# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Wais Hosseini' _publ_contact_author_email HOSSEINI@CHIMIE.U-STRASBG.FR _publ_section_title ; Direct synthesis and structural characterisation of tri- and tetra-nuclear silver metallaknotanes by selfassembly approach ; loop_ _publ_author_name 'Mir Wais Hosseini' 'Lionel Allouche' 'Julien Bourlier' 'Abdelaziz Jouaiti' ; N.Kyritsakas-Gruber ; 'Jean-Marc Planeix' # Attachment 'New_Cif_5-Ag.cif' data_5-Ag _database_code_depnum_ccdc_archive 'CCDC 701605' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C104 H112 Ag4 N8 O20, 4(F6 Sb)' _chemical_formula_sum 'C104 H112 Ag4 F24 N8 O20 Sb4' _chemical_formula_weight 3168.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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' Sb Sb -0.5866 1.5461 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 27.703(2) _cell_length_b 14.8580(11) _cell_length_c 28.187(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.174(4) _cell_angle_gamma 90.00 _cell_volume 11593.4(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7735 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 27.68 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.815 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6240 _exptl_absorpt_coefficient_mu 1.685 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6147 _exptl_absorpt_correction_T_max 0.8234 _exptl_absorpt_process_details sadabs _exptl_special_details ; The large Ueq(max)/Ue(min) in the non solvent part is due to the inherent floppiness of the chain and the pyridine. The crystal has a low diffracting powder so the wR and R values are large and there is a Low Bond Precision on C-C Bonds ; _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 292876 _diffrn_reflns_av_R_equivalents 0.0963 _diffrn_reflns_av_sigmaI/netI 0.0921 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 0.74 _diffrn_reflns_theta_max 27.68 _reflns_number_total 26844 _reflns_number_gt 14895 _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^)+(0.1377P)^2^+714.5133P] 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 SHELXL _refine_ls_extinction_coef 0.00075(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 26844 _refine_ls_number_parameters 1478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1924 _refine_ls_R_factor_gt 0.1262 _refine_ls_wR_factor_ref 0.3836 _refine_ls_wR_factor_gt 0.3660 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.37124(6) 0.74007(10) -0.09042(6) 0.0363(4) Uani 1 1 d . . . Ag2 Ag 0.14583(6) 1.03537(12) -0.12135(6) 0.0484(5) Uani 1 1 d . . . Ag3 Ag 0.36146(6) 1.03869(10) 0.13970(6) 0.0365(4) Uani 1 1 d . . . Ag4 Ag 0.11836(6) 0.70850(11) 0.11726(6) 0.0427(4) Uani 1 1 d . . . N1 N 0.3917(5) 0.8840(11) -0.0869(5) 0.027(3) Uani 1 1 d . . . C1 C 0.3939(9) 0.9353(17) -0.1217(8) 0.049(6) Uani 1 1 d . . . H1 H 0.3836 0.9115 -0.1517 0.059 Uiso 1 1 calc R . . C2 C 0.4098(8) 1.0230(14) -0.1211(8) 0.041(5) Uani 1 1 d . . . H2 H 0.4093 1.0576 -0.1495 0.049 Uiso 1 1 calc R . . C3 C 0.4259(8) 1.0589(14) -0.0800(7) 0.039(5) Uani 1 1 d . . . H3 H 0.4381 1.1186 -0.0787 0.047 Uiso 1 1 calc R . . C4 C 0.4241(6) 1.0063(12) -0.0391(7) 0.029(4) Uani 1 1 d . . . C5 C 0.4417(7) 1.0374(12) 0.0088(7) 0.034(4) Uani 1 1 d . . . H5 H 0.4551 1.0959 0.0127 0.041 Uiso 1 1 calc R . . C6 C 0.4386(7) 0.9852(12) 0.0447(6) 0.027(4) Uani 1 1 d . . . C7 C 0.4199(8) 0.8935(12) 0.0418(8) 0.040(5) Uani 1 1 d . . . H7 H 0.4189 0.8558 0.0690 0.049 Uiso 1 1 calc R . . C8 C 0.4041(7) 0.8650(13) -0.0018(7) 0.036(4) Uani 1 1 d . . . H8 H 0.3897 0.8071 -0.0046 0.043 Uiso 1 1 calc R . . C9 C 0.4079(7) 0.9169(11) -0.0425(7) 0.033(4) Uani 1 1 d . . . O1 O 0.4536(5) 1.0048(9) 0.0915(5) 0.038(3) Uani 1 1 d . . . C10 C 0.4746(7) 1.0915(13) 0.0993(7) 0.034(4) Uani 1 1 d . . . H10A H 0.4515 1.1391 0.0888 0.041 Uiso 1 1 calc R . . H10B H 0.5042 1.0977 0.0810 0.041 Uiso 1 1 calc R . . C11 C 0.4867(7) 1.1006(14) 0.1520(7) 0.038(5) Uani 1 1 d . . . H11A H 0.5023 1.0452 0.1647 0.045 Uiso 1 1 calc R . . H11B H 0.5085 1.1523 0.1584 0.045 Uiso 1 1 calc R . . O2 O 0.4407(5) 1.1149(9) 0.1730(5) 0.033(3) Uani 1 1 d . . . C12 C 0.4465(8) 1.1229(15) 0.2239(8) 0.047(5) Uani 1 1 d . . . H12A H 0.4577 1.0653 0.2380 0.056 Uiso 1 1 calc R . . H12B H 0.4703 1.1705 0.2325 0.056 Uiso 1 1 calc R . . C13 C 0.3997(9) 1.1461(17) 0.2403(8) 0.052(6) Uani 1 1 d . . . H13A H 0.3870 1.1988 0.2224 0.062 Uiso 1 1 calc R . . H13B H 0.4025 1.1625 0.2743 0.062 Uiso 1 1 calc R . . O3 O 0.3665(5) 1.0705(9) 0.2339(5) 0.038(3) Uani 1 1 d . . . C14 C 0.3203(7) 1.0794(13) 0.2546(7) 0.036(4) Uani 1 1 d . . . H14A H 0.3252 1.0942 0.2887 0.044 Uiso 1 1 calc R . . H14B H 0.3034 1.0207 0.2525 0.044 Uiso 1 1 calc R . . C15 C 0.2892(8) 1.1488(15) 0.2319(7) 0.041(5) Uani 1 1 d . . . H15A H 0.2569 1.1475 0.2456 0.049 Uiso 1 1 calc R . . H15B H 0.3035 1.2091 0.2378 0.049 Uiso 1 1 calc R . . O4 O 0.2849(5) 1.1325(11) 0.1823(5) 0.046(4) Uani 1 1 d . . . C16 C 0.2470(11) 1.1859(16) 0.1594(9) 0.060(7) Uani 1 1 d . . . H16A H 0.2398 1.2391 0.1790 0.073 Uiso 1 1 calc R . . H16B H 0.2573 1.2072 0.1280 0.073 Uiso 1 1 calc R . . C17 C 0.2047(8) 1.1300(18) 0.1536(8) 0.050(6) Uani 1 1 d . . . H17A H 0.1763 1.1692 0.1473 0.060 Uiso 1 1 calc R . . H17B H 0.1997 1.0981 0.1839 0.060 Uiso 1 1 calc R . . O5 O 0.2066(6) 1.0641(11) 0.1160(5) 0.049(4) Uani 1 1 d . . . C18 C 0.1976(7) 1.0912(14) 0.0700(7) 0.037(5) Uani 1 1 d . . . C19 C 0.1875(9) 1.1800(14) 0.0570(8) 0.050(6) Uani 1 1 d . . . H19 H 0.1881 1.2269 0.0799 0.060 Uiso 1 1 calc R . . C20 C 0.1763(8) 1.1976(12) 0.0087(7) 0.037(5) Uani 1 1 d . . . C21 C 0.1658(10) 1.2856(13) -0.0074(8) 0.052(6) Uani 1 1 d . . . H21 H 0.1646 1.3342 0.0144 0.063 Uiso 1 1 calc R . . C22 C 0.1573(9) 1.2997(14) -0.0545(8) 0.051(6) Uani 1 1 d . . . H22 H 0.1540 1.3592 -0.0664 0.061 Uiso 1 1 calc R . . C23 C 0.1535(9) 1.2268(15) -0.0854(8) 0.049(6) Uani 1 1 d . . . H23 H 0.1429 1.2366 -0.1174 0.059 Uiso 1 1 calc R . . N2 N 0.1644(7) 1.1437(12) -0.0710(6) 0.044(5) Uani 1 1 d . . . C24 C 0.1755(7) 1.1292(13) -0.0254(7) 0.035(4) Uani 1 1 d . . . C25 C 0.1856(7) 1.0388(13) -0.0090(8) 0.036(4) Uani 1 1 d . . . H25 H 0.1844 0.9897 -0.0306 0.043 Uiso 1 1 calc R . . C26 C 0.1970(7) 1.0250(13) 0.0378(8) 0.041(5) Uani 1 1 d . . . H26 H 0.2049 0.9657 0.0481 0.049 Uiso 1 1 calc R . . N3 N 0.3231(6) 0.6223(9) -0.0782(6) 0.032(4) Uani 1 1 d . . . C27 C 0.3404(7) 0.5457(11) -0.0893(8) 0.034(4) Uani 1 1 d . . . H27 H 0.3718 0.5425 -0.1016 0.041 Uiso 1 1 calc R . . C28 C 0.3133(7) 0.4646(15) -0.0835(8) 0.045(5) Uani 1 1 d . . . H28 H 0.3277 0.4079 -0.0896 0.054 Uiso 1 1 calc R . . C29 C 0.2672(8) 0.4688(15) -0.0694(9) 0.052(6) Uani 1 1 d . . . H29 H 0.2481 0.4159 -0.0671 0.063 Uiso 1 1 calc R . . C30 C 0.2480(7) 0.5549(14) -0.0582(7) 0.037(5) Uani 1 1 d . . . C31 C 0.2005(8) 0.5623(15) -0.0423(9) 0.052(6) Uani 1 1 d . . . H31 H 0.1817 0.5097 -0.0379 0.062 Uiso 1 1 calc R . . C32 C 0.1819(7) 0.6437(12) -0.0336(7) 0.033(4) Uani 1 1 d . . . C33 C 0.2111(8) 0.7243(14) -0.0398(8) 0.044(5) Uani 1 1 d . . . H33 H 0.1974 0.7819 -0.0344 0.053 Uiso 1 1 calc R . . C34 C 0.2573(7) 0.7181(14) -0.0532(7) 0.035(4) Uani 1 1 d . . . H34 H 0.2765 0.7708 -0.0558 0.042 Uiso 1 1 calc R . . C35 C 0.2777(7) 0.6302(13) -0.0636(7) 0.033(4) Uani 1 1 d . . . O6 O 0.1365(5) 0.6611(11) -0.0192(6) 0.053(4) Uani 1 1 d . . . C36 C 0.1055(8) 0.5843(17) -0.0171(10) 0.058(7) Uani 1 1 d . . . H36A H 0.1180 0.5422 0.0076 0.070 Uiso 1 1 calc R . . H36B H 0.1046 0.5525 -0.0480 0.070 Uiso 1 1 calc R . . C37 C 0.0558(8) 0.6143(17) -0.0058(9) 0.055(6) Uani 1 1 d . . . H37A H 0.0481 0.6714 -0.0225 0.066 Uiso 1 1 calc R . . H37B H 0.0320 0.5685 -0.0166 0.066 Uiso 1 1 calc R . . O7 O 0.0532(6) 0.6269(11) 0.0433(6) 0.053(4) Uani 1 1 d . . . C38 C 0.0056(10) 0.656(2) 0.0535(11) 0.080(10) Uani 1 1 d . . . H38A H -0.0183 0.6287 0.0308 0.096 Uiso 1 1 calc R . . H38B H 0.0031 0.7221 0.0513 0.096 Uiso 1 1 calc R . . C39 C -0.0036(10) 0.6251(19) 0.1031(12) 0.072(9) Uani 1 1 d . . . H39A H -0.0375 0.6375 0.1106 0.087 Uiso 1 1 calc R . . H39B H 0.0021 0.5595 0.1058 0.087 Uiso 1 1 calc R . . O8 O 0.0281(6) 0.6719(14) 0.1351(5) 0.062(5) Uani 1 1 d . . . C40 C 0.0210(12) 0.621(4) 0.1797(12) 0.071(9) Uani 1 1 d . . . H40A H -0.0115 0.6334 0.1915 0.085 Uiso 1 1 calc R . . H40B H 0.0239 0.5558 0.1738 0.085 Uiso 1 1 calc R . . C41 C 0.0557(8) 0.648(2) 0.2127(9) 0.071(9) Uani 1 1 d . . . H41A H 0.0498 0.7122 0.2202 0.085 Uiso 1 1 calc R . . H41B H 0.0512 0.6133 0.2421 0.085 Uiso 1 1 calc R . . O9 O 0.1021(5) 0.6398(11) 0.2009(5) 0.048(4) Uani 1 1 d . . . C42 C 0.1347(9) 0.6441(19) 0.2395(9) 0.057(7) Uani 1 1 d . . . H42A H 0.1315 0.5894 0.2592 0.069 Uiso 1 1 calc R . . H42B H 0.1272 0.6970 0.2593 0.069 Uiso 1 1 calc R . . C43 C 0.1864(8) 0.6514(13) 0.2232(8) 0.043(5) Uani 1 1 d . . . H43A H 0.2099 0.6443 0.2503 0.051 Uiso 1 1 calc R . . H43B H 0.1930 0.6049 0.1991 0.051 Uiso 1 1 calc R . . O10 O 0.1893(5) 0.7407(9) 0.2030(5) 0.039(3) Uani 1 1 d . . . C44 C 0.2362(8) 0.7676(13) 0.1923(7) 0.037(5) Uani 1 1 d . . . C45 