# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Darrin Richeson' _publ_contact_author_email darrin@science.uottawa.ca _publ_section_title ; The Interplay of Metal and Supporting Ligand in Labile Coordination to Pincer Complexes of Ag(I). ; _publ_author_name D.Richeson # Attachment '- combined structures.cif' data_dr024a _database_code_depnum_ccdc_archive 'CCDC 849370' #TrackingRef '- combined structures.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H60 Ag F3 N4 O3 S' _chemical_formula_weight 997.98 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1402(4) _cell_length_b 15.4794(5) _cell_length_c 15.6244(6) _cell_angle_alpha 98.249(3) _cell_angle_beta 110.516(2) _cell_angle_gamma 91.383(2) _cell_volume 2489.27(15) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 8406 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 24.75 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas n/a _exptl_crystal_density_diffrn 1.331 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 0.504 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9193 _exptl_absorpt_correction_T_max 0.9900 _exptl_absorpt_process_details 'SADABS, Bruker (2003)' _exptl_special_details ; Data collection is performed with four batch runs at phi = 0.00 deg (600 frames), at phi = 90.00 deg (600 frames), at phi = 180.00 deg (600 frames), and at phi = 270.00 deg (600 frames). A fifth batch run is collected at phi = 0.00 deg (50 frames) to monitor crystal and diffractometer stability. Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 40097 _diffrn_reflns_av_R_equivalents 0.0689 _diffrn_reflns_av_sigmaI/netI 0.0653 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 24.81 _reflns_number_total 8451 _reflns_number_gt 5745 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, Bruker (2009)' _computing_cell_refinement 'APEX II, Bruker (2009)' _computing_data_reduction 'XPREP, Bruker (2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL, Bruker (2004)' _computing_publication_material 'SHELXTL, Bruker (2004)' _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^)+(0.0448P)^2^]' _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 8451 _refine_ls_number_parameters 586 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0824 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.0942 _refine_ls_wR_factor_gt 0.0822 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.79308(3) 0.752642(17) 0.514279(19) 0.03931(11) Uani 1 1 d . . . N1 N 0.7697(3) 0.78423(16) 0.34796(17) 0.0316(6) Uani 1 1 d . . . N2 N 0.8257(2) 0.89651(16) 0.51206(18) 0.0285(6) Uani 1 1 d . . . N3 N 0.9343(2) 0.83216(17) 0.67299(17) 0.0306(6) Uani 1 1 d . . . C1 C 0.7417(3) 0.8638(2) 0.3446(2) 0.0307(8) Uani 1 1 d . . . C2 C 0.7974(3) 0.9283(2) 0.4322(2) 0.0294(8) Uani 1 1 d . . . C3 C 0.8200(3) 1.0165(2) 0.4307(2) 0.0365(8) Uani 1 1 d . . . H3A H 0.7987 1.0376 0.3734 0.044 Uiso 1 1 calc R . . C4 C 0.8737(3) 1.0729(2) 0.5131(2) 0.0388(9) Uani 1 1 d . . . H4A H 0.8900 1.1335 0.5135 0.047 Uiso 1 1 calc R . . C5 C 0.9033(3) 1.0406(2) 0.5946(2) 0.0358(8) Uani 1 1 d . . . H5A H 0.9408 1.0787 0.6521 0.043 Uiso 1 1 calc R . . C6 C 0.8783(3) 0.95181(19) 0.5925(2) 0.0277(7) Uani 1 1 d . . . C7 C 0.9134(3) 0.9128(2) 0.6793(2) 0.0298(8) Uani 1 1 d . . . C8 C 0.6600(3) 0.8995(2) 0.2608(2) 0.0325(8) Uani 1 1 d . . . C9 C 0.6751(4) 0.8779(2) 0.1759(2) 0.0454(10) Uani 1 1 d . . . H9A H 0.7406 0.8415 0.1708 0.054 Uiso 1 1 calc R . . C10 C 0.5953(4) 0.9090(3) 0.0989(3) 0.0606(12) Uani 1 1 d . . . H10A H 0.6056 0.8938 0.0409 0.073 Uiso 1 1 calc R . . C11 C 0.5008(4) 0.9621(3) 0.1062(3) 0.0610(12) Uani 1 1 d . . . H11A H 0.4449 0.9826 0.0530 0.073 Uiso 1 1 calc R . . C12 C 0.4871(4) 0.9856(2) 0.1906(3) 0.0499(10) Uani 1 1 d . . . H12A H 0.4231 1.0233 0.1958 0.060 Uiso 1 1 calc R . . C13 C 0.5657(3) 0.9546(2) 0.2669(2) 0.0390(9) Uani 1 1 d . . . H13A H 0.5558 0.9710 0.3248 0.047 Uiso 1 1 calc R . . C14 C 0.9258(3) 0.9745(2) 0.7661(2) 0.0346(8) Uani 1 1 d . . . C15 C 1.0387(4) 0.9841(3) 0.8417(3) 0.0513(10) Uani 1 1 d . . . H15A H 1.1069 0.9490 0.8403 0.062 Uiso 1 1 calc R . . C16 C 1.0531(5) 1.0444(3) 0.9195(3) 0.0715(13) Uani 1 1 d . . . H16A H 1.1320 1.0513 0.9707 0.086 Uiso 1 1 calc R . . C17 C 0.9552(5) 1.0942(3) 0.9237(3) 0.0719(14) Uani 1 1 d . . . H17A H 0.9656 1.1355 0.9775 0.086 Uiso 1 1 calc R . . C18 C 0.8421(5) 1.0842(3) 0.8497(3) 0.0704(13) Uani 1 1 d . . . H18A H 0.7727 1.1176 0.8524 0.085 Uiso 1 1 calc R . . C19 C 0.8282(4) 1.0248(2) 0.7700(3) 0.0521(10) Uani 1 1 d . . . H19A H 0.7502 1.0194 0.7181 0.063 Uiso 1 1 calc R . . C20 C 0.7092(3) 0.7152(2) 0.2729(2) 0.0316(8) Uani 1 1 d . . . C21 C 0.7803(3) 0.6519(2) 0.2422(2) 0.0344(8) Uani 1 1 d . . . C22 C 0.7082(4) 0.5850(2) 0.1728(2) 0.0420(9) Uani 1 1 d . . . H22A H 0.7522 0.5407 0.1503 0.050 Uiso 1 1 calc R . . C23 C 0.5759(4) 0.5795(2) 0.1347(2) 0.0452(9) Uani 1 1 d . . . H23A H 0.5321 0.5323 0.0868 0.054 Uiso 1 1 calc R . . C24 C 0.5056(3) 0.6412(2) 0.1650(2) 0.0357(8) Uani 1 1 d . . . C25 C 0.5764(3) 0.7070(2) 0.2361(2) 0.0335(8) Uani 1 1 d . . . H25A H 0.5312 0.7488 0.2610 0.040 Uiso 1 1 calc R . . C26 C 0.9281(3) 0.6561(2) 0.2802(2) 0.0403(9) Uani 1 1 d . . . C27 C 0.9789(4) 0.5803(3) 0.2313(3) 0.0612(12) Uani 1 1 d . . . H27A H 0.9466 0.5813 0.1645 0.092 Uiso 1 1 calc R . . H27B H 0.9495 0.5246 0.2431 0.092 Uiso 1 1 calc R . . H27C H 1.0731 0.5868 0.2552 0.092 Uiso 1 1 calc R . . C28 C 0.9829(4) 0.7408(2) 0.2623(3) 0.0559(11) Uani 1 1 d . . . H28A H 0.9493 0.7430 0.1957 0.084 Uiso 1 1 calc R . . H28B H 1.0769 0.7420 0.2842 0.084 Uiso 1 1 calc R . . H28C H 0.9576 0.7914 0.2955 0.084 Uiso 1 1 calc R . . C29 C 0.9804(4) 0.6516(3) 0.3839(3) 0.0644(12) Uani 1 1 d . . . H29A H 0.9504 0.6998 0.4172 0.097 Uiso 1 1 calc R . . H29B H 1.0746 0.6566 0.4067 0.097 Uiso 1 1 calc R . . H29C H 0.9497 0.5956 0.3943 0.097 Uiso 1 1 calc R . . C30 C 0.3600(4) 0.6425(2) 0.1218(3) 0.0499(10) Uani 1 1 d . . . C31 C 0.3010(5) 0.6393(4) 0.1952(3) 0.113(2) Uani 1 1 d . . . H31A H 0.3207 0.5850 0.2211 0.170 Uiso 1 1 calc R . . H31B H 0.2076 0.6410 0.1674 0.170 Uiso 1 1 calc R . . H31C H 0.3366 0.6897 0.2447 0.170 Uiso 1 1 calc R . . C32 C 0.2982(4) 0.5660(3) 0.0432(3) 0.0606(11) Uani 1 1 d . . . H32A H 0.3135 0.5107 0.0674 0.091 Uiso 1 1 calc R . . H32B H 0.3361 0.5670 -0.0047 0.091 Uiso 1 1 calc R . . H32C H 0.2055 0.5713 0.0163 0.091 Uiso 1 1 calc R . . C33 C 0.3299(4) 0.7272(3) 0.0798(3) 0.0877(16) Uani 1 1 d . . . H33A H 0.3692 0.7287 0.0329 0.132 Uiso 1 1 calc R . . H33B H 0.3647 0.7781 0.1288 0.132 Uiso 1 1 calc R . . H33C H 0.2366 0.7288 0.0511 0.132 Uiso 1 1 calc R . . C34 C 0.9522(3) 0.7843(2) 0.7474(2) 0.0311(8) Uani 1 1 d . . . C35 C 1.0580(3) 0.7333(2) 0.7765(2) 0.0368(8) Uani 1 1 d . . . C36 C 1.0547(4) 0.6827(2) 0.8424(2) 0.0475(10) Uani 1 1 d . . . H36A H 1.1254 0.6489 0.8663 0.057 Uiso 1 1 calc R . . C37 C 0.9550(4) 0.6785(2) 0.8752(2) 0.0476(10) Uani 1 1 d . . . H37A H 0.9580 0.6413 0.9191 0.057 Uiso 1 1 calc R . . C38 C 0.8507(3) 0.7278(2) 0.8452(2) 0.0361(8) Uani 1 1 d . . . C39 C 0.8525(3) 0.7807(2) 0.7812(2) 0.0338(8) Uani 1 1 d . . . H39A H 0.7829 0.8159 0.7596 0.041 Uiso 1 1 calc R . . C40 C 1.1684(3) 0.7325(2) 0.7388(2) 0.0434(9) Uani 1 1 d . . . C41 C 1.1196(4) 0.6994(3) 0.6347(3) 0.0690(13) Uani 1 1 d . . . H41A H 1.0532 0.7360 0.6028 0.103 Uiso 1 1 calc R . . H41B H 1.0832 0.6386 0.6223 0.103 Uiso 1 1 calc R . . H41C H 1.1912 0.7022 0.6122 0.103 Uiso 1 1 calc R . . C42 C 1.2362(4) 0.8246(3) 0.7593(3) 0.0619(12) Uani 1 1 d . . . H42A H 1.1740 0.8652 0.7305 0.093 Uiso 1 1 calc R . . H42B H 1.3053 0.8234 0.7340 0.093 Uiso 1 1 calc R . . H42C H 1.2726 0.8441 0.8264 0.093 Uiso 1 1 calc R . . C43 C 1.2725(4) 0.6725(3) 0.7848(3) 0.0663(12) Uani 1 1 d . . . H43A H 1.2337 0.6125 0.7734 0.099 Uiso 1 1 calc R . . H43B H 1.3094 0.6934 0.8516 0.099 Uiso 1 1 calc R . . H43C H 1.3404 0.6735 0.7585 0.099 Uiso 1 1 calc R . . C44 C 0.7332(3) 0.7177(2) 0.8740(2) 0.0420(9) Uani 1 1 d . . . C45 C 0.7727(4) 0.7037(3) 0.9745(3) 0.0651(12) Uani 1 1 d . . . H45A H 0.8223 0.6521 0.9831 0.098 Uiso 1 1 calc R . . H45B H 0.6957 0.6946 0.9897 0.098 Uiso 1 1 calc R . . H45C H 0.8257 0.7553 1.0152 0.098 Uiso 1 1 calc R . . C46 C 0.6470(4) 0.6387(3) 0.8108(3) 0.0625(12) Uani 1 1 d . . . H46A H 0.6953 0.5864 0.8167 0.094 Uiso 1 1 calc R . . H46B H 0.6183 0.6489 0.7465 0.094 Uiso 1 1 calc R . . H46C H 0.5721 0.6300 0.8286 0.094 Uiso 1 1 calc R . . C47 C 0.6551(4) 0.7989(3) 0.8627(3) 0.0566(11) Uani 1 1 d . . . H47A H 0.6278 0.8086 0.7983 0.085 Uiso 1 1 calc R . . H47B H 0.7087 0.8503 0.9035 0.085 Uiso 1 1 calc R . . H47C H 0.5792 0.7894 0.8792 0.085 Uiso 1 1 calc R . . S1 S 0.50562(10) 0.81945(6) 0.58032(7) 0.0489(3) Uani 1 1 d . . . O1 O 0.6008(3) 0.8892(2) 0.6241(2) 0.0986(11) Uani 1 1 d . . . O2 O 0.5605(4) 0.7400(2) 0.5719(3) 0.1232(14) Uani 1 1 d . . . O3 O 0.4004(3) 0.8192(3) 0.6081(2) 0.1255(16) Uani 1 1 d . . . C48 C 0.4378(4) 0.8360(4) 0.4628(3) 0.0741(14) Uani 1 1 d . . . F1 F 0.5194(3) 0.8365(3) 0.42077(19) 0.1431(15) Uani 1 1 d . . . F2 F 0.3359(3) 0.7848(3) 0.4144(2) 0.1349(14) Uani 1 1 d . . . F3 F 0.3944(3) 0.9174(3) 0.4589(3) 0.1356(14) Uani 1 1 d . . . N4 N 0.7391(3) 0.61424(18) 0.5070(2) 0.0420(7) Uani 1 1 d . . . C49 C 0.6827(4) 0.5606(2) 0.4271(3) 0.0533(11) Uani 1 1 d . . . H49A H 0.6736 0.5816 0.3711 0.064 Uiso 1 1 calc R . . C50 C 0.6372(4) 0.4765(3) 0.4222(3) 0.0707(13) Uani 1 1 d . . . H50A H 0.5979 0.4401 0.3638 0.085 Uiso 1 1 calc R . . C51 C 0.6486(5) 0.4454(3) 0.5017(4) 0.0752(14) Uani 1 1 d . . . H51A H 0.6164 0.3875 0.4999 0.090 Uiso 1 1 calc R . . C52 C 0.7071(5) 0.4991(3) 0.5835(3) 0.0712(13) Uani 1 1 d . . . H52A H 0.7178 0.4788 0.6401 0.085 Uiso 1 1 calc R . . C53 C 0.7508(4) 0.5826(2) 0.5841(3) 0.0549(11) Uani 1 1 d . . . H53A H 0.7911 0.6195 0.6420 0.066 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0535(2) 0.02423(14) 0.03848(18) 0.00471(11) 0.01480(14) -0.00131(12) N1 0.0376(17) 0.0271(15) 0.0286(16) 0.0018(13) 0.0110(14) 0.0047(13) N2 0.0317(16) 0.0242(14) 0.0307(16) 0.0039(13) 0.0126(14) 0.0023(12) N3 0.0329(17) 0.0289(16) 0.0297(16) 0.0045(12) 0.0109(13) 0.0020(12) C1 0.036(2) 0.0295(19) 0.030(2) 0.0056(15) 0.0160(17) 0.0042(15) C2 0.0288(19) 0.0280(18) 0.030(2) 0.0020(15) 0.0097(16) 0.0011(15) C3 0.048(2) 0.0309(19) 0.034(2) 0.0100(17) 0.0169(19) 0.0054(17) C4 0.050(2) 0.0245(18) 0.041(2) 0.0032(17) 0.0175(19) -0.0010(17) C5 0.039(2) 0.0267(18) 0.041(2) -0.0018(16) 0.0161(18) -0.0027(16) C6 0.0275(19) 0.0256(17) 0.030(2) 0.0001(15) 0.0119(16) 0.0009(15) C7 0.0278(19) 0.033(2) 0.0265(19) 0.0011(15) 0.0088(16) -0.0029(15) C8 0.042(2) 0.0283(18) 0.029(2) 0.0075(15) 0.0144(17) 0.0037(16) C9 0.062(3) 0.045(2) 0.040(2) 0.0153(18) 0.027(2) 0.0164(19) C10 0.094(3) 0.067(3) 0.035(2) 0.024(2) 0.034(2) 0.021(3) C11 0.077(3) 0.069(3) 0.048(3) 0.037(2) 0.024(2) 0.026(2) C12 0.057(3) 0.047(2) 0.054(3) 0.022(2) 0.024(2) 0.015(2) C13 0.052(2) 0.034(2) 0.034(2) 0.0088(17) 0.0181(19) 0.0048(18) C14 0.041(2) 0.0310(19) 0.031(2) 0.0003(16) 0.0142(19) -0.0059(17) C15 0.056(3) 0.052(2) 0.038(2) -0.004(2) 0.012(2) -0.001(2) C16 0.084(4) 0.073(3) 0.041(3) -0.011(2) 0.011(3) -0.005(3) C17 0.102(4) 0.060(3) 0.052(3) -0.024(2) 0.040(3) -0.021(3) C18 0.075(3) 0.063(3) 0.075(3) -0.022(3) 0.041(3) 0.000(3) C19 0.054(3) 0.046(2) 0.054(3) -0.008(2) 0.022(2) 0.000(2) C20 0.038(2) 0.0281(18) 0.0252(19) 0.0019(15) 0.0084(17) 0.0033(16) C21 0.044(2) 0.0284(18) 0.032(2) 0.0041(16) 0.0154(18) 0.0077(16) C22 0.051(3) 0.033(2) 0.040(2) -0.0043(17) 0.018(2) 0.0095(18) C23 0.048(3) 0.039(2) 0.040(2) -0.0076(18) 0.010(2) 0.0007(19) C24 0.041(2) 0.0323(19) 0.032(2) 0.0031(16) 0.0119(18) 0.0031(17) C25 0.044(2) 0.0293(19) 0.028(2) 0.0010(16) 0.0151(18) 0.0067(17) C26 0.041(2) 0.036(2) 0.042(2) -0.0026(17) 0.0148(19) 0.0075(17) C27 0.048(3) 0.054(3) 0.079(3) -0.008(2) 0.027(2) 0.009(2) C28 0.052(3) 0.045(2) 0.068(3) -0.002(2) 0.023(2) -0.003(2) C29 0.054(3) 0.091(3) 0.048(3) 0.014(2) 0.016(2) 0.028(2) C30 0.044(2) 0.048(2) 0.049(3) -0.009(2) 0.012(2) 0.0004(19) C31 0.062(3) 0.194(6) 0.075(4) -0.037(4) 0.038(3) -0.030(4) C32 0.054(3) 0.053(3) 0.058(3) -0.005(2) 0.004(2) -0.006(2) C33 0.067(3) 0.050(3) 0.104(4) -0.003(3) -0.016(3) 0.018(2) C34 0.039(2) 0.0261(17) 0.0225(18) -0.0002(14) 0.0057(16) -0.0025(16) C35 0.039(2) 0.0351(19) 0.032(2) 0.0053(16) 0.0069(18) 0.0013(17) C36 0.047(2) 0.049(2) 0.046(2) 0.0202(19) 0.011(2) 0.0130(19) C37 0.055(3) 0.048(2) 0.043(2) 