . ? F15A B4 F14A 112.3(14) . . ? F14 B4 F14A 135.8(14) . . ? F16A B4 F14A 98.9(12) . . ? F16 B4 F14A 123.4(14) . . ? F13A B4 F14A 98.0(11) . . ? Cl3 C129 Cl1 114.0(7) . . ? Cl3 C129 Cl2 104.2(8) . . ? Cl1 C129 Cl2 108.0(6) . . ? Cl5 C130 Cl6 107.6(11) . . ? Cl5 C130 Cl4 105.5(10) . . ? Cl6 C130 Cl4 109.4(11) . . ? Cl8 C131 Cl9 108.4(10) . . ? Cl8 C131 Cl7 111.6(11) . . ? Cl9 C131 Cl7 111.6(9) . . ? Cl12 C132 Cl11 102.7(9) . . ? Cl12 C132 Cl10 112.8(10) . . ? Cl11 C132 Cl10 107.6(9) . . ? Cl14 C133 Cl13 109.7(12) . . ? Cl14 C133 Cl15 122.1(11) . . ? Cl13 C133 Cl15 111.8(9) . . ? Cl18 C134 Cl16 112.2(8) . . ? Cl18 C134 Cl17 109.9(8) . . ? Cl16 C134 Cl17 108.6(7) . . ? Cl19 C135 Cl20 110.5(6) . . ? Cl19 C135 Cl21 108.9(8) . . ? Cl20 C135 Cl21 107.5(7) . . ? Cl24 C136 Cl22 113.8(8) . . ? Cl24 C136 Cl23 110.8(7) . . ? Cl22 C136 Cl23 108.3(8) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 30.10 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 2.044 _refine_diff_density_min -1.644 _refine_diff_density_rms 0.229 _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 0.000 0.000 0.000 210.5 85.6 2 0.978 0.329 0.057 10.0 0.0 3 0.707 0.354 0.177 22.6 4.3 4 0.793 0.854 0.323 22.6 3.9 5 0.500 0.500 0.500 210.6 85.4 6 0.522 0.829 0.442 10.0 -0.1 7 0.478 0.170 0.557 9.9 -0.1 8 0.207 0.146 0.677 22.6 4.1 9 0.293 0.646 0.823 22.6 3.7 10 0.022 0.670 0.942 9.9 -0.2 _platon_squeeze_details ; ; data_e2258b _database_code_depnum_ccdc_archive 'CCDC 895674' #TrackingRef 'web_deposit_cif_file_6_SylvieFERLAY_1344596913.3-AgPF6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 4(C64H68Ag2N4O4S4),8(F6P),8(CHCl3),2H2O _chemical_formula_sum 'C264 H284 Ag8 Cl24 F48 N16 O18 P8 S16' _chemical_formula_weight 7355.55 _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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 Cc _symmetry_space_group_name_Hall 'C -2yc' _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 27.8405(11) _cell_length_b 14.2705(4) _cell_length_c 22.4525(6) _cell_angle_alpha 90.00 _cell_angle_beta 102.331(2) _cell_angle_gamma 90.00 _cell_volume 8714.5(5) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8370 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 20.73 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.402 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3716 _exptl_absorpt_coefficient_mu 0.835 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9439 _exptl_absorpt_correction_T_max 0.9595 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 52532 _diffrn_reflns_av_R_equivalents 0.0568 _diffrn_reflns_av_sigmaI/netI 0.0903 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 28.35 _reflns_number_total 20104 _reflns_number_gt 12771 _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.3870P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(5) _refine_ls_number_reflns 20104 _refine_ls_number_parameters 843 _refine_ls_number_restraints 80 _refine_ls_R_factor_all 0.1566 _refine_ls_R_factor_gt 0.0895 _refine_ls_wR_factor_ref 0.3078 _refine_ls_wR_factor_gt 0.2517 _refine_ls_goodness_of_fit_ref 1.130 _refine_ls_restrained_S_all 1.298 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.011 _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 0.61918(4) -0.18957(9) 0.54469(5) 0.0579(3) Uani 1 1 d . . . Ag2 Ag 1.18694(3) -0.09764(8) 0.65965(5) 0.0523(3) Uani 1 1 d . . . S1 S 0.85485(10) 0.0191(2) 0.43286(12) 0.0359(6) Uani 1 1 d . . . C1 C 0.8963(4) -0.0618(9) 0.4771(5) 0.032(2) Uani 1 1 d . . . C2 C 0.8883(4) -0.1072(8) 0.5280(5) 0.032(2) Uani 1 1 d . . . C3 C 0.9174(4) -0.1820(8) 0.5535(5) 0.034(2) Uani 1 1 d . . . C4 C 0.9552(4) -0.2125(9) 0.5258(6) 0.038(3) Uani 1 1 d D . . H4 H 0.9751 -0.2640 0.5429 0.046 Uiso 1 1 calc R . . C5 C 0.9644(4) -0.1687(10) 0.4731(6) 0.038(3) Uani 1 1 d . . . C6 C 0.9354(4) -0.0923(9) 0.4495(5) 0.036(3) Uani 1 1 d . . . H6 H 0.9417 -0.0602 0.4149 0.043 Uiso 1 1 calc R . . O1 O 0.8511(3) -0.0760(6) 0.5556(4) 0.0351(18) Uani 1 1 d . . . C7 C 0.8062(4) -0.1281(10) 0.5333(6) 0.040(3) Uani 1 1 d . . . H7A H 0.8127 -0.1961 0.5383 0.048 Uiso 1 1 calc R . . H7B H 0.7937 -0.1150 0.4895 0.048 Uiso 1 1 calc R . . C8 C 0.7689(4) -0.0992(8) 0.5688(6) 0.034(2) Uani 1 1 d . . . C9 C 0.7229(4) -0.1418(8) 0.5545(6) 0.034(2) Uani 1 1 d . . . H9 H 0.7177 -0.1873 0.5228 0.041 Uiso 1 1 calc R . . N1 N 0.6861(4) -0.1247(9) 0.5808(5) 0.046(3) Uani 1 1 d . . . C10 C 0.6955(5) -0.0585(10) 0.6257(7) 0.049(3) Uani 1 1 d . . . H10 H 0.6701 -0.0460 0.6470 0.059 Uiso 1 1 calc R . . C11 C 0.7373(4) -0.0098(10) 0.6423(6) 0.042(3) Uani 1 1 d . . . H11 H 0.7408 0.0370 0.6730 0.050 Uiso 1 1 calc R . . C12 C 0.7763(4) -0.0305(9) 0.6123(6) 0.040(3) Uani 1 1 d . . . H12 H 0.8066 0.0025 0.6223 0.048 Uiso 1 1 calc R . . C13 C 1.0027(5) -0.2074(11) 0.4404(6) 0.051(4) Uani 1 1 d . . . C14 C 1.0470(11) -0.264(2) 0.4823(12) 0.068(5) Uani 1 1 d D . . H14A H 1.0726 -0.2194 0.5016 0.102 Uiso 1 1 calc R . . H14B H 1.0609 -0.3080 0.4571 0.102 Uiso 1 1 calc R . . H14C H 1.0348 -0.2980 0.5138 0.102 Uiso 1 1 calc R . . C15 C 0.9764(7) -0.2572(13) 0.3839(9) 0.068(5) Uani 1 1 d . . . H15A H 0.9994 -0.2698 0.3575 0.102 Uiso 1 1 calc R . . H15B H 0.9495 -0.2177 0.3622 0.102 Uiso 1 1 calc R . . H15C H 0.9630 -0.3165 0.3953 0.102 Uiso 1 1 calc R . . C16 C 1.0332(5) -0.1317(16) 0.4236(6) 0.067(5) Uani 1 1 d . . . H16A H 1.0142 -0.0969 0.3888 0.100 Uiso 1 1 calc R . . H16B H 1.0625 -0.1586 0.4126 0.100 Uiso 1 1 calc R . . H16C H 1.0432 -0.0891 0.4583 0.100 Uiso 1 1 calc R . . S2 S 0.90502(13) -0.2569(2) 0.60989(15) 0.0418(7) Uani 1 1 d . . . C17 C 0.8860(4) -0.1867(8) 0.6660(5) 0.031(2) Uani 1 1 d . . . C18 C 0.9126(4) -0.1083(7) 0.6906(5) 0.027(2) Uani 1 1 d . . . C19 C 0.9018(4) -0.0681(8) 0.7425(5) 0.028(2) Uani 1 1 d . . . C20 C 0.8627(4) -0.1028(8) 0.7668(5) 0.032(2) Uani 1 1 d . . . H20 H 0.8547 -0.0732 0.8013 0.039 Uiso 1 1 calc R . . C21 C 0.8353(4) -0.1806(9) 0.7406(5) 0.034(2) Uani 1 1 d . . . C22 C 0.8481(5) -0.2206(8) 0.6921(5) 0.037(3) Uani 1 1 d . . . H22 H 0.8305 -0.2745 0.6746 0.044 Uiso 1 1 calc R . . O2 O 0.9495(3) -0.0708(5) 0.6668(4) 0.0314(16) Uani 1 1 d . . . C23 C 0.9964(5) -0.1090(9) 0.6861(6) 0.042(3) Uani 1 1 d . . . H23A H 0.9949 -0.1780 0.6813 0.051 Uiso 1 1 calc R . . H23B H 1.0092 -0.0945 0.7297 0.051 Uiso 1 1 calc R . . C24 C 1.0300(4) -0.0682(8) 0.6485(5) 0.033(2) Uani 1 1 d . . . C25 C 1.0793(4) -0.0867(9) 0.6631(6) 0.039(3) Uani 1 1 d . . . H25 H 1.0910 -0.1250 0.6978 0.047 Uiso 1 1 calc R . . N2 N 1.1117(3) -0.0557(7) 0.6331(5) 0.041(2) Uani 1 1 d . . . C26 C 1.0952(4) -0.0068(10) 0.5814(6) 0.044(3) Uani 1 1 d . . . H26 H 1.1176 0.0119 0.5571 0.053 Uiso 1 1 calc R . . C27 C 1.0449(4) 0.0168(9) 0.5632(6) 0.038(3) Uani 1 1 d . . . H27 H 1.0334 0.0533 0.5276 0.045 Uiso 1 1 calc R . . C28 C 1.0131(4) -0.0137(9) 0.5977(5) 0.036(3) Uani 1 1 d . . . H28 H 0.9793 0.0027 0.5866 0.043 Uiso 1 1 calc R . . C29 C 0.7940(6) -0.2216(12) 0.7705(7) 0.076(3) Uani 1 1 d D . . C30 C 0.8241(13) -0.304(3) 0.809(2) 0.076(3) Uani 0.38(5) 1 d PD . 1 H30A H 0.8569 -0.2814 0.8282 0.115 Uiso 0.38(5) 1 calc PR . 1 H30B H 0.8270 -0.3564 0.7816 0.115 Uiso 0.38(5) 1 calc PR . 1 H30C H 0.8068 -0.3249 0.8401 0.115 Uiso 0.38(5) 1 calc PR . 1 C31 C 0.7535(6) -0.2677(13) 0.7201(6) 0.076(3) Uani 1 1 d D . . H31A H 0.7326 -0.3079 0.7392 0.115 Uiso 1 1 calc R . . H31B H 0.7691 -0.3054 0.6930 0.115 Uiso 1 1 calc R . . H31C H 0.7334 -0.2186 0.6964 0.115 Uiso 1 1 calc R . . C32 C 0.7721(13) -0.159(4) 0.813(2) 0.076(3) Uani 0.38(5) 1 d PD . 1 H32A H 0.7848 -0.0951 0.8114 0.115 Uiso 0.38(5) 1 calc PR . 1 H32B H 0.7813 -0.1831 0.8545 0.115 Uiso 0.38(5) 1 calc PR . 1 H32C H 0.7362 -0.1585 0.7995 0.115 Uiso 0.38(5) 1 calc PR . 1 S3 S 0.93929(10) 0.0192(2) 0.78571(13) 0.0320(6) Uani 1 1 d . . . C33 C 0.9500(4) 0.1073(7) 0.7338(5) 0.027(2) Uani 1 1 d . . . C34 C 0.9118(4) 0.1561(8) 0.6957(5) 0.031(2) Uani 1 1 d . . . C35 C 0.9250(5) 0.2280(8) 0.6576(6) 0.038(3) Uani 1 1 d . . . C36 C 0.9721(5) 0.2529(9) 0.6652(6) 0.045(3) Uani 1 1 d D . . H36 H 0.9800 0.3011 0.6397 0.055 Uiso 1 1 calc R . . C37 C 1.0116(4) 0.2126(8) 0.7089(5) 0.034(2) Uani 1 1 d . . . C38 C 0.9977(4) 0.1372(9) 0.7403(5) 0.036(3) Uani 1 1 d . . . H38 H 1.0227 0.1043 0.7679 0.043 Uiso 1 1 calc R . . O3 O 0.8639(3) 0.1290(6) 0.6891(4) 0.0404(19) Uani 1 1 d . . . C39 C 0.8428(5) 0.1560(11) 0.7393(7) 0.052(4) Uani 1 1 d . . . H39A H 0.8673 0.1462 0.7778 0.062 Uiso 1 1 calc R . . H39B H 0.8142 0.1152 0.7402 0.062 Uiso 1 1 calc R . . C40 C 0.8257(5) 0.2605(12) 0.7357(7) 0.056(4) Uani 1 1 d . . . C41 C 0.7775(5) 0.2792(11) 0.7061(7) 0.050(3) Uani 1 1 d . . . H41 H 0.7559 0.2291 0.6908 0.060 Uiso 1 1 calc R . . N3 N 0.7617(4) 0.3681(10) 0.6991(7) 0.062(4) Uani 1 1 d . . . C42 C 0.7917(6) 0.4372(14) 0.7192(12) 0.097(8) Uani 1 1 d . . . H42 H 0.7801 0.4999 0.7155 0.117 Uiso 1 1 calc R . . C43 C 0.8424(7) 0.4183(17) 0.7468(14) 0.111(10) Uani 1 1 d . . . H43 H 0.8666 0.4661 0.7548 0.133 Uiso 1 1 calc R . . C44 C 0.8529(7) 0.3266(17) 0.7604(12) 0.105(10) Uani 1 1 d . . . H44 H 0.8818 0.3118 0.7898 0.126 Uiso 1 1 calc R . . C45 C 1.0646(7) 0.2470(14) 0.7167(8) 0.069(2) Uani 1 1 d . . . C46 C 1.0918(7) 0.1770(14) 0.6906(8) 0.069(2) Uani 1 1 d . . . H46A H 1.0704 0.1492 0.6546 0.103 Uiso 1 1 calc R . . H46B H 1.1032 0.1279 0.7209 0.103 Uiso 1 1 calc R . . H46C H 1.1201 0.2065 0.6788 0.103 Uiso 1 1 calc R . . C47 C 1.0735(6) 0.3356(14) 0.6796(8) 0.069(2) Uani 1 1 d D . . H47A H 1.0734 0.3917 0.7048 0.103 Uiso 1 1 calc R . . H47B H 1.0473 0.3406 0.6428 0.103 Uiso 1 1 calc R . . H47C H 1.1054 0.3301 0.6680 0.103 Uiso 1 1 calc R . . C48 C 1.0869(7) 0.2604(14) 0.7829(8) 0.069(2) Uani 1 1 d . . . H48A H 1.0763 0.2096 0.8065 0.103 Uiso 1 1 calc R . . H48B H 1.0762 0.3206 0.7966 0.103 Uiso 1 1 calc R . . H48C H 1.1228 0.2596 0.7890 0.103 Uiso 1 1 calc R . . S4 S 0.88038(15) 0.2956(2) 0.60976(17) 0.0555(10) Uani 1 1 d . . . C49 C 0.8433(4) 0.2129(8) 0.5578(5) 0.034(2) Uani 1 1 d . . . C50 C 0.8636(4) 0.1549(9) 0.5240(6) 0.039(3) Uani 1 1 d . . . C51 C 0.8322(4) 0.0905(8) 0.4821(5) 0.033(2) Uani 1 1 d . . . C52 C 0.7823(4) 0.1036(8) 0.4760(5) 0.030(2) Uani 1 1 d . . . H52 H 0.7604 0.0646 0.4485 0.036 Uiso 1 1 calc R . . C53 C 0.7623(4) 0.1727(8) 0.5091(5) 0.029(2) Uani 1 1 d . . . C54 C 0.7930(5) 0.2213(9) 0.5498(6) 0.039(3) Uani 1 1 d . . . H54 H 0.7801 0.2640 0.5748 0.047 Uiso 1 1 calc R . . O4 O 0.9148(3) 0.1524(6) 0.5244(4) 0.0358(18) Uani 1 1 d . . . C55 C 0.9241(5) 0.2241(11) 0.4836(8) 0.053(3) Uani 1 1 d . . . H55A H 0.9247 0.2863 0.5033 0.063 Uiso 1 1 calc R . . H55B H 0.8978 0.2243 0.4461 0.063 Uiso 1 1 calc R . . C56 C 0.9724(5) 0.2044(11) 0.4682(8) 0.052(4) Uani 1 1 d . . . C57 C 1.0140(5) 0.2456(10) 0.5025(7) 0.048(3) Uani 1 1 d . . . H57 H 1.0102 0.2857 0.5349 0.057 Uiso 1 1 calc R . . N4 N 1.0594(4) 0.2328(8) 0.4931(6) 0.051(3) Uani 1 1 d . . . C58 C 1.0641(6) 0.1810(10) 0.4446(7) 0.049(3) Uani 1 1 d . . . H58 H 1.0959 0.1750 0.4358 0.059 Uiso 1 1 calc R . . C59 C 1.0262(6) 0.1371(11) 0.4077(8) 0.059(4) Uani 1 1 d . . . H59 H 1.0313 0.0988 0.3750 0.071 Uiso 1 1 calc R . . C60 C 0.9790(5) 0.1500(11) 0.4193(7) 0.054(4) Uani 1 1 d . . . H60 H 0.9514 0.1212 0.3936 0.064 Uiso 1 1 calc R . . C61 C 0.7069(4) 0.1915(10) 0.4924(5) 0.041(3) Uani 1 1 d . . . C62 C 0.6769(6) 0.0959(16) 0.4868(11) 0.084(3) Uani 1 1 d . . . H62A H 0.6989 0.0435 0.4835 0.126 Uiso 1 1 calc R . . H62B H 0.6502 0.0979 0.4504 0.126 Uiso 1 1 calc R . . H62C H 0.6630 0.0875 0.5230 0.126 Uiso 1 1 calc R . . C63 C 0.6918(7) 0.2472(17) 0.5433(10) 0.084(3) Uani 1 1 d . . . H63A H 0.6567 0.2375 0.5417 0.126 Uiso 1 1 calc R . . H63B H 0.6980 0.3139 0.5380 0.126 Uiso 1 1 calc R . . H63C H 0.7110 0.2259 0.5828 0.126 Uiso 1 1 calc R . . C64 C 0.6921(6) 0.2398(17) 0.4360(10) 0.084(3) Uani 1 1 d . . . H64A H 0.7203 0.2732 0.4266 0.126 Uiso 1 1 calc R . . H64B H 0.6661 0.2848 0.4391 0.126 Uiso 1 1 calc R . . H64C H 0.6796 0.1947 0.4035 0.126 Uiso 1 1 calc R . . P1 P 0.09929(17) 0.6436(3) 0.6722(2) 0.0694(12) Uani 1 1 d D . . F1 F 0.0506(6) 0.6980(13) 0.6342(8) 0.0694(12) Uani 0.46(3) 1 d PD A 1 F2 F 0.0641(7) 0.5573(10) 0.6859(9) 0.0694(12) Uani 0.46(3) 1 d PD A 1 F3 F 0.1050(8) 0.5947(12) 0.6075(6) 0.0694(12) Uani 0.46(3) 1 d PD A 1 F4 F 0.1493(5) 0.5874(12) 0.7052(8) 0.0694(12) Uani 0.46(3) 1 d PD A 1 F5 F 0.1334(7) 0.7301(10) 0.6562(9) 0.0694(12) Uani 0.46(3) 1 d PD A 1 F6 F 0.0959(8) 0.6950(13) 0.7355(6) 0.0694(12) Uani 0.46(3) 1 d PD A 1 P2 P 0.23040(19) 0.0715(3) 0.5422(3) 0.0835(17) Uani 1 1 d D . . F7 F 0.2153(6) 0.0766(11) 0.6126(6) 0.144(3) Uani 1 1 d D . . F8 F 0.1851(5) 0.1438(10) 0.5163(7) 0.144(3) Uani 1 1 d D . . F9 F 0.1932(5) -0.0209(9) 0.5233(8) 0.144(3) Uani 1 1 d D . . F10 F 0.2498(6) 0.0571(11) 0.4785(6) 0.144(3) Uani 1 1 d D . . F11 F 0.2775(5) -0.0036(10) 0.5755(8) 0.144(3) Uani 1 1 d D . . F12 F 0.2687(5) 0.1604(9) 0.5644(8) 0.144(3) Uani 1 1 d D . . C65 C 0.3646(17) 0.032(3) 0.489(2) 0.0917(18) Uani 0.50 1 d P . . H65 H 0.3456 0.0414 0.5219 0.110 Uiso 0.50 1 calc PR . . Cl1 Cl 0.4239(4) 0.0225(8) 0.5253(6) 0.0917(18) Uani 0.50 1 d P . . Cl2 Cl 0.3581(4) 0.1422(8) 0.4438(6) 0.0917(18) Uani 0.50 1 d P . . Cl3 Cl 0.3392(4) -0.0631(8) 0.4490(6) 0.0917(18) Uani 0.50 1 d P . . C66 C 0.6750(19) 0.460(3) 0.854(3) 0.099(2) Uani 0.50 1 d P . . H66 H 0.7015 0.4478 0.8911 0.118 Uiso 0.50 1 calc PR . . Cl4 Cl 0.6309(5) 0.5270(7) 0.8897(7) 0.099(2) Uani 0.50 1 d P . . Cl5 Cl 0.6824(5) 0.3490(8) 0.8068(7) 0.099(2) Uani 0.50 1 d P . . Cl6 Cl 0.7059(5) 0.5361(8) 0.8152(7) 0.099(2) Uani 0.50 1 d P . . C67 C 0.481(2) 0.065(3) 0.777(2) 0.0935(19) Uani 0.50 1 d P . . H67 H 0.5144 0.0735 0.7669 0.112 Uiso 0.50 1 calc PR . . Cl7 Cl 0.4642(5) 0.1733(8) 0.7861(6) 0.0935(19) Uani 0.50 1 d P . . Cl8 Cl 0.4865(5) -0.0277(7) 0.8078(6) 0.0935(19) Uani 0.50 1 d P . . Cl9 Cl 0.4399(5) 0.0296(8) 0.6961(6) 0.0935(19) Uani 0.50 1 d P . . O5 O 0.5523(9) 0.9511(14) 0.5391(11) 0.066(6) Uani 0.50 1 d P . . C69 C 0.1993(9) 0.6716(19) 0.8521(16) 0.127(3) Uani 0.50 1 d PD . . H69 H 0.1809 0.6951 0.8117 0.152 Uiso 0.50 1 calc PR . . Cl10 Cl 0.1567(6) 0.6474(12) 0.8981(7) 0.127(3) Uani 0.50 1 d PD . . Cl11 Cl 0.2479(6) 0.7452(11) 0.8783(7) 0.127(3) Uani 0.50 1 d PD . . Cl12 Cl 0.2323(6) 0.5749(11) 0.8405(7) 0.127(3) Uani 0.50 1 d PD . . C30A C 0.8140(10) -0.281(2) 0.8248(12) 0.076(3) Uani 0.62(5) 1 d PD . 2 H30D H 0.8440 -0.2523 0.8486 0.115 Uiso 0.62(5) 1 calc PR . 2 H30E H 0.8216 -0.3436 0.8114 0.115 Uiso 0.62(5) 1 calc PR . 2 H30F H 0.7895 -0.2861 0.8502 0.115 Uiso 0.62(5) 1 calc PR . 2 C32A C 0.7661(10) -0.1326(18) 0.7918(16) 0.076(3) Uani 0.62(5) 1 d PD . 2 H32D H 0.7311 -0.1471 0.7872 0.115 Uiso 0.62(5) 1 calc PR . 2 H32E H 0.7699 -0.0782 0.7666 0.115 Uiso 0.62(5) 1 calc PR . 2 H32F H 0.7804 -0.1186 0.8347 0.115 Uiso 0.62(5) 1 calc PR . 2 F1A F 0.1502(6) 0.7073(16) 0.6918(13) 0.0694(12) Uani 0.54(3) 1 d PD A 2 F2A F 0.0765(11) 0.7244(14) 0.6228(9) 0.0694(12) Uani 0.54(3) 1 d PD A 2 F3A F 0.1219(11) 0.5880(19) 0.6188(11) 0.0694(12) Uani 0.54(3) 1 d PD A 2 F4A F 0.0470(6) 0.5820(17) 0.6509(13) 0.0694(12) Uani 0.54(3) 1 d PD A 2 F5A F 0.1227(11) 0.5602(14) 0.7219(10) 0.0694(12) Uani 0.54(3) 1 d PD A 2 F6A F 0.0754(9) 0.6943(15) 0.7258(9) 0.0694(12) Uani 0.54(3) 1 d PD A 2 _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 0.0258(4) 0.0690(7) 0.0801(8) -0.0111(6) 0.0144(5) -0.0169(5) Ag2 0.0232(4) 0.0704(7) 0.0644(7) 0.0014(6) 0.0121(4) 0.0105(4) S1 0.0246(12) 0.0579(17) 0.0263(14) 0.0018(13) 0.0076(10) 0.0106(12) C1 0.013(4) 0.058(7) 0.026(5) 0.002(5) 0.004(4) 0.008(4) C2 0.028(5) 0.041(6) 0.033(6) -0.008(5) 0.019(5) -0.004(4) C3 0.030(5) 0.044(6) 0.032(6) -0.003(5) 0.016(5) -0.008(5) C4 0.026(5) 0.049(7) 0.038(6) 0.002(5) 0.004(5) 0.010(5) C5 0.024(5) 0.059(7) 0.034(6) 0.007(5) 0.012(5) 0.011(5) C6 0.024(5) 0.060(8) 0.027(6) 0.004(5) 0.011(4) 0.016(5) O1 0.019(3) 0.045(4) 0.046(5) -0.005(4) 0.016(3) 0.000(3) C7 0.019(5) 0.059(7) 0.043(7) -0.023(6) 0.010(5) -0.016(5) C8 0.023(5) 0.037(6) 0.045(7) 0.003(5) 0.014(5) 0.000(4) C9 0.018(5) 0.039(6) 0.045(7) -0.015(5) 0.009(4) -0.013(4) N1 0.024(5) 0.065(7) 0.051(6) -0.004(6) 0.013(4) -0.013(5) C10 0.045(7) 0.055(7) 0.063(9) -0.004(7) 0.047(7) 0.000(6) C11 0.030(6) 0.055(7) 0.037(6) -0.011(6) 0.002(5) -0.006(5) C12 0.026(5) 0.052(7) 0.043(7) -0.003(6) 0.007(5) -0.020(5) C13 0.040(7) 0.069(9) 0.049(8) 0.012(7) 0.024(6) 0.040(7) C14 0.057(9) 0.071(10) 0.090(12) -0.018(9) 0.049(9) 0.005(8) C15 0.057(9) 0.071(10) 0.090(12) -0.018(9) 0.049(9) 0.005(8) C16 0.024(6) 0.146(16) 0.035(7) -0.015(9) 0.014(5) 0.008(8) S2 0.0578(19) 0.0340(14) 0.0406(16) 0.0003(13) 0.0260(14) 0.0009(13) C17 0.024(5) 0.035(6) 0.035(6) 0.001(5) 0.010(4) -0.005(4) C18 0.022(5) 0.029(5) 0.036(6) 0.001(4) 0.018(4) -0.003(4) C19 0.031(5) 0.031(5) 0.022(5) 0.003(4) 0.003(4) -0.007(4) C20 0.023(5) 0.053(7) 0.021(5) -0.004(5) 0.008(4) -0.008(5) C21 0.030(6) 0.048(6) 0.026(5) 0.006(5) 0.009(4) -0.013(5) C22 0.047(7) 0.035(6) 0.032(6) -0.002(5) 0.018(5) -0.016(5) O2 0.024(4) 0.037(4) 0.037(4) 0.009(3) 0.014(3) -0.003(3) C23 0.033(6) 0.045(7) 0.051(8) 0.011(6) 0.014(5) -0.008(5) C24 0.022(5) 0.043(6) 0.035(6) 0.008(5) 0.011(4) -0.001(4) C25 0.025(5) 0.051(7) 0.043(7) 0.008(5) 0.013(5) 0.012(5) N2 0.017(4) 0.044(6) 0.066(7) 0.014(5) 0.015(4) 0.007(4) C26 0.018(5) 0.058(8) 0.058(8) 0.001(6) 0.013(5) -0.001(5) C27 0.019(5) 0.044(6) 0.053(7) 0.015(6) 0.012(5) 0.004(4) C28 0.024(5) 0.051(7) 0.036(6) 0.020(5) 0.015(5) -0.002(5) C29 0.064(6) 0.111(8) 0.063(6) 0.003(5) 0.036(5) -0.047(6) C30 0.064(6) 0.111(8) 0.063(6) 0.003(5) 0.036(5) -0.047(6) C31 0.064(6) 0.111(8) 0.063(6) 0.003(5) 0.036(5) -0.047(6) C32 0.064(6) 0.111(8) 0.063(6) 0.003(5) 0.036(5) -0.047(6) S3 0.0272(13) 0.0372(14) 0.0309(14) 0.0015(11) 0.0048(11) -0.0066(11) C33 0.030(5) 0.027(5) 0.021(5) -0.002(4) 0.001(4) 0.004(4) C34 0.028(5) 0.033(5) 0.033(6) -0.002(4) 0.007(4) -0.007(4) C35 0.042(7) 0.024(5) 0.044(7) 0.006(5) -0.001(5) -0.004(5) C36 0.054(8) 0.036(6) 0.041(7) 0.007(5) -0.002(6) -0.006(6) C37 0.030(6) 0.038(6) 0.032(6) 0.006(5) 0.005(5) -0.005(5) C38 0.024(5) 0.058(7) 0.026(5) -0.003(5) 0.003(4) 0.000(5) O3 0.018(4) 0.049(5) 0.048(5) -0.004(4) -0.006(3) 0.003(3) C39 0.030(6) 0.067(9) 0.054(8) -0.024(7) 0.000(6) 0.022(6) C40 0.027(6) 0.077(10) 0.061(9) -0.005(8) 0.003(6) 0.023(7) C41 0.024(6) 0.059(8) 0.070(9) 0.011(7) 0.015(6) 0.010(5) N3 0.026(5) 0.073(8) 0.087(9) -0.036(8) 0.014(6) 0.013(6) C42 0.026(7) 0.071(11) 0.18(2) -0.053(13) -0.019(10) 0.020(7) C43 0.038(9) 0.096(15) 0.17(2) -0.057(16) -0.033(12) 0.013(10) C44 0.047(10) 0.113(17) 0.131(19) -0.072(15) -0.036(12) 0.023(11) C45 0.058(5) 0.086(6) 0.062(5) 0.002(4) 0.013(4) -0.022(4) C46 0.058(5) 0.086(6) 0.062(5) 0.002(4) 0.013(4) -0.022(4) C47 0.058(5) 0.086(6) 0.062(5) 0.002(4) 0.013(4) -0.022(4) C48 0.058(5) 0.086(6) 0.062(5) 0.002(4) 0.013(4) -0.022(4) S4 0.065(2) 0.0349(16) 0.051(2) 0.0035(14) -0.0224(18) 0.0025(15) C49 0.035(6) 0.028(5) 0.033(6) -0.003(5) -0.008(5) 0.004(4) C50 0.015(5) 0.048(7) 0.052(7) 0.012(6) 0.002(5) -0.002(4) C51 0.026(5) 0.039(6) 0.035(6) 0.012(5) 0.009(4) 0.009(4) C52 0.020(5) 0.039(6) 0.030(6) 0.003(5) 0.004(4) 0.006(4) C53 0.019(5) 0.036(5) 0.036(6) 0.007(5) 0.012(4) 0.010(4) C54 0.035(6) 0.047(7) 0.036(6) 0.002(5) 0.008(5) 0.014(5) O4 0.019(4) 0.037(4) 0.051(5) 0.013(4) 0.005(3) -0.001(3) C55 0.032(7) 0.053(8) 0.071(10) 0.006(7) 0.004(6) 0.000(6) C56 0.028(6) 0.058(8) 0.067(10) 0.028(8) 0.004(6) -0.005(6) C57 0.028(6) 0.055(8) 0.060(9) -0.013(7) 0.009(6) -0.007(5) N4 0.028(5) 0.049(6) 0.076(8) -0.009(6) 0.011(5) -0.005(5) C58 0.047(8) 0.054(8) 0.048(8) 0.008(7) 0.015(6) 0.004(6) C59 0.062(9) 0.053(8) 0.064(10) 0.011(7) 0.016(8) -0.020(7) C60 0.034(7) 0.063(9) 0.056(8) 0.019(7) -0.008(6) -0.020(6) C61 0.022(5) 