C 0.2767(7) 0.7212(12) 0.1953(6) 0.033(4) Uani 1 1 d . . . H45 H 0.2757 0.6601 0.2051 0.039 Uiso 1 1 calc R . . C46 C 0.3226(7) 0.7599(12) 0.1842(7) 0.031(4) Uani 1 1 d . . . C47 C 0.3633(7) 0.7129(12) 0.1858(6) 0.030(4) Uani 1 1 d . . . H47 H 0.3631 0.6505 0.1931 0.036 Uiso 1 1 calc R . . C48 C 0.4066(8) 0.7574(14) 0.1764(7) 0.039(5) Uani 1 1 d . . . H48 H 0.4366 0.7267 0.1791 0.047 Uiso 1 1 calc R . . C49 C 0.4045(6) 0.8475(14) 0.1632(7) 0.037(5) Uani 1 1 d . . . H49 H 0.4338 0.8785 0.1576 0.044 Uiso 1 1 calc R . . N4 N 0.3628(6) 0.8917(11) 0.1582(5) 0.034(4) Uani 1 1 d . . . C50 C 0.3223(7) 0.8530(11) 0.1693(7) 0.031(4) Uani 1 1 d . . . C51 C 0.2772(7) 0.8982(15) 0.1656(7) 0.037(5) Uani 1 1 d . . . H51 H 0.2769 0.9584 0.1543 0.044 Uiso 1 1 calc R . . C52 C 0.2352(8) 0.8617(12) 0.1771(8) 0.039(5) Uani 1 1 d . . . H52 H 0.2060 0.8953 0.1754 0.046 Uiso 1 1 calc R . . N5 N 0.1448(8) 0.8885(15) -0.1367(6) 0.055(5) Uani 1 1 d . . . C53 C 0.1048(7) 0.8396(17) -0.1353(8) 0.046(6) Uani 1 1 d . . . H53 H 0.0752 0.8674 -0.1276 0.055 Uiso 1 1 calc R . . C54 C 0.1059(8) 0.7480(18) -0.1448(8) 0.053(6) Uani 1 1 d . . . H54 H 0.0774 0.7134 -0.1416 0.064 Uiso 1 1 calc R . . C55 C 0.1460(7) 0.7073(15) -0.1583(8) 0.041(5) Uani 1 1 d . . . H55 H 0.1459 0.6454 -0.1667 0.050 Uiso 1 1 calc R . . C56 C 0.1899(7) 0.7606(13) -0.1596(7) 0.033(4) Uani 1 1 d . . . C57 C 0.2322(6) 0.7176(12) -0.1728(7) 0.031(4) Uani 1 1 d . . . H57 H 0.2325 0.6557 -0.1813 0.037 Uiso 1 1 calc R . . C58 C 0.2749(7) 0.7705(11) -0.1729(6) 0.029(4) Uani 1 1 d . . . C59 C 0.2716(7) 0.8643(12) -0.1603(6) 0.030(4) Uani 1 1 d . . . H59 H 0.3000 0.8998 -0.1619 0.036 Uiso 1 1 calc R . . C60 C 0.2326(8) 0.9037(15) -0.1469(7) 0.043(5) Uani 1 1 d . . . H60 H 0.2335 0.9648 -0.1370 0.051 Uiso 1 1 calc R . . C61 C 0.1868(7) 0.8522(12) -0.1473(6) 0.029(4) Uani 1 1 d . . . O11 O 0.3188(5) 0.7472(8) -0.1854(5) 0.036(3) Uani 1 1 d . . . C62 C 0.3248(9) 0.6536(13) -0.1999(7) 0.043(5) Uani 1 1 d . . . H62A H 0.3050 0.6405 -0.2290 0.052 Uiso 1 1 calc R . . H62B H 0.3151 0.6120 -0.1744 0.052 Uiso 1 1 calc R . . C63 C 0.3795(7) 0.6438(15) -0.2091(6) 0.037(5) Uani 1 1 d . . . H63A H 0.3860 0.5852 -0.2243 0.044 Uiso 1 1 calc R . . H63B H 0.3902 0.6925 -0.2302 0.044 Uiso 1 1 calc R . . O12 O 0.4035(5) 0.6493(9) -0.1650(5) 0.035(3) Uani 1 1 d . . . C64 C 0.4541(7) 0.6428(14) -0.1716(8) 0.040(5) Uani 1 1 d . . . H64A H 0.4655 0.6976 -0.1878 0.048 Uiso 1 1 calc R . . H64B H 0.4608 0.5902 -0.1919 0.048 Uiso 1 1 calc R . . C65 C 0.4796(7) 0.6331(15) -0.1263(8) 0.041(5) Uani 1 1 d . . . H65A H 0.5148 0.6308 -0.1313 0.049 Uiso 1 1 calc R . . H65B H 0.4702 0.5755 -0.1116 0.049 Uiso 1 1 calc R . . O13 O 0.4695(4) 0.7074(9) -0.0937(5) 0.035(3) Uani 1 1 d . . . C66 C 0.4915(7) 0.7008(15) -0.0475(9) 0.047(6) Uani 1 1 d . . . H66A H 0.4862 0.7578 -0.0302 0.056 Uiso 1 1 calc R . . H66B H 0.5268 0.6929 -0.0503 0.056 Uiso 1 1 calc R . . C67 C 0.4721(7) 0.6242(13) -0.0193(8) 0.038(5) Uani 1 1 d . . . H67A H 0.4802 0.5665 -0.0347 0.046 Uiso 1 1 calc R . . H67B H 0.4875 0.6245 0.0130 0.046 Uiso 1 1 calc R . . O14 O 0.4211(5) 0.6313(9) -0.0161(4) 0.033(3) Uani 1 1 d . . . C68 C 0.4014(8) 0.5794(12) 0.0197(7) 0.035(4) Uani 1 1 d . . . H68A H 0.4221 0.5261 0.0262 0.042 Uiso 1 1 calc R . . H68B H 0.3690 0.5580 0.0091 0.042 Uiso 1 1 calc R . . C69 C 0.3976(7) 0.6353(14) 0.0656(7) 0.038(5) Uani 1 1 d . . . H69A H 0.3939 0.5946 0.0930 0.045 Uiso 1 1 calc R . . H69B H 0.4274 0.6710 0.0712 0.045 Uiso 1 1 calc R . . O15 O 0.3568(5) 0.6943(9) 0.0611(5) 0.037(3) Uani 1 1 d . . . C70 C 0.3133(8) 0.6630(14) 0.0711(7) 0.042(5) Uani 1 1 d . . . C71 C 0.3023(7) 0.5724(14) 0.0820(7) 0.040(5) Uani 1 1 d . . . H71 H 0.3262 0.5264 0.0828 0.048 Uiso 1 1 calc R . . C72 C 0.2516(9) 0.5541(14) 0.0919(8) 0.045(5) Uani 1 1 d . . . C73 C 0.2404(9) 0.4638(15) 0.1047(9) 0.053(6) Uani 1 1 d . . . H73 H 0.2646 0.4184 0.1063 0.063 Uiso 1 1 calc R . . C74 C 0.1941(8) 0.4457(13) 0.1143(9) 0.050(6) Uani 1 1 d . . . H74 H 0.1851 0.3863 0.1226 0.060 Uiso 1 1 calc R . . C75 C 0.1579(9) 0.5166(15) 0.1121(9) 0.053(6) Uani 1 1 d . . . H75 H 0.1253 0.5025 0.1182 0.063 Uiso 1 1 calc R . . N6 N 0.1701(6) 0.6030(11) 0.1014(6) 0.037(4) Uani 1 1 d . . . C76 C 0.2170(7) 0.6178(13) 0.0911(7) 0.035(4) Uani 1 1 d . . . C77 C 0.2303(8) 0.7082(14) 0.0801(7) 0.039(5) Uani 1 1 d . . . H77 H 0.2067 0.7546 0.0804 0.047 Uiso 1 1 calc R . . C78 C 0.2762(7) 0.7281(12) 0.0693(7) 0.032(4) Uani 1 1 d . . . H78 H 0.2838 0.7879 0.0602 0.038 Uiso 1 1 calc R . . N7 N 0.3504(6) 1.1525(10) 0.0902(5) 0.032(4) Uani 1 1 d . . . C79 C 0.3636(7) 1.2347(13) 0.1050(8) 0.037(4) Uani 1 1 d . . . H79 H 0.3741 1.2420 0.1373 0.044 Uiso 1 1 calc R . . C80 C 0.3629(8) 1.3118(15) 0.0750(9) 0.047(6) Uani 1 1 d . . . H80 H 0.3737 1.3687 0.0866 0.057 Uiso 1 1 calc R . . C81 C 0.3465(9) 1.3020(14) 0.0298(8) 0.050(6) Uani 1 1 d . . . H81 H 0.3449 1.3531 0.0096 0.060 Uiso 1 1 calc R . . C82 C 0.3315(7) 1.2168(11) 0.0118(7) 0.031(4) Uani 1 1 d . . . C83 C 0.3142(7) 1.2042(13) -0.0364(7) 0.037(5) Uani 1 1 d . . . H83 H 0.3127 1.2534 -0.0579 0.045 Uiso 1 1 calc R . . C84 C 0.3003(8) 1.1217(13) -0.0504(8) 0.040(5) Uani 1 1 d . . . C85 C 0.3042(6) 1.0461(13) -0.0182(7) 0.031(4) Uani 1 1 d . . . H85 H 0.2956 0.9877 -0.0292 0.037 Uiso 1 1 calc R . . C86 C 0.3201(7) 1.0574(12) 0.0273(7) 0.034(4) Uani 1 1 d . . . H86 H 0.3216 1.0077 0.0485 0.041 Uiso 1 1 calc R . . C87 C 0.3343(6) 1.1435(11) 0.0428(7) 0.029(4) Uani 1 1 d . . . O16 O 0.2853(5) 1.1013(10) -0.0959(5) 0.042(3) Uani 1 1 d . . . C88 C 0.2878(8) 1.1684(15) -0.1302(7) 0.042(5) Uani 1 1 d . . . H88A H 0.3212 1.1921 -0.1308 0.050 Uiso 1 1 calc R . . H88B H 0.2660 1.2187 -0.1223 0.050 Uiso 1 1 calc R . . C89 C 0.2736(8) 1.1318(14) -0.1765(8) 0.047(6) Uani 1 1 d . . . H89A H 0.2859 1.1712 -0.2017 0.057 Uiso 1 1 calc R . . H89B H 0.2881 1.0715 -0.1801 0.057 Uiso 1 1 calc R . . O17 O 0.2223(5) 1.1251(10) -0.1821(5) 0.044(4) Uani 1 1 d . . . C90 C 0.2106(11) 1.092(2) -0.2295(9) 0.072(8) Uani 1 1 d . . . H90A H 0.2127 1.0251 -0.2301 0.087 Uiso 1 1 calc R . . H90B H 0.2334 1.1163 -0.2523 0.087 Uiso 1 1 calc R . . C91 C 0.1588(13) 1.122(2) -0.2426(10) 0.081(10) Uani 1 1 d . . . H91A H 0.1560 1.1884 -0.2392 0.097 Uiso 1 1 calc R . . H91B H 0.1500 1.1057 -0.2758 0.097 Uiso 1 1 calc R . . O18 O 0.1271(5) 1.0766(19) -0.2098(8) 0.103(10) Uani 1 1 d . . . C92 C 0.0822(13) 1.129(3) -0.2210(10) 0.090(11) Uani 1 1 d . . . H92A H 0.0884 1.1942 -0.2166 0.108 Uiso 1 1 calc R . . H92B H 0.0712 1.1187 -0.2544 0.108 Uiso 1 1 calc R . . C93 C 0.0468(10) 1.099(2) -0.1897(9) 0.073(9) Uani 1 1 d . . . H93A H 0.0403 1.0345 -0.1949 0.088 Uiso 1 1 calc R . . H93B H 0.0163 1.1328 -0.1961 0.088 Uiso 1 1 calc R . . O19 O 0.0635(5) 1.1140(10) -0.1403(5) 0.042(3) Uani 1 1 d . . . C94 C 0.0227(7) 1.1119(16) -0.1097(7) 0.038(5) Uani 1 1 d . . . H94A H 0.0012 1.0610 -0.1186 0.046 Uiso 1 1 calc R . . H94B H 0.0039 1.1684 -0.1133 0.046 Uiso 1 1 calc R . . C95 C 0.0408(8) 1.1016(13) -0.0594(7) 0.040(5) Uani 1 1 d . . . H95A H 0.0666 1.1459 -0.0517 0.048 Uiso 1 1 calc R . . H95B H 0.0143 1.1103 -0.0373 0.048 Uiso 1 1 calc R . . O20 O 0.0592(5) 1.0124(9) -0.0561(5) 0.042(3) Uani 1 1 d . . . C96 C 0.0703(6) 0.9807(12) -0.0105(7) 0.028(4) Uani 1 1 d . . . C97 C 0.0688(7) 1.0310(13) 0.0300(7) 0.035(4) Uani 1 1 d . . . H97 H 0.0597 1.0926 0.0285 0.042 Uiso 1 1 calc R . . C98 C 0.0811(7) 0.9898(12) 0.0748(6) 0.029(4) Uani 1 1 d . . . C99 C 0.0819(8) 1.0383(14) 0.1190(8) 0.041(5) Uani 1 1 d . . . H99 H 0.0749 1.1008 0.1198 0.049 Uiso 1 1 calc R . . C100 C 0.0928(9) 0.9933(17) 0.1585(8) 0.053(6) Uani 1 1 d . . . H100 H 0.0938 1.0249 0.1878 0.063 Uiso 1 1 calc R . . C101 C 0.1024(7) 0.9043(15) 0.1586(7) 0.037(5) Uani 1 1 d . . . H101 H 0.1087 0.8751 0.1881 0.044 Uiso 1 1 calc R . . N8 N 0.1032(6) 0.8552(9) 0.1183(6) 0.035(4) Uani 1 1 d . . . C102 C 0.0933(7) 0.8979(13) 0.0763(7) 0.035(4) Uani 1 1 d . . . C103 C 0.0954(7) 0.8486(11) 0.0343(7) 0.039(5) Uani 1 1 d . . . H103 H 0.1045 0.7870 0.0350 0.046 Uiso 1 1 calc R . . C104 C 0.0840(8) 0.8902(13) -0.0079(7) 0.039(5) Uani 1 1 d . . . H104 H 0.0855 0.8565 -0.0365 0.046 Uiso 1 1 calc R . . Sb1 Sb 0.54974(5) 0.65694(9) 0.11253(6) 0.0408(4) Uani 1 1 d . . . F1 F 0.4965(5) 0.5808(10) 0.1043(6) 0.070(4) Uani 1 1 d . . . F2 F 0.6038(6) 0.7316(11) 0.1194(8) 0.092(6) Uani 1 1 d . . . F3 F 0.5830(6) 0.5698(10) 0.1482(6) 0.073(4) Uani 1 1 d . . . F4 F 0.5732(6) 0.6068(16) 0.0580(6) 0.096(6) Uani 1 1 d . . . F5 F 0.5161(6) 0.7425(9) 0.0771(6) 0.075(5) Uani 1 1 d . . . F6 F 0.5254(5) 0.7014(13) 0.1653(5) 0.080(5) Uani 1 1 d . . . Sb2 Sb 0.37810(7) 0.43246(10) 0.21965(5) 0.0492(4) Uani 1 1 d . . . F7 F 0.3274(7) 0.3618(11) 0.1943(6) 0.082(5) Uani 1 1 d . . . F8 F 0.4263(8) 0.5063(15) 0.2452(8) 0.115(8) Uani 1 1 d . . . F9 F 0.3777(9) 0.4898(13) 0.1615(6) 0.103(7) Uani 1 1 d . . . F10 F 0.3319(8) 0.5130(10) 0.2410(8) 0.104(7) Uani 1 1 d . . . F11 F 0.3759(6) 0.3690(10) 0.2769(5) 0.075(5) Uani 1 1 d . . . F12 F 0.4225(7) 0.3510(10) 0.1966(6) 0.082(5) Uani 1 1 d . . . Sb3 Sb 