0.0206(19) 0.017(2) 0.005(2) C38 0.039(2) 0.035(2) 0.029(2) 0.0027(16) 0.0070(17) -0.0031(17) C39 0.037(2) 0.0290(18) 0.031(2) 0.0035(15) 0.0080(17) -0.0003(15) C40 0.044(2) 0.045(2) 0.045(2) 0.0130(18) 0.017(2) 0.0131(18) C41 0.062(3) 0.097(4) 0.047(3) -0.001(2) 0.021(2) 0.026(3) C42 0.055(3) 0.063(3) 0.076(3) 0.015(2) 0.032(2) 0.006(2) C43 0.054(3) 0.074(3) 0.080(3) 0.027(3) 0.027(3) 0.024(2) C44 0.044(2) 0.048(2) 0.035(2) 0.0088(18) 0.0153(19) -0.0012(18) C45 0.071(3) 0.086(3) 0.046(3) 0.024(2) 0.025(2) -0.004(2) C46 0.054(3) 0.059(3) 0.070(3) 0.003(2) 0.022(2) -0.013(2) C47 0.061(3) 0.068(3) 0.051(3) 0.010(2) 0.032(2) 0.007(2) S1 0.0533(7) 0.0465(6) 0.0493(6) 0.0069(5) 0.0217(6) 0.0020(5) O1 0.092(3) 0.097(3) 0.075(2) 0.001(2) -0.002(2) -0.037(2) O2 0.137(3) 0.062(2) 0.148(4) 0.015(2) 0.022(3) 0.041(2) O3 0.083(3) 0.242(5) 0.087(3) 0.063(3) 0.059(2) 0.028(3) C48 0.044(3) 0.122(5) 0.063(3) 0.019(3) 0.025(3) 0.008(3) F1 0.089(2) 0.296(5) 0.069(2) 0.052(3) 0.0484(19) 0.033(3) F2 0.093(2) 0.200(4) 0.070(2) -0.020(2) -0.0041(19) -0.036(3) F3 0.110(3) 0.165(3) 0.149(3) 0.101(3) 0.036(2) 0.044(3) N4 0.052(2) 0.0320(16) 0.0413(19) 0.0030(15) 0.0168(17) -0.0003(15) C49 0.067(3) 0.045(2) 0.044(3) 0.000(2) 0.018(2) -0.009(2) C50 0.081(3) 0.049(3) 0.073(3) -0.015(2) 0.027(3) -0.018(2) C51 0.074(3) 0.035(2) 0.121(5) 0.009(3) 0.042(3) -0.008(2) C52 0.093(4) 0.051(3) 0.080(4) 0.034(3) 0.035(3) 0.007(3) C53 0.075(3) 0.041(2) 0.047(3) 0.010(2) 0.019(2) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N4 2.187(3) . ? Ag1 N2 2.255(2) . ? Ag1 N3 2.537(3) . ? Ag1 N1 2.638(2) . ? N1 C1 1.281(4) . ? N1 C20 1.423(4) . ? N2 C2 1.344(4) . ? N2 C6 1.344(4) . ? N3 C7 1.272(4) . ? N3 C34 1.426(4) . ? C1 C2 1.496(4) . ? C1 C8 1.500(4) . ? C2 C3 1.387(4) . ? C3 C4 1.375(4) . ? C4 C5 1.370(4) . ? C5 C6 1.389(4) . ? C6 C7 1.494(4) . ? C7 C14 1.503(4) . ? C8 C9 1.390(4) . ? C8 C13 1.388(4) . ? C9 C10 1.381(5) . ? C10 C11 1.376(5) . ? C11 C12 1.379(5) . ? C12 C13 1.368(5) . ? C14 C19 1.367(5) . ? C14 C15 1.378(5) . ? C15 C16 1.380(5) . ? C16 C17 1.366(6) . ? C17 C18 1.367(6) . ? C18 C19 1.395(5) . ? C20 C25 1.382(4) . ? C20 C21 1.410(4) . ? C21 C22 1.386(5) . ? C21 C26 1.537(5) . ? C22 C23 1.377(5) . ? C23 C24 1.385(5) . ? C24 C25 1.384(4) . ? C24 C30 1.525(5) . ? C26 C29 1.531(5) . ? C26 C28 1.534(5) . ? C26 C27 1.536(5) . ? C30 C31 1.515(5) . ? C30 C32 1.528(5) . ? C30 C33 1.542(5) . ? C34 C39 1.390(4) . ? C34 C35 1.411(4) . ? C35 C36 1.389(4) . ? C35 C40 1.539(5) . ? C36 C37 1.381(5) . ? C37 C38 1.383(5) . ? C38 C39 1.386(4) . ? C38 C44 1.538(5) . ? C40 C41 1.528(5) . ? C40 C42 1.534(5) . ? C40 C43 1.543(5) . ? C44 C46 1.525(5) . ? C44 C45 1.524(5) . ? C44 C47 1.541(5) . ? S1 O3 1.385(3) . ? S1 O2 1.397(3) . ? S1 O1 1.408(3) . ? S1 C48 1.784(5) . ? C48 F1 1.295(4) . ? C48 F2 1.294(5) . ? C48 F3 1.362(6) . ? N4 C53 1.331(4) . ? N4 C49 1.331(4) . ? C49 C50 1.367(5) . ? C50 C51 1.362(6) . ? C51 C52 1.354(6) . ? C52 C53 1.367(5) . ? 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 N4 Ag1 N2 173.64(11) . . ? N4 Ag1 N3 115.61(10) . . ? N2 Ag1 N3 69.01(9) . . ? N4 Ag1 N1 109.76(10) . . ? N2 Ag1 N1 67.72(8) . . ? N3 Ag1 N1 130.19(8) . . ? C1 N1 C20 122.3(3) . . ? C1 N1 Ag1 107.26(19) . . ? C20 N1 Ag1 116.35(18) . . ? C2 N2 C6 118.9(3) . . ? C2 N2 Ag1 121.7(2) . . ? C6 N2 Ag1 119.38(19) . . ? C7 N3 C34 122.6(3) . . ? C7 N3 Ag1 109.2(2) . . ? C34 N3 Ag1 115.35(18) . . ? N1 C1 C2 117.4(3) . . ? N1 C1 C8 126.4(3) . . ? C2 C1 C8 116.2(3) . . ? N2 C2 C3 121.8(3) . . ? N2 C2 C1 116.8(3) . . ? C3 C2 C1 121.4(3) . . ? C4 C3 C2 119.2(3) . . ? C3 C4 C5 119.1(3) . . ? C4 C5 C6 119.5(3) . . ? N2 C6 C5 121.5(3) . . ? N2 C6 C7 116.9(3) . . ? C5 C6 C7 121.6(3) . . ? N3 C7 C6 117.0(3) . . ? N3 C7 C14 126.8(3) . . ? C6 C7 C14 116.1(3) . . ? C9 C8 C13 118.8(3) . . ? C9 C8 C1 121.4(3) . . ? C13 C8 C1 119.9(3) . . ? C10 C9 C8 120.2(3) . . ? C11 C10 C9 120.0(3) . . ? C10 C11 C12 120.2(4) . . ? C13 C12 C11 119.9(4) . . ? C12 C13 C8 120.9(3) . . ? C19 C14 C15 118.9(3) . . ? C19 C14 C7 120.8(3) . . ? C15 C14 C7 120.2(3) . . ? C14 C15 C16 120.4(4) . . ? C17 C16 C15 120.7(4) . . ? C16 C17 C18 119.3(4) . . ? C17 C18 C19 120.1(4) . . ? C14 C19 C18 120.5(4) . . ? C25 C20 C21 120.4(3) . . ? C25 C20 N1 117.6(3) . . ? C21 C20 N1 121.7(3) . . ? C22 C21 C20 115.5(3) . . ? C22 C21 C26 121.1(3) . . ? C20 C21 C26 123.4(3) . . ? C23 C22 C21 123.4(3) . . ? C22 C23 C24 121.3(3) . . ? C25 C24 C23 115.9(3) . . ? C25 C24 C30 120.0(3) . . ? C23 C24 C30 124.1(3) . . ? C24 C25 C20 123.5(3) . . ? C29 C26 C28 110.0(3) . . ? C29 C26 C27 107.5(3) . . ? C28 C26 C27 106.4(3) . . ? C29 C26 C21 111.2(3) . . ? C28 C26 C21 109.8(3) . . ? C27 C26 C21 111.8(3) . . ? C31 C30 C24 109.7(3) . . ? C31 C30 C32 108.6(3) . . ? C24 C30 C32 112.9(3) . . ? C31 C30 C33 110.4(4) . . ? C24 C30 C33 108.4(3) . . ? C32 C30 C33 106.9(3) . . ? C39 C34 C35 121.4(3) . . ? C39 C34 N3 116.9(3) . . ? C35 C34 N3 121.2(3) . . ? C36 C35 C34 114.5(3) . . ? C36 C35 C40 122.1(3) . . ? C34 C35 C40 123.4(3) . . ? C37 C36 C35 124.0(3) . . ? C36 C37 C38 121.1(3) . . ? C37 C38 C39 116.4(3) . . ? C37 C38 C44 121.8(3) . . ? C39 C38 C44 121.6(3) . . ? C34 C39 C38 122.6(3) . . ? C41 C40 C42 109.6(3) . . ? C41 C40 C43 106.9(3) . . ? C42 C40 C43 106.4(3) . . ? C41 C40 C35 111.3(3) . . ? C42 C40 C35 110.4(3) . . ? C43 C40 C35 112.1(3) . . ? C46 C44 C45 109.5(3) . . ? C46 C44 C38 107.7(3) . . ? C45 C44 C38 111.5(3) . . ? C46 C44 C47 108.3(3) . . ? C45 C44 C47 108.2(3) . . ? C38 C44 C47 111.6(3) . . ? O3 S1 O2 116.8(3) . . ? O3 S1 O1 116.4(3) . . ? O2 S1 O1 111.2(3) . . ? O3 S1 C48 103.1(2) . . ? O2 S1 C48 102.1(3) . . ? O1 S1 C48 104.8(2) . . ? F1 C48 F2 111.7(5) . . ? F1 C48 F3 102.8(4) . . ? F2 C48 F3 103.2(4) . . ? F1 C48 S1 114.4(3) . . ? F2 C48 S1 113.6(4) . . ? F3 C48 S1 110.1(4) . . ? C53 N4 C49 117.0(3) . . ? C53 N4 Ag1 120.0(2) . . ? C49 N4 Ag1 122.6(2) . . ? N4 C49 C50 122.8(4) . . ? C51 C50 C49 119.4(4) . . ? C52 C51 C50 118.4(4) . . ? C51 C52 C53 119.6(4) . . ? N4 C53 C52 122.8(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Ag1 N1 C1 150.0(2) . . . . ? N2 Ag1 N1 C1 -23.8(2) . . . . ? N3 Ag1 N1 C1 -55.3(2) . . . . ? N4 Ag1 N1 C20 8.9(2) . . . . ? N2 Ag1 N1 C20 -164.9(2) . . . . ? N3 Ag1 N1 C20 163.7(2) . . . . ? N4 Ag1 N2 C2 -56.5(10) . . . . ? N3 Ag1 N2 C2 166.1(2) . . . . ? N1 Ag1 N2 C2 11.4(2) . . . . ? N4 Ag1 N2 C6 125.5(9) . . . . ? N3 Ag1 N2 C6 -11.9(2) . . . . ? N1 Ag1 N2 C6 -166.6(2) . . . . ? N4 Ag1 N3 C7 -151.5(2) . . . . ? N2 Ag1 N3 C7 23.7(2) . . . . ? N1 Ag1 N3 C7 54.9(2) . . . . ? N4 Ag1 N3 C34 -8.7(2) . . . . ? N2 Ag1 N3 C34 166.5(2) . . . . ? N1 Ag1 N3 C34 -162.33(19) . . . . ? C20 N1 C1 C2 171.4(3) . . . . ? Ag1 N1 C1 C2 33.2(3) . . . . ? C20 N1 C1 C8 -9.8(5) . . . . ? Ag1 N1 C1 C8 -148.1(3) . . . . ? C6 N2 C2 C3 -0.5(4) . . . . ? Ag1 N2 C2 C3 -178.6(2) . . . . ? C6 N2 C2 C1 178.7(3) . . . . ? Ag1 N2 C2 C1 0.7(4) . . . . ? N1 C1 C2 N2 -26.6(4) . . . . ? C8 C1 C2 N2 154.5(3) . . . . ? N1 C1 C2 C3 152.7(3) . . . . ? C8 C1 C2 C3 -26.2(4) . . . . ? N2 C2 C3 C4 0.5(5) . . . . ? C1 C2 C3 C4 -178.8(3) . . . . ? C2 C3 C4 C5 -0.1(5) . . . . ? C3 C4 C5 C6 -0.2(5) . . . . ? C2 N2 C6 C5 0.2(4) . . . . ? Ag1 N2 C6 C5 178.3(2) . . . . ? C2 N2 C6 C7 -177.4(3) . . . . ? Ag1 N2 C6 C7 0.7(3) . . . . ? C4 C5 C6 N2 0.2(5) . . . . ? C4 C5 C6 C7 177.7(3) . . . . ? C34 N3 C7 C6 -171.7(3) . . . . ? Ag1 N3 C7 C6 -32.2(3) . . . . ? C34 N3 C7 C14 11.3(5) . . . . ? Ag1 N3 C7 C14 150.8(3) . . . . ? N2 C6 C7 N3 24.1(4) . . . . ? C5 C6 C7 N3 -153.5(3) . . . . ? N2 C6 C7 C14 -158.5(3) . . . . ? C5 C6 C7 C14 23.8(4) . . . . ? N1 C1 C8 C9 -45.0(5) . . . . ? C2 C1 C8 C9 133.8(3) . . . . ? N1 C1 C8 C13 134.2(3) . . . . ? C2 C1 C8 C13 -47.1(4) . . . . ? C13 C8 C9 C10 -1.7(5) . . . . ? C1 C8 C9 C10 177.5(3) . . . . ? C8 C9 C10 C11 0.4(6) . . . . ? C9 C10 C11 C12 1.2(6) . . . . ? C10 C11 C12 C13 -1.4(6) . . . . ? C11 C12 C13 C8 0.1(5) . . . . ? C9 C8 C13 C12 1.4(5) . . . . ? C1 C8 C13 C12 -177.7(3) . . . . ? N3 C7 C14 C19 -129.3(4) . . . . ? C6 C7 C14 C19 53.6(4) . . . . ? N3 C7 C14 C15 53.7(5) . . . . ? C6 C7 C14 C15 -123.4(3) . . . . ? C19 C14 C15 C16 -0.9(5) . . . . ? C7 C14 C15 C16 176.2(3) . . . . ? C14 C15 C16 C17 1.4(6) . . . . ? C15 C16 C17 C18 -0.2(7) . . . . ? C16 C17 C18 C19 -1.4(7) . . . . ? C15 C14 C19 C18 -0.7(5) . . . . ? C7 C14 C19 C18 -177.8(3) . . . . ? C17 C18 C19 C14 1.9(6) . . . . ? C1 N1 C20 C25 -51.3(4) . . . . ? Ag1 N1 C20 C25 83.5(3) . . . . ? C1 N1 C20 C21 134.7(3) . . . . ? Ag1 N1 C20 C21 -90.5(3) . . . . ? C25 C20 C21 C22 1.9(4) . . . . ? N1 C20 C21 C22 175.7(3) . . . . ? C25 C20 C21 C26 -179.6(3) . . . . ? N1 C20 C21 C26 -5.8(4) . . . . ? C20 C21 C22 C23 0.3(5) . . . . ? C26 C21 C22 C23 -178.2(3) . . . . ? C21 C22 C23 C24 -0.7(5) . . . . ? C22 C23 C24 C25 -1.1(5) . . . . ? C22 C23 C24 C30 175.8(3) . . . . ? C23 C24 C25 C20 3.4(5) . . . . ? C30 C24 C25 C20 -173.7(3) . . . . ? C21 C20 C25 C24 -3.9(5) . . . . ? N1 C20 C25 C24 -178.0(3) . . . . ? C22 C21 C26 C29 -119.6(4) . . . . ? C20 C21 C26 C29 62.0(4) . . . . ? C22 C21 C26 C28 118.4(3) . . . . ? C20 C21 C26 C28 -60.0(4) . . . . ? C22 C21 C26 C27 0.6(4) . . . . ? C20 C21 C26 C27 -177.8(3) . . . . ? C25 C24 C30 C31 -59.9(5) . . . . ? C23 C24 C30 C31 123.3(4) . . . . ? C25 C24 C30 C32 178.9(3) . . . . ? C23 C24 C30 C32 2.1(5) . . . . ? C25 C24 C30 C33 60.6(4) . . . . ? C23 C24 C30 C33 -116.2(4) . . . . ? C7 N3 C34 C39 58.5(4) . . . . ? Ag1 N3 C34 C39 -78.8(3) . . . . ? C7 N3 C34 C35 -129.9(3) . . . . ? Ag1 N3 C34 C35 92.9(3) . . . . ? C39 C34 C35 C36 -1.8(5) . . . . ? N3 C34 C35 C36 -173.1(3) . . . . ? C39 C34 C35 C40 177.9(3) . . . . ? N3 C34 C35 C40 6.6(5) . . . . ? C34 C35 C36 C37 2.5(5) . . . . ? C40 C35 C36 C37 -177.2(3) . . . . ? C35 C36 C37 C38 -1.7(6) . . . . ? C36 C37 C38 C39 0.0(5) . . . . ? C36 C37 C38 C44 174.3(3) . . . . ? C35 C34 C39 C38 0.2(5) . . . . ? N3 C34 C39 C38 171.9(3) . . . . ? C37 C38 C39 C34 0.7(5) . . . . ? C44 C38 C39 C34 -173.6(3) . . . . ? C36 C35 C40 C41 118.0(4) . . . . ? C34 C35 C40 C41 -61.7(4) . . . . ? C36 C35 C40 C42 -120.1(4) . . . . ? C34 C35 C40 C42 60.3(4) . . . . ? C36 C35 C40 C43 -1.7(5) . . . . ? C34 C35 C40 C43 178.6(3) . . . . ? C37 C38 C44 C46 -81.8(4) . . . . ? C39 C38 C44 C46 92.2(4) . . . . ? C37 C38 C44 C45 38.3(5) . . . . ? C39 C38 C44 C45 -147.6(3) . . . . ? C37 C38 C44 C47 159.4(3) . . . . ? C39 C38 C44 C47 -26.6(5) . . . . ? O3 S1 C48 F1 -178.4(4) . . . . ? O2 S1 C48 F1 -56.8(5) . . . . ? O1 S1 C48 F1 59.3(5) . . . . ? O3 S1 C48 F2 -48.6(5) . . . . ? O2 S1 C48 F2 73.0(4) . . . . ? O1 S1 C48 F2 -170.9(4) . . . . ? O3 S1 C48 F3 66.5(4) . . . . ? O2 S1 C48 F3 -171.9(3) . . . . ? O1 S1 C48 F3 -55.8(4) . . . . ? N2 Ag1 N4 C53 -118.3(9) . . . . ? N3 Ag1 N4 C53 17.3(3) . . . . ? N1 Ag1 N4 C53 176.1(3) . . . . ? N2 Ag1 N4 C49 55.1(10) . . . . ? N3 Ag1 N4 C49 -169.4(3) . . . . ? N1 Ag1 N4 C49 -10.5(3) . . . . ? C53 N4 C49 C50 0.3(6) . . . . ? Ag1 N4 C49 C50 -173.2(3) . . . . ? N4 C49 C50 C51 0.4(7) . . . . ? C49 C50 C51 C52 -1.1(7) . . . . ? C50 C51 C52 C53 1.1(7) . . . . ? C49 N4 C53 C52 -0.3(6) . . . . ? Ag1 N4 C53 C52 173.4(3) . . . . ? C51 C52 C53 N4 -0.4(7) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 24.81 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.638 _refine_diff_density_min -0.599 _refine_diff_density_rms 0.061 data_dr025 _database_code_depnum_ccdc_archive 'CCDC 849371' #TrackingRef '- combined structures.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50.40 H54.10 Ag F3 N4 O3 S' _chemical_formula_weight 960.81 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' 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.3389(16) _cell_length_b 18.947(2) _cell_length_c 18.189(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.286(5) _cell_angle_gamma 90.00 _cell_volume 4890.0(10) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9233 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 28.28 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas n/a _exptl_crystal_density_diffrn 1.305 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1994 _exptl_absorpt_coefficient_mu 0.510 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8746 _exptl_absorpt_correction_T_max 0.9138 _exptl_absorpt_process_details 'SADABS, Bruker (2003)' _exptl_special_details ; Data collection is performed with three batch runs at phi = 0.00 deg (650 frames), at phi = 120.00 deg (650 frames), and at phi = 240.00 deg (650 frames). Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 99977 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_sigmaI/netI 0.0118 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 28.31 _reflns_number_total 12077 _reflns_number_gt 10422 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, Bruker (2009)' _computing_cell_refinement 'APEX II, Bruker (2009)' _computing_data_reduction 'XPREP, Bruker (2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL, Bruker (2004)' _computing_publication_material 'SHELXTL, Bruker (2004)' _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^)+(0.0553P)^2^+4.6942P] 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 12077 _refine_ls_number_parameters 586 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0483 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.1183 _refine_ls_wR_factor_gt 0.1109 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.342410(13) 0.331581(10) 0.836606(9) 0.03955(7) Uani 1 1 d . . . N1 N 0.50405(12) 0.33149(9) 0.91704(10) 0.0298(3) Uani 1 1 d . . . N2 N 0.33086(12) 0.30428(9) 0.95808(9) 0.0269(3) Uani 1 1 d . . . N3 N 0.17469(13) 0.34827(10) 0.86633(10) 0.0347(4) Uani 1 1 d . . . N4 N 0.3537(2) 0.37139(14) 0.72389(13) 0.0613(7) Uani 1 1 d . . . C1 C 0.50184(14) 0.29894(11) 0.97784(11) 0.0282(4) Uani 1 1 d . . . C2 C 0.40921(14) 0.29591(10) 1.00702(10) 0.0275(4) Uani 1 1 d . . . C3 C 0.40676(15) 0.29028(13) 1.08319(12) 0.0359(5) Uani 1 1 d . . . H3A H 0.4632 0.2830 1.1167 0.043 Uiso 1 1 calc R . . C4 C 0.32109(16) 0.29544(14) 1.10938(12) 0.0393(5) Uani 1 1 d . . . H4A H 0.3179 0.2935 1.1611 0.047 Uiso 1 1 calc R . . C5 C 0.24032(16) 0.30351(13) 1.05866(12) 0.0366(5) Uani 1 1 d . . . H5A H 0.1805 0.3067 1.0750 0.044 Uiso 1 1 calc R . . C6 C 0.24769(14) 0.30694(11) 0.98313(11) 0.0293(4) Uani 1 1 d . . . C7 C 0.16151(15) 0.31891(12) 0.92690(12) 0.0324(4) Uani 1 1 d . . . C8 C 0.58384(14) 0.26640(12) 1.02598(11) 0.0318(4) Uani 1 1 d . . . C9 C 0.65833(16) 0.30708(14) 1.05932(13) 0.0388(5) Uani 1 1 d . . . H9A H 0.6599 0.3563 1.0495 0.047 Uiso 1 1 calc R . . C10 C 0.73112(17) 0.27551(17) 1.10735(15) 0.0497(6) Uani 1 1 d . . . H10A H 0.7817 0.3035 1.1310 0.060 Uiso 1 1 calc R . . C11 C 0.72991(18) 0.20476(18) 1.12043(15) 0.0530(7) Uani 1 1 d . . . H11A H 0.7797 0.1835 1.1531 0.064 Uiso 1 1 calc R . . C12 C 0.6570(2) 0.16427(16) 1.0865(2) 0.0619(8) Uani 1 1 d . . . H12A H 0.6572 0.1148 1.0950 0.074 Uiso 1 1 calc R . . C13 C 0.5826(2) 0.19486(15) 1.03976(17) 0.0539(7) Uani 1 1 d . . . H13A H 0.5313 0.1667 1.0175 0.065 Uiso 1 1 calc R . . C14 C 0.06942(16) 0.29590(17) 0.94963(13) 0.0461(6) Uani 1 1 d . . . C15 C 0.0616(2) 0.22774(19) 0.97529(16) 0.0579(7) Uani 1 1 d . . . H15A H 0.1144 0.1969 0.9793 0.069 Uiso 1 1 calc R . . C16 C -0.0235(3) 0.2041(3) 0.9954(2) 0.0882(14) Uani 1 1 d . . . H16A H -0.0283 0.1572 1.0130 0.106 Uiso 1 1 calc R . . C17 C -0.0985(3) 0.2473(4) 0.9900(2) 0.0990(18) Uani 1 1 d . . . H17A H -0.1563 0.2302 1.0030 0.119 Uiso 1 1 calc R . . C18 C -0.0931(2) 0.3150(4) 0.9661(2) 0.0934(17) Uani 1 1 d . . . H18A H -0.1463 0.3451 0.9644 0.112 Uiso 1 1 calc R . . C19 C -0.0076(2) 0.3414(2) 0.94357(17) 0.0664(10) Uani 1 1 d . . . H19A H -0.0038 0.3881 0.9252 0.080 Uiso 1 1 calc R . . C20 C 0.59010(15) 0.34213(12) 0.88644(11) 0.0311(4) Uani 1 1 d . . . C21 C 0.63004(16) 0.28784(13) 0.84838(12) 0.0361(4) Uani 1 1 d . . . C22 C 0.70729(19) 0.30559(17) 0.81312(15) 0.0494(6) Uani 1 1 d . . . H22A H 0.7358 0.2699 0.7872 0.059 Uiso 1 1 calc R . . C23 C 0.7431(2) 0.37216(18) 0.81452(17) 0.0569(7) Uani 1 1 d . . . H23A H 0.7952 0.3823 0.7895 0.068 Uiso 1 1 calc R . . C24 C 0.7032(2) 0.42534(16) 0.85267(15) 0.0504(6) Uani 1 1 d . . . H24A H 0.7287 0.4717 0.8537 0.060 Uiso 1 1 calc R . . C25 C 0.62594(17) 0.41132(13) 0.88952(12) 0.0377(5) Uani 1 1 d . . . C26 C 0.59020(18) 0.21387(14) 0.84187(14) 0.0433(5) Uani 1 1 d . . . H26A H 0.5412 0.2101 0.8756 0.052 Uiso 1 1 calc R . . C27 C 0.6651(3) 0.15808(18) 0.8653(2) 0.0719(10) Uani 1 1 d . . . H27A H 0.6946 0.1672 0.9165 0.108 Uiso 1 1 calc R . . H27B H 0.7132 0.1599 0.8322 0.108 Uiso 1 1 calc R . . H27C H 0.6358 0.1112 0.8624 0.108 Uiso 1 1 calc R . . C28 C 0.5418(2) 0.2013(2) 0.76194(16) 0.0634(8) Uani 1 1 d . . . H28A H 0.4939 0.2377 0.7484 0.095 Uiso 1 1 calc R . . H28B H 0.5117 0.1547 0.7586 0.095 Uiso 1 1 calc R . . H28C H 0.5888 0.2033 0.7279 0.095 Uiso 1 1 calc R . . C29 C 0.58203(19) 0.46946(13) 0.93027(14) 0.0445(5) Uani 1 1 d . . . H29A H 0.5443 0.4461 0.9655 0.053 Uiso 1 1 calc R . . C30 C 0.6549(3) 0.51562(17) 0.9763(2) 0.0679(9) Uani 1 1 d . . . H30A H 0.6229 0.5524 1.0012 0.102 Uiso 1 1 calc R . . H30B H 0.6954 0.5377 0.9437 0.102 Uiso 1 1 calc R . . H30C H 0.6935 0.4866 1.0136 0.102 Uiso 1 1 calc R . . C31 C 0.5139(3) 0.5136(2) 0.8769(2) 0.0692(9) Uani 1 1 d . . . H31A H 0.4678 0.4825 0.8479 0.104 Uiso 1 1 calc R . . H31B H 0.5490 0.5396 0.8433 0.104 Uiso 1 1 calc R . . H31C H 0.4809 0.5470 0.9053 0.104 Uiso 1 1 calc R . . C32 C 0.10037(17) 0.36789(14) 0.80895(13) 0.0429(5) Uani 1 1 d . . . C33 C 0.04735(16) 0.31822(15) 0.76385(12) 0.0404(5) Uani 1 1 d . . . C34 C -0.0175(2) 0.34349(19) 0.70531(16) 0.0577(7) Uani 1 1 d . . . H34A H -0.0533 0.3108 0.6731 0.069 Uiso 1 1 calc R . . C35 C -0.0311(3) 0.4148(2) 0.6930(2) 0.0836(12) Uani 1 1 d . . . H35A H -0.0771 0.4308 0.6537 0.100 Uiso 1 1 calc R . . C36 C 0.0216(3) 0.4623(2) 0.7374(2) 0.0983(16) Uani 1 1 d . . . H36A H 0.0114 0.5114 0.7290 0.118 Uiso 1 1 calc R . . C37 C 0.0906(3) 0.44005(18) 0.7954(2) 0.0759(11) Uani 1 1 d . . . C38 C 0.05838(17) 0.23979(14) 0.77424(13) 0.0433(5) Uani 1 1 d . . . H38A H 0.1062 0.2312 0.8190 0.052 Uiso 1 1 calc R . . C39 C 0.0946(2) 0.2063(2) 0.70712(17) 0.0624(8) Uani 1 1 d . . . H39A H 0.1540 0.2288 0.6995 0.094 Uiso 1 1 calc R . . H39B H 0.0479 0.2129 0.6627 0.094 Uiso 1 1 calc R . . H39C H 0.1051 0.1557 0.7162 0.094 Uiso 1 1 calc R . . C40 C -0.0347(2) 0.2049(2) 0.78758(19) 0.0655(9) Uani 1 1 d . . . H40A H -0.0564 0.2262 0.8312 0.098 Uiso 1 1 calc R . . H40B H -0.0245 0.1542 0.7962 0.098 Uiso 1 1 calc R . . H40C H -0.0824 0.2119 0.7439 0.098 Uiso 1 1 calc R . . C41 C 0.1527(4) 0.49396(19) 0.8419(3) 0.115(2) Uani 1 1 d . . . H41A H 0.1951 0.4676 0.8810 0.138 Uiso 1 1 calc R . . C42 C 0.2158(4) 0.5344(3) 0.7938(4) 0.132(3) Uani 1 1 d . . . H42A H 0.2536 0.5006 0.7698 0.198 Uiso 1 1 calc R . . H42B H 0.2578 0.5664 0.8254 0.198 Uiso 1 1 calc R . . H42C H 0.1760 0.5617 0.7557 0.198 Uiso 1 1 calc R . . C43 C 0.0960(6) 0.5449(3) 0.8801(3) 0.142(3) Uani 1 1 d . . . H43A H 0.0564 0.5188 0.9103 0.214 Uiso 1 1 calc R . . H43B H 0.0561 0.5731 0.8429 0.214 Uiso 1 1 calc R . . H43C H 0.1386 0.5762 0.9122 0.214 Uiso 1 1 calc R . . C44 C 0.4344(4) 0.3971(3) 0.7068(2) 0.0852(12) Uani 1 1 d . . . H44A H 0.4887 0.3965 0.7436 0.102 Uiso 1 1 calc R . . C45 C 0.4417(4) 0.4247(3) 0.6374(3) 0.1121(18) Uani 1 1 d . . . H45A H 0.4987 0.4458 0.6274 0.135 Uiso 1 1 calc R . . C46 C 0.3656(5) 0.4208(3) 0.5840(2) 0.1126(18) Uani 1 1 d . . . H46A H 0.3699 0.4364 0.5349 0.135 Uiso 1 1 calc R . . C47 C 0.2813(5) 0.3939(3) 0.6011(3) 0.1100(18) Uani 1 1 d . . . H47A H 0.2267 0.3915 0.5648 0.132 Uiso 1 1 calc R . . C48 C 0.2797(4) 0.3704(2) 0.6738(2) 0.0857(12) Uani 1 1 d . . . H48A H 0.2222 0.3530 0.6870 0.103 Uiso 1 1 calc R . . S1 S 0.31451(5) 0.14556(4) 0.86765(4) 0.04587(14) Uani 1 1 d . . . O1 O 0.31545(16) 0.19479(11) 0.80802(12) 0.0579(5) Uani 1 1 d . . . O2 O 0.40118(17) 0.13835(15) 0.91524(14) 0.0735(6) Uani 1 1 d . . . O3 O 0.23285(19) 0.14918(13) 0.90419(16) 0.0746(7) Uani 1 1 d . . . C49 C 0.3008(3) 0.06104(18) 0.8193(3) 0.0784(11) Uani 1 1 d . . . F1 F 0.3743(2) 0.04885(16) 0.7840(2) 0.1296(12) Uani 1 1 d . . . F2 F 0.2963(3) 0.00877(12) 0.8661(2) 0.1267(11) Uani 1 1 d . . . F3 F 0.2242(2) 0.05748(14) 0.7713(2) 0.1306(12) Uani 1 1 d . . . C50 C 1.1215(17) 0.9610(10) 0.0656(14) 0.145(8) Uani 0.35 1 d PD A -1 H50A H 1.1579 1.0020 0.0862 0.217 Uiso 0.35 1 calc PR A -1 H50B H 1.1610 0.9315 0.0382 0.217 Uiso 0.35 1 calc PR A -1 H50C H 1.1014 0.9334 0.1061 0.217 Uiso 0.35 1 calc PR A -1 C51 C 1.036(2) 0.9855(14) 0.014(2) 0.132(16) Uani 0.35 1 d PD A -1 C52 C 0.962(2) 0.995(3) -0.005(4) 0.19(2) Uani 0.35 1 d PD A -1 C53 C 0.870(2) 1.0139(15) -0.0135(15) 0.188(15) Uani 0.35 1 d PD A -1 H53A H 0.8615 1.0587 -0.0405 0.282 Uiso 0.35 1 calc PR A -1 H53B H 0.8499 1.0194 0.0356 0.282 Uiso 0.35 1 calc PR A -1 H53C H 0.8315 0.9773 -0.0415 0.282 Uiso 0.35 1 calc PR A -1 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 0.04225(11) 0.04969(11) 0.02588(9) 0.00308(6) 0.00207(6) 0.00259(7) N1 0.0279(8) 0.0361(9) 0.0247(8) 0.0014(6) 0.0019(6) 0.0012(7) N2 0.0282(8) 0.0272(8) 0.0245(7) -0.0009(6) 0.0007(6) 0.0000(6) N3 0.0323(9) 0.0376(9) 0.0313(9) -0.0027(7) -0.0056(7) 0.0029(7) N4 0.088(2) 0.0569(15) 0.0380(12) 0.0035(10) 0.0071(12) 0.0101(14) C1 0.0284(9) 0.0299(9) 0.0252(8) -0.0002(7) 0.0002(7) 0.0012(7) C2 0.0279(9) 0.0296(9) 0.0240(8) 0.0022(7) 0.0004(7) -0.0009(7) C3 0.0320(10) 0.0477(12) 0.0263(9) 0.0074(9) -0.0012(8) 0.0001(9) C4 0.0378(11) 0.0565(14) 0.0235(9) 0.0051(9) 0.0037(8) -0.0043(10) C5 0.0307(10) 0.0503(13) 0.0292(10) -0.0007(9) 0.0062(8) -0.0031(9) C6 0.0286(9) 0.0332(10) 0.0254(9) -0.0020(7) 0.0008(7) -0.0010(8) C7 0.0274(10) 0.0404(11) 0.0278(9) -0.0075(8) -0.0012(7) 0.0026(8) C8 0.0289(10) 0.0398(11) 0.0259(9) 0.0052(8) 0.0017(7) 0.0048(8) C9 0.0292(10) 0.0492(13) 0.0364(11) 0.0048(10) -0.0012(8) -0.0001(9) C10 0.0272(11) 0.0753(19) 0.0441(13) 0.0112(12) -0.0036(9) 0.0023(11) C11 0.0334(12) 0.082(2) 0.0434(13) 0.0230(13) 0.0038(10) 0.0189(13) C12 0.0626(19) 0.0522(16) 0.0668(19) 0.0245(14) -0.0046(15) 0.0152(14) C13 0.0522(15) 0.0431(13) 0.0603(17) 0.0130(12) -0.0127(13) -0.0005(12) C14 0.0299(11) 0.0782(19) 0.0301(10) -0.0124(11) 0.0037(8) 0.0010(11) C15 0.0475(15) 0.083(2) 0.0456(14) -0.0047(14) 0.0137(12) -0.0218(14) C16 0.069(2) 0.143(4) 0.0582(19) -0.019(2) 0.0279(18) -0.051(3) C17 0.050(2) 0.188(6) 0.064(2) -0.030(3) 0.0234(17) -0.032(3) C18 0.0356(16) 0.188(5) 0.056(2) -0.039(3) 0.0046(14) 0.021(2) C19 0.0364(14) 0.118(3) 0.0433(15) -0.0221(16) 0.0002(11) 0.0194(15) C20 0.0292(10) 0.0420(11) 0.0217(8) 0.0043(8) 0.0021(7) 0.0014(8) C21 0.0347(11) 0.0462(12) 0.0265(9) -0.0002(8) 0.0010(8) 0.0038(9) C22 0.0472(14) 0.0643(16) 0.0393(13) -0.0050(12) 0.0145(11) 0.0057(12) C23 0.0500(15) 0.075(2) 0.0512(15) 0.0035(14) 0.0248(12) -0.0058(14) C24 0.0521(15) 0.0535(15) 0.0482(14) 0.0079(12) 0.0165(12) -0.0093(12) C25 0.0418(12) 0.0410(12) 0.0310(10) 0.0065(9) 0.0073(9) -0.0009(9) C26 0.0448(13) 0.0466(13) 0.0374(12) -0.0099(10) 0.0026(10) 0.0016(10) C27 0.068(2) 0.0520(17) 0.092(3) -0.0056(16) 0.0008(19) 0.0128(15) C28 0.0584(17) 0.087(2) 0.0434(15) -0.0233(15) 0.0024(12) -0.0108(16) C29 0.0534(14) 0.0387(12) 0.0434(13) 0.0024(10) 0.0133(11) -0.0016(10) C30 0.077(2) 0.0475(16) 0.078(2) -0.0147(15) 0.0067(17) -0.0037(15) C31 0.076(2) 0.070(2) 0.0619(19) 0.0044(16) 0.0128(16) 0.0283(17) C32 0.0407(12) 0.0492(13) 0.0345(11) -0.0017(10) -0.0094(9) 0.0089(10) C33 0.0284(10) 0.0633(15) 0.0279(10) -0.0051(10) -0.0014(8) 0.0020(10) C34 0.0405(14) 0.083(2) 0.0437(14) -0.0039(14) -0.0138(11) 0.0024(13) C35 0.077(2) 0.096(3) 0.063(2) 0.0101(19) -0.0387(18) 0.017(2) C36 0.122(4) 0.066(2) 0.086(3) 0.005(2) -0.056(3) 0.029(2) C37 0.097(3) 0.0513(17) 0.064(2) -0.0004(14) -0.0398(19) 0.0169(17) C38 0.0384(12) 0.0557(14) 0.0345(11) -0.0119(10) 0.0009(9) -0.0041(10) C39 0.0581(17) 0.079(2) 0.0492(16) -0.0230(15) 0.0048(13) 0.0083(15) C40 0.0568(18) 0.082(2) 0.0567(17) -0.0149(16) 0.0051(14) -0.0278(16) C41 0.168(5) 0.0421(18) 0.105(3) -0.0047(19) -0.084(3) 0.018(2) C42 0.105(4) 0.080(3) 0.197(7) -0.053(4) -0.027(4) 0.003(3) C43 0.252(8) 0.079(3) 0.093(4) -0.028(3) 0.016(4) -0.024(4) C44 0.106(3) 0.102(3) 0.0489(18) 0.0052(19) 0.0152(19) 0.018(3) C45 0.116(4) 0.155(5) 0.073(3) 0.009(3) 0.040(3) 0.002(4) C46 0.173(6) 0.118(4) 0.047(2) 0.011(2) 0.019(3) 0.010(4) C47 0.159(5) 0.102(4) 0.057(2) 0.010(2) -0.024(3) -0.011(3) C48 0.120(3) 0.070(2) 0.064(2) 0.0017(18) 0.001(2) -0.012(2) S1 0.0483(3) 0.0429(3) 0.0461(3) -0.0077(3) 0.0059(3) -0.0037(3) O1 0.0765(14) 0.0467(10) 0.0492(11) -0.0048(9) 0.0049(10) -0.0049(10) O2 0.0642(14) 0.0825(16) 0.0675(15) 0.0059(13) -0.0114(11) -0.0020(12) O3 0.0730(16) 0.0659(14) 0.0924(19) -0.0084(13) 0.0373(14) -0.0018(12) C49 0.094(3) 0.0446(17) 0.094(3) -0.0134(17) 0.005(2) 0.0059(17) F1 0.151(3) 0.101(2) 0.149(3) -0.0563(19) 