# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Yu-Bin Dong' _publ_contact_author_email yubindong@sdnu.edu.cn _publ_author_name 'Yu-Bin Dong' data_1 _database_code_depnum_ccdc_archive 'CCDC 791137' #TrackingRef '- CIF_1.1.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H29 Ag F6 N4 O3 P' _chemical_formula_weight 854.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Pban loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x+1/2, y, -z' 'x, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x-1/2, -y, z' '-x, y-1/2, z' _cell_length_a 16.936(3) _cell_length_b 13.756(2) _cell_length_c 15.609(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3636.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2402 _cell_measurement_theta_min 2.311 _cell_measurement_theta_max 20.856 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.561 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1724 _exptl_absorpt_coefficient_mu 0.673 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4086 _exptl_absorpt_correction_T_max 0.5074 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13999 _diffrn_reflns_av_R_equivalents 0.0551 _diffrn_reflns_av_sigmaI/netI 0.0425 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.03 _reflns_number_total 3226 _reflns_number_gt 2260 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0892P)^2^+2.4561P] 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 3226 _refine_ls_number_parameters 240 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0961 _refine_ls_R_factor_gt 0.0671 _refine_ls_wR_factor_ref 0.1815 _refine_ls_wR_factor_gt 0.1617 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.7500 0.2500 0.38717(4) 0.0653(3) Uani 1 2 d S . . C1 C 0.9394(3) 0.2348(3) 0.4326(3) 0.0408(11) Uani 1 1 d . . . C2 C 0.9748(3) 0.2173(4) 0.3493(3) 0.0416(11) Uani 1 1 d . . . C3 C 1.0549(3) 0.2391(4) 0.3385(4) 0.0591(15) Uani 1 1 d . . . H3 H 1.0838 0.2653 0.3836 0.071 Uiso 1 1 calc R . . C4 C 1.0907(4) 0.2218(5) 0.2608(4) 0.0721(18) Uani 1 1 d . . . H4 H 1.1440 0.2359 0.2537 0.087 Uiso 1 1 calc R . . C5 C 1.0484(4) 0.1841(5) 0.1943(3) 0.077(2) Uani 1 1 d . . . H5 H 1.0732 0.1733 0.1419 0.093 Uiso 1 1 calc R . . C6 C 0.9701(3) 0.1617(5) 0.2034(3) 0.0640(16) Uani 1 1 d . . . H6 H 0.9422 0.1353 0.1576 0.077 Uiso 1 1 calc R . . C7 C 0.9322(3) 0.1784(4) 0.2808(3) 0.0454(12) Uani 1 1 d . . . C8 C 0.8173(3) 0.0854(4) 0.2423(3) 0.0617(15) Uani 1 1 d . . . H8A H 0.8478 0.0258 0.2430 0.074 Uiso 1 1 calc R . . H8B H 0.8134 0.1080 0.1836 0.074 Uiso 1 1 calc R . . C9 C 0.7363(3) 0.0677(4) 0.2787(3) 0.0524(13) Uani 1 1 d . . . C10 C 0.7265(4) 0.0276(5) 0.3597(4) 0.0656(16) Uani 1 1 d . . . H10 H 0.7707 0.0107 0.3917 0.079 Uiso 1 1 calc R . . C11 C 0.6525(4) 0.0124(4) 0.3932(4) 0.0650(16) Uani 1 1 d . . . H11 H 0.6467 -0.0135 0.4478 0.078 Uiso 1 1 calc R . . C12 C 0.5871(3) 0.0358(4) 0.3451(3) 0.0551(13) Uani 1 1 d . . . C13 C 0.5953(3) 0.0749(4) 0.2638(4) 0.0658(16) Uani 1 1 d . . . H13 H 0.5510 0.0901 0.2314 0.079 Uiso 1 1 calc R . . C14 C 0.6700(3) 0.0909(5) 0.2315(3) 0.0657(16) Uani 1 1 d . . . H14 H 0.6757 0.1177 0.1772 0.079 Uiso 1 1 calc R . . C15 C 0.5080(4) 0.0218(4) 0.3791(4) 0.0668(18) Uani 1 1 d . . . C16 C 0.5804(12) 0.4864(16) 1.0044(10) 0.171(7) Uani 1 1 d . . . H16 H 0.6347 0.4763 1.0074 0.205 Uiso 1 1 calc R . . C17 C 0.5315(12) 0.4177(13) 0.9699(8) 0.166(7) Uani 1 1 d . . . H17 H 0.5535 0.3607 0.9486 0.199 Uiso 1 1 calc R . . C18 C 0.4527(10) 0.4295(11) 0.9655(7) 0.160(5) Uani 1 1 d . . . H18 H 0.4211 0.3809 0.9423 0.192 Uiso 1 1 calc R . . C19 C 0.2500 0.2500 0.9134(7) 0.233(11) Uiso 1 2 d SD . . H19 H 0.2500 0.2500 0.8538 0.280 Uiso 1 2 calc SR . . C20 C 0.2508(12) 0.3368(4) 0.9561(2) 0.332(15) Uiso 1 1 d D . . H20 H 0.2525 0.3950 0.9259 0.399 Uiso 1 1 calc R . . F1 F 0.6841(3) 0.2495(3) 0.9297(3) 0.1258(18) Uani 1 1 d . . . F2 F 0.7500 0.1357(4) 1.0000 0.113(2) Uani 1 2 d S . . F3 F 0.2500 0.2500 0.6011(4) 0.117(3) Uani 1 2 d S . . F4 F 0.3157(4) 0.1715(4) 0.4989(3) 0.145(2) Uani 1 1 d . . . N1 N 0.8661(2) 0.2397(3) 0.4562(2) 0.0450(10) Uani 1 1 d . . . N2 N 0.4460(4) 0.0127(4) 0.4057(4) 0.0850(17) Uani 1 1 d . . . O1 O 0.9883(3) 0.2500 0.5000 0.0445(11) Uani 1 2 d S . . O2 O 0.85444(19) 0.1579(3) 0.29497(19) 0.0519(9) Uani 1 1 d . . . P1 P 0.7500 0.2500 1.0000 0.0684(9) Uani 1 4 d S . . P2 P 0.2500 0.2500 0.5000 0.0601(8) Uani 1 4 d S . . 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 0.0375(4) 0.1072(6) 0.0511(4) 0.000 0.000 0.0115(3) C1 0.039(3) 0.041(3) 0.042(2) -0.005(2) -0.003(2) 0.000(2) C2 0.037(2) 0.048(3) 0.041(2) -0.002(2) 0.006(2) 0.003(2) C3 0.050(3) 0.082(4) 0.046(3) -0.008(3) 0.003(3) -0.001(3) C4 0.049(3) 0.112(5) 0.056(3) -0.011(3) 0.013(3) -0.002(3) C5 0.066(4) 0.121(6) 0.044(3) -0.013(4) 0.018(3) -0.005(4) C6 0.059(3) 0.095(5) 0.037(3) -0.014(3) 0.004(3) -0.005(3) C7 0.044(3) 0.054(3) 0.038(2) -0.004(2) -0.003(2) 0.002(2) C8 0.062(3) 0.073(4) 0.050(3) -0.014(3) -0.006(3) -0.012(3) C9 0.058(3) 0.052(3) 0.047(3) -0.004(3) -0.006(2) -0.013(3) C10 0.063(4) 0.073(4) 0.061(3) 0.016(3) -0.011(3) 0.002(3) C11 0.069(4) 0.069(4) 0.057(3) 0.014(3) 0.001(3) -0.006(3) C12 0.062(3) 0.046(3) 0.057(3) -0.004(3) -0.005(3) -0.010(3) C13 0.064(4) 0.077(4) 0.057(3) 0.005(3) -0.012(3) -0.010(3) C14 0.068(4) 0.084(4) 0.045(3) 0.010(3) -0.009(3) -0.014(3) C15 0.079(5) 0.054(4) 0.067(4) -0.002(3) -0.002(3) -0.015(3) C16 0.180(16) 0.211(19) 0.123(11) 0.076(11) 0.048(10) 0.075(14) C17 0.208(17) 0.189(15) 0.101(9) 0.064(9) 0.082(10) 0.111(13) C18 0.193(15) 0.175(13) 0.112(7) 0.034(8) 0.061(8) 0.067(10) F1 0.141(4) 0.135(4) 0.101(3) 0.005(3) -0.047(3) -0.001(3) F2 0.112(5) 0.073(4) 0.155(6) 0.000 -0.009(4) 0.000 F3 0.082(4) 0.194(8) 0.077(4) 0.000 0.000 -0.004(4) F4 0.141(5) 0.133(4) 0.161(5) 0.040(3) 0.041(3) 0.083(4) N1 0.037(2) 0.058(3) 0.0397(19) -0.007(2) -0.0022(17) 0.0009(19) N2 0.072(4) 0.087(4) 0.096(4) -0.008(3) 0.017(3) -0.024(3) O1 0.036(2) 0.057(3) 0.040(2) -0.006(2) 0.000 0.000 O2 0.047(2) 0.065(2) 0.0438(18) -0.0148(17) -0.0022(15) -0.0064(18) P1 0.080(2) 0.075(2) 0.0500(16) 0.000 0.000 0.000 P2 0.0456(15) 0.0545(17) 0.080(2) 0.000 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.247(4) . ? Ag1 N1 2.247(4) 2_655 ? C1 N1 1.297(6) . ? C1 O1 1.355(5) . ? C1 C2 1.453(7) . ? C2 C7 1.396(6) . ? C2 C3 1.398(7) . ? C3 C4 1.376(8) . ? C3 H3 0.9300 . ? C4 C5 1.365(8) . ? C4 H4 0.9300 . ? C5 C6 1.369(8) . ? C5 H5 0.9300 . ? C6 C7 1.386(6) . ? C6 H6 0.9300 . ? C7 O2 1.366(5) . ? C8 O2 1.438(6) . ? C8 C9 1.504(7) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C14 1.380(7) . ? C9 C10 1.390(8) . ? C10 C11 1.373(8) . ? C10 H10 0.9300 . ? C11 C12 1.377(7) . ? C11 H11 0.9300 . ? C12 C13 1.385(7) . ? C12 C15 1.453(8) . ? C13 C14 1.378(7) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 N2 1.138(7) . ? C16 C17 1.37(2) . ? C16 C18 1.369(18) 5_667 ? C16 H16 0.9300 . ? C17 C18 1.345(19) . ? C17 H17 0.9300 . ? C18 C16 1.369(19) 5_667 ? C18 H18 0.9300 . ? C19 C20 1.367(5) . ? C19 C20 1.367(5) 2 ? C19 H19 0.9300 . ? C20 C20 1.371(7) 3_557 ? C20 H20 0.9300 . ? F1 P1 1.566(5) . ? F2 P1 1.573(6) . ? F3 P2 1.578(6) . ? F4 P2 1.550(5) . ? N1 N1 1.395(8) 4_556 ? O1 C1 1.355(5) 4_556 ? P1 F1 1.566(5) 3_657 ? P1 F1 1.566(5) 2_655 ? P1 F1 1.566(5) 4_557 ? P1 F2 1.573(6) 2_655 ? P2 F4 1.550(5) 3_556 ? P2 F4 1.550(5) 4_556 ? P2 F4 1.550(5) 2 ? P2 F3 1.578(6) 3_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N1 122.7(2) . 2_655 ? N1 C1 O1 110.9(4) . . ? N1 C1 C2 131.2(4) . . ? O1 C1 C2 117.9(4) . . ? C7 C2 C3 119.4(4) . . ? C7 C2 C1 122.4(4) . . ? C3 C2 C1 118.2(5) . . ? C4 C3 C2 119.8(5) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C5 C4 C3 120.3(6) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 121.0(5) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C7 120.1(5) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? O2 C7 C6 123.6(4) . . ? O2 C7 C2 117.0(4) . . ? C6 C7 C2 119.5(4) . . ? O2 C8 C9 107.2(4) . . ? O2 C8 H8A 110.3 . . ? C9 C8 H8A 110.3 . . ? O2 C8 H8B 110.3 . . ? C9 C8 H8B 110.3 . . ? H8A C8 H8B 108.5 . . ? C14 C9 C10 118.7(5) . . ? C14 C9 C8 120.3(5) . . ? C10 C9 C8 121.1(5) . . ? C11 C10 C9 121.1(5) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C10 C11 C12 119.4(5) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? C11 C12 C13 120.6(5) . . ? C11 C12 C15 120.8(5) . . ? C13 C12 C15 118.6(5) . . ? C14 C13 C12 119.3(5) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C13 C14 C9 121.0(5) . . ? C13 C14 H14 119.5 . . ? C9 C14 H14 119.5 . . ? N2 C15 C12 178.7(7) . . ? C17 C16 C18 118.1(19) . 5_667 ? C17 C16 H16 121.0 . . ? C18 C16 H16 121.0 5_667 . ? C18 C17 C16 122.5(17) . . ? C18 C17 H17 118.7 . . ? C16 C17 H17 118.7 . . ? C17 C18 C16 119.4(15) . 5_667 ? C17 C18 H18 120.3 . . ? C16 C18 H18 120.3 5_667 . ? C20 C19 C20 121.7(10) . 2 ? C20 C19 H19 119.2 . . ? C20 C19 H19 119.2 2 . ? C19 C20 C20 119.1(5) . 3_557 ? C19 C20 H20 120.4 . . ? C20 C20 H20 120.4 3_557 . ? C1 N1 N1 106.8(3) . 4_556 ? C1 N1 Ag1 134.8(3) . . ? N1 N1 Ag1 117.20(12) 4_556 . ? C1 O1 C1 104.6(5) . 4_556 ? C7 O2 C8 118.3(4) . . ? F1 P1 F1 89.1(5) 3_657 2_655 ? F1 P1 F1 179.5(3) 3_657 . ? F1 P1 F1 90.9(5) 2_655 . ? F1 P1 F1 90.9(5) 3_657 4_557 ? F1 P1 F1 179.5(3) 2_655 4_557 ? F1 P1 F1 89.1(5) . 4_557 ? F1 P1 F2 89.74(17) 3_657 . ? F1 P1 F2 90.26(17) 2_655 . ? F1 P1 F2 89.74(17) . . ? F1 P1 F2 90.26(17) 4_557 . ? F1 P1 F2 90.26(17) 3_657 2_655 ? F1 P1 F2 89.74(17) 2_655 2_655 ? F1 P1 F2 90.26(17) . 2_655 ? F1 P1 F2 89.74(17) 4_557 2_655 ? F2 P1 F2 180.000(1) . 2_655 ? F4 P2 F4 178.8(3) 3_556 4_556 ? F4 P2 F4 88.3(5) 3_556 2 ? F4 P2 F4 91.7(5) 4_556 2 ? F4 P2 F4 91.7(5) 3_556 . ? F4 P2 F4 88.3(5) 4_556 . ? F4 P2 F4 178.8(3) 2 . ? F4 P2 F3 90.61(17) 3_556 3_556 ? F4 P2 F3 90.61(17) 4_556 3_556 ? F4 P2 F3 89.39(17) 2 3_556 ? F4 P2 F3 89.39(17) . 3_556 ? F4 P2 F3 89.39(17) 3_556 . ? F4 P2 F3 89.39(17) 4_556 . ? F4 P2 F3 90.61(17) 2 . ? F4 P2 F3 90.61(17) . . ? F3 P2 F3 180.000(2) 3_556 . ? 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 N1 C1 C2 C7 -16.3(8) . . . . ? O1 C1 C2 C7 164.4(4) . . . . ? N1 C1 C2 C3 164.6(5) . . . . ? O1 C1 C2 C3 -14.7(6) . . . . ? C7 C2 C3 C4 -0.3(8) . . . . ? C1 C2 C3 C4 178.8(5) . . . . ? C2 C3 C4 C5 0.5(10) . . . . ? C3 C4 C5 C6 -0.7(11) . . . . ? C4 C5 C6 C7 0.8(11) . . . . ? C5 C6 C7 O2 -179.8(6) . . . . ? C5 C6 C7 C2 -0.6(9) . . . . ? C3 C2 C7 O2 179.6(5) . . . . ? C1 C2 C7 O2 0.5(7) . . . . ? C3 C2 C7 C6 0.4(8) . . . . ? C1 C2 C7 C6 -178.7(5) . . . . ? O2 C8 C9 C14 115.3(6) . . . . ? O2 C8 C9 C10 -65.1(7) . . . . ? C14 C9 C10 C11 -1.0(9) . . . . ? C8 C9 C10 C11 179.4(6) . . . . ? C9 C10 C11 C12 1.1(9) . . . . ? C10 C11 C12 C13 -0.3(9) . . . . ? C10 C11 C12 C15 -179.2(6) . . . . ? C11 C12 C13 C14 -0.5(9) . . . . ? C15 C12 C13 C14 178.4(6) . . . . ? C12 C13 C14 C9 0.6(9) . . . . ? C10 C9 C14 C13 0.1(9) . . . . ? C8 C9 C14 C13 179.8(5) . . . . ? C11 C12 C15 N2 112(29) . . . . ? C13 C12 C15 N2 -67(29) . . . . ? C18 C16 C17 C18 -1(2) 5_667 . . . ? C16 C17 C18 C16 1(2) . . . 5_667 ? C20 C19 C20 C20 -1(2) 2 . . 3_557 ? O1 C1 N1 N1 0.6(6) . . . 4_556 ? C2 C1 N1 N1 -178.7(5) . . . 4_556 ? O1 C1 N1 Ag1 167.2(3) . . . . ? C2 C1 N1 Ag1 -12.1(8) . . . . ? N1 Ag1 N1 C1 -178.7(5) 2_655 . . . ? N1 Ag1 N1 N1 -13.1(4) 2_655 . . 4_556 ? N1 C1 O1 C1 -0.2(2) . . . 4_556 ? C2 C1 O1 C1 179.2(5) . . . 4_556 ? C6 C7 O2 C8 23.6(7) . . . . ? C2 C7 O2 C8 -155.6(5) . . . . ? C9 C8 O2 C7 172.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.717 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.076 #===End data_2 _database_code_depnum_ccdc_archive 'CCDC 791138' #TrackingRef '- CIF_1.1.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H20 Ag F6 N4 O3 Sb' _chemical_formula_weight 828.12 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 8.9896(12) _cell_length_b 31.618(4) _cell_length_c 12.7659(17) _cell_angle_alpha 90.00 _cell_angle_beta 105.991(2) _cell_angle_gamma 90.00 _cell_volume 3488.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6702 _cell_measurement_theta_min 2.357 _cell_measurement_theta_max 27.640 _exptl_crystal_description plan _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 1.402 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6040 _exptl_absorpt_correction_T_max 0.9332 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18015 _diffrn_reflns_av_R_equivalents 0.0451 _diffrn_reflns_av_sigmaI/netI 0.0502 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6450 _reflns_number_gt 5288 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0583P)^2^+3.4716P] 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 6450 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0544 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1202 _refine_ls_wR_factor_gt 0.1166 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.43449(4) -0.050273(11) 0.44238(3) 0.03762(13) Uani 1 1 d . . . N1 N 0.3459(4) 0.04903(11) 0.4264(3) 0.0275(8) Uani 1 1 d . . . N2 N 0.3258(4) 0.01283(11) 0.3607(3) 0.0287(8) Uani 1 1 d . . . N4 N 0.7164(9) 0.32873(19) 0.3819(5) 0.097(2) Uani 1 1 d . . . N3 N 1.1969(5) -0.07900(15) 0.4285(4) 0.0471(11) Uani 1 1 d . . . C1 C 1.0668(6) -0.07731(16) 0.3889(4) 0.0382(11) Uani 1 1 d . . . C2 C 0.9040(5) -0.07534(16) 0.3339(4) 0.0353(11) Uani 1 1 d . . . C3 C 0.8379(6) -0.10743(16) 0.2614(4) 0.0394(11) Uani 1 1 d . . . H3 H 0.8982 -0.1309 0.2513 0.047 Uiso 1 1 calc R . . C4 C 0.6832(6) -0.10462(15) 0.2044(4) 0.0366(11) Uani 1 1 d . . . H4 H 0.6363 -0.1267 0.1560 0.044 Uiso 1 1 calc R . . C5 C 0.5963(5) -0.06984(15) 0.2174(3) 0.0316(10) Uani 1 1 d . . . C6 C 0.6631(5) -0.03810(15) 0.2902(4) 0.0357(11) Uani 1 1 d . . . H6 H 0.6033 -0.0144 0.2999 0.043 Uiso 1 1 calc R . . C7 C 0.8165(6) -0.04104(15) 0.3484(4) 0.0368(11) Uani 1 1 d . . . H7 H 0.8623 -0.0194 0.3987 0.044 Uiso 1 1 calc R . . C8 C 0.4301(5) -0.06747(18) 0.1489(4) 0.0399(12) Uani 1 1 d . . . H8A H 0.4219 -0.0485 0.0858 0.048 Uiso 1 1 calc R . . H8B H 0.3933 -0.0959 0.1211 0.048 Uiso 1 1 calc R . . C9 C 0.1838(5) -0.04455(14) 0.1636(4) 0.0307(10) Uani 1 1 d . . . C10 C 0.0986(6) -0.06979(16) 0.0806(4) 0.0380(11) Uani 1 1 d . . . H10 H 0.1467 -0.0931 0.0562 0.046 Uiso 1 1 calc R . . C11 C -0.0567(5) -0.06146(16) 0.0321(4) 0.0376(11) Uani 1 1 d . . . H11 H -0.1137 -0.0791 -0.0251 0.045 Uiso 1 1 calc R . . C12 C -0.1289(5) -0.02791(15) 0.0663(4) 0.0326(10) Uani 1 1 d . . . H12 H -0.2356 -0.0225 0.0336 0.039 Uiso 1 1 calc R . . C13 C -0.0451(5) -0.00240(14) 0.1477(3) 0.0296(10) Uani 1 1 d . . . H13 H -0.0942 0.0211 0.1706 0.036 Uiso 1 1 calc R . . C14 C 0.1121(5) -0.01021(13) 0.1983(3) 0.0262(9) Uani 1 1 d . . . C15 C 0.1948(5) 0.01770(13) 0.2862(3) 0.0256(9) Uani 1 1 d . . . C16 C 0.2264(5) 0.07315(13) 0.3872(3) 0.0260(9) Uani 1 1 d . . . C17 C 0.1784(5) 0.11323(14) 0.4234(4) 0.0306(10) Uani 1 1 d . . . C18 C 0.0242(6) 0.12541(16) 0.3764(5) 0.0456(13) Uani 1 1 d . . . H18 H -0.0408 0.1084 0.3210 0.055 Uiso 1 1 calc R . . C19 C -0.0334(7) 0.16173(19) 0.4098(6) 0.0610(17) Uani 1 1 d . . . H19 H -0.1381 0.1696 0.3779 0.073 Uiso 1 1 calc R . . C20 C 0.0593(7) 0.18623(18) 0.4881(5) 0.0574(16) Uani 1 1 d . . . H20 H 0.0187 0.2113 0.5105 0.069 Uiso 1 1 calc R . . C21 C 0.2114(6) 0.17539(16) 0.5360(4) 0.0458(13) Uani 1 1 d . . . H21 H 0.2746 0.1930 0.5908 0.055 Uiso 1 1 calc R . . C22 C 0.2722(5) 0.13888(14) 0.5042(4) 0.0328(10) Uani 1 1 d . . . C23 C 0.5218(7) 0.15259(15) 0.6259(4) 0.0453(13) Uani 1 1 d . . . H23A H 0.6169 0.1368 0.6626 0.054 Uiso 1 1 calc R . . H23B H 0.4709 0.1611 0.6823 0.054 Uiso 1 1 calc R . . C24 C 0.5656(6) 0.19169(16) 0.5740(4) 0.0430(13) Uani 1 1 d . . . C25 C 0.6003(7) 0.18925(15) 0.4762(5) 0.0467(13) Uani 1 1 d . . . H25 H 0.5957 0.1625 0.4413 0.056 Uiso 1 1 calc R . . C26 C 0.6413(7) 0.22403(17) 0.4273(5) 0.0529(14) Uani 1 1 d . . . H26 H 0.6627 0.2215 0.3587 0.063 Uiso 1 1 calc R . . C27 C 0.6518(8) 0.26326(17) 0.4781(5) 0.0648(19) Uani 1 1 d . . . C28 C 0.6154(12) 0.2661(2) 0.5773(6) 0.094(3) Uani 1 1 d . . . H28 H 0.6194 0.2927 0.6126 0.112 Uiso 1 1 calc R . . C29 C 0.5736(11) 0.23030(19) 0.6242(5) 0.085(3) Uani 1 1 d . . . H29 H 0.5500 0.2324 0.6921 0.102 Uiso 1 1 calc R . . C30 C 0.6878(9) 0.3000(2) 0.4260(6) 0.073(2) Uani 1 1 d . . . F1 F 0.6442(5) 0.06717(12) 0.3103(3) 0.0782(12) Uani 1 1 d . . . F2 F 0.7414(4) 0.09229(14) 0.1423(4) 0.0859(13) Uani 1 1 d . . . F3 F 0.5020(6) 0.04168(12) 0.1097(3) 0.0935(15) Uani 1 1 d . . . F4 F 0.4629(5) 0.12130(12) 0.0465(3) 0.0689(10) Uani 1 1 d . . . F5 F 0.6060(5) 0.14640(10) 0.2435(3) 0.0694(10) Uani 1 1 d . . . F6 F 0.3646(5) 0.09559(14) 0.2107(3) 0.0866(13) Uani 1 1 d . . . O1 O 0.3380(4) -0.05154(10) 0.2149(2) 0.0339(7) Uani 1 1 d . . . O2 O 0.4200(4) 0.12527(10) 0.5493(3) 0.0376(8) Uani 1 1 d . . . O3 O 0.1284(3) 0.05503(9) 0.2986(2) 0.0275(7) Uani 1 1 d . . . Sb1 Sb 0.55325(4) 0.094047(11) 0.17774(3) 0.03864(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0274(2) 0.0359(2) 0.0398(2) -0.00506(15) -0.00706(16) 0.00396(15) N1 0.0240(19) 0.0289(19) 0.0266(19) -0.0027(15) 0.0022(15) -0.0021(15) N2 0.028(2) 0.0313(19) 0.0240(18) -0.0028(15) 0.0031(16) 0.0020(16) N4 0.137(6) 0.051(3) 0.076(4) 0.018(3) -0.018(4) -0.023(4) N3 0.034(3) 0.057(3) 0.044(3) 0.011(2) 0.001(2) -0.007(2) C1 0.032(3) 0.047(3) 0.035(3) 0.007(2) 0.009(2) -0.005(2) C2 0.026(2) 0.048(3) 0.031(2) 0.009(2) 0.006(2) -0.007(2) C3 0.032(3) 0.042(3) 0.044(3) 0.006(2) 0.009(2) 0.003(2) C4 0.033(3) 0.039(3) 0.036(3) -0.004(2) 0.005(2) -0.003(2) C5 0.025(2) 0.044(3) 0.025(2) 0.001(2) 0.0063(19) -0.002(2) C6 0.032(3) 0.040(3) 0.039(3) 0.002(2) 0.015(2) 0.004(2) C7 0.033(3) 0.044(3) 0.034(3) -0.003(2) 0.010(2) -0.008(2) C8 0.027(2) 0.063(3) 0.030(2) -0.004(2) 0.008(2) 0.004(2) C9 0.028(2) 0.034(2) 0.029(2) 0.0032(19) 0.0070(19) -0.0018(19) C10 0.033(3) 0.041(3) 0.036(3) -0.009(2) 0.002(2) -0.002(2) C11 0.029(2) 0.045(3) 0.033(2) -0.003(2) -0.003(2) -0.007(2) C12 0.020(2) 0.044(3) 0.029(2) 0.006(2) 0.0005(19) -0.006(2) C13 0.026(2) 0.032(2) 0.029(2) 0.0040(18) 0.0041(19) 0.0030(18) C14 0.024(2) 0.030(2) 0.024(2) 0.0037(17) 0.0055(18) -0.0046(18) C15 0.022(2) 0.029(2) 0.025(2) 0.0014(17) 0.0063(18) 0.0000(17) C16 0.022(2) 0.029(2) 0.027(2) 0.0014(18) 0.0080(18) -0.0037(18) C17 0.029(2) 0.030(2) 0.033(2) 0.0030(19) 0.0089(19) 0.0041(19) C18 0.031(3) 0.047(3) 0.056(3) -0.012(3) 0.007(2) 0.002(2) C19 0.038(3) 0.056(4) 0.086(5) -0.011(3) 0.012(3) 0.012(3) C20 0.051(3) 0.046(3) 0.080(4) -0.013(3) 