0.04597(6) 0.32276(10) 0.11426(7) 0.0530(5) Uani 1 1 d . . . F13 F -0.0137(5) 0.3804(10) 0.1103(6) 0.065(4) Uani 1 1 d . . . F14 F 0.1048(6) 0.2635(13) 0.1191(8) 0.104(7) Uani 1 1 d . . . F15 F 0.0670(6) 0.3934(11) 0.0643(6) 0.076(5) Uani 1 1 d . . . F16 F 0.0700(6) 0.4089(9) 0.1569(5) 0.065(4) Uani 1 1 d . . . F17 F 0.0238(7) 0.2379(10) 0.0705(8) 0.110(8) Uani 1 1 d . . . F18 F 0.0235(6) 0.2522(13) 0.1638(9) 0.117(8) Uani 1 1 d . . . Sb4 Sb 0.15459(7) 0.42536(11) 0.80676(6) 0.0532(5) Uani 1 1 d . . . F19 F 0.2015(7) 0.5043(12) 0.7872(9) 0.107(7) Uani 1 1 d . . . F20 F 0.1085(5) 0.3469(12) 0.8268(6) 0.071(4) Uani 1 1 d . . . F21 F 0.1541(8) 0.3676(14) 0.7491(6) 0.107(7) Uani 1 1 d . . . F22 F 0.2015(6) 0.3489(11) 0.8323(7) 0.082(5) Uani 1 1 d . . . F23 F 0.1518(9) 0.4848(16) 0.8644(6) 0.117(8) Uani 1 1 d . . . F24 F 0.1098(8) 0.5043(15) 0.7817(6) 0.105(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0388(8) 0.0274(7) 0.0430(9) -0.0049(6) 0.0059(7) -0.0093(6) Ag2 0.0474(10) 0.0468(10) 0.0505(10) -0.0203(8) -0.0021(8) 0.0074(8) Ag3 0.0431(9) 0.0267(7) 0.0400(8) 0.0067(6) 0.0036(7) -0.0043(6) Ag4 0.0436(9) 0.0350(8) 0.0497(10) 0.0122(7) 0.0050(7) 0.0104(7) N1 0.008(6) 0.040(9) 0.034(8) -0.005(7) -0.002(6) -0.008(6) C1 0.058(15) 0.055(14) 0.035(12) -0.006(11) 0.010(10) -0.013(12) C2 0.047(12) 0.034(11) 0.042(12) 0.008(9) 0.006(10) 0.007(9) C3 0.049(12) 0.029(10) 0.038(11) 0.004(8) 0.005(9) -0.008(9) C4 0.024(9) 0.021(9) 0.040(11) 0.007(8) -0.001(8) -0.007(7) C5 0.029(9) 0.018(8) 0.054(12) -0.010(8) -0.003(9) -0.013(7) C6 0.033(10) 0.026(9) 0.022(9) -0.007(7) -0.002(7) -0.003(7) C7 0.063(14) 0.015(9) 0.045(12) -0.001(8) 0.021(10) -0.005(9) C8 0.038(11) 0.021(9) 0.049(12) -0.004(8) 0.008(9) -0.007(8) C9 0.036(10) 0.008(8) 0.057(13) -0.006(8) -0.001(9) 0.000(7) O1 0.040(8) 0.026(7) 0.048(8) -0.014(6) -0.003(6) -0.009(6) C10 0.026(9) 0.030(10) 0.046(12) -0.008(8) 0.001(8) -0.010(8) C11 0.039(11) 0.030(10) 0.045(12) -0.008(9) 0.015(9) -0.004(8) O2 0.034(7) 0.030(7) 0.035(7) 0.003(6) 0.001(6) -0.003(6) C12 0.057(14) 0.036(12) 0.048(13) 0.000(10) 0.015(11) 0.000(10) C13 0.054(14) 0.058(15) 0.044(13) -0.009(11) 0.007(11) -0.005(12) O3 0.051(9) 0.021(6) 0.043(8) 0.002(6) 0.002(7) 0.002(6) C14 0.044(12) 0.030(10) 0.034(10) 0.013(8) 0.002(9) -0.006(9) C15 0.044(12) 0.050(13) 0.029(10) 0.007(9) 0.012(9) 0.000(10) O4 0.045(9) 0.059(10) 0.033(8) -0.008(7) 0.002(6) 0.002(7) C16 0.10(2) 0.036(12) 0.042(13) 0.000(10) -0.004(13) 0.016(13) C17 0.034(12) 0.075(17) 0.040(12) 0.020(12) -0.006(9) 0.012(11) O5 0.058(10) 0.050(9) 0.040(9) 0.001(7) 0.007(7) 0.003(8) C18 0.043(11) 0.041(11) 0.027(10) 0.003(8) 0.005(8) -0.005(9) C19 0.087(18) 0.021(10) 0.044(13) 0.003(9) 0.009(12) 0.024(11) C20 0.057(13) 0.013(8) 0.040(11) -0.004(7) -0.014(9) -0.010(8) C21 0.094(19) 0.011(9) 0.053(14) 0.003(9) 0.012(13) -0.001(10) C22 0.077(17) 0.018(10) 0.057(15) 0.003(9) -0.017(12) -0.015(10) C23 0.055(14) 0.043(13) 0.047(13) -0.007(10) -0.007(11) -0.015(11) N2 0.061(12) 0.031(9) 0.041(10) -0.011(8) 0.006(9) -0.026(8) C24 0.029(10) 0.031(10) 0.046(12) -0.008(9) 0.013(9) -0.004(8) C25 0.034(10) 0.022(9) 0.050(13) -0.003(8) -0.001(9) 0.000(8) C26 0.034(11) 0.025(10) 0.064(15) -0.006(9) -0.003(10) 0.002(8) N3 0.038(9) 0.012(7) 0.047(10) 0.003(6) 0.004(7) -0.006(6) C27 0.025(9) 0.011(8) 0.066(14) 0.000(8) 0.006(9) 0.006(7) C28 0.031(11) 0.038(12) 0.066(15) 0.012(11) -0.002(10) 0.006(9) C29 0.046(13) 0.031(11) 0.079(17) 0.016(11) 0.001(12) -0.002(10) C30 0.034(10) 0.041(12) 0.037(11) 0.000(9) 0.011(9) -0.013(9) C31 0.035(12) 0.038(12) 0.083(18) -0.016(12) 0.014(11) -0.007(9) C32 0.030(10) 0.022(9) 0.047(12) -0.004(8) -0.003(8) -0.003(7) C33 0.053(13) 0.031(11) 0.049(13) -0.012(9) 0.006(10) 0.000(10) C34 0.036(11) 0.034(11) 0.036(11) 0.003(8) 0.000(8) 0.008(8) C35 0.036(10) 0.028(10) 0.035(10) -0.011(8) -0.001(8) 0.009(8) O6 0.028(8) 0.049(9) 0.084(12) -0.023(9) 0.011(8) -0.001(7) C36 0.044(13) 0.049(14) 0.082(18) -0.034(13) 0.015(12) -0.010(11) C37 0.043(13) 0.047(14) 0.073(18) 0.006(12) -0.005(12) -0.012(11) O7 0.044(9) 0.053(10) 0.062(11) -0.016(8) 0.011(8) -0.004(7) C38 0.052(16) 0.10(2) 0.09(2) -0.021(19) 0.007(15) 0.046(16) C39 0.047(15) 0.055(16) 0.12(3) 0.016(16) -0.004(16) -0.024(13) O8 0.064(11) 0.089(14) 0.032(8) 0.022(9) -0.002(8) 0.022(10) C40 0.029(12) 0.13(3) 0.056(16) 0.010(17) 0.007(11) -0.006(14) C41 0.029(12) 0.13(3) 0.056(16) 0.010(17) 0.007(11) -0.006(14) O9 0.046(9) 0.059(10) 0.038(8) 0.006(7) 0.005(7) 0.000(7) C42 0.057(15) 0.067(17) 0.046(14) 0.005(12) -0.009(11) -0.022(13) C43 0.052(13) 0.026(10) 0.049(13) 0.007(9) -0.005(10) -0.008(9) O10 0.036(8) 0.033(7) 0.048(8) 0.008(6) 0.005(6) -0.004(6) C44 0.048(12) 0.032(10) 0.030(10) -0.011(8) 0.000(9) -0.012(9) C45 0.053(12) 0.022(9) 0.023(9) 0.005(7) -0.012(8) 0.002(8) C46 0.038(10) 0.018(8) 0.038(11) -0.008(7) 0.004(8) -0.006(8) C47 0.041(11) 0.018(8) 0.031(10) 0.009(7) 0.004(8) 0.005(8) C48 0.037(11) 0.034(11) 0.046(12) 0.007(9) 0.002(9) 0.005(9) C49 0.018(9) 0.039(11) 0.053(13) 0.001(9) -0.014(8) -0.008(8) N4 0.049(10) 0.028(8) 0.024(8) 0.008(6) -0.006(7) 0.003(7) C50 0.048(12) 0.014(8) 0.031(10) -0.002(7) 0.003(8) 0.005(8) C51 0.026(10) 0.049(12) 0.034(11) 0.005(9) -0.007(8) 0.005(9) C52 0.042(11) 0.015(9) 0.059(13) 0.014(8) 0.008(10) 0.010(8) N5 0.075(15) 0.072(14) 0.020(9) -0.004(9) 0.012(9) -0.013(12) C53 0.026(10) 0.071(16) 0.041(12) 0.005(11) -0.005(9) -0.014(10) C54 0.035(12) 0.073(18) 0.053(14) 0.009(12) 0.014(10) -0.025(12) C55 0.029(10) 0.041(12) 0.054(13) 0.003(10) -0.001(9) -0.016(9) C56 0.034(10) 0.030(10) 0.035(10) -0.003(8) 0.003(8) 0.003(8) C57 0.029(9) 0.022(9) 0.041(11) 0.012(8) 0.003(8) 0.004(7) C58 0.048(11) 0.008(7) 0.030(10) 0.003(7) -0.002(8) -0.004(7) C59 0.033(10) 0.025(9) 0.030(10) 0.001(7) -0.007(8) -0.006(8) C60 0.047(13) 0.040(12) 0.041(12) -0.008(9) -0.004(10) 0.009(10) C61 0.043(11) 0.023(9) 0.021(9) 0.007(7) 0.006(8) 0.012(8) O11 0.051(9) 0.007(5) 0.051(8) -0.004(5) 0.002(7) 0.003(5) C62 0.070(15) 0.027(10) 0.032(11) -0.009(8) -0.002(10) -0.004(10) C63 0.049(12) 0.050(12) 0.011(8) -0.008(8) 0.002(8) 0.020(10) O12 0.030(7) 0.033(7) 0.041(8) -0.003(6) 0.003(6) 0.003(6) C64 0.029(10) 0.035(11) 0.054(13) -0.010(9) -0.012(9) 0.001(8) C65 0.022(9) 0.046(12) 0.056(13) -0.018(10) 0.011(9) 0.004(8) O13 0.026(7) 0.035(7) 0.043(8) -0.009(6) 0.008(6) 0.002(6) C66 0.027(10) 0.038(12) 0.074(16) 0.005(11) -0.002(10) -0.010(9) C67 0.037(11) 0.030(10) 0.048(12) 0.002(9) 0.000(9) 0.000(8) O14 0.031(7) 0.038(7) 0.031(7) -0.005(6) -0.001(6) 0.001(6) C68 0.046(12) 0.024(9) 0.035(11) 0.006(8) 0.010(9) 0.005(8) C69 0.043(12) 0.038(11) 0.032(10) 0.010(9) 0.013(9) -0.007(9) O15 0.036(7) 0.029(7) 0.049(8) -0.001(6) 0.021(6) 0.001(6) C70 0.062(14) 0.034(11) 0.029(10) -0.001(8) 0.000(9) -0.020(10) C71 0.038(11) 0.034(11) 0.048(12) -0.001(9) 0.016(9) 0.003(9) C72 0.058(14) 0.031(11) 0.045(13) 0.004(9) 0.001(10) 0.003(10) C73 0.048(13) 0.032(11) 0.080(18) 0.007(11) 0.017(12) -0.001(10) C74 0.051(14) 0.015(9) 0.084(18) -0.010(10) 0.006(12) -0.006(9) C75 0.051(14) 0.033(12) 0.076(17) 0.005(11) 0.024(12) -0.017(10) N6 0.038(9) 0.038(9) 0.037(9) -0.021(7) 0.007(7) -0.006(7) C76 0.035(11) 0.036(11) 0.033(10) -0.005(8) 0.009(8) 0.017(9) C77 0.061(14) 0.031(10) 0.026(10) 0.004(8) -0.003(9) 0.005(10) C78 0.042(11) 0.022(9) 0.032(10) 0.001(7) 0.009(8) 0.004(8) N7 0.043(9) 0.025(8) 0.029(8) 0.010(6) 0.009(7) 0.005(7) C79 0.033(10) 0.034(11) 0.043(12) 0.003(9) 0.009(9) -0.001(8) C80 0.040(12) 0.034(11) 0.067(16) -0.009(11) -0.007(11) -0.007(9) C81 0.081(17) 0.022(10) 0.046(13) 0.016(9) -0.012(12) -0.005(10) C82 0.037(10) 0.014(8) 0.042(11) -0.002(7) -0.007(8) -0.010(7) C83 0.042(11) 0.024(9) 0.045(12) 0.007(8) -0.008(9) -0.002(8) C84 0.049(12) 0.020(9) 0.052(13) -0.005(9) 0.003(10) -0.013(9) C85 0.023(9) 0.029(9) 0.041(11) -0.001(8) -0.006(8) 0.007(7) C86 0.042(11) 0.024(9) 0.036(11) 0.014(8) 0.004(9) 0.003(8) C87 0.024(9) 0.018(8) 0.047(11) 0.001(8) 0.013(8) -0.005(7) O16 0.046(8) 0.036(8) 0.044(8) 0.004(6) -0.004(7) -0.013(7) C88 0.043(12) 0.050(13) 0.032(11) 0.023(10) -0.011(9) -0.011(10) C89 0.050(13) 0.026(10) 0.063(15) 0.010(10) -0.025(11) -0.016(9) O17 0.040(8) 0.042(8) 0.051(9) 0.001(7) -0.008(7) -0.014(7) C90 0.10(2) 0.08(2) 0.042(14) -0.004(14) 0.032(15) 0.002(17) C91 0.13(3) 0.064(19) 0.049(16) -0.016(14) 0.000(18) 0.036(19) O18 0.015(7) 0.20(3) 0.091(15) -0.106(17) -0.001(8) -0.013(11) C92 0.12(3) 0.10(3) 0.043(16) -0.018(17) -0.035(18) 0.01(2) C93 0.056(16) 0.12(3) 0.046(15) 0.023(16) -0.025(13) -0.016(16) O19 0.031(7) 0.047(9) 0.048(9) 0.004(7) 0.002(6) 0.004(6) C94 0.027(10) 0.060(14) 0.026(10) 0.004(9) 0.000(8) 0.014(9) C95 0.049(12) 0.028(10) 0.043(12) 0.005(9) 0.012(10) 0.013(9) O20 0.054(9) 0.031(7) 0.039(8) 0.013(6) -0.001(7) 0.014(7) C96 0.023(9) 0.024(9) 0.037(10) 0.006(8) -0.007(7) 0.010(7) C97 0.045(11) 0.030(10) 0.031(10) 0.017(8) 0.007(8) 0.017(9) C98 0.035(10) 0.020(8) 0.031(10) 0.001(7) -0.013(8) 0.003(7) C99 0.049(12) 0.028(10) 0.046(12) 0.004(9) 0.005(10) 0.008(9) C100 0.074(17) 0.056(15) 