0.072(9) 0.029(6) -0.008(6) 0.004(4) 0.012(5) C62 0.039(5) 0.111(9) 0.105(9) 0.006(7) 0.023(5) 0.032(5) C63 0.039(5) 0.111(9) 0.105(9) 0.006(7) 0.023(5) 0.032(5) C64 0.039(5) 0.111(9) 0.105(9) 0.006(7) 0.023(5) 0.032(5) P1 0.066(3) 0.049(2) 0.099(3) -0.018(2) 0.030(3) 0.002(2) F2 0.066(3) 0.049(2) 0.099(3) -0.018(2) 0.030(3) 0.002(2) F3 0.066(3) 0.049(2) 0.099(3) -0.018(2) 0.030(3) 0.002(2) F4 0.066(3) 0.049(2) 0.099(3) -0.018(2) 0.030(3) 0.002(2) F5 0.066(3) 0.049(2) 0.099(3) -0.018(2) 0.030(3) 0.002(2) F6 0.066(3) 0.049(2) 0.099(3) -0.018(2) 0.030(3) 0.002(2) F1A 0.066(3) 0.049(2) 0.099(3) -0.018(2) 0.030(3) 0.002(2) F2A 0.066(3) 0.049(2) 0.099(3) -0.018(2) 0.030(3) 0.002(2) F3A 0.066(3) 0.049(2) 0.099(3) -0.018(2) 0.030(3) 0.002(2) F4A 0.066(3) 0.049(2) 0.099(3) -0.018(2) 0.030(3) 0.002(2) F5A 0.066(3) 0.049(2) 0.099(3) -0.018(2) 0.030(3) 0.002(2) F6A 0.066(3) 0.049(2) 0.099(3) -0.018(2) 0.030(3) 0.002(2) P2 0.067(3) 0.059(2) 0.143(5) -0.013(3) 0.064(3) -0.020(2) F7 0.103(5) 0.126(5) 0.208(8) -0.004(5) 0.046(5) -0.008(4) F8 0.103(5) 0.126(5) 0.208(8) -0.004(5) 0.046(5) -0.008(4) F9 0.103(5) 0.126(5) 0.208(8) -0.004(5) 0.046(5) -0.008(4) F10 0.103(5) 0.126(5) 0.208(8) -0.004(5) 0.046(5) -0.008(4) F11 0.103(5) 0.126(5) 0.208(8) -0.004(5) 0.046(5) -0.008(4) F12 0.103(5) 0.126(5) 0.208(8) -0.004(5) 0.046(5) -0.008(4) C65 0.076(4) 0.085(4) 0.110(5) -0.028(3) 0.012(3) -0.009(3) Cl1 0.076(4) 0.085(4) 0.110(5) -0.028(3) 0.012(3) -0.009(3) Cl2 0.076(4) 0.085(4) 0.110(5) -0.028(3) 0.012(3) -0.009(3) Cl3 0.076(4) 0.085(4) 0.110(5) -0.028(3) 0.012(3) -0.009(3) C66 0.093(4) 0.072(3) 0.150(6) 0.005(4) 0.069(4) -0.013(3) Cl4 0.093(4) 0.072(3) 0.150(6) 0.005(4) 0.069(4) -0.013(3) Cl5 0.093(4) 0.072(3) 0.150(6) 0.005(4) 0.069(4) -0.013(3) Cl6 0.093(4) 0.072(3) 0.150(6) 0.005(4) 0.069(4) -0.013(3) C67 0.110(5) 0.070(3) 0.103(4) 0.017(3) 0.026(4) 0.009(3) Cl7 0.110(5) 0.070(3) 0.103(4) 0.017(3) 0.026(4) 0.009(3) Cl8 0.110(5) 0.070(3) 0.103(4) 0.017(3) 0.026(4) 0.009(3) Cl9 0.110(5) 0.070(3) 0.103(4) 0.017(3) 0.026(4) 0.009(3) O5 0.063(14) 0.039(10) 0.083(16) -0.027(10) -0.012(12) 0.012(9) C69 0.127(7) 0.122(6) 0.107(5) 0.047(5) -0.028(5) -0.007(5) Cl10 0.127(7) 0.122(6) 0.107(5) 0.047(5) -0.028(5) -0.007(5) Cl11 0.127(7) 0.122(6) 0.107(5) 0.047(5) -0.028(5) -0.007(5) Cl12 0.127(7) 0.122(6) 0.107(5) 0.047(5) -0.028(5) -0.007(5) C30A 0.064(6) 0.111(8) 0.063(6) 0.003(5) 0.036(5) -0.047(6) C32A 0.064(6) 0.111(8) 0.063(6) 0.003(5) 0.036(5) -0.047(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; _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 N1 2.083(10) . ? Ag1 N4 2.124(11) 3_445 ? Ag2 N3 2.136(12) 3_545 ? Ag2 N2 2.137(9) . ? S1 C51 1.719(12) . ? S1 C1 1.778(11) . ? C1 C2 1.373(16) . ? C1 C6 1.432(14) . ? C2 C3 1.387(17) . ? C2 O1 1.389(12) . ? C3 C4 1.402(15) . ? C3 S2 1.748(11) . ? C4 C5 1.409(18) . ? C4 H4 0.9500 . ? C5 C6 1.391(17) . ? C5 C13 1.524(15) . ? C6 H6 0.9500 . ? O1 C7 1.448(13) . ? C7 C8 1.496(15) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C12 1.368(18) . ? C8 C9 1.392(15) . ? C9 N1 1.311(15) . ? C9 H9 0.9500 . ? N1 C10 1.365(19) . ? C10 C11 1.339(19) . ? C10 H10 0.9500 . ? C11 C12 1.425(18) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C16 1.47(3) . ? C13 C15 1.50(3) . ? C13 C14 1.60(2) . ? C14 H14A 0.9801 . ? C14 H14B 0.9802 . ? C14 H14C 0.9801 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? S2 C17 1.776(12) . ? C17 C18 1.390(15) . ? C17 C22 1.398(15) . ? C18 O2 1.362(12) . ? C18 C19 1.389(16) . ? C19 C20 1.408(15) . ? C19 S3 1.775(11) . ? C20 C21 1.403(16) . ? C20 H20 0.9500 . ? C21 C22 1.343(17) . ? C21 C29 1.563(16) . ? C22 H22 0.9500 . ? O2 C23 1.396(15) . ? C23 C24 1.505(16) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.368(16) . ? C24 C28 1.377(16) . ? C25 N2 1.312(16) . ? C25 H25 0.9500 . ? N2 C26 1.349(18) . ? C26 C27 1.414(15) . ? C26 H26 0.9500 . ? C27 C28 1.366(15) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30A 1.493(17) . ? C29 C32 1.523(18) . ? C29 C31 1.561(15) . ? C29 C30 1.585(19) . ? C29 C32A 1.614(18) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? S3 C33 1.783(11) . ? C33 C38 1.372(16) . ? C33 C34 1.401(15) . ? C34 O3 1.364(13) . ? C34 C35 1.434(17) . ? C35 C36 1.335(18) . ? C35 S4 1.748(12) . ? C36 C37 1.428(18) . ? C36 H36 0.9500 . ? C37 C38 1.385(17) . ? C37 C45 1.53(2) . ? C38 H38 0.9500 . ? O3 C39 1.431(16) . ? C39 C40 1.56(2) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C44 1.26(3) . ? C40 C41 1.389(18) . ? C41 N3 1.34(2) . ? C41 H41 0.9500 . ? N3 C42 1.31(2) . ? N3 Ag2 2.136(12) 3_455 ? C42 C43 1.44(2) . ? C42 H42 0.9500 . ? C43 C44 1.36(3) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.45(3) . ? C45 C48 1.50(2) . ? C45 C47 1.56(3) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? S4 C49 1.818(11) . ? C49 C50 1.328(18) . ? C49 C54 1.377(17) . ? C50 O4 1.425(13) . ? C50 C51 1.463(18) . ? C51 C52 1.379(15) . ? C52 C53 1.419(15) . ? C52 H52 0.9500 . ? C53 C54 1.309(18) . ? C53 C61 1.530(15) . ? C54 H54 0.9500 . ? O4 C55 1.432(17) . ? C55 C56 1.49(2) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.38(2) . ? C56 C60 1.39(2) . ? C57 N4 1.339(17) . ? C57 H57 0.9500 . ? N4 C58 1.35(2) . ? N4 Ag1 2.124(11) 3 ? C58 C59 1.35(2) . ? C58 H58 0.9500 . ? C59 C60 1.41(2) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 C64 1.42(3) . ? C61 C63 1.52(2) . ? C61 C62 1.59(3) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? P1 F6 1.620(9) . ? P1 F2A 1.632(10) . ? P1 F1 1.636(9) . ? P1 F4 1.640(9) . ? P1 F5 1.642(9) . ? P1 F2 1.644(9) . ? P1 F3 1.650(9) . ? P1 F6A 1.659(10) . ? P1 F1A 1.662(10) . ? P1 F5A 1.666(10) . ? P1 F3A 1.669(10) . ? P1 F4A 1.680(10) . ? P2 F8 1.636(12) . ? P2 F10 1.647(12) . ? P2 F12 1.663(11) . ? P2 F9 1.675(11) . ? P2 F7 1.722(12) . ? P2 F11 1.735(12) . ? C65 Cl1 1.68(5) . ? C65 Cl3 1.70(4) . ? C65 Cl2 1.87(5) . ? C65 H65 1.0000 . ? C66 Cl6 1.74(4) . ? C66 Cl4 1.87(5) . ? C66 Cl5 1.94(5) . ? C66 H66 1.0000 . ? C67 Cl8 1.48(4) . ? C67 Cl7 1.65(5) . ? C67 Cl9 1.99(5) . ? C67 H67 1.0000 . ? C69 Cl12 1.71(2) . ? C69 Cl11 1.71(2) . ? C69 Cl10 1.76(2) . ? C69 H69 1.0000 . ? C30A H30D 0.9800 . ? C30A H30E 0.9800 . ? C30A H30F 0.9800 . ? C32A H32D 0.9800 . ? C32A H32E 0.9800 . ? C32A H32F 0.9800 . ? _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 N1 Ag1 N4 167.1(5) . 3_445 ? N3 Ag2 N2 171.6(5) 3_545 . ? C51 S1 C1 107.9(5) . . ? C2 C1 C6 119.3(10) . . ? C2 C1 S1 124.8(8) . . ? C6 C1 S1 114.7(8) . . ? C1 C2 C3 121.4(10) . . ? C1 C2 O1 119.2(10) . . ? C3 C2 O1 119.3(10) . . ? C2 C3 C4 119.0(10) . . ? C2 C3 S2 125.5(8) . . ? C4 C3 S2 114.5(9) . . ? C3 C4 C5 121.5(11) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C6 C5 C4 118.2(10) . . ? C6 C5 C13 120.7(11) . . ? C4 C5 C13 121.0(11) . . ? C5 C6 C1 120.4(11) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? C2 O1 C7 110.6(9) . . ? O1 C7 C8 108.7(9) . . ? O1 C7 H7A 110.0 . . ? C8 C7 H7A 110.0 . . ? O1 C7 H7B 110.0 . . ? C8 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? C12 C8 C9 118.0(10) . . ? C12 C8 C7 124.2(10) . . ? C9 C8 C7 117.7(10) . . ? N1 C9 C8 125.7(11) . . ? N1 C9 H9 117.2 . . ? C8 C9 H9 117.2 . . ? C9 N1 C10 114.7(10) . . ? C9 N1 Ag1 117.5(9) . . ? C10 N1 Ag1 127.5(8) . . ? C11 C10 N1 125.6(11) . . ? C11 C10 H10 117.2 . . ? N1 C10 H10 117.2 . . ? C10 C11 C12 117.7(12) . . ? C10 C11 H11 121.1 . . ? C12 C11 H11 121.1 . . ? C8 C12 C11 118.2(10) . . ? C8 C12 H12 120.9 . . ? C11 C12 H12 120.9 . . ? C16 C13 C15 109.7(12) . . ? C16 C13 C5 111.0(12) . . ? C15 C13 C5 108.2(12) . . ? C16 C13 C14 96.0(17) . . ? C15 C13 C14 115.9(17) . . ? C5 C13 C14 115.5(11) . . ? C3 S2 C17 107.7(5) . . ? C18 C17 C22 119.9(10) . . ? C18 C17 S2 121.4(8) . . ? C22 C17 S2 117.9(9) . . ? O2 C18 C19 118.9(9) . . ? O2 C18 C17 122.9(9) . . ? C19 C18 C17 118.2(9) . . ? C18 C19 C20 120.3(10) . . ? C18 C19 S3 122.7(8) . . ? C20 C19 S3 116.6(8) . . ? C21 C20 C19 120.7(10) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C22 C21 C20 117.5(10) . . ? C22 C21 C29 122.4(11) . . ? C20 C21 C29 119.9(11) . . ? C21 C22 C17 123.2(11) . . ? C21 C22 H22 118.4 . . ? C17 C22 H22 118.4 . . ? C18 O2 C23 117.3(8) . . ? O2 C23 C24 109.1(10) . . ? O2 C23 H23A 109.9 . . ? C24 C23 H23A 109.9 . . ? O2 C23 H23B 109.9 . . ? C24 C23 H23B 109.9 . . ? H23A C23 H23B 108.3 . . ? C25 C24 C28 117.1(10) . . ? C25 C24 C23 120.2(11) . . ? C28 C24 C23 122.7(10) . . ? N2 C25 C24 125.2(12) . . ? N2 C25 H25 117.4 . . ? C24 C25 H25 117.4 . . ? C25 N2 C26 118.1(10) . . ? C25 N2 Ag2 120.2(8) . . ? C26 N2 Ag2 121.2(8) . . ? N2 C26 C27 120.4(11) . . ? N2 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C28 C27 C26 118.8(12) . . ? C28 C27 H27 120.6 . . ? C26 C27 H27 120.6 . . ? C27 C28 C24 120.1(11) . . ? C27 C28 H28 119.9 . . ? C24 C28 H28 119.9 . . ? C30A C29 C31 116.0(14) . . ? C32 C29 C31 112.0(14) . . ? C30A C29 C21 112.6(14) . . ? C32 C29 C21 119(2) . . ? C31 C29 C21 109.3(10) . . ? C32 C29 C30 109.4(15) . . ? C31 C29 C30 107.3(13) . . ? C21 C29 C30 99.2(18) . . ? C30A C29 C32A 108.8(13) . . ? C31 C29 C32A 103.2(13) . . ? C21 C29 C32A 106.1(13) . . ? C30 C29 C32A 130.8(17) . . ? C19 S3 C33 107.4(5) . . ? C38 C33 C34 120.2(10) . . ? C38 C33 S3 116.3(8) . . ? C34 C33 S3 122.5(8) . . ? O3 C34 C33 121.5(10) . . ? O3 C34 C35 120.5(10) . . ? C33 C34 C35 117.5(10) . . ? C36 C35 C34 119.0(11) . . ? C36 C35 S4 118.8(9) . . ? C34 C35 S4 121.5(10) . . ? C35 C36 C37 124.9(12) . . ? C35 C36 H36 117.5 . . ? C37 C36 H36 117.6 . . ? C38 C37 C36 114.0(10) . . ? C38 C37 C45 123.9(12) . . ? C36 C37 C45 122.1(12) . . ? C33 C38 C37 123.7(11) . . ? C33 C38 H38 118.2 . . ? C37 C38 H38 118.2 . . ? C34 O3 C39 113.3(9) . . ? O3 C39 C40 112.8(13) . . ? O3 C39 H39A 109.0 . . ? C40 C39 H39A 109.0 . . ? O3 C39 H39B 109.0 . . ? C40 C39 H39B 109.0 . . ? H39A C39 H39B 107.8 . . ? C44 C40 C41 119.6(16) . . ? C44 C40 C39 123.0(14) . . ? C41 C40 C39 117.4(14) . . ? N3 C41 C40 119.9(15) . . ? N3 C41 H41 120.1 . . ? C40 C41 H41 120.1 . . ? C42 N3 C41 120.1(13) . . ? C42 N3 Ag2 117.7(11) . 3_455 ? C41 N3 Ag2 122.2(10) . 3_455 ? N3 C42 C43 120.2(17) . . ? N3 C42 H42 119.9 . . ? C43 C42 H42 119.9 . . ? C44 C43 C42 115(2) . . ? C44 C43 H43 122.6 . . ? C42 C43 H43 122.6 . . ? C40 C44 C43 122.7(18) . . ? C40 C44 H44 118.7 . . ? C43 C44 H44 118.6 . . ? C46 C45 C48 110.3(17) . . ? C46 C45 C37 107.8(14) . . ? C48 C45 C37 109.9(14) . . ? C46 C45 C47 100.7(15) . . ? C48 C45 C47 110.3(15) . . ? C37 C45 C47 117.3(14) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.4 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.4 . . ? 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 109.4 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C35 S4 C49 105.5(5) . . ? C50 C49 C54 121.6(11) . . ? C50 C49 S4 121.2(10) . . ? C54 C49 S4 116.7(9) . . ? C49 C50 O4 124.1(11) . . ? C49 C50 C51 119.4(10) . . ? O4 C50 C51 116.5(11) . . ? C52 C51 C50 115.4(10) . . ? C52 C51 S1 121.1(9) . . ? C50 C51 S1 122.4(9) . . ? C51 C52 C53 122.9(11) . . ? C51 C52 H52 118.6 . . ? C53 C52 H52 118.5 . . ? C54 C53 C52 117.5(10) . . ? C54 C53 C61 123.5(10) . . ? C52 C53 C61 118.8(10) . . ? C53 C54 C49 122.7(11) . . ? C53 C54 H54 118.6 . . ? C49 C54 H54 118.7 . . ? C50 O4 C55 107.2(9) . . ? O4 C55 C56 108.0(11) . . ? O4 C55 H55A 110.1 . . ? C56 C55 H55A 110.1 . . ? O4 C55 H55B 110.1 . . ? C56 C55 H55B 110.1 . . ? H55A C55 H55B 108.4 . . ? C57 C56 C60 116.3(13) . . ? C57 C56 C55 118.9(15) . . ? C60 C56 C55 124.7(13) . . ? N4 C57 C56 124.3(14) . . ? N4 C57 H57 117.9 . . ? C56 C57 H57 117.9 . . ? C57 N4 C58 117.4(12) . . ? C57 N4 Ag1 119.9(10) . 3 ? C58 N4 Ag1 121.9(9) . 3 ? N4 C58 C59 123.7(15) . . ? N4 C58 H58 118.2 . . ? C59 C58 H58 118.2 . . ? C58 C59 C60 117.8(16) . . ? C58 C59 H59 121.1 . . ? C60 C59 H59 121.1 . . ? C56 C60 C59 120.4(13) . . ? C56 C60 H60 119.8 . . ? C59 C60 H60 119.8 . . ? C64 C61 C63 109.9(14) . . ? C64 C61 C53 112.9(11) . . ? C63 C61 C53 109.4(11) . . ? C64 C61 C62 107.3(15) . . ? C63 C61 C62 106.4(14) . . ? C53 C61 C62 110.7(11) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.4 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? F6 P1 F2A 101.0(12) . . ? F6 P1 F1 92.6(8) . . ? F6 P1 F4 91.6(8) . . ? F2A P1 F4 145.3(12) . . ? F1 P1 F4 175.5(9) . . ? F6 P1 F5 89.8(8) . . ? F2A P1 F5 58.7(11) . . ? F1 P1 F5 89.0(8) . . ? F4 P1 F5 89.5(8) . . ? F6 P1 F2 91.5(8) . . ? F2A P1 F2 119.7(11) . . ? F1 P1 F2 89.6(8) . . ? F4 P1 F2 91.8(8) . . ? F5 P1 F2 178.1(9) . . ? F6 P1 F3 177.3(10) . . ? F2A P1 F3 78.2(12) . . ? F1 P1 F3 88.0(8) . . ? F4 P1 F3 87.7(8) . . ? F5 P1 F3 87.6(8) . . ? F2 P1 F3 91.1(8) . . ? F2A P1 F6A 91.6(9) . . ? F2A P1 F1A 88.9(9) . . ? F1 P1 F1A 116.3(11) . . ? F6A P1 F1A 91.3(9) . . ? F2A P1 F5A 179.1(11) . . ? F6A P1 F5A 89.3(9) . . ? F1A P1 F5A 91.4(9) . . ? F2A P1 F3A 89.9(10) . . ? F6A P1 F3A 177.3(11) . . ? F1A P1 F3A 91.1(10) . . ? F5A P1 F3A 89.2(10) . . ? F2A P1 F4A 89.3(9) . . ? F6A P1 F4A 88.7(9) . . ? F1A P1 F4A 178.2(11) . . ? F5A P1 F4A 90.4(9) . . ? F3A P1 F4A 89.0(9) . . ? F8 P2 F10 98.1(8) . . ? F8 P2 F12 91.2(7) . . ? F10 P2 F12 92.7(7) . . ? F8 P2 F9 91.1(7) . . ? F10 P2 F9 89.0(8) . . ? F12 P2 F9 177.0(9) . . ? F8 P2 F7 88.8(7) . . ? F10 P2 F7 173.1(8) . . ? F12 P2 F7 87.6(7) . . ? F9 P2 F7 90.4(7) . . ? F8 P2 F11 175.3(9) . . ? F10 P2 F11 86.5(7) . . ? F12 P2 F11 88.0(7) . . ? F9 P2 F11 89.6(7) . . ? F7 P2 F11 86.6(7) . . ? Cl1 C65 Cl3 117(3) . . ? Cl1 C65 Cl2 107(3) . . ? Cl3 C65 Cl2 114(3) . . ? Cl1 C65 H65 106.1 . . ? Cl3 C65 H65 106.1 . . ? Cl2 C65 H65 106.1 . . ? Cl6 C66 Cl4 110(2) . . ? Cl6 C66 Cl5 97(2) . . ? Cl4 C66 Cl5 144(3) . . ? Cl6 C66 H66 99.7 . . ? Cl4 C66 H66 99.7 . . ? Cl5 C66 H66 99.7 . . ? Cl8 C67 Cl7 141(4) . . ? Cl8 C67 Cl9 101(3) . . ? Cl7 C67 Cl9 103(2) . . ? Cl8 C67 H67 102.4 . . ? Cl7 C67 H67 102.4 . . ? Cl9 C67 H67 102.4 . . ? Cl12 C69 Cl11 97.8(15) . . ? Cl12 C69 Cl10 112.4(19) . . ? Cl11 C69 Cl10 120(2) . . ? Cl12 C69 H69 108.6 . . ? Cl11 C69 H69 108.6 . . ? Cl10 C69 H69 108.6 . . ? H30D C30A H30E 109.5 . . ? H30D C30A H30F 109.5 . . ? H30E C30A H30F 109.5 . . ? H32D C32A H32E 109.5 . . ? H32D C32A H32F 109.5 . . ? H32E C32A H32F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.276 _refine_diff_density_min -1.047 _refine_diff_density_rms 0.233 data_e2323a _database_code_depnum_ccdc_archive 'CCDC 895675' #TrackingRef 'web_deposit_cif_file_7_SylvieFERLAY_1344596913.3-AgSbF6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C548 H584 Ag16 Cl108 F96 N32 O32 S32 Sb16' _chemical_formula_weight 18482.91 _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' F F 0.0171 0.0103 '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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' _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 27.5820(9) _cell_length_b 28.4143(7) _cell_length_c 25.5819(9) _cell_angle_alpha 90.00 _cell_angle_beta 108.6540(10) _cell_angle_gamma 90.00 _cell_volume 18995.9(10) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9945 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 23.23 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9132 _exptl_absorpt_coefficient_mu 1.504 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8766 _exptl_absorpt_correction_T_max 0.9152 _exptl_absorpt_process_details sadabs _exptl_special_details ; Because of the flopiness of the tertiobutyl group and the F of the SbF6 the EADP command was used ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 202931 _diffrn_reflns_av_R_equivalents 0.1033 _diffrn_reflns_av_sigmaI/netI 0.1350 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 29.30 _reflns_number_total 51700 _reflns_number_gt 20984 _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. ; _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^)+(0.1788P)^2^+0.5448P] 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 51700 _refine_ls_number_parameters 2045 _refine_ls_number_restraints 112 _refine_ls_R_factor_all 0.2189 _refine_ls_R_factor_gt 0.0952 _refine_ls_wR_factor_ref 0.3034 _refine_ls_wR_factor_gt 0.2503 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.162 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.062 _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 0.02284(4) 0.24395(3) 0.34136(4) 0.0424(2) Uani 1 1 d . . . Ag2 Ag 0.25217(3) 0.72797(3) 0.25738(4) 0.0441(2) Uani 1 1 d . . . Ag3 Ag 0.24841(3) 0.22738(3) 0.24825(3) 0.0359(2) Uani 1 1 d . . . Ag4 Ag 0.47012(4) 0.21259(3) 0.14638(4) 0.0462(2) Uani 1 1 d . . . S1 S 0.06948(10) 0.46719(9) 0.06007(10) 0.0311(6) Uani 1 1 d . . . C1 C 0.0324(4) 0.4543(3) 0.1039(4) 0.026(2) Uani 1 1 d . . . C2 C 0.0202(4) 0.4891(3) 0.1359(4) 0.028(2) Uani 1 1 d . . . C3 C -0.0092(4) 0.4773(4) 0.1689(4) 0.029(2) Uani 1 1 d . . . C4 C -0.0300(4) 0.4322(3) 0.1657(4) 0.031(2) Uani 1 1 d . . . H4 H -0.0507 0.4247 0.1879 0.038 Uiso 1 1 calc R . . C5 C -0.0215(4) 0.3982(3) 0.1310(4) 0.030(2) Uani 1 1 d . . . C6 C 0.0119(4) 0.4104(3) 0.1019(4) 0.026(2) Uani 1 1 d . . . H6 H 0.0206 0.3871 0.0798 0.031 Uiso 1 1 calc R . . O1 O 0.0345(2) 0.5362(2) 0.1329(3) 0.0269(15) Uani 1 1 d . . . C7 C -0.0061(4) 0.5592(4) 0.0916(4) 0.039(3) Uani 1 1 d . . . H7A H -0.0382 0.5571 0.1009 0.047 Uiso 1 1 calc R . . H7B H -0.0117 0.5440 0.0553 0.047 Uiso 1 1 calc R . . C8 C 0.0089(4) 0.6103(3) 0.0892(4) 0.030(2) Uani 1 1 d . . . C9 C -0.0078(4) 0.6446(4) 0.1177(4) 0.033(2) Uani 1 1 d . . . H9 H -0.0298 0.6355 0.1379 0.040 Uiso 1 1 calc R . . N1 N 0.0054(3) 0.6899(3) 0.1183(3) 0.033(2) Uani 1 1 d . . . C10 C 0.0366(5) 0.7024(4) 0.0892(5) 0.040(3) Uani 1 1 d . . . H10 H 0.0477 0.7342 0.0908 0.048 Uiso 1 1 calc R . . C11 C 0.0530(5) 0.6710(4) 0.0572(5) 0.051(3) Uani 1 1 d . . . H11 H 0.0730 0.6812 0.0353 0.061 Uiso 1 1 calc R . . C12 C 0.0392(5) 0.6242(4) 0.0582(5) 0.045(3) Uani 1 1 d . . . H12 H 0.0507 0.6015 0.0374 0.054 Uiso 1 1 calc R . . C13 C -0.0514(4) 0.3516(3) 0.1207(4) 0.030(2) Uani 1 1 d . . . C14 C -0.0641(6) 0.3361(4) 0.1719(5) 0.059(4) Uani 1 1 d . . . H14A H -0.0862 0.3597 0.1808 0.089 Uiso 1 1 calc R . . H14B H -0.0325 0.3328 0.2030 0.089 Uiso 1 1 calc R . . H14C H -0.0820 0.3058 0.1647 0.089 Uiso 1 1 calc R . . C15 C -0.1011(5) 0.3580(4) 0.0741(6) 0.058(4) Uani 1 1 d . . . H15A H -0.1207 0.3286 0.0683 0.086 Uiso 1 1 calc R . . H15B H -0.0938 0.3665 0.0403 0.086 Uiso 1 1 calc R . . H15C H -0.1211 0.3831 0.0837 0.086 Uiso 1 1 calc R . . C16 C -0.0207(5) 0.3118(4) 0.1034(6) 0.057(4) Uani 1 1 d . . . H16A H -0.0416 0.2832 0.0945 0.085 Uiso 1 1 calc R . . H16B H 0.0107 0.3053 0.1338 0.085 Uiso 1 1 calc R . . H16C H -0.0119 0.3219 0.0709 0.085 Uiso 1 1 calc R . . S2 S -0.02920(10) 0.51969(9) 0.20841(11) 0.0340(6) Uani 1 1 d . . . C17 C 0.0273(4) 0.5413(3) 0.2588(4) 0.027(2) Uani 1 1 d . . . C18 C 0.0652(4) 0.5112(3) 0.2910(4) 0.025(2) Uani 1 1 d . . . C19 C 0.1035(4) 0.5306(3) 0.3363(4) 0.025(2) Uani 1 1 d . . . C20 C 0.1025(4) 0.5778(3) 0.3486(4) 0.035(2) Uani 1 1 d . . . H20 H 0.1282 0.5903 0.3797 0.042 Uiso 1 1 calc R . . C21 C 0.0641(4) 0.6079(3) 0.3159(4) 0.032(2) Uani 1 1 d . . . C22 C 0.0268(4) 0.5881(3) 0.2723(4) 0.027(2) Uani 1 1 d . . . H22 H -0.0003 0.6075 0.2507 0.033 Uiso 1 1 calc R . . O2 O 0.0668(3) 0.4647(2) 0.2770(3) 0.0292(15) Uani 1 1 d . . . C23 C 0.0449(4) 0.4327(3) 0.3054(5) 0.036(2) Uani 1 1 d . . . H23A H 0.0073 0.4373 0.2940 0.043 Uiso 1 1 calc R . . H23B H 0.0591 0.4380 0.3456 0.043 Uiso 1 1 calc R . . C24 C 0.0568(4) 0.3841(3) 0.2918(4) 0.031(2) Uani 1 1 d . . . C25 C 0.0394(4) 0.3459(3) 0.3146(4) 0.029(2) Uani 1 1 d . . . H25 H 0.0196 0.3514 0.3383 0.035 Uiso 1 1 calc R . . N2 N 0.0500(3) 0.3008(3) 0.3040(4) 0.033(2) Uani 1 1 d . . . C26 C 0.0768(4) 0.2925(4) 0.2696(4) 0.038(3) Uani 1 1 d . . . H26 H 0.0826 0.2610 0.2608 0.046 Uiso 1 1 calc R . . C27 C 0.0957(4) 0.3287(4) 0.2471(4) 