0.028(3) 0.012(3) C21 0.049(3) 0.040(3) 0.048(3) -0.010(2) 0.012(3) 0.003(2) C22 0.034(3) 0.032(2) 0.033(2) 0.0018(19) 0.010(2) 0.002(2) C23 0.054(3) 0.036(3) 0.037(3) -0.004(2) -0.003(2) -0.003(2) C24 0.047(3) 0.032(3) 0.040(3) -0.006(2) -0.004(2) 0.001(2) C25 0.056(3) 0.027(3) 0.060(3) -0.006(2) 0.021(3) 0.004(2) C26 0.061(4) 0.039(3) 0.059(4) 0.003(3) 0.016(3) 0.012(3) C27 0.087(5) 0.029(3) 0.061(4) 0.005(3) -0.008(3) -0.001(3) C28 0.187(9) 0.031(3) 0.055(4) -0.015(3) 0.019(5) -0.015(4) C29 0.164(8) 0.045(4) 0.039(3) -0.012(3) 0.017(4) -0.020(4) C30 0.104(6) 0.042(4) 0.058(4) 0.006(3) -0.006(4) -0.003(3) F1 0.099(3) 0.068(2) 0.048(2) 0.0095(18) -0.012(2) 0.000(2) F2 0.054(2) 0.123(4) 0.085(3) -0.017(3) 0.026(2) 0.010(2) F3 0.118(4) 0.060(2) 0.076(3) -0.020(2) -0.019(3) -0.016(2) F4 0.084(3) 0.080(2) 0.0357(17) 0.0163(17) 0.0061(17) 0.012(2) F5 0.096(3) 0.0454(19) 0.059(2) -0.0131(16) 0.007(2) -0.0069(18) F6 0.060(2) 0.126(4) 0.084(3) 0.029(3) 0.036(2) -0.007(2) O1 0.0267(17) 0.0438(19) 0.0277(16) -0.0066(14) 0.0017(13) 0.0053(14) O2 0.0429(19) 0.0304(17) 0.0329(17) -0.0061(13) -0.0006(15) 0.0020(14) O3 0.0222(15) 0.0313(16) 0.0248(15) -0.0014(12) -0.0007(12) 0.0032(12) Sb1 0.0369(2) 0.0454(2) 0.02994(19) -0.00280(14) 0.00298(14) -0.00478(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.210(3) 3_656 ? Ag1 N3 2.283(4) 1_455 ? Ag1 N2 2.337(4) . ? N1 C16 1.300(5) . ? N1 N2 1.401(5) . ? N1 Ag1 2.210(3) 3_656 ? N2 C15 1.303(5) . ? N4 C30 1.134(8) . ? N3 C1 1.140(6) . ? N3 Ag1 2.283(4) 1_655 ? C1 C2 1.440(6) . ? C2 C7 1.382(7) . ? C2 C3 1.391(7) . ? C3 C4 1.384(7) . ? C3 H3 0.9500 . ? C4 C5 1.386(7) . ? C4 H4 0.9500 . ? C5 C6 1.387(6) . ? C5 C8 1.511(6) . ? C6 C7 1.377(7) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 O1 1.426(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 O1 1.378(5) . ? C9 C10 1.378(6) . ? C9 C14 1.396(6) . ? C10 C11 1.387(6) . ? C10 H10 0.9500 . ? C11 C12 1.376(7) . ? C11 H11 0.9500 . ? C12 C13 1.367(6) . ? C12 H12 0.9500 . ? C13 C14 1.404(6) . ? C13 H13 0.9500 . ? C14 C15 1.460(6) . ? C15 O3 1.351(5) . ? C16 O3 1.354(5) . ? C16 C17 1.454(6) . ? C17 C22 1.398(6) . ? C17 C18 1.404(6) . ? C18 C19 1.375(8) . ? C18 H18 0.9500 . ? C19 C20 1.355(8) . ? C19 H19 0.9500 . ? C20 C21 1.378(8) . ? C20 H20 0.9500 . ? C21 C22 1.385(7) . ? C21 H21 0.9500 . ? C22 O2 1.364(5) . ? C23 O2 1.431(5) . ? C23 C24 1.506(7) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.370(8) . ? C24 C29 1.372(7) . ? C25 C26 1.364(8) . ? C25 H25 0.9500 . ? C26 C27 1.390(8) . ? C26 H26 0.9500 . ? C27 C28 1.396(10) . ? C27 C30 1.421(9) . ? C28 C29 1.379(9) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? F1 Sb1 1.869(3) . ? F2 Sb1 1.868(4) . ? F3 Sb1 1.867(4) . ? F4 Sb1 1.860(3) . ? F5 Sb1 1.858(3) . ? F6 Sb1 1.857(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N3 133.42(14) 3_656 1_455 ? N1 Ag1 N2 119.96(12) 3_656 . ? N3 Ag1 N2 92.18(14) 1_455 . ? C16 N1 N2 107.0(3) . . ? C16 N1 Ag1 138.8(3) . 3_656 ? N2 N1 Ag1 114.2(2) . 3_656 ? C15 N2 N1 106.4(3) . . ? C15 N2 Ag1 127.5(3) . . ? N1 N2 Ag1 117.5(2) . . ? C1 N3 Ag1 147.1(4) . 1_655 ? N3 C1 C2 177.2(6) . . ? C7 C2 C3 120.5(4) . . ? C7 C2 C1 120.5(4) . . ? C3 C2 C1 118.9(5) . . ? C4 C3 C2 119.1(5) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 120.4(4) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C4 C5 C6 120.0(4) . . ? C4 C5 C8 118.0(4) . . ? C6 C5 C8 121.9(4) . . ? C7 C6 C5 119.8(4) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C6 C7 C2 120.2(4) . . ? C6 C7 H7 119.9 . . ? C2 C7 H7 119.9 . . ? O1 C8 C5 108.6(4) . . ? O1 C8 H8A 110.0 . . ? C5 C8 H8A 110.0 . . ? O1 C8 H8B 110.0 . . ? C5 C8 H8B 110.0 . . ? H8A C8 H8B 108.4 . . ? O1 C9 C10 123.1(4) . . ? O1 C9 C14 117.8(4) . . ? C10 C9 C14 119.1(4) . . ? C9 C10 C11 120.7(5) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C12 C11 C10 120.7(4) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C13 C12 C11 119.2(4) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C12 C13 C14 121.3(4) . . ? C12 C13 H13 119.3 . . ? C14 C13 H13 119.3 . . ? C9 C14 C13 119.0(4) . . ? C9 C14 C15 122.2(4) . . ? C13 C14 C15 118.8(4) . . ? N2 C15 O3 110.9(4) . . ? N2 C15 C14 131.0(4) . . ? O3 C15 C14 118.0(3) . . ? N1 C16 O3 110.6(4) . . ? N1 C16 C17 132.5(4) . . ? O3 C16 C17 116.9(4) . . ? C22 C17 C18 118.7(4) . . ? C22 C17 C16 124.7(4) . . ? C18 C17 C16 116.6(4) . . ? C19 C18 C17 120.6(5) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C20 C19 C18 119.9(5) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C21 121.2(5) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C20 C21 C22 120.1(5) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? O2 C22 C21 123.8(4) . . ? O2 C22 C17 116.6(4) . . ? C21 C22 C17 119.6(4) . . ? O2 C23 C24 113.0(4) . . ? O2 C23 H23A 109.0 . . ? C24 C23 H23A 109.0 . . ? O2 C23 H23B 109.0 . . ? C24 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? C25 C24 C29 118.7(5) . . ? C25 C24 C23 120.5(4) . . ? C29 C24 C23 120.8(5) . . ? C26 C25 C24 122.0(5) . . ? C26 C25 H25 119.0 . . ? C24 C25 H25 119.0 . . ? C25 C26 C27 119.9(6) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C26 C27 C28 118.5(6) . . ? C26 C27 C30 120.5(6) . . ? C28 C27 C30 120.9(6) . . ? C29 C28 C27 120.1(6) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C24 C29 C28 120.8(6) . . ? C24 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? N4 C30 C27 178.1(8) . . ? C9 O1 C8 116.6(3) . . ? C22 O2 C23 117.6(4) . . ? C15 O3 C16 105.1(3) . . ? F6 Sb1 F5 90.5(2) . . ? F6 Sb1 F4 89.58(18) . . ? F5 Sb1 F4 89.32(16) . . ? F6 Sb1 F3 90.3(2) . . ? F5 Sb1 F3 179.0(2) . . ? F4 Sb1 F3 90.07(17) . . ? F6 Sb1 F2 179.11(19) . . ? F5 Sb1 F2 90.02(19) . . ? F4 Sb1 F2 89.74(19) . . ? F3 Sb1 F2 89.1(2) . . ? F6 Sb1 F1 90.34(19) . . ? F5 Sb1 F1 90.14(16) . . ? F4 Sb1 F1 179.45(17) . . ? F3 Sb1 F1 90.47(17) . . ? F2 Sb1 F1 90.3(2) . . ? 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 C16 N1 N2 C15 -0.1(5) . . . . ? Ag1 N1 N2 C15 -178.0(3) 3_656 . . . ? C16 N1 N2 Ag1 -150.3(3) . . . . ? Ag1 N1 N2 Ag1 31.8(3) 3_656 . . . ? N1 Ag1 N2 C15 -176.8(3) 3_656 . . . ? N3 Ag1 N2 C15 -32.1(4) 1_455 . . . ? N1 Ag1 N2 N1 -33.7(4) 3_656 . . . ? N3 Ag1 N2 N1 111.0(3) 1_455 . . . ? Ag1 N3 C1 C2 58(12) 1_655 . . . ? N3 C1 C2 C7 -122(11) . . . . ? N3 C1 C2 C3 55(11) . . . . ? C7 C2 C3 C4 -0.2(7) . . . . ? C1 C2 C3 C4 -176.9(5) . . . . ? C2 C3 C4 C5 1.5(7) . . . . ? C3 C4 C5 C6 -1.8(7) . . . . ? C3 C4 C5 C8 177.0(5) . . . . ? C4 C5 C6 C7 0.8(7) . . . . ? C8 C5 C6 C7 -178.0(4) . . . . ? C5 C6 C7 C2 0.5(7) . . . . ? C3 C2 C7 C6 -0.7(7) . . . . ? C1 C2 C7 C6 175.9(4) . . . . ? C4 C5 C8 O1 139.9(4) . . . . ? C6 C5 C8 O1 -41.3(6) . . . . ? O1 C9 C10 C11 179.6(4) . . . . ? C14 C9 C10 C11 -0.3(7) . . . . ? C9 C10 C11 C12 -0.2(8) . . . . ? C10 C11 C12 C13 0.9(7) . . . . ? C11 C12 C13 C14 -1.1(7) . . . . ? O1 C9 C14 C13 -179.8(4) . . . . ? C10 C9 C14 C13 0.1(6) . . . . ? O1 C9 C14 C15 -0.3(6) . . . . ? C10 C9 C14 C15 179.6(4) . . . . ? C12 C13 C14 C9 0.6(6) . . . . ? C12 C13 C14 C15 -178.9(4) . . . . ? N1 N2 C15 O3 0.5(5) . . . . ? Ag1 N2 C15 O3 146.8(3) . . . . ? N1 N2 C15 C14 -177.7(4) . . . . ? Ag1 N2 C15 C14 -31.4(7) . . . . ? C9 C14 C15 N2 -16.4(7) . . . . ? C13 C14 C15 N2 163.1(5) . . . . ? C9 C14 C15 O3 165.6(4) . . . . ? C13 C14 C15 O3 -14.9(6) . . . . ? N2 N1 C16 O3 -0.4(5) . . . . ? Ag1 N1 C16 O3 176.8(3) 3_656 . . . ? N2 N1 C16 C17 176.2(4) . . . . ? Ag1 N1 C16 C17 -6.6(8) 3_656 . . . ? N1 C16 C17 C22 11.9(8) . . . . ? O3 C16 C17 C22 -171.7(4) . . . . ? N1 C16 C17 C18 -164.9(5) . . . . ? O3 C16 C17 C18 11.5(6) . . . . ? C22 C17 C18 C19 -0.4(8) . . . . ? C16 C17 C18 C19 176.7(5) . . . . ? C17 C18 C19 C20 0.5(10) . . . . ? C18 C19 C20 C21 -0.3(10) . . . . ? C19 C20 C21 C22 0.0(10) . . . . ? C20 C21 C22 O2 -178.2(5) . . . . ? C20 C21 C22 C17 0.1(8) . . . . ? C18 C17 C22 O2 178.5(4) . . . . ? C16 C17 C22 O2 1.7(7) . . . . ? C18 C17 C22 C21 0.1(7) . . . . ? C16 C17 C22 C21 -176.7(5) . . . . ? O2 C23 C24 C25 -41.7(7) . . . . ? O2 C23 C24 C29 139.1(6) . . . . ? C29 C24 C25 C26 -0.4(9) . . . . ? C23 C24 C25 C26 -179.6(5) . . . . ? C24 C25 C26 C27 1.3(9) . . . . ? C25 C26 C27 C28 -1.8(10) . . . . ? C25 C26 C27 C30 -177.2(6) . . . . ? C26 C27 C28 C29 1.5(12) . . . . ? C30 C27 C28 C29 176.9(8) . . . . ? C25 C24 C29 C28 0.1(11) . . . . ? C23 C24 C29 C28 179.3(7) . . . . ? C27 C28 C29 C24 -0.6(13) . . . . ? C26 C27 C30 N4 4(27) . . . . ? C28 C27 C30 N4 -171(26) . . . . ? C10 C9 O1 C8 35.1(6) . . . . ? C14 C9 O1 C8 -145.0(4) . . . . ? C5 C8 O1 C9 175.8(4) . . . . ? C21 C22 O2 C23 -6.5(7) . . . . ? C17 C22 O2 C23 175.2(4) . . . . ? C24 C23 O2 C22 -69.7(6) . . . . ? N2 C15 O3 C16 -0.7(5) . . . . ? C14 C15 O3 C16 177.7(4) . . . . ? N1 C16 O3 C15 0.6(5) . . . . ? C17 C16 O3 C15 -176.5(4) . . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.119 0.250 0.080 405.6 166.6 2 -0.119 0.750 0.426 405.5 167.5 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.288 _refine_diff_density_min -0.827 _refine_diff_density_rms 0.131 #===End data_3 _database_code_depnum_ccdc_archive 'CCDC 791139' #TrackingRef '- CIF_1.1.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H46 Ag2 F6 N8 O12 S2' _chemical_formula_weight 1560.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 10.518(2) _cell_length_b 13.249(2) _cell_length_c 13.926(3) _cell_angle_alpha 83.357(3) _cell_angle_beta 82.318(3) _cell_angle_gamma 70.574(3) _cell_volume 1808.4(6) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2077 _cell_measurement_theta_min 4.829 _cell_measurement_theta_max 44.881 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 786 _exptl_absorpt_coefficient_mu 0.677 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8489 _exptl_absorpt_correction_T_max 0.9541 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9583 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_sigmaI/netI 0.0748 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6609 _reflns_number_gt 4975 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6609 _refine_ls_number_parameters 442 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.0925 _refine_ls_wR_factor_gt 0.0880 _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_restrained_S_all 0.952 _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 0.10799(3) 1.04415(2) -0.105045(19) 0.03202(10) Uani 1 1 d . . . N1 N 0.1157(3) 0.9450(2) 0.1113(2) 0.0261(7) Uani 1 1 d . . . N2 N 0.1721(3) 1.0129(2) 0.04836(19) 0.0241(7) Uani 1 1 d . . . N3 N 0.2228(3) 1.0932(2) 0.7562(2) 0.0364(8) Uani 1 1 d . . . N4 N -0.2208(4) 0.6080(3) -0.1975(3) 0.0508(10) Uani 1 1 d . . . O1 O 0.2634(2) 0.98401(18) 0.18535(15) 0.0247(5) Uani 1 1 d . . . O2 O 0.0720(3) 0.75558(18) 0.20841(17) 0.0338(6) Uani 1 1 d . . . O3 O 0.3935(2) 1.11386(19) 0.21673(16) 0.0296(6) Uani 1 1 d . . . O4 O 0.1582(3) 0.8513(2) -0.15010(18) 0.0439(7) Uani 1 1 d . . . O5 O 0.2113(3) 0.8845(2) -0.32208(18) 0.0387(7) Uani 1 1 d . . . O6 O 0.0129(3) 0.8335(2) -0.2627(2) 0.0480(7) Uani 1 1 d . . . S1 S 0.14508(10) 0.83166(7) -0.24687(7) 0.0303(2) Uani 1 1 d . . . C1 C 0.1728(3) 0.9297(3) 0.1917(2) 0.0235(8) Uani 1 1 d . . . C2 C 0.1530(4) 0.8689(3) 0.2836(2) 0.0261(8) Uani 1 1 d . . . C3 C 0.1867(4) 0.8994(3) 0.3667(3) 0.0385(10) Uani 1 1 d . . . H3 H 0.2212 0.9563 0.3614 0.046 Uiso 1 1 calc R . . C4 C 0.1702(4) 0.8472(3) 0.4561(3) 0.0451(11) Uani 1 1 d . . . H4 H 0.1911 0.8693 0.5113 0.054 Uiso 1 1 calc R . . C5 C 0.1225(4) 0.7620(3) 0.4627(3) 0.0452(11) Uani 1 1 d . . . H5 H 0.1119 0.7258 0.5230 0.054 Uiso 1 1 calc R . . C6 C 0.0901(4) 0.7291(3) 0.3821(3) 0.0381(10) Uani 1 1 d . . . H6 H 0.0585 0.6706 0.3882 0.046 Uiso 1 1 calc R . . C7 C 0.1040(4) 0.7823(3) 0.2919(3) 0.0287(8) Uani 1 1 d . . . C8 C 0.0167(4) 0.6691(3) 0.2187(3) 0.0356(9) Uani 1 1 d . . . H8A H -0.0567 0.6814 0.2707 0.043 Uiso 1 1 calc R . . H8B H 0.0861 0.6023 0.2357 0.043 Uiso 1 1 calc R . . C9 C -0.0351(4) 0.6608(3) 0.1261(3) 0.0297(9) Uani 1 1 d . . . C10 C -0.0032(4) 0.7109(3) 0.0377(3) 0.0319(9) Uani 1 1 d . . . H10 H 0.0532 0.7527 0.0341 0.038 Uiso 1 1 calc R . . C11 C -0.0544(4) 0.6994(3) -0.0450(3) 0.0338(9) Uani 1 1 d . . . H11 H -0.0340 0.7348 -0.1037 0.041 Uiso 1 1 calc R . . C12 C -0.1355(4) 0.6360(3) -0.0411(3) 0.0309(9) Uani 1 1 d . . . C13 C -0.1846(4) 0.6206(3) -0.1283(3) 0.0374(10) Uani 1 1 d . . . C14 C -0.1677(4) 0.5843(3) 0.0474(3) 0.0377(10) Uani 1 1 d . . . H14 H -0.2220 0.5408 0.0506 0.045 Uiso 1 1 calc R . . C15 C -0.1186(4) 0.5983(3) 0.1291(3) 0.0349(9) Uani 1 1 d . . . H15 H -0.1417 0.5651 0.1882 0.042 Uiso 1 1 calc R . . C16 C 0.2584(3) 1.0336(3) 0.0948(2) 0.0219(8) Uani 1 1 d . . . C17 C 0.3484(3) 1.0952(3) 0.0588(2) 0.0226(8) Uani 1 1 d . . . C18 C 0.3698(3) 1.1168(3) -0.0416(2) 0.0254(8) Uani 1 1 d . . . H18 H 0.3238 1.0933 -0.0822 0.030 Uiso 1 1 calc R . . C19 C 0.4555(4) 1.1710(3) -0.0818(3) 0.0324(9) Uani 1 1 d . . . H19 H 0.4661 1.1861 -0.1487 0.039 Uiso 1 1 calc R . . C20 C 0.5267(4) 1.2035(3) -0.0220(3) 0.0340(9) Uani 1 1 d . . . H20 H 0.5873 1.2390 -0.0492 0.041 Uiso 1 1 calc R . . C21 C 0.5096(4) 1.1842(3) 0.0772(3) 0.0306(9) Uani 1 1 d . . . H21 H 0.5589 1.2062 0.1164 0.037 Uiso 1 1 calc R . . C22 C 0.4189(3) 1.1320(3) 0.1190(2) 0.0249(8) Uani 1 1 d . . . C23 C 0.4535(4) 1.1625(3) 0.2770(2) 0.0300(9) Uani 1 1 d . . . H23A H 0.4315 1.2387 0.2580 0.036 Uiso 1 1 calc R . . H23B H 0.5513 1.1303 0.2694 0.036 Uiso 1 1 calc R . . C24 C 0.3998(4) 1.1458(3) 0.3814(2) 0.0262(8) Uani 1 1 d . . . C25 C 0.4782(4) 1.1474(3) 0.4537(3) 0.0317(9) Uani 1 1 d . . . H25 H 0.5622 1.1569 0.4362 0.038 Uiso 1 1 calc R . . C26 C 0.4343(4) 1.1351(3) 0.5508(3) 0.0350(9) Uani 1 1 d . . . H26 H 0.4870 1.1374 0.5985 0.042 Uiso 1 1 calc R . . C27 C 0.3090(4) 1.1192(3) 0.5760(3) 0.0304(9) Uani 1 1 d . . . C28 C 0.2302(4) 1.1172(3) 0.5047(3) 0.0330(9) Uani 1 1 d . . . H28 H 0.1474 1.1054 0.5219 0.040 Uiso 1 1 calc R . . C29 C 0.2752(4) 1.1328(3) 0.4072(2) 0.0314(9) Uani 1 1 d . . . H29 H 0.2207 1.1344 0.3593 0.038 Uiso 1 1 calc R . . C30 C 0.2616(4) 1.1042(3) 0.6771(3) 0.0308(9) Uani 1 1 d . . . C31 C 0.2475(4) 0.6911(3) -0.2523(3) 0.0384(10) Uani 1 1 d . . . C32 C 0.8760(7) 0.5693(4) 0.5286(5) 0.087(2) Uani 1 1 d D . . H32 H 0.7917 0.6167 0.5489 0.104 Uiso 1 1 calc R . . C33 C 0.9833(9) 0.5531(5) 0.5798(4) 0.082(2) Uani 1 1 d D . . H33 H 0.9709 0.5902 0.6349 0.099 Uiso 1 1 calc R . . C34 C 1.1080(7) 0.4844(5) 0.5531(5) 0.0781(17) Uani 1 1 d D . . H34 H 1.1804 0.4740 0.5890 0.094 Uiso 1 1 calc R . . F1 F 0.3743(2) 0.67549(19) -0.2359(2) 0.0701(8) Uani 1 1 d . . . F2 F 0.2547(3) 0.6567(2) -0.33896(19) 0.0849(10) Uani 1 1 d . . . F3 F 0.2037(3) 0.62650(19) -0.1880(2) 0.0761(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.03847(19) 0.0432(2) 0.02252(16) 0.00399(12) -0.00778(12) -0.02429(14) N1 0.0312(17) 0.0295(17) 0.0236(16) 0.0014(13) -0.0041(13) -0.0184(14) N2 0.0298(17) 0.0277(17) 0.0180(15) -0.0014(12) -0.0013(13) -0.0141(13) N3 0.049(2) 0.039(2) 0.0266(18) -0.0029(15) -0.0034(16) -0.0223(16) N4 0.056(3) 0.047(2) 0.045(2) -0.0088(18) -0.0122(19) -0.0063(18) O1 0.0268(14) 0.0305(14) 0.0200(12) 0.0044(10) -0.0054(10) -0.0143(11) O2 0.0536(18) 0.0273(15) 0.0279(14) 0.0026(11) -0.0059(12) -0.0237(12) O3 0.0369(15) 0.0426(16) 0.0195(13) -0.0047(11) 0.0002(11) -0.0270(12) O4 0.068(2) 0.0344(16) 0.0282(15) -0.0070(12) -0.0034(14) -0.0147(14) O5 0.0482(17) 0.0403(16) 0.0327(15) -0.0029(12) 0.0019(13) -0.0232(13) O6 0.0322(16) 0.0460(18) 0.066(2) 0.0046(15) -0.0109(14) -0.0140(13) S1 0.0344(6) 0.0301(5) 0.0287(5) -0.0009(4) -0.0028(4) -0.0141(4) C1 0.026(2) 0.024(2) 0.0218(19) -0.0035(15) -0.0014(15) -0.0102(15) C2 0.030(2) 0.029(2) 0.0199(18) 0.0050(15) -0.0044(15) -0.0122(16) C3 0.055(3) 0.043(2) 0.029(2) 0.0039(18) -0.0138(19) -0.029(2) C4 0.061(3) 0.064(3) 0.022(2) 0.005(2) -0.017(2) -0.034(2) C5 0.061(3) 0.052(3) 0.030(2) 0.017(2) -0.014(2) -0.032(2) C6 0.053(3) 0.036(2) 0.033(2) 0.0074(18) -0.0122(19) -0.025(2) C7 0.035(2) 0.025(2) 0.028(2) -0.0007(16) -0.0043(17) -0.0119(17) C8 0.053(3) 0.023(2) 0.034(2) 0.0043(16) -0.0058(19) -0.0186(18) C9 0.040(2) 0.018(2) 0.030(2) -0.0021(16) -0.0023(17) -0.0079(17) C10 0.039(2) 0.024(2) 0.036(2) -0.0025(17) -0.0004(18) -0.0162(17) C11 0.040(2) 0.031(2) 0.027(2) 0.0002(17) 0.0033(18) -0.0105(18) C12 0.035(2) 0.021(2) 0.031(2) -0.0054(16) -0.0029(17) -0.0010(16) C13 0.040(3) 0.028(2) 0.039(2) -0.0061(18) -0.007(2) -0.0006(18) C14 0.045(3) 0.027(2) 0.044(2) -0.0030(18) -0.002(2) -0.0173(19) C15 0.044(3) 0.030(2) 0.033(2) -0.0005(17) -0.0007(19) -0.0157(18) C16 0.029(2) 0.0200(19) 0.0147(17) 0.0006(14) 0.0010(15) -0.0077(15) C17 0.0222(19) 0.0247(19) 0.0200(18) -0.0011(14) 0.0007(14) -0.0075(15) C18 0.028(2) 0.026(2) 0.0225(19) -0.0007(15) -0.0030(15) -0.0096(16) C19 0.033(2) 0.036(2) 0.025(2) 0.0061(17) -0.0019(17) -0.0114(18) C20 0.030(2) 0.036(2) 0.038(2) 0.0012(18) 0.0044(18) -0.0180(18) C21 0.032(2) 0.037(2) 0.029(2) -0.0073(17) -0.0001(17) -0.0184(18) C22 0.024(2) 0.030(2) 0.0203(18) -0.0038(15) 0.0013(15) -0.0088(16) C23 0.034(2) 0.037(2) 0.0256(19) -0.0022(16) -0.0054(16) -0.0190(17) C24 0.030(2) 0.025(2) 0.027(2) -0.0025(15) -0.0020(16) -0.0144(16) C25 0.029(2) 0.039(2) 0.033(2) -0.0032(17) -0.0030(17) -0.0185(17) C26 0.038(2) 0.040(2) 0.031(2) -0.0010(17) -0.0137(18) -0.0158(18) C27 0.037(2) 0.029(2) 0.026(2) -0.0053(16) 0.0024(17) -0.0130(17) C28 0.029(2) 0.040(2) 0.034(2) -0.0079(18) 0.0029(17) -0.0179(18) C29 0.034(2) 0.039(2) 0.024(2) -0.0043(17) -0.0038(17) -0.0160(18) C30 0.040(2) 0.030(2) 0.029(2) -0.0051(17) -0.0024(18) -0.0188(18) C31 0.042(3) 0.036(2) 0.042(2) -0.006(2) -0.007(2) -0.017(2) C32 0.096(5) 0.043(3) 0.110(6) -0.003(4) 0.036(5) -0.025(3) C33 0.152(7) 0.052(4) 0.054(4) -0.010(3) 0.037(4) -0.064(4) C34 0.111(6) 0.062(4) 0.070(4) 0.023(3) -0.011(4) -0.049(4) F1 0.0411(16) 0.0459(16) 0.125(3) -0.0089(15) -0.0262(16) -0.0092(12) F2 0.128(3) 0.0568(19) 0.0613(18) -0.0294(15) -0.0360(18) 0.0005(17) F3 0.073(2) 0.0360(15) 0.103(2) 0.0124(15) 0.0269(17) -0.0159(13) _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 2.277(3) . ? Ag1 N3 2.285(3) 1_554 ? Ag1 N1 2.322(3) 2_575 ? Ag1 O4 2.566(3) . ? N1 C1 1.305(4) . ? N1 N2 1.400(4) . ? N1 Ag1 2.322(3) 2_575 ? N2 C16 1.297(4) . ? N3 C30 1.133(4) . ? N3 Ag1 2.285(3) 1_556 ? N4 C13 1.131(5) . ? O1 C16 1.352(4) . ? O1 C1 1.361(4) . ? O2 C7 1.367(4) . ? O2 C8 1.433(4) . ? O3 C22 1.360(4) . ? O3 C23 1.434(4) . ? O4 S1 1.435(3) . ? O5 S1 1.425(3) . ? O6 S1 1.428(3) . ? S1 C31 1.820(4) . ? C1 C2 1.461(4) . ? C2 C3 1.393(5) . ? C2 C7 1.394(5) . ? C3 C4 1.372(5) . ? C3 H3 0.9300 . ? C4 C5 1.369(6) . ? C4 H4 0.9300 . ? C5 C6 1.371(5) . ? C5 H5 0.9300 . ? C6 C7 1.383(5) . ? C6 H6 0.9300 . ? C8 C9 1.494(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.385(5) . ? C9 C15 1.387(5) . ? C10 C11 1.379(5) . ? C10 H10 0.9300 . ? C11 C12 1.375(5) . ? C11 H11 0.9300 . ? C12 C14 1.396(5) . ? C12 C13 1.442(5) . ? C14 C15 1.366(5) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.451(5) . ? C17 C18 1.397(4) . ? C17 C22 1.411(5) . ? C18 C19 1.359(5) . ? C18 H18 0.9300 . ? C19 C20 1.379(5) . ? C19 H19 0.9300 . ? C20 C21 1.375(5) . ? C20 H20 0.9300 . ? C21 C22 1.387(5) . ? C21 H21 0.9300 . ? C23 C24 1.507(5) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C29 1.373(5) . ? C24 C25 1.391(5) . ? C25 C26 1.378(5) . ? C25 H25 0.9300 . ? C26 C27 1.396(5) . ? C26 H26 0.9300 . ? C27 C28 1.384(5) . ? C27 C30 1.444(5) . ? C28 C29 1.393(5) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C31 F3 1.312(4) . ? C31 F2 1.323(4) . ? C31 F1 1.326(4) . ? C32 C33 1.360(6) . ? C32 C34 1.373(5) 2_766 ? C32 H32 0.9300 . ? C33 C34 1.356(6) . ? C33 H33 0.9300 . ? C34 C32 1.373(5) 2_766 ? C34 H34 0.9300 . ? 