0.028(11) -0.012(10) -0.004(11) -0.014(13) C101 0.033(10) 0.049(13) 0.028(10) 0.009(9) -0.008(8) 0.005(9) N8 0.047(10) 0.004(6) 0.056(11) 0.001(6) 0.012(8) 0.003(6) C102 0.025(9) 0.033(10) 0.048(12) 0.001(9) -0.002(8) -0.002(8) C103 0.053(13) 0.030(10) 0.033(11) -0.017(8) 0.009(9) -0.006(9) C104 0.053(13) 0.030(10) 0.033(11) -0.017(8) 0.009(9) -0.006(9) Sb1 0.0351(7) 0.0292(7) 0.0575(9) -0.0001(6) -0.0048(6) 0.0009(6) F1 0.056(9) 0.051(9) 0.101(12) 0.001(8) -0.030(8) 0.000(7) F2 0.069(11) 0.053(10) 0.152(18) 0.014(10) -0.018(11) -0.034(8) F3 0.091(12) 0.057(9) 0.070(10) 0.002(8) 0.001(8) 0.034(8) F4 0.073(11) 0.155(19) 0.059(10) -0.014(11) 0.002(8) 0.023(12) F5 0.069(10) 0.036(8) 0.116(13) 0.002(8) -0.046(9) 0.000(7) F6 0.053(9) 0.124(15) 0.061(9) -0.026(9) -0.013(7) 0.057(9) Sb2 0.0799(12) 0.0259(7) 0.0424(8) 0.0015(6) 0.0116(8) 0.0003(7) F7 0.098(13) 0.052(9) 0.096(13) -0.018(9) -0.009(10) -0.002(9) F8 0.119(17) 0.101(16) 0.126(17) -0.027(13) 0.026(14) -0.054(13) F9 0.17(2) 0.083(13) 0.054(10) 0.015(9) 0.011(11) 0.004(13) F10 0.123(16) 0.032(8) 0.162(19) 0.011(10) 0.057(14) 0.016(9) F11 0.109(13) 0.058(9) 0.060(9) 0.011(7) 0.034(9) 0.025(9) F12 0.111(14) 0.045(9) 0.093(12) 0.014(8) 0.041(10) 0.002(9) Sb3 0.0402(8) 0.0280(7) 0.0902(13) -0.0016(8) -0.0066(8) -0.0002(6) F13 0.044(8) 0.056(9) 0.094(11) -0.010(8) -0.009(7) 0.004(7) F14 0.068(11) 0.069(12) 0.17(2) 0.003(12) -0.012(12) 0.036(9) F15 0.063(10) 0.073(11) 0.092(12) 0.018(9) 0.016(9) -0.005(8) F16 0.075(10) 0.047(8) 0.074(10) -0.003(7) -0.007(8) -0.012(7) F17 0.112(15) 0.033(8) 0.18(2) -0.046(11) -0.048(14) 0.030(9) F18 0.070(11) 0.087(13) 0.19(2) 0.089(15) 0.004(13) -0.019(10) Sb4 0.0782(12) 0.0357(8) 0.0461(9) 0.0000(7) 0.0092(8) 0.0052(8) F19 0.098(14) 0.052(10) 0.17(2) 0.011(12) 0.030(14) -0.021(10) F20 0.051(8) 0.084(11) 0.079(11) -0.013(9) 0.001(7) 0.010(8) F21 0.156(19) 0.111(15) 0.057(10) -0.037(10) 0.048(11) -0.059(14) F22 0.079(11) 0.049(9) 0.118(14) 0.016(9) 0.001(10) 0.010(8) F23 0.18(2) 0.129(18) 0.043(10) -0.019(11) 0.014(11) 0.009(16) F24 0.132(17) 0.125(17) 0.056(10) 0.006(10) -0.017(10) 0.066(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.213(15) . ? Ag1 N3 2.235(14) . ? Ag2 N2 2.194(16) . ? Ag2 N5 2.22(2) . ? Ag2 O18 2.60(2) . ? Ag3 N7 2.207(14) . ? Ag3 N4 2.246(15) . ? Ag4 N6 2.181(17) . ? Ag4 N8 2.219(13) . ? N1 C1 1.25(3) . ? N1 C9 1.40(2) . ? C1 C2 1.37(3) . ? C1 H1 0.9500 . ? C2 C3 1.34(3) . ? C2 H2 0.9500 . ? C3 C4 1.40(3) . ? C3 H3 0.9500 . ? C4 C9 1.41(2) . ? C4 C5 1.49(3) . ? C5 C6 1.28(3) . ? C5 H5 0.9500 . ? C6 O1 1.40(2) . ? C6 C7 1.46(2) . ? C7 C8 1.36(3) . ? C7 H7 0.9500 . ? C8 C9 1.39(3) . ? C8 H8 0.9500 . ? O1 C10 1.43(2) . ? C10 C11 1.52(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 O2 1.44(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? O2 C12 1.44(3) . ? C12 C13 1.43(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 O3 1.46(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? O3 C14 1.43(2) . ? C14 C15 1.47(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 O4 1.42(2) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? O4 C16 1.45(3) . ? C16 C17 1.44(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 O5 1.44(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? O5 C18 1.37(2) . ? C18 C26 1.34(3) . ? C18 C19 1.39(3) . ? C19 C20 1.41(3) . ? C19 H19 0.9500 . ? C20 C24 1.40(3) . ? C20 C21 1.41(3) . ? C21 C22 1.36(3) . ? C21 H21 0.9500 . ? C22 C23 1.39(3) . ? C22 H22 0.9500 . ? C23 N2 1.33(3) . ? C23 H23 0.9500 . ? N2 C24 1.33(3) . ? C24 C25 1.44(3) . ? C25 C26 1.36(3) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? N3 C27 1.28(2) . ? N3 C35 1.34(2) . ? C27 C28 1.43(3) . ? C27 H27 0.9500 . ? C28 C29 1.35(3) . ? C28 H28 0.9500 . ? C29 C30 1.43(3) . ? C29 H29 0.9500 . ? C30 C35 1.40(3) . ? C30 C31 1.41(3) . ? C31 C32 1.34(3) . ? C31 H31 0.9500 . ? C32 O6 1.36(2) . ? C32 C33 1.46(3) . ? C33 C34 1.35(3) . ? C33 H33 0.9500 . ? C34 C35 1.46(3) . ? C34 H34 0.9500 . ? O6 C36 1.43(3) . ? C36 C37 1.49(3) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 O7 1.40(3) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? O7 C38 1.43(3) . ? C38 C39 1.50(4) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 O8 1.42(3) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? O8 C40 1.48(3) . ? C40 C41 1.37(4) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 O9 1.35(3) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? O9 C42 1.39(3) . ? C42 C43 1.53(3) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 O10 1.45(2) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? O10 C44 1.40(2) . ? C44 C45 1.32(3) . ? C44 C52 1.46(3) . ? C45 C46 1.44(3) . ? C45 H45 0.9500 . ? C46 C47 1.32(3) . ? C46 C50 1.45(2) . ? C47 C48 1.40(3) . ? C47 H47 0.9500 . ? C48 C49 1.39(3) . ? C48 H48 0.9500 . ? C49 N4 1.33(2) . ? C49 H49 0.9500 . ? N4 C50 1.31(3) . ? C50 C51 1.42(3) . ? C51 C52 1.33(3) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? N5 C61 1.33(3) . ? N5 C53 1.33(3) . ? C53 C54 1.39(4) . ? C53 H53 0.9500 . ? C54 C55 1.33(3) . ? C54 H54 0.9500 . ? C55 C56 1.45(3) . ? C55 H55 0.9500 . ? C56 C57 1.40(3) . ? C56 C61 1.41(3) . ? C57 C58 1.42(3) . ? C57 H57 0.9500 . ? C58 O11 1.32(2) . ? C58 C59 1.44(2) . ? C59 C60 1.30(3) . ? C59 H59 0.9500 . ? C60 C61 1.48(3) . ? C60 H60 0.9500 . ? O11 C62 1.46(2) . ? C62 C63 1.55(3) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 O12 1.39(2) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? O12 C64 1.42(2) . ? C64 C65 1.44(3) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 O13 1.47(2) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? O13 C66 1.42(3) . ? C66 C67 1.50(3) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 O14 1.42(2) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? O14 C68 1.40(2) . ? C68 C69 1.54(3) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 O15 1.43(2) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? O15 C70 1.33(2) . ? C70 C78 1.41(3) . ? C70 C71 1.42(3) . ? C71 C72 1.47(3) . ? C71 H71 0.9500 . ? C72 C76 1.35(3) . ? C72 C73 1.42(3) . ? C73 C74 1.35(3) . ? C73 H73 0.9500 . ? C74 C75 1.45(3) . ? C74 H74 0.9500 . ? C75 N6 1.36(3) . ? C75 H75 0.9500 . ? N6 C76 1.36(3) . ? C76 C77 1.43(3) . ? C77 C78 1.35(3) . ? C77 H77 0.9500 . ? C78 H78 0.9500 . ? N7 C79 1.34(3) . ? N7 C87 1.40(2) . ? C79 C80 1.42(3) . ? C79 H79 0.9500 . ? C80 C81 1.34(3) . ? C80 H80 0.9500 . ? C81 C82 1.42(3) . ? C81 H81 0.9500 . ? C82 C87 1.40(3) . ? C82 C83 1.43(3) . ? C83 C84 1.34(3) . ? C83 H83 0.9500 . ? C84 O16 1.37(2) . ? C84 C85 1.45(3) . ? C85 C86 1.35(3) . ? C85 H85 0.9500 . ? C86 C87 1.40(3) . ? C86 H86 0.9500 . ? O16 C88 1.39(2) . ? C88 C89 1.46(3) . ? C88 H88A 0.9900 . ? C88 H88B 0.9900 . ? C89 O17 1.43(3) . ? C89 H89A 0.9900 . ? C89 H89B 0.9900 . ? O17 C90 1.45(3) . ? C90 C91 1.54(4) . ? C90 H90A 0.9900 . ? C90 H90B 0.9900 . ? C91 O18 1.47(4) . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? O18 C92 1.49(4) . ? C92 C93 1.42(4) . ? C92 H92A 0.9900 . ? C92 H92B 0.9900 . ? C93 O19 1.47(3) . ? C93 H93A 0.9900 . ? C93 H93B 0.9900 . ? O19 C94 1.45(2) . ? C94 C95 1.49(3) . ? C94 H94A 0.9900 . ? C94 H94B 0.9900 . ? C95 O20 1.42(2) . ? C95 H95A 0.9900 . ? C95 H95B 0.9900 . ? O20 C96 1.39(2) . ? C96 C97 1.37(3) . ? C96 C104 1.40(3) . ? C97 C98 1.43(2) . ? C97 H97 0.9500 . ? C98 C102 1.41(3) . ? C98 C99 1.44(3) . ? C99 C100 1.32(3) . ? C99 H99 0.9500 . ? C100 C101 1.35(3) . ? C100 H100 0.9500 . ? C101 N8 1.35(3) . ? C101 H101 0.9500 . ? N8 C102 1.36(3) . ? C102 C103 1.39(3) . ? C103 C104 1.37(3) . ? C103 H103 0.9500 . ? C104 H104 0.9500 . ? Sb1 F6 1.782(14) . ? Sb1 F5 1.846(14) . ? Sb1 F4 1.848(17) . ? Sb1 F3 1.861(14) . ? Sb1 F1 1.866(14) . ? Sb1 F2 1.869(14) . ? Sb2 F9 1.847(17) . ? Sb2 F8 1.851(19) . ? Sb2 F12 1.861(16) . ? Sb2 F10 1.869(17) . ? Sb2 F11 1.873(14) . ? Sb2 F7 1.873(17) . ? Sb3 F17 1.852(17) . ? Sb3 F14 1.852(16) . ? Sb3 F13 1.862(14) . ? Sb3 F16 1.862(14) . ? Sb3 F15 1.868(16) . ? Sb3 F18 1.872(17) . ? Sb4 F24 1.830(17) . ? Sb4 F20 1.834(17) . ? Sb4 F21 1.838(15) . ? Sb4 F19 1.851(17) . ? Sb4 F22 1.851(16) . ? Sb4 F23 1.854(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N3 154.6(5) . . ? N2 Ag2 N5 147.8(7) . . ? N2 Ag2 O18 118.7(7) . . ? N5 Ag2 O18 92.5(7) . . ? N7 Ag3 N4 153.2(6) . . ? N6 Ag4 N8 146.5(6) . . ? C1 N1 C9 117.8(17) . . ? C1 N1 Ag1 125.2(14) . . ? C9 N1 Ag1 116.7(12) . . ? N1 C1 C2 127(2) . . ? N1 C1 H1 116.7 . . ? C2 C1 H1 116.7 . . ? C3 C2 C1 119(2) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 118.2(19) . . ? C2 C3 H3 120.9 . . ? C4 C3 H3 120.9 . . ? C3 C4 C9 119.6(18) . . ? C3 C4 C5 123.7(17) . . ? C9 C4 C5 116.5(17) . . ? C6 C5 C4 119.9(16) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 O1 126.4(16) . . ? C5 C6 C7 123.9(17) . . ? O1 C6 C7 109.8(16) . . ? C8 C7 C6 116.3(18) . . ? C8 C7 H7 121.8 . . ? C6 C7 H7 121.8 . . ? C7 C8 C9 122.8(18) . . ? C7 C8 H8 118.6 . . ? C9 C8 H8 118.6 . . ? C8 C9 N1 120.8(16) . . ? C8 C9 C4 120.2(18) . . ? N1 C9 C4 118.7(18) . . ? C6 O1 C10 115.9(15) . . ? O1 C10 C11 