0.065(2) 0.0159(19) F2 0.181(3) 0.0408(11) 0.157(3) 0.0119(14) 0.020(2) 0.0017(15) F3 0.143(2) 0.0733(16) 0.153(3) -0.0470(17) -0.058(2) -0.0046(16) C50 0.17(2) 0.091(12) 0.16(2) -0.026(13) -0.039(16) 0.010(12) C51 0.18(5) 0.050(9) 0.15(2) -0.033(13) -0.033(18) 0.000(10) C52 0.13(3) 0.16(4) 0.28(6) -0.15(4) -0.02(3) 0.02(3) C53 0.31(4) 0.13(2) 0.125(19) -0.021(15) 0.02(3) -0.08(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 N4 2.212(2) . ? Ag1 N2 2.2983(16) . ? Ag1 N1 2.5564(18) . ? Ag1 N3 2.559(2) . ? N1 C1 1.270(3) . ? N1 C20 1.439(3) . ? N2 C6 1.338(3) . ? N2 C2 1.338(2) . ? N3 C7 1.272(3) . ? N3 C32 1.429(3) . ? N4 C48 1.295(5) . ? N4 C44 1.332(5) . ? C1 C8 1.494(3) . ? C1 C2 1.501(3) . ? C2 C3 1.395(3) . ? C3 C4 1.383(3) . ? C4 C5 1.381(3) . ? C5 C6 1.395(3) . ? C6 C7 1.503(3) . ? C7 C14 1.504(3) . ? C8 C13 1.379(3) . ? C8 C9 1.384(3) . ? C9 C10 1.395(3) . ? C10 C11 1.362(4) . ? C11 C12 1.370(5) . ? C12 C13 1.392(4) . ? C14 C15 1.383(5) . ? C14 C19 1.393(4) . ? C15 C16 1.397(4) . ? C16 C17 1.344(7) . ? C17 C18 1.360(7) . ? C18 C19 1.437(6) . ? C20 C25 1.406(3) . ? C20 C21 1.407(3) . ? C21 C22 1.399(3) . ? C21 C26 1.512(4) . ? C22 C23 1.360(5) . ? C23 C24 1.392(4) . ? C24 C25 1.400(3) . ? C25 C29 1.514(3) . ? C26 C27 1.524(4) . ? C26 C28 1.537(4) . ? C29 C30 1.518(4) . ? C29 C31 1.524(4) . ? C32 C37 1.393(4) . ? C32 C33 1.399(3) . ? C33 C34 1.394(3) . ? C33 C38 1.503(4) . ? C34 C35 1.378(5) . ? C35 C36 1.363(6) . ? C36 C37 1.402(4) . ? C37 C41 1.528(5) . ? C38 C39 1.532(4) . ? C38 C40 1.539(4) . ? C41 C43 1.497(8) . ? C41 C42 1.548(9) . ? C44 C45 1.385(6) . ? C45 C46 1.354(8) . ? C46 C47 1.389(8) . ? C47 C48 1.399(6) . ? S1 O2 1.415(2) . ? S1 O3 1.429(2) . ? S1 O1 1.432(2) . ? S1 C49 1.824(4) . ? C49 F3 1.303(5) . ? C49 F2 1.314(5) . ? C49 F1 1.330(5) . ? C50 C51 1.503(18) . ? C51 C52 1.08(2) . ? C52 C53 1.365(14) . ? 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 N4 Ag1 N2 173.07(8) . . ? N4 Ag1 N1 110.45(9) . . ? N2 Ag1 N1 68.57(6) . . ? N4 Ag1 N3 110.49(9) . . ? N2 Ag1 N3 67.95(6) . . ? N1 Ag1 N3 132.94(6) . . ? C1 N1 C20 122.34(18) . . ? C1 N1 Ag1 111.36(13) . . ? C20 N1 Ag1 122.39(12) . . ? C6 N2 C2 118.82(17) . . ? C6 N2 Ag1 120.68(13) . . ? C2 N2 Ag1 119.75(13) . . ? C7 N3 C32 123.9(2) . . ? C7 N3 Ag1 112.97(14) . . ? C32 N3 Ag1 120.16(15) . . ? C48 N4 C44 119.5(3) . . ? C48 N4 Ag1 119.0(3) . . ? C44 N4 Ag1 121.5(2) . . ? N1 C1 C8 126.45(19) . . ? N1 C1 C2 117.44(17) . . ? C8 C1 C2 116.02(17) . . ? N2 C2 C3 122.06(19) . . ? N2 C2 C1 117.45(17) . . ? C3 C2 C1 120.29(17) . . ? C4 C3 C2 119.15(19) . . ? C5 C4 C3 118.6(2) . . ? C4 C5 C6 119.2(2) . . ? N2 C6 C5 122.12(19) . . ? N2 C6 C7 117.37(17) . . ? C5 C6 C7 120.38(19) . . ? N3 C7 C14 127.6(2) . . ? N3 C7 C6 116.41(19) . . ? C14 C7 C6 115.94(19) . . ? C13 C8 C9 119.8(2) . . ? C13 C8 C1 118.8(2) . . ? C9 C8 C1 121.3(2) . . ? C8 C9 C10 119.7(2) . . ? C11 C10 C9 120.3(3) . . ? C10 C11 C12 120.1(2) . . ? C11 C12 C13 120.7(3) . . ? C8 C13 C12 119.4(3) . . ? C15 C14 C19 120.2(3) . . ? C15 C14 C7 118.7(2) . . ? C19 C14 C7 121.1(3) . . ? C14 C15 C16 120.2(4) . . ? C17 C16 C15 120.4(5) . . ? C16 C17 C18 121.1(4) . . ? C17 C18 C19 120.6(4) . . ? C14 C19 C18 117.5(4) . . ? C25 C20 C21 121.9(2) . . ? C25 C20 N1 116.36(19) . . ? C21 C20 N1 121.4(2) . . ? C22 C21 C20 117.1(2) . . ? C22 C21 C26 120.2(2) . . ? C20 C21 C26 122.7(2) . . ? C23 C22 C21 122.4(3) . . ? C22 C23 C24 120.0(2) . . ? C23 C24 C25 120.7(3) . . ? C24 C25 C20 117.9(2) . . ? C24 C25 C29 120.6(2) . . ? C20 C25 C29 121.5(2) . . ? C21 C26 C27 112.2(2) . . ? C21 C26 C28 109.4(2) . . ? C27 C26 C28 111.2(3) . . ? C25 C29 C30 112.8(2) . . ? C25 C29 C31 111.2(2) . . ? C30 C29 C31 111.2(3) . . ? C37 C32 C33 121.6(2) . . ? C37 C32 N3 115.5(2) . . ? C33 C32 N3 122.6(2) . . ? C34 C33 C32 117.6(3) . . ? C34 C33 C38 118.8(2) . . ? C32 C33 C38 123.6(2) . . ? C35 C34 C33 121.6(3) . . ? C36 C35 C34 119.9(3) . . ? C35 C36 C37 121.1(4) . . ? C32 C37 C36 118.1(3) . . ? C32 C37 C41 121.5(3) . . ? C36 C37 C41 120.4(3) . . ? C33 C38 C39 110.6(2) . . ? C33 C38 C40 111.5(2) . . ? C39 C38 C40 110.4(2) . . ? C43 C41 C37 112.1(5) . . ? C43 C41 C42 110.2(4) . . ? C37 C41 C42 111.1(4) . . ? N4 C44 C45 122.2(4) . . ? C46 C45 C44 118.3(5) . . ? C45 C46 C47 119.8(4) . . ? C46 C47 C48 117.5(5) . . ? N4 C48 C47 122.5(5) . . ? O2 S1 O3 115.25(17) . . ? O2 S1 O1 115.01(15) . . ? O3 S1 O1 114.76(16) . . ? O2 S1 C49 103.54(18) . . ? O3 S1 C49 103.20(18) . . ? O1 S1 C49 102.62(17) . . ? F3 C49 F2 106.2(4) . . ? F3 C49 F1 108.6(4) . . ? F2 C49 F1 107.4(3) . . ? F3 C49 S1 113.0(3) . . ? F2 C49 S1 111.2(3) . . ? F1 C49 S1 110.4(3) . . ? C52 C51 C50 157(4) . . ? C51 C52 C53 167(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Ag1 N1 C1 -169.93(15) . . . . ? N2 Ag1 N1 C1 17.41(14) . . . . ? N3 Ag1 N1 C1 41.07(17) . . . . ? N4 Ag1 N1 C20 -11.74(18) . . . . ? N2 Ag1 N1 C20 175.60(17) . . . . ? N3 Ag1 N1 C20 -160.74(14) . . . . ? N4 Ag1 N2 C6 81.1(8) . . . . ? N1 Ag1 N2 C6 164.35(17) . . . . ? N3 Ag1 N2 C6 2.82(14) . . . . ? N4 Ag1 N2 C2 -88.8(8) . . . . ? N1 Ag1 N2 C2 -5.62(14) . . . . ? N3 Ag1 N2 C2 -167.14(16) . . . . ? N4 Ag1 N3 C7 172.32(16) . . . . ? N2 Ag1 N3 C7 -14.93(15) . . . . ? N1 Ag1 N3 C7 -38.69(19) . . . . ? N4 Ag1 N3 C32 11.07(19) . . . . ? N2 Ag1 N3 C32 -176.18(19) . . . . ? N1 Ag1 N3 C32 160.06(15) . . . . ? N2 Ag1 N4 C48 -104.3(8) . . . . ? N1 Ag1 N4 C48 175.1(3) . . . . ? N3 Ag1 N4 C48 -28.7(3) . . . . ? N2 Ag1 N4 C44 74.8(8) . . . . ? N1 Ag1 N4 C44 -5.8(3) . . . . ? N3 Ag1 N4 C44 150.5(3) . . . . ? C20 N1 C1 C8 -0.9(3) . . . . ? Ag1 N1 C1 C8 157.33(17) . . . . ? C20 N1 C1 C2 175.49(18) . . . . ? Ag1 N1 C1 C2 -26.3(2) . . . . ? C6 N2 C2 C3 -0.3(3) . . . . ? Ag1 N2 C2 C3 169.80(16) . . . . ? C6 N2 C2 C1 -175.22(18) . . . . ? Ag1 N2 C2 C1 -5.1(2) . . . . ? N1 C1 C2 N2 23.0(3) . . . . ? C8 C1 C2 N2 -160.26(18) . . . . ? N1 C1 C2 C3 -152.0(2) . . . . ? C8 C1 C2 C3 24.8(3) . . . . ? N2 C2 C3 C4 -1.8(3) . . . . ? C1 C2 C3 C4 172.9(2) . . . . ? C2 C3 C4 C5 2.3(4) . . . . ? C3 C4 C5 C6 -0.7(4) . . . . ? C2 N2 C6 C5 2.1(3) . . . . ? Ag1 N2 C6 C5 -168.00(17) . . . . ? C2 N2 C6 C7 177.93(18) . . . . ? Ag1 N2 C6 C7 7.9(2) . . . . ? C4 C5 C6 N2 -1.5(4) . . . . ? C4 C5 C6 C7 -177.3(2) . . . . ? C32 N3 C7 C14 3.1(4) . . . . ? Ag1 N3 C7 C14 -157.4(2) . . . . ? C32 N3 C7 C6 -175.6(2) . . . . ? Ag1 N3 C7 C6 23.9(2) . . . . ? N2 C6 C7 N3 -22.7(3) . . . . ? C5 C6 C7 N3 153.3(2) . . . . ? N2 C6 C7 C14 158.5(2) . . . . ? C5 C6 C7 C14 -25.6(3) . . . . ? N1 C1 C8 C13 -119.9(3) . . . . ? C2 C1 C8 C13 63.7(3) . . . . ? N1 C1 C8 C9 63.0(3) . . . . ? C2 C1 C8 C9 -113.4(2) . . . . ? C13 C8 C9 C10 -0.7(4) . . . . ? C1 C8 C9 C10 176.3(2) . . . . ? C8 C9 C10 C11 1.2(4) . . . . ? C9 C10 C11 C12 -0.1(4) . . . . ? C10 C11 C12 C13 -1.4(5) . . . . ? C9 C8 C13 C12 -0.7(4) . . . . ? C1 C8 C13 C12 -177.8(3) . . . . ? C11 C12 C13 C8 1.8(5) . . . . ? N3 C7 C14 C15 128.9(3) . . . . ? C6 C7 C14 C15 -52.3(3) . . . . ? N3 C7 C14 C19 -49.6(4) . . . . ? C6 C7 C14 C19 129.1(2) . . . . ? C19 C14 C15 C16 -0.1(4) . . . . ? C7 C14 C15 C16 -178.6(3) . . . . ? C14 C15 C16 C17 0.0(5) . . . . ? C15 C16 C17 C18 -1.1(6) . . . . ? C16 C17 C18 C19 2.2(6) . . . . ? C15 C14 C19 C18 1.1(4) . . . . ? C7 C14 C19 C18 179.6(2) . . . . ? C17 C18 C19 C14 -2.2(5) . . . . ? C1 N1 C20 C25 -108.1(2) . . . . ? Ag1 N1 C20 C25 96.1(2) . . . . ? C1 N1 C20 C21 78.6(3) . . . . ? Ag1 N1 C20 C21 -77.2(2) . . . . ? C25 C20 C21 C22 -0.3(3) . . . . ? N1 C20 C21 C22 172.6(2) . . . . ? C25 C20 C21 C26 -177.5(2) . . . . ? N1 C20 C21 C26 -4.6(3) . . . . ? C20 C21 C22 C23 -0.3(4) . . . . ? C26 C21 C22 C23 177.0(3) . . . . ? C21 C22 C23 C24 0.7(5) . . . . ? C22 C23 C24 C25 -0.4(5) . . . . ? C23 C24 C25 C20 -0.2(4) . . . . ? C23 C24 C25 C29 -179.3(3) . . . . ? C21 C20 C25 C24 0.5(3) . . . . ? N1 C20 C25 C24 -172.7(2) . . . . ? C21 C20 C25 C29 179.6(2) . . . . ? N1 C20 C25 C29 6.4(3) . . . . ? C22 C21 C26 C27 54.3(3) . . . . ? C20 C21 C26 C27 -128.6(3) . . . . ? C22 C21 C26 C28 -69.7(3) . . . . ? C20 C21 C26 C28 107.5(3) . . . . ? C24 C25 C29 C30 -43.9(3) . . . . ? C20 C25 C29 C30 137.0(3) . . . . ? C24 C25 C29 C31 81.8(3) . . . . ? C20 C25 C29 C31 -97.2(3) . . . . ? C7 N3 C32 C37 115.2(3) . . . . ? Ag1 N3 C32 C37 -85.7(3) . . . . ? C7 N3 C32 C33 -71.4(3) . . . . ? Ag1 N3 C32 C33 87.7(3) . . . . ? C37 C32 C33 C34 -1.3(4) . . . . ? N3 C32 C33 C34 -174.3(3) . . . . ? C37 C32 C33 C38 177.2(3) . . . . ? N3 C32 C33 C38 4.3(4) . . . . ? C32 C33 C34 C35 -1.6(5) . . . . ? C38 C33 C34 C35 179.8(3) . . . . ? C33 C34 C35 C36 1.9(7) . . . . ? C34 C35 C36 C37 0.7(8) . . . . ? C33 C32 C37 C36 3.8(6) . . . . ? N3 C32 C37 C36 177.2(4) . . . . ? C33 C32 C37 C41 -176.3(4) . . . . ? N3 C32 C37 C41 -2.9(6) . . . . ? C35 C36 C37 C32 -3.4(8) . . . . ? C35 C36 C37 C41 176.6(5) . . . . ? C34 C33 C38 C39 63.2(3) . . . . ? C32 C33 C38 C39 -115.3(3) . . . . ? C34 C33 C38 C40 -60.0(3) . . . . ? C32 C33 C38 C40 121.4(3) . . . . ? C32 C37 C41 C43 -120.5(5) . . . . ? C36 C37 C41 C43 59.4(7) . . . . ? C32 C37 C41 C42 115.8(4) . . . . ? C36 C37 C41 C42 -64.3(6) . . . . ? C48 N4 C44 C45 1.6(7) . . . . ? Ag1 N4 C44 C45 -177.5(4) . . . . ? N4 C44 C45 C46 -4.5(8) . . . . ? C44 C45 C46 C47 4.2(9) . . . . ? C45 C46 C47 C48 -1.3(9) . . . . ? C44 N4 C48 C47 1.6(6) . . . . ? Ag1 N4 C48 C47 -179.3(4) . . . . ? C46 C47 C48 N4 -1.7(8) . . . . ? O2 S1 C49 F3 -179.2(3) . . . . ? O3 S1 C49 F3 60.3(4) . . . . ? O1 S1 C49 F3 -59.2(4) . . . . ? O2 S1 C49 F2 61.5(4) . . . . ? O3 S1 C49 F2 -58.9(4) . . . . ? O1 S1 C49 F2 -178.5(3) . . . . ? O2 S1 C49 F1 -57.5(4) . . . . ? O3 S1 C49 F1 -178.0(3) . . . . ? O1 S1 C49 F1 62.5(3) . . . . ? C50 C51 C52 C53 53(38) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.605 _refine_diff_density_min -0.512 _refine_diff_density_rms 0.063 data_dr026a _database_code_depnum_ccdc_archive 'CCDC 849372' #TrackingRef '- combined structures.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H76 Ag F3 N3 O3 S' _chemical_formula_weight 1084.17 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' 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 Orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 31.0722(11) _cell_length_b 9.7664(4) _cell_length_c 19.8728(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6030.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9533 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 21.95 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas n/a _exptl_crystal_density_diffrn 1.194 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2284 _exptl_absorpt_coefficient_mu 0.421 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9319 _exptl_absorpt_correction_T_max 0.9592 _exptl_absorpt_process_details 'SADABS, Bruker (2003)' _exptl_special_details ; Data collection is performed with three batch runs at phi = 0.00 deg (650 frames), at phi = 120.00 deg (650 frames), and at phi = 240.00 deg (650 frames). Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 91642 _diffrn_reflns_av_R_equivalents 0.0584 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 21.98 _reflns_number_total 7330 _reflns_number_gt 6625 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, Bruker (2009)' _computing_cell_refinement 'APEX II, Bruker (2009)' _computing_data_reduction 'XPREP, Bruker (2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL, Bruker (2004)' _computing_publication_material 'SHELXTL, Bruker (2004)' _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^)+(0.1000P)^2^+0.6296P] 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 0.00(10) _refine_ls_number_reflns 7330 _refine_ls_number_parameters 637 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0538 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1277 _refine_ls_wR_factor_gt 0.1207 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.870389(11) 0.59169(4) -0.00037(3) 0.04065(16) Uani 1 1 d . . . N1 N 0.91997(13) 0.4754(5) 0.0898(2) 0.0332(10) Uani 1 1 d . . . N2 N 0.89820(14) 0.3856(4) -0.0349(2) 0.0284(10) Uani 1 1 d . . . N3 N 0.82256(13) 0.4762(5) -0.0844(2) 0.0322(10) Uani 1 1 d . . . C1 C 0.94872(18) 0.4089(6) 0.0560(3) 0.0379(14) Uani 1 1 d . . . C2 C 0.93220(14) 0.3324(4) -0.0044(3) 0.0279(10) Uani 1 1 d . . . C3 C 0.95104(18) 0.2120(6) -0.0256(3) 0.0399(14) Uani 1 1 d . . . H3A H 0.9755 0.1759 -0.0031 0.048 Uiso 1 1 calc R . . C4 C 0.93340(17) 0.1455(6) -0.0801(3) 0.0380(14) Uani 1 1 d . . . H4A H 0.9452 0.0612 -0.0951 0.046 Uiso 1 1 calc R . . C5 C 0.89871(17) 0.2013(5) -0.1126(3) 0.0378(13) Uani 1 1 d . . . H5A H 0.8863 0.1571 -0.1505 0.045 Uiso 1 1 calc R . . C6 C 0.88225(17) 0.3227(5) -0.0891(3) 0.0323(12) Uani 1 1 d . . . C7 C 0.84367(17) 0.3898(5) -0.1208(3) 0.0314(13) Uani 1 1 d . . . C8 C 0.99517(17) 0.3958(6) 0.0722(3) 0.0399(15) Uani 1 1 d . . . C9 C 1.00955(19) 0.3537(7) 0.1341(3) 0.0504(16) Uani 1 1 d . . . H9A H 0.9896 0.3314 0.1687 0.061 Uiso 1 1 calc R . . C10 C 1.0543(2) 0.3440(9) 0.1458(4) 0.067(2) Uani 1 1 d . . . H10A H 1.0645 0.3134 0.1883 0.080 Uiso 1 1 calc R . . C11 C 1.0827(2) 0.3780(10) 0.0968(5) 0.083(2) Uani 1 1 d . . . H11A H 1.1127 0.3698 0.1050 0.099 Uiso 1 1 calc R . . C12 C 1.0688(2) 0.4233(10) 0.0367(5) 0.090(3) Uani 1 1 d . . . H12A H 1.0890 0.4509 0.0034 0.107 Uiso 1 1 calc R . . C13 C 1.0240(2) 0.4299(9) 0.0230(4) 0.073(2) Uani 1 1 d . . . H13A H 1.0141 0.4578 -0.0201 0.088 Uiso 1 1 calc R . . C14 C 0.83365(18) 0.3567(6) -0.1927(3) 0.0382(14) Uani 1 1 d . . . C15 C 0.8651(2) 0.3692(8) -0.2417(3) 0.0480(17) Uani 1 1 d . . . H15A H 0.8934 0.3967 -0.2299 0.058 Uiso 1 1 calc R . . C16 C 0.8547(3) 0.3410(8) -0.3088(4) 0.070(2) Uani 1 1 d . . . H16A H 0.8760 0.3494 -0.3429 0.084 Uiso 1 1 calc R . . C17 C 0.8132(3) 0.3007(8) -0.3251(3) 0.067(2) Uani 1 1 d . . . H17A H 0.8060 0.2837 -0.3708 0.080 Uiso 1 1 calc R . . C18 C 0.7830(3) 0.2856(8) -0.2772(4) 0.070(2) Uani 1 1 d . . . H18A H 0.7551 0.2540 -0.2892 0.085 Uiso 1 1 calc R . . C19 C 0.7921(2) 0.3157(6) -0.2098(3) 0.0518(17) Uani 1 1 d . . . H19A H 0.7704 0.3083 -0.1763 0.062 Uiso 1 1 calc R . . C20 C 0.93077(19) 0.5598(6) 0.1462(3) 0.0378(14) Uani 1 1 d . . . C21 C 0.90868(19) 0.5444(6) 0.2078(3) 0.0451(15) Uani 1 1 d . . . C22 C 0.9204(2) 0.6372(7) 0.2573(3) 0.0580(18) Uani 1 1 d . . . H22A H 0.9080 0.6274 0.3007 0.070 Uiso 1 1 calc R . . C23 C 0.9488(3) 0.7421(8) 0.2471(4) 0.071(2) Uani 1 1 d . . . H23A H 0.9549 0.8035 0.2829 0.085 Uiso 1 1 calc R . . C24 C 0.9687(2) 0.7603(6) 0.1856(3) 0.0527(16) Uani 1 1 d . . . C25 C 0.95943(19) 0.6650(6) 0.1368(3) 0.0399(15) Uani 1 1 d . . . H25A H 0.9736 0.6722 0.0945 0.048 Uiso 1 1 calc R . . C26 C 0.8755(2) 0.4334(7) 0.2211(4) 0.0512(19) Uani 1 1 d . . . C27 C 0.8583(3) 0.4364(9) 0.2941(4) 0.077(2) Uani 1 1 d . . . H27A H 0.8824 0.4261 0.3256 0.116 Uiso 1 1 calc R . . H27B H 0.8379 0.3611 0.3006 0.116 Uiso 1 1 calc R . . H27C H 0.8438 0.5239 0.3024 0.116 Uiso 1 1 calc R . . C28 C 0.8948(2) 0.2893(7) 0.2109(3) 0.0602(18) Uani 1 1 d . . . H28A H 0.9199 0.2780 0.2404 0.090 Uiso 1 1 calc R . . H28B H 0.9037 0.2784 0.1639 0.090 Uiso 1 1 calc R . . H28C H 0.8731 0.2200 0.2221 0.090 Uiso 1 1 calc R . . C29 C 0.8367(2) 0.4509(9) 0.1745(4) 0.066(2) Uani 1 1 d . . . H29A H 0.8463 0.4491 0.1276 0.099 Uiso 1 1 calc R . . H29B H 0.8226 0.5387 0.1839 0.099 Uiso 1 1 calc R . . H29C H 0.8162 0.3762 0.1822 0.099 Uiso 1 1 calc R . . C30 C 1.0017(2) 0.8775(7) 0.1736(4) 0.066(2) Uani 1 1 d . . . C31 C 0.9999(5) 0.9821(12) 0.2319(6) 0.159(6) Uani 1 1 d . . . H31A H 1.0207 1.0553 0.2237 0.239 Uiso 1 1 calc R . . H31B H 1.0068 0.9359 0.2744 0.239 Uiso 1 1 calc R . . H31C H 0.9709 1.0212 0.2347 0.239 Uiso 1 1 calc R . . C32 C 1.0435(3) 0.8174(15) 0.1705(11) 0.190(9) Uani 1 1 d . . . H32A H 1.0447 0.7522 0.1331 0.285 Uiso 1 1 calc R . . H32B H 1.0496 0.7694 0.2128 0.285 Uiso 1 1 calc R . . H32C H 1.0651 0.8893 0.1636 0.285 Uiso 1 1 calc R . . C33 C 0.9893(3) 0.9559(10) 0.1107(5) 0.108(4) Uani 1 1 d . . . H33A H 0.9891 0.8935 0.0721 0.163 Uiso 1 1 calc R . . H33B H 1.0102 1.0293 0.1028 0.163 Uiso 1 1 calc R . . H33C H 0.9606 0.9957 0.1166 0.163 Uiso 1 1 calc R . . C34 C 0.79134(18) 0.5651(5) -0.1141(3) 0.0329(13) Uani 1 1 d . . . C35 C 0.74879(17) 0.5765(5) -0.0886(3) 0.0375(14) Uani 1 1 d . . . C36 C 0.72306(18) 0.6699(7) -0.1216(3) 0.0487(16) Uani 1 1 d . . . H36A H 0.6942 0.6804 -0.1067 0.058 Uiso 1 1 calc R . . C37 C 0.73701(19) 0.7501(6) -0.1755(3) 0.0491(16) Uani 1 1 d . . . H37A H 0.7176 0.8128 -0.1958 0.059 Uiso 1 1 calc R . . C38 C 0.77876(19) 0.7398(6) -0.1998(3) 0.0406(14) Uani 1 1 d . . . C39 C 0.80555(19) 0.6468(6) -0.1670(3) 0.0393(14) Uani 1 1 d . . . H39A H 0.8346 0.6390 -0.1812 0.047 Uiso 1 1 calc R . . C40 C 0.73233(19) 0.4953(7) -0.0276(3) 0.0454(15) Uani 1 1 d . . . C41 C 0.7591(2) 0.5222(8) 0.0348(3) 0.0586(18) Uani 1 1 d . . . H41A H 0.7894 0.5011 0.0254 0.088 Uiso 1 1 calc R . . H41B H 0.7489 0.4642 0.0717 0.088 Uiso 1 1 calc R . . H41C H 0.7565 0.6187 0.0477 0.088 Uiso 1 1 calc R . . C42 C 0.7343(2) 0.3403(7) -0.0439(4) 0.0593(18) Uani 1 1 d . . . H42A H 0.7640 0.3146 -0.0548 0.089 Uiso 1 1 calc R . . H42B H 0.7157 0.3204 -0.0824 0.089 Uiso 1 1 calc R . . H42C H 0.7245 0.2877 -0.0047 0.089 Uiso 1 1 calc R . . C43 C 0.6851(2) 0.5287(8) -0.0120(4) 0.068(2) Uani 1 1 d . . . H43A H 0.6675 0.5112 -0.0520 0.102 Uiso 1 1 calc R . . H43B H 0.6826 0.6252 0.0008 0.102 Uiso 1 1 calc R . . H43C H 0.6751 0.4709 0.0252 0.102 Uiso 1 1 calc R . . C44 C 0.7964(2) 0.8262(7) -0.2565(3) 0.0546(17) Uani 1 1 d . . . C45 C 0.8320(3) 0.9221(10) -0.2284(5) 0.105(4) Uani 1 1 d . . . H45A H 0.8194 0.9848 -0.1954 0.158 Uiso 1 1 calc R . . H45B H 0.8446 0.9750 -0.2654 0.158 Uiso 1 1 calc R . . H45C H 0.8545 0.8671 -0.2068 0.158 Uiso 1 1 calc R . . C46 C 0.8167(5) 0.7303(12) -0.3090(5) 0.150(6) Uani 1 1 d . . . H46A H 0.7946 0.6694 -0.3273 0.224 Uiso 1 1 calc R . . H46B H 0.8394 0.6756 -0.2876 0.224 Uiso 1 1 calc R . . H46C H 0.8292 0.7849 -0.3455 0.224 Uiso 1 1 calc R . . C47 C 0.7633(3) 0.9161(9) -0.2900(5) 0.094(3) Uani 1 1 d . . . H47A H 0.7402 0.8590 -0.3084 0.141 Uiso 1 1 calc R . . H47B H 0.7768 0.9681 -0.3264 0.141 Uiso 1 1 calc R . . H47C H 0.7512 0.9798 -0.2568 0.141 Uiso 1 1 calc R . . C48 C 0.85330(19) 0.8313(6) -0.0154(3) 0.0441(15) Uani 1 1 d . . . H48A H 0.8689 0.8153 -0.0558 0.053 Uiso 1 1 calc R . . C49 C 0.87389(18) 0.8151(6) 0.0446(3) 0.0410(15) Uani 1 1 d . . . H49A H 0.9036 0.7928 0.0434 0.049 Uiso 1 1 calc R . . C50 C 0.8533(2) 0.8298(6) 0.1119(3) 0.0483(15) Uani 1 1 d . . . H50A H 0.8701 0.7761 0.1450 0.058 Uiso 1 1 calc R . . H50B H 0.8241 0.7896 0.1098 0.058 Uiso 1 1 calc R . . C51 C 0.8497(2) 0.9751(7) 0.1369(3) 0.0592(17) Uani 1 1 d . . . H51A H 0.8782 1.0193 0.1318 0.071 Uiso 1 1 calc R . . H51B H 0.8431 0.9722 0.1856 0.071 Uiso 1 1 calc R . . C52 C 0.8164(3) 1.0659(7) 0.1031(4) 0.068(2) Uani 1 1 d . . . H52A H 0.8123 1.1489 0.1309 0.082 Uiso 1 1 calc R . . H52B H 0.7887 1.0163 0.1018 0.082 Uiso 1 1 calc R . . C53 C 0.8280(3) 1.1098(7) 0.0318(4) 0.063(2) Uani 1 1 d . . . H53A H 0.8593 1.0966 0.0251 0.076 Uiso 1 1 calc R . . H53B H 0.8219 1.2088 0.0270 0.076 Uiso 1 1 calc R . . C54 C 0.8036(2) 1.0317(6) -0.0239(3) 0.0552(18) Uani 1 1 d . . . H54A H 0.7728 1.0573 -0.0217 0.066 Uiso 1 1 calc R . . H54B H 0.8148 1.0621 -0.0681 0.066 Uiso 1 1 calc R . . C55 C 0.8071(2) 0.8731(6) -0.0202(3) 0.0431(15) Uani 1 1 d . . . H55A H 0.7912 0.8393 0.0196 0.052 Uiso 1 1 calc R . . H55B H 0.7940 0.8320 -0.0609 0.052 Uiso 1 1 calc R . . S1 S 0.95020(6) 0.69681(19) 0.88191(9) 0.0574(5) Uani 1 1 d . . . O1 O 0.9614(3) 0.8288(7) 0.8603(4) 0.128(3) Uani 1 1 d . . . O2 O 0.95401(15) 0.6695(6) 0.9525(2) 0.0690(13) Uani 1 1 d . . . O3 O 0.91195(17) 0.6416(8) 0.8534(3) 0.0973(19) Uani 1 1 d . . . C56 C 0.9913(3) 0.5811(11) 0.8447(4) 0.085(3) Uani 1 1 d . . . F1 F 1.02953(17) 0.6123(7) 0.8699(4) 0.128(2) Uani 1 1 d . . . F2 F 0.98223(19) 0.4538(6) 0.8604(3) 0.1073(17) Uani 1 1 d . . . F3 F 0.9939(3) 0.6018(10) 0.7821(3) 0.175(4) Uani 1 1 d . . . C61 C 0.5879(10) 0.025(4) 0.8742(16) 0.182(12) Uiso 0.50 1 d PD . . H61A H 0.5915 0.1220 0.8605 0.219 Uiso 0.50 1 calc PR . . H61B H 0.5720 -0.0204 0.8373 0.219 Uiso 0.50 1 calc PR . . C62 C 0.5592(10) 0.026(3) 0.9320(16) 0.178(12) Uiso 0.50 1 d PD . . H62A H 0.5625 -0.0576 0.9596 0.214 Uiso 0.50 1 calc PR . . H62B H 0.5288 0.0363 0.9183 0.214 Uiso 0.50 1 calc PR . . C63 C 0.5756(10) 0.154(4) 0.9694(18) 0.198(15) Uiso 0.50 1 d PD . . H63A H 0.5750 0.2299 0.9363 0.237 Uiso 0.50 1 calc PR . . H63B H 0.5535 0.1762 1.0036 0.237 Uiso 0.50 1 calc PR . . C64 C 0.6174(7) 0.164(2) 1.0039(15) 0.125(6) Uiso 0.50 1 d PD . . H64A H 0.6121 0.2219 1.0440 0.150 Uiso 0.50 1 calc PR . . H64B H 0.6359 0.2192 0.9737 0.150 Uiso 0.50 1 calc PR . . C57 C 0.6449(11) 0.050(3) 1.0278(19) 0.179(12) Uiso 0.50 1 d PD . . H57A H 0.6445 0.0243 1.0739 0.215 Uiso 0.50 1 calc PR . . C58 C 0.6679(8) -0.009(3) 0.9885(11) 0.130(7) Uiso 0.50 1 d PD . . H58A H 0.6868 -0.0772 1.0057 0.155 Uiso 0.50 1 calc PR . . C59 C 0.6685(7) 0.018(2) 0.9159(10) 0.115(6) Uiso 0.50 1 d PD . . H59A H 0.6955 -0.0206 0.8975 0.138 Uiso 0.50 1 calc PR . . H59B H 0.6698 0.1184 0.9094 0.138 Uiso 0.50 1 calc PR . . C60 C 0.6318(9) -0.036(4) 0.875(2) 0.205(16) Uiso 0.50 1 d PD . . H60A H 0.6418 -0.0365 0.8274 0.246 Uiso 0.50 1 calc PR . . H60B H 0.6282 -0.1334 0.8877 0.246 Uiso 0.50 1 calc PR . . 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 0.0425(3) 0.0358(2) 0.0437(2) -0.0092(3) -0.0026(3) 0.00641(16) N1 0.036(3) 0.033(3) 0.031(3) -0.001(2) -0.003(2) 0.000(2) N2 0.029(3) 0.031(2) 0.025(2) -0.008(2) 0.000(2) -0.001(2) N3 0.031(2) 0.034(3) 0.032(2) -0.001(2) -0.004(2) 0.002(2) C1 0.038(4) 0.046(4) 0.031(3) 0.010(3) -0.001(3) -0.001(3) C2 0.032(3) 0.025(2) 0.027(3) -0.002(3) 0.000(3) 0.001(2) C3 0.039(3) 0.041(3) 0.039(3) 0.001(3) 0.003(2) -0.001(3) C4 0.041(3) 0.033(3) 0.039(3) -0.007(3) 0.002(3) 0.008(3) C5 0.045(3) 0.031(3) 0.038(3) 0.000(3) -0.003(3) 0.007(3) C6 0.032(3) 0.031(3) 0.034(3) -0.003(3) 0.006(2) -0.005(2) C7 0.039(3) 0.025(3) 0.030(3) 0.005(3) 0.001(3) -0.009(2) C8 0.030(3) 0.052(4) 0.038(4) 0.002(3) -0.001(3) 0.001(3) C9 0.041(4) 0.063(4) 0.047(4) 0.011(3) -0.006(3) 0.005(3) C10 0.047(4) 0.097(6) 0.056(5) 0.020(4) -0.021(4) -0.003(4) C11 0.039(4) 0.111(7) 0.098(7) 0.018(5) -0.016(4) 0.002(4) C12 0.034(4) 0.149(9) 0.085(6) 0.037(6) 0.002(4) -0.008(4) C13 0.040(4) 0.115(7) 0.066(6) 0.027(4) -0.004(3) 0.006(4) C14 0.038(4) 0.039(3) 0.038(4) -0.010(3) -0.012(3) 0.013(3) C15 0.052(4) 0.060(4) 0.032(4) -0.008(4) -0.005(3) 0.014(3) C16 0.091(6) 0.078(5) 0.041(4) -0.006(4) 0.004(4) 0.022(5) C17 0.088(6) 0.080(5) 0.033(4) -0.008(4) -0.023(4) 0.029(5) C18 0.064(5) 0.076(5) 0.072(5) -0.022(4) -0.034(4) 0.009(4) C19 0.055(4) 0.047(4) 0.054(4) -0.019(3) -0.016(3) 0.014(3) C20 0.041(3) 0.033(3) 0.040(4) -0.004(3) -0.008(3) 0.009(3) C21 0.052(4) 0.041(3) 0.042(4) 0.005(3) -0.001(3) 0.014(3) C22 0.096(5) 0.040(4) 0.038(4) -0.005(3) 0.001(4) 0.009(4) C23 0.112(6) 0.055(5) 0.046(5) -0.012(4) -0.024(4) -0.005(4) C24 0.065(4) 0.041(4) 0.052(4) 0.000(3) -0.019(3) -0.004(3) C25 0.044(4) 0.035(4) 0.041(4) 0.009(3) -0.008(3) 0.002(3) C26 0.065(5) 0.047(4) 0.041(4) -0.003(3) 0.013(3) 0.002(3) C27 0.101(6) 0.070(5) 0.060(5) -0.002(4) 0.029(5) 0.000(5) C28 0.073(5) 0.055(4) 0.053(4) 0.004(3) 0.015(3) -0.010(3) C29 0.045(4) 0.083(5) 0.070(5) 0.011(4) 0.000(4) -0.007(4) C30 0.066(5) 0.044(4) 0.089(6) -0.006(4) -0.026(4) -0.015(3) C31 0.280(16) 0.100(9) 0.099(9) -0.047(7) 0.013(10) -0.100(10) C32 0.059(7) 0.132(10) 0.38(3) 0.077(13) -0.006(10) -0.024(7) C33 0.104(7) 0.085(6) 0.137(9) 0.051(6) -0.045(6) -0.041(5) C34 0.039(3) 0.030(3) 0.030(3) -0.004(3) -0.009(3) 0.010(2) C35 0.033(3) 0.032(3) 0.048(4) -0.002(3) -0.007(3) 0.000(2) C36 0.032(3) 0.059(4) 0.056(4) 0.002(3) -0.006(3) 0.003(3) C37 0.048(4) 0.044(4) 0.055(4) 0.007(3) -0.020(3) 0.011(3) C38 0.047(4) 0.033(3) 0.042(3) -0.005(3) -0.007(3) 0.005(3) C39 0.045(4) 0.038(3) 0.035(3) -0.002(3) 0.003(3) -0.001(3) C40 0.032(3) 0.056(4) 0.048(4) 0.002(3) 0.004(3) 0.003(3) C41 0.050(4) 0.078(5) 0.048(4) 0.001(4) 0.007(3) -0.012(4) C42 0.069(5) 0.042(4) 0.067(5) 0.002(3) 0.020(4) -0.012(3) C43 0.050(4) 0.074(4) 0.080(6) 0.010(4) 0.030(4) 0.021(3) C44 0.072(4) 0.052(4) 0.040(4) 0.017(3) -0.003(3) 0.009(3) C45 0.096(6) 0.112(7) 0.107(8) 0.070(6) -0.023(5) -0.044(5) C46 0.269(15) 0.113(8) 0.067(6) 0.035(6) 0.076(8) 0.082(9) C47 0.094(6) 0.101(7) 0.086(6) 0.043(5) -0.014(5) 0.004(5) C48 0.041(3) 0.042(3) 0.049(5) -0.006(3) 0.001(3) 0.008(3) C49 0.040(4) 0.027(3) 0.055(4) 0.000(3) -0.002(3) 0.004(2) C50 0.063(4) 0.044(4) 0.038(3) -0.011(3) -0.004(3) 0.011(3) C51 0.081(5) 0.060(4) 0.037(4) -0.013(3) -0.002(3) 0.011(4) C52 0.083(5) 0.047(4) 0.073(5) -0.013(4) 0.012(4) 0.002(3) C53 0.088(5) 0.027(3) 0.074(5) 0.001(3) 0.000(4) -0.001(3) C54 0.087(5) 0.032(3) 0.046(4) -0.007(3) -0.002(3) 0.012(3) C55 0.065(4) 0.033(3) 0.031(4) -0.010(2) -0.007(2) 0.005(3) S1 