0.037(2) Uani 1 1 d . . . H27 H 0.1163 0.3218 0.2245 0.044 Uiso 1 1 calc R . . C28 C 0.0858(4) 0.3750(4) 0.2562(4) 0.035(2) Uani 1 1 d . . . H28 H 0.0980 0.4000 0.2391 0.042 Uiso 1 1 calc R . . C29 C 0.0635(4) 0.6599(4) 0.3325(5) 0.041(3) Uani 1 1 d . . . C30 C 0.1169(5) 0.6794(4) 0.3601(6) 0.059(4) Uani 1 1 d . . . H30A H 0.1147 0.7132 0.3665 0.089 Uiso 1 1 calc R . . H30B H 0.1379 0.6742 0.3361 0.089 Uiso 1 1 calc R . . H30C H 0.1325 0.6634 0.3954 0.089 Uiso 1 1 calc R . . C31 C 0.0333(6) 0.6643(4) 0.3720(6) 0.068(4) Uani 1 1 d . . . H31A H 0.0565 0.6621 0.4100 0.102 Uiso 1 1 calc R . . H31B H 0.0080 0.6389 0.3652 0.102 Uiso 1 1 calc R . . H31C H 0.0157 0.6947 0.3666 0.102 Uiso 1 1 calc R . . C32 C 0.0372(5) 0.6913(4) 0.2811(5) 0.049(3) Uani 1 1 d . . . H32A H 0.0010 0.6828 0.2659 0.074 Uiso 1 1 calc R . . H32B H 0.0540 0.6864 0.2531 0.074 Uiso 1 1 calc R . . H32C H 0.0402 0.7245 0.2922 0.074 Uiso 1 1 calc R . . S3 S 0.14954(12) 0.49586(9) 0.38496(10) 0.0385(7) Uani 1 1 d . . . C33 C 0.1763(4) 0.4550(3) 0.3500(4) 0.028(2) Uani 1 1 d . . . C34 C 0.1911(4) 0.4653(3) 0.3048(4) 0.027(2) Uani 1 1 d . . . C35 C 0.2183(3) 0.4329(3) 0.2846(4) 0.027(2) Uani 1 1 d . . . C36 C 0.2317(4) 0.3899(3) 0.3106(4) 0.028(2) Uani 1 1 d . . . H36 H 0.2506 0.3680 0.2967 0.033 Uiso 1 1 calc R . . C37 C 0.2178(4) 0.3782(3) 0.3569(4) 0.027(2) Uani 1 1 d . . . C38 C 0.1904(4) 0.4114(3) 0.3755(4) 0.028(2) Uani 1 1 d . . . H38 H 0.1808 0.4041 0.4070 0.033 Uiso 1 1 calc R . . O3 O 0.1772(3) 0.5085(2) 0.2779(3) 0.0300(15) Uani 1 1 d . . . C39 C 0.2125(4) 0.5455(3) 0.2993(4) 0.035(2) Uani 1 1 d . . . H39A H 0.2456 0.5384 0.2936 0.042 Uiso 1 1 calc R . . H39B H 0.2185 0.5492 0.3393 0.042 Uiso 1 1 calc R . . C40 C 0.1903(4) 0.5896(4) 0.2696(4) 0.033(2) Uani 1 1 d . . . C41 C 0.2185(4) 0.6308(4) 0.2791(4) 0.036(2) Uani 1 1 d . . . H41 H 0.2521 0.6296 0.3048 0.043 Uiso 1 1 calc R . . N3 N 0.2024(3) 0.6721(3) 0.2552(4) 0.039(2) Uani 1 1 d . . . C42 C 0.1537(5) 0.6729(4) 0.2191(5) 0.046(3) Uani 1 1 d . . . H42 H 0.1405 0.7017 0.2012 0.055 Uiso 1 1 calc R . . C43 C 0.1229(4) 0.6333(4) 0.2075(5) 0.040(3) Uani 1 1 d . . . H43 H 0.0890 0.6351 0.1825 0.048 Uiso 1 1 calc R . . C44 C 0.1418(4) 0.5913(4) 0.2322(4) 0.035(2) Uani 1 1 d . . . H44 H 0.1214 0.5636 0.2236 0.042 Uiso 1 1 calc R . . C45 C 0.2349(4) 0.3323(4) 0.3888(4) 0.033(2) Uani 1 1 d . . . C46 C 0.1911(6) 0.3114(4) 0.4056(6) 0.063(4) Uani 1 1 d . . . H46A H 0.1771 0.3356 0.4241 0.095 Uiso 1 1 calc R . . H46B H 0.2040 0.2850 0.4309 0.095 Uiso 1 1 calc R . . H46C H 0.1642 0.3003 0.3727 0.095 Uiso 1 1 calc R . . C47 C 0.2807(6) 0.3453(5) 0.4416(6) 0.072(5) Uani 1 1 d . . . H47A H 0.3090 0.3580 0.4305 0.107 Uiso 1 1 calc R . . H47B H 0.2922 0.3170 0.4641 0.107 Uiso 1 1 calc R . . H47C H 0.2695 0.3689 0.4631 0.107 Uiso 1 1 calc R . . C48 C 0.2522(7) 0.2967(4) 0.3535(6) 0.071(5) Uani 1 1 d . . . H48A H 0.2251 0.2929 0.3179 0.107 Uiso 1 1 calc R . . H48B H 0.2590 0.2663 0.3726 0.107 Uiso 1 1 calc R . . H48C H 0.2834 0.3080 0.3473 0.107 Uiso 1 1 calc R . . S4 S 0.24936(10) 0.44571(11) 0.23497(11) 0.0393(7) Uani 1 1 d . . . C49 C 0.2053(4) 0.4785(4) 0.1817(4) 0.033(2) Uani 1 1 d . . . C50 C 0.1594(4) 0.4603(4) 0.1490(4) 0.029(2) Uani 1 1 d . . . C51 C 0.1287(4) 0.4882(3) 0.1053(4) 0.024(2) Uani 1 1 d . . . C52 C 0.1472(4) 0.5295(3) 0.0922(4) 0.029(2) Uani 1 1 d . . . H52 H 0.1264 0.5467 0.0613 0.035 Uiso 1 1 calc R . . C53 C 0.1955(4) 0.5481(4) 0.1220(4) 0.033(2) Uani 1 1 d . . . C54 C 0.2236(4) 0.5226(4) 0.1696(4) 0.033(2) Uani 1 1 d . . . H54 H 0.2549 0.5349 0.1934 0.040 Uiso 1 1 calc R . . O4 O 0.1448(3) 0.4151(2) 0.1570(3) 0.0289(15) Uani 1 1 d . . . C55 C 0.1649(5) 0.3833(4) 0.1245(5) 0.040(3) Uani 1 1 d . . . H55A H 0.2021 0.3887 0.1332 0.048 Uiso 1 1 calc R . . H55B H 0.1482 0.3899 0.0848 0.048 Uiso 1 1 calc R . . C56 C 0.1556(4) 0.3341(3) 0.1361(4) 0.030(2) Uani 1 1 d . . . C57 C 0.1930(4) 0.3093(3) 0.1760(4) 0.030(2) Uani 1 1 d . . . H57 H 0.2236 0.3254 0.1957 0.037 Uiso 1 1 calc R . . N4 N 0.1883(3) 0.2640(3) 0.1884(3) 0.0302(19) Uani 1 1 d . . . C58 C 0.1453(4) 0.2410(4) 0.1574(5) 0.041(3) Uani 1 1 d . . . H58 H 0.1420 0.2084 0.1634 0.049 Uiso 1 1 calc R . . C59 C 0.1066(4) 0.2637(4) 0.1177(5) 0.043(3) Uani 1 1 d . . . H59 H 0.0761 0.2473 0.0987 0.052 Uiso 1 1 calc R . . C60 C 0.1123(5) 0.3103(4) 0.1056(5) 0.044(3) Uani 1 1 d . . . H60 H 0.0867 0.3257 0.0768 0.053 Uiso 1 1 calc R . . C61 C 0.2192(4) 0.5910(4) 0.1038(4) 0.035(2) Uani 1 1 d . . . C62 C 0.2537(10) 0.5730(7) 0.0736(10) 0.035(2) Uani 1 1 d . . . H62A H 0.2725 0.5993 0.0646 0.047 Uiso 1 1 calc R . . H62B H 0.2332 0.5574 0.0395 0.047 Uiso 1 1 calc R . . H62C H 0.2779 0.5504 0.0969 0.047 Uiso 1 1 calc R . . C63 C 0.1803(6) 0.6224(6) 0.0666(9) 0.035(2) Uani 1 1 d . . . H63A H 0.1634 0.6407 0.0883 0.047 Uiso 1 1 calc R . . H63B H 0.1548 0.6034 0.0392 0.047 Uiso 1 1 calc R . . H63C H 0.1970 0.6439 0.0477 0.047 Uiso 1 1 calc R . . C64 C 0.2493(9) 0.6204(7) 0.1515(7) 0.035(2) Uani 1 1 d . . . H64A H 0.2561 0.6512 0.1382 0.047 Uiso 1 1 calc R . . H64B H 0.2818 0.6047 0.1706 0.047 Uiso 1 1 calc R . . H64C H 0.2298 0.6246 0.1772 0.047 Uiso 1 1 calc R . . S5 S 0.43513(10) -0.00885(9) 0.44404(10) 0.0319(6) Uani 1 1 d . . . C65 C 0.3750(4) -0.0285(3) 0.4004(4) 0.027(2) Uani 1 1 d . . . C66 C 0.3431(4) -0.0019(3) 0.3572(4) 0.025(2) Uani 1 1 d . . . C67 C 0.2955(4) -0.0192(3) 0.3257(4) 0.028(2) Uani 1 1 d . . . C68 C 0.2785(4) -0.0622(3) 0.3406(4) 0.032(2) Uani 1 1 d . . . H68 H 0.2464 -0.0743 0.3183 0.038 Uiso 1 1 calc R . . C69 C 0.3061(4) -0.0876(4) 0.3857(4) 0.033(2) Uani 1 1 d . . . C70 C 0.3561(4) -0.0712(3) 0.4141(4) 0.032(2) Uani 1 1 d . . . H70 H 0.3777 -0.0896 0.4433 0.039 Uiso 1 1 calc R . . O5 O 0.3578(3) 0.0433(2) 0.3484(3) 0.0266(14) Uani 1 1 d . . . C71 C 0.3396(5) 0.0760(3) 0.3807(5) 0.041(3) Uani 1 1 d . . . H71A H 0.3588 0.0716 0.4204 0.049 Uiso 1 1 calc R . . H71B H 0.3029 0.0701 0.3752 0.049 Uiso 1 1 calc R . . C72 C 0.3467(5) 0.1250(4) 0.3638(5) 0.038(3) Uani 1 1 d . . . C73 C 0.3072(4) 0.1479(3) 0.3238(4) 0.029(2) Uani 1 1 d . . . H73 H 0.2766 0.1310 0.3062 0.035 Uiso 1 1 calc R . . N5 N 0.3106(3) 0.1934(3) 0.3089(3) 0.033(2) Uani 1 1 d . . . C74 C 0.3530(4) 0.2167(4) 0.3347(5) 0.039(3) Uani 1 1 d . . . H74 H 0.3548 0.2490 0.3260 0.047 Uiso 1 1 calc R . . C75 C 0.3946(5) 0.1967(5) 0.3736(5) 0.056(4) Uani 1 1 d . . . H75 H 0.4253 0.2140 0.3891 0.068 Uiso 1 1 calc R . . C76 C 0.3906(5) 0.1522(4) 0.3888(5) 0.052(3) Uani 1 1 d . . . H76 H 0.4182 0.1387 0.4174 0.063 Uiso 1 1 calc R . . C77 C 0.2859(7) -0.1297(6) 0.4060(8) 0.087(3) Uani 1 1 d . . . C78 C 0.2662(7) -0.1142(5) 0.4515(7) 0.087(3) Uani 1 1 d . . . H78A H 0.2857 -0.0867 0.4701 0.130 Uiso 1 1 calc R . . H78B H 0.2701 -0.1398 0.4781 0.130 Uiso 1 1 calc R . . H78C H 0.2299 -0.1058 0.4359 0.130 Uiso 1 1 calc R . . C79 C 0.3297(7) -0.1673(5) 0.4320(7) 0.087(3) Uani 1 1 d . . . H79A H 0.3182 -0.1985 0.4164 0.130 Uiso 1 1 calc R . . H79B H 0.3372 -0.1682 0.4721 0.130 Uiso 1 1 calc R . . H79C H 0.3607 -0.1585 0.4234 0.130 Uiso 1 1 calc R . . C80 C 0.2420(7) -0.1535(5) 0.3593(7) 0.087(3) Uani 1 1 d . . . H80A H 0.2141 -0.1309 0.3445 0.130 Uiso 1 1 calc R . . H80B H 0.2292 -0.1808 0.3742 0.130 Uiso 1 1 calc R . . H80C H 0.2550 -0.1637 0.3297 0.130 Uiso 1 1 calc R . . S6 S 0.25135(10) 0.01425(10) 0.27356(11) 0.0359(6) Uani 1 1 d . . . C81 C 0.2780(4) 0.0229(3) 0.2196(4) 0.028(2) Uani 1 1 d . . . C82 C 0.3036(4) -0.0105(3) 0.1999(4) 0.0228(19) Uani 1 1 d . . . C83 C 0.3156(4) -0.0020(3) 0.1514(4) 0.028(2) Uani 1 1 d . . . C84 C 0.3006(4) 0.0393(3) 0.1230(4) 0.031(2) Uani 1 1 d . . . H84 H 0.3080 0.0443 0.0896 0.038 Uiso 1 1 calc R . . C85 C 0.2746(4) 0.0743(3) 0.1420(4) 0.032(2) Uani 1 1 d . . . C86 C 0.2634(4) 0.0655(3) 0.1903(4) 0.025(2) Uani 1 1 d . . . H86 H 0.2456 0.0886 0.2039 0.030 Uiso 1 1 calc R . . O6 O 0.3199(2) -0.0514(2) 0.2295(3) 0.0271(15) Uani 1 1 d . . . C87 C 0.2843(4) -0.0898(3) 0.2103(4) 0.036(2) Uani 1 1 d . . . H87A H 0.2768 -0.0945 0.1701 0.043 Uiso 1 1 calc R . . H87B H 0.2518 -0.0832 0.2176 0.043 Uiso 1 1 calc R . . C88 C 0.3098(4) -0.1336(3) 0.2419(4) 0.032(2) Uani 1 1 d . . . C89 C 0.2821(4) -0.1748(4) 0.2345(5) 0.039(3) Uani 1 1 d . . . H89 H 0.2479 -0.1747 0.2101 0.047 Uiso 1 1 calc R . . N6 N 0.3014(4) -0.2150(3) 0.2602(4) 0.040(2) Uani 1 1 d . . . C90 C 0.3508(5) -0.2150(4) 0.2929(5) 0.044(3) Uani 1 1 d . . . H90 H 0.3658 -0.2438 0.3093 0.053 Uiso 1 1 calc R . . C91 C 0.3798(4) -0.1754(4) 0.3031(5) 0.040(3) Uani 1 1 d . . . H91 H 0.4137 -0.1763 0.3280 0.049 Uiso 1 1 calc R . . C92 C 0.3598(4) -0.1341(3) 0.2773(4) 0.030(2) Uani 1 1 d . . . H92 H 0.3800 -0.1063 0.2836 0.036 Uiso 1 1 calc R . . C93 C 0.2565(4) 0.1194(4) 0.1073(4) 0.036(2) Uani 1 1 d . . . C94 C 0.2353(6) 0.1553(5) 0.1392(6) 0.066(4) Uani 1 1 d . . . H94A H 0.2029 0.1435 0.1425 0.099 Uiso 1 1 calc R . . H94B H 0.2293 0.1853 0.1194 0.099 Uiso 1 1 calc R . . H94C H 0.2600 0.1598 0.1761 0.099 Uiso 1 1 calc R . . C95 C 0.2143(5) 0.1044(4) 0.0530(5) 0.056(4) Uani 1 1 d . . . H95A H 0.1878 0.0864 0.0621 0.083 Uiso 1 1 calc R . . H95B H 0.2296 0.0847 0.0309 0.083 Uiso 1 1 calc R . . H95C H 0.1991 0.1325 0.0319 0.083 Uiso 1 1 calc R . . C96 C 0.3006(5) 0.1417(4) 0.0924(5) 0.049(3) Uani 1 1 d . . . H96A H 0.2882 0.1694 0.0690 0.073 Uiso 1 1 calc R . . H96B H 0.3146 0.1188 0.0723 0.073 Uiso 1 1 calc R . . H96C H 0.3275 0.1513 0.1262 0.073 Uiso 1 1 calc R . . S7 S 0.34013(11) -0.04590(9) 0.11758(10) 0.0347(6) Uani 1 1 d . . . C97 C 0.3908(4) -0.0765(3) 0.1672(4) 0.026(2) Uani 1 1 d . . . C98 C 0.4297(4) -0.0545(3) 0.2082(4) 0.025(2) Uani 1 1 d . . . C99 C 0.4702(4) -0.0802(3) 0.2400(4) 0.028(2) Uani 1 1 d . . . C100 C 0.4726(4) -0.1289(3) 0.2310(4) 0.031(2) Uani 1 1 d . . . H100 H 0.5008 -0.1466 0.2536 0.037 Uiso 1 1 calc R . . C101 C 0.4340(4) -0.1514(3) 0.1893(4) 0.029(2) Uani 1 1 d . . . C102 C 0.3935(4) -0.1237(3) 0.1583(4) 0.030(2) Uani 1 1 d . . . H102 H 0.3666 -0.1382 0.1299 0.035 Uiso 1 1 calc R . . O7 O 0.4267(3) -0.0066(2) 0.2186(3) 0.0276(15) Uani 1 1 d . . . C103 C 0.4475(4) 0.0243(3) 0.1877(5) 0.035(2) Uani 1 1 d . . . H10A H 0.4323 0.0178 0.1478 0.041 Uiso 1 1 calc R . . H10B H 0.4850 0.0200 0.1982 0.041 Uiso 1 1 calc R . . C104 C 0.4352(4) 0.0730(3) 0.2001(4) 0.029(2) Uani 1 1 d . . . C105 C 0.4519(4) 0.1101(4) 0.1754(4) 0.034(2) Uani 1 1 d . . . H105 H 0.4709 0.1033 0.1512 0.041 Uiso 1 1 calc R . . N7 N 0.4425(3) 0.1562(3) 0.1841(4) 0.037(2) Uani 1 1 d . . . C106 C 0.4144(5) 0.1640(4) 0.2181(5) 0.045(3) Uani 1 1 d . . . H106 H 0.4070 0.1957 0.2247 0.055 Uiso 1 1 calc R . . C107 C 0.3963(4) 0.1300(4) 0.2429(5) 0.043(3) Uani 1 1 d . . . H107 H 0.3767 0.1373 0.2663 0.051 Uiso 1 1 calc R . . C108 C 0.4070(4) 0.0847(4) 0.2337(5) 0.040(3) Uani 1 1 d . . . H108 H 0.3944 0.0602 0.2510 0.048 Uiso 1 1 calc R . . C109 C 0.4378(4) -0.2043(4) 0.1776(5) 0.040(3) Uani 1 1 d . . . C110 C 0.4669(5) -0.2314(4) 0.2320(5) 0.046(3) Uani 1 1 d . . . H11A H 0.4678 -0.2650 0.2239 0.068 Uiso 1 1 calc R . . H11B H 0.4490 -0.2267 0.2592 0.068 Uiso 1 1 calc R . . H11C H 0.5019 -0.2193 0.2469 0.068 Uiso 1 1 calc R . . C111 C 0.4682(6) -0.2111(4) 0.1370(6) 0.060(4) Uani 1 1 d . . . H11D H 0.4765 -0.2445 0.1355 0.090 Uiso 1 1 calc R . . H11E H 0.4999 -0.1927 0.1495 0.090 Uiso 1 1 calc R . . H11F H 0.4476 -0.2004 0.1002 0.090 Uiso 1 1 calc R . . C112 C 0.3862(5) -0.2267(4) 0.1524(6) 0.058(4) Uani 1 1 d . . . H11G H 0.3711 -0.2156 0.1144 0.086 Uiso 1 1 calc R . . H11H H 0.3638 -0.2180 0.1739 0.086 Uiso 1 1 calc R . . H11I H 0.3900 -0.2609 0.1525 0.086 Uiso 1 1 calc R . . S8 S 0.52635(10) -0.05513(9) 0.28629(12) 0.0358(6) Uani 1 1 d . . . C113 C 0.5069(3) -0.0142(3) 0.3284(4) 0.028(2) Uani 1 1 d D . . C114 C 0.4794(3) -0.0273(3) 0.3626(3) 0.025(2) Uani 1 1 d D . . H114 H 0.4458 -0.0210 0.3337 0.030 Uiso 1 1 calc R . . C115 C 0.4705(3) 0.0059(4) 0.3986(4) 0.030(2) Uani 1 1 d D . . C116 C 0.4901(4) 0.0508(3) 0.4001(4) 0.026(2) Uani 1 1 d D . . H116 H 0.4825 0.0736 0.4234 0.031 Uiso 1 1 calc R . . C117 C 0.5203(4) 0.0633(3) 0.3689(4) 0.029(2) Uani 1 1 d D . . C118 C 0.5260(4) 0.0319(3) 0.3315(4) 0.029(2) Uani 1 1 d D . . H118 H 0.5435 0.0413 0.3067 0.035 Uiso 1 1 calc R . . O8 O 0.4674(3) -0.0751(2) 0.3674(3) 0.0305(15) Uani 1 1 d . . . C119 C 0.5116(5) -0.0992(4) 0.4049(5) 0.049(3) Uani 1 1 d . . . H11J H 0.5403 -0.0990 0.3896 0.059 Uiso 1 1 calc R . . H11K H 0.5229 -0.0830 0.4411 0.059 Uiso 1 1 calc R . . C120 C 0.4965(4) -0.1478(4) 0.4116(5) 0.038(3) Uani 1 1 d . . . C121 C 0.5137(4) -0.1850(4) 0.3861(5) 0.036(2) Uani 1 1 d . . . H121 H 0.5349 -0.1778 0.3643 0.044 Uiso 1 1 calc R . . N8 N 0.5018(4) -0.2307(3) 0.3911(4) 0.039(2) Uani 1 1 d . . . C122 C 0.4720(5) -0.2394(4) 0.4223(6) 0.048(3) Uani 1 1 d . . . H122 H 0.4612 -0.2709 0.4245 0.058 Uiso 1 1 calc R . . C123 C 0.4566(6) -0.2065(5) 0.4504(6) 0.066(4) Uani 1 1 d . . . H123 H 0.4381 -0.2152 0.4744 0.079 Uiso 1 1 calc R . . C124 C 0.4675(6) -0.1595(4) 0.4448(5) 0.055(3) Uani 1 1 d . . . H124 H 0.4551 -0.1358 0.4634 0.066 Uiso 1 1 calc R . . C125 C 0.5479(4) 0.1112(3) 0.3758(4) 0.033(2) Uani 1 1 d D . . C126 C 0.6057(6) 0.1040(7) 0.3818(9) 0.035(4) Uani 0.468(19) 1 d PD . . H12A H 0.6087 0.0929 0.3467 0.052 Uiso 0.468(19) 1 calc PR . 1 H12B H 0.6207 0.0806 0.4106 0.052 Uiso 0.468(19) 1 calc PR . 1 H12C H 0.6240 0.1339 0.3919 0.052 Uiso 0.468(19) 1 calc PR . 1 C127 C 0.5457(8) 0.1379(7) 0.4278(7) 0.035(4) Uani 0.468(19) 1 d PD . . H12D H 0.5748 0.1595 0.4403 0.052 Uiso 0.468(19) 1 calc PR . 1 H12E H 0.5472 0.1152 0.4572 0.052 Uiso 0.468(19) 1 calc PR . 1 H12F H 0.5137 0.1558 0.4189 0.052 Uiso 0.468(19) 1 calc PR . 1 C128 C 0.5234(7) 0.1413(7) 0.3238(7) 0.035(4) Uani 0.468(19) 1 d PD . . H12G H 0.5448 0.1690 0.3244 0.052 Uiso 0.468(19) 1 calc PR . 1 H12H H 0.4892 0.1515 0.3231 0.052 Uiso 0.468(19) 1 calc PR . 1 H12I H 0.5205 0.1226 0.2908 0.052 Uiso 0.468(19) 1 calc PR . 1 Sb1 Sb 0.14269(3) 0.15126(3) 0.29372(3) 0.0418(2) Uani 1 1 d . . . F1 F 0.1874(3) 0.1399(3) 0.2522(3) 0.061(2) Uani 1 1 d . . . F2 F 0.1918(4) 0.1314(5) 0.3560(4) 0.130(5) Uani 1 1 d . . . F3 F 0.0965(4) 0.1666(4) 0.3314(5) 0.111(4) Uani 1 1 d . . . F4 F 0.0943(3) 0.1729(5) 0.2300(4) 0.121(5) Uani 1 1 d . . . F5 F 0.1698(5) 0.2118(3) 0.3074(6) 0.122(4) Uani 1 1 d . . . F6 F 0.1143(4) 0.0931(3) 0.2774(5) 0.108(4) Uani 1 1 d . . . Sb2 Sb 0.35328(3) 0.30743(3) 0.19901(4) 0.0460(2) Uani 1 1 d . . . F7 F 0.4040(3) 0.2858(4) 0.2621(5) 0.114(4) Uani 1 1 d . . . F8 F 0.3237(4) 0.2485(3) 0.1921(5) 0.103(3) Uani 1 1 d . . . F9 F 0.3824(5) 0.3664(3) 0.2120(5) 0.129(4) Uani 1 1 d . . . F10 F 0.3018(4) 0.3267(5) 0.1373(4) 0.125(4) Uani 1 1 d . . . F11 F 0.3132(3) 0.3210(3) 0.2446(4) 0.080(3) Uani 1 1 d . . . F12 F 0.3943(5) 0.2867(4) 0.1589(6) 0.137(5) Uani 1 1 d . . . Sb3 Sb 0.88310(4) 0.32762(3) 0.31644(5) 0.0623(3) Uani 1 1 d D . . F13 F 0.9369(5) 0.3645(4) 0.3650(5) 0.0623(3) Uani 0.609(6) 1 d PD . . F14 F 0.8353(5) 0.3649(5) 0.3379(6) 0.0623(3) Uani 0.609(6) 1 d PD . . F15 F 0.9326(5) 0.2896(5) 0.3035(6) 0.0623(3) Uani 0.609(6) 1 d PD . . F16 F 0.8306(5) 0.2924(4) 0.2733(5) 0.0623(3) Uani 0.609(6) 1 d PD . . F17 F 0.8879(5) 0.2885(4) 0.3788(5) 0.0623(3) Uani 0.609(6) 1 d PD . . F18 F 0.8799(5) 0.3674(4) 0.2593(5) 0.0623(3) Uani 0.609(6) 1 d PD . . Sb4 Sb 0.61543(3) 0.13293(3) 0.19166(4) 0.0587(3) Uani 1 1 d D . . F19 F 0.6381(6) 0.1623(5) 0.2650(5) 0.0587(3) Uani 0.545(5) 1 d PD D 1 F20 F 0.5660(5) 0.1795(4) 0.1721(6) 0.0587(3) Uani 0.545(5) 1 d PD D 1 F21 F 0.5965(6) 0.1049(5) 0.1261(5) 0.0587(3) Uani 0.545(5) 1 d PD D 1 F22 F 0.6671(5) 0.0869(4) 0.2205(6) 0.0587(3) Uani 0.545(5) 1 d PD D 1 F23 F 0.5713(5) 0.0952(5) 0.2177(6) 0.0587(3) Uani 0.545(5) 1 d PD D 1 F24 F 0.6622(5) 0.1714(5) 0.1735(6) 0.0587(3) Uani 0.545(5) 1 d PD D 1 C129 C 0.9170(8) 0.5270(6) 0.3276(7) 0.095(6) Uani 1 1 d . . . H129 H 0.9181 0.5431 0.2932 0.113 Uiso 1 1 calc R . . Cl1 Cl 0.9790(2) 0.5300(2) 0.3773(3) 0.1124(18) Uani 1 1 d . . . Cl2 Cl 0.9011(2) 0.4685(2) 0.3124(3) 0.127(2) Uani 1 1 d . . . Cl3 Cl 0.8727(2) 0.5555(3) 0.3512(3) 0.147(3) Uani 1 1 d . . . C130 C 0.7917(11) 0.2873(7) 0.4283(9) 0.052(7) Uani 0.50 1 d P . . H130 H 0.8169 0.3020 0.4125 0.062 Uiso 0.50 1 calc PR . . Cl4 Cl 0.8288(6) 0.2674(3) 0.4925(3) 0.144(6) Uani 0.50 1 d P . . Cl5 Cl 0.7637(4) 0.2464(2) 0.3833(3) 0.074(2) Uani 0.50 1 d P . . Cl6 Cl 0.7508(3) 0.3324(3) 0.4299(4) 0.073(2) Uani 0.50 1 d P . . C131 C 0.1737(6) 0.0222(5) 0.4029(7) 0.076(5) Uani 1 1 d . . . H131 H 0.1627 0.0544 0.3882 0.091 Uiso 1 1 calc R . . Cl7 Cl 0.23912(18) 0.02265(16) 0.4359(2) 0.0893(13) Uani 1 1 d . . . Cl8 Cl 0.15825(16) -0.01794(19) 0.3473(2) 0.0955(15) Uani 1 1 d . . . Cl9 Cl 0.14047(19) 0.0063(2) 0.4482(2) 0.1097(19) Uani 1 1 d . . . C132 C 0.4098(7) 0.4323(5) 0.3251(6) 0.082(5) Uani 1 1 d . . . H132 H 0.4050 0.4173 0.2884 0.098 Uiso 1 1 calc R . . Cl10 Cl 0.4719(3) 0.4203(3) 0.3687(3) 0.149(3) Uani 1 1 d . . . Cl11 Cl 0.3649(2) 0.4097(2) 0.3527(2) 0.1150(19) Uani 1 1 d . . . Cl12 Cl 0.4022(2) 0.49210(17) 0.3161(2) 0.1070(17) Uani 1 1 d . . . C133 C 0.3275(5) 0.1835(5) 0.5120(6) 0.062(4) Uani 1 1 d . . . H133 H 0.3107 0.1855 0.5412 0.074 Uiso 1 1 calc R . . Cl13 Cl 0.36695(16) 0.13512(14) 0.52396(17) 0.0756(11) Uani 1 1 d . . . Cl14 Cl 0.28047(15) 0.18001(18) 0.44710(15) 0.0861(14) Uani 1 1 d . . . Cl15 Cl 0.3644(3) 0.23509(18) 0.5139(3) 0.144(3) Uani 1 1 d . . . C134 C 0.1615(6) 0.1941(9) 0.4746(7) 0.111(8) Uani 1 1 d . . . H134 H 0.1752 0.1988 0.4432 0.133 Uiso 1 1 calc R . . Cl16 Cl 0.1414(3) 0.1335(3) 0.4746(2) 0.152(3) Uani 1 1 d . . . Cl17 Cl 0.21066(17) 0.2069(3) 0.53684(19) 0.166(4) Uani 1 1 d . . . Cl18 Cl 0.1120(2) 0.2298(3) 0.4658(2) 0.135(2) Uani 1 1 d . . . C135 C 0.6643(5) 0.9488(5) 0.3890(6) 0.062(4) Uani 1 1 d . . . H135 H 0.6457 0.9182 0.3786 0.074 Uiso 1 1 calc R . . Cl19 Cl 0.63842(15) 0.97902(12) 0.43594(17) 0.0662(10) Uani 1 1 d . . . Cl20 Cl 0.65404(15) 0.98177(16) 0.33003(17) 0.0771(11) Uani 1 1 d . . . Cl21 Cl 0.72796(16) 0.93697(16) 0.4209(2) 0.0877(13) Uani 1 1 d . . . C136 C 0.9774(11) 0.6271(10) 0.5245(10) 0.226(6) Uani 0.50 1 d PD . . H136 H 1.0100 0.6095 0.5419 0.271 Uiso 0.50 1 calc PR . . Cl22 Cl 0.9501(7) 0.6242(7) 0.4539(6) 0.226(6) Uani 0.50 1 d PD . . Cl23 Cl 0.9245(8) 0.6127(7) 0.5438(6) 0.226(6) Uani 0.50 1 d PD . . Cl24 Cl 0.9790(7) 0.6873(7) 0.5267(7) 0.226(6) Uani 0.50 1 d PD . . C137 C 0.4483(8) 0.1464(9) 0.9855(9) 0.045(6) Uani 0.50 1 d P . . H137 H 0.4317 0.1186 0.9627 0.054 Uiso 0.50 1 calc PR . . Cl25 Cl 0.4366(5) 0.1929(3) 0.9424(4) 0.099(3) Uani 0.50 1 d P . . Cl26 Cl 0.5109(4) 0.1314(4) 1.0164(6) 0.179(8) Uani 0.50 1 d P . . Cl27 Cl 0.4186(4) 0.1535(2) 1.0344(3) 0.074(2) Uani 0.50 1 d P . . C138 C 0.696(2) 0.1506(12) 0.0604(11) 0.14(2) Uani 0.50 1 d P . . H138 H 0.6796 0.1356 0.0861 0.163 Uiso 0.50 1 calc PR . . Cl28 Cl 0.7387(4) 0.1137(4) 0.0563(4) 0.094(3) Uani 0.50 1 d P . . Cl29 Cl 0.7253(5) 0.2014(4) 0.0946(5) 0.115(4) Uani 0.50 1 d P . . Cl30 Cl 0.6459(5) 0.1551(8) -0.0029(4) 0.200(9) Uani 0.50 1 d P . . C139 C 0.6546(8) 0.0044(9) 0.0164(8) 0.112(15) Uani 0.50 1 d PD . . H139 H 0.6498 0.0289 -0.0129 0.134 Uiso 0.50 1 calc PR . . Cl31 Cl 0.6208(6) -0.0422(4) -0.0139(4) 0.158(7) Uani 0.50 1 d PD . . Cl32 Cl 0.7167(5) -0.0110(5) 0.0361(5) 0.221(11) Uani 0.50 1 d PD . . Cl33 Cl 0.6366(6) 0.0300(3) 0.0687(5) 0.154(6) Uani 0.50 1 d PD . . C140 C 0.1290(8) 0.9428(7) 0.0498(7) 0.034(5) Uani 0.50 1 d P . . H140 H 0.1196 0.9375 0.0840 0.040 Uiso 0.50 1 calc PR . . Cl34 Cl 0.1200(3) 0.8903(3) 0.0135(3) 0.085(3) Uani 0.50 1 d P . . Cl35 Cl 0.1912(3) 0.9645(3) 0.0698(4) 0.077(2) Uani 0.50 1 d P . . Cl36 Cl 0.0876(3) 0.9861(3) 0.0104(3) 0.093(3) Uani 0.50 1 d P . . F19A F 0.6692(6) 0.1694(6) 0.2321(6) 0.0587(3) Uani 0.455(5) 1 d PD D 2 F20A F 0.6119(7) 0.0978(5) 0.2471(6) 0.0587(3) Uani 0.455(5) 1 d PD D 2 F21A F 0.5581(6) 0.0989(6) 0.1411(6) 0.0587(3) Uani 0.455(5) 1 d PD D 2 F22A F 0.6575(6) 0.1003(6) 0.1594(7) 0.0587(3) Uani 0.455(5) 1 d PD D 2 F23A F 0.5692(6) 0.1675(6) 0.2133(7) 0.0587(3) Uani 0.455(5) 1 d PD D 2 F24A F 0.6148(7) 0.1683(6) 0.1275(5) 0.0587(3) Uani 0.455(5) 1 d PD D 2 F13A F 0.9210(7) 0.3725(6) 0.2926(8) 0.0623(3) Uani 0.391(6) 1 d PD C 2 F14A F 0.8527(7) 0.3698(6) 0.3486(8) 0.0623(3) Uani 0.391(6) 1 d PD C 2 F15A F 0.9152(7) 0.2813(6) 0.2811(8) 0.0623(3) Uani 0.391(6) 1 d PD C 2 F16A F 0.8460(7) 0.2777(6) 0.3331(8) 0.0623(3) Uani 0.391(6) 1 d PD C 2 F17A F 0.9381(6) 0.3178(7) 0.3802(6) 0.0623(3) Uani 0.391(6) 1 d PD C 2 F18A F 0.8321(6) 0.3324(7) 0.2476(6) 0.0623(3) Uani 0.391(6) 1 d PD C 2 C12A C 0.5128(9) 0.1497(7) 0.3887(12) 0.082(8) Uani 0.532(19) 1 d PD . 