107.7(16) . . ? O1 C10 H10A 110.2 . . ? C11 C10 H10A 110.2 . . ? O1 C10 H10B 110.2 . . ? C11 C10 H10B 110.2 . . ? H10A C10 H10B 108.5 . . ? O2 C11 C10 104.5(16) . . ? O2 C11 H11A 110.9 . . ? C10 C11 H11A 110.9 . . ? O2 C11 H11B 110.9 . . ? C10 C11 H11B 110.9 . . ? H11A C11 H11B 108.9 . . ? C11 O2 C12 110.8(15) . . ? C13 C12 O2 105.9(19) . . ? C13 C12 H12A 110.6 . . ? O2 C12 H12A 110.6 . . ? C13 C12 H12B 110.6 . . ? O2 C12 H12B 110.6 . . ? H12A C12 H12B 108.7 . . ? C12 C13 O3 110(2) . . ? C12 C13 H13A 109.6 . . ? O3 C13 H13A 109.6 . . ? C12 C13 H13B 109.6 . . ? O3 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? C14 O3 C13 116.6(15) . . ? O3 C14 C15 113.7(15) . . ? O3 C14 H14A 108.8 . . ? C15 C14 H14A 108.8 . . ? O3 C14 H14B 108.8 . . ? C15 C14 H14B 108.8 . . ? H14A C14 H14B 107.7 . . ? O4 C15 C14 109.5(18) . . ? O4 C15 H15A 109.8 . . ? C14 C15 H15A 109.8 . . ? O4 C15 H15B 109.8 . . ? C14 C15 H15B 109.8 . . ? H15A C15 H15B 108.2 . . ? C15 O4 C16 112.3(16) . . ? C17 C16 O4 107.9(19) . . ? C17 C16 H16A 110.1 . . ? O4 C16 H16A 110.1 . . ? C17 C16 H16B 110.1 . . ? O4 C16 H16B 110.1 . . ? H16A C16 H16B 108.4 . . ? C16 C17 O5 114.9(19) . . ? C16 C17 H17A 108.5 . . ? O5 C17 H17A 108.5 . . ? C16 C17 H17B 108.5 . . ? O5 C17 H17B 108.5 . . ? H17A C17 H17B 107.5 . . ? C18 O5 C17 119.0(17) . . ? C26 C18 O5 115.0(19) . . ? C26 C18 C19 121(2) . . ? O5 C18 C19 123.6(19) . . ? C18 C19 C20 117.7(19) . . ? C18 C19 H19 121.1 . . ? C20 C19 H19 121.1 . . ? C24 C20 C19 121.7(18) . . ? C24 C20 C21 117.0(19) . . ? C19 C20 C21 121.3(18) . . ? C22 C21 C20 119(2) . . ? C22 C21 H21 120.5 . . ? C20 C21 H21 120.5 . . ? C21 C22 C23 120(2) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? N2 C23 C22 121(2) . . ? N2 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C24 N2 C23 119.1(18) . . ? C24 N2 Ag2 123.2(14) . . ? C23 N2 Ag2 116.1(15) . . ? N2 C24 C20 123.0(19) . . ? N2 C24 C25 119.6(18) . . ? C20 C24 C25 117.3(19) . . ? C26 C25 C24 119.0(18) . . ? C26 C25 H25 120.5 . . ? C24 C25 H25 120.5 . . ? C18 C26 C25 122.9(19) . . ? C18 C26 H26 118.5 . . ? C25 C26 H26 118.5 . . ? C27 N3 C35 121.1(16) . . ? C27 N3 Ag1 115.4(13) . . ? C35 N3 Ag1 123.3(12) . . ? N3 C27 C28 121.3(18) . . ? N3 C27 H27 119.4 . . ? C28 C27 H27 119.4 . . ? C29 C28 C27 120(2) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C30 118(2) . . ? C28 C29 H29 121.0 . . ? C30 C29 H29 121.0 . . ? C35 C30 C31 122(2) . . ? C35 C30 C29 117.8(18) . . ? C31 C30 C29 120.0(19) . . ? C32 C31 C30 120(2) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C31 C32 O6 126.3(18) . . ? C31 C32 C33 120.0(19) . . ? O6 C32 C33 113.7(17) . . ? C34 C33 C32 120.8(19) . . ? C34 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C33 C34 C35 119.7(19) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? N3 C35 C30 121.6(17) . . ? N3 C35 C34 121.0(18) . . ? C30 C35 C34 117.4(18) . . ? C32 O6 C36 115.1(16) . . ? O6 C36 C37 109.3(19) . . ? O6 C36 H36A 109.8 . . ? C37 C36 H36A 109.8 . . ? O6 C36 H36B 109.8 . . ? C37 C36 H36B 109.8 . . ? H36A C36 H36B 108.3 . . ? O7 C37 C36 110(2) . . ? O7 C37 H37A 109.8 . . ? C36 C37 H37A 109.8 . . ? O7 C37 H37B 109.8 . . ? C36 C37 H37B 109.8 . . ? H37A C37 H37B 108.2 . . ? C37 O7 C38 109(2) . . ? O7 C38 C39 107(2) . . ? O7 C38 H38A 110.4 . . ? C39 C38 H38A 110.4 . . ? O7 C38 H38B 110.4 . . ? C39 C38 H38B 110.4 . . ? H38A C38 H38B 108.6 . . ? O8 C39 C38 109(2) . . ? O8 C39 H39A 109.9 . . ? C38 C39 H39A 109.9 . . ? O8 C39 H39B 109.9 . . ? C38 C39 H39B 109.9 . . ? H39A C39 H39B 108.3 . . ? C39 O8 C40 101(2) . . ? C41 C40 O8 108(3) . . ? C41 C40 H40A 110.0 . . ? O8 C40 H40A 110.0 . . ? C41 C40 H40B 110.0 . . ? O8 C40 H40B 110.0 . . ? H40A C40 H40B 108.4 . . ? O9 C41 C40 117(3) . . ? O9 C41 H41A 108.0 . . ? C40 C41 H41A 108.0 . . ? O9 C41 H41B 108.0 . . ? C40 C41 H41B 108.0 . . ? H41A C41 H41B 107.2 . . ? C41 O9 C42 113.7(19) . . ? O9 C42 C43 110.9(19) . . ? O9 C42 H42A 109.5 . . ? C43 C42 H42A 109.5 . . ? O9 C42 H42B 109.5 . . ? C43 C42 H42B 109.5 . . ? H42A C42 H42B 108.1 . . ? O10 C43 C42 104.5(18) . . ? O10 C43 H43A 110.9 . . ? C42 C43 H43A 110.9 . . ? O10 C43 H43B 110.9 . . ? C42 C43 H43B 110.9 . . ? H43A C43 H43B 108.9 . . ? C44 O10 C43 114.3(16) . . ? C45 C44 O10 129.1(19) . . ? C45 C44 C52 121.8(19) . . ? O10 C44 C52 109.1(18) . . ? C44 C45 C46 122.3(17) . . ? C44 C45 H45 118.9 . . ? C46 C45 H45 118.9 . . ? C47 C46 C45 122.6(17) . . ? C47 C46 C50 120.7(18) . . ? C45 C46 C50 116.7(17) . . ? C46 C47 C48 118.5(17) . . ? C46 C47 H47 120.7 . . ? C48 C47 H47 120.7 . . ? C49 C48 C47 118.5(18) . . ? C49 C48 H48 120.7 . . ? C47 C48 H48 120.7 . . ? N4 C49 C48 121.9(18) . . ? N4 C49 H49 119.0 . . ? C48 C49 H49 119.0 . . ? C50 N4 C49 120.5(16) . . ? C50 N4 Ag3 118.4(12) . . ? C49 N4 Ag3 120.7(13) . . ? N4 C50 C51 122.4(17) . . ? N4 C50 C46 119.5(17) . . ? C51 C50 C46 118.0(18) . . ? C52 C51 C50 124(2) . . ? C52 C51 H51 117.8 . . ? C50 C51 H51 117.8 . . ? C51 C52 C44 116.8(19) . . ? C51 C52 H52 121.6 . . ? C44 C52 H52 121.6 . . ? C61 N5 C53 122(2) . . ? C61 N5 Ag2 115.9(15) . . ? C53 N5 Ag2 122.5(18) . . ? N5 C53 C54 120(2) . . ? N5 C53 H53 119.8 . . ? C54 C53 H53 119.8 . . ? C55 C54 C53 122(2) . . ? C55 C54 H54 119.1 . . ? C53 C54 H54 119.1 . . ? C54 C55 C56 118(2) . . ? C54 C55 H55 121.1 . . ? C56 C55 H55 121.1 . . ? C57 C56 C61 124.5(18) . . ? C57 C56 C55 118.0(18) . . ? C61 C56 C55 117.5(18) . . ? C56 C57 C58 117.1(17) . . ? C56 C57 H57 121.4 . . ? C58 C57 H57 121.4 . . ? O11 C58 C57 129.0(15) . . ? O11 C58 C59 112.7(16) . . ? C57 C58 C59 118.2(17) . . ? C60 C59 C58 124.8(19) . . ? C60 C59 H59 117.6 . . ? C58 C59 H59 117.6 . . ? C59 C60 C61 119.2(19) . . ? C59 C60 H60 120.4 . . ? C61 C60 H60 120.4 . . ? N5 C61 C56 120.7(19) . . ? N5 C61 C60 123.2(18) . . ? C56 C61 C60 116.1(17) . . ? C58 O11 C62 115.9(15) . . ? O11 C62 C63 104.9(17) . . ? O11 C62 H62A 110.8 . . ? C63 C62 H62A 110.8 . . ? O11 C62 H62B 110.8 . . ? C63 C62 H62B 110.8 . . ? H62A C62 H62B 108.8 . . ? O12 C63 C62 106.3(14) . . ? O12 C63 H63A 110.5 . . ? C62 C63 H63A 110.5 . . ? O12 C63 H63B 110.5 . . ? C62 C63 H63B 110.5 . . ? H63A C63 H63B 108.7 . . ? C63 O12 C64 108.6(14) . . ? O12 C64 C65 110.0(17) . . ? O12 C64 H64A 109.7 . . ? C65 C64 H64A 109.7 . . ? O12 C64 H64B 109.7 . . ? C65 C64 H64B 109.7 . . ? H64A C64 H64B 108.2 . . ? C64 C65 O13 112.2(17) . . ? C64 C65 H65A 109.2 . . ? O13 C65 H65A 109.2 . . ? C64 C65 H65B 109.2 . . ? O13 C65 H65B 109.2 . . ? H65A C65 H65B 107.9 . . ? C66 O13 C65 115.8(16) . . ? O13 C66 C67 112.8(17) . . ? O13 C66 H66A 109.0 . . ? C67 C66 H66A 109.0 . . ? O13 C66 H66B 109.0 . . ? C67 C66 H66B 109.0 . . ? H66A C66 H66B 107.8 . . ? O14 C67 C66 110.7(16) . . ? O14 C67 H67A 109.5 . . ? C66 C67 H67A 109.5 . . ? O14 C67 H67B 109.5 . . ? C66 C67 H67B 109.5 . . ? H67A C67 H67B 108.1 . . ? C68 O14 C67 114.9(15) . . ? O14 C68 C69 110.5(15) . . ? O14 C68 H68A 109.5 . . ? C69 C68 H68A 109.5 . . ? O14 C68 H68B 109.5 . . ? C69 C68 H68B 109.5 . . ? H68A C68 H68B 108.1 . . ? O15 C69 C68 109.6(16) . . ? O15 C69 H69A 109.8 . . ? C68 C69 H69A 109.8 . . ? O15 C69 H69B 109.8 . . ? C68 C69 H69B 109.8 . . ? H69A C69 H69B 108.2 . . ? C70 O15 C69 119.0(16) . . ? O15 C70 C78 114.6(17) . . ? O15 C70 C71 126(2) . . ? C78 C70 C71 120(2) . . ? C70 C71 C72 115.7(19) . . ? C70 C71 H71 122.2 . . ? C72 C71 H71 122.2 . . ? C76 C72 C73 120(2) . . ? C76 C72 C71 123(2) . . ? C73 C72 C71 116(2) . . ? C74 C73 C72 117(2) . . ? C74 C73 H73 121.5 . . ? C72 C73 H73 121.5 . . ? C73 C74 C75 120(2) . . ? C73 C74 H74 119.8 . . ? C75 C74 H74 119.8 . . ? N6 C75 C74 121(2) . . ? N6 C75 H75 119.5 . . ? C74 C75 H75 119.5 . . ? C76 N6 C75 116.4(18) . . ? C76 N6 Ag4 124.7(13) . . ? C75 N6 Ag4 117.5(14) . . ? C72 C76 N6 125(2) . . ? C72 C76 C77 118(2) . . ? N6 C76 C77 117.0(17) . . ? C78 C77 C76 120.5(19) . . ? C78 C77 H77 119.8 . . ? C76 C77 H77 119.8 . . ? C77 C78 C70 122.2(18) . . ? C77 C78 H78 118.9 . . ? C70 C78 H78 118.9 . . ? C79 N7 C87 117.4(15) . . ? C79 N7 Ag3 118.1(13) . . ? C87 N7 Ag3 124.2(12) . . ? N7 C79 C80 123.4(19) . . ? N7 C79 H79 118.3 . . ? C80 C79 H79 118.3 . . ? C81 C80 C79 118.2(19) . . ? C81 C80 H80 120.9 . . ? C79 C80 H80 120.9 . . ? C80 C81 C82 121.3(19) . . ? C80 C81 H81 119.3 . . ? C82 C81 H81 119.3 . . ? C87 C82 C81 117.5(17) . . ? C87 C82 C83 120.0(16) . . ? C81 C82 C83 122.6(17) . . ? C84 C83 C82 118.8(18) . . ? C84 C83 H83 120.6 . . ? C82 C83 H83 120.6 . . ? C83 C84 O16 123.7(19) . . ? C83 C84 C85 120.7(19) . . ? O16 C84 C85 115.5(16) . . ? C86 C85 C84 121.0(18) . . ? C86 C85 H85 119.5 . . ? C84 C85 H85 119.5 . . ? C85 C86 C87 119.1(17) . . ? C85 C86 H86 120.5 . . ? C87 C86 H86 120.5 . . ? C82 C87 N7 122.1(16) . . ? C82 C87 C86 120.5(18) . . ? N7 C87 C86 117.4(16) . . ? C84 O16 C88 118.1(16) . . ? O16 C88 C89 109.7(18) . . ? O16 C88 H88A 109.7 . . ? C89 C88 H88A 109.7 . . ? O16 C88 H88B 109.7 . . ? C89 C88 H88B 109.7 . . ? H88A C88 H88B 108.2 . . ? O17 C89 C88 111(2) . . ? O17 C89 H89A 109.4 . . ? C88 C89 H89A 109.4 . . ? O17 C89 H89B 109.4 . . ? C88 C89 H89B 109.4 . . ? H89A C89 H89B 108.0 . . ? C89 O17 C90 108.2(19) . . ? O17 