0.0578(11) 0.0554(11) 0.0590(12) 0.0110(9) 0.0179(9) 0.0043(8) O1 0.170(7) 0.070(4) 0.143(6) 0.041(4) 0.033(5) 0.001(4) O2 0.069(3) 0.091(4) 0.047(3) -0.009(3) 0.011(2) 0.002(3) O3 0.060(4) 0.135(5) 0.096(4) 0.030(4) -0.020(3) -0.007(4) C56 0.088(7) 0.115(8) 0.053(6) 0.027(5) 0.014(5) 0.000(5) F1 0.057(3) 0.189(7) 0.138(5) 0.040(4) 0.028(3) 0.018(3) F2 0.137(5) 0.088(4) 0.097(4) -0.001(3) 0.027(3) 0.026(3) F3 0.173(6) 0.296(10) 0.055(3) 0.055(4) 0.046(4) 0.116(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.296(4) . ? Ag1 C49 2.360(6) . ? Ag1 C48 2.418(5) . ? Ag1 N3 2.503(4) . ? Ag1 N1 2.622(4) . ? N1 C1 1.292(7) . ? N1 C20 1.432(7) . ? N2 C2 1.324(6) . ? N2 C6 1.335(7) . ? N3 C7 1.291(7) . ? N3 C34 1.430(7) . ? C1 C8 1.484(8) . ? C1 C2 1.505(8) . ? C2 C3 1.379(8) . ? C3 C4 1.378(8) . ? C4 C5 1.370(8) . ? C5 C6 1.373(8) . ? C6 C7 1.505(8) . ? C7 C14 1.497(8) . ? C8 C13 1.368(9) . ? C8 C9 1.371(9) . ? C9 C10 1.413(9) . ? C10 C11 1.356(11) . ? C11 C12 1.346(12) . ? C12 C13 1.420(10) . ? C14 C19 1.394(9) . ? C14 C15 1.385(9) . ? C15 C16 1.397(10) . ? C16 C17 1.388(11) . ? C17 C18 1.345(11) . ? C18 C19 1.400(10) . ? C20 C25 1.372(8) . ? C20 C21 1.412(9) . ? C21 C22 1.386(9) . ? C21 C26 1.518(10) . ? C22 C23 1.367(11) . ? C23 C24 1.381(10) . ? C24 C25 1.375(9) . ? C24 C30 1.555(9) . ? C26 C28 1.542(10) . ? C26 C29 1.532(10) . ? C26 C27 1.547(11) . ? C30 C32 1.428(14) . ? C30 C33 1.516(12) . ? C30 C31 1.545(13) . ? C34 C39 1.391(8) . ? C34 C35 1.421(8) . ? C35 C36 1.379(8) . ? C35 C40 1.536(9) . ? C36 C37 1.396(9) . ? C37 C38 1.388(8) . ? C38 C39 1.394(8) . ? C38 C44 1.511(9) . ? C40 C42 1.549(10) . ? C40 C41 1.517(9) . ? C40 C43 1.534(8) . ? C44 C47 1.508(11) . ? C44 C46 1.537(11) . ? C44 C45 1.553(12) . ? C48 C49 1.361(8) . ? C48 C55 1.495(9) . ? C49 C50 1.490(9) . ? C50 C51 1.508(9) . ? C51 C52 1.518(10) . ? C52 C53 1.523(11) . ? C53 C54 1.544(10) . ? C54 C55 1.554(9) . ? S1 O1 1.403(7) . ? S1 O3 1.423(6) . ? S1 O2 1.433(5) . ? S1 C56 1.859(10) . ? C56 F3 1.264(10) . ? C56 F2 1.312(10) . ? C56 F1 1.325(11) . ? C61 C62 1.454(19) . ? C61 C60 1.492(19) . ? C62 C63 1.542(19) . ? C63 C64 1.471(18) . ? C64 C57 1.480(19) . ? C57 C58 1.21(4) . ? C58 C59 1.467(18) . ? C59 C60 1.501(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 C49 155.02(18) . . ? N2 Ag1 C48 153.41(18) . . ? C49 Ag1 C48 33.1(2) . . ? N2 Ag1 N3 68.21(15) . . ? C49 Ag1 N3 134.12(17) . . ? C48 Ag1 N3 102.91(17) . . ? N2 Ag1 N1 66.63(15) . . ? C49 Ag1 N1 96.61(18) . . ? C48 Ag1 N1 129.25(17) . . ? N3 Ag1 N1 127.53(14) . . ? C1 N1 C20 122.3(5) . . ? C1 N1 Ag1 105.6(3) . . ? C20 N1 Ag1 115.0(3) . . ? C2 N2 C6 119.1(4) . . ? C2 N2 Ag1 120.5(3) . . ? C6 N2 Ag1 120.3(3) . . ? C7 N3 C34 120.6(4) . . ? C7 N3 Ag1 111.5(3) . . ? C34 N3 Ag1 113.9(3) . . ? N1 C1 C8 127.1(5) . . ? N1 C1 C2 115.3(5) . . ? C8 C1 C2 117.5(5) . . ? N2 C2 C3 122.2(5) . . ? N2 C2 C1 116.3(4) . . ? C3 C2 C1 121.5(5) . . ? C4 C3 C2 118.2(5) . . ? C3 C4 C5 119.8(5) . . ? C6 C5 C4 118.5(5) . . ? N2 C6 C5 122.2(5) . . ? N2 C6 C7 115.7(5) . . ? C5 C6 C7 122.0(5) . . ? N3 C7 C6 117.0(5) . . ? N3 C7 C14 124.8(5) . . ? C6 C7 C14 118.1(5) . . ? C13 C8 C9 120.1(6) . . ? C13 C8 C1 117.4(5) . . ? C9 C8 C1 122.5(5) . . ? C8 C9 C10 119.3(6) . . ? C11 C10 C9 120.4(6) . . ? C12 C11 C10 120.7(7) . . ? C11 C12 C13 120.0(8) . . ? C8 C13 C12 119.6(7) . . ? C19 C14 C15 120.5(6) . . ? C19 C14 C7 119.1(5) . . ? C15 C14 C7 120.4(5) . . ? C16 C15 C14 119.4(7) . . ? C17 C16 C15 119.5(7) . . ? C18 C17 C16 120.9(6) . . ? C17 C18 C19 120.9(7) . . ? C14 C19 C18 118.7(7) . . ? C25 C20 C21 120.9(6) . . ? C25 C20 N1 118.5(5) . . ? C21 C20 N1 120.2(5) . . ? C22 C21 C20 114.7(6) . . ? C22 C21 C26 121.4(6) . . ? C20 C21 C26 123.9(6) . . ? C23 C22 C21 123.7(6) . . ? C22 C23 C24 121.0(6) . . ? C23 C24 C25 116.4(6) . . ? C23 C24 C30 121.7(6) . . ? C25 C24 C30 121.9(7) . . ? C20 C25 C24 123.1(6) . . ? C21 C26 C28 111.4(5) . . ? C21 C26 C29 110.4(6) . . ? C28 C26 C29 109.2(6) . . ? C21 C26 C27 112.6(6) . . ? C28 C26 C27 106.0(7) . . ? C29 C26 C27 107.0(6) . . ? C32 C30 C33 113.8(10) . . ? C32 C30 C31 109.7(11) . . ? C33 C30 C31 106.0(8) . . ? C32 C30 C24 107.7(7) . . ? C33 C30 C24 109.3(6) . . ? C31 C30 C24 110.3(8) . . ? C39 C34 C35 121.4(5) . . ? C39 C34 N3 116.5(5) . . ? C35 C34 N3 122.1(5) . . ? C36 C35 C34 114.9(5) . . ? C36 C35 C40 121.6(5) . . ? C34 C35 C40 123.5(5) . . ? C35 C36 C37 123.8(6) . . ? C38 C37 C36 121.1(5) . . ? C37 C38 C39 116.2(5) . . ? C37 C38 C44 123.9(5) . . ? C39 C38 C44 119.8(5) . . ? C38 C39 C34 122.6(5) . . ? C42 C40 C41 108.6(6) . . ? C42 C40 C35 109.0(5) . . ? C41 C40 C35 111.9(5) . . ? C42 C40 C43 106.7(5) . . ? C41 C40 C43 108.8(5) . . ? C35 C40 C43 111.6(5) . . ? C47 C44 C38 114.0(6) . . ? C47 C44 C46 109.7(7) . . ? C38 C44 C46 108.3(6) . . ? C47 C44 C45 107.1(7) . . ? C38 C44 C45 109.1(6) . . ? C46 C44 C45 108.6(9) . . ? C49 C48 C55 122.6(5) . . ? C49 C48 Ag1 71.1(3) . . ? C55 C48 Ag1 118.9(4) . . ? C48 C49 C50 124.9(5) . . ? C48 C49 Ag1 75.8(4) . . ? C50 C49 Ag1 114.1(4) . . ? C49 C50 C51 114.7(6) . . ? C50 C51 C52 117.0(6) . . ? C51 C52 C53 114.5(6) . . ? C52 C53 C54 114.4(6) . . ? C55 C54 C53 115.1(5) . . ? C48 C55 C54 110.0(5) . . ? O1 S1 O3 115.7(5) . . ? O1 S1 O2 116.8(5) . . ? O3 S1 O2 112.8(3) . . ? O1 S1 C56 105.4(5) . . ? O3 S1 C56 100.6(5) . . ? O2 S1 C56 102.7(3) . . ? F3 C56 F2 113.5(10) . . ? F3 C56 F1 106.2(8) . . ? F2 C56 F1 108.7(8) . . ? F3 C56 S1 109.8(7) . . ? F2 C56 S1 109.5(6) . . ? F1 C56 S1 109.0(7) . . ? C62 C61 C60 124(3) . . ? C61 C62 C63 101(3) . . ? C64 C63 C62 125(3) . . ? C63 C64 C57 128(3) . . ? C58 C57 C64 120(3) . . ? C57 C58 C59 124(3) . . ? C58 C59 C60 118(3) . . ? C61 C60 C59 124(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ag1 N1 C1 32.0(3) . . . . ? C49 Ag1 N1 C1 -128.7(4) . . . . ? C48 Ag1 N1 C1 -122.8(4) . . . . ? N3 Ag1 N1 C1 64.7(4) . . . . ? N2 Ag1 N1 C20 170.0(4) . . . . ? C49 Ag1 N1 C20 9.3(4) . . . . ? C48 Ag1 N1 C20 15.2(5) . . . . ? N3 Ag1 N1 C20 -157.3(3) . . . . ? C49 Ag1 N2 C2 32.5(7) . . . . ? C48 Ag1 N2 C2 114.2(5) . . . . ? N3 Ag1 N2 C2 -171.0(4) . . . . ? N1 Ag1 N2 C2 -18.4(4) . . . . ? C49 Ag1 N2 C6 -142.6(5) . . . . ? C48 Ag1 N2 C6 -61.0(6) . . . . ? N3 Ag1 N2 C6 13.9(4) . . . . ? N1 Ag1 N2 C6 166.5(4) . . . . ? N2 Ag1 N3 C7 -22.9(3) . . . . ? C49 Ag1 N3 C7 143.6(4) . . . . ? C48 Ag1 N3 C7 130.8(4) . . . . ? N1 Ag1 N3 C7 -55.1(4) . . . . ? N2 Ag1 N3 C34 -163.5(4) . . . . ? C49 Ag1 N3 C34 2.9(5) . . . . ? C48 Ag1 N3 C34 -9.9(4) . . . . ? N1 Ag1 N3 C34 164.2(3) . . . . ? C20 N1 C1 C8 6.6(8) . . . . ? Ag1 N1 C1 C8 140.7(5) . . . . ? C20 N1 C1 C2 -176.2(5) . . . . ? Ag1 N1 C1 C2 -42.1(5) . . . . ? C6 N2 C2 C3 -1.8(7) . . . . ? Ag1 N2 C2 C3 -177.0(4) . . . . ? C6 N2 C2 C1 179.6(5) . . . . ? Ag1 N2 C2 C1 4.4(6) . . . . ? N1 C1 C2 N2 30.2(7) . . . . ? C8 C1 C2 N2 -152.3(5) . . . . ? N1 C1 C2 C3 -148.4(5) . . . . ? C8 C1 C2 C3 29.1(7) . . . . ? N2 C2 C3 C4 -0.4(8) . . . . ? C1 C2 C3 C4 178.1(5) . . . . ? C2 C3 C4 C5 1.6(8) . . . . ? C3 C4 C5 C6 -0.5(8) . . . . ? C2 N2 C6 C5 3.0(7) . . . . ? Ag1 N2 C6 C5 178.2(4) . . . . ? C2 N2 C6 C7 -179.9(4) . . . . ? Ag1 N2 C6 C7 -4.8(6) . . . . ? C4 C5 C6 N2 -1.8(8) . . . . ? C4 C5 C6 C7 -178.7(5) . . . . ? C34 N3 C7 C6 167.0(4) . . . . ? Ag1 N3 C7 C6 29.3(5) . . . . ? C34 N3 C7 C14 -10.3(8) . . . . ? Ag1 N3 C7 C14 -147.9(4) . . . . ? N2 C6 C7 N3 -18.5(7) . . . . ? C5 C6 C7 N3 158.6(5) . . . . ? N2 C6 C7 C14 159.0(5) . . . . ? C5 C6 C7 C14 -24.0(7) . . . . ? N1 C1 C8 C13 -126.8(7) . . . . ? C2 C1 C8 C13 56.1(8) . . . . ? N1 C1 C8 C9 52.1(9) . . . . ? C2 C1 C8 C9 -125.1(6) . . . . ? C13 C8 C9 C10 -1.1(10) . . . . ? C1 C8 C9 C10 -179.9(6) . . . . ? C8 C9 C10 C11 1.1(12) . . . . ? C9 C10 C11 C12 0.9(14) . . . . ? C10 C11 C12 C13 -2.9(15) . . . . ? C9 C8 C13 C12 -0.9(11) . . . . ? C1 C8 C13 C12 178.0(7) . . . . ? C11 C12 C13 C8 2.9(14) . . . . ? N3 C7 C14 C19 -53.7(8) . . . . ? C6 C7 C14 C19 129.1(5) . . . . ? N3 C7 C14 C15 125.1(6) . . . . ? C6 C7 C14 C15 -52.1(8) . . . . ? C19 C14 C15 C16 0.3(10) . . . . ? C7 C14 C15 C16 -178.4(6) . . . . ? C14 C15 C16 C17 -0.1(11) . . . . ? C15 C16 C17 C18 -1.5(12) . . . . ? C16 C17 C18 C19 2.8(12) . . . . ? C15 C14 C19 C18 0.9(9) . . . . ? C7 C14 C19 C18 179.7(6) . . . . ? C17 C18 C19 C14 -2.5(10) . . . . ? C1 N1 C20 C25 57.7(7) . . . . ? Ag1 N1 C20 C25 -72.6(6) . . . . ? C1 N1 C20 C21 -129.4(6) . . . . ? Ag1 N1 C20 C21 100.3(5) . . . . ? C25 C20 C21 C22 -3.7(8) . . . . ? N1 C20 C21 C22 -176.5(5) . . . . ? C25 C20 C21 C26 178.1(5) . . . . ? N1 C20 C21 C26 5.3(9) . . . . ? C20 C21 C22 C23 4.3(10) . . . . ? C26 C21 C22 C23 -177.4(7) . . . . ? C21 C22 C23 C24 -1.5(11) . . . . ? C22 C23 C24 C25 -2.2(10) . . . . ? C22 C23 C24 C30 -178.9(6) . . . . ? C21 C20 C25 C24 0.3(9) . . . . ? N1 C20 C25 C24 173.2(5) . . . . ? C23 C24 C25 C20 2.7(9) . . . . ? C30 C24 C25 C20 179.4(6) . . . . ? C22 C21 C26 C28 -120.0(7) . . . . ? C20 C21 C26 C28 58.1(8) . . . . ? C22 C21 C26 C29 118.5(7) . . . . ? C20 C21 C26 C29 -63.5(8) . . . . ? C22 C21 C26 C27 -1.1(9) . . . . ? C20 C21 C26 C27 177.0(6) . . . . ? C23 C24 C30 C32 106.7(12) . . . . ? C25 C24 C30 C32 -69.8(12) . . . . ? C23 C24 C30 C33 -129.2(8) . . . . ? C25 C24 C30 C33 54.3(9) . . . . ? C23 C24 C30 C31 -13.1(11) . . . . ? C25 C24 C30 C31 170.4(9) . . . . ? C7 N3 C34 C39 -55.5(7) . . . . ? Ag1 N3 C34 C39 81.3(5) . . . . ? C7 N3 C34 C35 128.5(5) . . . . ? Ag1 N3 C34 C35 -94.7(5) . . . . ? C39 C34 C35 C36 2.1(8) . . . . ? N3 C34 C35 C36 178.0(5) . . . . ? C39 C34 C35 C40 -176.0(5) . . . . ? N3 C34 C35 C40 -0.2(8) . . . . ? C34 C35 C36 C37 -0.8(9) . . . . ? C40 C35 C36 C37 177.4(6) . . . . ? C35 C36 C37 C38 0.2(9) . . . . ? C36 C37 C38 C39 -0.8(8) . . . . ? C36 C37 C38 C44 -178.1(6) . . . . ? C37 C38 C39 C34 2.1(8) . . . . ? C44 C38 C39 C34 179.5(5) . . . . ? C35 C34 C39 C38 -2.9(8) . . . . ? N3 C34 C39 C38 -178.9(5) . . . . ? C36 C35 C40 C42 119.8(6) . . . . ? C34 C35 C40 C42 -62.2(7) . . . . ? C36 C35 C40 C41 -120.1(6) . . . . ? C34 C35 C40 C41 57.9(8) . . . . ? C36 C35 C40 C43 2.1(8) . . . . ? C34 C35 C40 C43 -179.8(6) . . . . ? C37 C38 C44 C47 -6.1(9) . . . . ? C39 C38 C44 C47 176.7(6) . . . . ? C37 C38 C44 C46 -128.4(8) . . . . ? C39 C38 C44 C46 54.3(9) . . . . ? C37 C38 C44 C45 113.6(8) . . . . ? C39 C38 C44 C45 -63.7(8) . . . . ? N2 Ag1 C48 C49 -130.0(4) . . . . ? N3 Ag1 C48 C49 163.1(3) . . . . ? N1 Ag1 C48 C49 -10.8(4) . . . . ? N2 Ag1 C48 C55 112.5(5) . . . . ? C49 Ag1 C48 C55 -117.5(6) . . . . ? N3 Ag1 C48 C55 45.6(4) . . . . ? N1 Ag1 C48 C55 -128.3(4) . . . . ? C55 C48 C49 C50 3.1(10) . . . . ? Ag1 C48 C49 C50 -109.7(6) . . . . ? C55 C48 C49 Ag1 112.8(5) . . . . ? N2 Ag1 C49 C48 125.8(4) . . . . ? N3 Ag1 C49 C48 -23.3(5) . . . . ? N1 Ag1 C49 C48 171.6(3) . . . . ? N2 Ag1 C49 C50 -112.0(5) . . . . ? C48 Ag1 C49 C50 122.3(6) . . . . ? N3 Ag1 C49 C50 99.0(5) . . . . ? N1 Ag1 C49 C50 -66.2(4) . . . . ? C48 C49 C50 C51 -82.7(8) . . . . ? Ag1 C49 C50 C51 -171.8(4) . . . . ? C49 C50 C51 C52 72.9(8) . . . . ? C50 C51 C52 C53 -72.2(9) . . . . ? C51 C52 C53 C54 103.3(8) . . . . ? C52 C53 C54 C55 -54.1(9) . . . . ? C49 C48 C55 C54 90.4(7) . . . . ? Ag1 C48 C55 C54 175.5(4) . . . . ? C53 C54 C55 C48 -51.8(7) . . . . ? O1 S1 C56 F3 -52.2(10) . . . . ? O3 S1 C56 F3 68.4(9) . . . . ? O2 S1 C56 F3 -175.0(8) . . . . ? O1 S1 C56 F2 -177.5(7) . . . . ? O3 S1 C56 F2 -56.9(7) . . . . ? O2 S1 C56 F2 59.7(7) . . . . ? O1 S1 C56 F1 63.6(7) . . . . ? O3 S1 C56 F1 -175.7(6) . . . . ? O2 S1 C56 F1 -59.1(7) . . . . ? C60 C61 C62 C63 84(4) . . . . ? C61 C62 C63 C64 -70(4) . . . . ? C62 C63 C64 C57 -20(6) . . . . ? C63 C64 C57 C58 81(5) . . . . ? C64 C57 C58 C59 -4(5) . . . . ? C57 C58 C59 C60 -75(4) . . . . ? C62 C61 C60 C59 -66(6) . . . . ? C58 C59 C60 C61 75(5) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 21.98 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.572 _refine_diff_density_min -0.507 _refine_diff_density_rms 0.083 data_dr020 _database_code_depnum_ccdc_archive 'CCDC 849373' #TrackingRef '- combined structures.