2 H12J H 0.5001 0.1707 0.3569 0.123 Uiso 0.532(19) 1 calc PR . 2 H12K H 0.5326 0.1679 0.4210 0.123 Uiso 0.532(19) 1 calc PR . 2 H12L H 0.4839 0.1345 0.3963 0.123 Uiso 0.532(19) 1 calc PR . 2 C12B C 0.5956(8) 0.1038(8) 0.4271(9) 0.082(8) Uani 0.532(19) 1 d PD . 2 H12M H 0.5869 0.1109 0.4606 0.123 Uiso 0.532(19) 1 calc PR . 2 H12N H 0.6232 0.1247 0.4250 0.123 Uiso 0.532(19) 1 calc PR . 2 H12O H 0.6070 0.0710 0.4284 0.123 Uiso 0.532(19) 1 calc PR . 2 C12C C 0.5625(11) 0.1231(8) 0.3254(8) 0.082(8) Uani 0.532(19) 1 d PD . 2 H12P H 0.5569 0.1567 0.3173 0.123 Uiso 0.532(19) 1 calc PR . 2 H12Q H 0.5413 0.1047 0.2940 0.123 Uiso 0.532(19) 1 calc PR . 2 H12R H 0.5986 0.1155 0.3323 0.123 Uiso 0.532(19) 1 calc PR . 2 _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 0.0510(6) 0.0246(5) 0.0506(5) 0.0068(4) 0.0150(4) -0.0109(4) Ag2 0.0488(5) 0.0212(5) 0.0590(6) 0.0052(4) 0.0125(4) -0.0118(4) Ag3 0.0371(5) 0.0287(5) 0.0429(5) 0.0064(3) 0.0143(4) 0.0118(3) Ag4 0.0458(5) 0.0209(5) 0.0722(6) 0.0091(4) 0.0194(5) -0.0070(4) S1 0.0375(15) 0.0274(14) 0.0276(12) 0.0011(10) 0.0094(11) -0.0022(11) C1 0.023(5) 0.020(5) 0.032(5) 0.004(4) 0.005(4) 0.005(4) C2 0.019(5) 0.025(6) 0.035(5) 0.003(4) 0.003(4) 0.002(4) C3 0.016(4) 0.035(6) 0.033(5) 0.001(4) 0.003(4) 0.005(4) C4 0.029(5) 0.021(6) 0.047(6) 0.000(4) 0.016(5) -0.007(4) C5 0.031(5) 0.019(6) 0.036(5) 0.000(4) 0.004(4) -0.004(4) C6 0.036(6) 0.022(5) 0.022(4) -0.002(4) 0.012(4) 0.001(4) O1 0.024(3) 0.014(4) 0.038(4) 0.001(3) 0.004(3) 0.002(3) C7 0.033(6) 0.034(7) 0.038(6) -0.004(4) -0.006(5) 0.000(5) C8 0.030(5) 0.023(6) 0.039(6) 0.002(4) 0.011(4) 0.003(4) C9 0.029(5) 0.034(7) 0.032(5) -0.004(4) 0.004(4) 0.005(5) N1 0.042(5) 0.017(5) 0.039(5) 0.001(3) 0.012(4) 0.011(4) C10 0.050(7) 0.020(6) 0.048(7) 0.009(5) 0.013(6) 0.004(5) C11 0.073(9) 0.036(8) 0.057(8) 0.013(6) 0.039(7) 0.002(6) C12 0.066(9) 0.021(6) 0.050(7) -0.003(5) 0.023(6) 0.014(5) C13 0.032(5) 0.016(5) 0.036(5) -0.005(4) 0.002(4) -0.003(4) C14 0.088(11) 0.037(8) 0.057(8) -0.003(6) 0.028(8) -0.028(7) C15 0.047(8) 0.041(8) 0.073(9) -0.010(6) 0.001(7) -0.008(6) C16 0.055(8) 0.028(7) 0.085(10) -0.014(6) 0.017(7) -0.012(6) S2 0.0252(13) 0.0303(15) 0.0485(15) -0.0119(11) 0.0144(11) -0.0003(11) C17 0.025(5) 0.023(6) 0.037(5) 0.003(4) 0.016(4) 0.002(4) C18 0.030(5) 0.019(5) 0.028(5) -0.005(4) 0.012(4) 0.004(4) C19 0.030(5) 0.019(5) 0.028(5) -0.005(4) 0.012(4) 0.004(4) C20 0.047(7) 0.018(6) 0.034(5) -0.003(4) 0.005(5) 0.007(5) C21 0.041(6) 0.018(5) 0.036(5) -0.006(4) 0.011(5) 0.000(4) C22 0.031(5) 0.009(5) 0.041(6) 0.000(4) 0.012(4) 0.005(4) O2 0.041(4) 0.011(4) 0.041(4) -0.003(3) 0.019(3) 0.002(3) C23 0.048(7) 0.015(6) 0.054(7) 0.002(4) 0.030(5) 0.016(5) C24 0.027(5) 0.021(6) 0.047(6) -0.004(4) 0.014(5) -0.002(4) C25 0.034(6) 0.027(6) 0.030(5) 0.002(4) 0.016(4) -0.001(4) N2 0.034(5) 0.013(5) 0.048(5) 0.006(3) 0.006(4) -0.001(3) C26 0.055(7) 0.016(6) 0.048(6) 0.005(4) 0.021(6) 0.004(5) C27 0.045(7) 0.022(6) 0.046(6) 0.001(4) 0.019(5) 0.004(5) C28 0.038(6) 0.031(6) 0.039(6) 0.004(4) 0.018(5) -0.004(5) C29 0.043(7) 0.018(6) 0.054(7) -0.009(5) 0.003(5) 0.005(5) C30 0.057(9) 0.023(7) 0.080(9) -0.015(6) -0.005(7) -0.005(6) C31 0.103(13) 0.028(8) 0.085(10) -0.005(6) 0.047(9) 0.013(7) C32 0.062(8) 0.021(6) 0.061(8) 0.003(5) 0.013(7) 0.007(5) S3 0.0595(19) 0.0231(15) 0.0299(13) 0.0015(10) 0.0103(12) 0.0175(13) C33 0.037(6) 0.017(5) 0.027(5) -0.001(4) 0.008(4) -0.002(4) C34 0.030(5) 0.016(5) 0.032(5) 0.013(4) 0.005(4) 0.008(4) C35 0.018(5) 0.028(6) 0.032(5) 0.008(4) 0.005(4) 0.002(4) C36 0.036(6) 0.022(5) 0.022(4) 0.010(4) 0.005(4) 0.010(4) C37 0.034(6) 0.014(5) 0.031(5) 0.005(4) 0.009(4) 0.000(4) C38 0.038(6) 0.020(5) 0.027(5) 0.004(4) 0.013(4) 0.004(4) O3 0.025(4) 0.021(4) 0.038(4) 0.009(3) 0.002(3) -0.001(3) C39 0.029(5) 0.014(5) 0.050(6) 0.004(4) -0.003(5) -0.001(4) C40 0.031(6) 0.030(6) 0.039(6) 0.005(4) 0.010(5) 0.004(4) C41 0.027(5) 0.036(7) 0.039(6) 0.013(5) 0.004(5) -0.006(5) N3 0.036(5) 0.022(5) 0.053(6) 0.016(4) 0.004(4) 0.000(4) C42 0.042(7) 0.025(7) 0.060(7) 0.012(5) 0.000(6) 0.005(5) C43 0.023(5) 0.027(6) 0.062(7) 0.014(5) 0.004(5) -0.001(4) C44 0.038(6) 0.020(6) 0.040(6) -0.001(4) 0.003(5) 0.002(4) C45 0.046(7) 0.027(6) 0.029(5) 0.006(4) 0.016(5) 0.014(5) C46 0.087(11) 0.023(7) 0.094(10) 0.032(6) 0.049(9) 0.011(6) C47 0.070(10) 0.059(9) 0.060(8) 0.028(7) -0.014(7) 0.019(8) C48 0.134(15) 0.027(7) 0.070(9) 0.017(6) 0.058(10) 0.037(8) S4 0.0272(13) 0.0503(18) 0.0433(15) 0.0257(13) 0.0151(12) 0.0148(12) C49 0.037(6) 0.036(6) 0.034(5) 0.016(4) 0.024(5) 0.012(5) C50 0.032(5) 0.032(6) 0.029(5) 0.005(4) 0.016(4) 0.002(4) C51 0.028(5) 0.019(5) 0.028(5) 0.003(4) 0.011(4) -0.002(4) C52 0.039(6) 0.024(6) 0.024(5) 0.005(4) 0.008(4) 0.007(4) C53 0.026(5) 0.033(6) 0.039(6) 0.010(4) 0.012(4) -0.001(4) C54 0.028(5) 0.034(6) 0.036(5) 0.007(4) 0.007(4) 0.006(4) O4 0.041(4) 0.010(3) 0.044(4) 0.009(3) 0.024(3) 0.007(3) C55 0.049(7) 0.028(6) 0.058(7) 0.003(5) 0.038(6) 0.004(5) C56 0.032(6) 0.025(6) 0.037(5) 0.002(4) 0.016(5) 0.005(4) C57 0.032(6) 0.024(6) 0.040(6) -0.005(4) 0.018(5) -0.004(4) N4 0.031(5) 0.025(5) 0.038(5) 0.008(3) 0.017(4) 0.011(4) C58 0.038(6) 0.020(6) 0.070(8) 0.006(5) 0.026(6) 0.006(5) C59 0.034(6) 0.045(8) 0.048(7) -0.006(5) 0.011(5) 0.000(5) C60 0.049(7) 0.038(7) 0.044(6) 0.009(5) 0.013(6) 0.020(6) C61 0.042(6) 0.025(6) 0.043(6) 0.006(4) 0.021(5) -0.006(5) C62 0.042(6) 0.025(6) 0.043(6) 0.006(4) 0.021(5) -0.006(5) C63 0.042(6) 0.025(6) 0.043(6) 0.006(4) 0.021(5) -0.006(5) C64 0.042(6) 0.025(6) 0.043(6) 0.006(4) 0.021(5) -0.006(5) S5 0.0362(15) 0.0281(14) 0.0300(13) 0.0032(10) 0.0085(11) -0.0004(11) C65 0.025(5) 0.029(6) 0.029(5) 0.000(4) 0.010(4) 0.005(4) C66 0.028(5) 0.016(5) 0.036(5) 0.006(4) 0.017(4) 0.007(4) C67 0.029(5) 0.029(6) 0.032(5) 0.009(4) 0.018(4) 0.008(4) C68 0.037(6) 0.027(6) 0.035(5) 0.005(4) 0.017(5) 0.000(4) C69 0.040(6) 0.028(6) 0.037(6) -0.003(4) 0.019(5) -0.001(5) C70 0.044(6) 0.018(6) 0.037(6) 0.005(4) 0.016(5) 0.004(4) O5 0.039(4) 0.013(3) 0.035(4) 0.005(3) 0.021(3) 0.004(3) C71 0.059(8) 0.020(6) 0.057(7) 0.006(5) 0.036(6) 0.009(5) C72 0.049(7) 0.023(6) 0.047(6) 0.009(5) 0.024(6) 0.011(5) C73 0.036(6) 0.022(6) 0.037(5) 0.004(4) 0.021(5) 0.004(4) N5 0.040(5) 0.015(5) 0.044(5) 0.009(3) 0.014(4) 0.005(4) C74 0.045(7) 0.019(6) 0.051(7) 0.004(5) 0.011(5) -0.001(5) C75 0.037(7) 0.049(9) 0.067(9) 0.011(6) -0.006(6) 0.004(6) C76 0.043(7) 0.044(8) 0.058(8) 0.005(6) -0.001(6) 0.008(6) C77 0.111(7) 0.057(5) 0.110(7) 0.026(4) 0.060(6) -0.007(4) C78 0.111(7) 0.057(5) 0.110(7) 0.026(4) 0.060(6) -0.007(4) C79 0.111(7) 0.057(5) 0.110(7) 0.026(4) 0.060(6) -0.007(4) C80 0.111(7) 0.057(5) 0.110(7) 0.026(4) 0.060(6) -0.007(4) S6 0.0283(13) 0.0451(17) 0.0390(14) 0.0200(12) 0.0172(11) 0.0128(12) C81 0.020(5) 0.029(6) 0.034(5) 0.011(4) 0.007(4) 0.000(4) C82 0.029(5) 0.011(5) 0.029(5) 0.002(3) 0.010(4) -0.001(4) C83 0.028(5) 0.016(5) 0.037(5) -0.001(4) 0.007(4) 0.014(4) C84 0.038(6) 0.026(6) 0.032(5) 0.006(4) 0.014(5) 0.006(4) C85 0.041(6) 0.023(6) 0.035(5) 0.010(4) 0.015(5) 0.010(4) C86 0.028(5) 0.022(5) 0.026(5) -0.002(4) 0.008(4) 0.006(4) O6 0.022(3) 0.016(4) 0.040(4) 0.009(3) 0.005(3) 0.000(3) C87 0.027(5) 0.025(6) 0.047(6) 0.004(4) 0.001(5) -0.008(4) C88 0.035(6) 0.023(6) 0.035(5) 0.001(4) 0.010(5) -0.001(4) C89 0.033(6) 0.026(6) 0.051(7) 0.011(5) 0.004(5) -0.008(5) N6 0.044(6) 0.017(5) 0.062(6) 0.011(4) 0.021(5) -0.001(4) C90 0.050(7) 0.015(6) 0.063(8) 0.018(5) 0.011(6) 0.001(5) C91 0.021(5) 0.028(6) 0.066(8) 0.012(5) 0.005(5) 0.000(4) C92 0.029(5) 0.015(5) 0.044(6) -0.001(4) 0.008(5) -0.014(4) C93 0.043(6) 0.027(6) 0.038(6) 0.008(4) 0.013(5) 0.012(5) C94 0.100(12) 0.048(8) 0.073(9) 0.030(7) 0.060(9) 0.037(8) C95 0.057(8) 0.050(8) 0.049(7) 0.023(6) 0.000(6) 0.014(6) C96 0.066(9) 0.031(7) 0.054(7) 0.021(5) 0.027(6) 0.004(6) S7 0.0476(17) 0.0242(15) 0.0301(13) 0.0001(10) 0.0093(12) 0.0121(12) C97 0.031(5) 0.017(5) 0.031(5) 0.003(4) 0.013(4) 0.006(4) C98 0.032(5) 0.013(5) 0.034(5) -0.001(4) 0.017(4) 0.002(4) C99 0.032(5) 0.016(5) 0.039(5) 0.000(4) 0.016(4) -0.003(4) C100 0.032(6) 0.027(6) 0.034(5) -0.006(4) 0.011(4) 0.004(4) C101 0.034(6) 0.013(5) 0.044(6) -0.005(4) 0.016(5) 0.002(4) C102 0.036(6) 0.021(6) 0.031(5) -0.004(4) 0.009(4) 0.006(4) O7 0.041(4) 0.005(3) 0.042(4) -0.002(3) 0.021(3) -0.002(3) C103 0.041(6) 0.018(6) 0.057(7) 0.001(4) 0.033(5) 0.001(4) C104 0.028(5) 0.026(6) 0.037(5) -0.003(4) 0.017(4) -0.001(4) C105 0.037(6) 0.026(6) 0.042(6) -0.001(4) 0.016(5) -0.007(5) N7 0.039(5) 0.015(5) 0.059(6) 0.003(4) 0.018(5) -0.001(4) C106 0.051(7) 0.012(6) 0.079(9) -0.005(5) 0.029(7) 0.010(5) C107 0.044(7) 0.026(7) 0.070(8) -0.005(5) 0.036(6) 0.002(5) C108 0.046(7) 0.023(6) 0.060(7) -0.003(5) 0.027(6) 0.007(5) C109 0.040(6) 0.022(6) 0.059(7) -0.008(5) 0.016(6) 0.000(5) C110 0.047(7) 0.017(6) 0.062(8) 0.006(5) 0.003(6) 0.002(5) C111 0.091(11) 0.037(8) 0.069(9) -0.019(6) 0.050(8) -0.002(7) C112 0.059(9) 0.015(6) 0.077(9) 0.000(5) -0.010(7) -0.002(5) S8 0.0259(13) 0.0287(15) 0.0531(16) -0.0157(12) 0.0131(12) 0.0000(11) C113 0.021(5) 0.017(5) 0.048(6) -0.008(4) 0.012(4) 0.001(4) C114 0.021(5) 0.017(5) 0.032(5) -0.002(4) 0.003(4) 0.005(4) C115 0.024(5) 0.034(6) 0.029(5) 0.011(4) 0.005(4) 0.009(4) C116 0.035(5) 0.004(5) 0.033(5) -0.002(3) 0.002(4) 0.001(4) C117 0.036(6) 0.018(5) 0.029(5) 0.000(4) 0.005(4) 0.002(4) C118 0.034(6) 0.020(6) 0.035(5) -0.004(4) 0.013(4) 0.001(4) O8 0.027(4) 0.017(4) 0.045(4) -0.001(3) 0.007(3) 0.000(3) C119 0.055(8) 0.011(6) 0.063(8) 0.003(5) -0.007(6) 0.004(5) C120 0.042(7) 0.016(6) 0.050(7) 0.002(4) 0.008(5) 0.013(5) C121 0.030(6) 0.024(6) 0.056(7) -0.007(5) 0.014(5) 0.006(4) N8 0.037(5) 0.019(5) 0.060(6) 0.005(4) 0.016(5) 0.007(4) C122 0.051(8) 0.017(6) 0.085(9) 0.006(5) 0.032(7) -0.002(5) C123 0.088(12) 0.051(9) 0.074(10) 0.018(7) 0.046(9) 0.013(8) C124 0.081(10) 0.039(8) 0.057(8) -0.005(6) 0.036(7) 0.006(7) C125 0.041(6) 0.020(6) 0.033(5) -0.008(4) 0.007(5) -0.009(4) C126 0.029(7) 0.014(7) 0.058(9) -0.010(5) 0.008(6) -0.012(5) C127 0.029(7) 0.014(7) 0.058(9) -0.010(5) 0.008(6) -0.012(5) C128 0.029(7) 0.014(7) 0.058(9) -0.010(5) 0.008(6) -0.012(5) Sb1 0.0321(4) 0.0375(5) 0.0586(5) 0.0013(3) 0.0183(4) -0.0042(3) F1 0.046(4) 0.075(5) 0.070(5) -0.004(4) 0.030(4) 0.000(4) F2 0.078(7) 0.234(14) 0.060(6) 0.053(7) -0.004(5) -0.004(8) F3 0.101(8) 0.122(9) 0.151(10) -0.014(7) 0.097(8) -0.018(7) F4 0.043(5) 0.216(13) 0.099(8) 0.073(8) 0.013(5) 0.029(7) F5 0.142(10) 0.070(7) 0.201(12) -0.051(7) 0.118(10) -0.043(7) F6 0.124(9) 0.065(6) 0.156(10) -0.035(6) 0.077(8) -0.057(6) Sb2 0.0323(4) 0.0376(5) 0.0710(6) 0.0031(4) 0.0205(4) -0.0015(3) F7 0.050(6) 0.143(10) 0.132(9) 0.066(7) 0.005(6) 0.021(6) F8 0.094(7) 0.066(6) 0.163(10) -0.009(6) 0.063(7) -0.023(5) F9 0.157(11) 0.065(7) 0.167(11) -0.007(7) 0.057(9) -0.061(7) F10 0.091(8) 0.181(12) 0.077(7) 0.051(7) -0.010(6) 0.010(8) F11 0.063(6) 0.101(7) 0.078(6) -0.020(5) 0.024(5) 0.016(5) F12 0.126(10) 0.147(10) 0.202(13) -0.026(9) 0.144(10) -0.015(8) Sb3 0.0393(5) 0.0529(6) 0.0959(8) -0.0053(5) 0.0234(5) 0.0002(4) F13 0.0393(5) 0.0529(6) 0.0959(8) -0.0053(5) 0.0234(5) 0.0002(4) F14 0.0393(5) 0.0529(6) 0.0959(8) -0.0053(5) 0.0234(5) 0.0002(4) F15 0.0393(5) 0.0529(6) 0.0959(8) -0.0053(5) 0.0234(5) 0.0002(4) F16 0.0393(5) 0.0529(6) 0.0959(8) -0.0053(5) 0.0234(5) 0.0002(4) F17 0.0393(5) 0.0529(6) 0.0959(8) -0.0053(5) 0.0234(5) 0.0002(4) F18 0.0393(5) 0.0529(6) 0.0959(8) -0.0053(5) 0.0234(5) 0.0002(4) Sb4 0.0411(5) 0.0428(6) 0.0939(7) -0.0027(5) 0.0238(5) 0.0009(4) F19 0.0411(5) 0.0428(6) 0.0939(7) -0.0027(5) 0.0238(5) 0.0009(4) F20 0.0411(5) 0.0428(6) 0.0939(7) -0.0027(5) 0.0238(5) 0.0009(4) F21 0.0411(5) 0.0428(6) 0.0939(7) -0.0027(5) 0.0238(5) 0.0009(4) F22 0.0411(5) 0.0428(6) 0.0939(7) -0.0027(5) 0.0238(5) 0.0009(4) F23 0.0411(5) 0.0428(6) 0.0939(7) -0.0027(5) 0.0238(5) 0.0009(4) F24 0.0411(5) 0.0428(6) 0.0939(7) -0.0027(5) 0.0238(5) 0.0009(4) C129 0.141(18) 0.087(13) 0.083(11) 0.040(9) 0.074(12) 0.057(12) Cl1 0.088(4) 0.127(4) 0.145(5) 0.012(4) 0.070(4) 0.010(3) Cl2 0.120(5) 0.114(5) 0.161(5) 0.041(4) 0.063(4) -0.003(4) Cl3 0.125(5) 0.210(7) 0.129(5) 0.049(5) 0.072(4) 0.101(5) C130 0.11(2) 0.007(11) 0.058(14) 0.014(9) 0.053(14) 0.017(11) Cl4 0.248(15) 0.072(6) 0.045(4) 0.004(4) -0.049(7) 0.010(7) Cl5 0.132(7) 0.028(4) 0.054(4) -0.001(3) 0.015(4) 0.002(4) Cl6 0.062(5) 0.058(5) 0.101(6) -0.033(4) 0.028(4) 0.002(4) C131 0.096(12) 0.052(9) 0.103(12) 0.041(8) 0.065(10) 0.035(8) Cl7 0.082(3) 0.093(3) 0.110(3) -0.018(3) 0.055(3) -0.026(2) Cl8 0.045(2) 0.136(4) 0.102(3) 0.010(3) 0.019(2) 0.010(2) Cl9 0.092(3) 0.140(4) 0.129(4) 0.065(3) 0.079(3) 0.043(3) C132 0.138(17) 0.061(10) 0.052(8) 0.020(7) 0.038(10) 0.008(10) Cl10 0.133(5) 0.171(6) 0.180(6) 0.076(5) 0.103(5) 0.054(5) Cl11 0.096(4) 0.138(5) 0.097(4) 0.027(3) 0.012(3) -0.034(3) Cl12 0.158(5) 0.067(3) 0.113(4) -0.004(3) 0.068(4) 0.009(3) C133 0.051(8) 0.058(9) 0.066(9) 0.008(7) 0.004(7) 0.010(7) Cl13 0.074(3) 0.062(2) 0.079(3) 0.0204(19) 0.008(2) 0.022(2) Cl14 0.056(2) 0.139(4) 0.053(2) -0.001(2) 0.0036(18) 0.036(2) Cl15 0.158(6) 0.063(3) 0.160(5) 0.039(3) -0.021(5) -0.012(3) C134 0.045(9) 0.22(3) 0.058(10) 0.046(13) 0.007(8) -0.004(12) Cl16 0.144(6) 0.233(8) 0.086(4) 0.052(4) 0.047(4) 0.019(6) Cl17 0.042(2) 0.396(11) 0.055(3) 0.023(4) 0.011(2) -0.021(4) Cl18 0.078(4) 0.223(7) 0.089(4) 0.042(4) 0.004(3) -0.018(4) C135 0.051(8) 0.044(8) 0.097(11) -0.010(7) 0.031(8) -0.002(6) Cl19 0.065(2) 0.051(2) 0.093(3) 0.0056(18) 0.039(2) 0.0134(17) Cl20 0.053(2) 0.101(3) 0.080(3) -0.001(2) 0.023(2) -0.016(2) Cl21 0.061(2) 0.096(3) 0.109(3) -0.004(3) 0.031(2) 0.035(2) C136 0.208(11) 0.282(13) 0.143(7) -0.045(8) -0.007(8) -0.088(10) Cl22 0.208(11) 0.282(13) 0.143(7) -0.045(8) -0.007(8) -0.088(10) Cl23 0.208(11) 0.282(13) 0.143(7) -0.045(8) -0.007(8) -0.088(10) Cl24 0.208(11) 0.282(13) 0.143(7) -0.045(8) -0.007(8) -0.088(10) C137 0.026(11) 0.059(16) 0.045(13) -0.005(11) 0.006(10) -0.010(11) Cl25 0.190(11) 0.037(4) 0.096(6) 0.015(4) 0.084(7) 0.008(5) Cl26 0.062(6) 0.152(11) 0.243(15) -0.126(11) -0.065(8) 0.036(6) Cl27 0.143(8) 0.042(4) 0.038(3) -0.003(3) 0.028(4) 0.002(4) C138 0.33(7) 0.07(2) 0.048(17) -0.024(16) 0.11(3) -0.10(3) Cl28 0.100(7) 0.108(8) 0.075(6) 0.023(5) 0.031(5) -0.004(6) Cl29 0.134(10) 0.089(7) 0.124(8) 0.048(6) 0.043(7) 0.006(6) Cl30 0.099(9) 0.43(3) 0.077(7) 0.128(11) 0.039(6) 0.097(12) C139 0.14(3) 0.19(4) 0.033(14) -0.037(19) 0.063(19) -0.07(3) Cl31 0.309(19) 0.103(8) 0.117(8) -0.033(6) 0.145(11) -0.104(10) Cl32 0.223(16) 0.212(15) 0.132(10) -0.078(10) -0.079(11) 0.176(14) Cl33 0.33(2) 0.071(6) 0.139(9) -0.029(6) 0.183(12) -0.047(9) C140 0.036(12) 0.038(13) 0.017(9) 0.005(8) -0.006(8) -0.008(9) Cl34 0.093(6) 0.068(5) 0.064(4) -0.032(4) -0.018(4) 0.008(4) Cl35 0.039(4) 0.065(5) 0.110(6) 0.012(4) 0.001(4) -0.021(3) Cl36 0.071(5) 0.106(7) 0.075(5) -0.004(5) -0.013(4) 0.050(5) F19A 0.0411(5) 0.0428(6) 0.0939(7) -0.0027(5) 0.0238(5) 0.0009(4) F20A 0.0411(5) 0.0428(6) 0.0939(7) -0.0027(5) 0.0238(5) 0.0009(4) F21A 0.0411(5) 0.0428(6) 0.0939(7) -0.0027(5) 0.0238(5) 0.0009(4) F22A 0.0411(5) 0.0428(6) 0.0939(7) -0.0027(5) 0.0238(5) 0.0009(4) F23A 0.0411(5) 0.0428(6) 0.0939(7) -0.0027(5) 0.0238(5) 0.0009(4) F24A 0.0411(5) 0.0428(6) 0.0939(7) -0.0027(5) 0.0238(5) 0.0009(4) F13A 0.0393(5) 0.0529(6) 0.0959(8) -0.0053(5) 0.0234(5) 0.0002(4) F14A 0.0393(5) 0.0529(6) 0.0959(8) -0.0053(5) 0.0234(5) 0.0002(4) F15A 0.0393(5) 0.0529(6) 0.0959(8) -0.0053(5) 0.0234(5) 0.0002(4) F16A 0.0393(5) 0.0529(6) 0.0959(8) -0.0053(5) 0.0234(5) 0.0002(4) F17A 0.0393(5) 0.0529(6) 0.0959(8) -0.0053(5) 0.0234(5) 0.0002(4) F18A 0.0393(5) 0.0529(6) 0.0959(8) -0.0053(5) 0.0234(5) 0.0002(4) C12A 0.115(18) 0.032(10) 0.113(16) -0.010(9) 0.057(13) -0.038(10) C12B 0.115(18) 0.032(10) 0.113(16) -0.010(9) 0.057(13) -0.038(10) C12C 0.115(18) 0.032(10) 0.113(16) -0.010(9) 0.057(13) -0.038(10) _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. ; _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 N2 2.130(8) . ? Ag1 N1 2.130(8) 2_545 ? Ag2 N3 2.088(9) . ? Ag2 N6 2.100(9) 1_565 ? Ag3 N4 2.134(8) . ? Ag3 N5 2.140(8) . ? Ag4 N7 2.133(9) . ? Ag4 N8 2.144(9) 2_655 ? S1 C1 1.780(10) . ? S1 C51 1.778(10) . ? C1 C6 1.365(13) . ? C1 C2 1.394(13) . ? C2 C3 1.385(14) . ? C2 O1 1.403(11) . ? C3 C4 1.397(14) . ? C3 S2 1.769(10) . ? C4 C5 1.383(14) . ? C4 H4 0.9500 . ? C5 C6 1.399(14) . ? C5 C13 1.538(13) . ? C6 H6 0.9500 . ? O1 C7 1.429(11) . ? C7 C8 1.516(15) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.381(14) . ? C8 C12 1.384(15) . ? C9 N1 1.337(13) . ? C9 H9 0.9500 . ? N1 C10 1.354(14) . ? N1 Ag1 2.130(8) 2 ? C10 C11 1.381(16) . ? C10 H10 0.9500 . ? C11 C12 1.386(16) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C15 1.513(15) . ? C13 C14 1.526(15) . ? C13 C16 1.557(16) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9801 . ? C16 H16B 0.9801 . ? C16 H16C 0.9801 . ? S2 C17 1.784(10) . ? C17 C22 1.376(13) . ? C17 C18 1.399(13) . ? C18 O2 1.373(11) . ? C18 C19 1.408(13) . ? C19 C20 1.380(14) . ? C19 S3 1.767(10) . ? C20 C21 1.407(14) . ? C20 H20 0.9500 . ? C21 C22 1.374(13) . ? C21 C29 1.538(14) . ? C22 H22 0.9500 . ? O2 C23 1.416(12) . ? C23 C24 1.485(13) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.390(13) . ? C24 C28 1.414(14) . ? C25 N2 1.360(13) . ? C25 H25 0.9500 . ? N2 C26 1.340(14) . ? C26 C27 1.361(14) . ? C26 H26 0.9500 . ? C27 C28 1.380(14) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C31 1.508(18) . ? C29 C30 1.521(16) . ? C29 C32 1.561(15) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? S3 C33 1.766(10) . ? C33 C34 1.374(13) . ? C33 C38 1.398(13) . ? C34 C35 1.386(14) . ? C34 O3 1.398(10) . ? C35 C36 1.384(12) . ? C35 S4 1.781(10) . ? C36 C37 1.397(13) . ? C36 H36 0.9500 . ? C37 C38 1.382(13) . ? C37 C45 1.532(13) . ? C38 H38 0.9500 . ? O3 C39 1.419(11) . ? C39 C40 1.492(14) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C44 1.374(14) . ? C40 C41 1.385(14) . ? C41 N3 1.332(13) . ? C41 H41 0.9500 . ? N3 C42 1.365(14) . ? C42 C43 1.385(15) . ? C42 H42 0.9500 . ? C43 C44 1.372(14) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.525(16) . ? C45 C48 1.530(15) . ? C45 C47 1.570(16) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? S4 C49 1.772(10) . ? C49 C50 1.375(14) . ? C49 C54 1.421(14) . ? C50 O4 1.383(12) . ? C50 C51 1.410(13) . ? C51 C52 1.364(13) . ? C52 C53 1.410(14) . ? C52 H52 0.9500 . ? C53 C54 1.416(13) . ? C53 C61 1.522(14) . ? C54 H54 0.9500 . ? O4 C55 1.451(12) . ? C55 C56 1.470(14) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C60 1.378(15) . ? C56 C57 1.387(14) . ? C57 N4 1.342(12) . ? C57 H57 0.9500 . ? N4 C58 1.363(14) . ? C58 C59 1.376(15) . ? C58 H58 0.9500 . ? C59 C60 1.379(16) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 C63 1.483(17) . ? C61 C64 1.494(19) . ? C61 C62 1.50(2) . ? C62 H62A 0.9801 . ? C62 H62B 0.9801 . ? C62 H62C 0.9801 . ? C63 H63A 0.9801 . ? C63 H63B 0.9801 . ? C63 H63C 0.9801 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? S5 C65 1.769(10) . ? S5 C115 1.790(10) . ? C65 C66 1.394(13) . ? C65 C70 1.407(14) . ? C66 O5 1.388(11) . ? C66 C67 1.392(13) . ? C67 C68 1.405(13) . ? C67 S6 1.769(10) . ? C68 C69 1.367(14) . ? C68 H68 0.9500 . ? C69 C70 1.416(15) . ? C69 C77 1.482(17) . ? C70 H70 0.9500 . ? O5 C71 1.436(12) . ? C71 C72 1.490(14) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 C73 1.395(14) . ? C72 C76 1.408(16) . ? C73 N5 1.359(12) . ? C73 H73 0.9500 . ? N5 C74 1.322(13) . ? C74 C75 1.379(15) . ? C74 H74 0.9500 . ? C75 C76 1.337(17) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? C77 C78 1.50(2) . ? C77 C80 1.56(2) . ? C77 C79 1.59(2) . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 H79A 0.9812 . ? C79 H79B 0.9811 . ? C79 H79C 0.9812 . ? C80 H80A 0.9800 . ? C80 H80B 0.9801 . ? C80 H80C 0.9801 . ? S6 C81 1.776(10) . ? C81 C82 1.372(13) . ? C81 C86 1.412(13) . ? C82 O6 1.382(10) . ? C82 C83 1.405(13) . ? C83 C84 1.372(13) . ? C83 S7 1.772(9) . ? C84 C85 1.400(14) . ? C84 H84 0.9500 . ? C85 C86 1.389(13) . ? C85 C93 1.549(13) . ? C86 H86 0.9500 . ? O6 C87 1.445(11) . ? C87 C88 1.528(14) . ? C87 H87A 0.9900 . ? C87 H87B 0.9900 . ? C88 C89 1.377(14) . ? C88 C92 1.387(14) . ? C89 N6 1.341(13) . ? C89 H89 0.9500 . ? N6 C90 1.352(14) . ? N6 Ag2 2.100(9) 1_545 ? C90 C91 1.356(15) . ? C90 H90 0.9500 . ? C91 C92 1.373(14) . ? C91 H91 0.9500 . ? C92 H92 0.9500 . ? C93 C96 1.524(16) . ? C93 C94 1.534(16) . ? C93 C95 1.559(16) . ? C94 H94A 0.9800 . ? C94 H94B 0.9800 . ? C94 H94C 0.9800 . ? C95 H95A 0.9800 . ? C95 H95B 0.9800 . ? C95 H95C 0.9800 . ? C96 H96A 0.9800 . ? C96 H96B 0.9800 . ? C96 H96C 0.9800 . ? S7 C97 1.785(9) . ? C97 C102 1.368(13) . ? C97 C98 1.385(13) . ? C98 C99 1.364(13) . ? C98 O7 1.395(11) . ? C99 C100 1.407(13) . ? C99 S8 1.771(10) . ? C100 C101 1.398(14) . ? C100 H100 0.9500 . ? C101 C102 1.389(14) . ? C101 C109 1.542(14) . ? C102 H102 0.9500 . ? O7 C103 1.417(11) . ? C103 C104 1.484(14) . ? C103 H10A 0.9900 . ? C103 H10B 0.9900 . ? C104 C108 1.371(14) . ? C104 C105 1.382(14) . ? C105 N7 1.367(13) . ? C105 H105 0.9500 . ? N7 C106 1.357(14) . ? C106 C107 1.336(16) . ? C106 H106 0.9500 . ? C107 C108 1.358(14) . ? C107 H107 0.9500 . ? C108 H108 0.9500 . ? C109 C112 1.505(16) . ? C109 C111 1.542(16) . ? C109 C110 1.567(15) . ? C110 H11A 0.9800 . ? C110 H11B 0.9800 . ? C110 H11C 0.9800 . ? C111 H11D 0.9800 . ? C111 H11E 0.9800 . ? C111 H11F 0.9800 . ? C112 H11G 0.9800 . ? C112 H11H 0.9800 . ? C112 H11I 0.9800 . ? S8 C113 1.780(9) . ? C113 C114 1.378(13) . ? C113 C118 1.407(13) . ? C114 C115 1.395(13) . ? C114 O8 1.410(11) . ? C114 H114 1.0000 . ? C115 C116 1.381(13) . ? C116 C117 1.370(14) . ? C116 H116 0.9500 . ? C117 C118 1.353(13) . ? C117 C125 1.544(13) . ? C118 H118 0.9500 . ? O8 C119 1.459(12) . ? C119 C120 1.467(15) . ? C119 H11J 0.9900 . ? C119 H11K 0.9900 . ? C120 C124 1.382(17) . ? C120 C121 1.402(14) . ? C121 N8 1.355(13) . ? C121 H121 0.9500 . ? N8 C122 1.340(15) . ? N8 Ag4 2.144(9) 2_645 ? C122 C123 1.327(18) . ? C122 H122 0.9500 . ? C123 C124 1.385(18) . ? C123 H123 0.9500 . ? C124 H124 0.9500 . ? C125 C12C 1.505(15) . ? C125 C128 1.545(15) . ? C125 C12B 1.547(16) . ? C125 C127 1.549(14) . ? C125 C12A 1.564(16) . ? C125 C126 1.564(15) . ? C126 H12A 0.9800 . ? C126 H12B 0.9800 . ? C126 H12C 0.9800 . ? C127 H12D 0.9801 . ? C127 H12E 0.9801 . ? C127 H12F 0.9801 . ? C128 H12G 0.9800 . ? C128 H12H 0.9800 . ? C128 H12I 0.9800 . ? Sb1 F6 1.819(8) . ? Sb1 F2 1.820(9) . ? Sb1 F4 1.851(9) . ? Sb1 F5 1.863(9) . ? Sb1 F3 1.878(9) . ? Sb1 F1 1.895(7) . ? Sb2 F10 1.836(9) . ? Sb2 F9 1.843(9) . ? Sb2 F8 1.845(9) . ? Sb2 F12 1.849(9) . ? Sb2 F7 1.870(9) . ? Sb2 F11 1.886(8) . ? Sb3 F14A 1.805(12) . ? Sb3 F16 1.815(10) . ? Sb3 F18 1.828(10) . ? Sb3 F15 1.852(10) . ? Sb3 F17A 1.858(11) . ? Sb3 F13A 1.870(12) . ? Sb3 F18A 1.875(11) . ? Sb3 F16A 1.875(12) . ? Sb3 F14 1.905(10) . ? Sb3 F17 1.914(10) . ? Sb3 F13 1.915(9) . ? Sb3 F15A 1.961(12) . ? Sb4 F20A 1.762(11) . ? Sb4 F21 1.777(10) . ? Sb4 F23A 1.831(12) . ? Sb4 F19A 1.834(11) . ? Sb4 F20 1.849(10) . ? Sb4 F24 1.860(11) . ? Sb4 F22A 1.871(12) . ? Sb4 F23 1.896(11) . ? Sb4 F22 1.901(10) . ? Sb4 F24A 1.920(11) . ? Sb4 F21A 1.949(11) . ? Sb4 F19 1.964(10) . ? C129 Cl3 1.726(16) . ? C129 Cl2 1.73(2) . ? C129 Cl1 1.78(2) . ? C129 H129 1.0000 . ? C130 Cl5 1.64(3) . ? C130 Cl6 1.72(2) . ? C130 Cl4 1.73(2) . ? C130 H130 1.0000 . ? C131 Cl7 1.729(17) . ? C131 Cl9 1.753(14) . ? C131 Cl8 1.765(18) . ? C131 H131 1.0000 . ? C132 Cl12 1.718(15) . ? C132 Cl11 1.734(17) . ? C132 Cl10 1.753(19) . ? C132 H132 1.0000 . ? C133 Cl13 1.719(14) . ? C133 Cl14 1.752(13) . ? C133 Cl15 1.776(15) . ? C133 H133 1.0000 . ? C134 Cl18 1.66(2) . ? C134 Cl17 1.767(17) . ? C134 Cl16 1.81(2) . ? C134 H134 1.0000 . ? C135 Cl21 1.717(14) . ? C135 Cl20 1.719(15) . ? C135 Cl19 1.799(14) . ? C135 H135 1.0000 . ? C136 Cl24 1.71(2) . ? C136 Cl22 1.72(2) . ? C136 Cl23 1.73(2) . ? C136 H136 1.0000 . ? C137 Cl25 1.69(3) . ? C137 Cl26 1.71(2) . ? C137 Cl27 1.71(2) . ? C137 H137 1.0000 . ? C138 Cl28 1.61(5) . ? C138 Cl29 1.75(3) . ? C138 Cl30 1.76(4) . ? C138 H138 1.0000 . ? C139 Cl31 1.662(18) . ? C139 Cl32 1.681(19) . ? C139 Cl33 1.729(16) . ? C139 H139 1.0000 . ? C140 Cl34 1.73(2) . ? C140 Cl35 1.74(2) . ? C140 Cl36 1.76(2) . ? C140 H140 1.0000 . ? C12A H12J 0.9800 . ? C12A H12K 0.9800 . ? C12A H12L 0.9800 . ? C12B H12M 0.9803 . ? C12B H12N 0.9803 . ? C12B H12O 0.9803 . ? C12C H12P 0.9800 . ? C12C H12Q 0.9800 . ? C12C H12R 0.9800 . ? _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 N2 Ag1 N1 176.7(3) . 2_545 ? N3 Ag2 N6 178.9(4) . 1_565 ? N4 Ag3 N5 177.5(3) . . ? N7 Ag4 N8 179.7(4) . 2_655 ? C1 S1 C51 104.6(4) . . ? C6 C1 C2 119.7(9) . . ? C6 C1 S1 118.7(7) . . ? C2 C1 S1 121.4(7) . . ? C3 C2 C1 119.0(9) . . ? C3 C2 O1 119.6(9) . . ? C1 C2 O1 121.2(9) . . ? C2 C3 C4 119.7(9) . . ? C2 C3 S2 122.2(8) . . ? C4 C3 S2 117.5(8) . . ? C5 C4 C3 121.9(9) . . ? C5 C4 H4 119.0 . . ? C3 C4 H4 119.1 . . ? C4 C5 C6 116.4(9) . . ? C4 C5 C13 121.3(9) . . ? C6 C5 C13 122.0(9) . . ? C1 C6 C5 122.9(9) . . ? C1 C6 H6 118.6 . . ? C5 C6 H6 118.6 . . ? C2 O1 C7 108.0(7) . . ? O1 C7 C8 107.9(8) . . ? O1 C7 H7A 110.1 . . ? C8 C7 H7A 110.1 . . ? O1 C7 H7B 110.1 . . ? C8 C7 H7B 110.2 . . ? H7A C7 H7B 108.4 . . ? C9 C8 C12 117.8(10) . . ? C9 C8 C7 121.0(10) . . ? C12 C8 C7 121.3(10) . . ? N1 C9 C8 123.5(10) . . ? N1 C9 H9 118.2 . . ? C8 C9 H9 118.3 . . ? C9 N1 C10 117.6(9) . . ? C9 N1 Ag1 124.0(7) . 2 ? C10 N1 Ag1 118.2(7) . 2 ? N1 C10 C11 122.9(10) . . ? N1 C10 H10 118.6 . . ? C11 C10 H10 118.5 . . ? C10 C11 C12 117.8(11) . . ? C10 C11 H11 121.1 . . ? C12 C11 H11 121.1 . . ? C11 C12 C8 120.3(10) . . ? C11 C12 H12 119.8 . . ? C8 C12 H12 119.9 . . ? C15 C13 C14 108.0(10) . . ? C15 C13 C5 109.4(8) . . ? C14 C13 C5 111.0(8) . . ? C15 C13 C16 107.6(9) . . ? C14 C13 C16 109.3(10) . . ? C5 C13 C16 111.3(9) . . ? C3 S2 C17 106.7(4) . . ? C22 C17 C18 120.6(9) . . ? C22 C17 S2 116.0(7) . . ? C18 C17 S2 122.1(7) . . ? O2 C18 C17 121.0(8) . . ? O2 C18 C19 120.9(8) . . ? C17 C18 C19 117.9(9) . . ? C20 C19 C18 120.2(9) . . ? C20 C19 S3 116.5(7) . . ? C18 C19 S3 122.8(8) . . ? C19 C20 C21 121.5(9) . . ? C19 C20 H20 119.3 . . ? C21 C20 H20 119.2 . . ? C22 C21 C20 117.4(9) . . ? C22 C21 C29 123.0(9) . . ? C20 C21 C29 119.5(9) . . ? C17 C22 C21 122.3(9) . . ? C17 C22 H22 118.9 . . ? C21 C22 H22 118.8 . . ? C18 O2 C23 115.4(7) . . ? O2 C23 C24 108.2(8) . . ? O2 C23 H23A 110.1 . . ? C24 C23 H23A 110.0 . . ? O2 C23 H23B 110.1 . . ? C24 C23 H23B 110.1 . . ? H23A C23 H23B 108.4 . . ? C25 C24 C28 118.0(9) . . ? C25 C24 C23 119.7(9) . . ? C28 C24 C23 122.3(9) . . ? N2 C25 C24 121.9(9) . . ? N2 C25 H25 119.0 . . ? C24 C25 H25 119.1 . . ? C26 N2 C25 119.6(8) . . ? C26 N2 Ag1 120.6(7) . . ? C25 N2 Ag1 119.8(7) . . ? N2 C26 C27 120.9(9) . . ? N2 C26 H26 119.5 . . ? C27 C26 H26 119.6 . . ? C26 C27 C28 121.6(10) . . ? C26 C27 H27 119.1 . . ? C28 C27 H27 119.3 . . ? C27 C28 C24 117.8(10) . . ? C27 C28 H28 121.1 . . ? C24 C28 H28 121.1 . . ? C31 C29 C30 108.6(11) . . ? C31 C29 C21 108.8(10) . . ? C30 C29 C21 112.6(9) . . ? C31 C29 C32 108.0(10) . . ? C30 C29 C32 107.6(10) . . ? C21 C29 C32 111.2(9) . . ? C33 S3 C19 109.4(4) . . ? C34 C33 C38 117.9(9) . . ? C34 C33 S3 124.9(7) . . ? C38 C33 S3 116.4(7) . . ? C33 C34 C35 120.9(8) . . ? C33 C34 O3 119.3(9) . . ? C35 C34 O3 119.7(8) . . ? C34 C35 C36 120.0(9) . . ? C34 C35 S4 124.8(7) . . ? C36 C35 S4 114.0(7) . . ? C35 C36 C37 120.9(9) . . ? C35 C36 H36 119.6 . . ? C37 C36 H36 119.5 . . ? C38 C37 C36 117.3(8) . . ? C38 C37 C45 120.5(8) . . ? C36 C37 C45 122.1(9) . . ? C37 C38 C33 123.0(9) . . ? C37 C38 H38 118.5 . . ? C33 C38 H38 118.5 . . ? C34 O3 C39 114.5(7) . . ? O3 C39 C40 107.9(8) . . ? O3 C39 H39A 110.1 . . ? C40 C39 H39A 110.1 . . ? O3 C39 H39B 110.1 . . ? C40 C39 H39B 110.1 . . ? H39A C39 H39B 108.4 . . ? C44 C40 C41 117.4(9) . . ? C44 C40 C39 122.2(9) . . ? C41 C40 C39 120.4(9) . . ? N3 C41 C40 125.4(10) . . ? N3 C41 H41 117.3 . . ? C40 C41 H41 117.3 . . ? C41 N3 C42 115.9(9) . . ? C41 N3 Ag2 122.5(7) . . ? C42 N3 Ag2 120.1(7) . . ? N3 C42 C43 122.3(10) . . ? N3 C42 H42 118.9 . . ? C43 C42 H42 118.8 . . ? C44 C43 C42 119.6(10) . . ? C44 C43 H43 120.2 . . ? C42 C43 H43 120.3 . . ? C43 C44 C40 119.5(10) . . ? C43 C44 H44 120.2 . . ? C40 C44 H44 120.3 . . ? C46 C45 C37 110.1(9) . . ? C46 C45 C48 109.5(11) . . ? C37 C45 C48 110.6(8) . . ? C46 C45 C47 109.9(10) . . ? C37 C45 C47 106.5(9) . . ? C48 C45 C47 110.3(11) . . ? C49 S4 C35 106.7(4) . . ? C50 C49 C54 121.3(9) . . ? C50 C49 S4 122.8(8) . . ? C54 C49 S4 115.3(8) . . ? C49 C50 O4 120.9(9) . . ? C49 C50 C51 118.3(9) . . ? O4 C50 C51 120.8(9) . . ? C52 C51 C50 120.2(9) . . ? C52 C51 S1 117.8(7) . . ? C50 C51 S1 121.4(7) . . ? C51 C52 C53 123.5(9) . . ? C51 C52 H52 118.2 . . ? C53 C52 H52 118.3 . . ? C52 C53 C54 115.8(9) . . ? C52 C53 C61 123.9(9) . . ? C54 C53 C61 120.2(9) . . ? C53 C54 C49 120.3(10) . . ? C53 C54 H54 119.8 . . ? C49 C54 H54 119.8 . . ? C50 O4 C55 108.0(7) . . ? O4 C55 C56 110.6(8) . . ? O4 C55 H55A 109.5 . . ? C56 C55 H55A 109.5 . . ? O4 C55 H55B 109.5 . . ? C56 C55 H55B 109.5 . . ? H55A C55 H55B 108.1 . . ? C60 C56 C57 118.3(10) . . ? C60 C56 C55 121.9(10) . . ? C57 C56 C55 119.7(10) . . ? N4 C57 C56 123.7(10) . . ? N4 C57 H57 118.1 . . ? C56 C57 H57 118.1 . . ? C57 N4 C58 117.0(9) . . ? C57 N4 Ag3 121.8(7) . . ? C58 N4 Ag3 121.0(7) . . ? N4 C58 C59 122.0(10) . . ? N4 C58 H58 119.1 . . ? C59 C58 H58 119.0 . . ? C58 C59 C60 119.9(11) . . ? C58 C59 H59 120.0 . . ? C60 C59 H59 120.1 . . ? C56 C60 C59 118.9(10) . . ? C56 C60 H60 120.6 . . ? C59 C60 H60 120.5 . . ? C63 C61 C64 106.7(14) . . ? C63 C61 C62 108.8(15) . . ? C64 C61 C62 109.5(16) . . ? C63 C61 C53 112.7(10) . . ? C64 C61 C53 112.2(10) . . ? C62 C61 C53 106.9(10) . . ? C65 S5 C115 105.0(4) . . ? C66 C65 C70 118.4(9) . . ? C66 C65 S5 123.7(8) . . ? C70 C65 S5 117.5(7) . . ? O5 C66 C65 119.3(9) . . ? O5 C66 C67 120.3(8) . . ? C65 C66 C67 120.4(9) . . ? C66 C67 C68 119.0(9) . . ? C66 C67 S6 122.8(7) . . ? C68 C67 S6 117.6(8) . . ? C69 C68 C67 122.9(10) . . ? C69 C68 H68 118.5 . . ? C67 C68 H68 118.5 . . ? C68 C69 C70 116.5(10) . . ? C68 C69 C77 123.4(12) . . ? C70 C69 C77 120.0(11) . . ? C65 C70 C69 122.2(9) . . ? C65 C70 H70 118.9 . . ? C69 C70 H70 118.9 . . ? C66 O5 C71 109.2(7) . . ? O5 C71 C72 109.5(8) . . ? O5 C71 H71A 109.8 . . ? C72 C71 H71A 109.8 . . ? O5 C71 H71B 109.8 . . ? C72 C71 H71B 109.8 . . ? H71A C71 H71B 108.2 . . ? C73 C72 C76 115.7(10) . . ? C73 C72 C71 120.4(11) . . ? C76 C72 C71 123.7(11) . . ? N5 C73 C72 122.8(10) . . ? N5 C73 H73 118.6 . . ? C72 C73 H73 118.6 . . ? C74 N5 C73 117.8(9) . . ? C74 N5 Ag3 120.8(7) . . ? C73 N5 Ag3 121.4(7) . . ? N5 C74 C75 123.5(11) . . ? N5 C74 H74 118.2 . . ? C75 C74 H74 118.3 . . ? C76 C75 C74 118.3(12) . . ? C76 C75 H75 120.9 . . ? C74 C75 H75 120.9 . . ? C75 C76 C72 121.7(11) . . ? C75 C76 H76 119.1 . . ? C72 C76 H76 119.1 . . ? C78 C77 C69 107.7(13) . . ? C78 C77 C80 109.6(15) . . ? C69 C77 C80 111.7(13) . . ? C78 C77 C79 106.8(14) . . ? C69 C77 C79 111.7(13) . . ? C80 C77 C79 109.2(14) . . ? C67 S6 C81 107.7(4) . . ? C82 C81 C86 119.4(9) . . ? C82 C81 S6 125.3(7) . . ? C86 C81 S6 114.4(7) . . ? C81 C82 O6 119.8(8) . . ? C81 C82 C83 120.0(8) . . ? O6 C82 C83 120.2(8) . . ? C84 C83 C82 120.0(8) . . ? C84 C83 S7 116.2(8) . . ? C82 C83 S7 123.0(7) . . ? C83 C84 C85 121.6(9) . . ? C83 C84 H84 119.2 . . ? C85 C84 H84 119.2 . . ? C86 C85 C84 117.8(9) . . ? C86 C85 C93 122.4(9) . . ? C84 C85 C93 119.7(9) . . ? C85 C86 C81 121.3(9) . . ? C85 C86 H86 119.3 . . ? C81 C86 H86 119.4 . . ? C82 O6 C87 112.4(7) . . ? O6 C87 C88 106.6(8) . . ? O6 C87 H87A 110.4 . . ? C88 C87 H87A 110.4 . . ? O6 C87 H87B 110.4 . . ? C88 C87 H87B 110.4 . . ? H87A C87 H87B 108.6 . . ? C89 C88 C92 118.2(9) . . ? C89 C88 C87 118.5(9) . . ? C92 C88 C87 123.2(9) . . ? N6 C89 C88 122.8(10) . . ? N6 C89 H89 118.6 . . ? C88 C89 H89 118.6 . . ? C89 N6 C90 117.8(9) . . ? C89 N6 Ag2 119.3(7) . 1_545 ? C90 N6 Ag2 122.3(7) . 1_545 ? N6 C90 C91 122.3(9) . . ? N6 C90 H90 118.9 . . ? C91 C90 H90 118.9 . . ? C90 C91 C92 119.8(10) . . ? C90 C91 H91 120.1 . . ? C92 C91 H91 120.1 . . ? C91 C92 C88 118.9(9) . . ? C91 C92 H92 120.5 . . ? C88 C92 H92 120.6 . . ? C96 C93 C94 109.2(10) . . ? C96 C93 C85 110.6(9) . . ? C94 C93 C85 110.6(9) . . ? C96 C93 C95 108.6(9) . . ? C94 C93 C95 110.6(10) . . ? C85 C93 C95 107.1(9) . . ? C83 S7 C97 109.3(4) . . ? C102 C97 C98 119.9(9) . . ? C102 C97 S7 115.5(7) . . ? C98 C97 S7 124.0(7) . . ? C99 C98 C97 119.9(9) . . ? C99 C98 O7 119.7(9) . . ? C97 C98 O7 120.4(8) . . ? C98 C99 C100 120.1(9) . . ? C98 C99 S8 123.9(7) . . ? C100 C99 S8 115.3(8) . . ? C101 C100 C99 120.6(9) . . ? C101 C100 H100 119.7 . . ? C99 C100 H100 119.7 . . ? C102 C101 C100 117.0(9) . . ? C102 C101 C109 122.2(9) . . ? C100 C101 C109 120.7(9) . . ? C97 C102 C101 122.5(9) . . ? C97 C102 H102 118.7 . . ? C101 C102 H102 118.8 . . ? C98 O7 C103 116.0(7) . . ? O7 C103 C104 107.3(8) . . ? O7 C103 H10A 110.2 . . ? C104 C103 H10A 110.2 . . ? O7 C103 H10B 110.3 . . ? C104 C103 H10B 110.3 . . ? H10A C103 H10B 108.5 . . ? C108 C104 C105 116.2(10) . . ? C108 C104 C103 125.0(9) . . ? C105 C104 C103 118.8(9) . . ? N7 C105 C104 123.1(10) . . ? N7 C105 H105 118.4 . . ? C104 C105 H105 118.4 . . ? C106 N7 C105 116.0(9) . . ? C106 N7 Ag4 121.9(7) . . ? C105 N7 Ag4 122.1(7) . . ? C107 C106 N7 124.3(10) . . ? C107 C106 H106 117.9 . . ? N7 C106 H106 117.8 . . ? C106 C107 C108 117.9(11) . . ? C106 C107 H107 121.0 . . ? C108 C107 H107 121.1 . . ? C107 C108 C104 122.4(11) . . ? C107 C108 H108 118.8 . . ? C104 C108 H108 118.8 . . ? C112 C109 C101 112.4(9) . . ? C112 C109 C111 107.6(11) . . ? C101 C109 C111 109.8(9) . . ? C112 C109 C110 108.5(10) . . ? C101 C109 C110 110.8(9) . . ? C111 C109 C110 107.6(10) . . ? C99 S8 C113 107.4(4) . . ? C114 C113 C118 119.2(9) . . ? C114 C113 S8 122.8(7) . . ? C118 C113 S8 117.5(8) . . ? C113 C114 C115 119.0(9) . . ? C113 C114 O8 120.4(8) . . ? C115 C114 O8 119.9(8) . . ? C113 C114 H114 92.8 . . ? C115 C114 H114 92.9 . . ? O8 C114 H114 92.8 . . ? C116 C115 C114 119.6(9) . . ? C116 C115 S5 119.2(8) . . ? C114 C115 S5 121.2(8) . . ? C117 C116 C115 121.9(9) . . ? C117 C116 H116 119.0 . . ? C115 C116 H116 119.0 . . ? C118 C117 C116 118.1(9) . . ? C118 C117 C125 119.8(9) . . ? C116 C117 C125 122.1(8) . . ? C117 C118 C113 121.8(10) . . ? C117 C118 H118 119.1 . . ? C113 C118 H118 119.1 . . ? C114 O8 C119 109.9(7) . . ? C120 C119 O8 108.1(9) . . ? C120 C119 H11J 110.0 . . ? O8 C119 H11J 110.1 . . ? C120 C119 H11K 110.1 . . ? O8 C119 H11K 110.1 . . ? H11J C119 H11K 108.4 . . ? C124 C120 C121 116.9(10) . . ? C124 C120 C119 122.7(11) . . ? C121 C120 C119 120.3(11) . . ? N8 C121 C120 123.4(11) . . ? N8 C121 H121 118.3 . . ? C120 C121 H121 118.3 . . ? C122 N8 C121 116.5(9) . . ? C122 N8 Ag4 120.4(7) . 2_645 ? C121 N8 Ag4 123.0(8) . 2_645 ? C123 C122 N8 123.7(11) . . ? C123 C122 H122 118.1 . . ? N8 C122 H122 118.2 . . ? C122 C123 C124 120.4(13) . . ? C122 C123 H123 119.8 . . ? C124 C123 H123 119.7 . . ? C120 C124 C123 118.9(12) . . ? C120 C124 H124 120.5 . . ? C123 C124 H124 120.6 . . ? C12C C125 C117 110.9(11) . . ? C12C C125 C128 45.7(12) . . ? C117 C125 C128 109.0(10) . . ? C12C C125 C12B 111.8(13) . . ? C117 C125 C12B 103.3(11) . . ? C128 C125 C12B 145.8(13) . . ? C12C C125 C127 136.1(13) . . ? C117 C125 C127 112.0(10) . . ? C128 C125 C127 110.0(11) . . ? C12B C125 C127 66.1(12) . . ? C12C C125 C12A 112.1(12) . . ? C117 C125 C12A 108.9(11) . . ? C128 C125 C12A 70.4(12) . . ? C12B C125 C12A 109.4(12) . . ? C127 C125 C12A 43.9(12) . . ? C12C C125 C126 64.6(13) . . ? C117 C125 C126 110.2(10) . . ? C128 C125 C126 108.0(11) . . ? C12B C125 C126 48.4(12) . . ? C127 C125 C126 107.4(10) . . ? C12A C125 C126 138.7(13) . . ? F6 Sb1 F2 93.7(6) . . ? F6 Sb1 F4 87.8(6) . . ? F2 Sb1 F4 178.1(5) . . ? F6 Sb1 F5 177.4(6) . . ? F2 Sb1 F5 88.9(6) . . ? F4 Sb1 F5 89.6(6) . . ? F6 Sb1 F3 90.9(5) . . ? F2 Sb1 F3 93.5(5) . . ? F4 Sb1 F3 87.5(5) . . ? F5 Sb1 F3 89.2(4) . . ? F6 Sb1 F1 91.5(4) . . ? F2 Sb1 F1 90.1(4) . . ? F4 Sb1 F1 88.8(4) . . ? F5 Sb1 F1 88.2(4) . . ? F3 Sb1 F1 175.5(4) . . ? F10 Sb2 F9 93.3(6) . . ? F10 Sb2 F8 89.5(5) . . ? F9 Sb2 F8 175.0(5) . . ? F10 Sb2 F12 93.4(6) . . ? F9 Sb2 F12 94.6(6) . . ? F8 Sb2 F12 89.3(5) . . ? F10 Sb2 F7 177.7(5) . . ? F9 Sb2 F7 88.9(6) . . ? F8 Sb2 F7 88.3(5) . . ? F12 Sb2 F7 87.2(6) . . ? F10 Sb2 F11 91.4(5) . . ? F9 Sb2 F11 90.6(5) . . ? F8 Sb2 F11 85.2(4) . . ? F12 Sb2 F11 172.6(5) . . ? F7 Sb2 F11 87.7(5) . . ? F14A Sb3 F16 104.3(8) . . ? F14A Sb3 F18 92.5(9) . . ? F16 Sb3 F18 91.7(5) . . ? F14A Sb3 F15 161.0(7) . . ? F16 Sb3 F15 93.4(6) . . ? F18 Sb3 F15 93.9(6) . . ? F14A Sb3 F17A 93.8(7) . . ? F16 Sb3 F17A 136.0(7) . . ? F18 Sb3 F17A 127.7(7) . . ? F15 Sb3 F17A 68.2(7) . . ? F14A Sb3 F13A 94.9(8) . . ? F16 Sb3 F13A 126.7(7) . . ? F18 Sb3 F13A 37.5(6) . . ? F15 Sb3 F13A 79.6(8) . . ? F17A Sb3 F13A 90.2(7) . . ? F14A Sb3 F18A 93.6(7) . . ? F16 Sb3 F18A 41.9(7) . . ? F18 Sb3 F18A 51.2(7) . . ? F15 Sb3 F18A 104.3(7) . . ? F17A Sb3 F18A 172.6(8) . . ? F13A Sb3 F18A 88.5(7) . . ? F14A Sb3 F16A 91.8(8) . . ? F16 Sb3 F16A 48.3(7) . . ? F18 Sb3 F16A 139.4(7) . . ? F15 Sb3 F16A 94.9(8) . . ? F17A Sb3 F16A 92.2(7) . . ? F13A Sb3 F16A 172.7(8) . . ? F18A Sb3 F16A 88.2(7) . . ? F14A Sb3 F14 14.9(7) . . ? F16 Sb3 F14 89.5(5) . . ? F18 Sb3 F14 91.4(6) . . ? F15 Sb3 F14 173.9(6) . . ? F17A Sb3 F14 106.1(8) . . ? F13A Sb3 F14 103.0(8) . . ? F18A Sb3 F14 81.4(8) . . ? F16A Sb3 F14 83.0(8) . . ? F14A Sb3 F17 85.6(8) . . ? F16 Sb3 F17 90.9(5) . . ? F18 Sb3 F17 177.1(6) . . ? F15 Sb3 F17 87.3(5) . . ? F17A Sb3 F17 50.4(7) . . ? F13A Sb3 F17 140.4(7) . . ? F18A Sb3 F17 131.0(7) . . ? F16A Sb3 F17 43.0(6) . . ? F14 Sb3 F17 87.3(6) . . ? F14A Sb3 F13 73.6(7) . . ? F16 Sb3 F13 177.0(6) . . ? F18 Sb3 F13 90.5(5) . . ? F15 Sb3 F13 88.5(5) . . ? F17A Sb3 F13 42.9(7) . . ? F13A Sb3 F13 55.9(7) . . ? F18A Sb3 F13 139.7(7) . . ? F16A Sb3 F13 129.3(7) . . ? F14 Sb3 F13 88.4(5) . . ? F17 Sb3 F13 86.8(5) . . ? F14A Sb3 F15A 179.2(8) . . ? F16 Sb3 F15A 74.9(7) . . ? F18 Sb3 F15A 87.7(8) . . ? F15 Sb3 F15A 19.7(6) . . ? F17A Sb3 F15A 86.7(7) . . ? F13A Sb3 F15A 85.8(7) . . ? F18A Sb3 F15A 85.9(7) . . ? F16A Sb3 F15A 87.5(7) . . ? F14 Sb3 F15A 164.3(7) . . ? F17 Sb3 F15A 94.2(8) . . ? F13 Sb3 F15A 107.2(7) . . ? F20A Sb4 F21 115.5(7) . . ? F20A Sb4 F23A 80.6(7) . . ? F21 Sb4 F23A 120.2(7) . . ? F20A Sb4 F19A 96.3(7) . . ? F21 Sb4 F19A 136.5(8) . . ? F23A Sb4 F19A 92.4(7) . . ? F20A Sb4 F20 113.4(8) . . ? F21 Sb4 F20 95.6(6) . . ? F23A Sb4 F20 34.3(7) . . ? F19A Sb4 F20 98.1(7) . . ? F20A Sb4 F24 139.1(7) . . ? F21 Sb4 F24 92.6(6) . . ? F23A Sb4 