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 N3 127.65(11) . 1_554 ? N2 Ag1 N1 113.58(9) . 2_575 ? N3 Ag1 N1 117.83(11) 1_554 2_575 ? N2 Ag1 O4 100.64(9) . . ? N3 Ag1 O4 94.26(10) 1_554 . ? N1 Ag1 O4 83.49(9) 2_575 . ? C1 N1 N2 106.3(3) . . ? C1 N1 Ag1 123.9(2) . 2_575 ? N2 N1 Ag1 119.9(2) . 2_575 ? C16 N2 N1 106.9(3) . . ? C16 N2 Ag1 137.3(2) . . ? N1 N2 Ag1 115.4(2) . . ? C30 N3 Ag1 162.1(3) . 1_556 ? C16 O1 C1 104.4(3) . . ? C7 O2 C8 116.1(3) . . ? C22 O3 C23 116.6(3) . . ? S1 O4 Ag1 120.04(14) . . ? O5 S1 O6 115.76(17) . . ? O5 S1 O4 114.78(16) . . ? O6 S1 O4 114.79(18) . . ? O5 S1 C31 103.21(17) . . ? O6 S1 C31 104.00(18) . . ? O4 S1 C31 101.70(17) . . ? N1 C1 O1 111.1(3) . . ? N1 C1 C2 131.5(3) . . ? O1 C1 C2 117.5(3) . . ? C3 C2 C7 119.0(3) . . ? C3 C2 C1 117.5(3) . . ? C7 C2 C1 123.5(3) . . ? C4 C3 C2 121.2(4) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C5 C4 C3 118.9(4) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C4 C5 C6 121.3(4) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C5 C6 C7 120.3(4) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? O2 C7 C6 124.0(3) . . ? O2 C7 C2 116.8(3) . . ? C6 C7 C2 119.2(3) . . ? O2 C8 C9 110.4(3) . . ? O2 C8 H8A 109.6 . . ? C9 C8 H8A 109.6 . . ? O2 C8 H8B 109.6 . . ? C9 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? C10 C9 C15 118.4(4) . . ? C10 C9 C8 123.7(3) . . ? C15 C9 C8 117.9(3) . . ? C11 C10 C9 120.6(4) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C12 C11 C10 120.3(3) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C14 119.8(4) . . ? C11 C12 C13 120.3(3) . . ? C14 C12 C13 119.9(4) . . ? N4 C13 C12 178.8(4) . . ? C15 C14 C12 119.2(4) . . ? C15 C14 H14 120.4 . . ? C12 C14 H14 120.4 . . ? C14 C15 C9 121.7(4) . . ? C14 C15 H15 119.1 . . ? C9 C15 H15 119.1 . . ? N2 C16 O1 111.3(3) . . ? N2 C16 C17 128.0(3) . . ? O1 C16 C17 120.6(3) . . ? C18 C17 C22 117.9(3) . . ? C18 C17 C16 118.2(3) . . ? C22 C17 C16 123.9(3) . . ? C19 C18 C17 122.2(3) . . ? C19 C18 H18 118.9 . . ? C17 C18 H18 118.9 . . ? C18 C19 C20 119.1(3) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C21 C20 C19 121.1(3) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C20 C21 C22 120.1(3) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? O3 C22 C21 123.1(3) . . ? O3 C22 C17 117.3(3) . . ? C21 C22 C17 119.5(3) . . ? O3 C23 C24 108.9(3) . . ? O3 C23 H23A 109.9 . . ? C24 C23 H23A 109.9 . . ? O3 C23 H23B 109.9 . . ? C24 C23 H23B 109.9 . . ? H23A C23 H23B 108.3 . . ? C29 C24 C25 119.3(3) . . ? C29 C24 C23 122.4(3) . . ? C25 C24 C23 118.2(3) . . ? C26 C25 C24 121.4(3) . . ? C26 C25 H25 119.3 . . ? C24 C25 H25 119.3 . . ? C25 C26 C27 118.7(3) . . ? C25 C26 H26 120.7 . . ? C27 C26 H26 120.7 . . ? C28 C27 C26 120.4(3) . . ? C28 C27 C30 119.7(3) . . ? C26 C27 C30 119.8(3) . . ? C27 C28 C29 119.8(3) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C24 C29 C28 120.3(3) . . ? C24 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? N3 C30 C27 179.2(5) . . ? F3 C31 F2 107.5(3) . . ? F3 C31 F1 106.0(3) . . ? F2 C31 F1 106.0(3) . . ? F3 C31 S1 113.6(3) . . ? F2 C31 S1 111.9(3) . . ? F1 C31 S1 111.3(3) . . ? C33 C32 C34 120.0(6) . 2_766 ? C33 C32 H32 120.0 . . ? C34 C32 H32 120.0 2_766 . ? C34 C33 C32 122.0(5) . . ? C34 C33 H33 119.0 . . ? C32 C33 H33 119.0 . . ? C33 C34 C32 118.0(5) . 2_766 ? C33 C34 H34 121.0 . . ? C32 C34 H34 121.0 2_766 . ? 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 C1 N1 N2 C16 0.0(4) . . . . ? Ag1 N1 N2 C16 147.0(2) 2_575 . . . ? C1 N1 N2 Ag1 174.7(2) . . . . ? Ag1 N1 N2 Ag1 -38.3(3) 2_575 . . . ? N3 Ag1 N2 C16 17.1(4) 1_554 . . . ? N1 Ag1 N2 C16 -151.6(3) 2_575 . . . ? O4 Ag1 N2 C16 121.0(3) . . . . ? N3 Ag1 N2 N1 -155.5(2) 1_554 . . . ? N1 Ag1 N2 N1 35.9(3) 2_575 . . . ? O4 Ag1 N2 N1 -51.6(2) . . . . ? N2 Ag1 O4 S1 -173.77(18) . . . . ? N3 Ag1 O4 S1 -44.2(2) 1_554 . . . ? N1 Ag1 O4 S1 73.38(19) 2_575 . . . ? Ag1 O4 S1 O5 49.4(2) . . . . ? Ag1 O4 S1 O6 -88.4(2) . . . . ? Ag1 O4 S1 C31 160.01(18) . . . . ? N2 N1 C1 O1 0.2(4) . . . . ? Ag1 N1 C1 O1 -145.1(2) 2_575 . . . ? N2 N1 C1 C2 178.3(3) . . . . ? Ag1 N1 C1 C2 33.0(5) 2_575 . . . ? C16 O1 C1 N1 -0.3(4) . . . . ? C16 O1 C1 C2 -178.7(3) . . . . ? N1 C1 C2 C3 -155.5(4) . . . . ? O1 C1 C2 C3 22.6(5) . . . . ? N1 C1 C2 C7 25.3(6) . . . . ? O1 C1 C2 C7 -156.7(3) . . . . ? C7 C2 C3 C4 -1.3(6) . . . . ? C1 C2 C3 C4 179.5(4) . . . . ? C2 C3 C4 C5 1.5(6) . . . . ? C3 C4 C5 C6 -0.6(7) . . . . ? C4 C5 C6 C7 -0.5(7) . . . . ? C8 O2 C7 C6 2.2(5) . . . . ? C8 O2 C7 C2 -177.6(3) . . . . ? C5 C6 C7 O2 -179.0(4) . . . . ? C5 C6 C7 C2 0.7(6) . . . . ? C3 C2 C7 O2 179.9(3) . . . . ? C1 C2 C7 O2 -0.9(5) . . . . ? C3 C2 C7 C6 0.1(5) . . . . ? C1 C2 C7 C6 179.3(3) . . . . ? C7 O2 C8 C9 170.4(3) . . . . ? O2 C8 C9 C10 14.9(5) . . . . ? O2 C8 C9 C15 -165.8(3) . . . . ? C15 C9 C10 C11 0.5(5) . . . . ? C8 C9 C10 C11 179.8(3) . . . . ? C9 C10 C11 C12 -1.5(6) . . . . ? C10 C11 C12 C14 1.0(6) . . . . ? C10 C11 C12 C13 -177.5(3) . . . . ? C11 C12 C13 N4 50(20) . . . . ? C14 C12 C13 N4 -128(20) . . . . ? C11 C12 C14 C15 0.4(6) . . . . ? C13 C12 C14 C15 178.9(3) . . . . ? C12 C14 C15 C9 -1.4(6) . . . . ? C10 C9 C15 C14 0.9(6) . . . . ? C8 C9 C15 C14 -178.4(3) . . . . ? N1 N2 C16 O1 -0.1(4) . . . . ? Ag1 N2 C16 O1 -173.1(2) . . . . ? N1 N2 C16 C17 176.2(3) . . . . ? Ag1 N2 C16 C17 3.2(6) . . . . ? C1 O1 C16 N2 0.3(4) . . . . ? C1 O1 C16 C17 -176.4(3) . . . . ? N2 C16 C17 C18 -15.3(5) . . . . ? O1 C16 C17 C18 160.7(3) . . . . ? N2 C16 C17 C22 166.7(3) . . . . ? O1 C16 C17 C22 -17.3(5) . . . . ? C22 C17 C18 C19 0.2(5) . . . . ? C16 C17 C18 C19 -177.9(3) . . . . ? C17 C18 C19 C20 1.8(5) . . . . ? C18 C19 C20 C21 -1.7(6) . . . . ? C19 C20 C21 C22 -0.5(6) . . . . ? C23 O3 C22 C21 7.1(5) . . . . ? C23 O3 C22 C17 -172.9(3) . . . . ? C20 C21 C22 O3 -177.6(3) . . . . ? C20 C21 C22 C17 2.5(5) . . . . ? C18 C17 C22 O3 177.7(3) . . . . ? C16 C17 C22 O3 -4.3(5) . . . . ? C18 C17 C22 C21 -2.3(5) . . . . ? C16 C17 C22 C21 175.7(3) . . . . ? C22 O3 C23 C24 172.7(3) . . . . ? O3 C23 C24 C29 -26.8(5) . . . . ? O3 C23 C24 C25 155.3(3) . . . . ? C29 C24 C25 C26 0.6(5) . . . . ? C23 C24 C25 C26 178.5(3) . . . . ? C24 C25 C26 C27 1.0(5) . . . . ? C25 C26 C27 C28 -0.8(5) . . . . ? C25 C26 C27 C30 178.9(3) . . . . ? C26 C27 C28 C29 -1.0(5) . . . . ? C30 C27 C28 C29 179.4(3) . . . . ? C25 C24 C29 C28 -2.4(5) . . . . ? C23 C24 C29 C28 179.7(3) . . . . ? C27 C28 C29 C24 2.6(5) . . . . ? Ag1 N3 C30 C27 69(30) 1_556 . . . ? C28 C27 C30 N3 -45(30) . . . . ? C26 C27 C30 N3 136(30) . . . . ? O5 S1 C31 F3 -179.8(3) . . . . ? O6 S1 C31 F3 -58.6(3) . . . . ? O4 S1 C31 F3 61.0(3) . . . . ? O5 S1 C31 F2 -57.9(3) . . . . ? O6 S1 C31 F2 63.4(3) . . . . ? O4 S1 C31 F2 -177.1(3) . . . . ? O5 S1 C31 F1 60.6(3) . . . . ? O6 S1 C31 F1 -178.2(3) . . . . ? O4 S1 C31 F1 -58.7(3) . . . . ? C34 C32 C33 C34 -0.2(9) 2_766 . . . ? C32 C33 C34 C32 0.2(9) . . . 2_766 ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.500 0.500 0.073 358.7 91.5 _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.662 _refine_diff_density_min -0.354 _refine_diff_density_rms 0.080 #===End data_4 _database_code_depnum_ccdc_archive 'CCDC 791140' #TrackingRef '- CIF_1.1.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H20 Ag2 F12 N4 O3 Sb2' _chemical_formula_weight 1171.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.8309(13) _cell_length_b 13.545(2) _cell_length_c 17.271(3) _cell_angle_alpha 73.472(2) _cell_angle_beta 89.038(2) _cell_angle_gamma 80.625(3) _cell_volume 1731.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2591 _cell_measurement_theta_min 2.461 _cell_measurement_theta_max 24.484 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.247 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 2.761 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6664 _exptl_absorpt_correction_T_max 0.8743 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9143 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0522 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6323 _reflns_number_gt 4770 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0682P)^2^+1.5424P] 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 6323 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1312 _refine_ls_wR_factor_gt 0.1212 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.67262(9) 0.52657(5) 0.19820(3) 0.0568(2) Uani 1 1 d . . . Ag2 Ag 0.56190(9) 0.78001(5) 0.20945(3) 0.0543(2) Uani 1 1 d . . . N1 N 0.6799(7) 0.5546(4) 0.3172(3) 0.0311(12) Uani 1 1 d . . . N2 N 0.6805(7) 0.6589(4) 0.3148(3) 0.0339(13) Uani 1 1 d . . . N3 N 0.5873(10) 1.1365(5) -0.1032(4) 0.0583(19) Uani 1 1 d . . . N4 N 0.4131(11) 0.3951(6) -0.0744(4) 0.071(2) Uani 1 1 d . . . C1 C 0.5084(12) 0.3776(6) -0.0219(5) 0.055(2) Uani 1 1 d . . . C2 C 0.6353(11) 0.3620(6) 0.0410(4) 0.0467(19) Uani 1 1 d . . . C3 C 0.5941(10) 0.3257(5) 0.1210(4) 0.0426(17) Uani 1 1 d . . . H3 H 0.4853 0.3082 0.1346 0.051 Uiso 1 1 calc R . . C4 C 0.7176(11) 0.3156(6) 0.1815(4) 0.0459(18) Uani 1 1 d . . . C5 C 0.8781(11) 0.3429(7) 0.1590(5) 0.058(2) Uani 1 1 d . . . H5 H 0.9604 0.3378 0.1988 0.069 Uiso 1 1 calc R . . C6 C 0.9187(12) 0.3778(8) 0.0782(6) 0.070(3) Uani 1 1 d . . . H6 H 1.0281 0.3940 0.0643 0.084 Uiso 1 1 calc R . . C7 C 0.7982(12) 0.3881(7) 0.0195(5) 0.062(2) Uani 1 1 d . . . H7 H 0.8242 0.4124 -0.0346 0.074 Uiso 1 1 calc R . . C8 C 0.6825(12) 0.2707(6) 0.2675(4) 0.053(2) Uani 1 1 d . . . H8A H 0.5671 0.2527 0.2728 0.064 Uiso 1 1 calc R . . H8B H 0.7653 0.2077 0.2905 0.064 Uiso 1 1 calc R . . C9 C 0.6975(9) 0.3163(5) 0.3923(4) 0.0372(16) Uani 1 1 d . . . C10 C 0.6834(11) 0.2152(6) 0.4371(4) 0.0494(19) Uani 1 1 d . . . H10 H 0.6681 0.1656 0.4111 0.059 Uiso 1 1 calc R . . C11 C 0.6921(12) 0.1888(6) 0.5199(5) 0.056(2) Uani 1 1 d . . . H11 H 0.6763 0.1221 0.5495 0.068 Uiso 1 1 calc R . . C12 C 0.7234(12) 0.2582(6) 0.5600(4) 0.054(2) Uani 1 1 d . . . H12 H 0.7394 0.2373 0.6159 0.065 Uiso 1 1 calc R . . C13 C 0.7306(11) 0.3588(6) 0.5163(4) 0.0482(19) Uani 1 1 d . . . H13 H 0.7444 0.4074 0.5434 0.058 Uiso 1 1 calc R . . C14 C 0.7179(9) 0.3906(5) 0.4325(4) 0.0338(15) Uani 1 1 d . . . C15 C 0.7159(8) 0.5007(5) 0.3904(4) 0.0326(14) Uani 1 1 d . . . C16 C 0.7243(8) 0.6597(5) 0.3870(4) 0.0337(15) Uani 1 1 d . . . C17 C 0.7572(9) 0.7416(5) 0.4212(4) 0.0339(15) Uani 1 1 d . . . C18 C 0.7733(10) 0.7204(6) 0.5039(4) 0.0448(18) Uani 1 1 d . . . H18 H 0.7609 0.6544 0.5363 0.054 Uiso 1 1 calc R . . C19 C 0.8063(12) 0.7922(6) 0.5394(4) 0.057(2) Uani 1 1 d . . . H19 H 0.8114 0.7770 0.5954 0.068 Uiso 1 1 calc R . . C20 C 0.8328(12) 0.8898(6) 0.4908(5) 0.055(2) Uani 1 1 d . . . H20 H 0.8611 0.9386 0.5147 0.065 Uiso 1 1 calc R . . C21 C 0.8176(11) 0.9151(6) 0.4070(4) 0.0484(19) Uani 1 1 d . . . H21 H 0.8345 0.9804 0.3749 0.058 Uiso 1 1 calc R . . C22 C 0.7770(9) 0.8414(5) 0.3728(4) 0.0383(16) Uani 1 1 d . . . C23 C 0.8369(10) 0.9446(6) 0.2399(4) 0.0452(18) Uani 1 1 d . . . H23A H 0.9542 0.9421 0.2584 0.054 Uiso 1 1 calc R . . H23B H 0.7684 1.0107 0.2408 0.054 Uiso 1 1 calc R . . C24 C 0.8360(9) 0.9323(5) 0.1563(4) 0.0390(16) Uani 1 1 d . . . C25 C 0.9217(11) 0.8424(6) 0.1428(5) 0.054(2) Uani 1 1 d . . . H25 H 0.9804 0.7900 0.1855 0.065 Uiso 1 1 calc R . . C26 C 0.9221(14) 0.8287(7) 0.0675(5) 0.070(3) Uani 1 1 d . . . H26 H 0.9799 0.7668 0.0596 0.084 Uiso 1 1 calc R . . C27 C 0.8383(12) 0.9048(7) 0.0037(5) 0.060(2) Uani 1 1 d . . . H27 H 0.8381 0.8952 -0.0474 0.072 Uiso 1 1 calc R . . C28 C 0.7538(10) 0.9965(6) 0.0165(4) 0.0440(18) Uani 1 1 d . . . C29 C 0.7557(9) 1.0107(5) 0.0919(4) 0.0392(16) Uani 1 1 d . . . H29 H 0.7025 1.0737 0.0996 0.047 Uiso 1 1 calc R . . C30 C 0.6621(11) 1.0764(6) -0.0515(5) 0.0494(19) Uani 1 1 d . . . O1 O 0.7463(6) 0.5612(3) 0.4375(2) 0.0338(10) Uani 1 1 d . . . O2 O 0.6966(7) 0.3469(3) 0.3096(3) 0.0412(12) Uani 1 1 d . . . O3 O 0.7629(7) 0.8591(4) 0.2900(2) 0.0418(12) Uani 1 1 d . . . F1 F 0.3466(7) 0.4743(5) 0.3433(4) 0.098(2) Uani 1 1 d . . . F2 F 0.2960(7) 0.6419(4) 0.2136(4) 0.0898(19) Uani 1 1 d . . . F3 F 0.0591(7) 0.6082(5) 0.3208(4) 0.0947(19) Uani 1 1 d . . . F4 F 0.0102(7) 0.5848(4) 0.1776(3) 0.0763(16) Uani 1 1 d . . . F5 F 0.0573(7) 0.4222(4) 0.3021(3) 0.0777(16) Uani 1 1 d . . . F6 F 0.2495(7) 0.2220(4) 0.2434(4) 0.0820(17) Uani 1 1 d . . . F7 F 0.4583(9) 0.0599(5) 0.3264(4) 0.107(2) Uani 1 1 d . . . F8 F 0.4270(9) 0.0954(6) 0.1686(4) 0.115(2) Uani 1 1 d . . . F9 F 0.3063(10) -0.0629(4) 0.2650(4) 0.106(2) Uani 1 1 d . . . F10 F 0.1195(8) 0.0628(5) 0.3361(3) 0.0900(19) Uani 1 1 d . . . F11 F 0.0903(8) 0.1029(5) 0.1809(3) 0.0787(16) Uani 1 1 d . . . F12 F 0.3053(10) 0.4600(5) 0.1949(4) 0.112(2) Uani 1 1 d . . . Sb1 Sb 0.27641(7) 0.07984(4) 0.25357(3) 0.04902(17) Uani 1 1 d . . . Sb2 Sb 0.18036(6) 0.53067(4) 0.25945(3) 0.04644(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0770(5) 0.0625(4) 0.0306(3) -0.0085(3) -0.0103(3) -0.0182(3) Ag2 0.0705(4) 0.0469(4) 0.0354(3) 0.0059(3) -0.0244(3) -0.0101(3) N1 0.038(3) 0.033(3) 0.019(3) -0.002(2) -0.009(2) -0.006(2) N2 0.041(3) 0.034(3) 0.023(3) -0.001(2) -0.009(2) -0.008(2) N3 0.072(5) 0.054(4) 0.038(4) 0.006(3) -0.019(4) -0.014(4) N4 0.094(6) 0.072(5) 0.038(4) -0.012(4) -0.021(4) 0.003(4) C1 0.081(6) 0.048(5) 0.033(4) -0.012(4) 0.001(4) -0.003(4) C2 0.066(5) 0.039(4) 0.034(4) -0.012(3) -0.009(4) 0.002(4) C3 0.052(4) 0.038(4) 0.036(4) -0.011(3) -0.008(3) -0.002(3) C4 0.065(5) 0.038(4) 0.036(4) -0.014(3) -0.004(4) -0.005(4) C5 0.050(5) 0.066(6) 0.053(5) -0.016(4) -0.010(4) 0.000(4) C6 0.055(6) 0.081(7) 0.073(7) -0.024(5) 0.009(5) -0.003(5) C7 0.075(6) 0.069(6) 0.036(4) -0.011(4) 0.013(4) -0.005(5) C8 0.083(6) 0.038(4) 0.038(4) -0.009(3) -0.003(4) -0.012(4) C9 0.040(4) 0.038(4) 0.032(4) -0.007(3) -0.003(3) -0.006(3) C10 0.072(6) 0.036(4) 0.040(4) -0.009(3) -0.001(4) -0.010(4) C11 0.075(6) 0.044(5) 0.038(4) 0.008(4) -0.001(4) -0.009(4) C12 0.082(6) 0.044(4) 0.025(4) 0.004(3) 0.001(4) -0.009(4) C13 0.070(5) 0.047(4) 0.028(4) -0.009(3) -0.004(4) -0.010(4) C14 0.042(4) 0.028(3) 0.026(3) 0.000(3) -0.009(3) -0.004(3) C15 0.033(4) 0.037(4) 0.030(3) -0.012(3) -0.004(3) -0.007(3) C16 0.033(4) 0.031(4) 0.031(3) 0.000(3) 0.000(3) -0.004(3) C17 0.041(4) 0.033(4) 0.025(3) -0.005(3) -0.006(3) -0.008(3) C18 0.064(5) 0.040(4) 0.026(3) 0.000(3) 0.000(3) -0.013(4) C19 0.092(7) 0.057(5) 0.022(4) -0.010(4) 0.000(4) -0.020(5) C20 0.082(6) 0.046(5) 0.039(4) -0.016(4) -0.007(4) -0.012(4) C21 0.077(6) 0.039(4) 0.028(4) -0.004(3) -0.009(4) -0.014(4) C22 0.047(4) 0.044(4) 0.022(3) -0.005(3) -0.001(3) -0.011(3) C23 0.057(5) 0.043(4) 0.031(4) 0.002(3) -0.006(3) -0.016(4) C24 0.047(4) 0.040(4) 0.027(3) 0.002(3) -0.005(3) -0.019(3) C25 0.069(6) 0.047(5) 0.035(4) 0.000(4) -0.008(4) 0.003(4) C26 0.102(8) 0.045(5) 0.050(5) -0.010(4) 0.002(5) 0.018(5) C27 0.088(7) 0.057(5) 0.029(4) -0.006(4) -0.002(4) -0.003(5) C28 0.048(4) 0.042(4) 0.035(4) 0.003(3) -0.005(3) -0.011(3) C29 0.045(4) 0.036(4) 0.028(4) 0.005(3) -0.004(3) -0.006(3) C30 0.054(5) 0.056(5) 0.033(4) -0.001(4) -0.006(4) -0.016(4) O1 0.048(3) 0.030(2) 0.020(2) -0.0018(18) -0.004(2) -0.008(2) O2 0.064(3) 0.034(3) 0.026(2) -0.005(2) -0.002(2) -0.012(2) O3 0.068(3) 0.036(3) 0.020(2) 0.002(2) -0.007(2) -0.023(2) F1 0.049(3) 0.116(5) 0.097(4) 0.021(4) -0.023(3) -0.016(3) F2 0.068(4) 0.072(4) 0.117(5) 0.003(3) 0.011(3) -0.032(3) F3 0.068(4) 0.136(5) 0.101(5) -0.076(4) 0.007(3) -0.004(4) F4 0.076(3) 0.080(4) 0.058(3) 0.007(3) -0.028(3) -0.015(3) F5 0.078(4) 0.072(3) 0.076(4) 0.001(3) 0.002(3) -0.031(3) F6 0.084(4) 0.046(3) 0.113(5) -0.018(3) -0.015(3) -0.012(3) F7 0.097(5) 0.094(5) 0.125(5) -0.024(4) -0.058(4) -0.004(4) F8 0.108(5) 0.132(6) 0.111(5) -0.041(4) 0.063(4) -0.037(4) F9 0.137(6) 0.047(3) 0.138(6) -0.034(4) 0.005(5) -0.015(3) F10 0.109(5) 0.128(5) 0.052(3) -0.041(3) 0.027(3) -0.054(4) F11 0.092(4) 0.095(4) 0.055(3) -0.019(3) -0.011(3) -0.032(3) F12 0.133(6) 0.087(4) 0.116(5) -0.041(4) 0.062(5) -0.005(4) Sb1 0.0575(3) 0.0460(3) 0.0470(3) -0.0151(2) 0.0024(3) -0.0149(2) Sb2 0.0390(3) 0.0489(3) 0.0452(3) -0.0045(2) 0.0022(2) -0.0054(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 2.161(7) 2_665 ? Ag1 N1 2.197(5) . ? Ag2 N3 2.115(6) 2_675 ? Ag2 N2 2.174(5) . ? N1 C15 1.277(8) . ? N1 N2 1.402(7) . ? N2 C16 1.302(8) . ? N3 C30 1.118(9) . ? N3 Ag2 2.115(6) 2_675 ? N4 C1 1.131(10) . ? N4 Ag1 2.161(7) 2_665 ? C1 C2 1.432(11) . ? C2 C3 1.380(10) . ? C2 C7 1.395(12) . ? C3 C4 1.397(10) . ? C3 H3 0.9300 . ? C4 C5 1.386(11) . ? C4 C8 1.477(10) . ? C5 C6 1.390(12) . ? C5 H5 0.9300 . ? C6 C7 1.357(12) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 O2 1.440(8) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O2 1.368(8) . ? C9 C10 1.390(10) . ? C9 C14 1.406(9) . ? C10 C11 1.371(10) . ? C10 H10 0.9300 . ? C11 C12 1.370(11) . ? C11 H11 0.9300 . ? C12 C13 1.367(10) . ? C12 H12 0.9300 . ? C13 C14 1.387(9) . ? C13 H13 0.9300 . ? C14 C15 1.459(9) . ? C15 O1 1.356(7) . ? C16 O1 1.355(7) . ? C16 C17 1.455(9) . ? C17 C18 1.378(9) . ? C17 C22 1.404(9) . ? C18 C19 1.347(10) . ? C18 H18 0.9300 . ? C19 C20 1.395(11) . ? C19 H19 0.9300 . ? C20 C21 1.391(10) . ? C20 H20 0.9300 . ? C21 C22 1.376(10) . ? C21 H21 0.9300 . ? C22 O3 1.384(7) . ? C23 O3 1.435(8) . ? C23 C24 1.500(10) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.371(11) . ? C24 C29 1.376(9) . ? C25 C26 1.364(11) . ? C25 H25 0.9300 . ? C26 C27 1.366(11) . ? C26 H26 0.9300 . ? C27 C28 1.383(11) . ? C27 H27 0.9300 . ? C28 C29 1.371(10) . ? C28 C30 1.455(10) . ? C29 H29 0.9300 . ? F1 Sb2 1.867(5) . ? F2 Sb2 1.860(5) . ? F3 Sb2 1.845(6) . ? F4 Sb2 1.862(5) . ? F5 Sb2 1.858(5) . ? F6 Sb1 1.860(5) . ? F7 Sb1 1.851(6) . ? F8 Sb1 1.854(6) . ? F9 Sb1 1.862(5) . ? F10 Sb1 1.855(5) . ? F11 Sb1 1.867(5) . ? F12 Sb2 1.839(6) . ? 