C90 C91 107(2) . . ? O17 C90 H90A 110.3 . . ? C91 C90 H90A 110.3 . . ? O17 C90 H90B 110.3 . . ? C91 C90 H90B 110.3 . . ? H90A C90 H90B 108.6 . . ? O18 C91 C90 107(2) . . ? O18 C91 H91A 110.4 . . ? C90 C91 H91A 110.4 . . ? O18 C91 H91B 110.4 . . ? C90 C91 H91B 110.4 . . ? H91A C91 H91B 108.6 . . ? C91 O18 C92 98(3) . . ? C91 O18 Ag2 127.7(15) . . ? C92 O18 Ag2 117.5(15) . . ? C93 C92 O18 107(3) . . ? C93 C92 H92A 110.3 . . ? O18 C92 H92A 110.3 . . ? C93 C92 H92B 110.3 . . ? O18 C92 H92B 110.3 . . ? H92A C92 H92B 108.5 . . ? C92 C93 O19 110(2) . . ? C92 C93 H93A 109.6 . . ? O19 C93 H93A 109.6 . . ? C92 C93 H93B 109.6 . . ? O19 C93 H93B 109.6 . . ? H93A C93 H93B 108.1 . . ? C94 O19 C93 109.7(16) . . ? O19 C94 C95 109.0(16) . . ? O19 C94 H94A 109.9 . . ? C95 C94 H94A 109.9 . . ? O19 C94 H94B 109.9 . . ? C95 C94 H94B 109.9 . . ? H94A C94 H94B 108.3 . . ? O20 C95 C94 105.4(17) . . ? O20 C95 H95A 110.7 . . ? C94 C95 H95A 110.7 . . ? O20 C95 H95B 110.7 . . ? C94 C95 H95B 110.7 . . ? H95A C95 H95B 108.8 . . ? C96 O20 C95 116.3(15) . . ? C97 C96 O20 125.0(16) . . ? C97 C96 C104 120.0(17) . . ? O20 C96 C104 115.1(17) . . ? C96 C97 C98 119.2(17) . . ? C96 C97 H97 120.4 . . ? C98 C97 H97 120.4 . . ? C102 C98 C97 119.4(18) . . ? C102 C98 C99 117.6(17) . . ? C97 C98 C99 123.0(17) . . ? C100 C99 C98 118(2) . . ? C100 C99 H99 120.9 . . ? C98 C99 H99 120.9 . . ? C99 C100 C101 122(2) . . ? C99 C100 H100 118.9 . . ? C101 C100 H100 118.9 . . ? C100 C101 N8 122.6(18) . . ? C100 C101 H101 118.7 . . ? N8 C101 H101 118.7 . . ? C101 N8 C102 118.0(16) . . ? C101 N8 Ag4 123.5(13) . . ? C102 N8 Ag4 118.5(13) . . ? N8 C102 C103 118.7(17) . . ? N8 C102 C98 121.2(18) . . ? C103 C102 C98 120.1(18) . . ? C104 C103 C102 119.1(16) . . ? C104 C103 H103 120.5 . . ? C102 C103 H103 120.5 . . ? C103 C104 C96 122.2(17) . . ? C103 C104 H104 118.9 . . ? C96 C104 H104 118.9 . . ? F6 Sb1 F5 89.8(8) . . ? F6 Sb1 F4 177.6(10) . . ? F5 Sb1 F4 90.8(9) . . ? F6 Sb1 F3 90.2(7) . . ? F5 Sb1 F3 179.3(7) . . ? F4 Sb1 F3 89.2(8) . . ? F6 Sb1 F1 90.3(8) . . ? F5 Sb1 F1 88.3(6) . . ? F4 Sb1 F1 87.4(8) . . ? F3 Sb1 F1 91.1(7) . . ? F6 Sb1 F2 91.2(9) . . ? F5 Sb1 F2 91.9(7) . . ? F4 Sb1 F2 91.1(9) . . ? F3 Sb1 F2 88.7(8) . . ? F1 Sb1 F2 178.5(9) . . ? F9 Sb2 F8 93.0(10) . . ? F9 Sb2 F12 88.4(8) . . ? F8 Sb2 F12 92.6(9) . . ? F9 Sb2 F10 90.5(9) . . ? F8 Sb2 F10 89.3(10) . . ? F12 Sb2 F10 177.8(10) . . ? F9 Sb2 F11 176.4(9) . . ? F8 Sb2 F11 90.6(9) . . ? F12 Sb2 F11 91.0(7) . . ? F10 Sb2 F11 90.0(8) . . ? F9 Sb2 F7 86.6(9) . . ? F8 Sb2 F7 177.5(9) . . ? F12 Sb2 F7 89.9(8) . . ? F10 Sb2 F7 88.2(9) . . ? F11 Sb2 F7 89.8(8) . . ? F17 Sb3 F14 89.7(9) . . ? F17 Sb3 F13 90.0(7) . . ? F14 Sb3 F13 178.7(9) . . ? F17 Sb3 F16 178.0(9) . . ? F14 Sb3 F16 89.2(8) . . ? F13 Sb3 F16 91.1(7) . . ? F17 Sb3 F15 89.2(10) . . ? F14 Sb3 F15 91.4(9) . . ? F13 Sb3 F15 89.9(7) . . ? F16 Sb3 F15 89.2(7) . . ? F17 Sb3 F18 90.3(11) . . ? F14 Sb3 F18 89.7(9) . . ? F13 Sb3 F18 89.0(8) . . ? F16 Sb3 F18 91.3(9) . . ? F15 Sb3 F18 178.8(8) . . ? F24 Sb4 F20 93.2(9) . . ? F24 Sb4 F21 88.6(10) . . ? F20 Sb4 F21 89.7(7) . . ? F24 Sb4 F19 87.3(10) . . ? F20 Sb4 F19 179.3(9) . . ? F21 Sb4 F19 90.8(9) . . ? F24 Sb4 F22 177.9(10) . . ? F20 Sb4 F22 88.7(7) . . ? F21 Sb4 F22 92.2(10) . . ? F19 Sb4 F22 90.8(9) . . ? F24 Sb4 F23 88.9(9) . . ? F20 Sb4 F23 88.8(9) . . ? F21 Sb4 F23 177.1(11) . . ? F19 Sb4 F23 90.7(11) . . ? F22 Sb4 F23 90.3(10) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.68 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 2.007 _refine_diff_density_min -1.908 _refine_diff_density_rms 0.345 # Attachment 'New_CIF_4-Ag.cif' data_for _database_code_depnum_ccdc_archive 'CCDC 701606' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C84 H96 Ag3 N6 O18), 6(As F6), 2( C H Cl3), C H Cl3' _chemical_formula_sum 'C171 H195 Ag6 As6 Cl9 F36 N12 O36' _chemical_formula_weight 5094.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 '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 C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.3000(8) _cell_length_b 20.1815(5) _cell_length_c 18.7343(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.442(2) _cell_angle_gamma 90.00 _cell_volume 10957.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6298 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 19.88 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5100 _exptl_absorpt_coefficient_mu 1.630 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8039 _exptl_absorpt_correction_T_max 0.8539 _exptl_absorpt_process_details sadabs _exptl_special_details ; The large Ueq(max)/Ue(min) in the non solvent part is due to the inherent floppiness of the chain. The crystal has a low diffracting powder so the wR and R values are large and there is a Low Bond Precision on C-C Bonds ; _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 57564 _diffrn_reflns_av_R_equivalents 0.0639 _diffrn_reflns_av_sigmaI/netI 0.0632 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 27.52 _reflns_number_total 12616 _reflns_number_gt 6312 _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_number_reflns 12616 _refine_ls_number_parameters 584 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.2084 _refine_ls_R_factor_gt 0.1339 _refine_ls_wR_factor_ref 0.4315 _refine_ls_wR_factor_gt 0.3822 _refine_ls_goodness_of_fit_ref 1.453 _refine_ls_restrained_S_all 1.453 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.012 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.0000 0.02174(5) 0.7500 0.0582(4) Uani 1 2 d S . . Ag2 Ag -0.06498(4) 0.35305(4) 0.91005(5) 0.0669(4) Uani 1 1 d . . . N1 N 0.0686(3) 0.0432(4) 0.7213(4) 0.051(2) Uani 1 1 d . . . C1 C 0.1072(5) 0.0172(6) 0.7554(7) 0.065(3) Uani 1 1 d . . . H1 H 0.1053 -0.0125 0.7942 0.078 Uiso 1 1 calc R . . C2 C 0.1500(5) 0.0314(7) 0.7371(8) 0.076(4) Uani 1 1 d . . . H2 H 0.1766 0.0120 0.7645 0.092 Uiso 1 1 calc R . . C3 C 0.1554(4) 0.0706(6) 0.6832(7) 0.066(3) Uani 1 1 d . . . H3 H 0.1850 0.0772 0.6695 0.080 Uiso 1 1 calc R . . C4 C 0.1147(4) 0.1040(5) 0.6446(6) 0.053(3) Uani 1 1 d . . . C5 C 0.1168(4) 0.1477(5) 0.5876(5) 0.052(3) Uani 1 1 d . . . H5 H 0.1451 0.1561 0.5702 0.062 Uiso 1 1 calc R . . C6 C 0.0765(4) 0.1783(5) 0.5574(6) 0.052(3) Uani 1 1 d . . . C7 C 0.0355(4) 0.1624(5) 0.5786(6) 0.053(3) Uani 1 1 d . . . H7 H 0.0083 0.1834 0.5553 0.064 Uiso 1 1 calc R . . C8 C 0.0318(4) 0.1186(4) 0.6307(5) 0.049(3) Uani 1 1 d . . . H8 H 0.0023 0.1081 0.6431 0.059 Uiso 1 1 calc R . . C9 C 0.0713(3) 0.0883(5) 0.6671(5) 0.047(2) Uani 1 1 d . . . O1 O 0.0749(3) 0.2251(4) 0.5020(4) 0.0594(19) Uani 1 1 d . . . C10 C 0.1149(5) 0.2427(6) 0.4755(7) 0.072(3) Uani 1 1 d . . . H10A H 0.1260 0.2046 0.4495 0.086 Uiso 1 1 calc R . . H10B H 0.1392 0.2542 0.5162 0.086 Uiso 1 1 calc R . . C11 C 0.1064(6) 0.3003(8) 0.4257(7) 0.085(4) Uani 1 1 d . . . H11A H 0.1334 0.3084 0.4008 0.103 Uiso 1 1 calc R . . H11B H 0.0791 0.2921 0.3889 0.103 Uiso 1 1 calc R . . O2 O 0.0986(4) 0.3552(5) 0.4691(6) 0.099(3) Uani 1 1 d . . . C12 C 0.1088(6) 0.4182(8) 0.4468(9) 0.104(6) Uani 1 1 d . . . H12A H 0.0959 0.4239 0.3953 0.125 Uiso 1 1 calc R . . H12B H 0.1427 0.4236 0.4515 0.125 Uiso 1 1 calc R . . C13 C 0.0901(11) 0.468(2) 0.489(2) 0.247 Uani 1 1 d . . . H13A H 0.0997 0.5118 0.4720 0.297 Uiso 1 1 calc R . . H13B H 0.0561 0.4660 0.4774 0.297 Uiso 1 1 calc R . . O3 O 0.1008(7) 0.4663(18) 0.5574(16) 0.247 Uani 1 1 d . . . C14 C 0.0776(11) 0.511(2) 0.5883(18) 0.247 Uani 1 1 d D . . H14A H 0.0481 0.4922 0.5990 0.297 Uiso 1 1 calc R . . H14B H 0.0708 0.5500 0.5565 0.297 Uiso 1 1 calc R . . C15 C 0.1078(8) 0.530(2) 0.6557(17) 0.247 Uani 1 1 d D . . H15A H 0.1078 0.4923 0.6901 0.297 Uiso 1 1 calc R . . H15B H 0.0936 0.5680 0.6768 0.297 Uiso 1 1 calc R . . O4 O 0.1574(6) 0.5469(15) 0.6511(13) 0.247 Uani 1 1 d D . . C16 C 0.1836(9) 0.5964(17) 0.7003(19) 0.247 Uani 1 1 d D . . H16A H 0.1868 0.6392 0.6759 0.297 Uiso 1 1 calc R . . H16B H 0.1693 0.6037 0.7444 0.297 Uiso 1 1 calc R . . C17 C 0.2279(9) 0.561(2) 0.7160(18) 0.247 Uani 1 1 d D . . H17A H 0.2545 0.5920 0.7212 0.297 Uiso 1 1 calc R . . H17B H 0.2315 0.5273 0.6791 0.297 Uiso 1 1 calc R . . O5 O 0.2206(7) 0.5295(18) 0.7898(15) 0.247 Uani 1 1 d D . . C18 C 0.2160(9) 0.4641(10) 0.7727(14) 0.143(9) Uani 1 1 d . . . H18A H 0.2470 0.4447 0.7727 0.172 Uiso 1 1 calc R . . H18B H 0.1989 0.4599 0.7232 0.172 Uiso 1 1 calc R . . C19 C 0.1905(6) 0.4240(9) 0.8246(11) 0.112(6) Uani 1 1 d . . . H19A H 0.1974 0.3762 0.8210 0.135 Uiso 1 1 calc R . . H19B H 0.2004 0.4385 0.8750 0.135 Uiso 1 1 calc R . . O6 O 0.1427(4) 0.4356(5) 0.8043(5) 0.086(3) Uani 1 1 d . . . C20 C 0.1123(4) 0.4103(6) 0.8419(8) 0.068(3) Uani 1 1 d . . . C21 C 0.1233(5) 0.3686(6) 0.9027(8) 0.071(3) Uani 1 1 d . . . H21 H 0.1546 0.3566 0.9180 0.085 Uiso 1 1 calc R . . C22 C 0.0895(6) 0.3453(6) 0.9401(8) 0.081(4) Uani 1 1 d . . . C23 C 0.0963(7) 0.3049(7) 0.9969(8) 0.090(4) Uani 1 1 d . . . H23 H 0.1260 0.2858 1.0099 0.108 Uiso 1 1 calc R . . C24 C 0.0628(7) 0.2898(8) 1.0369(12) 0.111(6) Uani 1 1 d . . . H24 H 0.0700 