F24 111.5(7) . . ? F19A Sb4 F24 46.2(7) . . ? F20 Sb4 F24 91.3(6) . . ? F20A Sb4 F22A 106.0(7) . . ? F21 Sb4 F22A 53.0(7) . . ? F23A Sb4 F22A 171.9(7) . . ? F19A Sb4 F22A 91.4(7) . . ? F20 Sb4 F22A 137.9(7) . . ? F24 Sb4 F22A 66.6(7) . . ? F20A Sb4 F23 35.9(6) . . ? F21 Sb4 F23 93.0(6) . . ? F23A Sb4 F23 66.9(7) . . ? F19A Sb4 F23 128.0(7) . . ? F20 Sb4 F23 89.9(6) . . ? F24 Sb4 F23 174.2(6) . . ? F22A Sb4 F23 115.8(7) . . ? F20A Sb4 F22 61.7(7) . . ? F21 Sb4 F22 90.9(6) . . ? F23A Sb4 F22 139.5(7) . . ? F19A Sb4 F22 78.4(7) . . ? F20 Sb4 F22 173.3(7) . . ? F24 Sb4 F22 90.4(6) . . ? F22A Sb4 F22 48.4(7) . . ? F23 Sb4 F22 87.8(6) . . ? F20A Sb4 F24A 175.3(7) . . ? F21 Sb4 F24A 60.5(7) . . ? F23A Sb4 F24A 99.3(7) . . ? F19A Sb4 F24A 88.4(6) . . ? F20 Sb4 F24A 65.8(7) . . ? F24 Sb4 F24A 45.3(6) . . ? F22A Sb4 F24A 73.7(6) . . ? F23 Sb4 F24A 139.9(7) . . ? F22 Sb4 F24A 119.5(7) . . ? F20A Sb4 F21A 90.6(7) . . ? F21 Sb4 F21A 38.8(7) . . ? F23A Sb4 F21A 88.3(6) . . ? F19A Sb4 F21A 173.1(7) . . ? F20 Sb4 F21A 78.7(7) . . ? F24 Sb4 F21A 127.3(7) . . ? F22A Sb4 F21A 87.0(6) . . ? F23 Sb4 F21A 58.5(7) . . ? F22 Sb4 F21A 105.4(7) . . ? F24A Sb4 F21A 84.7(6) . . ? F20A Sb4 F19 63.6(7) . . ? F21 Sb4 F19 178.1(7) . . ? F23A Sb4 F19 61.5(7) . . ? F19A Sb4 F19 43.0(7) . . ? F20 Sb4 F19 86.3(6) . . ? F24 Sb4 F19 87.4(6) . . ? F22A Sb4 F19 125.4(7) . . ? F23 Sb4 F19 87.0(6) . . ? F22 Sb4 F19 87.2(5) . . ? F24A Sb4 F19 120.5(7) . . ? F21A Sb4 F19 141.9(7) . . ? Cl3 C129 Cl2 111.8(12) . . ? Cl3 C129 Cl1 110.8(10) . . ? Cl2 C129 Cl1 108.9(9) . . ? Cl3 C129 H129 108.4 . . ? Cl2 C129 H129 108.5 . . ? Cl1 C129 H129 108.4 . . ? Cl5 C130 Cl6 112.2(17) . . ? Cl5 C130 Cl4 115.9(12) . . ? Cl6 C130 Cl4 114.5(13) . . ? Cl5 C130 H130 104.3 . . ? Cl6 C130 H130 104.2 . . ? Cl4 C130 H130 104.0 . . ? Cl7 C131 Cl9 111.3(9) . . ? Cl7 C131 Cl8 110.2(8) . . ? Cl9 C131 Cl8 109.0(9) . . ? Cl7 C131 H131 108.8 . . ? Cl9 C131 H131 108.8 . . ? Cl8 C131 H131 108.8 . . ? Cl12 C132 Cl11 110.4(10) . . ? Cl12 C132 Cl10 109.3(10) . . ? Cl11 C132 Cl10 110.4(8) . . ? Cl12 C132 H132 109.0 . . ? Cl11 C132 H132 108.9 . . ? Cl10 C132 H132 108.9 . . ? Cl13 C133 Cl14 111.0(8) . . ? Cl13 C133 Cl15 109.3(8) . . ? Cl14 C133 Cl15 108.5(8) . . ? Cl13 C133 H133 109.3 . . ? Cl14 C133 H133 109.4 . . ? Cl15 C133 H133 109.3 . . ? Cl18 C134 Cl17 111.0(14) . . ? Cl18 C134 Cl16 110.1(10) . . ? Cl17 C134 Cl16 110.1(10) . . ? Cl18 C134 H134 108.5 . . ? Cl17 C134 H134 108.5 . . ? Cl16 C134 H134 108.6 . . ? Cl21 C135 Cl20 112.3(8) . . ? Cl21 C135 Cl19 109.8(8) . . ? Cl20 C135 Cl19 109.7(7) . . ? Cl21 C135 H135 108.4 . . ? Cl20 C135 H135 108.2 . . ? Cl19 C135 H135 108.3 . . ? Cl24 C136 Cl22 94.7(14) . . ? Cl24 C136 Cl23 104.0(16) . . ? Cl22 C136 Cl23 99.4(15) . . ? Cl24 C136 H136 118.3 . . ? Cl22 C136 H136 118.2 . . ? Cl23 C136 H136 118.3 . . ? Cl25 C137 Cl26 116.8(15) . . ? Cl25 C137 Cl27 110.4(14) . . ? Cl26 C137 Cl27 110.0(14) . . ? Cl25 C137 H137 106.3 . . ? Cl26 C137 H137 106.4 . . ? Cl27 C137 H137 106.3 . . ? Cl28 C138 Cl29 109(3) . . ? Cl28 C138 Cl30 111.2(16) . . ? Cl29 C138 Cl30 120(2) . . ? Cl28 C138 H138 104.8 . . ? Cl29 C138 H138 104.9 . . ? Cl30 C138 H138 104.9 . . ? Cl31 C139 Cl32 107.3(14) . . ? Cl31 C139 Cl33 116.0(12) . . ? Cl32 C139 Cl33 113.3(13) . . ? Cl31 C139 H139 106.5 . . ? Cl32 C139 H139 106.5 . . ? Cl33 C139 H139 106.6 . . ? Cl34 C140 Cl35 115.0(14) . . ? Cl34 C140 Cl36 109.8(10) . . ? Cl35 C140 Cl36 108.7(12) . . ? Cl34 C140 H140 107.7 . . ? Cl35 C140 H140 107.7 . . ? Cl36 C140 H140 107.7 . . ? H12J C12A H12K 109.5 . . ? H12J C12A H12L 109.5 . . ? H12K C12A H12L 109.5 . . ? H12M C12B H12N 109.4 . . ? H12M C12B H12O 109.4 . . ? H12N C12B H12O 109.4 . . ? H12P C12C H12Q 109.5 . . ? H12P C12C H12R 109.5 . . ? H12Q C12C H12R 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 29.30 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.286 _refine_diff_density_min -1.181 _refine_diff_density_rms 0.218 data_e2087a _database_code_depnum_ccdc_archive 'CCDC 895676' #TrackingRef 'web_deposit_cif_file_8_SylvieFERLAY_1344596913.4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H68 N4 O4 S4, C H Cl3' _chemical_formula_sum 'C65 H69 Cl3 N4 O4 S4' _chemical_formula_weight 1204.83 _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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0521(2) _cell_length_b 14.4897(3) _cell_length_c 20.2847(4) _cell_angle_alpha 79.7800(10) _cell_angle_beta 88.9880(10) _cell_angle_gamma 74.2200(10) _cell_volume 3074.80(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9966 _cell_measurement_theta_min 2.79 _cell_measurement_theta_max 27.90 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1268 _exptl_absorpt_coefficient_mu 0.336 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9608 _exptl_absorpt_correction_T_max 0.9736 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 46446 _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 28.18 _reflns_number_total 14517 _reflns_number_gt 10885 _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. ; _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^)+(0.1087P)^2^+5.1286P] 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 14517 _refine_ls_number_parameters 746 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1003 _refine_ls_R_factor_gt 0.0775 _refine_ls_wR_factor_ref 0.2299 _refine_ls_wR_factor_gt 0.2103 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.023 _refine_ls_shift/su_mean 0.000 _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 S1 S 0.73476(8) 0.21481(6) 0.07597(4) 0.0312(2) Uani 1 1 d . . . C1 C 0.8735(3) 0.1387(2) 0.12007(14) 0.0227(6) Uani 1 1 d . . . C2 C 0.9505(3) 0.1750(2) 0.15624(14) 0.0216(6) Uani 1 1 d . . . C3 C 1.0641(3) 0.1121(2) 0.18487(15) 0.0219(6) Uani 1 1 d . . . C4 C 1.1010(3) 0.0162(2) 0.17422(15) 0.0223(6) Uani 1 1 d . . . H4 H 1.1774 -0.0262 0.1947 0.027 Uiso 1 1 calc R . . C5 C 1.0292(3) -0.0195(2) 0.13422(14) 0.0212(6) Uani 1 1 d . . . C6 C 0.9138(3) 0.0424(2) 0.10921(15) 0.0233(6) Uani 1 1 d . . . H6 H 0.8608 0.0188 0.0840 0.028 Uiso 1 1 calc R . . O1 O 0.9165(2) 0.27184(15) 0.16293(11) 0.0266(5) Uani 1 1 d . . . C7 C 0.9707(4) 0.3282(2) 0.1114(2) 0.0429(9) Uani 1 1 d . . . H7A H 0.9409 0.3227 0.0669 0.051 Uiso 1 1 calc R . . H7B H 1.0634 0.3024 0.1142 0.051 Uiso 1 1 calc R . . C8 C 0.9347(3) 0.4329(2) 0.11903(18) 0.0328(7) Uani 1 1 d . . . C9 C 0.8373(4) 0.4740(3) 0.1568(2) 0.0397(8) Uani 1 1 d . . . H9 H 0.7921 0.4346 0.1835 0.048 Uiso 1 1 calc R . . C10 C 0.8057(4) 0.5743(3) 0.1554(2) 0.0417(9) Uani 1 1 d . . . H10 H 0.7372 0.6019 0.1813 0.050 Uiso 1 1 calc R . . N1 N 0.8658(3) 0.6337(2) 0.12007(19) 0.0470(8) Uani 1 1 d . . . C11 C 0.9632(4) 0.5918(3) 0.0861(2) 0.0483(10) Uani 1 1 d . . . H11 H 1.0092 0.6323 0.0614 0.058 Uiso 1 1 calc R . . C12 C 1.0020(4) 0.4935(3) 0.0844(2) 0.0428(9) Uani 1 1 d . . . H12 H 1.0735 0.4676 0.0599 0.051 Uiso 1 1 calc R . . C13 C 1.0802(3) -0.1235(2) 0.11985(16) 0.0263(6) Uani 1 1 d . . . C14 C 1.0915(4) -0.1973(2) 0.18480(18) 0.0362(8) Uani 1 1 d . . . H14A H 1.1524 -0.1877 0.2156 0.054 Uiso 1 1 calc R . . H14B H 1.1201 -0.2635 0.1750 0.054 Uiso 1 1 calc R . . H14C H 1.0093 -0.1882 0.2055 0.054 Uiso 1 1 calc R . . C15 C 1.2104(3) -0.1334(3) 0.08875(19) 0.0355(8) Uani 1 1 d . . . H15A H 1.2033 -0.0831 0.0487 0.053 Uiso 1 1 calc R . . H15B H 1.2413 -0.1980 0.0764 0.053 Uiso 1 1 calc R . . H15C H 1.2694 -0.1255 0.1214 0.053 Uiso 1 1 calc R . . C16 C 0.9945(4) -0.1451(3) 0.0696(2) 0.0382(8) Uani 1 1 d . . . H16A H 0.9114 -0.1410 0.0886 0.057 Uiso 1 1 calc R . . H16B H 1.0312 -0.2107 0.0600 0.057 Uiso 1 1 calc R . . H16C H 0.9860 -0.0973 0.0280 0.057 Uiso 1 1 calc R . . S2 S 1.17530(7) 0.15397(6) 0.22506(4) 0.02951(19) Uani 1 1 d . . . C17 C 1.0904(3) 0.2111(2) 0.28883(15) 0.0238(6) Uani 1 1 d . . . C18 C 1.0308(3) 0.1605(2) 0.33826(15) 0.0240(6) Uani 1 1 d . . . C19 C 0.9690(3) 0.2081(2) 0.38835(15) 0.0248(6) Uani 1 1 d . . . C20 C 0.9752(3) 0.3023(2) 0.39135(16) 0.0259(6) Uani 1 1 d . . . H20 H 0.9332 0.3338 0.4259 0.031 Uiso 1 1 calc R . . C21 C 1.0415(3) 0.3514(2) 0.34489(16) 0.0247(6) Uani 1 1 d . A . C22 C 1.0950(3) 0.3050(2) 0.29266(15) 0.0251(6) Uani 1 1 d . . . H22 H 1.1359 0.3383 0.2587 0.030 Uiso 1 1 calc R . . O2 O 1.0346(2) 0.06444(15) 0.33755(11) 0.0293(5) Uani 1 1 d . . . C23 C 1.1499(4) -0.0007(2) 0.3684(2) 0.0410(9) Uani 1 1 d . . . H23A H 1.1524 0.0027 0.4167 0.049 Uiso 1 1 calc R . . H23B H 1.2224 0.0197 0.3475 0.049 Uiso 1 1 calc R . . C24 C 1.1599(4) -0.1034(2) 0.36039(17) 0.0379(8) Uani 1 1 d . . . C25 C 1.0571(5) -0.1389(3) 0.3574(2) 0.0459(10) Uani 1 1 d . . . H25 H 0.9742 -0.0971 0.3566 0.055 Uiso 1 1 calc R . . C26 C 1.0770(6) -0.2372(3) 0.3556(2) 0.0584(13) Uani 1 1 d . . . H26 H 1.0047 -0.2605 0.3543 0.070 Uiso 1 1 calc R . . N2 N 1.1877(5) -0.3010(3) 0.3556(2) 0.0638(12) Uani 1 1 d . . . C27 C 1.2856(6) -0.2656(3) 0.3572(3) 0.0721(16) Uani 1 1 d . . . H27 H 1.3671 -0.3091 0.3569 0.087 Uiso 1 1 calc R . . C28 C 1.2766(5) -0.1683(3) 0.3594(3) 0.0608(13) Uani 1 1 d . . . H28 H 1.3506 -0.1470 0.3601 0.073 Uiso 1 1 calc R . . C29 C 1.0579(3) 0.4515(2) 0.35093(17) 0.0289(7) Uani 1 1 d D . . C30 C 1.0075(6) 0.4835(4) 0.4175(3) 0.0404(15) Uani 0.679(7) 1 d PD A 1 H30A H 1.0501 0.4341 0.4554 0.061 Uiso 0.679(7) 1 calc PR A 1 H30B H 0.9167 0.4908 0.4189 0.061 Uiso 0.679(7) 1 calc PR A 1 H30C H 1.0237 0.5460 0.4203 0.061 Uiso 0.679(7) 1 calc PR A 1 C31 C 1.2022(5) 0.4400(4) 0.3546(4) 0.0464(16) Uani 0.679(7) 1 d PD A 1 H31A H 1.2167 0.5009 0.3628 0.070 Uiso 0.679(7) 1 calc PR A 1 H31B H 1.2391 0.4252 0.3122 0.070 Uiso 0.679(7) 1 calc PR A 1 H31C H 1.2413 0.3868 0.3913 0.070 Uiso 0.679(7) 1 calc PR A 1 C32 C 0.9966(7) 0.5279(4) 0.2927(3) 0.0506(18) Uani 0.679(7) 1 d PD A 1 H32A H 1.0104 0.5904 0.2975 0.076 Uiso 0.679(7) 1 calc PR A 1 H32B H 0.9061 0.5341 0.2914 0.076 Uiso 0.679(7) 1 calc PR A 1 H32C H 1.0332 0.5092 0.2511 0.076 Uiso 0.679(7) 1 calc PR A 1 C30A C 0.9227(11) 0.5241(8) 0.3554(8) 0.050(4) Uani 0.321(7) 1 d PD A 2 H30D H 0.8816 0.4999 0.3954 0.075 Uiso 0.321(7) 1 calc PR A 2 H30E H 0.8717 0.5284 0.3154 0.075 Uiso 0.321(7) 1 calc PR A 2 H30F H 0.9315 0.5888 0.3581 0.075 Uiso 0.321(7) 1 calc PR A 2 C31A C 1.1391(16) 0.4441(9) 0.4088(6) 0.056(4) Uani 0.321(7) 1 d PD A 2 H31D H 1.1382 0.5096 0.4155 0.084 Uiso 0.321(7) 1 calc PR A 2 H31E H 1.2253 0.4078 0.4009 0.084 Uiso 0.321(7) 1 calc PR A 2 H31F H 1.1083 0.4099 0.4489 0.084 Uiso 0.321(7) 1 calc PR A 2 C32A C 1.1062(13) 0.5011(8) 0.2847(5) 0.038(3) Uani 0.321(7) 1 d PD A 2 H32D H 1.1070 0.5674 0.2887 0.057 Uiso 0.321(7) 1 calc PR A 2 H32E H 1.0503 0.5039 0.2471 0.057 Uiso 0.321(7) 1 calc PR A 2 H32F H 1.1916 0.4631 0.2770 0.057 Uiso 0.321(7) 1 calc PR A 2 S3 S 0.90173(9) 0.14599(7) 0.45651(4) 0.0349(2) Uani 1 1 d . . . C33 C 0.7847(3) 0.1058(2) 0.41982(15) 0.0271(6) Uani 1 1 d . . . C34 C 0.6864(3) 0.1708(2) 0.38011(16) 0.0277(6) Uani 1 1 d . . . C35 C 0.5931(3) 0.1356(2) 0.35545(16) 0.0271(6) Uani 1 1 d . . . C36 C 0.5956(3) 0.0381(2) 0.37542(17) 0.0287(7) Uani 1 1 d . . . H36 H 0.5326 0.0147 0.3581 0.034 Uiso 1 1 calc R . . C37 C 0.6874(3) -0.0260(2) 0.41988(16) 0.0274(6) Uani 1 1 d . . . C38 C 0.7852(3) 0.0081(2) 0.43937(16) 0.0280(6) Uani 1 1 d . . . H38 H 0.8534 -0.0357 0.4664 0.034 Uiso 1 1 calc R . . O3 O 0.6791(2) 0.26908(16) 0.36708(12) 0.0324(5) Uani 1 1 d . . . C39 C 0.6159(6) 0.3132(3) 0.4213(3) 0.0658(15) Uani 1 1 d . . . H39A H 0.6542 0.2743 0.4647 0.079 Uiso 1 1 calc R . . H39B H 0.5261 0.3141 0.4201 0.079 Uiso 1 1 calc R . . C40 C 0.6266(4) 0.4146(3) 0.4152(2) 0.0393(8) Uani 1 1 d . . . C41 C 0.6227(6) 0.4760(4) 0.3558(3) 0.0741(17) Uani 1 1 d . . . H41 H 0.6138 0.4538 0.3153 0.089 Uiso 1 1 calc R . . C42 C 0.6311(6) 0.5681(4) 0.3530(4) 0.0846(19) Uani 1 1 d . . . H42 H 0.6319 0.6077 0.3104 0.101 Uiso 1 1 calc R . . N3 N 0.6382(5) 0.6039(3) 0.4063(3) 0.0771(13) Uani 1 1 d . . . C43 C 0.6533(5) 0.5510(4) 0.4644(3) 0.0664(14) Uani 1 1 d . . . H43 H 0.6673 0.5773 0.5024 0.080 Uiso 1 1 calc R . . C44 C 0.6490(5) 0.4479(5) 0.4725(3) 0.0694(14) Uani 1 1 d . . . H44 H 0.6611 0.4066 0.5152 0.083 Uiso 1 1 calc R . . C45 C 0.6833(5) -0.1313(4) 0.4450(4) 0.0792(9) Uani 1 1 d . . . C46 C 0.7946(5) -0.2063(4) 0.4352(4) 0.0792(9) Uani 1 1 d . . . H46A H 0.7818 -0.2704 0.4526 0.119 Uiso 1 1 calc R . . H46B H 0.8664 -0.1985 0.4591 0.119 Uiso 1 1 calc R . . H46C H 0.8112 -0.2010 0.3873 0.119 Uiso 1 1 calc R . . C47 C 0.5593(5) -0.1471(4) 0.4404(4) 0.0792(9) Uani 1 1 d . . . H47A H 0.5321 -0.1352 0.3932 0.119 Uiso 1 1 calc R . . H47B H 0.4991 -0.1024 0.4641 0.119 Uiso 1 1 calc R . . H47C H 0.5633 -0.2146 0.4607 0.119 Uiso 1 1 calc R . . C48 C 0.6868(5) -0.1454(4) 0.5287(4) 0.0792(9) Uani 1 1 d . . . H48A H 0.6680 -0.2068 0.5478 0.119 Uiso 1 1 calc R . . H48B H 0.6239 -0.0909 0.5427 0.119 Uiso 1 1 calc R . . H48C H 0.7706 -0.1468 0.5447 0.119 Uiso 1 1 calc R . . S4 S 0.45868(8) 0.21398(6) 0.30807(5) 0.0361(2) Uani 1 1 d . . . C49 C 0.5198(3) 0.2730(2) 0.23610(17) 0.0271(6) Uani 1 1 d . . . C50 C 0.6014(3) 0.2215(2) 0.19343(16) 0.0246(6) Uani 1 1 d . . . C51 C 0.6402(3) 0.2732(2) 0.13653(15) 0.0245(6) Uani 1 1 d . . . C52 C 0.5899(3) 0.3747(2) 0.11966(16) 0.0266(6) Uani 1 1 d . . . H52 H 0.6171 0.4090 0.0805 0.032 Uiso 1 1 calc R . . C53 C 0.5015(3) 0.4261(2) 0.15874(17) 0.0269(6) Uani 1 1 d . . . C54 C 0.4703(3) 0.3736(2) 0.21803(18) 0.0293(7) Uani 1 1 d . . . H54 H 0.4135 0.4075 0.2470 0.035 Uiso 1 1 calc R . . O4 O 0.6396(2) 0.12057(15) 0.20701(12) 0.0283(5) Uani 1 1 d . . . C55 C 0.5494(4) 0.0826(3) 0.1781(2) 0.0434(9) Uani 1 1 d . . . H55A H 0.5485 0.1005 0.1287 0.052 Uiso 1 1 calc R . . H55B H 0.4643 0.1122 0.1934 0.052 Uiso 1 1 calc R . . C56 C 0.5811(3) -0.0261(2) 0.1981(2) 0.0369(8) Uani 1 1 d . . . C57 C 0.7026(4) -0.0855(3) 0.2052(3) 0.0692(17) Uani 1 1 d . . . H57 H 0.7721 -0.0584 0.2013 0.083 Uiso 1 1 calc R . . C58 C 0.7213(5) -0.1854(3) 0.2182(4) 0.087(2) Uani 1 1 d . . . H58 H 0.8057 -0.2251 0.2219 0.104 Uiso 1 1 calc R . . N4 N 0.6312(4) -0.2297(2) 0.2258(2) 0.0610(11) Uani 1 1 d . . . C59 C 0.5148(4) -0.1719(3) 0.2206(3) 0.0556(12) Uani 1 1 d . . . H59 H 0.4474 -0.2013 0.2265 0.067 Uiso 1 1 calc R . . C60 C 0.4856(4) -0.0710(3) 0.2071(3) 0.0512(11) Uani 1 1 d . . . H60 H 0.4003 -0.0331 0.2040 0.061 Uiso 1 1 calc R . . C61 C 0.4324(3) 0.5350(2) 0.13674(18) 0.0311(7) Uani 1 1 d . . . C62 C 0.2981(4) 0.5417(3) 0.1142(3) 0.0549(12) Uani 1 1 d . . . H62A H 0.2535 0.5168 0.1524 0.082 Uiso 1 1 calc R . . H62B H 0.3013 0.5027 0.0790 0.082 Uiso 1 1 calc R . . H62C H 0.2538 0.6099 0.0966 0.082 Uiso 1 1 calc R . . C63 C 0.4284(4) 0.5907(3) 0.1942(2) 0.0422(9) Uani 1 1 d . . . H63A H 0.5144 0.5864 0.2083 0.063 Uiso 1 1 calc R . . H63B H 0.3859 0.5622 0.2320 0.063 Uiso 1 1 calc R . . H63C H 0.3824 0.6592 0.1793 0.063 Uiso 1 1 calc R . . C64 C 0.4949(4) 0.5840(3) 0.0776(2) 0.0451(9) Uani 1 1 d . . . H64A H 0.4474 0.6526 0.0649 0.068 Uiso 1 1 calc R . . H64B H 0.4958 0.5508 0.0394 0.068 Uiso 1 1 calc R . . H64C H 0.5814 0.5798 0.0907 0.068 Uiso 1 1 calc R . . C65 C 0.3246(4) 0.2023(3) -0.0028(2) 0.0429(9) Uani 1 1 d . . . H65 H 0.2672 0.2347 -0.0428 0.051 Uiso 1 1 calc R . . Cl1 Cl 0.26031(12) 0.11683(9) 0.04660(6) 0.0624(3) Uani 1 1 d . . . Cl2 Cl 0.47273(13) 0.14634(11) -0.03052(8) 0.0740(4) Uani 1 1 d . . . Cl3 Cl 0.33591(12) 0.29156(9) 0.04364(6) 0.0598(3) Uani 1 1 d . . . _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 S1 0.0345(4) 0.0263(4) 0.0250(4) -0.0082(3) -0.0053(3) 0.0073(3) C1 0.0246(14) 0.0199(14) 0.0213(13) -0.0045(11) 0.0017(11) -0.0018(11) C2 0.0261(14) 0.0150(13) 0.0237(14) -0.0075(10) 0.0073(11) -0.0034(11) C3 0.0237(14) 0.0202(14) 0.0248(14) -0.0095(11) 0.0057(11) -0.0077(11) C4 0.0213(13) 0.0193(14) 0.0257(14) -0.0066(11) 0.0015(11) -0.0031(11) C5 0.0238(14) 0.0159(13) 0.0235(14) -0.0069(10) 0.0039(11) -0.0029(11) C6 0.0259(14) 0.0208(14) 0.0233(14) -0.0065(11) -0.0009(11) -0.0046(11) O1 0.0324(11) 0.0149(10) 0.0327(11) -0.0094(8) 0.0089(9) -0.0044(8) C7 0.057(2) 0.0214(16) 0.051(2) -0.0103(15) 0.0218(19) -0.0109(16) C8 0.0344(17) 0.0204(15) 0.0425(19) -0.0047(13) -0.0012(14) -0.0062(13) C9 0.0359(18) 0.0264(17) 0.060(2) -0.0136(16) 0.0067(17) -0.0108(14) C10 0.0364(19) 0.0261(17) 0.062(2) -0.0156(17) -0.0014(17) -0.0030(15) N1 0.052(2) 0.0237(15) 0.065(2) -0.0073(15) -0.0094(17) -0.0089(14) C11 0.059(3) 0.0289(19) 0.060(3) -0.0040(17) 0.004(2) -0.0199(18) C12 0.045(2) 0.0292(18) 0.055(2) -0.0058(16) 0.0039(18) -0.0126(16) C13 0.0316(16) 0.0156(13) 0.0300(15) -0.0071(11) 0.0003(13) -0.0019(12) C14 0.046(2) 0.0212(16) 0.0374(18) -0.0022(13) 0.0015(15) -0.0047(14) C15 0.0392(19) 0.0256(16) 0.0390(18) -0.0125(14) 0.0070(15) -0.0003(14) C16 0.044(2) 0.0254(17) 0.047(2) -0.0168(15) -0.0068(16) -0.0057(15) S2 0.0246(4) 0.0317(4) 0.0395(4) -0.0195(3) 0.0065(3) -0.0119(3) C17 0.0246(14) 0.0216(14) 0.0289(15) -0.0096(12) 0.0022(12) -0.0091(12) C18 0.0289(15) 0.0179(13) 0.0282(15) -0.0067(11) -0.0044(12) -0.0096(12) C19 0.0285(15) 0.0259(15) 0.0239(14) -0.0026(11) -0.0006(12) -0.0151(12) C20 0.0282(15) 0.0245(15) 0.0290(15) -0.0100(12) 0.0028(12) -0.0107(12) C21 0.0249(14) 0.0213(14) 0.0317(15) -0.0079(12) 0.0014(12) -0.0104(12) C22 0.0285(15) 0.0226(14) 0.0281(15) -0.0067(12) 0.0038(12) -0.0122(12) O2 0.0385(12) 0.0195(10) 0.0346(12) -0.0072(9) -0.0043(10) -0.0140(9) C23 0.058(2) 0.0240(17) 0.0409(19) -0.0034(14) -0.0182(17) -0.0118(16) C24 0.064(2) 0.0234(16) 0.0250(16) -0.0016(13) -0.0067(16) -0.0114(16) C25 0.070(3) 0.0307(19) 0.044(2) -0.0153(16) 0.017(2) -0.0220(19) C26 0.100(4) 0.036(2) 0.052(2) -0.0164(19) 0.025(3) -0.035(3) N2 0.110(4) 0.0252(17) 0.053(2) -0.0045(15) 0.005(2) -0.014(2) C27 0.090(4) 0.033(2) 0.078(4) -0.009(2) -0.032(3) 0.010(2) C28 0.063(3) 0.039(2) 0.075(3) -0.008(2) -0.026(2) -0.004(2) C29 0.0354(17) 0.0187(14) 0.0377(17) -0.0122(12) 0.0090(14) -0.0122(13) C30 0.055(4) 0.028(3) 0.047(3) -0.020(2) 0.015(3) -0.017(2) C31 0.040(3) 0.041(3) 0.073(4) -0.028(3) 0.015(3) -0.025(3) C32 0.078(5) 0.028(3) 0.044(3) -0.002(2) -0.011(3) -0.014(3) C30A 0.058(8) 0.020(5) 0.075(9) -0.018(6) 0.033(7) -0.012(5) C31A 0.099(12) 0.033(6) 0.049(8) -0.007(5) -0.017(8) -0.037(7) C32A 0.059(8) 0.024(5) 0.041(6) -0.009(4) 0.015(5) -0.026(5) S3 0.0528(5) 0.0419(5) 0.0220(4) -0.0048(3) 0.0014(3) -0.0334(4) C33 0.0344(16) 0.0306(16) 0.0233(14) -0.0074(12) 0.0067(12) -0.0194(13) C34 0.0348(17) 0.0254(15) 0.0277(15) -0.0072(12) 0.0110(13) -0.0155(13) C35 0.0280(15) 0.0245(15) 0.0303(15) -0.0064(12) 0.0079(12) -0.0090(12) C36 0.0277(15) 0.0281(16) 0.0341(16) -0.0085(13) 0.0045(13) -0.0126(13) C37 0.0309(16) 0.0246(15) 0.0305(16) -0.0075(12) 0.0034(13) -0.0124(13) C38 0.0342(17) 0.0274(16) 0.0266(15) -0.0058(12) 0.0031(13) -0.0151(13) O3 0.0412(13) 0.0222(11) 0.0378(13) -0.0075(9) 0.0122(10) -0.0146(10) C39 0.092(4) 0.036(2) 0.079(3) -0.026(2) 0.048(3) -0.027(2) C40 0.048(2) 0.0256(17) 0.045(2) -0.0105(15) 0.0055(17) -0.0093(15) C41 0.100(4) 0.060(3) 0.065(3) 0.018(2) -0.036(3) -0.044(3) C42 0.111(5) 0.040(3) 0.100(5) 0.004(3) -0.036(4) -0.024(3) N3 0.082(3) 0.054(3) 0.098(4) -0.023(3) -0.002(3) -0.015(2) C43 0.066(3) 0.074(4) 0.072(3) -0.045(3) 0.008(3) -0.019(3) C44 0.061(3) 0.095(4) 0.050(3) -0.015(3) 0.013(2) -0.016(3) C45 0.0597(15) 0.0427(13) 0.130(3) 0.0089(15) 0.0016(17) -0.0213(11) C46 0.0597(15) 0.0427(13) 0.130(3) 0.0089(15) 0.0016(17) -0.0213(11) C47 0.0597(15) 0.0427(13) 0.130(3) 0.0089(15) 0.0016(17) -0.0213(11) C48 0.0597(15) 0.0427(13) 0.130(3) 0.0089(15) 0.0016(17) -0.0213(11) S4 0.0240(4) 0.0296(4) 0.0494(5) 0.0018(4) 0.0097(4) -0.0048(3) C49 0.0201(14) 0.0210(14) 0.0386(17) -0.0039(12) 0.0017(12) -0.0039(11) C50 0.0203(13) 0.0150(13) 0.0355(16) -0.0051(11) -0.0053(12) 0.0009(11) C51 0.0221(14) 0.0199(14) 0.0285(15) -0.0069(11) -0.0037(11) 