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H64 Ag F3 N3 O3 S' _chemical_formula_weight 1000.01 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' 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 Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 32.106(3) _cell_length_b 20.658(2) _cell_length_c 19.954(2) _cell_angle_alpha 90.00 _cell_angle_beta 118.949(5) _cell_angle_gamma 90.00 _cell_volume 11581(2) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9966 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 28.14 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.147 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4184 _exptl_absorpt_coefficient_mu 0.433 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8425 _exptl_absorpt_correction_T_max 0.9787 _exptl_absorpt_process_details 'SADABS, Bruker (2003)' _exptl_special_details ; Data collection is performed with three batch runs at phi = 0.00 deg (650 frames), at phi = 120.00 deg (650 frames), and at phi = 240.00 deg (650 frames). Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 94508 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0294 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 28.54 _reflns_number_total 14448 _reflns_number_gt 10528 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, Bruker (2009)' _computing_cell_refinement 'APEX II, Bruker (2009)' _computing_data_reduction 'XPREP, Bruker (2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL, Bruker (2004)' _computing_publication_material 'SHELXTL, Bruker (2004)' _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^)+(0.1015P)^2^+6.3488P] 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 14448 _refine_ls_number_parameters 614 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0722 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1600 _refine_ls_wR_factor_gt 0.1396 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.614860(6) 0.687579(10) 0.508172(11) 0.03832(8) Uani 1 1 d . . . N1 N 0.64179(7) 0.80746(9) 0.53830(12) 0.0322(4) Uani 1 1 d . . . N2 N 0.69316(7) 0.69997(9) 0.54288(11) 0.0253(4) Uani 1 1 d . . . N3 N 0.64809(7) 0.59970(10) 0.44525(11) 0.0313(4) Uani 1 1 d . . . C1 C 0.68609(9) 0.80614(11) 0.58813(14) 0.0291(5) Uani 1 1 d . . . C2 C 0.71564(8) 0.75449(11) 0.57910(12) 0.0269(4) Uani 1 1 d . . . C3 C 0.76398(8) 0.76340(13) 0.60605(14) 0.0343(5) Uani 1 1 d . . . H3A H 0.7789 0.8025 0.6312 0.041 Uiso 1 1 calc R . . C4 C 0.79024(9) 0.71531(13) 0.59621(15) 0.0371(5) Uani 1 1 d . . . H4A H 0.8233 0.7209 0.6135 0.044 Uiso 1 1 calc R . . C5 C 0.76726(8) 0.65851(13) 0.56043(14) 0.0333(5) Uani 1 1 d . . . H5A H 0.7845 0.6240 0.5540 0.040 Uiso 1 1 calc R . . C6 C 0.71856(8) 0.65253(11) 0.53407(12) 0.0268(4) Uani 1 1 d . . . C7 C 0.69261(8) 0.59320(11) 0.49145(13) 0.0277(5) Uani 1 1 d . . . C8 C 0.71225(9) 0.85212(12) 0.65313(15) 0.0362(5) Uani 1 1 d . . . C9 C 0.74176(12) 0.82773(16) 0.72567(17) 0.0511(7) Uani 1 1 d . . . H9A H 0.7433 0.7824 0.7347 0.061 Uiso 1 1 calc R . . C10 C 0.76918(15) 0.8702(2) 0.7854(2) 0.0705(11) Uani 1 1 d . . . H10A H 0.7890 0.8537 0.8354 0.085 Uiso 1 1 calc R . . C11 C 0.76773(15) 0.9352(2) 0.7726(2) 0.0683(11) Uani 1 1 d . . . H11A H 0.7872 0.9635 0.8132 0.082 Uiso 1 1 calc R . . C12 C 0.73878(15) 0.95919(17) 0.7024(3) 0.0677(10) Uani 1 1 d . . . H12A H 0.7378 1.0046 0.6941 0.081 Uiso 1 1 calc R . . C13 C 0.71006(12) 0.91808(15) 0.6414(2) 0.0526(7) Uani 1 1 d . . . H13A H 0.6893 0.9356 0.5923 0.063 Uiso 1 1 calc R . . C14 C 0.72199(8) 0.53368(12) 0.50418(14) 0.0328(5) Uani 1 1 d . . . C15 C 0.72294(10) 0.50163(14) 0.44396(17) 0.0435(6) Uani 1 1 d . . . H15A H 0.7048 0.5175 0.3932 0.052 Uiso 1 1 calc R . . C16 C 0.75057(12) 0.44616(16) 0.4580(2) 0.0573(8) Uani 1 1 d . . . H16A H 0.7513 0.4243 0.4167 0.069 Uiso 1 1 calc R . . C17 C 0.77656(13) 0.42301(16) 0.5305(2) 0.0636(9) Uani 1 1 d . . . H17A H 0.7953 0.3851 0.5396 0.076 Uiso 1 1 calc R . . C18 C 0.77577(12) 0.45453(16) 0.5913(2) 0.0583(8) Uani 1 1 d . . . H18A H 0.7936 0.4380 0.6418 0.070 Uiso 1 1 calc R . . C19 C 0.74893(10) 0.51025(14) 0.57797(16) 0.0432(6) Uani 1 1 d . . . H19A H 0.7490 0.5325 0.6197 0.052 Uiso 1 1 calc R . . C20 C 0.60987(9) 0.84887(12) 0.54960(15) 0.0354(5) Uani 1 1 d . . . C21 C 0.57851(10) 0.89131(14) 0.49252(17) 0.0438(6) Uani 1 1 d . . . C22 C 0.54615(11) 0.92355(16) 0.5103(2) 0.0541(8) Uani 1 1 d . . . H22A H 0.5247 0.9540 0.4746 0.065 Uiso 1 1 calc R . . C23 C 0.54436(12) 0.91284(16) 0.5767(2) 0.0566(8) Uani 1 1 d . . . H23A H 0.5215 0.9355 0.5849 0.068 Uiso 1 1 calc R . . C24 C 0.57494(10) 0.86986(14) 0.63228(18) 0.0453(7) Uani 1 1 d . A . C25 C 0.60759(9) 0.83808(13) 0.61641(16) 0.0380(6) Uani 1 1 d . . . H25A H 0.6290 0.8080 0.6527 0.046 Uiso 1 1 calc R . . C26 C 0.57817(12) 0.90325(17) 0.4166(2) 0.0571(8) Uani 1 1 d . . . C27 C 0.54132(15) 0.9549(2) 0.3677(2) 0.0775(12) Uani 1 1 d . . . H27A H 0.5094 0.9404 0.3559 0.116 Uiso 1 1 calc R . . H27B H 0.5424 0.9613 0.3199 0.116 Uiso 1 1 calc R . . H27C H 0.5487 0.9958 0.3961 0.116 Uiso 1 1 calc R . . C28 C 0.56628(19) 0.8406(2) 0.3693(2) 0.0850(13) Uani 1 1 d . . . H28A H 0.5353 0.8243 0.3601 0.128 Uiso 1 1 calc R . . H28B H 0.5908 0.8081 0.3975 0.128 Uiso 1 1 calc R . . H28C H 0.5652 0.8495 0.3202 0.128 Uiso 1 1 calc R . . C29 C 0.62711(14) 0.9293(2) 0.4318(2) 0.0769(12) Uani 1 1 d . . . H29A H 0.6519 0.8976 0.4620 0.115 Uiso 1 1 calc R . . H29B H 0.6339 0.9702 0.4601 0.115 Uiso 1 1 calc R . . H29C H 0.6266 0.9367 0.3829 0.115 Uiso 1 1 calc R . . C30 C 0.57260(12) 0.85439(17) 0.7055(2) 0.0579(8) Uani 1 1 d . . . C31 C 0.5383(5) 0.9016(6) 0.7124(8) 0.102(4) Uani 0.50 1 d P A 1 H31A H 0.5138 0.9149 0.6611 0.153 Uiso 0.50 1 calc PR A 1 H31B H 0.5559 0.9398 0.7415 0.153 Uiso 0.50 1 calc PR A 1 H31C H 0.5231 0.8805 0.7390 0.153 Uiso 0.50 1 calc PR A 1 C32 C 0.6196(6) 0.8538(13) 0.7675(9) 0.156(10) Uani 0.50 1 d P A 1 H32A H 0.6315 0.8983 0.7797 0.234 Uiso 0.50 1 calc PR A 1 H32B H 0.6401 0.8286 0.7535 0.234 Uiso 0.50 1 calc PR A 1 H32C H 0.6197 0.8342 0.8123 0.234 Uiso 0.50 1 calc PR A 1 C33 C 0.5517(8) 0.7895(7) 0.6952(11) 0.129(7) Uani 0.50 1 d P A 1 H33A H 0.5181 0.7911 0.6560 0.193 Uiso 0.50 1 calc PR A 1 H33B H 0.5544 0.7746 0.7437 0.193 Uiso 0.50 1 calc PR A 1 H33C H 0.5688 0.7595 0.6789 0.193 Uiso 0.50 1 calc PR A 1 C31' C 0.5710(4) 0.9160(6) 0.7473(6) 0.085(3) Uani 0.50 1 d P A 2 H31D H 0.5436 0.9424 0.7127 0.127 Uiso 0.50 1 calc PR A 2 H31E H 0.6003 0.9408 0.7636 0.127 Uiso 0.50 1 calc PR A 2 H31F H 0.5679 0.9040 0.7923 0.127 Uiso 0.50 1 calc PR A 2 C32' C 0.6173(7) 0.8179(6) 0.7662(9) 0.077(4) Uani 0.50 1 d P A 2 H32D H 0.6209 0.7771 0.7444 0.115 Uiso 0.50 1 calc PR A 2 H32E H 0.6137 0.8087 0.8113 0.115 Uiso 0.50 1 calc PR A 2 H32F H 0.6456 0.8448 0.7812 0.115 Uiso 0.50 1 calc PR A 2 C33' C 0.5303(5) 0.8129(9) 0.6886(10) 0.115(7) Uani 0.50 1 d P A 2 H33D H 0.5012 0.8349 0.6514 0.173 Uiso 0.50 1 calc PR A 2 H33E H 0.5289 0.8053 0.7360 0.173 Uiso 0.50 1 calc PR A 2 H33F H 0.5331 0.7714 0.6674 0.173 Uiso 0.50 1 calc PR A 2 C34 C 0.61972(8) 0.54547(12) 0.40285(14) 0.0325(5) Uani 1 1 d . . . C35 C 0.58933(8) 0.55108(13) 0.32340(14) 0.0357(5) Uani 1 1 d . . . C36 C 0.56180(9) 0.49630(15) 0.28923(16) 0.0453(7) Uani 1 1 d . . . H36A H 0.5411 0.4969 0.2355 0.054 Uiso 1 1 calc R . . C37 C 0.56300(10) 0.44151(15) 0.32905(18) 0.0494(7) Uani 1 1 d . . . H37A H 0.5429 0.4062 0.3021 0.059 Uiso 1 1 calc R . . C38 C 0.59253(9) 0.43610(14) 0.40701(17) 0.0430(6) Uani 1 1 d . . . C39 C 0.62034(9) 0.49003(13) 0.44238(15) 0.0378(6) Uani 1 1 d . . . H39A H 0.6407 0.4889 0.4962 0.045 Uiso 1 1 calc R . . C40 C 0.58757(9) 0.61061(14) 0.27632(15) 0.0411(6) Uani 1 1 d . . . C41 C 0.57340(13) 0.67154(16) 0.30498(19) 0.0561(8) Uani 1 1 d . . . H41A H 0.5424 0.6646 0.3020 0.084 Uiso 1 1 calc R . . H41B H 0.5715 0.7086 0.2730 0.084 Uiso 1 1 calc R . . H41C H 0.5973 0.6802 0.3582 0.084 Uiso 1 1 calc R . . C42 C 0.63652(11) 0.62202(17) 0.28160(18) 0.0536(8) Uani 1 1 d . . . H42A H 0.6457 0.5836 0.2631 0.080 Uiso 1 1 calc R . . H42B H 0.6603 0.6303 0.3350 0.080 Uiso 1 1 calc R . . H42C H 0.6347 0.6594 0.2501 0.080 Uiso 1 1 calc R . . C43 C 0.55180(13) 0.60271(18) 0.19146(18) 0.0607(9) Uani 1 1 d . . . H43A H 0.5200 0.5949 0.1854 0.091 Uiso 1 1 calc R . . H43B H 0.5611 0.5659 0.1706 0.091 Uiso 1 1 calc R . . H43C H 0.5513 0.6422 0.1639 0.091 Uiso 1 1 calc R . . C44 C 0.59648(12) 0.37448(16) 0.4527(2) 0.0553(8) Uani 1 1 d . . . C45 C 0.64714(18) 0.3465(2) 0.4830(3) 0.0955(15) Uani 1 1 d . . . H45A H 0.6521 0.3353 0.4396 0.143 Uiso 1 1 calc R . . H45B H 0.6507 0.3076 0.5134 0.143 Uiso 1 1 calc R . . H45C H 0.6707 0.3788 0.5151 0.143 Uiso 1 1 calc R . . C46 C 0.5616(2) 0.3227(3) 0.4071(4) 0.138(3) Uani 1 1 d . . . H46A H 0.5652 0.3119 0.3623 0.206 Uiso 1 1 calc R . . H46B H 0.5292 0.3383 0.3901 0.206 Uiso 1 1 calc R . . H46C H 0.5676 0.2841 0.4390 0.206 Uiso 1 1 calc R . . C47 C 0.5918(2) 0.3903(3) 0.5237(3) 0.1018(17) Uani 1 1 d . . . H47A H 0.5602 0.4086 0.5078 0.153 Uiso 1 1 calc R . . H47B H 0.6162 0.4218 0.5555 0.153 Uiso 1 1 calc R . . H47C H 0.5958 0.3506 0.5532 0.153 Uiso 1 1 calc R . . C48 C 0.50919(12) 0.74848(19) 0.4678(3) 0.0769(12) Uani 1 1 d . . . H48A H 0.4769 0.7410 0.4593 0.115 Uiso 1 1 calc R . . H48B H 0.5077 0.7678 0.4218 0.115 Uiso 1 1 calc R . . H48C H 0.5259 0.7780 0.5112 0.115 Uiso 1 1 calc R . . C49 C 0.53497(10) 0.68646(17) 0.4845(2) 0.0499(7) Uani 1 1 d . . . C50 C 0.54708(10) 0.63149(17) 0.49564(18) 0.0491(7) Uani 1 1 d . . . C51 C 0.55314(14) 0.56106(18) 0.5080(3) 0.0693(10) Uani 1 1 d . . . H51A H 0.5235 0.5420 0.5016 0.104 Uiso 1 1 calc R . . H51B H 0.5789 0.5524 0.5599 0.104 Uiso 1 1 calc R . . H51C H 0.5611 0.5419 0.4706 0.104 Uiso 1 1 calc R . . C52 C 0.64360(14) 0.60161(18) 0.7351(2) 0.0594(8) Uani 1 1 d . . . F1 F 0.59773(9) 0.60928(16) 0.68523(15) 0.0955(8) Uani 1 1 d . . . F2 F 0.65146(11) 0.63351(15) 0.79704(14) 0.1015(9) Uani 1 1 d . . . F3 F 0.65054(12) 0.53981(13) 0.75308(19) 0.1072(10) Uani 1 1 d . . . S2 S 0.68109(3) 0.62961(4) 0.69602(4) 0.04422(17) Uani 1 1 d . . . O1 O 0.66715(11) 0.69538(10) 0.67692(16) 0.0643(7) Uani 1 1 d . . . O2 O 0.66855(9) 0.58756(11) 0.63174(14) 0.0604(6) Uani 1 1 d . . . O3 O 0.72797(10) 0.61973(15) 0.75813(16) 0.0763(7) Uani 1 1 d . . . C53 C 0.75370(18) 0.2475(2) 0.5321(2) 0.0785(12) Uani 1 1 d . . . C54 C 0.7588(3) 0.2426(4) 0.6059(4) 0.135(2) Uani 1 1 d . . . H54A H 0.7576 0.2859 0.6248 0.203 Uiso 1 1 calc R . . H54B H 0.7895 0.2224 0.6403 0.203 Uiso 1 1 calc R . . H54C H 0.7330 0.2161 0.6040 0.203 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02371(11) 0.04399(14) 0.04730(13) -0.00488(8) 0.01722(9) -0.00398(7) N1 0.0289(10) 0.0290(11) 0.0411(11) 0.0001(8) 0.0188(9) 0.0027(8) N2 0.0223(9) 0.0276(10) 0.0278(9) 0.0003(7) 0.0135(7) -0.0006(7) N3 0.0273(9) 0.0327(11) 0.0315(9) -0.0035(8) 0.0125(8) -0.0032(8) C1 0.0302(11) 0.0251(12) 0.0362(12) -0.0020(9) 0.0193(10) -0.0017(9) C2 0.0246(10) 0.0281(11) 0.0289(10) 0.0000(9) 0.0135(8) -0.0014(9) C3 0.0278(11) 0.0337(13) 0.0420(13) -0.0075(10) 0.0174(10) -0.0084(10) C4 0.0234(11) 0.0398(14) 0.0470(14) -0.0069(11) 0.0162(10) -0.0030(10) C5 0.0255(11) 0.0361(13) 0.0385(12) -0.0032(10) 0.0156(10) 0.0017(10) C6 0.0258(10) 0.0286(12) 0.0272(10) -0.0011(9) 0.0139(9) 0.0010(9) C7 0.0268(11) 0.0292(12) 0.0303(10) -0.0007(9) 0.0163(9) -0.0009(9) C8 0.0371(13) 0.0319(13) 0.0468(14) -0.0125(11) 0.0260(11) -0.0065(10) C9 0.0582(19) 0.0489(17) 0.0453(15) -0.0137(13) 0.0245(14) -0.0117(14) C10 0.074(2) 0.085(3) 0.0490(18) -0.0277(18) 0.0271(17) -0.023(2) C11 0.076(2) 0.071(3) 0.072(2) -0.044(2) 0.047(2) -0.031(2) C12 0.079(2) 0.0409(18) 0.102(3) -0.0318(19) 0.059(2) -0.0243(17) C13 0.0570(19) 0.0345(15) 0.073(2) -0.0103(14) 0.0372(17) -0.0084(13) C14 0.0283(11) 0.0269(12) 0.0434(13) -0.0033(10) 0.0176(10) -0.0011(9) C15 0.0415(14) 0.0403(15) 0.0499(15) -0.0116(12) 0.0231(12) -0.0002(12) C16 0.0595(19) 0.0411(17) 0.079(2) -0.0155(16) 0.0393(18) 0.0051(15) C17 0.059(2) 0.0358(17) 0.100(3) 0.0039(17) 0.042(2) 0.0152(15) C18 0.0539(18) 0.0458(18) 0.073(2) 0.0176(16) 0.0292(17) 0.0153(15) C19 0.0429(15) 0.0407(15) 0.0470(15) 0.0042(12) 0.0226(12) 0.0057(12) C20 0.0308(12) 0.0278(12) 0.0511(14) -0.0009(10) 0.0226(11) 0.0031(10) C21 0.0407(14) 0.0364(15) 0.0590(17) 0.0050(12) 0.0278(13) 0.0069(11) C22 0.0433(16) 0.0449(17) 0.078(2) 0.0122(15) 0.0320(16) 0.0191(13) C23 0.0510(18) 0.0474(18) 0.088(2) 0.0001(16) 0.0472(18) 0.0128(14) C24 0.0446(15) 0.0383(15) 0.0660(18) -0.0073(13) 0.0371(14) -0.0014(12) C25 0.0346(13) 0.0307(13) 0.0542(15) -0.0014(11) 0.0258(12) 0.0018(10) C26 0.0556(19) 0.057(2) 0.0621(19) 0.0192(16) 0.0309(16) 0.0219(15) C27 0.064(2) 0.088(3) 0.078(2) 0.038(2) 0.033(2) 0.036(2) C28 0.113(4) 0.083(3) 0.059(2) 0.011(2) 0.042(2) 0.024(3) C29 0.065(2) 0.099(3) 0.085(3) 0.044(2) 0.051(2) 0.028(2) C30 0.0573(19) 0.061(2) 0.075(2) -0.0048(17) 