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 N1 141.1(3) 2_665 . ? N3 Ag2 N2 163.9(2) 2_675 . ? C15 N1 N2 106.3(5) . . ? C15 N1 Ag1 137.5(5) . . ? N2 N1 Ag1 114.7(3) . . ? C16 N2 N1 107.3(5) . . ? C16 N2 Ag2 133.1(5) . . ? N1 N2 Ag2 117.9(3) . . ? C30 N3 Ag2 166.8(7) . 2_675 ? C1 N4 Ag1 151.9(8) . 2_665 ? N4 C1 C2 175.6(10) . . ? C3 C2 C7 121.2(7) . . ? C3 C2 C1 120.3(8) . . ? C7 C2 C1 118.4(7) . . ? C2 C3 C4 119.3(7) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 118.7(7) . . ? C5 C4 C8 120.3(7) . . ? C3 C4 C8 120.9(8) . . ? C4 C5 C6 121.3(8) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C7 C6 C5 119.9(9) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C6 C7 C2 119.6(8) . . ? C6 C7 H7 120.2 . . ? C2 C7 H7 120.2 . . ? O2 C8 C4 108.5(6) . . ? O2 C8 H8A 110.0 . . ? C4 C8 H8A 110.0 . . ? O2 C8 H8B 110.0 . . ? C4 C8 H8B 110.0 . . ? H8A C8 H8B 108.4 . . ? O2 C9 C10 122.8(6) . . ? O2 C9 C14 117.8(6) . . ? C10 C9 C14 119.5(6) . . ? C11 C10 C9 119.6(7) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C12 C11 C10 121.7(7) . . ? C12 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? C13 C12 C11 118.6(7) . . ? C13 C12 H12 120.7 . . ? C11 C12 H12 120.7 . . ? C12 C13 C14 122.0(7) . . ? C12 C13 H13 119.0 . . ? C14 C13 H13 119.0 . . ? C13 C14 C9 118.4(6) . . ? C13 C14 C15 118.6(6) . . ? C9 C14 C15 122.9(6) . . ? N1 C15 O1 111.7(6) . . ? N1 C15 C14 132.5(6) . . ? O1 C15 C14 115.6(5) . . ? N2 C16 O1 109.8(6) . . ? N2 C16 C17 133.5(6) . . ? O1 C16 C17 116.8(5) . . ? C18 C17 C22 118.5(6) . . ? C18 C17 C16 119.3(6) . . ? C22 C17 C16 122.3(6) . . ? C19 C18 C17 122.2(7) . . ? C19 C18 H18 118.9 . . ? C17 C18 H18 118.9 . . ? C18 C19 C20 119.0(7) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C21 C20 C19 121.0(7) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C22 C21 C20 118.5(7) . . ? C22 C21 H21 120.7 . . ? C20 C21 H21 120.7 . . ? C21 C22 O3 122.4(6) . . ? C21 C22 C17 120.7(6) . . ? O3 C22 C17 116.8(6) . . ? O3 C23 C24 105.9(5) . . ? O3 C23 H23A 110.6 . . ? C24 C23 H23A 110.6 . . ? O3 C23 H23B 110.6 . . ? C24 C23 H23B 110.6 . . ? H23A C23 H23B 108.7 . . ? C25 C24 C29 118.9(7) . . ? C25 C24 C23 119.5(6) . . ? C29 C24 C23 121.6(7) . . ? C26 C25 C24 120.8(7) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C25 C26 C27 120.7(8) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C26 C27 C28 119.0(8) . . ? C26 C27 H27 120.5 . . ? C28 C27 H27 120.5 . . ? C29 C28 C27 120.3(7) . . ? C29 C28 C30 121.2(7) . . ? C27 C28 C30 118.6(7) . . ? C28 C29 C24 120.3(7) . . ? C28 C29 H29 119.8 . . ? C24 C29 H29 119.8 . . ? N3 C30 C28 178.0(9) . . ? C16 O1 C15 104.9(5) . . ? C9 O2 C8 118.5(5) . . ? C22 O3 C23 117.3(5) . . ? F7 Sb1 F8 90.8(4) . . ? F7 Sb1 F10 91.3(3) . . ? F8 Sb1 F10 177.7(3) . . ? F7 Sb1 F6 88.2(3) . . ? F8 Sb1 F6 90.6(3) . . ? F10 Sb1 F6 90.3(3) . . ? F7 Sb1 F9 90.9(3) . . ? F8 Sb1 F9 89.5(3) . . ? F10 Sb1 F9 89.6(3) . . ? F6 Sb1 F9 179.0(3) . . ? F7 Sb1 F11 178.5(3) . . ? F8 Sb1 F11 90.0(3) . . ? F10 Sb1 F11 88.0(3) . . ? F6 Sb1 F11 90.6(2) . . ? F9 Sb1 F11 90.4(3) . . ? F12 Sb2 F3 176.9(3) . . ? F12 Sb2 F5 92.4(3) . . ? F3 Sb2 F5 90.6(3) . . ? F12 Sb2 F2 87.8(3) . . ? F3 Sb2 F2 89.2(3) . . ? F5 Sb2 F2 177.6(2) . . ? F12 Sb2 F4 89.2(3) . . ? F3 Sb2 F4 90.1(3) . . ? F5 Sb2 F4 88.0(2) . . ? F2 Sb2 F4 89.6(2) . . ? F12 Sb2 F1 91.5(3) . . ? F3 Sb2 F1 89.3(3) . . ? F5 Sb2 F1 90.5(2) . . ? F2 Sb2 F1 91.9(3) . . ? F4 Sb2 F1 178.4(2) . . ? 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 C15 170.0(7) 2_665 . . . ? N4 Ag1 N1 N2 -26.7(7) 2_665 . . . ? C15 N1 N2 C16 2.6(7) . . . . ? Ag1 N1 N2 C16 -165.8(4) . . . . ? C15 N1 N2 Ag2 -164.6(4) . . . . ? Ag1 N1 N2 Ag2 27.1(5) . . . . ? N3 Ag2 N2 C16 -143.6(9) 2_675 . . . ? N3 Ag2 N2 N1 19.5(12) 2_675 . . . ? Ag1 N4 C1 C2 12(13) 2_665 . . . ? N4 C1 C2 C3 147(12) . . . . ? N4 C1 C2 C7 -30(12) . . . . ? C7 C2 C3 C4 0.4(11) . . . . ? C1 C2 C3 C4 -177.1(7) . . . . ? C2 C3 C4 C5 0.3(11) . . . . ? C2 C3 C4 C8 -176.0(7) . . . . ? C3 C4 C5 C6 -1.3(12) . . . . ? C8 C4 C5 C6 175.0(8) . . . . ? C4 C5 C6 C7 1.6(14) . . . . ? C5 C6 C7 C2 -1.0(14) . . . . ? C3 C2 C7 C6 0.0(13) . . . . ? C1 C2 C7 C6 177.5(8) . . . . ? C5 C4 C8 O2 62.6(10) . . . . ? C3 C4 C8 O2 -121.2(8) . . . . ? O2 C9 C10 C11 177.4(8) . . . . ? C14 C9 C10 C11 -0.9(12) . . . . ? C9 C10 C11 C12 -3.4(14) . . . . ? C10 C11 C12 C13 5.9(14) . . . . ? C11 C12 C13 C14 -4.1(13) . . . . ? C12 C13 C14 C9 -0.2(12) . . . . ? C12 C13 C14 C15 176.2(7) . . . . ? O2 C9 C14 C13 -175.8(7) . . . . ? C10 C9 C14 C13 2.7(11) . . . . ? O2 C9 C14 C15 8.0(10) . . . . ? C10 C9 C14 C15 -173.5(7) . . . . ? N2 N1 C15 O1 -1.9(7) . . . . ? Ag1 N1 C15 O1 162.3(4) . . . . ? N2 N1 C15 C14 173.0(7) . . . . ? Ag1 N1 C15 C14 -22.7(12) . . . . ? C13 C14 C15 N1 -167.7(7) . . . . ? C9 C14 C15 N1 8.5(12) . . . . ? C13 C14 C15 O1 7.1(10) . . . . ? C9 C14 C15 O1 -176.7(6) . . . . ? N1 N2 C16 O1 -2.2(7) . . . . ? Ag2 N2 C16 O1 162.2(4) . . . . ? N1 N2 C16 C17 175.7(7) . . . . ? Ag2 N2 C16 C17 -19.9(12) . . . . ? N2 C16 C17 C18 169.0(8) . . . . ? O1 C16 C17 C18 -13.1(10) . . . . ? N2 C16 C17 C22 -12.4(12) . . . . ? O1 C16 C17 C22 165.5(6) . . . . ? C22 C17 C18 C19 0.3(12) . . . . ? C16 C17 C18 C19 179.0(8) . . . . ? C17 C18 C19 C20 -2.9(14) . . . . ? C18 C19 C20 C21 3.0(14) . . . . ? C19 C20 C21 C22 -0.5(14) . . . . ? C20 C21 C22 O3 -178.6(8) . . . . ? C20 C21 C22 C17 -2.2(12) . . . . ? C18 C17 C22 C21 2.3(11) . . . . ? C16 C17 C22 C21 -176.3(7) . . . . ? C18 C17 C22 O3 178.9(7) . . . . ? C16 C17 C22 O3 0.3(10) . . . . ? O3 C23 C24 C25 -58.4(9) . . . . ? O3 C23 C24 C29 123.7(7) . . . . ? C29 C24 C25 C26 -2.6(12) . . . . ? C23 C24 C25 C26 179.5(8) . . . . ? C24 C25 C26 C27 0.7(15) . . . . ? C25 C26 C27 C28 0.4(15) . . . . ? C26 C27 C28 C29 0.6(13) . . . . ? C26 C27 C28 C30 -178.8(8) . . . . ? C27 C28 C29 C24 -2.5(11) . . . . ? C30 C28 C29 C24 176.8(6) . . . . ? C25 C24 C29 C28 3.5(11) . . . . ? C23 C24 C29 C28 -178.6(7) . . . . ? Ag2 N3 C30 C28 -60(28) 2_675 . . . ? C29 C28 C30 N3 -88(27) . . . . ? C27 C28 C30 N3 91(27) . . . . ? N2 C16 O1 C15 1.1(7) . . . . ? C17 C16 O1 C15 -177.3(6) . . . . ? N1 C15 O1 C16 0.6(7) . . . . ? C14 C15 O1 C16 -175.3(6) . . . . ? C10 C9 O2 C8 -0.7(11) . . . . ? C14 C9 O2 C8 177.7(7) . . . . ? C4 C8 O2 C9 -169.4(7) . . . . ? C21 C22 O3 C23 16.6(11) . . . . ? C17 C22 O3 C23 -160.0(7) . . . . ? C24 C23 O3 C22 168.7(6) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.449 _refine_diff_density_min -0.761 _refine_diff_density_rms 0.133 #===End data_5 _database_code_depnum_ccdc_archive 'CCDC 791141' #TrackingRef '- CIF_1.1.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H11 Ag F3 N2 O5 S' _chemical_formula_weight 508.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 7.8557(10) _cell_length_b 18.207(2) _cell_length_c 13.4719(17) _cell_angle_alpha 90.00 _cell_angle_beta 103.544(2) _cell_angle_gamma 90.00 _cell_volume 1873.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5320 _cell_measurement_theta_min 2.667 _cell_measurement_theta_max 28.241 _exptl_crystal_description bar _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.802 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1004 _exptl_absorpt_coefficient_mu 1.247 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5745 _exptl_absorpt_correction_T_max 0.8855 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9857 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 25.49 _reflns_number_total 3596 _reflns_number_gt 3212 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0986P)^2^+3.7599P] 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 3596 _refine_ls_number_parameters 268 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0533 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1557 _refine_ls_wR_factor_gt 0.1528 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.132 _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 F2 F 1.1697(7) 0.7500 -0.0020(5) 0.086(2) Uani 1 2 d S . . F1 F 1.4129(5) 0.6911(2) 0.0246(4) 0.0738(12) Uani 1 1 d . . . C16 C 1.3326(10) 0.7500 0.0508(8) 0.053(2) Uani 1 2 d S . . O5 O 1.5255(6) 0.7500 0.2339(4) 0.0490(15) Uani 1 2 d S . . S1 S 1.3406(2) 0.7500 0.18716(17) 0.0407(5) Uani 1 2 d S . . O4 O 1.2521(5) 0.6836(2) 0.2010(4) 0.0572(11) Uani 1 1 d . . . Ag1 Ag 0.96275(5) 0.65332(2) 0.26274(3) 0.03645(19) Uani 1 1 d . . . O3 O 0.8558(7) 0.7500 0.3622(4) 0.0429(12) Uani 1 2 d S . . H3A H 0.9154 0.7500 0.4356 0.052 Uiso 1 2 d SR . . H3B H 0.7270 0.7500 0.3530 0.052 Uiso 1 2 d SR . . C1 C 0.8063(5) 0.6908(2) 0.0232(3) 0.0251(9) Uani 1 1 d . . . C2 C 0.7978(6) 0.6190(2) -0.0256(3) 0.0302(9) Uani 1 1 d . . . C3 C 0.8144(7) 0.6169(3) -0.1265(4) 0.0406(11) Uani 1 1 d . . . H3 H 0.8300 0.6614 -0.1600 0.049 Uiso 1 1 calc R . . C4 C 0.8085(8) 0.5511(3) -0.1788(4) 0.0497(14) Uani 1 1 d . . . H4 H 0.8208 0.5502 -0.2472 0.060 Uiso 1 1 calc R . . C5 C 0.7843(7) 0.4863(3) -0.1293(5) 0.0481(14) Uani 1 1 d . . . H5 H 0.7789 0.4409 -0.1648 0.058 Uiso 1 1 calc R . . C6 C 0.7682(7) 0.4867(3) -0.0298(4) 0.0408(12) Uani 1 1 d . . . H6 H 0.7524 0.4418 0.0029 0.049 Uiso 1 1 calc R . . C7 C 0.7749(6) 0.5528(2) 0.0233(4) 0.0312(10) Uani 1 1 d . . . C8 C 0.7214(7) 0.4913(3) 0.1708(4) 0.0406(11) Uani 1 1 d . . . H8A H 0.8164 0.4548 0.1757 0.049 Uiso 1 1 calc R . . H8B H 0.6111 0.4696 0.1306 0.049 Uiso 1 1 calc R . . C9 C 0.7024(6) 0.5123(3) 0.2751(4) 0.0361(11) Uani 1 1 d . . . C10 C 0.6099(7) 0.5746(3) 0.2887(4) 0.0407(12) Uani 1 1 d . . . H10 H 0.5602 0.6043 0.2313 0.049 Uiso 1 1 calc R . . C11 C 0.5881(7) 0.5948(3) 0.3837(4) 0.0460(13) Uani 1 1 d . . . H11 H 0.5224 0.6375 0.3909 0.055 Uiso 1 1 calc R . . C12 C 0.6632(7) 0.5523(3) 0.4699(4) 0.0463(13) Uani 1 1 d . . . H12 H 0.6526 0.5662 0.5361 0.056 Uiso 1 1 calc R . . C13 C 0.7536(6) 0.4890(3) 0.4549(4) 0.0435(13) Uani 1 1 d . . . C14 C 0.7753(7) 0.4688(3) 0.3591(4) 0.0410(12) Uani 1 1 d . . . H14 H 0.8393 0.4258 0.3512 0.049 Uiso 1 1 calc R . . C15 C 0.8278(7) 0.4457(3) 0.5433(4) 0.0480(14) Uani 1 1 d . . . C17 C 0.6948(11) 0.7500 0.6254(10) 0.152(6) Uani 1 2 d SDU . . F3 F 0.598(3) 0.7500 0.5272(11) 0.244(7) Uani 1 2 d SDU . . F4 F 0.613(2) 0.6915(10) 0.6581(15) 0.399(13) Uani 1 1 d DU . . N1 N 0.8410(5) 0.71130(19) 0.1181(3) 0.0241(7) Uani 1 1 d . . . N2 N 0.8883(6) 0.4123(3) 0.6143(4) 0.0521(13) Uani 1 1 d . . . O1 O 0.7810(6) 0.7500 -0.0401(3) 0.0276(9) Uani 1 2 d S . . O2 O 0.7625(5) 0.55748(18) 0.1226(3) 0.0373(8) Uani 1 1 d . . . O6 O 0.9896(19) 0.7500 0.7496(6) 0.278(13) Uani 1 2 d SDU . . O7 O 0.9540(14) 0.6863(7) 0.5892(12) 0.269(9) Uani 1 1 d DU . . S2 S 0.9425(6) 0.7500 0.6449(2) 0.1020(12) Uani 1 2 d SDU . . 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 F2 0.035(3) 0.138(6) 0.074(4) 0.000 -0.006(3) 0.000 F1 0.056(2) 0.074(3) 0.094(3) -0.029(2) 0.024(2) -0.003(2) C16 0.031(4) 0.050(5) 0.077(6) 0.000 0.012(4) 0.000 O5 0.034(3) 0.039(3) 0.071(4) 0.000 0.006(3) 0.000 S1 0.0285(8) 0.0213(8) 0.0735(13) 0.000 0.0144(8) 0.000 O4 0.043(2) 0.029(2) 0.103(3) 0.005(2) 0.024(2) -0.0068(17) Ag1 0.0443(3) 0.0313(3) 0.0303(3) 0.00744(13) 0.00185(18) 0.00446(14) O3 0.042(3) 0.047(3) 0.041(3) 0.000 0.013(2) 0.000 C1 0.027(2) 0.021(2) 0.026(2) 0.0022(17) 0.0046(16) 0.0009(17) C2 0.033(2) 0.025(2) 0.029(2) -0.0054(18) 0.0018(18) 0.0034(18) C3 0.052(3) 0.038(3) 0.031(2) -0.005(2) 0.007(2) 0.003(2) C4 0.059(3) 0.048(3) 0.038(3) -0.019(3) 0.003(2) 0.005(3) C5 0.045(3) 0.039(3) 0.055(3) -0.025(3) 0.001(2) 0.003(2) C6 0.038(3) 0.025(2) 0.056(3) -0.005(2) 0.005(2) 0.001(2) C7 0.033(2) 0.021(2) 0.037(2) -0.0038(18) 0.0031(19) 0.0002(18) C8 0.047(3) 0.022(2) 0.050(3) 0.009(2) 0.006(2) 0.000(2) C9 0.030(2) 0.028(2) 0.048(3) 0.012(2) 0.006(2) -0.0041(19) C10 0.038(3) 0.035(3) 0.047(3) 0.018(2) 0.004(2) 0.001(2) C11 0.048(3) 0.039(3) 0.051(3) 0.017(2) 0.012(2) 0.008(2) C12 0.049(3) 0.045(3) 0.047(3) 0.015(3) 0.013(2) -0.004(2) C13 0.028(2) 0.046(3) 0.054(3) 0.027(3) 0.003(2) -0.004(2) C14 0.033(2) 0.030(3) 0.057(3) 0.014(2) 0.005(2) 0.000(2) C15 0.037(3) 0.052(3) 0.052(3) 0.019(3) 0.004(2) -0.006(2) C17 0.185(9) 0.187(18) 0.101(9) 0.000 0.066(8) 0.000 F3 0.295(14) 0.262(18) 0.137(9) 0.000 -0.028(11) 0.000 F4 0.278(13) 0.47(3) 0.44(2) 0.30(2) 0.061(16) -0.072(16) N1 0.0289(18) 0.0173(17) 0.0251(17) 0.0007(14) 0.0042(14) -0.0009(14) N2 0.042(2) 0.059(3) 0.051(3) 0.029(3) 0.003(2) 0.002(2) O1 0.037(2) 0.021(2) 0.022(2) 0.000 0.0017(17) 0.000 O2 0.050(2) 0.0205(16) 0.0404(19) 0.0020(14) 0.0083(15) -0.0054(14) O6 0.267(16) 0.51(4) 0.050(6) 0.000 0.034(8) 0.000 O7 0.157(9) 0.248(12) 0.347(17) -0.215(13) -0.055(10) 0.071(10) S2 0.184(4) 0.088(2) 0.0471(15) 0.000 0.055(2) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 F2 C16 1.311(10) . ? F1 C16 1.333(6) . ? C16 F1 1.333(6) 4_575 ? C16 S1 1.823(10) . ? O5 S1 1.442(5) . ? S1 O4 1.429(4) . ? S1 O4 1.429(4) 4_575 ? O4 Ag1 2.654(4) . ? Ag1 N2 2.152(4) 3_766 ? Ag1 N1 2.226(3) . ? Ag1 O3 2.475(4) . ? O3 Ag1 2.475(4) 4_575 ? O3 H3A 0.9900 . ? O3 H3B 0.9900 . ? C1 N1 1.298(5) . ? C1 O1 1.360(5) . ? C1 C2 1.458(6) . ? C2 C3 1.397(7) . ? C2 C7 1.404(7) . ? C3 C4 1.384(7) . ? C3 H3 0.9500 . ? C4 C5 1.390(9) . ? C4 H4 0.9500 . ? C5 C6 1.376(8) . ? C5 H5 0.9500 . ? C6 C7 1.395(7) . ? C6 H6 0.9500 . ? C7 O2 1.366(6) . ? C8 O2 1.440(6) . ? C8 C9 1.497(8) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.383(7) . ? C9 C14 1.390(7) . ? C10 C11 1.381(8) . ? C10 H10 0.9500 . ? C11 C12 1.405(8) . ? C11 H11 0.9500 . ? C12 C13 1.393(8) . ? C12 H12 0.9500 . ? C13 C14 1.390(8) . ? C13 C15 1.434(7) . ? C14 H14 0.9500 . ? C15 N2 1.138(7) . ? C17 F3 1.363(9) . ? C17 F4 1.369(9) . ? C17 F4 1.369(9) 4_575 ? C17 S2 1.901(8) . ? N1 N1 1.409(7) 4_575 ? N2 Ag1 2.152(4) 3_766 ? O1 C1 1.360(5) 4_575 ? O6 S2 1.372(8) . ? O7 S2 1.395(7) . ? S2 O7 1.395(7) 4_575 ? 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 F2 C16 F1 108.6(6) . . ? F2 C16 F1 108.6(6) . 4_575 ? F1 C16 F1 107.1(7) . 4_575 ? F2 C16 S1 110.3(6) . . ? F1 C16 S1 111.1(5) . . ? F1 C16 S1 111.1(5) 4_575 . ? O4 S1 O4 115.6(4) . 4_575 ? O4 S1 O5 114.5(2) . . ? O4 S1 O5 114.5(2) 4_575 . ? O4 S1 C16 103.2(3) . . ? O4 S1 C16 103.2(3) 4_575 . ? O5 S1 C16 103.5(4) . . ? S1 O4 Ag1 134.0(2) . . ? N2 Ag1 N1 169.06(17) 3_766 . ? N2 Ag1 O3 99.81(19) 3_766 . ? N1 Ag1 O3 90.33(14) . . ? N2 Ag1 O4 90.29(17) 3_766 . ? N1 Ag1 O4 81.45(14) . . ? O3 Ag1 O4 116.49(13) . . ? Ag1 O3 Ag1 90.66(17) 4_575 . ? Ag1 O3 H3A 113.5 4_575 . ? Ag1 O3 H3A 113.5 . . ? Ag1 O3 H3B 113.5 4_575 . ? Ag1 O3 H3B 113.5 . . ? H3A O3 H3B 110.8 . . ? N1 C1 O1 110.8(4) . . ? N1 C1 C2 132.8(4) . . ? O1 C1 C2 116.3(4) . . ? C3 C2 C7 119.0(4) . . ? C3 C2 C1 117.3(4) . . ? C7 C2 C1 123.7(4) . . ? C4 C3 C2 121.3(5) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C3 C4 C5 118.9(5) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C6 C5 C4 121.1(5) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C5 C6 C7 120.2(5) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? O2 C7 C6 123.5(4) . . ? O2 C7 C2 116.9(4) . . ? C6 C7 C2 119.6(4) . . ? O2 C8 C9 107.0(4) . . ? O2 C8 H8A 110.3 . . ? C9 C8 H8A 110.3 . . ? O2 C8 H8B 110.3 . . ? C9 C8 H8B 110.3 . . ? H8A C8 H8B 108.6 . . ? C10 C9 C14 119.2(5) . . ? C10 C9 C8 120.3(4) . . ? C14 C9 C8 120.5(5) . . ? C11 C10 C9 121.6(5) . . ? C11 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? C10 C11 C12 120.0(5) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C13 C12 C11 117.8(5) . . ? C13 C12 H12 121.1 . . ? C11 C12 H12 121.1 . . ? C14 C13 C12 122.0(5) . . ? C14 C13 C15 120.8(5) . . ? C12 C13 C15 117.2(6) . . ? C9 C14 C13 119.3(5) . . ? C9 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? N2 C15 C13 178.8(7) . . ? F3 C17 F4 96.6(11) . . ? F3 C17 F4 96.6(11) . 4_575 ? F4 C17 F4 102(2) . 4_575 ? F3 C17 S2 117.1(13) . . ? F4 C17 S2 119.9(9) . . ? F4 C17 S2 119.9(9) 4_575 . ? C1 N1 N1 106.7(2) . 4_575 ? C1 N1 Ag1 132.4(3) . . ? N1 N1 Ag1 118.31(9) 4_575 . ? C15 N2 Ag1 170.8(5) . 3_766 ? C1 O1 C1 104.9(5) 4_575 . ? C7 O2 C8 117.7(4) . . ? O6 S2 O7 121.1(8) . . ? O6 S2 O7 121.1(8) . 4_575 ? O7 S2 O7 112.4(17) . 4_575 ? O6 S2 C17 99.4(6) . . ? O7 S2 C17 96.8(5) . . ? O7 S2 C17 96.8(5) 4_575 . ? 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 F2 C16 S1 O4 60.39(19) . . . . ? F1 C16 S1 O4 -60.0(5) . . . . ? F1 C16 S1 O4 -179.2(4) 4_575 . . . ? F2 C16 S1 O4 -60.39(19) . . . 4_575 ? F1 C16 S1 O4 179.2(4) . . . 4_575 ? F1 C16 S1 O4 60.0(5) 4_575 . . 4_575 ? F2 C16 S1 O5 180.000(1) . . . . ? F1 C16 S1 O5 59.6(4) . . . . ? F1 C16 S1 O5 -59.6(4) 4_575 . . . ? O4 S1 O4 Ag1 -5.9(7) 4_575 . . . ? O5 S1 O4 Ag1 130.4(4) . . . . ? C16 S1 O4 Ag1 -117.8(4) . . . . ? S1 O4 Ag1 N2 -121.3(4) . . . 3_766 ? S1 O4 Ag1 N1 65.9(4) . . . . ? S1 O4 Ag1 O3 -20.2(5) . . . . ? N2 Ag1 O3 Ag1 128.76(17) 3_766 . . 4_575 ? N1 Ag1 O3 Ag1 -47.12(16) . . . 4_575 ? O4 Ag1 O3 Ag1 33.5(2) . . . 4_575 ? N1 C1 C2 C3 -159.1(5) . . . . ? O1 C1 C2 C3 17.6(6) . . . . ? N1 C1 C2 C7 20.6(8) . . . . ? O1 C1 C2 C7 -162.7(4) . . . . ? C7 C2 C3 C4 0.1(8) . . . . ? C1 C2 C3 C4 179.8(5) . . . . ? C2 C3 C4 C5 0.5(8) . . . . ? C3 C4 C5 C6 -0.7(9) . . . . ? C4 C5 C6 C7 0.4(8) . . . . ? C5 C6 C7 O2 -179.0(5) . . . . ? C5 C6 C7 C2 0.2(7) . . . . ? C3 C2 C7 O2 178.8(4) . . . . ? C1 C2 C7 O2 -0.8(7) . . . . ? C3 C2 C7 C6 -0.4(7) . . . . ? C1 C2 C7 C6 179.9(4) . . . . ? O2 C8 C9 C10 44.0(6) . . . . ? O2 C8 C9 C14 -136.9(5) . . . . ? C14 C9 C10 C11 -0.1(8) . . . . ? C8 C9 C10 C11 179.1(5) . . . . ? C9 C10 C11 C12 1.1(8) . . . . ? C10 C11 C12 C13 -2.0(8) . . . . ? C11 C12 C13 C14 2.0(8) . . . . ? C11 C12 C13 C15 -179.3(5) . . . . ? C10 C9 C14 C13 0.0(7) . . . . ? C8 C9 C14 C13 -179.1(5) . . . . ? C12 C13 C14 C9 -1.1(8) . . . . ? C15 C13 C14 C9 -179.7(5) . . . . ? C14 C13 C15 N2 123(34) . . . . ? C12 C13 C15 N2 -56(34) . . . . ? O1 C1 N1 N1 -0.8(4) . . . 4_575 ? C2 C1 N1 N1 176.1(4) . . . 4_575 ? O1 C1 N1 Ag1 -161.5(3) . . . . ? C2 C1 N1 Ag1 15.3(7) . . . . ? N2 Ag1 N1 C1 36.7(10) 3_766 . . . ? O3 Ag1 N1 C1 -165.2(4) . . . . ? O4 Ag1 N1 C1 78.1(4) . . . . ? N2 Ag1 N1 N1 -122.3(8) 3_766 . . 