0.0013(11) C52 0.0262(15) 0.0206(14) 0.0282(15) -0.0018(12) -0.0053(12) 0.0002(12) C53 0.0227(14) 0.0179(14) 0.0370(17) -0.0053(12) -0.0056(12) 0.0003(11) C54 0.0232(14) 0.0200(15) 0.0426(18) -0.0092(13) 0.0035(13) -0.0001(12) O4 0.0266(11) 0.0141(10) 0.0418(13) -0.0038(9) -0.0045(9) -0.0017(8) C55 0.040(2) 0.0230(17) 0.068(3) -0.0073(17) -0.0141(18) -0.0092(15) C56 0.0377(18) 0.0225(16) 0.053(2) -0.0143(15) 0.0051(16) -0.0084(14) C57 0.034(2) 0.0240(19) 0.147(5) -0.011(2) 0.019(3) -0.0089(16) C58 0.042(2) 0.026(2) 0.187(7) -0.018(3) 0.029(3) -0.0026(19) N4 0.058(2) 0.0265(17) 0.104(3) -0.0209(19) 0.025(2) -0.0160(16) C59 0.054(3) 0.036(2) 0.086(3) -0.017(2) 0.003(2) -0.024(2) C60 0.036(2) 0.033(2) 0.088(3) -0.018(2) -0.002(2) -0.0103(16) C61 0.0294(16) 0.0158(14) 0.0424(19) -0.0055(13) -0.0073(14) 0.0043(12) C62 0.038(2) 0.030(2) 0.090(3) -0.009(2) -0.026(2) 0.0024(16) C63 0.054(2) 0.0204(16) 0.048(2) -0.0079(15) -0.0032(18) -0.0003(15) C64 0.060(2) 0.0230(17) 0.042(2) 0.0022(15) -0.0029(18) 0.0022(16) C65 0.047(2) 0.039(2) 0.039(2) 0.0055(16) -0.0035(17) -0.0134(17) Cl1 0.0702(7) 0.0673(7) 0.0587(7) 0.0042(6) -0.0001(6) -0.0434(6) Cl2 0.0618(8) 0.0716(9) 0.0872(10) -0.0231(7) 0.0270(7) -0.0117(6) Cl3 0.0714(7) 0.0506(6) 0.0638(7) -0.0164(5) 0.0084(6) -0.0237(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C1 1.774(3) . ? S1 C51 1.778(3) . ? C1 C2 1.393(4) . ? C1 C6 1.400(4) . ? C2 O1 1.381(3) . ? C2 C3 1.400(4) . ? C3 C4 1.393(4) . ? C3 S2 1.778(3) . ? C4 C5 1.397(4) . ? C4 H4 0.9500 . ? C5 C6 1.388(4) . ? C5 C13 1.538(4) . ? C6 H6 0.9500 . ? O1 C7 1.435(4) . ? C7 C8 1.495(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.372(5) . ? C8 C12 1.392(5) . ? C9 C10 1.395(5) . ? C9 H9 0.9500 . ? C10 N1 1.331(5) . ? C10 H10 0.9500 . ? N1 C11 1.330(6) . ? C11 C12 1.377(5) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.526(5) . ? C13 C16 1.530(5) . ? C13 C15 1.542(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? S2 C17 1.776(3) . ? C17 C22 1.391(4) . ? C17 C18 1.398(4) . ? C18 O2 1.383(3) . ? C18 C19 1.394(4) . ? C19 C20 1.397(4) . ? C19 S3 1.778(3) . ? C20 C21 1.397(4) . ? C20 H20 0.9500 . ? C21 C22 1.393(4) . ? C21 C29 1.535(4) . ? C22 H22 0.9500 . ? O2 C23 1.439(4) . ? C23 C24 1.500(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.375(6) . ? C24 C28 1.377(6) . ? C25 C26 1.388(5) . ? C25 H25 0.9500 . ? C26 N2 1.317(7) . ? C26 H26 0.9500 . ? N2 C27 1.320(7) . ? C27 C28 1.394(7) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C31A 1.462(11) . ? C29 C32 1.495(6) . ? C29 C30 1.551(6) . ? C29 C31 1.559(6) . ? C29 C32A 1.564(10) . ? C29 C30A 1.588(11) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C30A H30D 0.9800 . ? C30A H30E 0.9800 . ? C30A H30F 0.9800 . ? C31A H31D 0.9800 . ? C31A H31E 0.9800 . ? C31A H31F 0.9800 . ? C32A H32D 0.9800 . ? C32A H32E 0.9800 . ? C32A H32F 0.9800 . ? S3 C33 1.779(3) . ? C33 C34 1.386(5) . ? C33 C38 1.399(4) . ? C34 O3 1.381(4) . ? C34 C35 1.403(4) . ? C35 C36 1.392(4) . ? C35 S4 1.779(3) . ? C36 C37 1.389(5) . ? C36 H36 0.9500 . ? C37 C38 1.394(4) . ? C37 C45 1.533(6) . ? C38 H38 0.9500 . ? O3 C39 1.444(5) . ? C39 C40 1.488(5) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.358(6) . ? C40 C44 1.385(7) . ? C41 C42 1.354(7) . ? C41 H41 0.9500 . ? C42 N3 1.291(8) . ? C42 H42 0.9500 . ? N3 C43 1.274(8) . ? C43 C44 1.488(8) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.441(8) . ? C45 C47 1.458(7) . ? C45 C48 1.673(10) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? S4 C49 1.776(3) . ? C49 C54 1.394(4) . ? C49 C50 1.398(4) . ? C50 O4 1.385(3) . ? C50 C51 1.388(4) . ? C51 C52 1.404(4) . ? C52 C53 1.387(4) . ? C52 H52 0.9500 . ? C53 C54 1.396(5) . ? C53 C61 1.542(4) . ? C54 H54 0.9500 . ? O4 C55 1.440(4) . ? C55 C56 1.499(5) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C60 1.376(5) . ? C56 C57 1.379(6) . ? C57 C58 1.382(6) . ? C57 H57 0.9500 . ? C58 N4 1.318(6) . ? C58 H58 0.9500 . ? N4 C59 1.325(6) . ? C59 C60 1.386(6) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 C63 1.525(5) . ? C61 C64 1.534(5) . ? C61 C62 1.534(5) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 Cl1 1.748(4) . ? C65 Cl2 1.750(4) . ? C65 Cl3 1.761(4) . ? C65 H65 1.0000 . ? _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 C1 S1 C51 105.84(14) . . ? C2 C1 C6 120.0(3) . . ? C2 C1 S1 122.2(2) . . ? C6 C1 S1 117.1(2) . . ? O1 C2 C1 120.7(3) . . ? O1 C2 C3 120.3(3) . . ? C1 C2 C3 119.0(3) . . ? C4 C3 C2 119.8(3) . . ? C4 C3 S2 117.3(2) . . ? C2 C3 S2 122.3(2) . . ? C3 C4 C5 121.9(3) . . ? C3 C4 H4 119.0 . . ? C5 C4 H4 119.0 . . ? C6 C5 C4 117.3(3) . . ? C6 C5 C13 123.3(3) . . ? C4 C5 C13 119.4(3) . . ? C5 C6 C1 121.8(3) . . ? C5 C6 H6 119.1 . . ? C1 C6 H6 119.1 . . ? C2 O1 C7 110.5(2) . . ? O1 C7 C8 110.4(3) . . ? 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 . . ? C9 C8 C12 117.5(3) . . ? C9 C8 C7 124.3(3) . . ? C12 C8 C7 118.2(3) . . ? C8 C9 C10 119.0(4) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? N1 C10 C9 123.8(4) . . ? N1 C10 H10 118.1 . . ? C9 C10 H10 118.1 . . ? C11 N1 C10 116.2(3) . . ? N1 C11 C12 124.3(4) . . ? N1 C11 H11 117.8 . . ? C12 C11 H11 117.8 . . ? C11 C12 C8 119.0(4) . . ? C11 C12 H12 120.5 . . ? C8 C12 H12 120.5 . . ? C14 C13 C16 109.2(3) . . ? C14 C13 C5 109.9(3) . . ? C16 C13 C5 111.4(3) . . ? C14 C13 C15 110.0(3) . . ? C16 C13 C15 107.6(3) . . ? C5 C13 C15 108.7(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C17 S2 C3 104.63(13) . . ? C22 C17 C18 120.1(3) . . ? C22 C17 S2 118.1(2) . . ? C18 C17 S2 121.4(2) . . ? O2 C18 C19 120.9(3) . . ? O2 C18 C17 120.2(3) . . ? C19 C18 C17 118.9(3) . . ? C18 C19 C20 119.9(3) . . ? C18 C19 S3 121.5(2) . . ? C20 C19 S3 117.9(2) . . ? C21 C20 C19 121.8(3) . . ? C21 C20 H20 119.1 . . ? C19 C20 H20 119.1 . . ? C22 C21 C20 117.2(3) . . ? C22 C21 C29 120.6(3) . . ? C20 C21 C29 122.3(3) . . ? C17 C22 C21 121.9(3) . . ? C17 C22 H22 119.1 . . ? C21 C22 H22 119.1 . . ? C18 O2 C23 111.0(2) . . ? O2 C23 C24 110.6(3) . . ? O2 C23 H23A 109.5 . . ? C24 C23 H23A 109.5 . . ? O2 C23 H23B 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 108.1 . . ? C25 C24 C28 117.0(4) . . ? C25 C24 C23 123.2(4) . . ? C28 C24 C23 119.7(4) . . ? C24 C25 C26 118.6(4) . . ? C24 C25 H25 120.7 . . ? C26 C25 H25 120.7 . . ? N2 C26 C25 125.5(5) . . ? N2 C26 H26 117.3 . . ? C25 C26 H26 117.3 . . ? C27 N2 C26 115.3(4) . . ? N2 C27 C28 124.1(5) . . ? N2 C27 H27 118.0 . . ? C28 C27 H27 118.0 . . ? C24 C28 C27 119.5(5) . . ? C24 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? C31A C29 C32 137.2(6) . . ? C31A C29 C21 111.0(5) . . ? C32 C29 C21 111.5(3) . . ? C31A C29 C30 56.6(7) . . ? C32 C29 C30 110.0(4) . . ? C21 C29 C30 112.2(3) . . ? C31A C29 C31 50.6(7) . . ? C32 C29 C31 110.8(4) . . ? C21 C29 C31 107.0(3) . . ? C30 C29 C31 105.2(4) . . ? C31A C29 C32A 111.8(8) . . ? C32 C29 C32A 45.5(6) . . ? C21 C29 C32A 111.7(4) . . ? C30 C29 C32A 135.5(5) . . ? C31 C29 C32A 67.6(6) . . ? C31A C29 C30A 111.7(9) . . ? C32 C29 C30A 58.1(6) . . ? C21 C29 C30A 108.4(5) . . ? C30 C29 C30A 57.7(6) . . ? C31 C29 C30A 144.4(5) . . ? C32A C29 C30A 101.7(7) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? C29 C30A H30D 109.5 . . ? C29 C30A H30E 109.5 . . ? H30D C30A H30E 109.5 . . ? C29 C30A H30F 109.5 . . ? H30D C30A H30F 109.5 . . ? H30E C30A H30F 109.5 . . ? C29 C31A H31D 109.5 . . ? C29 C31A H31E 109.5 . . ? H31D C31A H31E 109.5 . . ? C29 C31A H31F 109.5 . . ? H31D C31A H31F 109.5 . . ? H31E C31A H31F 109.5 . . ? C29 C32A H32D 109.5 . . ? C29 C32A H32E 109.5 . . ? H32D C32A H32E 109.5 . . ? C29 C32A H32F 109.5 . . ? H32D C32A H32F 109.5 . . ? H32E C32A H32F 109.5 . . ? C19 S3 C33 105.52(14) . . ? C34 C33 C38 120.3(3) . . ? C34 C33 S3 121.5(2) . . ? C38 C33 S3 117.7(3) . . ? O3 C34 C33 120.1(3) . . ? O3 C34 C35 120.9(3) . . ? C33 C34 C35 119.0(3) . . ? C36 C35 C34 119.6(3) . . ? C36 C35 S4 117.5(2) . . ? C34 C35 S4 122.4(2) . . ? C37 C36 C35 122.0(3) . . ? C37 C36 H36 119.0 . . ? C35 C36 H36 119.0 . . ? C36 C37 C38 117.6(3) . . ? C36 C37 C45 121.1(3) . . ? C38 C37 C45 121.2(4) . . ? C37 C38 C33 121.1(3) . . ? C37 C38 H38 119.4 . . ? C33 C38 H38 119.4 . . ? C34 O3 C39 108.8(3) . . ? O3 C39 C40 110.1(3) . . ? O3 C39 H39A 109.6 . . ? C40 C39 H39A 109.6 . . ? O3 C39 H39B 109.6 . . ? C40 C39 H39B 109.6 . . ? H39A C39 H39B 108.2 . . ? C41 C40 C44 116.9(4) . . ? C41 C40 C39 123.9(4) . . ? C44 C40 C39 119.1(4) . . ? C42 C41 C40 121.6(6) . . ? C42 C41 H41 119.2 . . ? C40 C41 H41 119.2 . . ? N3 C42 C41 122.2(6) . . ? N3 C42 H42 118.9 . . ? C41 C42 H42 118.9 . . ? C43 N3 C42 121.7(5) . . ? N3 C43 C44 119.6(5) . . ? N3 C43 H43 120.2 . . ? C44 C43 H43 120.2 . . ? C40 C44 C43 117.3(5) . . ? C40 C44 H44 121.4 . . ? C43 C44 H44 121.4 . . ? C46 C45 C47 120.3(5) . . ? C46 C45 C37 116.1(4) . . ? C47 C45 C37 114.6(4) . . ? C46 C45 C48 100.3(5) . . ? C47 C45 C48 94.7(5) . . ? C37 C45 C48 105.5(5) . . ? 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 . . ? C49 S4 C35 105.06(14) . . ? C54 C49 C50 119.8(3) . . ? C54 C49 S4 117.1(2) . . ? C50 C49 S4 122.6(2) . . ? O4 C50 C51 120.9(3) . . ? O4 C50 C49 120.2(3) . . ? C51 C50 C49 118.8(3) . . ? C50 C51 C52 120.1(3) . . ? C50 C51 S1 122.5(2) . . ? C52 C51 S1 116.7(2) . . ? C53 C52 C51 121.7(3) . . ? C53 C52 H52 119.1 . . ? C51 C52 H52 119.1 . . ? C52 C53 C54 117.1(3) . . ? C52 C53 C61 122.7(3) . . ? C54 C53 C61 120.1(3) . . ? C49 C54 C53 122.1(3) . . ? C49 C54 H54 119.0 . . ? C53 C54 H54 119.0 . . ? C50 O4 C55 109.6(2) . . ? O4 C55 C56 110.8(3) . . ? O4 C55 H55A 109.5 . . ? C56 C55 H55A 109.5 . . ? O4 C55 H55B 109.5 . . ? C56 C55 H55B 109.5 . . ? H55A C55 H55B 108.1 . . ? C60 C56 C57 117.0(3) . . ? C60 C56 C55 119.5(3) . . ? C57 C56 C55 123.4(3) . . ? C56 C57 C58 118.7(4) . . ? C56 C57 H57 120.6 . . ? C58 C57 H57 120.6 . . ? N4 C58 C57 125.1(4) . . ? N4 C58 H58 117.5 . . ? C57 C58 H58 117.5 . . ? C58 N4 C59 115.7(4) . . ? N4 C59 C60 123.8(4) . . ? N4 C59 H59 118.1 . . ? C60 C59 H59 118.1 . . ? C56 C60 C59 119.6(4) . . ? C56 C60 H60 120.2 . . ? C59 C60 H60 120.2 . . ? C63 C61 C64 108.0(3) . . ? C63 C61 C62 109.8(3) . . ? C64 C61 C62 108.0(3) . . ? C63 C61 C53 111.1(3) . . ? C64 C61 C53 112.2(3) . . ? C62 C61 C53 107.6(3) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? Cl1 C65 Cl2 111.1(2) . . ? Cl1 C65 Cl3 109.4(2) . . ? Cl2 C65 Cl3 110.2(2) . . ? Cl1 C65 H65 108.7 . . ? Cl2 C65 H65 108.7 . . ? Cl3 C65 H65 108.7 . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 28.18 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 0.785 _refine_diff_density_min -0.483 _refine_diff_density_rms 0.094 data_e2326a _database_code_depnum_ccdc_archive 'CCDC 895677' #TrackingRef 'web_deposit_cif_file_9_SylvieFERLAY_1344596913.4-AgPF6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C67 H75 Ag N5 O5 S4,F6 P,C H4 O,C H Cl3' _chemical_formula_sum 'C69 H80 Ag Cl3 F6 N5 O6 P S4' _chemical_formula_weight 1562.81 _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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.8181(3) _cell_length_b 32.1705(6) _cell_length_c 15.1669(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.7100(10) _cell_angle_gamma 90.00 _cell_volume 7215.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9183 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 29.27 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3232 _exptl_absorpt_coefficient_mu 0.598 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9538 _exptl_absorpt_correction_T_max 0.9650 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 84333 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -45 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 30.05 _reflns_number_total 20904 _reflns_number_gt 15583 _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. ; _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^)+(0.0938P)^2^+12.6866P] 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 20904 _refine_ls_number_parameters 860 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0831 _refine_ls_R_factor_gt 0.0608 _refine_ls_wR_factor_ref 0.1833 _refine_ls_wR_factor_gt 0.1664 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _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 0.74758(2) 0.044020(7) 0.113481(18) 0.03760(9) Uani 1 1 d . . . S1 S 0.55023(5) 0.29207(2) 0.15049(5) 0.02659(15) Uani 1 1 d . . . C1 C 0.55669(19) 0.27022(8) 0.25808(18) 0.0213(5) Uani 1 1 d . . . C2 C 0.57676(19) 0.29309(8) 0.33484(18) 0.0205(5) Uani 1 1 d . . . C3 C 0.5654(2) 0.27403(9) 0.41644(18) 0.0229(5) Uani 1 1 d . . . C4 C 0.5342(2) 0.23321(9) 0.42031(19) 0.0253(6) Uani 1 1 d . . . H4 H 0.5269 0.2208 0.4763 0.030 Uiso 1 1 calc R . . C5 C 0.5135(2) 0.21020(9) 0.34402(19) 0.0242(5) Uani 1 1 d . . . C6 C 0.5258(2) 0.22923(9) 0.26322(19) 0.0232(5) Uani 1 1 d . . . H6 H 0.5128 0.2140 0.2102 0.028 Uiso 1 1 calc R . . O1 O 0.61128(14) 0.33274(6) 0.33195(14) 0.0229(4) Uani 1 1 d . . . C7 C 0.5455(2) 0.36536(9) 0.3317(2) 0.0288(6) Uani 1 1 d . . . H7A H 0.5053 0.3612 0.3806 0.035 Uiso 1 1 calc R . . H7B H 0.5079 0.3651 0.2753 0.035 Uiso 1 1 calc R . . C8 C 0.5940(2) 0.40630(9) 0.34283(19) 0.0249(6) Uani 1 1 d . . . C9 C 0.6877(2) 0.40930(9) 0.3526(2) 0.0274(6) Uani 1 1 d . . . H9 H 0.7246 0.3852 0.3514 0.033 Uiso 1 1 calc R . . C10 C 0.7258(2) 0.44839(9) 0.3643(2) 0.0291(6) Uani 1 1 d . . . H10 H 0.7899 0.4501 0.3714 0.035 Uiso 1 1 calc R . . N1 N 0.67921(19) 0.48372(8) 0.36627(17) 0.0288(5) Uani 1 1 d . . . C11 C 0.5896(3) 0.48047(10) 0.3550(3) 0.0366(7) Uani 1 1 d . . . H11 H 0.5547 0.5052 0.3548 0.044 Uiso 1 1 calc R . . C12 C 0.5445(2) 0.44292(10) 0.3435(3) 0.0362(7) Uani 1 1 d . . . H12 H 0.4803 0.4422 0.3361 0.043 Uiso 1 1 calc R . . C13 C 0.4766(2) 0.16581(10) 0.3511(2) 0.0335(7) Uani 1 1 d . . . C14 C 0.5324(4) 0.14148(13) 0.4242(3) 0.0596(7) Uani 1 1 d . . . H14A H 0.5088 0.1131 0.4278 0.089 Uiso 1 1 calc R . . H14B H 0.5277 0.1555 0.4812 0.089 Uiso 1 1 calc R . . H14C H 0.5959 0.1405 0.4100 0.089 Uiso 1 1 calc R . . C15 C 0.4858(4) 0.14144(13) 0.2672(3) 0.0596(7) Uani 1 1 d . . . H15A H 0.4497 0.1547 0.2186 0.089 Uiso 1 1 calc R . . H15B H 0.4641 0.1130 0.2752 0.089 Uiso 1 1 calc R . . H15C H 0.5494 0.1408 0.2533 0.089 Uiso 1 1 calc R . . C16 C 0.3810(4) 0.16867(13) 0.3830(3) 0.0596(7) Uani 1 1 d . . . H16A H 0.3394 0.1786 0.3346 0.089 Uiso 1 1 calc R . . H16B H 0.3806 0.1881 0.4327 0.089 Uiso 1 1 calc R . . H16C H 0.3617 0.1411 0.4021 0.089 Uiso 1 1 calc R . . S2 S 0.57384(6) 0.30050(3) 0.51895(5) 0.03164(18) Uani 1 1 d . . . C17 C 0.6724(2) 0.33146(9) 0.52666(18) 0.0226(5) Uani 1 1 d . . . C18 C 0.7572(2) 0.31778(8) 0.50357(16) 0.0202(5) Uani 1 1 d . . . C19 C 0.83249(19) 0.34248(8) 0.52477(17) 0.0206(5) Uani 1 1 d . . . C20 C 0.8229(2) 0.37997(8) 0.56976(18) 0.0222(5) Uani 1 1 d . . . H20 H 0.8751 0.3964 0.5842 0.027 Uiso 1 1 calc R . . C21 C 0.7389(2) 0.39399(8) 0.59407(17) 0.0219(5) Uani 1 1 d . . . C22 C 0.6641(2) 0.36931(9) 0.57075(18) 0.0247(6) Uani 1 1 d . . . H22 H 0.6059 0.3784 0.5851 0.030 Uiso 1 1 calc R . . O2 O 0.76504(14) 0.28072(6) 0.45878(12) 0.0220(4) Uani 1 1 d . . . C23 C 0.7843(3) 0.24589(9) 0.5155(2) 0.0324(7) Uani 1 1 d . . . H23A H 0.7373 0.2433 0.5587 0.039 Uiso 1 1 calc R . . H23B H 0.8435 0.2498 0.5486 0.039 Uiso 1 1 calc R . . C24 C 0.7863(2) 0.20730(9) 0.46019(19) 0.0261(6) Uani 1 1 d . . . C25 C 0.8121(3) 0.16975(11) 0.4995(2) 0.0400(8) Uani 1 1 d . . . H25 H 0.8290 0.1685 0.5610 0.048 Uiso 1 1 calc R . . C26 C 0.8130(3) 0.13422(10) 0.4483(2) 0.0412(8) Uani 1 1 d . . . H26 H 0.8305 0.1088 0.4764 0.049 Uiso 1 1 calc R . . N2 N 0.7906(2) 0.13360(8) 0.3616(2) 0.0348(6) Uani 1 1 d . . . C27 C 0.7656(2) 0.16997(10) 0.3250(2) 0.0319(7) Uani 1 1 d . . . H27 H 0.7486 0.1702 0.2635 0.038 Uiso 1 1 calc R . . C28 C 0.7628(2) 0.20718(9) 0.3702(2) 0.0279(6) Uani 1 1 d . . . H28 H 0.7452 0.2321 0.3403 0.033 Uiso 1 1 calc R . . C29 C 0.7289(2) 0.43437(9) 0.64688(19) 0.0270(6) Uani 1 1 d . . . C30 C 0.6545(5) 0.46129(16) 0.6044(4) 0.083(2) Uani 1 1 d . . . H30A H 0.5961 0.4474 0.6086 0.125 Uiso 1 1 calc R . . H30B H 0.6655 0.4658 0.5421 0.125 Uiso 1 1 calc R . . H30C H 0.6537 0.4881 0.6350 0.125 Uiso 1 1 calc R . . C31 C 0.8157(4) 0.45990(14) 0.6515(4) 0.0754(19) Uani 1 1 d . . . H31A H 0.8072 0.4850 0.6866 0.113 Uiso 1 1 calc R . . H31B H 0.8304 0.4677 0.5917 0.113 Uiso 1 1 calc R . . H31C H 0.8652 0.4434 0.6794 0.113 Uiso 1 1 calc R . . C32 C 0.7093(4) 0.42316(12) 0.7402(3) 0.0648(16) Uani 1 1 d . . . H32A H 0.6999 0.4486 0.7740 0.097 Uiso 1 1 calc R . . H32B H 0.7605 0.4076 0.7679 0.097 Uiso 1 1 calc R . . H32C H 0.6547 0.4060 0.7394 0.097 Uiso 1 1 calc R . . S3 S 0.94574(5) 0.32655(2) 0.51245(5) 0.02415(14) Uani 1 1 d . . . C33 C 0.95105(19) 0.30186(9) 0.40833(17) 0.0208(5) Uani 1 1 d . . . C34 C 0.92916(18) 0.32240(8) 0.32857(18) 0.0193(5) Uani 1 1 d . . . C35 C 0.94034(19) 0.30065(9) 0.24956(17) 0.0206(5) Uani 1 1 d . . . C36 C 0.9788(2) 0.26111(9) 0.25178(18) 0.0231(5) Uani 1 1 d . . . H36 H 0.9865 0.2471 0.1976 0.028 Uiso 1 1 calc R . . C37 C 1.0066(2) 0.24125(9) 0.33105(19) 0.0229(5) Uani 1 1 d . . . C38 C 0.9891(2) 0.26195(9) 0.40892(18) 0.0232(5) Uani 1 1 d . . . H38 H 1.0033 0.2486 0.4640 0.028 Uiso 1 1 calc R . . O3 O 0.89292(14) 0.36173(6) 0.33018(14) 0.0240(4) Uani 1 1 d . . . C39 C 0.9459(2) 0.39490(10) 0.2947(2) 0.0306(6) Uani 1 1 d . . . H39A H 0.9045 0.4166 0.2694 0.037 Uiso 1 1 calc R . . H39B H 0.9804 0.3837 0.2463 0.037 Uiso 1 1 calc R . . C40 C 1.0109(2) 0.41443(9) 0.3636(2) 0.0275(6) Uani 1 1 d . . . C41 C 0.9824(2) 0.43004(10) 0.4426(2) 0.0315(6) Uani 1 1 d . . . H41 H 0.9205 0.4285 0.4549 0.038 Uiso 1 1 calc R . . C42 C 1.0444(2) 0.44781(10) 0.5030(2) 0.0314(6) Uani 1 1 d . . . H42 H 1.0234 0.4584 0.5565 0.038 Uiso 1 1 calc R . . N3 N 1.1321(2) 0.45091(9) 0.4902(2) 0.0349(6) Uani 1 1 d . . . C43 C 1.1591(3) 0.43712(13) 0.4128(3) 0.0418(8) Uani 1 1 d . . . H43 H 1.2211 0.4399 0.4015 0.050 Uiso 1 1 calc R . . C44 C 1.1012(3) 0.41893(12) 0.3485(2) 0.0373(7) Uani 1 1 d . . . H44 H 1.1234 0.4096 0.2945 0.045 Uiso 1 1 calc R . . C45 C 1.0560(2) 0.19939(9) 0.3287(2) 0.0281(6) Uani 1 1 d . . . C46 C 1.0053(3) 0.16955(10) 0.2626(2) 0.0359(7) Uani 1 1 d . . . H46A H 1.0340 0.1421 0.2661 0.054 Uiso 1 1 calc R . . H46B H 1.0077 0.1805 0.2026 0.054 Uiso 1 1 calc R . . H46C H 0.9421 0.1671 0.2773 0.054 Uiso 1 1 calc R . . C47 C 1.0632(4) 0.17841(12) 0.4174(3) 0.0550(12) Uani 1 1 d . . . H47A H 1.0977 0.1961 0.4600 0.082 Uiso 1 1 calc R . . H47B H 1.0942 0.1517 0.4126 0.082 Uiso 1 1 calc R . . H47C H 1.0025 0.1738 0.4375 0.082 Uiso 1 1 calc R . . C48 C 1.1496(3) 0.20656(12) 0.2948(4) 0.0523(11) Uani 1 1 d . . . H48A H 1.1850 0.2246 0.3361 0.078 Uiso 1 1 calc R . . H48B H 1.1433 0.2199 0.2366 0.078 Uiso 1 1 calc R . . H48C H 1.1806 0.1798 0.2899 0.078 Uiso 1 1 calc R . . S4 S 0.91840(5) 0.32223(2) 0.14255(4) 0.02312(14) Uani 1 1 d . . . C49 C 0.80411(19) 0.33831(8) 0.13923(17) 0.0199(5) Uani 1 1 d . . . C50 C 0.7331(2) 0.31047(8) 0.14980(17) 0.0204(5) Uani 1 1 d . . . C51 C 0.6448(2) 0.32546(8) 0.14422(17) 0.0214(5) Uani 1 1 d . . . C52 C 0.6269(2) 0.36678(9) 0.12009(18) 0.0231(5) Uani 1 1 d . . . H52 H 0.5662 0.3764 0.1164 0.028 Uiso 1 1 calc R . . C53 C 0.6960(2) 0.39404(8) 0.10137(17) 0.0216(5) Uani 1 1 d . . . C54 C 0.7846(2) 0.37932(8) 0.11494(17) 0.0217(5) Uani 1 1 d . . . H54 H 0.8333 0.3979 0.1073 0.026 Uiso 1 1 calc R . . O4 O 0.74924(15) 0.26831(6) 0.16179(13) 0.0242(4) Uani 1 1 d . . . C55 C 0.7559(3) 0.24857(10) 0.0763(2) 0.0359(8) Uani 1 1 d . . . H55A H 0.8122 0.2576 0.0501 0.043 Uiso 1 1 calc R . . H55B H 0.7040 0.2569 0.0359 0.043 Uiso 1 1 calc R . . C56 C 0.7565(2) 0.20217(9) 0.0879(2) 0.0286(6) Uani 1 1 d . . . C57 C 0.8354(2) 0.17949(11) 0.0898(3) 0.0364(7) Uani 1 1 d . . . H57 H 0.8917 0.1931 