0.2653 1.0804 0.133 Uiso 1 1 calc R . . C25 C 0.0192(6) 0.3096(7) 1.0146(8) 0.089(4) Uani 1 1 d . . . H25 H -0.0044 0.2967 1.0414 0.107 Uiso 1 1 calc R . . N2 N 0.0078(4) 0.3483(5) 0.9537(6) 0.078(3) Uani 1 1 d . . . C26 C 0.0414(5) 0.3665(6) 0.9166(6) 0.060(3) Uani 1 1 d . . . C27 C 0.0321(5) 0.4065(7) 0.8578(7) 0.071(3) Uani 1 1 d . . . H27 H 0.0012 0.4199 0.8418 0.086 Uiso 1 1 calc R . . C28 C 0.0662(5) 0.4276(6) 0.8218(8) 0.078(4) Uani 1 1 d . . . H28 H 0.0583 0.4554 0.7810 0.094 Uiso 1 1 calc R . . N3 N -0.1218(3) 0.3164(4) 0.8311(5) 0.054(2) Uani 1 1 d . . . C29 C -0.1646(5) 0.3224(6) 0.8449(8) 0.074(4) Uani 1 1 d . . . H29 H -0.1708 0.3502 0.8833 0.089 Uiso 1 1 calc R . . C30 C -0.2012(5) 0.2885(7) 0.8036(8) 0.075(4) Uani 1 1 d . . . H30 H -0.2314 0.2931 0.8159 0.090 Uiso 1 1 calc R . . C31 C -0.1954(4) 0.2509(6) 0.7490(7) 0.065(3) Uani 1 1 d . . . H31 H -0.2209 0.2300 0.7205 0.078 Uiso 1 1 calc R . . C32 C -0.1505(4) 0.2422(5) 0.7336(6) 0.055(3) Uani 1 1 d . . . C33 C -0.1390(3) 0.1996(5) 0.6748(5) 0.047(2) Uani 1 1 d . . . H33 H -0.1627 0.1774 0.6438 0.057 Uiso 1 1 calc R . . C34 C -0.0951(3) 0.1925(4) 0.6658(5) 0.042(2) Uani 1 1 d . . . C35 C -0.0596(4) 0.2276(5) 0.7069(5) 0.047(2) Uani 1 1 d . . . H35 H -0.0289 0.2232 0.6967 0.056 Uiso 1 1 calc R . . C36 C -0.0682(4) 0.2685(5) 0.7622(6) 0.049(2) Uani 1 1 d . . . H36 H -0.0437 0.2918 0.7903 0.059 Uiso 1 1 calc R . . C37 C -0.1144(4) 0.2757(5) 0.7767(5) 0.046(2) Uani 1 1 d . . . O7 O -0.0801(2) 0.1522(3) 0.6137(4) 0.0529(17) Uani 1 1 d . . . C38 C -0.1126(4) 0.1104(5) 0.5718(7) 0.062(3) Uani 1 1 d . . . H38A H -0.1329 0.1367 0.5354 0.074 Uiso 1 1 calc R . . H38B H -0.1320 0.0873 0.6029 0.074 Uiso 1 1 calc R . . C39 C -0.0851(5) 0.0614(6) 0.5354(6) 0.065(3) Uani 1 1 d . . . H39A H -0.1050 0.0396 0.4949 0.078 Uiso 1 1 calc R . . H39B H -0.0595 0.0840 0.5162 0.078 Uiso 1 1 calc R . . O8 O -0.0673(3) 0.0137(4) 0.5882(4) 0.064(2) Uani 1 1 d . . . C40 C -0.0403(6) -0.0349(7) 0.5620(7) 0.088(5) Uani 1 1 d . . . H40A H -0.0088 -0.0172 0.5620 0.106 Uiso 1 1 calc R . . H40B H -0.0533 -0.0452 0.5115 0.106 Uiso 1 1 calc R . . C41 C -0.0374(7) -0.0966(7) 0.6048(8) 0.096(5) Uani 1 1 d . . . H41A H -0.0690 -0.1135 0.6060 0.116 Uiso 1 1 calc R . . H41B H -0.0206 -0.1304 0.5806 0.116 Uiso 1 1 calc R . . O9 O -0.0151(4) -0.0882(4) 0.6762(5) 0.086(3) Uani 1 1 d . . . C42 C -0.0166(11) -0.1458(7) 0.7128(10) 0.157(11) Uani 1 1 d . . . H42A H -0.0079 -0.1827 0.6826 0.188 Uiso 1 1 calc R . . H42B H -0.0486 -0.1537 0.7217 0.188 Uiso 1 1 calc R . . As1 As 0.24268(14) 0.2455(2) 0.01695(19) 0.0769(10) Uani 0.50 1 d P . . F1 F 0.2677(9) 0.2003(14) 0.0699(19) 0.364(18) Uani 1 1 d . . . F2 F 0.1984(6) 0.2152(11) -0.0053(9) 0.220(8) Uani 1 1 d . . . F3 F 0.2412(6) 0.3014(10) 0.0496(12) 0.213 Uani 1 1 d . . . As2 As 0.2500 0.7500 0.0000 0.1161(11) Uani 1 2 d S . . F4 F 0.2857(4) 0.8134(6) -0.0150(6) 0.136(4) Uani 1 1 d . . . F5 F 0.2865(3) 0.7308(6) 0.0784(6) 0.132(4) Uani 1 1 d . . . F6 F 0.2199(3) 0.8001(6) 0.0485(6) 0.126(4) Uani 1 1 d . . . As3 As 0.0000 0.36727(14) 0.2500 0.1085(9) Uani 1 2 d S . . F7 F 0.0505(6) 0.3630(7) 0.2615(8) 0.190(8) Uani 1 1 d . . . F8 F -0.0026(6) 0.4207(8) 0.3150(10) 0.216(8) Uani 1 1 d . . . F9 F 0.0028(6) 0.3113(9) 0.3147(7) 0.192(7) Uani 1 1 d . . . C43 C 0.1361(8) 0.1880(14) 0.1975(11) 0.089(3) Uani 0.25 1 d PD . . H43 H 0.1184 0.2293 0.2047 0.107 Uiso 0.25 1 calc PR . . Cl1 Cl 0.1801(5) 0.2018(7) 0.1458(7) 0.089(3) Uani 0.25 1 d PD . . Cl2 Cl 0.1023(6) 0.1283(7) 0.1454(7) 0.089(3) Uani 0.25 1 d PD . . Cl3 Cl 0.1670(6) 0.1592(7) 0.2765(7) 0.089(3) Uani 0.25 1 d PD . . C44 C 0.2259(6) 0.9661(13) 0.9830(13) 0.1163(17) Uani 0.50 1 d PD . . H44 H 0.2360 0.9283 1.0161 0.140 Uiso 0.50 1 calc PR . . Cl4 Cl 0.2713(3) 0.9854(5) 0.9375(6) 0.1163(17) Uani 0.50 1 d PD . . Cl5 Cl 0.1742(3) 0.9428(5) 0.9303(6) 0.1163(17) Uani 0.50 1 d PD . . Cl6 Cl 0.2101(3) 1.0302(5) 1.0356(6) 0.1163(17) Uani 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0697(8) 0.0458(6) 0.0680(8) 0.000 0.0401(6) 0.000 Ag2 0.0831(8) 0.0593(6) 0.0596(6) -0.0129(4) 0.0143(5) 0.0008(4) N1 0.065(6) 0.044(4) 0.048(5) 0.000(4) 0.023(4) 0.004(4) C1 0.071(8) 0.062(7) 0.065(7) 0.013(5) 0.022(6) 0.012(6) C2 0.072(9) 0.080(8) 0.079(9) 0.007(7) 0.019(7) 0.019(7) C3 0.059(7) 0.072(7) 0.073(8) 0.005(6) 0.027(6) 0.004(6) C4 0.054(7) 0.041(5) 0.066(7) -0.007(5) 0.019(5) -0.007(4) C5 0.058(7) 0.059(6) 0.043(5) -0.011(5) 0.022(5) -0.021(5) C6 0.066(7) 0.041(5) 0.053(6) -0.006(4) 0.023(5) -0.008(5) C7 0.068(7) 0.040(5) 0.054(6) -0.010(4) 0.019(5) 0.005(5) C8 0.063(7) 0.033(4) 0.059(6) -0.015(4) 0.035(5) -0.004(4) C9 0.046(6) 0.045(5) 0.055(6) -0.013(4) 0.028(5) -0.001(4) O1 0.065(5) 0.061(4) 0.054(4) 0.008(3) 0.017(4) -0.005(4) C10 0.084(9) 0.071(7) 0.067(8) 0.003(6) 0.032(7) -0.024(7) C11 0.092(11) 0.114(11) 0.054(7) 0.015(8) 0.026(7) -0.018(9) O2 0.150(10) 0.073(6) 0.087(7) 0.025(5) 0.067(7) -0.003(6) C12 0.109(13) 0.112(12) 0.093(11) 0.062(10) 0.018(10) -0.013(10) C13 0.108 0.406 0.223 0.000 0.005 0.000 O3 0.108 0.406 0.223 0.000 0.005 0.000 C14 0.108 0.406 0.223 0.000 0.005 0.000 C15 0.108 0.406 0.223 0.000 0.005 0.000 O4 0.108 0.406 0.223 0.000 0.005 0.000 C16 0.108 0.406 0.223 0.000 0.005 0.000 C17 0.108 0.406 0.223 0.000 0.005 0.000 O5 0.108 0.406 0.223 0.000 0.005 0.000 C18 0.15(2) 0.100(13) 0.19(2) -0.036(14) 0.060(17) -0.036(13) C19 0.092(13) 0.102(12) 0.140(16) -0.024(11) 0.007(11) -0.032(10) O6 0.085(7) 0.101(7) 0.071(6) -0.005(5) 0.010(5) 0.001(5) C20 0.055(8) 0.072(8) 0.079(9) -0.009(7) 0.012(7) -0.007(6) C21 0.064(8) 0.060(7) 0.090(10) -0.012(6) 0.015(7) 0.002(6) C22 0.112(12) 0.055(7) 0.072(9) -0.015(6) 0.000(8) -0.005(7) C23 0.107(13) 0.080(9) 0.082(10) 0.012(8) 0.014(9) 0.029(9) C24 0.112(15) 0.082(10) 0.127(15) 0.024(10) -0.024(12) 0.008(10) C25 0.111(13) 0.077(9) 0.073(9) 0.005(7) -0.005(9) -0.007(8) N2 0.096(9) 0.076(7) 0.063(7) -0.027(6) 0.012(6) -0.015(6) C26 0.076(8) 0.056(6) 0.046(6) -0.011(5) 0.007(6) 0.004(5) C27 0.063(8) 0.094(9) 0.057(7) -0.026(7) 0.007(6) -0.014(7) C28 0.099(11) 0.066(7) 0.068(8) -0.008(6) 0.006(8) -0.001(7) N3 0.057(6) 0.049(5) 0.058(5) 0.004(4) 0.018(4) 0.020(4) C29 0.075(9) 0.072(8) 0.081(9) -0.005(7) 0.031(7) 0.023(7) C30 0.051(7) 0.096(9) 0.084(9) 0.016(8) 0.027(7) 0.015(7) C31 0.038(6) 0.073(7) 0.086(9) -0.006(6) 0.018(6) 0.006(5) C32 0.039(6) 0.050(6) 0.075(7) 0.005(5) 0.007(5) 0.005(4) C33 0.044(6) 0.056(6) 0.040(5) -0.011(4) 0.001(4) -0.004(4) C34 0.046(6) 0.037(4) 0.045(5) 0.002(4) 0.007(4) 0.000(4) C35 0.044(6) 0.048(5) 0.050(6) -0.004(4) 0.011(4) 0.010(4) C36 0.041(6) 0.050(5) 0.054(6) -0.003(4) -0.001(4) 0.005(4) C37 0.059(6) 0.043(5) 0.038(5) 0.007(4) 0.013(5) 0.008(4) O7 0.049(4) 0.059(4) 0.051(4) -0.014(3) 0.006(3) -0.003(3) C38 0.062(7) 0.054(6) 0.064(7) -0.014(5) -0.004(6) 0.011(5) C39 0.078(8) 0.072(7) 0.044(6) -0.015(5) 0.007(6) 0.006(6) O8 0.085(6) 0.055(4) 0.057(5) -0.014(4) 0.024(4) -0.001(4) C40 0.137(14) 0.071(8) 0.056(8) -0.015(6) 0.015(8) 0.013(8) C41 0.143(15) 0.063(8) 0.081(10) -0.007(7) 0.009(10) 0.001(8) O9 0.127(8) 0.053(5) 0.072(6) -0.013(4) -0.004(6) 0.006(5) C42 0.31(3) 0.053(8) 0.090(12) -0.004(8) -0.028(16) -0.033(13) As1 0.061(3) 0.090(2) 0.073(3) 0.003(2) -0.0121(17) 0.0007(18) F1 0.22(2) 0.31(3) 0.50(4) 0.12(3) -0.15(3) 0.08(2) F2 0.152(13) 0.27(2) 0.198(15) -0.016(14) -0.098(11) 0.017(13) F3 0.138 0.224 0.268 0.000 0.000 0.000 As2 0.0812(16) 0.156(2) 0.122(2) 0.0627(18) 0.0532(15) 0.0516(16) F4 0.113(8) 0.169(10) 0.143(9) 0.055(8) 0.077(7) 0.042(7) F5 0.092(7) 0.171(10) 0.143(9) 0.056(8) 0.049(6) 0.057(7) F6 0.088(7) 0.157(9) 0.146(9) 0.042(7) 0.060(6) 0.045(6) As3 0.133(3) 0.0950(17) 0.0886(18) 0.000 -0.0130(17) 0.000 F7 0.242(17) 0.174(12) 0.182(13) 0.090(10) 0.119(13) 0.132(12) F8 0.225(17) 0.174(13) 0.227(16) -0.107(12) -0.044(14) -0.001(12) F9 0.231(17) 0.257(18) 0.089(8) 0.016(9) 0.026(9) -0.092(14) C43 0.109(6) 0.097(5) 0.047(4) 0.021(4) -0.035(4) -0.044(5) Cl1 0.109(6) 0.097(5) 0.047(4) 0.021(4) -0.035(4) -0.044(5) Cl2 0.109(6) 0.097(5) 0.047(4) 0.021(4) -0.035(4) -0.044(5) Cl3 0.109(6) 0.097(5) 0.047(4) 0.021(4) -0.035(4) -0.044(5) C44 0.084(3) 0.111(4) 0.152(5) 0.023(3) 0.014(3) 0.000(3) Cl4 0.084(3) 0.111(4) 0.152(5) 0.023(3) 0.014(3) 0.000(3) Cl5 0.084(3) 0.111(4) 0.152(5) 0.023(3) 0.014(3) 0.000(3) Cl6 0.084(3) 0.111(4) 0.152(5) 0.023(3) 0.014(3) 0.000(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. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.198(9) . ? Ag1 N1 2.198(9) 2_556 ? Ag2 N2 2.171(13) . ? Ag2 N3 2.187(10) . ? Ag2 O2 2.599(9) 2_556 ? N1 C1 1.323(15) . ? N1 C9 1.375(13) . ? C1 C2 1.378(19) . ? C1 H1 0.9500 . ? C2 C3 1.310(17) . ? C2 H2 0.9500 . ? C3 C4 1.465(17) . ? C3 H3 0.9500 . ? C4 C5 1.393(15) . ? C4 C9 1.434(14) . ? C5 C6 1.379(16) . ? C5 H5 0.9500 . ? C6 C7 1.360(15) . ? C6 O1 1.399(12) . ? C7 C8 1.333(14) . ? C7 H7 0.9500 . ? C8 C9 1.395(15) . ? C8 H8 0.9500 . ? O1 C10 1.386(14) . ? C10 C11 1.489(19) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 O2 1.412(18) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? O2 C12 1.385(16) . ? O2 Ag2 2.599(9) 2_556 ? C12 C13 1.43(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 O3 1.28(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? O3 C14 1.31(4) . ? C14 C15 1.48(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 O4 1.510(18) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? O4 C16 1.49(4) . ? C16 C17 1.47(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 O5 1.57(4) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? O5 C18 1.36(4) . ? C18 C19 1.54(3) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 O6 1.41(2) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? O6 C20 1.317(16) . ? C20 C28 1.39(2) . ? C20 C21 1.415(19) . ? C21 C22 1.38(2) . ? C21 H21 0.9500 . ? C22 C23 1.33(2) . ? C22 C26 1.47(2) . ? C23 C24 1.35(3) . ? C23 H23 0.9500 . ? C24 C25 1.34(2) . ? C24 H24 0.9500 . ? C25 N2 1.382(18) . ? C25 H25 0.9500 . ? N2 C26 1.338(17) . ? C26 C27 1.362(18) . ? C27 C28 1.351(19) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? N3 C29 1.324(15) . ? N3 C37 1.350(12) . ? C29 C30 1.40(2) . ? C29 H29 0.9500 . ? C30 C31 1.305(18) . ? C30 H30 0.9500 . ? C31 C32 1.400(15) . ? C31 H31 0.9500 . ? C32 C37 1.405(15) . ? C32 C33 1.474(15) . ? C33 C34 1.331(14) . ? C33 H33 0.9500 . ? C34 O7 1.390(11) . ? C34 C35 1.393(14) . ? C35 C36 1.377(13) . ? C35 H35 0.9500 . ? C36 C37 1.427(14) . ? C36 H36 0.9500 . ? O7 C38 1.419(13) . ? C38 C39 1.501(15) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 O8 1.421(14) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? O8 C40 1.395(16) . ? C40 C41 1.48(2) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 O9 1.409(17) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? O9 C42 1.353(18) . ? C42 C42 1.58(4) 2_556 ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? As1 As1 0.837(5) 7 ? As1 F3 1.29(2) . ? As1 F2 1.440(17) . ? As1 F1 1.46(2) . ? As1 F3 1.69(2) 7 ? As1 F2 1.94(2) 7 ? As1 F1 1.95(3) 7 ? F1 As1 1.95(3) 7 ? F2 As1 1.94(2) 7 ? F3 As1 1.69(2) 7 ? As2 F6 1.691(10) 7_565 ? As2 F6 1.691(10) . ? As2 F4 1.702(12) . ? As2 F4 1.702(12) 7_565 ? As2 F5 1.729(11) . ? As2 F5 1.729(11) 7_565 ? As3 F7 1.467(18) . ? As3 F7 1.467(18) 2 ? As3 F8 1.637(14) 2 ? As3 F8 1.637(14) . ? As3 F9 1.650(15) 2 ? As3 F9 1.650(15) . ? C43 Cl3 1.719(19) . ? C43 Cl1 1.75(2) . ? C43 Cl2 1.762(19) . ? C43 H43 1.0000 . ? C44 Cl4 1.727(18) . ? C44 Cl6 1.728(18) . ? C44 Cl5 1.747(18) . ? C44 H44 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N1 157.3(4) . 2_556 ? N2 Ag2 N3 148.0(3) . . ? N2 Ag2 O2 98.6(4) . 2_556 ? N3 Ag2 O2 104.2(4) . 2_556 ? C1 N1 C9 118.7(9) . . ? C1 N1 Ag1 123.5(7) . . ? C9 N1 Ag1 117.7(7) . . ? N1 C1 C2 123.0(11) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C3 C2 C1 122.2(13) . . ? C3 C2 H2 118.9 . . ? C1 C2 H2 118.9 . . ? C2 C3 C4 118.6(12) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C5 C4 C9 120.5(10) . . ? C5 C4 C3 123.0(10) . . ? C9 C4 C3 116.5(10) . . ? C6 C5 C4 117.8(10) . . ? C6 C5 H5 121.1 . . ? C4 C5 H5 121.1 . . ? C7 C6 C5 121.1(10) . . ? C7 C6 O1 116.1(10) . . ? C5 C6 O1 122.8(9) . . ? C8 C7 C6 122.7(11) . . ? C8 C7 H7 118.7 . . ? C6 C7 H7 118.7 . . ? C7 C8 C9 119.9(10) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? N1 C9 C8 121.2(9) . . ? N1 C9 C4 120.9(10) . . ? C8 C9 C4 117.9(9) . . ? C10 O1 C6 119.9(9) . . ? O1 C10 C11 110.5(12) . . ? O1 C10 H10A 109.5 . . ? C11 C10 H10A 109.6 . . ? O1 C10 H10B 109.6 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? O2 C11 C10 106.1(10) . . ? O2 C11 H11A 110.5 . . ? C10 C11 H11A 110.5 . . ? O2 C11 H11B 110.5 . . ? C10 C11 H11B 110.5 . . ? H11A C11 H11B 108.7 . . ? C12 O2 C11 119.1(12) . . ? C12 O2 Ag2 113.8(10) . 2_556 ? C11 O2 Ag2 127.1(7) . 2_556 ? O2 C12 C13 111(2) . . ? O2 C12 H12A 109.4 . . ? C13 C12 H12A 109.3 . . ? O2 C12 H12B 109.3 . . ? C13 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? O3 C13 C12 118(4) . . ? O3 C13 H13A 107.7 . . ? C12 C13 H13A 107.7 . . ? O3 C13 H13B 107.8 . . ? C12 C13 H13B 107.8 . . ? H13A C13 H13B 107.1 . . ? C13 O3 C14 111(3) . . ? O3 C14 C15 105(3) . . ? O3 C14 H14A 110.7 . . ? C15 C14 H14A 110.7 . . ? O3 C14 H14B 110.6 . . ? C15 C14 H14B 110.6 . . ? H14A C14 H14B 108.7 . . ? C14 C15 O4 118(3) . . ? C14 C15 H15A 107.8 . . ? O4 C15 H15A 107.7 . . ? C14 C15 H15B 107.8 . . ? O4 C15 H15B 107.9 . . ? H15A C15 H15B 107.2 . . ? C16 O4 C15 122(3) . . ? C17 C16 O4 99(2) . . ? C17 C16 H16A 112.0 . . ? O4 C16 H16A 112.0 . . ? C17 C16 H16B 111.9 . . ? O4 C16 H16B 111.9 . . ? H16A C16 H16B 109.6 . . ? C16 C17 O5 98(3) . . ? C16 C17 H17A 112.1 . . ? O5 C17 H17A 112.1 . . ? C16 C17 H17B 112.1 . . ? O5 C17 H17B 112.2 . . ? H17A C17 H17B 109.8 . . ? C18 O5 C17 102(3) . . ? O5 C18 C19 114(2) . . ? O5 C18 H18A 108.8 . . ? C19 C18 H18A 108.9 . . ? O5 C18 H18B 108.8 . . ? C19 C18 H18B 108.8 . . ? H18A C18 H18B 107.7 . . ? O6 C19 C18 107.2(17) . . ? O6 C19 H19A 110.3 . . ? C18 C19 H19A 110.3 . . ? O6 C19 H19B 110.3 . . ? C18 C19 H19B 110.2 . . ? H19A C19 H19B 108.5 . . ? C20 O6 C19 120.9(13) . . ? O6 C20 C28 117.7(13) . . ? O6 C20 C21 124.5(12) . . ? C28 C20 C21 117.7(13) . . ? C22 C21 C20 121.0(13) . . ? C22 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? C23 C22 C21 125.5(17) . . ? C23 C22 C26 116.1(16) . . ? C21 C22 C26 118.4(13) . . ? C22 C23 C24 123.0(17) . . ? C22 C23 H23 118.5 . . ? C24 C23 H23 118.5 . . ? C25 C24 C23 119.5(17) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C24 C25 N2 121.9(17) . . ? C24 C25 H25 119.0 . . ? N2 C25 H25 119.0 . . ? C26 N2 C25 118.4(14) . . ? C26 N2 Ag2 123.4(9) . . ? C25 N2 Ag2 116.2(11) . . ? N2 C26 C27 120.5(13) . . ? N2 C26 C22 120.6(12) . . ? C27 C26 C22 118.8(13) . . ? C28 C27 C26 121.0(14) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C20 123.0(14) . . ? C27 C28 H28 118.5 . . ? C20 C28 H28 118.5 . . ? C29 N3 C37 117.7(11) . . ? C29 N3 Ag2 119.1(8) . . ? C37 N3 Ag2 121.7(7) . . ? N3 C29 C30 121.1(12) . . ? N3 C29 H29 119.4 . . ? C30 C29 H29 119.5 . . ? C31 C30 C29 122.6(12) . . ? C31 C30 H30 118.7 . . ? C29 C30 H30 118.7 . . ? C30 C31 C32 118.0(12) . . ? C30 C31 H31 121.0 . . ? C32 C31 H31 121.0 . . ? C31 C32 C37 118.1(11) . . ? C31 C32 C33 123.4(10) . . ? C37 C32 C33 118.4(9) . . ? C34 C33 C32 119.2(9) . . ? C34 C33 H33 120.4 . . ? C32 C33 H33 120.4 . . ? C33 C34 O7 124.3(9) . . ? C33 C34 C35 122.3(9) . . ? O7 C34 C35 113.5(8) . . ? C36 C35 C34 121.0(9) . . ? C36 C35 H35 119.5 . . ? C34 C35 H35 119.5 . . ? C35 C36 C37 119.3(9) . . ? C35 C36 H36 120.4 . . ? C37 C36 H36 120.4 . . ? N3 C37 C32 122.5(10) . . ? N3 C37 C36 117.8(10) . . ? C32 C37 C36 119.7(9) . . ? C34 O7 C38 118.8(8) . . ? O7 C38 C39 106.4(9) . . ? O7 C38 H38A 110.4 . . ? C39 C38 H38A 110.4 . . ? O7 C38 H38B 110.4 . . ? C39 C38 H38B 110.4 . . ? H38A C38 H38B 108.6 . . ? O8 C39 C38 107.2(9) . . ? O8 C39 H39A 110.3 . . ? C38 C39 H39A 110.3 . . ? O8 C39 H39B 110.2 . . ? C38 C39 H39B 110.3 . . ? H39A C39 H39B 108.5 . . ? C40 O8 C39 113.6(9) . . ? O8 C40 C41 113.1(13) . . ? O8 C40 H40A 108.9 . . ? C41 C40 H40A 108.9 . . ? O8 C40 H40B 109.0 . . ? C41 C40 H40B 109.0 . . ? H40A C40 H40B 107.8 . . ? O9 C41 C40 113.3(12) . . ? O9 C41 H41A 108.9 . . ? C40 C41 H41A 108.9 . . ? O9 C41 H41B 108.9 . . ? C40 C41 H41B 108.9 . . ? H41A C41 H41B 107.7 . . ? C42 O9 C41 109.4(11) . . ? O9 C42 C42 112.7(16) . 2_556 ? O9 C42 H42A 109.1 . . ? C42 C42 H42A 109.2 2_556 . ? O9 C42 H42B 109.0 . . ? C42 C42 H42B 108.9 2_556 . ? H42A C42 H42B 107.8 . . ? F3 As1 F2 114.7(11) . . ? F3 As1 F1 105.8(17) . . ? F2 As1 F1 105.9(14) . . ? F3 As1 F3 151.1(6) . 7 ? F2 As1 F3 83.5(10) . 7 ? F1 As1 F3 89.2(16) . 7 ? F3 As1 F2 77.7(10) . 7 ? F2 As1 F2 156.9(5) . 7 ? F1 As1 F2 88.0(13) . 7 ? F3 As1 F2 78.2(8) 7 7 ? F3 As1 F1 83.8(14) . 7 ? F2 As1 F1 88.4(11) . 7 ? F1 As1 F1 156.7(6) . 7 ? F3 As1 F1 73.9(12) 7 7 ? F2 As1 F1 73.1(9) 7 7 ? F6 As2 F6 180.0(5) 7_565 . ? F6 As2 F4 88.8(5) 7_565 . ? F6 As2 F4 91.2(5) . . ? F6 As2 F4 91.2(5) 7_565 7_565 ? F6 As2 F4 88.8(5) . 7_565 ? F4 As2 F4 179.994(2) . 7_565 ? F6 As2 F5 90.9(5) 7_565 . ? F6 As2 F5 89.1(5) . . ? F4 As2 F5 89.4(6) . . ? F4 As2 F5 90.6(6) 7_565 . ? F6 As2 F5 89.1(5) 7_565 7_565 ? F6 As2 F5 90.9(5) . 7_565 ? F4 As2 F5 90.6(6) . 7_565 ? F4 As2 F5 89.4(6) 7_565 7_565 ? F5 As2 F5 180.0(6) . 7_565 ? F7 As3 F7 173.2(12) . 2 ? F7 As3 F8 89.5(8) . 2 ? F7 As3 F8 95.0(9) 2 2 ? F7 As3 F8 95.0(9) . . ? F7 As3 F8 89.5(8) 2 . ? F8 As3 F8 97.5(15) 2 . ? F7 As3 F9 90.5(9) . 2 ? F7 As3 F9 84.9(8) 2 2 ? F8 As3 F9 84.7(10) 2 2 ? F8 As3 F9 174.2(10) . 2 ? F7 As3 F9 84.9(8) . . ? F7 As3 F9 90.5(9) 2 . ? F8 As3 F9 174.2(10) 2 . ? F8 As3 F9 84.7(10) . . ? F9 As3 F9 93.6(12) 2 . ? Cl3 C43 Cl1 101.1(14) . . ? Cl3 C43 Cl2 115.3(16) . . ? Cl1 C43 Cl2 101.6(14) . . ? Cl3 C43 H43 112.6 . . ? Cl1 C43 H43 112.6 . . ? Cl2 C43 H43 112.6 . . ? Cl4 C44 Cl6 113.7(14) . . ? Cl4 C44 Cl5 116.7(14) . . ? Cl6 C44 Cl5 103.9(12) . . ? Cl4 C44 H44 107.4 . . ? Cl6 C44 H44 107.4 . . ? Cl5 C44 H44 107.4 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.873 _refine_diff_density_min -1.991 _refine_diff_density_rms 0.313