0.0480(18) 0.0038(16) C31 0.138(10) 0.116(9) 0.107(9) 0.014(7) 0.102(8) 0.033(9) C32 0.066(7) 0.35(3) 0.051(6) -0.030(14) 0.030(5) -0.004(16) C33 0.23(2) 0.084(8) 0.154(13) 0.009(8) 0.162(16) -0.025(11) C31' 0.099(7) 0.093(7) 0.073(6) -0.020(5) 0.050(6) 0.031(6) C32' 0.112(10) 0.074(6) 0.074(7) 0.017(5) 0.068(7) 0.023(6) C33' 0.101(9) 0.173(18) 0.110(9) -0.047(10) 0.081(8) -0.071(10) C34 0.0244(11) 0.0348(13) 0.0363(12) -0.0069(10) 0.0132(9) -0.0026(9) C35 0.0247(11) 0.0402(14) 0.0381(12) -0.0060(10) 0.0121(10) -0.0019(10) C36 0.0296(13) 0.0522(17) 0.0430(14) -0.0109(13) 0.0089(11) -0.0072(12) C37 0.0330(13) 0.0451(17) 0.0594(17) -0.0135(14) 0.0139(13) -0.0130(12) C38 0.0337(13) 0.0385(15) 0.0575(16) -0.0066(12) 0.0224(12) -0.0069(11) C39 0.0315(12) 0.0391(14) 0.0422(13) -0.0034(11) 0.0174(11) -0.0058(10) C40 0.0342(13) 0.0446(16) 0.0366(13) -0.0005(11) 0.0108(10) -0.0018(11) C41 0.0567(19) 0.0493(18) 0.0517(17) 0.0066(14) 0.0178(15) 0.0115(15) C42 0.0453(16) 0.059(2) 0.0536(17) 0.0090(15) 0.0218(14) -0.0079(14) C43 0.0571(19) 0.064(2) 0.0408(15) 0.0038(15) 0.0081(14) 0.0011(17) C44 0.0543(18) 0.0396(17) 0.076(2) 0.0019(15) 0.0345(17) -0.0098(14) C45 0.087(3) 0.073(3) 0.125(4) 0.035(3) 0.051(3) 0.014(3) C46 0.132(5) 0.081(4) 0.134(5) 0.015(3) 0.012(4) -0.062(4) C47 0.142(5) 0.078(3) 0.118(4) 0.020(3) 0.089(4) -0.005(3) C48 0.0405(17) 0.058(2) 0.125(3) -0.013(2) 0.034(2) -0.0016(16) C49 0.0277(13) 0.058(2) 0.0611(18) -0.0130(15) 0.0194(13) -0.0082(13) C50 0.0299(13) 0.055(2) 0.0639(18) -0.0108(15) 0.0244(13) -0.0101(13) C51 0.055(2) 0.053(2) 0.107(3) -0.007(2) 0.045(2) -0.0140(16) C52 0.070(2) 0.063(2) 0.0540(18) 0.0165(16) 0.0373(17) 0.0054(17) F1 0.0611(14) 0.153(3) 0.0851(16) 0.0225(16) 0.0451(13) 0.0041(15) F2 0.133(2) 0.130(2) 0.0752(15) -0.0087(15) 0.0769(17) -0.0169(19) F3 0.140(2) 0.0698(16) 0.150(2) 0.0468(16) 0.100(2) 0.0070(16) S2 0.0519(4) 0.0377(4) 0.0486(4) 0.0097(3) 0.0286(3) 0.0051(3) O1 0.097(2) 0.0382(12) 0.0814(17) 0.0182(11) 0.0625(16) 0.0158(11) O2 0.0741(16) 0.0553(14) 0.0651(14) -0.0081(11) 0.0441(13) -0.0061(11) O3 0.0572(15) 0.0852(19) 0.0739(16) 0.0131(14) 0.0217(13) 0.0043(14) C53 0.099(3) 0.048(2) 0.083(3) -0.004(2) 0.039(3) 0.009(2) C54 0.173(7) 0.122(5) 0.099(4) 0.010(4) 0.056(4) 0.024(5) _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 N2 2.2757(19) . ? Ag1 C50 2.369(3) . ? Ag1 C49 2.373(3) . ? Ag1 N1 2.596(2) . ? N1 C1 1.282(3) . ? N1 C20 1.434(3) . ? N2 C6 1.340(3) . ? N2 C2 1.344(3) . ? N3 C7 1.279(3) . ? N3 C34 1.433(3) . ? C1 C2 1.496(3) . ? C1 C8 1.495(3) . ? C2 C3 1.387(3) . ? C3 C4 1.377(4) . ? C4 C5 1.386(4) . ? C5 C6 1.393(3) . ? C6 C7 1.494(3) . ? C7 C14 1.495(3) . ? C8 C13 1.379(4) . ? C8 C9 1.385(4) . ? C9 C10 1.395(4) . ? C10 C11 1.363(6) . ? C11 C12 1.345(6) . ? C12 C13 1.403(5) . ? C14 C15 1.385(4) . ? C14 C19 1.385(4) . ? C15 C16 1.392(4) . ? C16 C17 1.360(5) . ? C17 C18 1.386(5) . ? C18 C19 1.384(4) . ? C20 C25 1.388(4) . ? C20 C21 1.403(4) . ? C21 C22 1.416(4) . ? C21 C26 1.529(4) . ? C22 C23 1.372(5) . ? C23 C24 1.389(5) . ? C24 C25 1.397(4) . ? C24 C30 1.532(4) . ? C26 C28 1.537(6) . ? C26 C29 1.546(5) . ? C26 C27 1.540(4) . ? C30 C33 1.468(16) . ? C30 C32 1.414(16) . ? C30 C33' 1.500(13) . ? C30 C31' 1.536(9) . ? C30 C32' 1.554(17) . ? C30 C31 1.527(11) . ? C34 C39 1.385(4) . ? C34 C35 1.408(3) . ? C35 C36 1.394(4) . ? C35 C40 1.532(4) . ? C36 C37 1.373(4) . ? C37 C38 1.380(4) . ? C38 C39 1.388(4) . ? C38 C44 1.534(4) . ? C40 C43 1.526(4) . ? C40 C41 1.539(4) . ? C40 C42 1.541(4) . ? C44 C46 1.496(6) . ? C44 C47 1.531(6) . ? C44 C45 1.548(6) . ? C48 C49 1.473(5) . ? C49 C50 1.186(4) . ? C50 C51 1.473(5) . ? C52 F3 1.315(4) . ? C52 F2 1.312(4) . ? C52 F1 1.329(4) . ? C52 S2 1.817(3) . ? S2 O1 1.424(2) . ? S2 O2 1.436(2) . ? S2 O3 1.427(3) . ? C53 C53 1.189(9) 7_656 ? C53 C54 1.403(7) . ? 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 N2 Ag1 C50 155.49(10) . . ? N2 Ag1 C49 171.94(9) . . ? C50 Ag1 C49 28.96(10) . . ? N2 Ag1 N1 68.11(7) . . ? C50 Ag1 N1 132.61(9) . . ? C49 Ag1 N1 105.20(9) . . ? C1 N1 C20 120.0(2) . . ? C1 N1 Ag1 106.23(15) . . ? C20 N1 Ag1 114.97(15) . . ? C6 N2 C2 118.73(19) . . ? C6 N2 Ag1 122.06(15) . . ? C2 N2 Ag1 118.98(14) . . ? C7 N3 C34 120.8(2) . . ? N1 C1 C2 116.9(2) . . ? N1 C1 C8 127.3(2) . . ? C2 C1 C8 115.8(2) . . ? N2 C2 C3 121.9(2) . . ? N2 C2 C1 117.11(19) . . ? C3 C2 C1 121.0(2) . . ? C4 C3 C2 119.8(2) . . ? C3 C4 C5 118.3(2) . . ? C6 C5 C4 119.3(2) . . ? N2 C6 C5 121.9(2) . . ? N2 C6 C7 117.86(19) . . ? C5 C6 C7 120.2(2) . . ? N3 C7 C14 127.0(2) . . ? N3 C7 C6 116.4(2) . . ? C14 C7 C6 116.47(19) . . ? C13 C8 C9 119.3(3) . . ? C13 C8 C1 121.3(3) . . ? C9 C8 C1 119.2(2) . . ? C10 C9 C8 119.5(3) . . ? C11 C10 C9 120.6(4) . . ? C12 C11 C10 120.1(3) . . ? C11 C12 C13 120.8(3) . . ? C8 C13 C12 119.5(3) . . ? C15 C14 C19 119.4(2) . . ? C15 C14 C7 121.5(2) . . ? C19 C14 C7 119.1(2) . . ? C14 C15 C16 119.9(3) . . ? C17 C16 C15 120.5(3) . . ? C16 C17 C18 120.2(3) . . ? C17 C18 C19 119.7(3) . . ? C18 C19 C14 120.3(3) . . ? C25 C20 C21 121.9(2) . . ? C25 C20 N1 115.4(2) . . ? C21 C20 N1 122.1(2) . . ? C20 C21 C22 114.6(3) . . ? C20 C21 C26 124.2(2) . . ? C22 C21 C26 121.2(3) . . ? C23 C22 C21 123.0(3) . . ? C22 C23 C24 122.1(3) . . ? C23 C24 C25 115.9(3) . . ? C23 C24 C30 123.6(3) . . ? C25 C24 C30 120.4(3) . . ? C20 C25 C24 122.4(3) . . ? C28 C26 C21 110.7(3) . . ? C28 C26 C29 109.9(3) . . ? C21 C26 C29 110.0(3) . . ? C28 C26 C27 107.9(3) . . ? C21 C26 C27 112.0(3) . . ? C29 C26 C27 106.2(3) . . ? C33 C30 C32 109.6(14) . . ? C33 C30 C33' 31.2(9) . . ? C32 C30 C33' 131.1(12) . . ? C33 C30 C31' 134.3(8) . . ? C32 C30 C31' 80.4(11) . . ? C33' C30 C31' 109.2(8) . . ? C33 C30 C32' 81.5(10) . . ? C32 C30 C32' 28.6(12) . . ? C33' C30 C32' 107.0(10) . . ? C31' C30 C32' 103.9(7) . . ? C33 C30 C24 106.7(6) . . ? C32 C30 C24 108.2(8) . . ? C33' C30 C24 111.3(7) . . ? C31' C30 C24 112.1(5) . . ? C32' C30 C24 113.1(6) . . ? C33 C30 C31 107.2(9) . . ? C32 C30 C31 115.9(11) . . ? C33' C30 C31 76.7(9) . . ? C31' C30 C31 37.4(6) . . ? C32' C30 C31 132.4(8) . . ? C24 C30 C31 108.9(5) . . ? C39 C34 C35 121.4(2) . . ? C39 C34 N3 118.7(2) . . ? C35 C34 N3 119.8(2) . . ? C36 C35 C34 114.4(2) . . ? C36 C35 C40 121.7(2) . . ? C34 C35 C40 123.8(2) . . ? C37 C36 C35 123.5(3) . . ? C36 C37 C38 122.1(3) . . ? C37 C38 C39 115.5(3) . . ? C37 C38 C44 123.4(3) . . ? C39 C38 C44 121.1(3) . . ? C34 C39 C38 123.1(3) . . ? C43 C40 C35 112.3(2) . . ? C43 C40 C41 107.5(3) . . ? C35 C40 C41 111.0(2) . . ? C43 C40 C42 106.7(3) . . ? C35 C40 C42 110.3(2) . . ? C41 C40 C42 108.9(3) . . ? C46 C44 C47 109.6(4) . . ? C46 C44 C38 114.1(3) . . ? C47 C44 C38 110.8(3) . . ? C46 C44 C45 107.8(4) . . ? C47 C44 C45 105.9(4) . . ? C38 C44 C45 108.1(3) . . ? C50 C49 C48 166.5(3) . . ? C50 C49 Ag1 75.4(2) . . ? C48 C49 Ag1 118.1(2) . . ? C49 C50 C51 169.1(3) . . ? C49 C50 Ag1 75.7(2) . . ? C51 C50 Ag1 115.2(2) . . ? F3 C52 F2 107.5(3) . . ? F3 C52 F1 107.5(3) . . ? F2 C52 F1 106.5(3) . . ? F3 C52 S2 111.4(3) . . ? F2 C52 S2 112.3(3) . . ? F1 C52 S2 111.4(2) . . ? O1 S2 O2 114.98(16) . . ? O1 S2 O3 115.58(18) . . ? O2 S2 O3 114.27(17) . . ? O1 S2 C52 103.36(16) . . ? O2 S2 C52 103.50(16) . . ? O3 S2 C52 102.77(17) . . ? C53 C53 C54 175.7(7) 7_656 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ag1 N1 C1 -29.31(15) . . . . ? C50 Ag1 N1 C1 135.00(18) . . . . ? C49 Ag1 N1 C1 145.93(17) . . . . ? N2 Ag1 N1 C20 -164.52(19) . . . . ? C50 Ag1 N1 C20 -0.2(2) . . . . ? C49 Ag1 N1 C20 10.7(2) . . . . ? C50 Ag1 N2 C6 40.3(3) . . . . ? C49 Ag1 N2 C6 156.9(7) . . . . ? N1 Ag1 N2 C6 -168.36(18) . . . . ? C50 Ag1 N2 C2 -134.1(2) . . . . ? C49 Ag1 N2 C2 -17.5(8) . . . . ? N1 Ag1 N2 C2 17.25(15) . . . . ? C20 N1 C1 C2 170.5(2) . . . . ? Ag1 N1 C1 C2 38.0(2) . . . . ? C20 N1 C1 C8 -12.0(4) . . . . ? Ag1 N1 C1 C8 -144.5(2) . . . . ? C6 N2 C2 C3 1.3(3) . . . . ? Ag1 N2 C2 C3 175.90(17) . . . . ? C6 N2 C2 C1 -179.7(2) . . . . ? Ag1 N2 C2 C1 -5.1(3) . . . . ? N1 C1 C2 N2 -26.5(3) . . . . ? C8 C1 C2 N2 155.7(2) . . . . ? N1 C1 C2 C3 152.5(2) . . . . ? C8 C1 C2 C3 -25.3(3) . . . . ? N2 C2 C3 C4 -0.3(4) . . . . ? C1 C2 C3 C4 -179.3(2) . . . . ? C2 C3 C4 C5 -1.1(4) . . . . ? C3 C4 C5 C6 1.6(4) . . . . ? C2 N2 C6 C5 -0.8(3) . . . . ? Ag1 N2 C6 C5 -175.22(17) . . . . ? C2 N2 C6 C7 -178.09(19) . . . . ? Ag1 N2 C6 C7 7.5(3) . . . . ? C4 C5 C6 N2 -0.7(4) . . . . ? C4 C5 C6 C7 176.6(2) . . . . ? C34 N3 C7 C14 5.1(4) . . . . ? C34 N3 C7 C6 -178.6(2) . . . . ? N2 C6 C7 N3 23.0(3) . . . . ? C5 C6 C7 N3 -154.3(2) . . . . ? N2 C6 C7 C14 -160.3(2) . . . . ? C5 C6 C7 C14 22.4(3) . . . . ? N1 C1 C8 C13 -52.5(4) . . . . ? C2 C1 C8 C13 125.0(3) . . . . ? N1 C1 C8 C9 131.9(3) . . . . ? C2 C1 C8 C9 -50.6(3) . . . . ? C13 C8 C9 C10 -0.8(5) . . . . ? C1 C8 C9 C10 174.9(3) . . . . ? C8 C9 C10 C11 -1.1(5) . . . . ? C9 C10 C11 C12 1.8(6) . . . . ? C10 C11 C12 C13 -0.6(6) . . . . ? C9 C8 C13 C12 1.9(5) . . . . ? C1 C8 C13 C12 -173.7(3) . . . . ? C11 C12 C13 C8 -1.3(5) . . . . ? N3 C7 C14 C15 53.6(4) . . . . ? C6 C7 C14 C15 -122.7(3) . . . . ? N3 C7 C14 C19 -126.6(3) . . . . ? C6 C7 C14 C19 57.1(3) . . . . ? C19 C14 C15 C16 0.5(4) . . . . ? C7 C14 C15 C16 -179.7(3) . . . . ? C14 C15 C16 C17 0.2(5) . . . . ? C15 C16 C17 C18 0.0(5) . . . . ? C16 C17 C18 C19 -0.9(5) . . . . ? C17 C18 C19 C14 1.6(5) . . . . ? C15 C14 C19 C18 -1.4(4) . . . . ? C7 C14 C19 C18 178.8(3) . . . . ? C1 N1 C20 C25 -58.5(3) . . . . ? Ag1 N1 C20 C25 70.1(3) . . . . ? C1 N1 C20 C21 129.6(3) . . . . ? Ag1 N1 C20 C21 -101.7(2) . . . . ? C25 C20 C21 C22 2.4(4) . . . . ? N1 C20 C21 C22 173.7(3) . . . . ? C25 C20 C21 C26 -177.7(3) . . . . ? N1 C20 C21 C26 -6.4(4) . . . . ? C20 C21 C22 C23 -2.0(5) . . . . ? C26 C21 C22 C23 178.1(3) . . . . ? C21 C22 C23 C24 1.0(6) . . . . ? C22 C23 C24 C25 -0.1(5) . . . . ? C22 C23 C24 C30 -177.2(3) . . . . ? C21 C20 C25 C24 -1.7(4) . . . . ? N1 C20 C25 C24 -173.6(2) . . . . ? C23 C24 C25 C20 0.5(4) . . . . ? C30 C24 C25 C20 177.7(3) . . . . ? C20 C21 C26 C28 62.3(4) . . . . ? C22 C21 C26 C28 -117.8(4) . . . . ? C20 C21 C26 C29 -59.3(4) . . . . ? C22 C21 C26 C29 120.6(3) . . . . ? C20 C21 C26 C27 -177.2(3) . . . . ? C22 C21 C26 C27 2.7(5) . . . . ? C23 C24 C30 C33 105.6(9) . . . . ? C25 C24 C30 C33 -71.3(9) . . . . ? C23 C24 C30 C32 -136.5(11) . . . . ? C25 C24 C30 C32 46.6(12) . . . . ? C23 C24 C30 C33' 73.0(9) . . . . ? C25 C24 C30 C33' -104.0(8) . . . . ? C23 C24 C30 C31' -49.7(6) . . . . ? C25 C24 C30 C31' 133.4(6) . . . . ? C23 C24 C30 C32' -166.6(7) . . . . ? C25 C24 C30 C32' 16.4(7) . . . . ? C23 C24 C30 C31 -9.7(8) . . . . ? C25 C24 C30 C31 173.3(7) . . . . ? C7 N3 C34 C39 53.6(3) . . . . ? C7 N3 C34 C35 -131.1(2) . . . . ? C39 C34 C35 C36 -1.7(4) . . . . ? N3 C34 C35 C36 -176.9(2) . . . . ? C39 C34 C35 C40 -179.0(2) . . . . ? N3 C34 C35 C40 5.8(4) . . . . ? C34 C35 C36 C37 1.3(4) . . . . ? C40 C35 C36 C37 178.7(3) . . . . ? C35 C36 C37 C38 -1.0(5) . . . . ? C36 C37 C38 C39 0.9(4) . . . . ? C36 C37 C38 C44 -177.0(3) . . . . ? C35 C34 C39 C38 1.8(4) . . . . ? N3 C34 C39 C38 177.0(2) . . . . ? C37 C38 C39 C34 -1.3(4) . . . . ? C44 C38 C39 C34 176.7(3) . . . . ? C36 C35 C40 C43 2.1(4) . . . . ? C34 C35 C40 C43 179.2(3) . . . . ? C36 C35 C40 C41 122.4(3) . . . . ? C34 C35 C40 C41 -60.5(3) . . . . ? C36 C35 C40 C42 -116.8(3) . . . . ? C34 C35 C40 C42 60.3(3) . . . . ? C37 C38 C44 C46 -6.3(6) . . . . ? C39 C38 C44 C46 175.9(4) . . . . ? C37 C38 C44 C47 -130.7(4) . . . . ? C39 C38 C44 C47 51.5(4) . . . . ? C37 C38 C44 C45 113.6(4) . . . . ? C39 C38 C44 C45 -64.2(4) . . . . ? N2 Ag1 C49 C50 -130.0(6) . . . . ? N1 Ag1 C49 C50 -163.3(2) . . . . ? N2 Ag1 C49 C48 50.4(9) . . . . ? C50 Ag1 C49 C48 -179.6(4) . . . . ? N1 Ag1 C49 C48 17.2(3) . . . . ? C48 C49 C50 C51 -5(3) . . . . ? Ag1 C49 C50 C51 177(2) . . . . ? C48 C49 C50 Ag1 178(100) . . . . ? N2 Ag1 C50 C49 165.0(2) . . . . ? N1 Ag1 C50 C49 22.2(3) . . . . ? N2 Ag1 C50 C51 -14.3(4) . . . . ? C49 Ag1 C50 C51 -179.3(4) . . . . ? N1 Ag1 C50 C51 -157.1(2) . . . . ? F3 C52 S2 O1 177.3(3) . . . . ? F2 C52 S2 O1 -62.0(3) . . . . ? F1 C52 S2 O1 57.3(3) . . . . ? F3 C52 S2 O2 57.1(3) . . . . ? F2 C52 S2 O2 177.8(3) . . . . ? F1 C52 S2 O2 -62.9(3) . . . . ? F3 C52 S2 O3 -62.1(3) . . . . ? F2 C52 S2 O3 58.6(3) . . . . ? F1 C52 S2 O3 177.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 28.54 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.095 _refine_diff_density_min -0.493 _refine_diff_density_rms 0.113