0.0847 0.044 Uiso 1 1 calc R . . C58 C 0.8323(2) 0.13671(11) 0.0991(3) 0.0380(8) Uani 1 1 d . . . H58 H 0.8876 0.1217 0.1014 0.046 Uiso 1 1 calc R . . N4 N 0.75525(19) 0.11539(8) 0.10504(18) 0.0304(6) Uani 1 1 d . . . C59 C 0.6783(2) 0.13755(9) 0.1013(2) 0.0300(6) Uani 1 1 d . . . H59 H 0.6226 0.1232 0.1039 0.036 Uiso 1 1 calc R . . C60 C 0.6766(2) 0.18058(9) 0.0937(2) 0.0293(6) Uani 1 1 d . . . H60 H 0.6207 0.1951 0.0925 0.035 Uiso 1 1 calc R . . C61 C 0.6788(2) 0.43772(8) 0.06449(19) 0.0259(6) Uani 1 1 d . . . C62 C 0.7184(4) 0.43975(11) -0.0264(2) 0.0523(12) Uani 1 1 d . . . H62A H 0.7028 0.4665 -0.0544 0.078 Uiso 1 1 calc R . . H62B H 0.6935 0.4171 -0.0636 0.078 Uiso 1 1 calc R . . H62C H 0.7844 0.4370 -0.0192 0.078 Uiso 1 1 calc R . . C63 C 0.5775(3) 0.44773(11) 0.0533(3) 0.0489(10) Uani 1 1 d . . . H63A H 0.5510 0.4457 0.1108 0.073 Uiso 1 1 calc R . . H63B H 0.5475 0.4279 0.0121 0.073 Uiso 1 1 calc R . . H63C H 0.5692 0.4760 0.0301 0.073 Uiso 1 1 calc R . . C64 C 0.7234(3) 0.47010(10) 0.1258(2) 0.0360(7) Uani 1 1 d . . . H64A H 0.6961 0.4692 0.1829 0.054 Uiso 1 1 calc R . . H64B H 0.7148 0.4978 0.0996 0.054 Uiso 1 1 calc R . . H64C H 0.7883 0.4642 0.1345 0.054 Uiso 1 1 calc R . . O5 O 0.6159(2) 0.03893(13) 0.2135(2) 0.0653(10) Uani 1 1 d . . . C65 C 0.6294(3) 0.04504(14) 0.2924(3) 0.0496(10) Uani 1 1 d . . . H65 H 0.6798 0.0618 0.3114 0.060 Uiso 1 1 calc R . . N5 N 0.5781(3) 0.02979(12) 0.3541(2) 0.0490(8) Uani 1 1 d . . . C66 C 0.5010(4) 0.0030(2) 0.3292(4) 0.0781(17) Uani 1 1 d . . . H66A H 0.4954 -0.0001 0.2648 0.117 Uiso 1 1 calc R . . H66B H 0.4457 0.0156 0.3493 0.117 Uiso 1 1 calc R . . H66C H 0.5103 -0.0243 0.3568 0.117 Uiso 1 1 calc R . . C67 C 0.6025(4) 0.03590(17) 0.4476(3) 0.0664(15) Uani 1 1 d . . . H67A H 0.6524 0.0559 0.4547 0.100 Uiso 1 1 calc R . . H67B H 0.6213 0.0093 0.4744 0.100 Uiso 1 1 calc R . . H67C H 0.5501 0.0466 0.4767 0.100 Uiso 1 1 calc R . . P1 P 0.81236(7) 0.05946(3) 0.66595(6) 0.0352(2) Uani 1 1 d . . . F1 F 0.7383(2) 0.09391(8) 0.6394(2) 0.0628(7) Uani 1 1 d . . . F2 F 0.8890(2) 0.09358(8) 0.65683(19) 0.0587(7) Uani 1 1 d . . . F3 F 0.8078(2) 0.07237(9) 0.76806(16) 0.0646(8) Uani 1 1 d . . . F4 F 0.88600(19) 0.02539(8) 0.69345(18) 0.0573(7) Uani 1 1 d . . . F5 F 0.7344(2) 0.02574(9) 0.6751(2) 0.0668(8) Uani 1 1 d . . . F6 F 0.8179(2) 0.04710(7) 0.56472(16) 0.0566(7) Uani 1 1 d . . . C68 C 0.7489(4) 0.17392(13) 0.7663(3) 0.0520(10) Uani 1 1 d . . . H68 H 0.7730 0.1452 0.7587 0.062 Uiso 1 1 calc R . . Cl1 Cl 0.66096(8) 0.18354(4) 0.68464(10) 0.0656(3) Uani 1 1 d . . . Cl2 Cl 0.83579(8) 0.20998(5) 0.75687(10) 0.0723(4) Uani 1 1 d . . . Cl3 Cl 0.70045(16) 0.17772(5) 0.87022(10) 0.0943(6) Uani 1 1 d . . . C69 C 0.9446(3) 0.05586(14) 0.3264(3) 0.0545(11) Uani 1 1 d . . . H69A H 0.9939 0.0762 0.3306 0.082 Uiso 1 1 calc R . . H69B H 0.9681 0.0289 0.3083 0.082 Uiso 1 1 calc R . . H69C H 0.9190 0.0530 0.3840 0.082 Uiso 1 1 calc R . . O6 O 0.8775(3) 0.06925(10) 0.2639(2) 0.0656(10) Uani 1 1 d . . . H6A H 0.8385 0.0830 0.2892 0.098 Uiso 1 1 calc R . . _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 0.04995(18) 0.02026(11) 0.04288(15) 0.00564(9) 0.00521(12) 0.01026(10) S1 0.0288(4) 0.0273(3) 0.0228(3) 0.0043(3) -0.0049(3) -0.0097(3) C1 0.0228(13) 0.0193(12) 0.0218(12) 0.0008(9) 0.0016(10) -0.0023(10) C2 0.0215(13) 0.0162(11) 0.0240(12) -0.0016(9) 0.0034(10) -0.0029(9) C3 0.0236(14) 0.0224(12) 0.0232(12) -0.0033(10) 0.0035(10) -0.0040(10) C4 0.0288(15) 0.0244(13) 0.0232(12) 0.0009(10) 0.0062(11) -0.0044(11) C5 0.0259(14) 0.0187(12) 0.0285(13) -0.0023(10) 0.0056(11) -0.0050(10) C6 0.0252(14) 0.0188(12) 0.0258(13) -0.0035(10) 0.0030(11) -0.0054(10) O1 0.0225(10) 0.0151(8) 0.0311(10) -0.0016(7) 0.0025(8) -0.0031(7) C7 0.0252(15) 0.0198(13) 0.0411(16) -0.0043(12) -0.0014(12) -0.0005(11) C8 0.0292(15) 0.0180(12) 0.0269(13) -0.0017(10) -0.0022(11) -0.0006(10) C9 0.0309(16) 0.0172(12) 0.0340(15) 0.0008(11) 0.0001(12) 0.0003(11) C10 0.0292(16) 0.0218(13) 0.0357(15) 0.0000(11) -0.0020(12) -0.0036(11) N1 0.0374(15) 0.0190(11) 0.0291(12) -0.0006(9) -0.0049(11) -0.0010(10) C11 0.0413(19) 0.0184(13) 0.0488(19) -0.0050(13) -0.0073(15) 0.0034(12) C12 0.0300(17) 0.0234(14) 0.054(2) -0.0049(14) -0.0091(15) 0.0025(12) C13 0.0405(19) 0.0208(13) 0.0405(17) -0.0016(12) 0.0116(14) -0.0107(12) C14 0.086(2) 0.0331(11) 0.0598(15) 0.0007(10) 0.0070(14) -0.0184(12) C15 0.086(2) 0.0331(11) 0.0598(15) 0.0007(10) 0.0070(14) -0.0184(12) C16 0.086(2) 0.0331(11) 0.0598(15) 0.0007(10) 0.0070(14) -0.0184(12) S2 0.0320(4) 0.0387(4) 0.0254(3) -0.0115(3) 0.0116(3) -0.0138(3) C17 0.0262(14) 0.0231(12) 0.0187(11) -0.0027(10) 0.0035(10) -0.0034(10) C18 0.0281(14) 0.0174(11) 0.0151(10) -0.0032(9) 0.0012(10) 0.0007(10) C19 0.0243(13) 0.0200(12) 0.0173(11) -0.0026(9) 0.0003(10) 0.0042(10) C20 0.0266(14) 0.0204(12) 0.0197(11) -0.0035(9) 0.0007(10) -0.0009(10) C21 0.0323(15) 0.0156(11) 0.0179(11) -0.0025(9) 0.0036(10) 0.0030(10) C22 0.0278(15) 0.0250(13) 0.0221(12) -0.0036(10) 0.0073(11) 0.0013(11) O2 0.0320(11) 0.0152(8) 0.0189(8) -0.0036(7) 0.0019(8) 0.0001(7) C23 0.057(2) 0.0180(12) 0.0223(13) -0.0009(10) 0.0036(13) 0.0015(13) C24 0.0343(16) 0.0194(12) 0.0251(13) -0.0013(10) 0.0051(12) -0.0014(11) C25 0.068(3) 0.0259(15) 0.0268(15) 0.0026(12) 0.0074(16) 0.0048(16) C26 0.065(3) 0.0185(13) 0.0408(18) 0.0026(13) 0.0096(17) 0.0032(15) N2 0.0461(17) 0.0227(12) 0.0364(14) -0.0064(11) 0.0081(12) -0.0014(11) C27 0.0374(18) 0.0277(15) 0.0305(15) -0.0078(12) 0.0009(13) -0.0001(13) C28 0.0328(16) 0.0235(13) 0.0274(14) -0.0015(11) 0.0020(12) 0.0021(11) C29 0.0392(17) 0.0195(12) 0.0227(12) -0.0058(10) 0.0051(12) 0.0022(11) C30 0.112(5) 0.056(3) 0.075(3) -0.038(3) -0.044(3) 0.057(3) C31 0.075(3) 0.035(2) 0.121(5) -0.045(3) 0.050(3) -0.023(2) C32 0.142(5) 0.0288(18) 0.0269(17) -0.0102(14) 0.027(2) -0.008(2) S3 0.0240(3) 0.0268(3) 0.0209(3) -0.0063(2) -0.0035(3) 0.0051(3) C33 0.0197(13) 0.0220(12) 0.0206(12) -0.0037(9) -0.0006(10) 0.0046(10) C34 0.0181(12) 0.0173(11) 0.0225(12) -0.0010(9) 0.0007(10) 0.0023(9) C35 0.0201(13) 0.0219(12) 0.0200(11) 0.0005(9) 0.0017(10) 0.0022(10) C36 0.0265(14) 0.0217(12) 0.0210(12) -0.0024(10) 0.0022(10) 0.0046(10) C37 0.0232(14) 0.0202(12) 0.0252(13) 0.0009(10) 0.0011(10) 0.0056(10) C38 0.0247(14) 0.0233(13) 0.0211(12) 0.0003(10) -0.0010(10) 0.0053(10) O3 0.0265(10) 0.0179(9) 0.0275(10) -0.0015(7) 0.0015(8) 0.0050(8) C39 0.0425(18) 0.0222(13) 0.0263(14) 0.0017(11) -0.0028(13) -0.0018(12) C40 0.0355(17) 0.0173(12) 0.0296(14) 0.0007(10) 0.0018(12) 0.0009(11) C41 0.0330(17) 0.0291(15) 0.0324(15) -0.0031(12) 0.0032(13) -0.0008(12) C42 0.0350(17) 0.0277(14) 0.0314(15) -0.0022(12) 0.0018(13) -0.0002(12) N3 0.0381(16) 0.0309(14) 0.0352(14) 0.0009(11) -0.0013(12) -0.0048(12) C43 0.0333(19) 0.050(2) 0.0422(19) -0.0012(16) 0.0059(15) -0.0035(16) C44 0.0373(19) 0.0404(18) 0.0349(16) -0.0045(14) 0.0076(14) 0.0018(15) C45 0.0319(16) 0.0212(13) 0.0311(14) -0.0005(11) 0.0008(12) 0.0096(11) C46 0.0418(19) 0.0272(15) 0.0384(17) -0.0040(13) -0.0006(15) 0.0046(13) C47 0.099(4) 0.0326(18) 0.0324(18) 0.0024(14) -0.003(2) 0.030(2) C48 0.0310(19) 0.0321(18) 0.094(3) -0.002(2) 0.007(2) 0.0097(15) S4 0.0259(3) 0.0242(3) 0.0196(3) 0.0030(2) 0.0043(2) 0.0037(3) C49 0.0253(14) 0.0186(11) 0.0156(10) 0.0004(9) 0.0009(9) 0.0008(10) C50 0.0302(14) 0.0140(11) 0.0165(11) 0.0037(9) -0.0017(10) -0.0008(10) C51 0.0280(14) 0.0179(11) 0.0180(11) 0.0009(9) -0.0004(10) -0.0034(10) C52 0.0264(14) 0.0210(12) 0.0214(12) 0.0020(10) -0.0020(10) 0.0011(10) C53 0.0301(15) 0.0170(11) 0.0171(11) 0.0020(9) -0.0024(10) 0.0001(10) C54 0.0289(14) 0.0161(11) 0.0199(11) 0.0025(9) 0.0006(10) -0.0025(10) O4 0.0359(12) 0.0131(8) 0.0233(9) 0.0025(7) 0.0000(8) 0.0007(8) C55 0.062(2) 0.0196(13) 0.0261(14) -0.0013(11) 0.0023(14) -0.0015(14) C56 0.0426(18) 0.0191(12) 0.0242(13) -0.0022(10) 0.0022(12) -0.0007(12) C57 0.0295(17) 0.0312(16) 0.048(2) -0.0047(14) 0.0026(14) -0.0045(13) C58 0.0314(17) 0.0259(15) 0.056(2) -0.0027(14) -0.0021(15) 0.0077(13) N4 0.0344(15) 0.0189(11) 0.0373(14) -0.0016(10) -0.0025(11) 0.0025(10) C59 0.0303(16) 0.0221(13) 0.0375(16) -0.0038(12) 0.0020(13) -0.0006(11) C60 0.0302(16) 0.0220(13) 0.0352(15) -0.0026(11) -0.0019(12) 0.0052(11) C61 0.0393(17) 0.0152(11) 0.0227(12) 0.0027(10) -0.0026(11) 0.0019(11) C62 0.104(4) 0.0257(16) 0.0286(16) 0.0111(13) 0.0153(19) 0.0151(19) C63 0.046(2) 0.0265(16) 0.072(3) 0.0135(17) -0.018(2) 0.0057(15) C64 0.049(2) 0.0180(13) 0.0395(17) -0.0019(12) -0.0063(15) -0.0004(13) O5 0.0510(19) 0.108(3) 0.0379(15) 0.0110(17) 0.0066(13) -0.0002(19) C65 0.042(2) 0.058(3) 0.049(2) 0.0114(19) 0.0077(18) 0.0087(18) N5 0.053(2) 0.052(2) 0.0428(17) 0.0121(15) 0.0108(15) 0.0138(16) C66 0.070(4) 0.095(5) 0.070(3) 0.020(3) 0.011(3) -0.018(3) C67 0.092(4) 0.067(3) 0.041(2) 0.008(2) 0.014(2) 0.034(3) P1 0.0474(5) 0.0242(4) 0.0346(4) 0.0042(3) 0.0080(4) 0.0023(3) F1 0.0702(18) 0.0422(13) 0.0750(18) 0.0071(13) -0.0020(14) 0.0208(12) F2 0.0687(17) 0.0409(13) 0.0674(16) -0.0036(12) 0.0105(13) -0.0198(12) F3 0.091(2) 0.0678(18) 0.0371(12) -0.0009(12) 0.0167(13) 0.0160(15) F4 0.0634(16) 0.0440(13) 0.0644(16) 0.0079(12) 0.0032(13) 0.0178(12) F5 0.0611(17) 0.0503(15) 0.090(2) 0.0197(15) 0.0138(15) -0.0127(13) F6 0.098(2) 0.0360(12) 0.0361(11) -0.0020(9) 0.0073(12) -0.0021(12) C68 0.075(3) 0.037(2) 0.045(2) -0.0077(17) 0.013(2) 0.0011(19) Cl1 0.0430(6) 0.0660(7) 0.0879(9) -0.0106(7) 0.0045(6) 0.0069(5) Cl2 0.0407(6) 0.0953(10) 0.0811(9) -0.0113(8) 0.0046(6) -0.0112(6) Cl3 0.1641(18) 0.0650(8) 0.0576(7) -0.0030(6) 0.0368(9) -0.0220(10) C69 0.063(3) 0.036(2) 0.063(3) 0.0008(19) -0.001(2) 0.0057(19) O6 0.094(3) 0.0449(17) 0.0540(18) -0.0196(14) -0.0218(18) 0.0244(17) _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. ; _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 N1 2.234(3) 2_645 ? Ag1 N4 2.303(3) . ? Ag1 N3 2.457(3) 4_565 ? Ag1 O5 2.553(3) . ? S1 C51 1.774(3) . ? S1 C1 1.774(3) . ? C1 C2 1.393(4) . ? C1 C6 1.400(4) . ? C2 O1 1.376(3) . ? C2 C3 1.401(4) . ? C3 C4 1.395(4) . ? C3 S2 1.770(3) . ? C4 C5 1.391(4) . ? C4 H4 0.9500 . ? C5 C6 1.392(4) . ? C5 C13 1.535(4) . ? C6 H6 0.9500 . ? O1 C7 1.432(4) . ? C7 C8 1.505(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C12 1.388(4) . ? C8 C9 1.390(4) . ? C9 C10 1.386(4) . ? C9 H9 0.9500 . ? C10 N1 1.331(4) . ? C10 H10 0.9500 . ? N1 C11 1.332(5) . ? N1 Ag1 2.234(3) 2_655 ? C11 C12 1.387(5) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C15 1.509(6) . ? C13 C16 1.530(6) . ? C13 C14 1.551(6) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? S2 C17 1.766(3) . ? C17 C18 1.397(4) . ? C17 C22 1.398(4) . ? C18 O2 1.381(3) . ? C18 C19 1.390(4) . ? C19 C20 1.397(4) . ? C19 S3 1.776(3) . ? C20 C21 1.396(4) . ? C20 H20 0.9500 . ? C21 C22 1.391(4) . ? C21 C29 1.538(4) . ? C22 H22 0.9500 . ? O2 C23 1.431(3) . ? C23 C24 1.500(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C28 1.387(4) . ? C24 C25 1.390(4) . ? C25 C26 1.382(5) . ? C25 H25 0.9500 . ? C26 N2 1.336(5) . ? C26 H26 0.9500 . ? N2 C27 1.337(4) . ? C27 C28 1.381(4) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C32 1.507(5) . ? C29 C30 1.513(5) . ? C29 C31 1.523(6) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? S3 C33 1.774(3) . ? C33 C34 1.398(4) . ? C33 C38 1.402(4) . ? C34 O3 1.375(3) . ? C34 C35 1.407(4) . ? C35 C36 1.394(4) . ? C35 S4 1.776(3) . ? C36 C37 1.399(4) . ? C36 H36 0.9500 . ? C37 C38 1.395(4) . ? C37 C45 1.535(4) . ? C38 H38 0.9500 . ? O3 C39 1.448(4) . ? C39 C40 1.511(4) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C44 1.379(5) . ? C40 C41 1.390(4) . ? C41 C42 1.379(5) . ? C41 H41 0.9500 . ? C42 N3 1.330(5) . ? C42 H42 0.9500 . ? N3 C43 1.340(5) . ? N3 Ag1 2.457(3) 4_666 ? C43 C44 1.388(5) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C47 1.503(5) . ? C45 C48 1.528(5) . ? C45 C46 1.547(5) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? S4 C49 1.768(3) . ? C49 C54 1.395(4) . ? C49 C50 1.399(4) . ? C50 O4 1.387(3) . ? C50 C51 1.391(4) . ? C51 C52 1.400(4) . ? C52 C53 1.391(4) . ? C52 H52 0.9500 . ? C53 C54 1.399(4) . ? C53 C61 1.528(4) . ? C54 H54 0.9500 . ? O4 C55 1.453(4) . ? C55 C56 1.503(4) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.378(5) . ? C56 C60 1.380(5) . ? C57 C58 1.385(5) . ? C57 H57 0.9500 . ? C58 N4 1.340(5) . ? C58 H58 0.9500 . ? N4 C59 1.343(4) . ? C59 C60 1.389(4) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 C64 1.519(4) . ? C61 C62 1.534(5) . ? C61 C63 1.534(5) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? O5 C65 1.216(5) . ? C65 N5 1.337(5) . ? C65 H65 0.9500 . ? N5 C67 1.454(6) . ? N5 C66 1.460(7) . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? P1 F4 1.584(3) . ? P1 F2 1.592(3) . ? P1 F1 1.593(3) . ? P1 F6 1.593(3) . ? P1 F5 1.597(3) . ? P1 F3 1.609(3) . ? C68 Cl2 1.746(5) . ? C68 Cl1 1.766(5) . ? C68 Cl3 1.777(4) . ? C68 H68 1.0000 . ? C69 O6 1.396(6) . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? O6 H6A 0.8400 . ? _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 N1 Ag1 N4 148.01(10) 2_645 . ? N1 Ag1 N3 118.06(9) 2_645 4_565 ? N4 Ag1 N3 85.75(10) . 4_565 ? N1 Ag1 O5 104.22(12) 2_645 . ? N4 Ag1 O5 98.01(12) . . ? N3 Ag1 O5 86.26(10) 4_565 . ? C51 S1 C1 107.07(13) . . ? C2 C1 C6 120.3(2) . . ? C2 C1 S1 123.7(2) . . ? C6 C1 S1 115.2(2) . . ? O1 C2 C1 121.5(2) . . ? O1 C2 C3 120.0(2) . . ? C1 C2 C3 118.4(2) . . ? C4 C3 C2 120.5(3) . . ? C4 C3 S2 114.9(2) . . ? C2 C3 S2 124.0(2) . . ? C5 C4 C3 121.5(3) . . ? C5 C4 H4 119.3 . . ? C3 C4 H4 119.3 . . ? C4 C5 C6 117.6(3) . . ? C4 C5 C13 119.8(3) . . ? C6 C5 C13 122.6(3) . . ? C5 C6 C1 121.7(3) . . ? C5 C6 H6 119.2 . . ? C1 C6 H6 119.2 . . ? C2 O1 C7 115.1(2) . . ? O1 C7 C8 108.7(2) . . ? O1 C7 H7A 109.9 . . ? C8 C7 H7A 109.9 . . ? O1 C7 H7B 109.9 . . ? C8 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? C12 C8 C9 117.7(3) . . ? C12 C8 C7 119.7(3) . . ? C9 C8 C7 122.6(3) . . ? C10 C9 C8 118.2(3) . . ? C10 C9 H9 120.9 . . ? C8 C9 H9 120.9 . . ? N1 C10 C9 124.7(3) . . ? N1 C10 H10 117.6 . . ? C9 C10 H10 117.6 . . ? C10 N1 C11 116.4(3) . . ? C10 N1 Ag1 119.8(2) . 2_655 ? C11 N1 Ag1 123.8(2) . 2_655 ? N1 C11 C12 123.6(3) . . ? N1 C11 H11 118.2 . . ? C12 C11 H11 118.2 . . ? C11 C12 C8 119.3(3) . . ? C11 C12 H12 120.3 . . ? C8 C12 H12 120.3 . . ? C15 C13 C16 115.7(4) . . ? C15 C13 C5 111.8(3) . . ? C16 C13 C5 107.9(3) . . ? C15 C13 C14 105.6(3) . . ? C16 C13 C14 105.4(3) . . ? C5 C13 C14 110.1(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C17 S2 C3 109.91(13) . . ? C18 C17 C22 120.2(3) . . ? C18 C17 S2 124.0(2) . . ? C22 C17 S2 115.1(2) . . ? O2 C18 C19 121.1(2) . . ? O2 C18 C17 120.1(2) . . ? C19 C18 C17 118.9(2) . . ? C18 C19 C20 120.1(3) . . ? C18 C19 S3 124.1(2) . . ? C20 C19 S3 115.3(2) . . ? C21 C20 C19 121.9(3) . . ? C21 C20 H20 119.1 . . ? C19 C20 H20 119.1 . . ? C22 C21 C20 117.3(2) . . ? C22 C21 C29 120.8(3) . . ? C20 C21 C29 121.9(3) . . ? C21 C22 C17 121.7(3) . . ? C21 C22 H22 119.2 . . ? C17 C22 H22 119.2 . . ? C18 O2 C23 113.6(2) . . ? O2 C23 C24 108.8(2) . . ? O2 C23 H23A 109.9 . . ? C24 C23 H23A 109.9 . . ? O2 C23 H23B 109.9 . . ? C24 C23 H23B 109.9 . . ? H23A C23 H23B 108.3 . . ? C28 C24 C25 117.7(3) . . ? C28 C24 C23 122.7(3) . . ? C25 C24 C23 119.6(3) . . ? C26 C25 C24 119.3(3) . . ? C26 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? N2 C26 C25 123.7(3) . . ? N2 C26 H26 118.2 . . ? C25 C26 H26 118.2 . . ? C26 N2 C27 116.1(3) . . ? N2 C27 C28 124.6(3) . . ? N2 C27 H27 117.7 . . ? C28 C27 H27 117.7 . . ? C27 C28 C24 118.5(3) . . ? C27 C28 H28 120.7 . . ? C24 C28 H28 120.7 . . ? C32 C29 C30 110.9(4) . . ? C32 C29 C31 107.4(4) . . ? C30 C29 C31 107.5(4) . . ? C32 C29 C21 108.5(3) . . ? C30 C29 C21 110.7(3) . . ? C31 C29 C21 111.7(3) . . ? 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 . . ? C33 S3 C19 108.63(13) . . ? C34 C33 C38 120.6(2) . . ? C34 C33 S3 122.5(2) . . ? C38 C33 S3 116.4(2) . . ? O3 C34 C33 119.2(2) . . ? O3 C34 C35 122.7(2) . . ? C33 C34 C35 117.9(2) . . ? C36 C35 C34 120.3(2) . . ? C36 C35 S4 115.4(2) . . ? C34 C35 S4 124.0(2) . . ? C35 C36 C37 122.3(2) . . ? C35 C36 H36 118.9 . . ? C37 C36 H36 118.9 . . ? C38 C37 C36 116.7(2) . . ? C38 C37 C45 123.6(3) . . ? C36 C37 C45 119.7(2) . . ? C37 C38 C33 121.9(3) . . ? C37 C38 H38 119.1 . . ? C33 C38 H38 119.1 . . ? C34 O3 C39 116.7(2) . . ? O3 C39 C40 112.7(2) . . ? O3 C39 H39A 109.0 . . ? C40 C39 H39A 109.0 . . ? O3 C39 H39B 109.0 . . ? C40 C39 H39B 109.0 . . ? H39A C39 H39B 107.8 . . ? C44 C40 C41 117.2(3) . . ? C44 C40 C39 120.7(3) . . ? C41 C40 C39 122.1(3) . . ? C42 C41 C40 119.8(3) . . ? C42 C41 H41 120.1 . . ? C40 C41 H41 120.1 . . ? N3 C42 C41 123.3(3) . . ? N3 C42 H42 118.3 . . ? C41 C42 H42 118.3 . . ? C42 N3 C43 116.9(3) . . ? C42 N3 Ag1 122.2(2) . 4_666 ? C43 N3 Ag1 117.1(3) . 4_666 ? N3 C43 C44 123.3(4) . . ? N3 C43 H43 118.3 . . ? C44 C43 H43 118.3 . . ? C40 C44 C43 119.4(3) . . ? C40 C44 H44 120.3 . . ? C43 C44 H44 120.3 . . ? C47 C45 C48 110.9(4) . . ? C47 C45 C37 112.3(3) . . ? C48 C45 C37 108.7(3) . . ? C47 C45 C46 107.8(3) . . ? C48 C45 C46 106.8(3) . . ? C37 C45 C46 110.3(3) . . ? 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 . . ? C49 S4 C35 104.99(12) . . ? C54 C49 C50 119.4(3) . . ? C54 C49 S4 117.7(2) . . ? C50 C49 S4 122.4(2) . . ? O4 C50 C51 120.0(2) . . ? O4 C50 C49 121.1(3) . . ? C51 C50 C49 118.8(2) . . ? C50 C51 C52 120.5(3) . . ? C50 C51 S1 122.0(2) . . ? C52 C51 S1 116.8(2) . . ? C53 C52 C51 121.5(3) . . ? C53 C52 H52 119.3 . . ? C51 C52 H52 119.3 . . ? C52 C53 C54 116.9(2) . . ? C52 C53 C61 123.2(3) . . ? C54 C53 C61 119.8(3) . . ? C49 C54 C53 122.4(3) . . ? C49 C54 H54 118.8 . . ? C53 C54 H54 118.8 . . ? C50 O4 C55 109.4(2) . . ? O4 C55 C56 109.3(2) . . ? O4 C55 H55A 109.8 . . ? C56 C55 H55A 109.8 . . ? O4 C55 H55B 109.8 . . ? C56 C55 H55B 109.8 . . ? H55A C55 H55B 108.3 . . ? C57 C56 C60 117.6(3) . . ? C57 C56 C55 121.7(3) . . ? C60 C56 C55 120.6(3) . . ? C56 C57 C58 119.6(3) . . ? C56 C57 H57 120.2 . . ? C58 C57 H57 120.2 . . ? N4 C58 C57 123.4(3) . . ? N4 C58 H58 118.3 . . ? C57 C58 H58 118.3 . . ? C58 N4 C59 116.7(3) . . ? C58 N4 Ag1 124.0(2) . . ? C59 N4 Ag1 119.1(2) . . ? N4 C59 C60 122.9(3) . . ? N4 C59 H59 118.5 . . ? C60 C59 H59 118.5 . . ? C56 C60 C59 119.7(3) . . ? C56 C60 H60 120.1 . . ? C59 C60 H60 120.1 . . ? C64 C61 C53 110.5(2) . . ? C64 C61 C62 110.1(3) . . ? C53 C61 C62 107.7(2) . . ? C64 C61 C63 107.9(3) . . ? C53 C61 C63 111.8(3) . . ? C62 C61 C63 108.7(3) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C65 O5 Ag1 119.4(3) . . ? O5 C65 N5 124.4(5) . . ? O5 C65 H65 117.8 . . ? N5 C65 H65 117.8 . . ? C65 N5 C67 121.1(5) . . ? C65 N5 C66 120.4(4) . . ? C67 N5 C66 118.2(4) . . ? N5 C66 H66A 109.5 . . ? N5 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? N5 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? N5 C67 H67A 109.5 . . ? N5 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? N5 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? F4 P1 F2 90.95(16) . . ? F4 P1 F1 179.37(17) . . ? F2 P1 F1 88.99(16) . . ? F4 P1 F6 90.18(15) . . ? F2 P1 F6 90.37(15) . . ? F1 P1 F6 90.44(16) . . ? F4 P1 F5 89.81(16) . . ? F2 P1 F5 179.21(17) . . ? F1 P1 F5 90.25(17) . . ? F6 P1 F5 89.82(17) . . ? F4 P1 F3 89.79(15) . . ? F2 P1 F3 88.88(16) . . ? F1 P1 F3 89.59(16) . . ? F6 P1 F3 179.25(19) . . ? F5 P1 F3 90.93(18) . . ? Cl2 C68 Cl1 109.9(2) . . ? Cl2 C68 Cl3 111.7(2) . . ? Cl1 C68 Cl3 106.7(3) . . ? Cl2 C68 H68 109.5 . . ? Cl1 C68 H68 109.5 . . ? Cl3 C68 H68 109.5 . . ? O6 C69 H69A 109.5 . . ? O6 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? O6 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C69 O6 H6A 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 2.512 _refine_diff_density_min -1.939 _refine_diff_density_rms 0.111