4_575 ? O3 Ag1 N1 N1 35.82(11) . . . 4_575 ? O4 Ag1 N1 N1 -80.94(11) . . . 4_575 ? C13 C15 N2 Ag1 -85(35) . . . 3_766 ? N1 C1 O1 C1 1.2(6) . . . 4_575 ? C2 C1 O1 C1 -176.2(3) . . . 4_575 ? C6 C7 O2 C8 -6.9(7) . . . . ? C2 C7 O2 C8 173.9(4) . . . . ? C9 C8 O2 C7 -175.8(4) . . . . ? F3 C17 S2 O6 180.000(4) . . . . ? F4 C17 S2 O6 -63.8(14) . . . . ? F4 C17 S2 O6 63.8(14) 4_575 . . . ? F3 C17 S2 O7 -56.8(9) . . . . ? F4 C17 S2 O7 59.4(17) . . . . ? F4 C17 S2 O7 -173.0(16) 4_575 . . . ? F3 C17 S2 O7 56.8(9) . . . 4_575 ? F4 C17 S2 O7 173.0(16) . . . 4_575 ? F4 C17 S2 O7 -59.4(17) 4_575 . . 4_575 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3B O5 0.99 1.97 2.760(7) 134.7 1_455 O3 H3A O7 0.99 2.33 3.19(2) 145.1 . O3 H3A O7 0.99 2.33 3.19(2) 145.1 4_575 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.344 0.750 0.710 74.0 23.8 2 0.656 0.250 0.290 74.0 23.6 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.109 _refine_diff_density_min -1.685 _refine_diff_density_rms 0.144 #===End data_6 _database_code_depnum_ccdc_archive 'CCDC 791142' #TrackingRef '- CIF_1.1.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H31 Ag F6 N4 O4 Sb' _chemical_formula_weight 939.28 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 23.985(3) _cell_length_b 19.144(3) _cell_length_c 8.5795(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.577(3) _cell_angle_gamma 90.00 _cell_volume 3939.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3468 _cell_measurement_theta_min 2.374 _cell_measurement_theta_max 25.867 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1860 _exptl_absorpt_coefficient_mu 1.253 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5730 _exptl_absorpt_correction_T_max 0.7877 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10000 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 25.09 _reflns_number_total 3605 _reflns_number_gt 3069 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0892P)^2^+36.2943P] 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 3605 _refine_ls_number_parameters 239 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_gt 0.0648 _refine_ls_wR_factor_ref 0.1772 _refine_ls_wR_factor_gt 0.1691 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.5000 0.40636(3) 0.5000 0.0438(3) Uani 1 2 d S . . N1 N 0.41723(17) 0.4635(2) 0.5206(5) 0.0280(10) Uani 1 1 d . . . N2 N 0.0015(2) 0.1749(4) 1.2883(8) 0.0569(16) Uani 1 1 d . . . C1 C 0.3679(2) 0.4437(3) 0.5623(6) 0.0254(11) Uani 1 1 d . . . C2 C 0.3459(2) 0.3733(3) 0.5768(6) 0.0264(11) Uani 1 1 d . . . C3 C 0.3700(2) 0.3196(3) 0.4921(7) 0.0344(13) Uani 1 1 d . . . H3 H 0.3991 0.3289 0.4243 0.041 Uiso 1 1 calc R . . C4 C 0.3504(3) 0.2528(3) 0.5097(8) 0.0403(15) Uani 1 1 d . . . H4 H 0.3664 0.2166 0.4532 0.048 Uiso 1 1 calc R . . C5 C 0.3075(3) 0.2386(3) 0.6096(8) 0.0412(15) Uani 1 1 d . . . H5 H 0.2952 0.1929 0.6222 0.049 Uiso 1 1 calc R . . C6 C 0.2826(2) 0.2923(3) 0.6918(7) 0.0344(13) Uani 1 1 d . . . C7 C 0.3016(2) 0.3601(3) 0.6777(6) 0.0312(12) Uani 1 1 d . . . H7 H 0.2853 0.3961 0.7339 0.037 Uiso 1 1 calc R . . C8 C 0.2102(3) 0.3254(3) 0.8645(8) 0.0444(16) Uani 1 1 d . . . H8A H 0.1969 0.3604 0.7913 0.053 Uiso 1 1 calc R . . H8B H 0.2346 0.3480 0.9397 0.053 Uiso 1 1 calc R . . C9 C 0.1614(3) 0.2923(4) 0.9472(8) 0.0436(15) Uani 1 1 d . . . C10 C 0.1495(3) 0.2226(4) 0.9324(8) 0.0449(15) Uani 1 1 d . . . H10 H 0.1704 0.1949 0.8660 0.054 Uiso 1 1 calc R . . C11 C 0.1065(3) 0.1933(4) 1.0156(8) 0.0488(17) Uani 1 1 d . . . H11 H 0.0987 0.1459 1.0054 0.059 Uiso 1 1 calc R . . C12 C 0.0749(3) 0.2342(4) 1.1142(8) 0.0463(16) Uani 1 1 d . . . C13 C 0.0860(3) 0.3057(4) 1.1270(10) 0.065(2) Uani 1 1 d . . . H13 H 0.0643 0.3339 1.1906 0.078 Uiso 1 1 calc R . . C14 C 0.1295(3) 0.3338(4) 1.0440(10) 0.060(2) Uani 1 1 d . . . H14 H 0.1375 0.3812 1.0532 0.072 Uiso 1 1 calc R . . C15 C 0.0329(3) 0.2022(4) 1.2100(9) 0.0506(18) Uani 1 1 d . . . C16 C 0.4518(4) 0.5000 0.9176(14) 0.110(6) Uani 1 2 d SDU . . H16 H 0.4184 0.5000 0.8616 0.132 Uiso 1 2 calc SR . . C17 C 0.5010(6) 0.5000 0.8400(8) 0.165(10) Uani 1 2 d SDU . . H17 H 0.5015 0.5000 0.7316 0.198 Uiso 1 2 calc SR . . C18 C 0.5491(4) 0.5000 0.9224(15) 0.166(11) Uani 1 2 d SDU . . H18 H 0.5830 0.5000 0.8708 0.199 Uiso 1 2 calc SR . . C20 C 0.3597(10) 0.0603(14) 0.432(3) 0.215(10) Uiso 1 1 d D . . H20A H 0.3360 0.1009 0.4435 0.258 Uiso 1 1 calc R . . H20B H 0.3862 0.0678 0.3492 0.258 Uiso 1 1 calc R . . C21 C 0.3870(13) 0.0393(3) 0.581(3) 0.314(18) Uiso 1 1 d D . . H21A H 0.3663 0.0571 0.6691 0.377 Uiso 1 1 calc R . . H21B H 0.4248 0.0571 0.5867 0.377 Uiso 1 1 calc R . . O1 O 0.3346(2) 0.5000 0.5933(6) 0.0260(11) Uani 1 2 d S . . O2 O 0.23965(18) 0.2726(2) 0.7842(5) 0.0437(11) Uani 1 1 d . . . O3 O 0.3302(17) 0.0000 0.414(5) 0.37(2) Uiso 1 2 d SD . . Sb1 Sb 0.22485(4) 0.0000 0.86752(10) 0.0612(3) Uani 1 2 d S . . F1 F 0.1658(6) 0.0000 0.7355(11) 0.148(5) Uani 1 2 d S . . F2 F 0.2844(6) 0.0000 1.003(3) 0.232(10) Uani 1 2 d S . . F3 F 0.2592(5) 0.0702(5) 0.7647(15) 0.204(5) Uani 1 1 d . . . F4 F 0.1890(3) 0.0667(4) 0.9851(10) 0.129(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0265(4) 0.0291(4) 0.0762(6) 0.000 0.0263(3) 0.000 N1 0.023(2) 0.029(2) 0.032(3) -0.001(2) 0.0097(18) 0.0007(19) N2 0.038(3) 0.065(4) 0.068(4) 0.020(3) 0.017(3) -0.009(3) C1 0.023(3) 0.032(3) 0.022(3) -0.002(2) 0.008(2) 0.002(2) C2 0.020(2) 0.034(3) 0.025(3) 0.000(2) 0.003(2) -0.003(2) C3 0.030(3) 0.041(3) 0.032(3) -0.004(3) 0.011(2) -0.006(2) C4 0.036(3) 0.037(3) 0.048(4) -0.015(3) 0.007(3) -0.004(3) C5 0.038(3) 0.034(3) 0.051(4) 0.001(3) 0.004(3) -0.007(3) C6 0.028(3) 0.041(3) 0.034(3) 0.004(3) 0.009(2) -0.009(3) C7 0.031(3) 0.035(3) 0.028(3) 0.001(2) 0.007(2) -0.004(2) C8 0.047(4) 0.037(4) 0.049(4) 0.004(3) 0.023(3) -0.008(3) C9 0.040(3) 0.050(4) 0.040(4) 0.009(3) 0.011(3) -0.008(3) C10 0.045(4) 0.047(4) 0.043(4) 0.004(3) 0.014(3) -0.007(3) C11 0.048(4) 0.049(4) 0.050(4) 0.009(3) 0.006(3) -0.017(3) C12 0.034(3) 0.059(4) 0.046(4) 0.016(3) 0.012(3) -0.009(3) C13 0.060(5) 0.059(5) 0.077(6) 0.004(4) 0.038(4) -0.006(4) C14 0.059(4) 0.046(4) 0.075(5) 0.004(4) 0.030(4) -0.010(4) C15 0.036(3) 0.060(4) 0.056(4) 0.016(4) 0.010(3) -0.006(3) C16 0.126(10) 0.125(15) 0.081(11) 0.000 0.047(9) 0.000 C17 0.067(10) 0.19(2) 0.24(3) 0.000 0.037(10) 0.000 C18 0.131(11) 0.092(14) 0.27(4) 0.000 -0.041(18) 0.000 O1 0.021(2) 0.030(3) 0.027(3) 0.000 0.008(2) 0.000 O2 0.043(2) 0.044(2) 0.045(3) 0.003(2) 0.0205(19) -0.013(2) Sb1 0.0815(6) 0.0404(4) 0.0616(5) 0.000 -0.0037(4) 0.000 F1 0.181(11) 0.193(12) 0.067(6) 0.000 -0.052(7) 0.000 F2 0.163(12) 0.138(11) 0.39(3) 0.000 -0.185(15) 0.000 F3 0.186(9) 0.130(7) 0.297(14) 0.109(9) 0.094(9) -0.017(7) F4 0.141(6) 0.099(5) 0.145(6) -0.062(5) 0.012(5) 0.005(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.275(4) 2_656 ? Ag1 N1 2.275(4) . ? Ag1 N2 2.392(6) 8_554 ? Ag1 N2 2.392(6) 7_557 ? N1 C1 1.297(7) . ? N1 N1 1.397(9) 6_565 ? N2 C15 1.141(8) . ? N2 Ag1 2.392(6) 7_557 ? C1 O1 1.368(6) . ? C1 C2 1.454(8) . ? C2 C3 1.387(8) . ? C2 C7 1.401(7) . ? C3 C4 1.372(9) . ? C3 H3 0.9300 . ? C4 C5 1.374(9) . ? C4 H4 0.9300 . ? C5 C6 1.386(9) . ? C5 H5 0.9300 . ? C6 O2 1.360(7) . ? C6 C7 1.380(8) . ? C7 H7 0.9300 . ? C8 O2 1.416(8) . ? C8 C9 1.513(8) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.371(10) . ? C9 C14 1.386(10) . ? C10 C11 1.378(9) . ? C10 H10 0.9300 . ? C11 C12 1.384(10) . ? C11 H11 0.9300 . ? C12 C13 1.398(11) . ? C12 C15 1.444(9) . ? C13 C14 1.379(10) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C16 C17 1.362(8) . ? C16 C18 1.373(7) 5_667 ? C16 H16 0.9300 . ? C17 C18 1.346(9) . ? C17 H17 0.9300 . ? C18 C16 1.373(7) 5_667 ? C18 H18 0.9300 . ? C20 O3 1.363(10) . ? C20 C21 1.484(10) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C21 1.503(10) 6 ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? O1 C1 1.368(6) 6_565 ? O3 C20 1.363(10) 6 ? Sb1 F1 1.805(10) . ? Sb1 F3 1.811(7) 6 ? Sb1 F3 1.811(7) . ? Sb1 F2 1.831(11) . ? Sb1 F4 1.846(7) . ? Sb1 F4 1.846(7) 6 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N1 122.5(2) 2_656 . ? N1 Ag1 N2 103.52(18) 2_656 8_554 ? N1 Ag1 N2 113.04(18) . 8_554 ? N1 Ag1 N2 113.04(18) 2_656 7_557 ? N1 Ag1 N2 103.52(18) . 7_557 ? N2 Ag1 N2 98.9(3) 8_554 7_557 ? C1 N1 N1 107.0(3) . 6_565 ? C1 N1 Ag1 132.9(4) . . ? N1 N1 Ag1 118.74(11) 6_565 . ? C15 N2 Ag1 139.5(6) . 7_557 ? N1 C1 O1 111.1(5) . . ? N1 C1 C2 128.8(5) . . ? O1 C1 C2 120.1(4) . . ? C3 C2 C7 120.9(5) . . ? C3 C2 C1 119.3(5) . . ? C7 C2 C1 119.9(5) . . ? C4 C3 C2 119.2(5) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 120.8(6) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C4 C5 C6 120.0(6) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? O2 C6 C7 124.4(6) . . ? O2 C6 C5 115.0(5) . . ? C7 C6 C5 120.6(5) . . ? C6 C7 C2 118.5(5) . . ? C6 C7 H7 120.8 . . ? C2 C7 H7 120.8 . . ? O2 C8 C9 108.8(5) . . ? O2 C8 H8A 109.9 . . ? C9 C8 H8A 109.9 . . ? O2 C8 H8B 109.9 . . ? C9 C8 H8B 109.9 . . ? H8A C8 H8B 108.3 . . ? C10 C9 C14 119.8(6) . . ? C10 C9 C8 121.7(6) . . ? C14 C9 C8 118.4(6) . . ? C9 C10 C11 120.3(7) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C10 C11 C12 120.3(7) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C13 119.8(6) . . ? C11 C12 C15 119.9(7) . . ? C13 C12 C15 120.2(7) . . ? C14 C13 C12 119.1(7) . . ? C14 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? C13 C14 C9 120.7(7) . . ? C13 C14 H14 119.6 . . ? C9 C14 H14 119.6 . . ? N2 C15 C12 176.8(8) . . ? C17 C16 C18 120.8(6) . 5_667 ? C17 C16 H16 119.6 . . ? C18 C16 H16 119.6 5_667 . ? C18 C17 C16 119.0(6) . . ? C18 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? C17 C18 C16 120.2(6) . 5_667 ? C17 C18 H18 119.9 . . ? C16 C18 H18 119.9 5_667 . ? O3 C20 C21 95(3) . . ? O3 C20 H20A 112.7 . . ? C21 C20 H20A 112.7 . . ? O3 C20 H20B 112.7 . . ? C21 C20 H20B 112.7 . . ? H20A C20 H20B 110.1 . . ? C20 C21 C21 105.7(11) . 6 ? C20 C21 H21A 110.6 . . ? C21 C21 H21A 110.6 6 . ? C20 C21 H21B 110.6 . . ? C21 C21 H21B 110.6 6 . ? H21A C21 H21B 108.7 . . ? C1 O1 C1 103.9(5) 6_565 . ? C6 O2 C8 118.0(5) . . ? C20 O3 C20 116(4) 6 . ? F1 Sb1 F3 93.0(5) . 6 ? F1 Sb1 F3 93.0(5) . . ? F3 Sb1 F3 95.8(8) 6 . ? F1 Sb1 F2 179.5(9) . . ? F3 Sb1 F2 87.3(7) 6 . ? F3 Sb1 F2 87.3(7) . . ? F1 Sb1 F4 88.6(4) . . ? F3 Sb1 F4 175.5(5) 6 . ? F3 Sb1 F4 88.3(5) . . ? F2 Sb1 F4 91.1(6) . . ? F1 Sb1 F4 88.6(4) . 6 ? F3 Sb1 F4 88.3(5) 6 6 ? F3 Sb1 F4 175.5(5) . 6 ? F2 Sb1 F4 91.1(6) . 6 ? F4 Sb1 F4 87.6(6) . 6 ? 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 N1 Ag1 N1 C1 -164.6(5) 2_656 . . . ? N2 Ag1 N1 C1 70.4(5) 8_554 . . . ? N2 Ag1 N1 C1 -35.5(5) 7_557 . . . ? N1 Ag1 N1 N1 0.0 2_656 . . 6_565 ? N2 Ag1 N1 N1 -124.93(19) 8_554 . . 6_565 ? N2 Ag1 N1 N1 129.11(18) 7_557 . . 6_565 ? N1 N1 C1 O1 -1.1(5) 6_565 . . . ? Ag1 N1 C1 O1 164.9(4) . . . . ? N1 N1 C1 C2 178.3(5) 6_565 . . . ? Ag1 N1 C1 C2 -15.7(9) . . . . ? N1 C1 C2 C3 -23.9(9) . . . . ? O1 C1 C2 C3 155.4(5) . . . . ? N1 C1 C2 C7 154.9(6) . . . . ? O1 C1 C2 C7 -25.7(8) . . . . ? C7 C2 C3 C4 -0.9(9) . . . . ? C1 C2 C3 C4 177.9(5) . . . . ? C2 C3 C4 C5 0.0(9) . . . . ? C3 C4 C5 C6 1.4(10) . . . . ? C4 C5 C6 O2 178.4(6) . . . . ? C4 C5 C6 C7 -1.9(10) . . . . ? O2 C6 C7 C2 -179.3(5) . . . . ? C5 C6 C7 C2 0.9(9) . . . . ? C3 C2 C7 C6 0.5(8) . . . . ? C1 C2 C7 C6 -178.4(5) . . . . ? O2 C8 C9 C10 -3.1(9) . . . . ? O2 C8 C9 C14 174.6(7) . . . . ? C14 C9 C10 C11 -1.2(11) . . . . ? C8 C9 C10 C11 176.6(7) . . . . ? C9 C10 C11 C12 0.3(11) . . . . ? C10 C11 C12 C13 1.3(11) . . . . ? C10 C11 C12 C15 -175.2(7) . . . . ? C11 C12 C13 C14 -1.9(13) . . . . ? C15 C12 C13 C14 174.5(8) . . . . ? C12 C13 C14 C9 1.1(13) . . . . ? C10 C9 C14 C13 0.5(13) . . . . ? C8 C9 C14 C13 -177.3(8) . . . . ? Ag1 N2 C15 C12 13(17) 7_557 . . . ? C11 C12 C15 N2 53(17) . . . . ? C13 C12 C15 N2 -123(16) . . . . ? C18 C16 C17 C18 0.000(3) 5_667 . . . ? C16 C17 C18 C16 0.000(2) . . . 5_667 ? O3 C20 C21 C21 24(3) . . . 6 ? N1 C1 O1 C1 1.6(7) . . . 6_565 ? C2 C1 O1 C1 -177.8(3) . . . 6_565 ? C7 C6 O2 C8 3.9(9) . . . . ? C5 C6 O2 C8 -176.4(6) . . . . ? C9 C8 O2 C6 174.8(5) . . . . ? C21 C20 O3 C20 -48(5) . . . 6 ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.250 0.497 0.219 529.9 13 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 3.087 _refine_diff_density_min -1.348 _refine_diff_density_rms 0.145 #===End data_7 _database_code_depnum_ccdc_archive 'CCDC 791143' #TrackingRef '- CIF_1.1.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H23 Ag F6 N4 O3 P' _chemical_formula_weight 776.39 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' P P 0.1023 0.0942 '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/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 24.406(4) _cell_length_b 18.749(3) _cell_length_c 8.3657(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.991(2) _cell_angle_gamma 90.00 _cell_volume 3827.3(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2164 _cell_measurement_theta_min 2.729 _cell_measurement_theta_max 22.705 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.347 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1556 _exptl_absorpt_coefficient_mu 0.632 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8840 _exptl_absorpt_correction_T_max 0.9223 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9689 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3469 _reflns_number_gt 2737 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0945P)^2^+1.9623P] 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 3469 _refine_ls_number_parameters 228 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0744 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1616 _refine_ls_wR_factor_gt 0.1538 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.5000 0.09557(3) 0.0000 0.0442(2) Uani 1 2 d S . . C1 C 0.36944(16) 0.0571(3) 0.0520(5) 0.0309(10) Uani 1 1 d . . . C2 C 0.34779(17) 0.1290(3) 0.0698(5) 0.0312(10) Uani 1 1 d . . . C3 C 0.37166(18) 0.1846(3) -0.0136(6) 0.0380(11) Uani 1 1 d . . . H3 H 0.4006 0.1760 -0.0818 0.046 Uiso 1 1 calc R . . C4 C 0.35182(19) 0.2528(3) 0.0062(6) 0.0456(13) Uani 1 1 d . . . H4 H 0.3676 0.2904 -0.0490 0.055 Uiso 1 1 calc R . . C5 C 0.30877(19) 0.2659(3) 0.1071(6) 0.0411(12) Uani 1 1 d . . . H5 H 0.2958 0.3122 0.1203 0.049 Uiso 1 1 calc R . . C6 C 0.28506(17) 0.2099(3) 0.1885(5) 0.0347(11) Uani 1 1 d . . . C7 C 0.30371(17) 0.1419(3) 0.1704(5) 0.0325(10) Uani 1 1 d . . . H7 H 0.2873 0.1045 0.2245 0.039 Uiso 1 1 calc R . . C8 C 0.2133(2) 0.1741(3) 0.3600(6) 0.0449(12) Uani 1 1 d . . . H8A H 0.2371 0.1501 0.4371 0.054 Uiso 1 1 calc R . . H8B H 0.2009 0.1392 0.2817 0.054 Uiso 1 1 calc R . . C9 C 0.16484(19) 0.2059(3) 0.4433(6) 0.0406(12) Uani 1 1 d . . . C10 C 0.1328(2) 0.1624(3) 0.5376(7) 0.0614(16) Uani 1 1 d . . . H10 H 0.1405 0.1139 0.5444 0.074 Uiso 1 1 calc R . . C11 C 0.0894(2) 0.1900(3) 0.6216(7) 0.0621(16) Uani 1 1 d . . . H11 H 0.0684 0.1606 0.6858 0.074 Uiso 1 1 calc R . . C12 C 0.07750(19) 0.2629(3) 0.6090(6) 0.0457(13) Uani 1 1 d . . . C13 C 0.1088(2) 0.3057(3) 0.5138(6) 0.0437(12) Uani 1 1 d . . . H13 H 0.1007 0.3541 0.5051 0.052 Uiso 1 1 calc R . . C14 C 0.1524(2) 0.2776(3) 0.4305(6) 0.0433(12) Uani 1 1 d . . . H14 H 0.1733 0.3070 0.3660 0.052 Uiso 1 1 calc R . . C15 C 0.0352(2) 0.2946(3) 0.7042(6) 0.0477(13) Uani 1 1 d . . . C16 C 0.4999(4) 0.0000 0.3330(9) 0.171(8) Uani 1 2 d SD . . H16 H 0.4996 0.0000 0.2218 0.205 Uiso 1 2 calc SR . . C17 C 0.4523(3) 0.0000 0.4160(11) 0.100(4) Uani 1 2 d SD . . H17 H 0.4191 0.0000 0.3600 0.120 Uiso 1 2 calc SR . . C18 C 0.4521(3) 0.0000 0.5817(13) 0.155(7) Uani 1 2 d SD . . H18 H 0.4190 0.0000 0.6349 0.186 Uiso 1 2 calc SR . . F1 F 0.1847(2) 0.4411(2) 0.4834(6) 0.0990(14) Uani 1 1 d . . . F2 F 0.2623(3) 0.5000 0.5146(14) 0.168(4) Uani 1 2 d S . . F3 F 0.2469(3) 0.4396(3) 0.2994(9) 0.162(3) Uani 1 1 d . . . F4 F 0.1701(4) 0.5000 0.2603(8) 0.147(3) Uani 1 2 d S . . N1 N 0.41806(14) 0.0375(2) 0.0105(4) 0.0319(9) Uani 1 1 d . . . N2 N 0.00330(18) 0.3207(3) 0.7839(6) 0.0579(13) Uani 1 1 d . . . O1 O 0.33684(16) 0.0000 0.0823(5) 0.0308(10) Uani 1 2 d S . . O2 O 0.24225(13) 0.22892(19) 0.2838(4) 0.0441(8) Uani 1 1 d . . . P2 P 0.21552(10) 0.5000 0.3861(3) 0.0559(6) Uani 1 2 d S . . 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 0.0235(3) 0.0426(4) 0.0672(4) 0.000 0.0209(2) 0.000 C1 0.020(2) 0.049(3) 0.024(2) 0.003(2) 0.0074(17) 0.0012(19) C2 0.020(2) 0.045(3) 0.028(2) 0.000(2) 0.0003(17) 0.0042(19) C3 0.022(2) 0.053(3) 0.038(3) 0.008(2) 0.0048(19) 0.006(2) C4 0.034(3) 0.058(3) 0.044(3) 0.017(3) 0.007(2) 0.009(2) C5 0.037(3) 0.045(3) 0.041(3) 0.000(2) 0.000(2) 0.009(2) C6 0.025(2) 0.053(3) 0.026(2) -0.003(2) 0.0019(18) 0.008(2) C7 0.026(2) 0.047(3) 0.025(2) -0.002(2) 0.0018(18) 0.001(2) C8 0.039(3) 0.046(3) 0.050(3) -0.005(3) 0.015(2) 0.003(2) C9 0.031(3) 0.052(3) 0.039(3) -0.009(2) 0.007(2) 0.006(2) C10 0.058(4) 0.053(4) 0.074(4) 0.001(3) 0.032(3) 0.009(3) C11 0.056(4) 0.060(4) 0.070(4) 0.000(3) 0.028(3) 0.006(3) C12 0.028(2) 0.067(4) 0.042(3) -0.013(3) 0.005(2) 0.004(2) C13 0.038(3) 0.049(3) 0.044(3) -0.006(2) 0.002(2) 0.012(2) C14 0.039(3) 0.056(3) 0.036(3) -0.005(2) 0.008(2) 0.004(2) C15 0.034(3) 0.064(4) 0.046(3) -0.012(3) 0.002(2) 0.005(2) C16 0.100(12) 0.134(14) 0.28(2) 0.000 0.070(15) 0.000 C17 0.105(10) 0.116(10) 0.081(8) 0.000 0.049(7) 0.000 C18 0.109(12) 0.158(16) 0.196(19) 0.000 -0.060(13) 0.000 F1 0.114(4) 0.076(3) 0.108(3) 0.029(3) 0.011(3) -0.006(3) F2 0.116(6) 0.118(6) 0.268(11) 0.000 -0.112(7) 0.000 F3 0.159(6) 0.108(4) 0.222(7) -0.055(5) 0.094(5) 0.006(4) F4 0.196(8) 0.165(7) 0.076(4) 0.000 -0.082(5) 0.000 N1 0.0239(19) 0.043(2) 0.029(2) 0.0015(16) 0.0077(15) -0.0015(16) N2 0.037(3) 0.078(4) 0.059(3) -0.014(3) 0.013(2) 0.006(2) O1 0.018(2) 0.046(3) 0.029(2) 0.000 0.0059(17) 0.000 O2 0.0337(18) 0.050(2) 0.049(2) -0.0055(17) 0.0151(15) 0.0074(15) P2 0.0682(15) 0.0499(13) 0.0496(13) 0.000 -0.0008(10) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.280(3) 2_655 ? Ag1 N1 2.280(3) . ? Ag1 N2 2.397(5) 7_556 ? Ag1 N2 2.397(5) 8_554 ? C1 N1 1.295(5) . ? C1 O1 1.360(5) . ? C1 C2 1.457(7) . ? C2 C3 1.388(7) . ? C2 C7 1.399(6) . ? C3 C4 1.378(7) . ? C3 H3 0.9300 . ? C4 C5 1.381(6) . ? C4 H4 0.9300 . ? C5 C6 1.384(7) . ? C5 H5 0.9300 . ? C6 C7 1.363(7) . ? C6 O2 1.372(5) . ? C7 H7 0.9300 . ? C8 O2 1.407(6) . ? C8 C9 1.506(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C14 1.382(7) . ? C9 C10 1.387(8) . ? C10 C11 1.381(7) . ? C10 H10 0.9300 . ? C11 C12 1.401(8) . ? C11 H11 0.9300 . ? C12 C13 1.372(7) . ? C12 C15 1.443(7) . ? C13 C14 1.387(7) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 N2 1.144(6) . ? C16 C18 1.360(6) 5_656 ? C16 C17 1.364(8) . ? C16 H16 0.9300 . ? C17 C18 1.386(8) . ? C17 H17 0.9300 . ? C18 C16 1.360(6) 5_656 ? C18 H18 0.9300 . ? F1 P2 1.570(5) . ? F2 P2 1.554(7) . ? F3 P2 1.554(5) . ? F4 P2 1.515(7) . ? N1 N1 1.405(7) 6 ? N2 Ag1 2.397(5) 7_556 ? O1 C1 1.360(5) 6 ? P2 F3 1.554(5) 6_565 ? P2 F1 1.570(5) 6_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N1 122.93(19) 2_655 . ? N1 Ag1 N2 112.52(14) 2_655 7_556 ? N1 Ag1 N2 104.05(14) . 7_556 ? N1 Ag1 N2 104.05(14) 2_655 8_554 ? N1 Ag1 N2 112.52(14) . 8_554 ? N2 Ag1 N2 98.2(3) 7_556 8_554 ? N1 C1 O1 111.6(4) . . ? N1 C1 C2 128.7(4) . . ? O1 C1 C2 119.7(3) . . ? C3 C2 C7 120.4(4) . . ? C3 C2 C1 119.2(4) . . ? C7 C2 C1 120.4(4) . . ? C4 C3 C2 119.0(4) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 120.8(5) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C4 C5 C6 119.6(5) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C7 C6 O2 124.5(4) . . ? C7 C6 C5 120.8(4) . . ? O2 C6 C5 114.7(4) . . ? C6 C7 C2 119.4(4) . . ? C6 C7 H7 120.3 . . ? C2 C7 H7 120.3 . . ? O2 C8 C9 108.9(4) . . ? O2 C8 H8A 109.9 . . ? C9 C8 H8A 109.9 . . ? O2 C8 H8B 109.9 . . ? C9 C8 H8B 109.9 . . ? H8A C8 H8B 108.3 . . ? C14 C9 C10 119.4(5) . . ? C14 C9 C8 121.5(5) . . ? C10 C9 C8 119.1(5) . . ? C11 C10 C9 120.9(6) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 C12 119.2(5) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C13 C12 C11 119.8(5) . . ? C13 C12 C15 119.4(5) . . ? C11 C12 C15 120.6(5) . . ? C12 C13 C14 120.6(5) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C9 C14 C13 120.1(5) . . ? C9 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? N2 C15 C12 177.1(6) . . ? C18 C16 C17 117.7(7) 5_656 . ? C18 C16 H16 121.1 5_656 . ? C17 C16 H16 121.1 . . ? C16 C17 C18 121.8(7) . . ? C16 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? C16 C18 C17 120.5(8) 5_656 . ? C16 C18 H18 119.7 5_656 . ? C17 C18 H18 119.7 . . ? C1 N1 N1 106.5(3) . 6 ? C1 N1 Ag1 133.1(3) . . ? N1 N1 Ag1 118.53(9) 6 . ? C15 N2 Ag1 138.8(4) . 7_556 ? C1 O1 C1 103.8(4) . 6 ? C6 O2 C8 117.8(4) . . ? F4 P2 F2 179.7(6) . . ? F4 P2 F3 92.1(4) . . ? F2 P2 F3 87.7(5) . . ? F4 P2 F3 92.1(4) . 6_565 ? F2 P2 F3 87.7(5) . 6_565 ? F3 P2 F3 93.5(5) . 6_565 ? F4 P2 F1 90.5(3) . . ? F2 P2 F1 89.6(4) . . ? F3 P2 F1 88.5(3) . . ? F3 P2 F1 176.6(4) 6_565 . ? F4 P2 F1 90.5(3) . 6_565 ? F2 P2 F1 89.6(4) . 6_565 ? F3 P2 F1 176.6(4) . 6_565 ? F3 P2 F1 88.5(3) 6_565 6_565 ? F1 P2 F1 89.4(4) . 6_565 ? 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 N1 C1 C2 C3 24.3(7) . . . . ? O1 C1 C2 C3 -156.4(4) . . . . ? N1 C1 C2 C7 -155.3(4) . . . . ? O1 C1 C2 C7 24.0(6) . . . . ? C7 C2 C3 C4 1.0(7) . . . . ? C1 C2 C3 C4 -178.6(4) . . . . ? C2 C3 C4 C5 -0.1(7) . . . . ? C3 C4 C5 C6 -0.4(7) . . . . ? C4 C5 C6 C7 0.1(7) . . . . ? C4 C5 C6 O2 -179.2(4) . . . . ? O2 C6 C7 C2 -180.0(4) . . . . ? C5 C6 C7 C2 0.8(6) . . . . ? C3 C2 C7 C6 -1.3(6) . . . . ? C1 C2 C7 C6 178.3(4) . . . . ? O2 C8 C9 C14 3.8(7) . . . . ? O2 C8 C9 C10 -174.8(5) . . . . ? C14 C9 C10 C11 -1.5(9) . . . . ? C8 C9 C10 C11 177.1(5) . . . . ? C9 C10 C11 C12 0.9(9) . . . . ? C10 C11 C12 C13 0.0(9) . . . . ? C10 C11 C12 C15 -175.4(5) . . . . ? C11 C12 C13 C14 -0.3(8) . . . . ? C15 C12 C13 C14 175.1(5) . . . . ? C10 C9 C14 C13 1.2(8) . . . . ? C8 C9 C14 C13 -177.5(5) . . . . ? C12 C13 C14 C9 -0.3(8) . . . . ? C13 C12 C15 N2 -75(13) . . . . ? C11 C12 C15 N2 101(13) . . . . ? C18 C16 C17 C18 0.000(1) 5_656 . . . ? C16 C17 C18 C16 0.000(1) . . . 5_656 ? O1 C1 N1 N1 0.9(4) . . . 6 ? C2 C1 N1 N1 -179.7(4) . . . 6 ? O1 C1 N1 Ag1 -162.5(3) . . . . ? C2 C1 N1 Ag1 16.8(7) . . . . ? N1 Ag1 N1 C1 161.9(4) 2_655 . . . ? N2 Ag1 N1 C1 32.7(4) 7_556 . . . ? N2 Ag1 N1 C1 -72.5(4) 8_554 . . . ? N1 Ag1 N1 N1 0.0 2_655 . . 6 ? N2 Ag1 N1 N1 -129.24(13) 7_556 . . 6 ? N2 Ag1 N1 N1 125.57(14) 8_554 . . 6 ? C12 C15 N2 Ag1 12(14) . . . 7_556 ? N1 C1 O1 C1 -1.4(6) . . . 6 ? C2 C1 O1 C1 179.2(2) . . . 6 ? C7 C6 O2 C8 -4.3(6) . . . . ? C5 C6 O2 C8 174.9(4) . . . . ? C9 C8 O2 C6 -174.1(4) . . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 -0.012 534.4 34.0 2 0.500 0.500 -0.015 534.4 34.0 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.437 _refine_diff_density_min -0.845 _refine_diff_density_rms 0.103 #===End data_8 _database_code_depnum_ccdc_archive 'CCDC 791144' #TrackingRef '- CIF_1.1.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H23 Ag Cl N4 O7' _chemical_formula_weight 730.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 24.970(19) _cell_length_b 18.714(14) _cell_length_c 8.194(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.02(2) _cell_angle_gamma 90.00 _cell_volume 3829(5) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2320 _cell_measurement_theta_min 2.485 _cell_measurement_theta_max 21.061 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.268 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1476 _exptl_absorpt_coefficient_mu 0.641 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7835 _exptl_absorpt_correction_T_max 0.7927 _exptl_absorpt_process_details sadbs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10143 _diffrn_reflns_av_R_equivalents 0.0550 _diffrn_reflns_av_sigmaI/netI 0.0736 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 25.50 _reflns_number_total 3650 _reflns_number_gt 2188 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0790P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3650 _refine_ls_number_parameters 219 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0881 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1485 _refine_ls_wR_factor_gt 0.1364 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.976 _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 0.0000 0.09568(3) 0.0000 0.0673(3) Uani 1 2 d S . . C1 C 0.12923(17) 0.0579(2) 0.0384(5) 0.0492(10) Uani 1 1 d . . . C2 C 0.15038(16) 0.1294(2) 0.0574(5) 0.0494(10) Uani 1 1 d . . . C3 C 0.12609(19) 0.1853(3) -0.0209(5) 0.0624(12) Uani 1 1 d . . . H3 H 0.0973 0.1772 -0.0905 0.075 Uiso 1 1 calc R . . C4 C 0.1447(2) 0.2540(3) 0.0045(6) 0.0713(14) Uani 1 1 d . . . H4 H 0.1276 0.2922 -0.0458 0.086 Uiso 1 1 calc R . . C5 C 0.1882(2) 0.2664(3) 0.1031(6) 0.0671(13) Uani 1 1 d . . . H5 H 0.2011 0.3126 0.1175 0.081 Uiso 1 1 calc R . . C6 C 0.21260(17) 0.2097(3) 0.1803(5) 0.0564(11) Uani 1 1 d . . . C7 C 0.19474(16) 0.1411(3) 0.1578(5) 0.0531(11) Uani 1 1 d . . . H7 H 0.2119 0.1030 0.2085 0.064 Uiso 1 1 calc R . . C8 C 0.2844(2) 0.1736(3) 0.3515(6) 0.0714(14) Uani 1 1 d . . . H8A H 0.2955 0.1390 0.2702 0.086 Uiso 1 1 calc R . . H8B H 0.2624 0.1493 0.4319 0.086 Uiso 1 1 calc R . . C9 C 0.33314(19) 0.2058(3) 0.4333(5) 0.0626(13) Uani 1 1 d . . . C10 C 0.3422(2) 0.2781(3) 0.4292(5) 0.0655(13) Uani 1 1 d . . . H10 H 0.3194 0.3078 0.3704 0.079 Uiso 1 1 calc R . . C11 C 0.3856(2) 0.3070(3) 0.5134(6) 0.0711(14) Uani 1 1 d . . . H11 H 0.3920 0.3559 0.5097 0.085 Uiso 1 1 calc R . . C12 C 0.4187(2) 0.2635(3) 0.6011(6) 0.0685(14) Uani 1 1 d . . . C13 C 0.4099(2) 0.1908(3) 0.6012(7) 0.0938(18) Uani 1 1 d . . . H13 H 0.4333 0.1608 0.6570 0.113 Uiso 1 1 calc R . . C14 C 0.3667(2) 0.1622(3) 0.5193(7) 0.0925(18) Uani 1 1 d . . . H14 H 0.3604 0.1132 0.5226 0.111 Uiso 1 1 calc R . . C15 C 0.4612(2) 0.2937(3) 0.6973(6) 0.0736(14) Uani 1 1 d . . . Cl2 Cl 0.20880(17) 0.0000 0.5891(4) 0.1273(10) Uani 1 2 d S . . N1 N 0.08158(13) 0.03791(17) 0.0004(4) 0.0514(9) Uani 1 1 d . . . N2 N 0.49278(18) 0.3200(3) 0.7761(5) 0.0856(14) Uani 1 1 d . . . O1 O 0.16150(15) 0.0000 0.0631(4) 0.0520(10) Uani 1 2 d S . . O2 O 0.25484(13) 0.22844(17) 0.2771(4) 0.0702(9) Uani 1 1 d . . . O3 O 0.1783(9) 0.0000 0.4517(14) 0.283(8) Uani 1 2 d S . . O4 O 0.2054(5) 0.0592(4) 0.6713(8) 0.270(6) Uani 1 1 d . . . O5 O 0.2529(7) 0.0000 0.497(3) 0.328(10) Uani 1 2 d S . . C16 C 0.5029(5) 0.5000 0.6709(6) 0.223(10) Uani 1 2 d SD . . H16 H 0.5046 0.5000 0.7842 0.268 Uiso 1 2 calc SR . . C18 C 0.4508(4) 0.5000 0.4195(13) 0.229(10) Uani 1 2 d SD . . H18 H 0.4178 0.5000 0.3672 0.275 Uiso 1 2 calc SR . . C17 C 0.4533(4) 0.5000 0.5928(13) 0.194(7) Uani 1 2 d SD . . H17 H 0.4219 0.5000 0.6538 0.233 Uiso 1 2 calc SR . . 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 0.0435(3) 0.0723(4) 0.0860(4) 0.000 -0.0251(3) 0.000 C1 0.040(2) 0.072(3) 0.036(2) 0.001(2) -0.0100(19) 0.003(2) C2 0.042(2) 0.068(3) 0.038(2) 0.003(2) -0.0069(19) -0.006(2) C3 0.052(3) 0.081(3) 0.054(3) 0.008(2) -0.011(2) -0.009(2) C4 0.066(3) 0.081(4) 0.067(3) 0.020(3) -0.012(3) 0.001(3) C5 0.063(3) 0.068(3) 0.070(3) 0.004(2) -0.005(3) -0.019(2) C6 0.044(3) 0.077(3) 0.048(3) 0.000(2) -0.004(2) -0.012(2) C7 0.039(2) 0.074(3) 0.046(2) -0.001(2) -0.0078(19) -0.002(2) C8 0.065(3) 0.079(3) 0.070(3) -0.009(3) -0.021(3) -0.014(3) C9 0.053(3) 0.082(4) 0.053(3) -0.011(2) -0.010(2) -0.010(2) C10 0.060(3) 0.078(3) 0.058(3) -0.001(2) -0.011(2) -0.013(3) C11 0.065(3) 0.085(4) 0.063(3) -0.004(3) -0.007(3) -0.021(3) C12 0.055(3) 0.093(4) 0.057(3) -0.021(3) -0.007(2) -0.016(3) C13 0.088(4) 0.092(4) 0.101(4) -0.006(3) -0.046(4) -0.005(3) C14 0.089(4) 0.081(4) 0.108(4) -0.007(3) -0.046(4) -0.014(3) C15 0.062(3) 0.093(4) 0.066(3) -0.016(3) -0.009(3) -0.014(3) Cl2 0.193(4) 0.0891(19) 0.099(2) 0.000 0.030(2) 0.000 N1 0.0355(19) 0.0596(19) 0.059(2) 0.0014(16) -0.0148(17) -0.0015(15) N2 0.064(3) 0.109(3) 0.084(3) -0.027(3) -0.025(2) -0.011(3) O1 0.035(2) 0.077(3) 0.044(2) 0.000 -0.0125(18) 0.000 O2 0.058(2) 0.079(2) 0.074(2) -0.0051(17) -0.0238(17) -0.0134(16) O3 0.43(3) 0.310(17) 0.107(7) 0.000 -0.016(12) 0.000 O4 0.536(18) 0.109(4) 0.164(6) -0.043(4) -0.010(8) 0.083(8) O5 0.30(2) 0.258(15) 0.43(2) 0.000 0.22(2) 0.000 C16 0.26(2) 0.129(11) 0.283(19) 0.000 -0.19(2) 0.000 C18 0.195(18) 0.28(2) 0.211(18) 0.000 0.121(16) 0.000 C17 0.256(19) 0.206(14) 0.120(9) 0.000 -0.117(11) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.306(4) 2 ? Ag1 N1 2.306(4) . ? Ag1 N2 2.427(5) 7_556 ? Ag1 N2 2.427(5) 8_454 ? C1 N1 1.285(5) . ? C1 O1 1.365(5) . ? C1 C2 1.447(6) . ? C2 C3 1.370(6) . ? C2 C7 1.397(5) . ? C3 C4 1.382(7) . ? C3 H3 0.9300 . ? C4 C5 1.373(6) . ? C4 H4 0.9300 . ? C5 C6 1.377(6) . ? C5 H5 0.9300 . ? C6 O2 1.365(5) . ? C6 C7 1.371(6) . ? C7 H7 0.9300 . ? C8 O2 1.403(6) . ? C8 C9 1.514(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C14 1.366(7) . ? C9 C10 1.371(7) . ? C10 C11 1.394(6) . ? C10 H10 0.9300 . ? C11 C12 1.364(7) . ? C11 H11 0.9300 . ? C12 C13 1.378(8) . ? C12 C15 1.437(6) . ? C13 C14 1.378(7) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 N2 1.131(6) . ? Cl2 O4 1.300(6) . ? Cl2 O4 1.300(6) 6 ? Cl2 O5 1.335(13) . ? Cl2 O3 1.358(13) . ? N1 N1 1.419(6) 6 ? N2 Ag1 2.427(5) 7_556 ? O1 C1 1.365(5) 6 ? C16 C18 1.373(6) 5_666 ? C16 C17 1.393(8) . ? C16 H16 0.9300 . ? C18 C16 1.373(6) 5_666 ? C18 C17 1.421(8) . ? C18 H18 0.9300 . ? C17 H17 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N1 124.09(17) 2 . ? N1 Ag1 N2 111.81(14) 2 7_556 ? N1 Ag1 N2 103.80(13) . 7_556 ? N1 Ag1 N2 103.80(13) 2 8_454 ? N1 Ag1 N2 111.81(14) . 8_454 ? N2 Ag1 N2 98.8(2) 7_556 8_454 ? N1 C1 O1 110.6(4) . . ? N1 C1 C2 129.3(4) . . ? O1 C1 C2 120.2(3) . . ? C3 C2 C7 120.4(4) . . ? C3 C2 C1 119.7(4) . . ? C7 C2 C1 119.9(4) . . ? C2 C3 C4 119.4(4) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 120.8(5) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 119.3(4) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? O2 C6 C7 124.8(4) . . ? O2 C6 C5 114.2(4) . . ? C7 C6 C5 121.0(4) . . ? C6 C7 C2 119.0(4) . . ? C6 C7 H7 120.5 . . ? C2 C7 H7 120.5 . . ? O2 C8 C9 108.9(4) . . ? O2 C8 H8A 109.9 . . ? C9 C8 H8A 109.9 . . ? O2 C8 H8B 109.9 . . ? C9 C8 H8B 109.9 . . ? H8A C8 H8B 108.3 . . ? C14 C9 C10 120.1(4) . . ? C14 C9 C8 118.9(5) . . ? C10 C9 C8 120.9(4) . . ? C9 C10 C11 119.9(5) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C12 C11 C10 120.1(5) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 119.4(5) . . ? C11 C12 C15 120.1(5) . . ? C13 C12 C15 120.4(5) . . ? C12 C13 C14 120.6(5) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C9 C14 C13 119.9(5) . . ? C9 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? N2 C15 C12 176.4(6) . . ? O4 Cl2 O4 117.0(7) . 6 ? O4 Cl2 O5 110.3(7) . . ? O4 Cl2 O5 110.3(7) 6 . ? O4 Cl2 O3 113.2(6) . . ? O4 Cl2 O3 113.2(6) 6 . ? O5 Cl2 O3 89.6(11) . . ? C1 N1 N1 106.9(3) . 6 ? C1 N1 Ag1 133.0(3) . . ? N1 N1 Ag1 117.96(8) 6 . ? C15 N2 Ag1 140.0(4) . 7_556 ? C1 O1 C1 105.0(4) 6 . ? C6 O2 C8 118.1(4) . . ? C18 C16 C17 120.0(5) 5_666 . ? C18 C16 H16 120.0 5_666 . ? C17 C16 H16 120.0 . . ? C16 C18 C17 120.2(10) 5_666 . ? C16 C18 H18 119.9 5_666 . ? C17 C18 H18 119.9 . . ? C16 C17 C18 119.8(9) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? 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 N1 C1 C2 C3 -24.1(7) . . . . ? O1 C1 C2 C3 156.5(4) . . . . ? N1 C1 C2 C7 154.7(4) . . . . ? O1 C1 C2 C7 -24.7(6) . . . . ? C7 C2 C3 C4 -2.1(7) . . . . ? C1 C2 C3 C4 176.6(4) . . . . ? C2 C3 C4 C5 2.0(7) . . . . ? C3 C4 C5 C6 -1.6(7) . . . . ? C4 C5 C6 O2 -179.0(4) . . . . ? C4 C5 C6 C7 1.3(7) . . . . ? O2 C6 C7 C2 178.9(4) . . . . ? C5 C6 C7 C2 -1.4(7) . . . . ? C3 C2 C7 C6 1.8(6) . . . . ? C1 C2 C7 C6 -176.9(4) . . . . ? O2 C8 C9 C14 177.4(5) . . . . ? O2 C8 C9 C10 1.0(6) . . . . ? C14 C9 C10 C11 -0.2(8) . . . . ? C8 C9 C10 C11 176.3(4) . . . . ? C9 C10 C11 C12 -0.7(7) . . . . ? C10 C11 C12 C13 2.2(8) . . . . ? C10 C11 C12 C15 -175.5(5) . . . . ? C11 C12 C13 C14 -2.8(9) . . . . ? C15 C12 C13 C14 174.9(5) . . . . ? C10 C9 C14 C13 -0.4(9) . . . . ? C8 C9 C14 C13 -176.9(5) . . . . ? C12 C13 C14 C9 1.9(9) . . . . ? C11 C12 C15 N2 47(10) . . . . ? C13 C12 C15 N2 -131(10) . . . . ? O1 C1 N1 N1 0.3(4) . . . 6 ? C2 C1 N1 N1 -179.1(4) . . . 6 ? O1 C1 N1 Ag1 162.7(3) . . . . ? C2 C1 N1 Ag1 -16.8(7) . . . . ? N1 Ag1 N1 C1 -160.8(4) 2 . . . ? N2 Ag1 N1 C1 -31.9(4) 7_556 . . . ? N2 Ag1 N1 C1 73.7(4) 8_454 . . . ? N1 Ag1 N1 N1 0.0 2 . . 6 ? N2 Ag1 N1 N1 128.90(13) 7_556 . . 6 ? N2 Ag1 N1 N1 -125.51(13) 8_454 . . 6 ? C12 C15 N2 Ag1 13(10) . . . 7_556 ? N1 C1 O1 C1 -0.5(6) . . . 6 ? C2 C1 O1 C1 179.0(2) . . . 6 ? C7 C6 O2 C8 4.1(6) . . . . ? C5 C6 O2 C8 -175.6(4) . . . . ? C9 C8 O2 C6 172.5(4) . . . . ? C18 C16 C17 C18 0.000(1) 5_666 . . . ? C16 C18 C17 C16 0.000(1) 5_666 . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.500 0.000 -0.012 566.1 20.5 2 0.000 0.500 -0.014 566.1 20.5 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.028 _refine_diff_density_min -0.580 _refine_diff_density_rms 0.087 #===End data_9 _database_code_depnum_ccdc_archive 'CCDC 791145' #TrackingRef '- CIF_1.1.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H20 Ag F6 N4 O3 Sb' _chemical_formula_weight 828.12 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' Sb Sb -0.5866 1.5461 '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/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 14.038(3) _cell_length_b 18.203(3) _cell_length_c 13.527(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.894(3) _cell_angle_gamma 90.00 _cell_volume 3423.9(10) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2426 _cell_measurement_theta_min 2.237 _cell_measurement_theta_max 20.751 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.607 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 1.428 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6274 _exptl_absorpt_correction_T_max 0.8361 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8639 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3108 _reflns_number_gt 2437 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1295P)^2^+32.3780P] 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 3108 _refine_ls_number_parameters 243 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1073 _refine_ls_R_factor_gt 0.0923 _refine_ls_wR_factor_ref 0.2609 _refine_ls_wR_factor_gt 0.2513 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _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 0.5000 0.39967(5) 0.0000 0.0674(4) Uani 1 2 d S . . N1 N 0.4150(5) 0.4620(4) 0.1036(5) 0.0551(17) Uani 1 1 d . . . N2 N 0.4225(10) 0.3219(9) 0.8799(11) 0.133(5) Uani 1 1 d . . . C1 C 0.3758(6) 0.4413(5) 0.1799(6) 0.0485(19) Uani 1 1 d . . . C2 C 0.3574(7) 0.3652(5) 0.2089(7) 0.061(2) Uani 1 1 d . . . C3 C 0.3351(7) 0.3150(6) 0.1326(8) 0.067(2) Uani 1 1 d . . . H3 H 0.3278 0.3292 0.0660 0.081 Uiso 1 1 calc R . . C4 C 0.3243(8) 0.2422(6) 0.1599(10) 0.081(3) Uani 1 1 d . . . H4 H 0.3112 0.2069 0.1102 0.097 Uiso 1 1 calc R . . C5 C 0.3321(7) 0.2209(6) 0.2572(9) 0.076(3) Uani 1 1 d . . . H5 H 0.3237 0.1719 0.2734 0.091 Uiso 1 1 calc R . . C6 C 0.3528(7) 0.2731(5) 0.3320(8) 0.064(2) Uani 1 1 d . A . C7 C 0.3659(7) 0.3446(5) 0.3086(7) 0.058(2) Uani 1 1 d . . . H7 H 0.3805 0.3794 0.3587 0.070 Uiso 1 1 calc R . . C8 C 0.3590(11) 0.1841(7) 0.4673(10) 0.094(4) Uani 1 1 d . A . H8A H 0.4028 0.1545 0.4345 0.113 Uiso 1 1 calc R . . H8B H 0.2942 0.1670 0.4446 0.113 Uiso 1 1 calc R . . C9 C 0.3801(9) 0.1722(7) 0.5751(8) 0.080(3) Uani 1 1 d . . . C13 C 0.4051(7) 0.2231(6) 0.7487(7) 0.065(2) Uani 1 1 d . . . C14 C 0.3919(7) 0.2411(8) 0.6421(12) 0.106(5) Uani 1 1 d . A . H14 H 0.3908 0.2889 0.6175 0.127 Uiso 1 1 calc R . . C15 C 0.4156(8) 0.2791(8) 0.8221(11) 0.090(4) Uani 1 1 d . A . O1 O 0.3485(6) 0.5000 0.2310(6) 0.055(2) Uani 1 2 d S . . O2 O 0.3666(6) 0.2573(5) 0.4375(7) 0.104(3) Uani 1 1 d . . . F1 F 0.312(2) 0.5000 0.472(3) 0.188(15) Uani 0.50 2 d SP . . F2 F 0.4494(18) 0.4288(11) 0.5542(19) 0.162(8) Uani 0.50 1 d P . . F3 F 0.2908(18) 0.4245(11) 0.6372(18) 0.155(8) Uani 0.50 1 d P . . F4 F 0.4364(19) 0.5000 0.711(3) 0.168(13) Uani 0.50 2 d SP . . F5 F 0.8133(12) 0.5000 -0.0813(13) 0.078(4) Uani 0.50 2 d SP . . F6 F 0.9385(12) 0.5752(11) 0.0300(12) 0.121(6) Uani 0.50 1 d P . . F7 F 0.7627(9) 0.5735(6) 0.0648(10) 0.080(3) Uani 0.50 1 d P . . F8 F 0.885(3) 0.5000 0.1828(17) 0.193(16) Uani 0.50 2 d SP . . Sb1 Sb 0.36710(17) 0.5000 0.5961(2) 0.0852(8) Uani 0.50 2 d SP . . Sb2 Sb 0.85481(15) 0.5000 0.05045(15) 0.0701(6) Uani 0.50 2 d SP . . C10 C 0.369(2) 0.1094(16) 0.631(2) 0.088(7) Uiso 0.50 1 d P A 1 H10 H 0.3529 0.0695 0.5890 0.106 Uiso 0.50 1 calc PR A 1 C11 C 0.374(2) 0.0905(16) 0.717(2) 0.091(7) Uiso 0.50 1 d P A 1 H11 H 0.3694 0.0422 0.7384 0.110 Uiso 0.50 1 calc PR A 1 C12 C 0.387(2) 0.1509(14) 0.7787(19) 0.074(6) Uiso 0.50 1 d P A 1 H12 H 0.3827 0.1434 0.8460 0.089 Uiso 0.50 1 calc PR A 1 C11' C 0.431(4) 0.101(3) 0.701(4) 0.155(16) Uiso 0.50 1 d P A 2 H11' H 0.4500 0.0535 0.7212 0.186 Uiso 0.50 1 calc PR A 2 C12' C 0.428(2) 0.1518(15) 0.774(2) 0.081(7) Uiso 0.50 1 d P A 2 H12' H 0.4419 0.1383 0.8407 0.097 Uiso 0.50 1 calc PR A 2 C10' C 0.412(3) 0.111(2) 0.613(3) 0.120(12) Uiso 0.50 1 d P A 2 H10' H 0.4210 0.0722 0.5699 0.144 Uiso 0.50 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.1000(9) 0.0466(6) 0.0606(7) 0.000 0.0287(6) 0.000 N1 0.062(4) 0.044(4) 0.057(4) -0.008(3) 0.004(3) 0.003(3) N2 0.113(9) 0.144(12) 0.146(11) -0.085(10) 0.031(8) -0.046(8) C1 0.050(5) 0.049(5) 0.046(4) -0.003(4) 0.006(4) -0.004(4) C2 0.058(5) 0.063(6) 0.064(6) -0.003(5) 0.017(4) -0.005(4) C3 0.066(6) 0.068(6) 0.068(6) -0.006(5) 0.010(5) -0.020(5) C4 0.083(7) 0.063(6) 0.101(9) -0.023(6) 0.026(6) -0.026(6) C5 0.065(6) 0.058(6) 0.105(9) 0.019(6) 0.014(6) -0.008(5) C6 0.058(5) 0.055(5) 0.079(6) 0.007(5) 0.014(5) -0.004(4) C7 0.062(5) 0.048(5) 0.066(6) 0.005(4) 0.015(4) -0.002(4) C8 0.119(10) 0.073(8) 0.090(8) -0.004(6) 0.009(7) 0.000(7) C9 0.096(8) 0.090(8) 0.050(5) -0.008(5) 0.002(5) 0.000(7) C13 0.064(6) 0.065(6) 0.064(6) 0.009(5) 0.005(4) 0.001(5) C14 0.048(6) 0.107(10) 0.165(13) 0.068(10) 0.022(7) 0.011(6) C15 0.059(6) 0.102(9) 0.113(10) -0.035(8) 0.019(6) -0.024(6) O1 0.058(5) 0.060(5) 0.049(5) 0.000 0.011(4) 0.000 O2 0.080(5) 0.101(6) 0.138(7) 0.077(6) 0.036(5) 0.018(4) F1 0.12(2) 0.21(4) 0.23(4) 0.000 0.02(2) 0.000 F2 0.21(2) 0.094(12) 0.19(2) 0.019(14) 0.060(18) 0.036(14) F3 0.19(2) 0.105(13) 0.168(18) 0.003(13) 0.008(15) -0.063(14) F4 0.093(17) 0.22(3) 0.17(3) 0.000 -0.047(17) 0.000 F5 0.066(10) 0.085(12) 0.081(11) 0.000 0.001(8) 0.000 F6 0.115(12) 0.146(14) 0.101(11) -0.036(10) 0.010(9) -0.059(11) F7 0.079(7) 0.054(6) 0.107(9) -0.020(6) 0.009(7) -0.004(6) F8 0.24(4) 0.29(5) 0.050(12) 0.000 0.016(17) 0.000 Sb1 0.0878(15) 0.0438(10) 0.1127(18) 0.000 -0.0267(13) 0.000 Sb2 0.0772(13) 0.0735(13) 0.0576(11) 0.000 0.0023(9) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.266(7) . ? Ag1 N1 2.266(7) 2_655 ? Ag1 N2 2.312(12) 1_554 ? Ag1 N2 2.312(12) 2_656 ? N1 C1 1.291(11) . ? N1 N1 1.383(14) 6_565 ? N2 C15 1.098(15) . ? N2 Ag1 2.312(12) 1_556 ? C1 O1 1.357(9) . ? C1 C2 1.472(13) . ? C2 C3 1.382(14) . ? C2 C7 1.389(13) . ? C3 C4 1.389(15) . ? C3 H3 0.9300 . ? C4 C5 1.361(16) . ? C4 H4 0.9300 . ? C5 C6 1.390(15) . ? C5 H5 0.9300 . ? C6 C7 1.358(13) . ? C6 O2 1.442(13) . ? C7 H7 0.9300 . ? C8 O2 1.399(15) . ? C8 C9 1.464(16) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10' 1.29(4) . ? C9 C10 1.39(3) . ? C9 C14 1.54(2) . ? C13 C12' 1.37(3) . ? C13 C12 1.41(3) . ? C13 C15 1.416(16) . ? C13 C14 1.465(17) . ? C14 H14 0.9300 . ? O1 C1 1.357(9) 6_565 ? F1 Sb1 1.75(4) . ? F2 Sb1 1.88(2) . ? F3 Sb1 1.873(19) . ? F4 Sb1 1.71(3) . ? F5 Sb2 1.797(17) . ? F6 Sb2 1.850(16) . ? F7 Sb2 1.889(12) . ? F8 Sb2 1.78(2) . ? Sb1 F3 1.873(19) 6_565 ? Sb1 F2 1.88(2) 6_565 ? Sb2 F6 1.850(16) 6_565 ? Sb2 F7 1.889(12) 6_565 ? C10 C11 1.21(4) . ? C10 H10 0.9300 . ? C11 C12 1.38(4) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C11' C10' 1.20(6) . ? C11' C12' 1.36(5) . ? C11' H11' 0.9300 . ? C12' H12' 0.9300 . ? C10' H10' 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N1 119.9(4) . 2_655 ? N1 Ag1 N2 120.3(4) . 1_554 ? N1 Ag1 N2 96.2(4) 2_655 1_554 ? N1 Ag1 N2 96.2(4) . 2_656 ? N1 Ag1 N2 120.3(4) 2_655 2_656 ? N2 Ag1 N2 104.4(9) 1_554 2_656 ? C1 N1 N1 107.0(5) . 6_565 ? C1 N1 Ag1 131.8(6) . . ? N1 N1 Ag1 120.05(19) 6_565 . ? C15 N2 Ag1 157.2(12) . 1_556 ? N1 C1 O1 111.0(7) . . ? N1 C1 C2 126.7(8) . . ? O1 C1 C2 122.2(7) . . ? C3 C2 C7 121.8(9) . . ? C3 C2 C1 117.0(8) . . ? C7 C2 C1 121.1(8) . . ? C2 C3 C4 117.1(10) . . ? C2 C3 H3 121.5 . . ? C4 C3 H3 121.5 . . ? C5 C4 C3 122.1(10) . . ? C5 C4 H4 119.0 . . ? C3 C4 H4 119.0 . . ? C4 C5 C6 119.4(10) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C7 C6 C5 120.4(10) . . ? C7 C6 O2 114.7(9) . . ? C5 C6 O2 124.8(9) . . ? C6 C7 C2 119.3(9) . . ? C6 C7 H7 120.4 . . ? C2 C7 H7 120.4 . . ? O2 C8 C9 114.5(11) . . ? O2 C8 H8A 108.6 . . ? C9 C8 H8A 108.6 . . ? O2 C8 H8B 108.6 . . ? C9 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? C10' C9 C10 29.3(18) . . ? C10' C9 C8 122(2) . . ? C10 C9 C8 129.9(16) . . ? C10' C9 C14 118(2) . . ? C10 C9 C14 111.1(15) . . ? C8 C9 C14 117.1(11) . . ? C12' C13 C12 24.8(13) . . ? C12' C13 C15 120.5(15) . . ? C12 C13 C15 118.3(14) . . ? C12' C13 C14 116.8(15) . . ? C12 C13 C14 119.2(14) . . ? C15 C13 C14 121.1(11) . . ? C13 C14 C9 112.7(10) . . ? C13 C14 H14 123.7 . . ? C9 C14 H14 123.7 . . ? N2 C15 C13 178.7(15) . . ? C1 O1 C1 104.0(9) . 6_565 ? C8 O2 C6 118.0(11) . . ? F4 Sb1 F1 171.9(16) . . ? F4 Sb1 F3 90.5(11) . . ? F1 Sb1 F3 95.0(10) . . ? F4 Sb1 F3 90.5(11) . 6_565 ? F1 Sb1 F3 95.0(10) . 6_565 ? F3 Sb1 F3 94.4(17) . 6_565 ? F4 Sb1 F2 88.7(11) . 6_565 ? F1 Sb1 F2 85.5(11) . 6_565 ? F3 Sb1 F2 176.5(11) . 6_565 ? F3 Sb1 F2 89.0(11) 6_565 6_565 ? F4 Sb1 F2 88.7(11) . . ? F1 Sb1 F2 85.5(11) . . ? F3 Sb1 F2 89.0(11) . . ? F3 Sb1 F2 176.5(11) 6_565 . ? F2 Sb1 F2 87.5(14) 6_565 . ? F8 Sb2 F5 175.1(14) . . ? F8 Sb2 F6 94.6(10) . 6_565 ? F5 Sb2 F6 88.7(6) . 6_565 ? F8 Sb2 F6 94.6(10) . . ? F5 Sb2 F6 88.7(6) . . ? F6 Sb2 F6 95.5(13) 6_565 . ? F8 Sb2 F7 88.3(10) . 6_565 ? F5 Sb2 F7 88.2(6) . 6_565 ? F6 Sb2 F7 87.1(7) 6_565 6_565 ? F6 Sb2 F7 176.0(7) . 6_565 ? F8 Sb2 F7 88.3(10) . . ? F5 Sb2 F7 88.2(6) . . ? F6 Sb2 F7 176.0(7) 6_565 . ? F6 Sb2 F7 87.1(7) . . ? F7 Sb2 F7 90.2(7) 6_565 . ? C11 C10 C9 140(3) . . ? C11 C10 H10 110.1 . . ? C9 C10 H10 110.1 . . ? C10 C11 C12 110(3) . . ? C10 C11 H11 125.0 . . ? C12 C11 H11 125.0 . . ? C11 C12 C13 126(2) . . ? C11 C12 H12 117.2 . . ? C13 C12 H12 117.2 . . ? C10' C11' C12' 126(5) . . ? C10' C11' H11' 116.8 . . ? C12' C11' H11' 116.8 . . ? C11' C12' C13 120(3) . . ? C11' C12' H12' 120.1 . . ? C13 C12' H12' 120.1 . . ? C11' C10' C9 123(4) . . ? C11' C10' H10' 118.5 . . ? C9 C10' H10' 118.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ag1 N1 C1 -166.0(8) 2_655 . . . ? N2 Ag1 N1 C1 75.2(9) 1_554 . . . ? N2 Ag1 N1 C1 -35.6(9) 2_656 . . . ? N1 Ag1 N1 N1 0.000(1) 2_655 . . 6_565 ? N2 Ag1 N1 N1 -118.8(5) 1_554 . . 6_565 ? N2 Ag1 N1 N1 130.5(4) 2_656 . . 6_565 ? N1 N1 C1 O1 0.6(8) 6_565 . . . ? Ag1 N1 C1 O1 168.0(6) . . . . ? N1 N1 C1 C2 178.0(7) 6_565 . . . ? Ag1 N1 C1 C2 -14.7(13) . . . . ? N1 C1 C2 C3 -33.2(13) . . . . ? O1 C1 C2 C3 143.9(9) . . . . ? N1 C1 C2 C7 144.2(9) . . . . ? O1 C1 C2 C7 -38.7(13) . . . . ? C7 C2 C3 C4 -1.8(15) . . . . ? C1 C2 C3 C4 175.6(9) . . . . ? C2 C3 C4 C5 1.9(17) . . . . ? C3 C4 C5 C6 -0.8(17) . . . . ? C4 C5 C6 C7 -0.6(15) . . . . ? C4 C5 C6 O2 -177.5(9) . . . . ? C5 C6 C7 C2 0.7(14) . . . . ? O2 C6 C7 C2 178.0(8) . . . . ? C3 C2 C7 C6 0.5(14) . . . . ? C1 C2 C7 C6 -176.8(8) . . . . ? O2 C8 C9 C10' -153(2) . . . . ? O2 C8 C9 C10 172(2) . . . . ? O2 C8 C9 C14 9.2(17) . . . . ? C12' C13 C14 C9 15.3(19) . . . . ? C12 C13 C14 C9 -12.6(18) . . . . ? C15 C13 C14 C9 -178.9(10) . . . . ? C10' C9 C14 C13 -22(3) . . . . ? C10 C9 C14 C13 9.7(19) . . . . ? C8 C9 C14 C13 175.4(10) . . . . ? Ag1 N2 C15 C13 132(86) 1_556 . . . ? C12' C13 C15 N2 -65(89) . . . . ? C12 C13 C15 N2 -37(89) . . . . ? C14 C13 C15 N2 130(89) . . . . ? N1 C1 O1 C1 -0.9(12) . . . 6_565 ? C2 C1 O1 C1 -178.4(5) . . . 6_565 ? C9 C8 O2 C6 176.2(10) . . . . ? C7 C6 O2 C8 -176.9(10) . . . . ? C5 C6 O2 C8 0.2(15) . . . . ? C10' C9 C10 C11 102(7) . . . . ? C8 C9 C10 C11 -172(4) . . . . ? C14 C9 C10 C11 -8(5) . . . . ? C9 C10 C11 C12 7(6) . . . . ? C10 C11 C12 C13 -8(4) . . . . ? C12' C13 C12 C11 -78(5) . . . . ? C15 C13 C12 C11 179(2) . . . . ? C14 C13 C12 C11 13(3) . . . . ? C10' C11' C12' C13 -3(7) . . . . ? C12 C13 C12' C11' 98(5) . . . . ? C15 C13 C12' C11' -170(3) . . . . ? C14 C13 C12' C11' -5(4) . . . . ? C12' C11' C10' C9 -4(9) . . . . ? C10 C9 C10' C11' -67(6) . . . . ? C8 C9 C10' C11' 179(4) . . . . ? C14 C9 C10' C11' 17(6) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.280 _refine_diff_density_min -0.868 _refine_diff_density_rms 0.159 #===End data_10 _database_code_depnum_ccdc_archive 'CCDC 791146' #TrackingRef '- CIF_1.1.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H28 Ag F6 N4 O4 P' _chemical_formula_weight 809.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc 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' _cell_length_a 13.9206(17) _cell_length_b 18.112(2) _cell_length_c 26.968(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.037(2) _cell_angle_gamma 90.00 _cell_volume 6695.6(14) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5944 _cell_measurement_theta_min 2.243 _cell_measurement_theta_max 26.671 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3264 _exptl_absorpt_coefficient_mu 0.728 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7643 _exptl_absorpt_correction_T_max 0.8924 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17227 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0464 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.50 _reflns_number_total 10139 _reflns_number_gt 8706 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0889P)^2^+5.7645P] 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 0.20(3) _refine_ls_number_reflns 10139 _refine_ls_number_parameters 902 _refine_ls_number_restraints 50 _refine_ls_R_factor_all 0.0632 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1394 _refine_ls_wR_factor_gt 0.1310 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.027 _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 0.06192(3) -0.08723(3) 0.903090(18) 0.04230(15) Uani 1 1 d . . . Ag2 Ag 0.05464(3) 0.11363(3) 0.896630(19) 0.04306(15) Uani 1 1 d . . . C1 C -0.0210(6) -0.2285(6) 1.3011(3) 0.056(2) Uani 1 1 d . . . C2 C -0.0204(6) -0.2855(4) 1.2653(3) 0.0464(18) Uani 1 1 d . . . C3 C 0.0037(9) -0.3562(6) 1.2818(4) 0.085(3) Uani 1 1 d . . . H3 H 0.0134 -0.3671 1.3168 0.102 Uiso 1 1 calc R . . C4 C 0.0139(10) -0.4112(6) 1.2476(4) 0.094(3) Uani 1 1 d U . . H4 H 0.0400 -0.4580 1.2587 0.113 Uiso 1 1 calc R . . C5 C -0.0144(11) -0.3968(5) 1.1975(4) 0.108(5) Uani 1 1 d . . . H5 H -0.0195 -0.4366 1.1742 0.129 Uiso 1 1 calc R . . C6 C -0.0356(6) -0.3268(4) 1.1797(3) 0.0478(18) Uani 1 1 d . . . C7 C -0.0411(5) -0.2700(4) 1.2134(3) 0.0357(15) Uani 1 1 d . . . H7 H -0.0585 -0.2216 1.2017 0.043 Uiso 1 1 calc R . . C8 C -0.0582(5) -0.3157(4) 1.1236(3) 0.0424(16) Uani 1 1 d . . . H8A H -0.0112 -0.3436 1.1072 0.051 Uiso 1 1 calc R . . H8B H -0.1247 -0.3340 1.1102 0.051 Uiso 1 1 calc R . . C9 C -0.0683(5) -0.2190(4) 1.0632(2) 0.0356(15) Uani 1 1 d . . . C10 C -0.0939(5) -0.2669(4) 1.0239(3) 0.0445(18) Uani 1 1 d . . . H10 H -0.1002 -0.3180 1.0306 0.053 Uiso 1 1 calc R . . C11 C -0.1108(6) -0.2417(5) 0.9741(3) 0.045(2) Uani 1 1 d . . . H11 H -0.1288 -0.2752 0.9470 0.054 Uiso 1 1 calc R . . C12 C -0.1010(5) -0.1679(4) 0.9650(3) 0.0389(17) Uani 1 1 d . . . H12 H -0.1140 -0.1500 0.9314 0.047 Uiso 1 1 calc R . . C13 C -0.0721(5) -0.1190(4) 1.0046(3) 0.0395(18) Uani 1 1 d . . . C14 C -0.0567(5) -0.1440(4) 1.0543(3) 0.0381(15) Uani 1 1 d . . . H14 H -0.0386 -0.1106 1.0814 0.046 Uiso 1 1 calc R . . C15 C -0.0534(5) -0.0436(4) 0.9917(3) 0.0357(16) Uani 1 1 d . . . C16 C -0.0496(5) 0.0753(4) 0.9944(3) 0.0333(15) Uani 1 1 d . . . C17 C -0.0655(5) 0.1493(4) 1.0117(2) 0.0359(15) Uani 1 1 d . . . C18 C -0.0861(5) 0.2056(5) 0.9752(3) 0.0431(18) Uani 1 1 d . . . H18 H -0.0908 0.1947 0.9404 0.052 Uiso 1 1 calc R . . C19 C -0.0988(6) 0.2743(5) 0.9905(3) 0.0455(19) Uani 1 1 d . . . H19 H -0.1136 0.3120 0.9658 0.055 Uiso 1 1 calc R . . C20 C -0.0912(6) 0.2930(4) 1.0412(3) 0.0442(18) Uani 1 1 d . . . H20 H -0.1006 0.3425 1.0510 0.053 Uiso 1 1 calc R . . C21 C -0.0697(5) 0.2380(4) 1.0768(2) 0.0337(14) Uani 1 1 d . . . C22 C -0.0589(5) 0.1656(4) 1.0624(3) 0.0355(15) Uani 1 1 d . . . H22 H -0.0471 0.1275 1.0870 0.043 Uiso 1 1 calc R . . C23 C -0.0663(6) 0.3252(4) 1.1428(3) 0.0423(17) Uani 1 1 d . . . H23A H -0.1315 0.3453 1.1287 0.051 Uiso 1 1 calc R . . H23B H -0.0165 0.3551 1.1299 0.051 Uiso 1 1 calc R . . C24 C -0.0498(6) 0.3294(4) 1.1997(3) 0.0442(17) Uani 1 1 d . . . C25 C -0.0370(5) 0.2682(4) 1.2310(3) 0.0401(17) Uani 1 1 d . . . H25 H -0.0364 0.2202 1.2168 0.048 Uiso 1 1 calc R . . C26 C -0.0251(5) 0.2766(5) 1.2827(3) 0.0471(19) Uani 1 1 d . . . C27 C -0.0162(6) 0.2143(5) 1.3157(3) 0.051(2) Uani 1 1 d . . . C28 C -0.0274(8) 0.3461(6) 1.3040(3) 0.072(3) Uani 1 1 d . . . H28 H -0.0182 0.3515 1.3396 0.086 Uiso 1 1 calc R . . C29 C -0.0436(10) 0.4085(6) 1.2727(4) 0.087(4) Uani 1 1 d . . . H29 H -0.0494 0.4561 1.2867 0.104 Uiso 1 1 calc R . . C30 C -0.0509(10) 0.3998(6) 1.2217(4) 0.087(4) Uani 1 1 d . . . H30 H -0.0568 0.4422 1.2007 0.105 Uiso 1 1 calc R . . C31 C 0.1583(5) 0.2109(5) 0.4934(3) 0.0465(19) Uani 1 1 d . . . C32 C 0.1719(5) 0.2735(4) 0.5265(3) 0.0372(16) Uani 1 1 d . . . C33 C 0.1739(5) 0.3429(5) 0.5061(3) 0.0476(19) Uani 1 1 d . . . H33 H 0.1648 0.3493 0.4706 0.057 Uiso 1 1 calc R . . C34 C 0.1891(6) 0.4030(5) 0.5377(3) 0.0501(19) Uani 1 1 d . . . H34 H 0.1903 0.4513 0.5241 0.060 Uiso 1 1 calc R . . C35 C 0.2025(6) 0.3929(4) 0.5882(3) 0.0454(18) Uani 1 1 d . . . H35 H 0.2121 0.4351 0.6094 0.054 Uiso 1 1 calc R . . C36 C 0.2027(5) 0.3234(4) 0.6104(2) 0.0383(15) Uani 1 1 d . . . C37 C 0.1845(5) 0.2613(4) 0.5786(3) 0.0409(17) Uani 1 1 d . . . H37 H 0.1808 0.2131 0.5920 0.049 Uiso 1 1 calc R . . C38 C 0.2220(6) 0.3179(4) 0.6663(3) 0.0453(17) Uani 1 1 d . . . H38A H 0.2886 0.3361 0.6795 0.054 Uiso 1 1 calc R . . H38B H 0.1750 0.3491 0.6803 0.054 Uiso 1 1 calc R . . C39 C 0.2189(5) 0.2318(4) 0.7321(2) 0.0331(14) Uani 1 1 d . . . C40 C 0.2361(6) 0.2862(4) 0.7694(3) 0.0456(18) Uani 1 1 d . . . H40 H 0.2446 0.3360 0.7599 0.055 Uiso 1 1 calc R . . C41 C 0.2410(6) 0.2697(4) 0.8192(3) 0.0412(17) Uani 1 1 d . . . H41 H 0.2520 0.3077 0.8439 0.049 Uiso 1 1 calc R . . C42 C 0.2296(5) 0.1951(4) 0.8339(3) 0.0344(15) Uani 1 1 d . . . H42 H 0.2342 0.1822 0.8684 0.041 Uiso 1 1 calc R . . C43 C 0.2118(5) 0.1423(4) 0.7968(2) 0.0316(14) Uani 1 1 d . . . C44 C 0.2079(5) 0.1584(4) 0.7458(2) 0.0341(15) Uani 1 1 d . . . H44 H 0.1981 0.1205 0.7211 0.041 Uiso 1 1 calc R . . C45 C 0.1951(5) 0.0667(4) 0.8128(3) 0.0300(15) Uani 1 1 d . . . C46 C 0.1993(5) -0.0507(4) 0.8180(3) 0.0313(15) Uani 1 1 d . . . C47 C 0.2176(5) -0.1289(4) 0.8080(3) 0.0316(15) Uani 1 1 d . . . C48 C 0.2362(5) -0.1761(4) 0.8492(3) 0.0418(16) Uani 1 1 d . . . H48 H 0.2433 -0.1572 0.8825 0.050 Uiso 1 1 calc R . . C49 C 0.2442(6) -0.2514(5) 0.8410(3) 0.052(2) Uani 1 1 d . . . H49 H 0.2563 -0.2842 0.8689 0.062 Uiso 1 1 calc R . . C50 C 0.2350(5) -0.2783(4) 0.7934(3) 0.0426(17) Uani 1 1 d . . . H50 H 0.2393 -0.3299 0.7881 0.051 Uiso 1 1 calc R . . C51 C 0.2194(5) -0.2313(4) 0.7527(3) 0.0407(16) Uani 1 1 d . . . C52 C 0.2103(5) -0.1560(4) 0.7584(3) 0.0365(15) Uani 1 1 d . . . H52 H 0.1997 -0.1238 0.7302 0.044 Uiso 1 1 calc R . . C53 C 0.1924(5) -0.2208(3) 0.6638(2) 0.0353(14) Uani 1 1 d . . . H53A H 0.2435 -0.1827 0.6643 0.042 Uiso 1 1 calc R . . H53B H 0.1290 -0.1956 0.6627 0.042 Uiso 1 1 calc R . . C54 C 0.1886(5) -0.2696(4) 0.6179(3) 0.0366(14) Uani 1 1 d . . . C55 C 0.2000(6) -0.3445(4) 0.6214(3) 0.0494(19) Uani 1 1 d . . . H55 H 0.2104 -0.3672 0.6537 0.059 Uiso 1 1 calc R . . C56 C 0.1965(7) -0.3889(4) 0.5780(3) 0.053(2) Uani 1 1 d . . . H56 H 0.2040 -0.4409 0.5812 0.064 Uiso 1 1 calc R . . C57 C 0.1819(6) -0.3556(5) 0.5302(3) 0.0507(19) Uani 1 1 d . . . H57 H 0.1812 -0.3841 0.5005 0.061 Uiso 1 1 calc R . . C58 C 0.1687(5) -0.2804(4) 0.5278(2) 0.0344(15) Uani 1 1 d . . . C59 C 0.1725(5) -0.2372(4) 0.5714(3) 0.0353(15) Uani 1 1 d . . . H59 H 0.1638 -0.1853 0.5686 0.042 Uiso 1 1 calc R . . C60 C 0.1527(5) -0.2424(4) 0.4805(3) 0.0424(17) Uani 1 1 d . . . C61 C 0.9062(8) 0.9954(10) 0.1779(5) 0.152(9) Uani 1 1 d D . . H61A H 0.9214 1.0349 0.1550 0.182 Uiso 1 1 calc R . . H61B H 0.9134 0.9471 0.1617 0.182 Uiso 1 1 calc R . . C62 C 0.9754(11) 1.0000(10) 0.2281(6) 0.143(8) Uani 1 1 d D . . H62A H 1.0188 0.9563 0.2335 0.171 Uiso 1 1 calc R . . H62B H 1.0158 1.0452 0.2302 0.171 Uiso 1 1 calc R . . C63 C 0.9073(11) 1.0020(8) 0.2658(6) 0.128(6) Uani 1 1 d D . . H63A H 0.9103 1.0508 0.2826 0.154 Uiso 1 1 calc R . . H63B H 0.9254 0.9636 0.2919 0.154 Uiso 1 1 calc R . . C64 C 0.8051(10) 0.9878(6) 0.2365(4) 0.106(5) Uani 1 1 d D . . H64A H 0.7859 0.9357 0.2400 0.128 Uiso 1 1 calc R . . H64B H 0.7568 1.0202 0.2487 0.128 Uiso 1 1 calc R . . C67 C 0.3599(16) -0.0095(11) 0.9957(8) 0.185(9) Uani 1 1 d DU . . H67A H 0.3322 -0.0507 1.0128 0.222 Uiso 1 1 calc R . . H67B H 0.4137 0.0137 1.0195 0.222 Uiso 1 1 calc R . . C66 C 0.394(2) -0.0353(11) 0.9474(12) 0.33(2) Uani 1 1 d DU . . H66A H 0.4537 -0.0657 0.9548 0.392 Uiso 1 1 calc R . . H66B H 0.3423 -0.0632 0.9252 0.392 Uiso 1 1 calc R . . C65 C 0.413(2) 0.0388(14) 0.9248(11) 0.239(12) Uani 1 1 d DU . . H65A H 0.4786 0.0587 0.9386 0.287 Uiso 1 1 calc R . . H65B H 0.4031 0.0379 0.8876 0.287 Uiso 1 1 calc R . . O8 O 0.3403(17) 0.0740(13) 0.9429(8) 0.292(11) Uani 1 1 d DU . . F1 F 0.2479(6) 0.5015(4) 0.4401(2) 0.104(2) Uani 1 1 d . . . F2 F 0.2864(6) 0.5515(4) 0.3713(3) 0.102(2) Uani 1 1 d . . . F3 F 0.2873(6) 0.4305(5) 0.3805(4) 0.133(3) Uani 1 1 d . . . F4 F 0.1338(6) 0.4299(5) 0.3940(3) 0.130(3) Uani 1 1 d . . . F5 F 0.1304(8) 0.5505(6) 0.3816(5) 0.192(5) Uani 1 1 d . . . F6 F 0.1731(7) 0.4792(6) 0.3235(3) 0.143(4) Uani 1 1 d . . . F7 F 0.1287(8) -0.0662(5) 0.1311(3) 0.140(3) Uani 1 1 d . . . F8 F 0.2382(8) 0.0084(5) 0.1720(4) 0.149(4) Uani 1 1 d . . . F9 F 0.1128(7) 0.0557(5) 0.1265(4) 0.140(3) Uani 1 1 d . . . F10 F 0.2523(6) 0.0643(4) 0.1003(4) 0.132(3) Uani 1 1 d . . . F11 F 0.1380(7) -0.0089(6) 0.0594(3) 0.143(4) Uani 1 1 d . . . F12 F 0.2685(9) -0.0546(5) 0.1044(5) 0.188(5) Uani 1 1 d . . . N1 N 0.1528(4) 0.0489(3) 0.8505(2) 0.0349(13) Uani 1 1 d . . . N2 N 0.1545(5) -0.0283(3) 0.8537(2) 0.0365(14) Uani 1 1 d . . . N3 N 0.1500(6) 0.1640(5) 0.4651(3) 0.066(2) Uani 1 1 d . . . N4 N 0.1391(5) -0.2109(4) 0.4434(2) 0.0585(18) Uani 1 1 d . . . N5 N -0.0137(4) 0.0552(3) 0.9556(2) 0.0363(13) Uani 1 1 d . . . N6 N -0.0155(5) -0.0221(3) 0.9541(2) 0.0352(14) Uani 1 1 d . . . N7 N -0.0215(5) -0.1828(5) 1.3309(3) 0.0589(19) Uani 1 1 d . . . N8 N -0.0096(5) 0.1657(5) 1.3431(3) 0.0549(18) Uani 1 1 d . . . O1 O 0.2264(4) 0.0060(2) 0.79053(18) 0.0329(11) Uani 1 1 d . . . O2 O 0.2131(4) 0.2434(3) 0.68139(17) 0.0447(12) Uani 1 1 d . . . O3 O 0.2134(4) -0.2650(3) 0.70714(18) 0.0485(12) Uani 1 1 d . . . O4 O -0.0761(4) 0.0145(2) 1.01959(18) 0.0337(11) Uani 1 1 d . . . O5 O -0.0518(4) -0.2393(3) 1.11331(17) 0.0439(12) Uani 1 1 d . . . O6 O -0.0600(4) 0.2497(3) 1.12755(17) 0.0403(12) Uani 1 1 d . . . O7 O 0.8105(6) 1.0036(5) 0.1868(3) 0.093(3) Uani 1 1 d D . . C68 C 0.2824(12) 0.0464(9) 0.9747(7) 0.145(6) Uani 1 1 d DU . . H68A H 0.2214 0.0236 0.9568 0.174 Uiso 1 1 calc R . . H68B H 0.2683 0.0826 0.9999 0.174 Uiso 1 1 calc R . . P1 P 0.2075(2) 0.49230(13) 0.38294(9) 0.0655(7) Uani 1 1 d . . . P2 P 0.1922(2) -0.00083(11) 0.11392(11) 0.0627(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0639(3) 0.0358(2) 0.0313(3) 0.0029(3) 0.0194(2) -0.0001(3) Ag2 0.0659(3) 0.0377(3) 0.0301(3) -0.0023(2) 0.0209(2) -0.0018(3) C1 0.038(4) 0.082(6) 0.050(5) 0.000(5) 0.012(4) -0.014(4) C2 0.054(4) 0.044(4) 0.038(4) -0.001(3) -0.001(3) -0.014(4) C3 0.144(10) 0.058(6) 0.048(5) 0.019(4) 0.002(6) -0.014(6) C4 0.141(8) 0.055(5) 0.077(6) 0.010(5) -0.005(6) -0.014(5) C5 0.209(15) 0.037(5) 0.061(7) 0.004(4) -0.023(8) -0.025(7) C6 0.060(4) 0.043(4) 0.040(4) -0.004(3) 0.006(3) -0.013(4) C7 0.035(3) 0.031(4) 0.040(4) 0.009(3) 0.002(3) -0.001(3) C8 0.049(4) 0.035(4) 0.041(4) -0.001(3) 0.003(3) -0.010(3) C9 0.039(4) 0.041(4) 0.027(3) 0.001(3) 0.007(3) -0.007(3) C10 0.058(4) 0.037(4) 0.039(4) -0.005(3) 0.010(3) -0.009(4) C11 0.047(4) 0.057(5) 0.033(4) -0.013(3) 0.013(3) -0.013(4) C12 0.040(4) 0.049(5) 0.027(3) -0.004(3) 0.004(3) -0.018(3) C13 0.040(4) 0.041(4) 0.040(4) -0.007(3) 0.012(3) -0.012(3) C14 0.049(4) 0.036(4) 0.032(3) -0.005(3) 0.013(3) -0.008(3) C15 0.042(4) 0.034(4) 0.030(3) 0.000(3) 0.005(3) -0.005(3) C16 0.033(4) 0.042(4) 0.027(3) 0.007(3) 0.012(3) 0.000(3) C17 0.041(4) 0.041(4) 0.027(3) 0.002(3) 0.009(3) 0.004(3) C18 0.047(4) 0.053(5) 0.030(4) -0.001(3) 0.009(3) 0.009(4) C19 0.052(4) 0.049(5) 0.038(4) 0.015(4) 0.014(4) 0.011(4) C20 0.063(5) 0.042(4) 0.030(4) 0.006(3) 0.014(3) 0.011(4) C21 0.035(3) 0.033(3) 0.033(3) 0.001(3) 0.003(3) 0.004(3) C22 0.036(3) 0.035(4) 0.036(4) 0.012(3) 0.006(3) 0.003(3) C23 0.062(4) 0.031(4) 0.034(4) 0.000(3) 0.007(3) 0.010(3) C24 0.056(4) 0.039(4) 0.040(4) -0.006(3) 0.015(3) -0.005(3) C25 0.052(4) 0.029(4) 0.039(4) -0.001(3) 0.007(3) 0.008(3) C26 0.040(4) 0.058(5) 0.041(4) 0.001(4) 0.000(3) 0.004(4) C27 0.040(4) 0.070(6) 0.041(4) -0.008(4) 0.001(3) 0.007(4) C28 0.112(8) 0.067(6) 0.031(4) -0.005(4) -0.004(5) -0.025(6) C29 0.143(11) 0.059(7) 0.057(6) -0.012(5) 0.012(7) -0.018(7) C30 0.167(12) 0.043(5) 0.059(7) -0.013(4) 0.036(7) -0.027(7) C31 0.047(4) 0.061(5) 0.030(4) -0.004(4) 0.000(3) -0.005(4) C32 0.034(3) 0.042(4) 0.034(4) -0.004(3) 0.004(3) -0.005(3) C33 0.049(4) 0.061(5) 0.036(4) 0.012(3) 0.014(3) 0.002(4) C34 0.066(5) 0.038(4) 0.046(4) 0.007(3) 0.010(4) 0.003(4) C35 0.057(4) 0.031(4) 0.052(5) 0.005(3) 0.018(4) 0.005(3) C36 0.039(4) 0.045(4) 0.031(3) 0.006(3) 0.004(3) 0.002(3) C37 0.048(4) 0.045(4) 0.033(4) 0.009(3) 0.016(3) 0.003(3) C38 0.061(4) 0.034(4) 0.041(4) 0.001(3) 0.010(3) -0.006(3) C39 0.035(3) 0.038(4) 0.027(3) 0.001(3) 0.010(3) 0.000(3) C40 0.061(5) 0.037(4) 0.040(4) 0.000(3) 0.014(4) -0.012(4) C41 0.054(4) 0.033(4) 0.038(4) -0.012(3) 0.012(3) -0.015(3) C42 0.045(4) 0.032(4) 0.028(3) -0.006(3) 0.012(3) -0.009(3) C43 0.035(3) 0.034(4) 0.028(3) -0.001(3) 0.013(3) -0.004(3) C44 0.042(4) 0.033(4) 0.026(3) 0.006(3) 0.004(3) -0.005(3) C45 0.036(4) 0.028(3) 0.027(4) -0.003(3) 0.008(3) 0.003(3) C46 0.034(3) 0.030(4) 0.031(4) 0.004(3) 0.010(3) 0.002(3) C47 0.040(4) 0.024(3) 0.033(4) -0.001(3) 0.013(3) 0.006(3) C48 0.056(4) 0.040(4) 0.032(3) -0.001(3) 0.013(3) 0.005(3) C49 0.068(5) 0.045(5) 0.043(5) 0.015(4) 0.011(4) 0.016(4) C50 0.053(4) 0.028(4) 0.045(4) 0.011(3) 0.004(3) 0.009(3) C51 0.042(4) 0.041(4) 0.039(4) 0.001(3) 0.009(3) 0.006(3) C52 0.038(4) 0.036(4) 0.038(4) 0.002(3) 0.012(3) 0.007(3) C53 0.049(4) 0.027(3) 0.031(3) -0.005(3) 0.011(3) 0.003(3) C54 0.040(4) 0.040(4) 0.030(3) -0.004(3) 0.008(3) -0.003(3) C55 0.081(5) 0.028(4) 0.040(4) 0.002(3) 0.015(4) 0.006(4) C56 0.074(5) 0.038(4) 0.048(5) 0.003(3) 0.009(4) 0.011(4) C57 0.059(5) 0.055(5) 0.042(4) -0.002(4) 0.021(4) 0.001(4) C58 0.036(3) 0.042(4) 0.026(3) 0.006(3) 0.008(3) 0.004(3) C59 0.039(4) 0.025(3) 0.042(4) -0.003(3) 0.009(3) -0.002(3) C60 0.045(4) 0.050(4) 0.036(4) 0.014(3) 0.015(3) 0.012(3) C61 0.084(10) 0.29(3) 0.090(12) 0.049(12) 0.038(9) 0.028(11) C62 0.087(11) 0.20(2) 0.125(16) 0.011(11) -0.034(12) 0.000(10) C63 0.146(15) 0.159(15) 0.066(9) -0.001(8) -0.020(10) -0.008(10) C64 0.172(15) 0.081(8) 0.070(8) 0.003(6) 0.034(9) -0.021(8) C67 0.203(12) 0.175(12) 0.181(13) 0.034(9) 0.043(9) 0.069(9) C66 0.35(2) 0.31(2) 0.33(2) 0.022(10) 0.054(11) 0.020(10) C65 0.227(15) 0.259(15) 0.243(15) 0.018(10) 0.075(10) -0.006(10) O8 0.300(13) 0.288(14) 0.291(14) 0.013(10) 0.059(9) -0.023(10) F1 0.127(6) 0.125(6) 0.052(4) 0.008(3) -0.003(4) -0.048(4) F2 0.145(6) 0.073(4) 0.086(5) 0.001(3) 0.015(4) -0.036(4) F3 0.130(6) 0.091(5) 0.171(8) 0.010(5) 0.007(6) -0.003(5) F4 0.125(6) 0.170(7) 0.081(5) 0.032(5) -0.022(4) -0.081(5) F5 0.189(10) 0.166(9) 0.233(12) 0.098(9) 0.073(9) 0.103(8) F6 0.142(7) 0.213(10) 0.064(5) 0.012(5) -0.010(5) -0.056(6) F7 0.203(9) 0.099(5) 0.111(6) 0.011(5) 0.009(6) -0.059(6) F8 0.164(9) 0.183(10) 0.085(6) 0.009(5) -0.021(6) -0.021(6) F9 0.129(6) 0.120(7) 0.180(9) 0.010(6) 0.049(6) 0.026(5) F10 0.127(6) 0.066(4) 0.208(9) -0.014(5) 0.048(6) -0.036(4) F11 0.122(7) 0.222(11) 0.068(5) 0.016(5) -0.027(5) -0.046(6) F12 0.198(10) 0.110(7) 0.247(13) 0.000(8) 0.013(9) 0.106(7) N1 0.053(3) 0.031(3) 0.023(3) -0.001(2) 0.012(2) -0.006(3) N2 0.055(4) 0.023(3) 0.033(3) 0.001(2) 0.011(3) 0.000(3) N3 0.082(5) 0.068(5) 0.049(4) -0.015(4) 0.011(4) -0.024(4) N4 0.072(4) 0.064(4) 0.045(4) 0.006(3) 0.024(3) 0.014(4) N5 0.045(3) 0.037(3) 0.027(3) -0.001(2) 0.008(2) -0.002(3) N6 0.050(4) 0.035(3) 0.025(3) -0.002(2) 0.019(3) -0.003(3) N7 0.050(4) 0.082(5) 0.043(4) -0.014(4) 0.005(3) -0.015(4) N8 0.058(4) 0.071(5) 0.038(3) 0.019(3) 0.015(3) 0.018(4) O1 0.041(3) 0.033(3) 0.027(2) -0.0004(18) 0.014(2) 0.001(2) O2 0.066(3) 0.041(3) 0.028(2) 0.006(2) 0.010(2) -0.005(2) O3 0.079(3) 0.035(3) 0.032(3) 0.000(2) 0.010(2) 0.005(3) O4 0.038(2) 0.038(3) 0.027(2) -0.0015(19) 0.011(2) -0.004(2) O5 0.061(3) 0.036(3) 0.033(3) 0.001(2) 0.004(2) -0.009(2) O6 0.060(3) 0.031(2) 0.030(2) 0.0028(19) 0.010(2) 0.006(2) O7 0.085(5) 0.122(7) 0.070(5) 0.028(4) 0.009(4) 0.015(4) C68 0.152(9) 0.143(9) 0.139(9) 0.019(8) 0.024(8) -0.029(8) P1 0.0810(16) 0.0621(14) 0.0457(13) 0.0132(10) -0.0106(12) -0.0055(12) P2 0.0720(15) 0.0292(10) 0.0732(17) 0.0011(9) -0.0251(14) 0.0009(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N6 2.228(6) . ? Ag1 N8 2.251(7) 2_554 ? Ag1 N2 2.275(7) . ? Ag1 N3 2.349(7) 2 ? Ag2 N5 2.253(6) . ? Ag2 N7 2.277(7) 2_554 ? Ag2 N1 2.319(6) . ? Ag2 N4 2.358(7) 2 ? C1 N7 1.154(11) . ? C1 C2 1.415(12) . ? C2 C3 1.377(13) . ? C2 C7 1.408(10) . ? C3 C4 1.382(16) . ? C3 H3 0.9500 . ? C4 C5 1.365(15) . ? C4 H4 0.9500 . ? C5 C6 1.370(12) . ? C5 H5 0.9500 . ? C6 C7 1.384(10) . ? C6 C8 1.502(10) . ? C7 H7 0.9500 . ? C8 O5 1.419(8) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.368(10) . ? C9 O5 1.381(8) . ? C9 C14 1.394(10) . ? C10 C11 1.400(11) . ? C10 H10 0.9500 . ? C11 C12 1.369(12) . ? C11 H11 0.9500 . ? C12 C13 1.392(10) . ? C12 H12 0.9500 . ? C13 C14 1.393(10) . ? C13 C15 1.444(11) . ? C14 H14 0.9500 . ? C15 N6 1.281(10) . ? C15 O4 1.363(9) . ? C16 N5 1.288(9) . ? C16 O4 1.379(8) . ? C16 C17 1.448(11) . ? C17 C22 1.387(9) . ? C17 C18 1.410(10) . ? C18 C19 1.332(12) . ? C18 H18 0.9500 . ? C19 C20 1.395(11) . ? C19 H19 0.9500 . ? C20 C21 1.380(10) . ? C20 H20 0.9500 . ? C21 O6 1.369(8) . ? C21 C22 1.383(10) . ? C22 H22 0.9500 . ? C23 O6 1.434(8) . ? C23 C24 1.514(9) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.385(11) . ? C24 C30 1.407(13) . ? C25 C26 1.384(10) . ? C25 H25 0.9500 . ? C26 C28 1.386(13) . ? C26 C27 1.429(13) . ? C27 N8 1.142(11) . ? C28 C29 1.407(15) . ? C28 H28 0.9500 . ? C29 C30 1.370(15) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 N3 1.134(11) . ? C31 C32 1.434(11) . ? C32 C33 1.374(11) . ? C32 C37 1.404(10) . ? C33 C34 1.376(12) . ? C33 H33 0.9500 . ? C34 C35 1.355(11) . ? C34 H34 0.9500 . ? C35 C36 1.394(10) . ? C35 H35 0.9500 . ? C36 C37 1.409(11) . ? C36 C38 1.488(9) . ? C37 H37 0.9500 . ? C38 O2 1.422(9) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 O2 1.372(8) . ? C39 C44 1.395(10) . ? C39 C40 1.399(10) . ? C40 C41 1.367(10) . ? C40 H40 0.9500 . ? C41 C42 1.425(10) . ? C41 H41 0.9500 . ? C42 C43 1.374(9) . ? C42 H42 0.9500 . ? C43 C44 1.398(9) . ? C43 C45 1.467(10) . ? C44 H44 0.9500 . ? C45 N1 1.303(9) . ? C45 O1 1.361(8) . ? C46 N2 1.300(10) . ? C46 O1 1.357(8) . ? C46 C47 1.472(10) . ? C47 C48 1.391(10) . ? C47 C52 1.412(9) . ? C48 C49 1.388(11) . ? C48 H48 0.9500 . ? C49 C50 1.359(11) . ? C49 H49 0.9500 . ? C50 C51 1.374(10) . ? C50 H50 0.9500 . ? C51 O3 1.362(8) . ? C51 C52 1.381(10) . ? C52 H52 0.9500 . ? C53 O3 1.405(8) . ? C53 C54 1.514(9) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C59 1.366(9) . ? C54 C55 1.367(10) . ? C55 C56 1.414(11) . ? C55 H55 0.9500 . ? C56 C57 1.407(11) . ? C56 H56 0.9500 . ? C57 C58 1.375(11) . ? C57 H57 0.9500 . ? C58 C59 1.406(9) . ? C58 C60 1.434(9) . ? C59 H59 0.9500 . ? C60 N4 1.138(9) . ? C61 O7 1.402(9) . ? C61 C62 1.523(10) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.507(10) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.525(10) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 O7 1.384(9) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C67 C68 1.515(10) . ? C67 C66 1.536(10) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C66 C65 1.516(10) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C65 O8 1.361(10) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? O8 C68 1.368(10) . ? F1 P1 1.556(7) . ? F2 P1 1.604(7) . ? F3 P1 1.586(9) . ? F4 P1 1.589(7) . ? F5 P1 1.499(9) . ? F6 P1 1.609(8) . ? F7 P2 1.594(8) . ? F8 P2 1.594(10) . ? F9 P2 1.585(9) . ? F10 P2 1.528(7) . ? F11 P2 1.538(9) . ? F12 P2 1.495(9) . ? N1 N2 1.400(9) . ? N3 Ag1 2.349(7) 2_554 ? N4 Ag2 2.358(7) 2_554 ? N5 N6 1.401(9) . ? N7 Ag2 2.277(7) 2 ? N8 Ag1 2.251(7) 2 ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? 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 N6 Ag1 N8 125.2(2) . 2_554 ? N6 Ag1 N2 119.88(17) . . ? N8 Ag1 N2 95.7(2) 2_554 . ? N6 Ag1 N3 97.0(3) . 2 ? N8 Ag1 N3 104.4(3) 2_554 2 ? N2 Ag1 N3 114.6(3) . 2 ? N5 Ag2 N7 127.7(2) . 2_554 ? N5 Ag2 N1 120.06(17) . . ? N7 Ag2 N1 95.7(2) 2_554 . ? N5 Ag2 N4 101.9(2) . 2 ? N7 Ag2 N4 97.3(3) 2_554 2 ? N1 Ag2 N4 112.3(2) . 2 ? N7 C1 C2 179.1(10) . . ? C3 C2 C7 120.2(8) . . ? C3 C2 C1 119.1(8) . . ? C7 C2 C1 120.6(8) . . ? C2 C3 C4 120.1(9) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 118.6(11) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? C4 C5 C6 122.1(10) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C5 C6 C7 119.4(8) . . ? C5 C6 C8 118.1(8) . . ? C7 C6 C8 122.4(7) . . ? C6 C7 C2 118.7(7) . . ? C6 C7 H7 120.6 . . ? C2 C7 H7 120.6 . . ? O5 C8 C6 108.6(6) . . ? O5 C8 H8A 110.0 . . ? C6 C8 H8A 110.0 . . ? O5 C8 H8B 110.0 . . ? C6 C8 H8B 110.0 . . ? H8A C8 H8B 108.4 . . ? C10 C9 O5 124.4(6) . . ? C10 C9 C14 120.5(6) . . ? O5 C9 C14 115.1(6) . . ? C9 C10 C11 120.9(7) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C12 C11 C10 119.0(7) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C11 C12 C13 120.5(7) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C12 C13 C14 120.4(7) . . ? C12 C13 C15 117.1(7) . . ? C14 C13 C15 122.3(7) . . ? C13 C14 C9 118.6(6) . . ? C13 C14 H14 120.7 . . ? C9 C14 H14 120.7 . . ? N6 C15 O4 111.7(6) . . ? N6 C15 C13 126.5(7) . . ? O4 C15 C13 121.9(7) . . ? N5 C16 O4 110.5(6) . . ? N5 C16 C17 128.8(7) . . ? O4 C16 C17 120.7(6) . . ? C22 C17 C18 120.3(7) . . ? C22 C17 C16 121.8(6) . . ? C18 C17 C16 117.9(6) . . ? C19 C18 C17 118.9(7) . . ? C19 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? C18 C19 C20 122.5(7) . . ? C18 C19 H19 118.7 . . ? C20 C19 H19 118.7 . . ? C21 C20 C19 118.5(7) . . ? C21 C20 H20 120.8 . . ? C19 C20 H20 120.8 . . ? O6 C21 C20 123.7(6) . . ? O6 C21 C22 115.5(6) . . ? C20 C21 C22 120.7(6) . . ? C21 C22 C17 119.1(6) . . ? C21 C22 H22 120.5 . . ? C17 C22 H22 120.5 . . ? O6 C23 C24 109.5(5) . . ? O6 C23 H23A 109.8 . . ? C24 C23 H23A 109.8 . . ? O6 C23 H23B 109.8 . . ? C24 C23 H23B 109.8 . . ? H23A C23 H23B 108.2 . . ? C25 C24 C30 118.6(8) . . ? C25 C24 C23 123.9(7) . . ? C30 C24 C23 117.5(8) . . ? C26 C25 C24 120.4(7) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C25 C26 C28 120.7(8) . . ? C25 C26 C27 121.6(8) . . ? C28 C26 C27 117.7(8) . . ? N8 C27 C26 178.2(10) . . ? C26 C28 C29 119.6(8) . . ? C26 C28 H28 120.2 . . ? C29 C28 H28 120.2 . . ? C30 C29 C28 119.1(11) . . ? C30 C29 H29 120.4 . . ? C28 C29 H29 120.4 . . ? C29 C30 C24 121.5(11) . . ? C29 C30 H30 119.2 . . ? C24 C30 H30 119.2 . . ? N3 C31 C32 175.5(9) . . ? C33 C32 C37 122.5(7) . . ? C33 C32 C31 119.0(7) . . ? C37 C32 C31 118.5(7) . . ? C32 C33 C34 119.2(7) . . ? C32 C33 H33 120.4 . . ? C34 C33 H33 120.4 . . ? C35 C34 C33 119.7(8) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C34 C35 C36 122.9(8) . . ? C34 C35 H35 118.6 . . ? C36 C35 H35 118.6 . . ? C35 C36 C37 118.3(7) . . ? C35 C36 C38 118.8(7) . . ? C37 C36 C38 123.0(6) . . ? C32 C37 C36 117.4(7) . . ? C32 C37 H37 121.3 . . ? C36 C37 H37 121.3 . . ? O2 C38 C36 110.2(6) . . ? O2 C38 H38A 109.6 . . ? C36 C38 H38A 109.6 . . ? O2 C38 H38B 109.6 . . ? C36 C38 H38B 109.6 . . ? H38A C38 H38B 108.1 . . ? O2 C39 C44 114.8(6) . . ? O2 C39 C40 125.6(6) . . ? C44 C39 C40 119.6(6) . . ? C41 C40 C39 121.8(7) . . ? C41 C40 H40 119.1 . . ? C39 C40 H40 119.1 . . ? C40 C41 C42 119.4(7) . . ? C40 C41 H41 120.3 . . ? C42 C41 H41 120.3 . . ? C43 C42 C41 118.2(6) . . ? C43 C42 H42 120.9 . . ? C41 C42 H42 120.9 . . ? C42 C43 C44 122.8(7) . . ? C42 C43 C45 117.0(6) . . ? C44 C43 C45 120.2(6) . . ? C39 C44 C43 118.2(6) . . ? C39 C44 H44 120.9 . . ? C43 C44 H44 120.9 . . ? N1 C45 O1 111.6(6) . . ? N1 C45 C43 125.3(6) . . ? O1 C45 C43 123.1(6) . . ? N2 C46 O1 112.5(6) . . ? N2 C46 C47 123.8(6) . . ? O1 C46 C47 123.7(6) . . ? C48 C47 C52 121.0(6) . . ? C48 C47 C46 117.4(6) . . ? C52 C47 C46 121.4(6) . . ? C49 C48 C47 119.1(7) . . ? C49 C48 H48 120.5 . . ? C47 C48 H48 120.5 . . ? C50 C49 C48 120.4(7) . . ? C50 C49 H49 119.8 . . ? C48 C49 H49 119.8 . . ? C49 C50 C51 120.5(7) . . ? C49 C50 H50 119.7 . . ? C51 C50 H50 119.7 . . ? O3 C51 C50 114.8(6) . . ? O3 C51 C52 123.4(7) . . ? C50 C51 C52 121.8(7) . . ? C51 C52 C47 117.1(7) . . ? C51 C52 H52 121.4 . . ? C47 C52 H52 121.4 . . ? O3 C53 C54 108.7(5) . . ? O3 C53 H53A 110.0 . . ? C54 C53 H53A 110.0 . . ? O3 C53 H53B 110.0 . . ? C54 C53 H53B 110.0 . . ? H53A C53 H53B 108.3 . . ? C59 C54 C55 119.2(6) . . ? C59 C54 C53 118.4(6) . . ? C55 C54 C53 122.4(6) . . ? C54 C55 C56 121.3(7) . . ? C54 C55 H55 119.3 . . ? C56 C55 H55 119.3 . . ? C57 C56 C55 119.6(7) . . ? C57 C56 H56 120.2 . . ? C55 C56 H56 120.2 . . ? C58 C57 C56 117.6(7) . . ? C58 C57 H57 121.2 . . ? C56 C57 H57 121.2 . . ? C57 C58 C59 121.9(6) . . ? C57 C58 C60 121.0(7) . . ? C59 C58 C60 117.1(7) . . ? C54 C59 C58 120.3(6) . . ? C54 C59 H59 119.8 . . ? C58 C59 H59 119.8 . . ? N4 C60 C58 178.4(8) . . ? O7 C61 C62 108.2(11) . . ? O7 C61 H61A 110.0 . . ? C62 C61 H61A 110.0 . . ? O7 C61 H61B 110.0 . . ? C62 C61 H61B 110.0 . . ? H61A C61 H61B 108.4 . . ? C63 C62 C61 103.1(11) . . ? C63 C62 H62A 111.1 . . ? C61 C62 H62A 111.1 . . ? C63 C62 H62B 111.1 . . ? C61 C62 H62B 111.1 . . ? H62A C62 H62B 109.1 . . ? C62 C63 C64 106.6(11) . . ? C62 C63 H63A 110.4 . . ? C64 C63 H63A 110.4 . . ? C62 C63 H63B 110.4 . . ? C64 C63 H63B 110.4 . . ? H63A C63 H63B 108.6 . . ? O7 C64 C63 105.3(10) . . ? O7 C64 H64A 110.7 . . ? C63 C64 H64A 110.7 . . ? O7 C64 H64B 110.7 . . ? C63 C64 H64B 110.7 . . ? H64A C64 H64B 108.8 . . ? C68 C67 C66 100.9(8) . . ? C68 C67 H67A 111.6 . . ? C66 C67 H67A 111.6 . . ? C68 C67 H67B 111.6 . . ? C66 C67 H67B 111.6 . . ? H67A C67 H67B 109.4 . . ? C65 C66 C67 100.1(8) . . ? C65 C66 H66A 111.8 . . ? C67 C66 H66A 111.8 . . ? C65 C66 H66B 111.8 . . ? C67 C66 H66B 111.8 . . ? H66A C66 H66B 109.5 . . ? O8 C65 C66 94.3(16) . . ? O8 C65 H65A 112.9 . . ? C66 C65 H65A 112.9 . . ? O8 C65 H65B 112.9 . . ? C66 C65 H65B 112.9 . . ? H65A C65 H65B 110.3 . . ? C65 O8 C68 128(2) . . ? C45 N1 N2 106.8(5) . . ? C45 N1 Ag2 133.0(5) . . ? N2 N1 Ag2 118.6(4) . . ? C46 N2 N1 105.8(5) . . ? C46 N2 Ag1 133.0(5) . . ? N1 N2 Ag1 119.9(4) . . ? C31 N3 Ag1 154.4(7) . 2_554 ? C60 N4 Ag2 146.7(6) . 2_554 ? C16 N5 N6 107.3(5) . . ? C16 N5 Ag2 135.3(5) . . ? N6 N5 Ag2 117.2(4) . . ? C15 N6 N5 106.8(5) . . ? C15 N6 Ag1 129.6(5) . . ? N5 N6 Ag1 122.5(4) . . ? C1 N7 Ag2 151.4(7) . 2 ? C27 N8 Ag1 158.0(7) . 2 ? C46 O1 C45 103.2(6) . . ? C39 O2 C38 116.0(6) . . ? C51 O3 C53 117.9(5) . . ? C15 O4 C16 103.7(6) . . ? C9 O5 C8 116.5(5) . . ? C21 O6 C23 115.8(5) . . ? C64 O7 C61 111.0(10) . . ? O8 C68 C67 91.2(15) . . ? O8 C68 H68A 113.4 . . ? C67 C68 H68A 113.4 . . ? O8 C68 H68B 113.4 . . ? C67 C68 H68B 113.4 . . ? H68A C68 H68B 110.7 . . ? F5 P1 F1 94.8(6) . . ? F5 P1 F3 176.3(6) . . ? F1 P1 F3 89.0(5) . . ? F5 P1 F4 91.2(7) . . ? F1 P1 F4 91.4(4) . . ? F3 P1 F4 89.2(5) . . ? F5 P1 F2 92.1(6) . . ? F1 P1 F2 88.8(4) . . ? F3 P1 F2 87.5(5) . . ? F4 P1 F2 176.6(5) . . ? F5 P1 F6 89.5(6) . . ? F1 P1 F6 175.6(6) . . ? F3 P1 F6 86.8(6) . . ? F4 P1 F6 89.5(4) . . ? F2 P1 F6 90.0(4) . . ? F12 P2 F10 91.5(7) . . ? F12 P2 F11 91.1(7) . . ? F10 P2 F11 92.3(6) . . ? F12 P2 F9 177.5(7) . . ? F10 P2 F9 89.1(5) . . ? F11 P2 F9 91.3(6) . . ? F12 P2 F7 90.7(6) . . ? F10 P2 F7 176.6(6) . . ? F11 P2 F7 90.1(5) . . ? F9 P2 F7 88.6(6) . . ? F12 P2 F8 93.5(6) . . ? F10 P2 F8 90.7(5) . . ? F11 P2 F8 174.4(6) . . ? F9 P2 F8 84.1(6) . . ? F7 P2 F8 86.6(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N7 C1 C2 C3 -15(52) . . . . ? N7 C1 C2 C7 167(100) . . . . ? C7 C2 C3 C4 4.2(16) . . . . ? C1 C2 C3 C4 -173.8(10) . . . . ? C2 C3 C4 C5 -9.6(19) . . . . ? C3 C4 C5 C6 12(2) . . . . ? C4 C5 C6 C7 -9(2) . . . . ? C4 C5 C6 C8 175.2(12) . . . . ? C5 C6 C7 C2 2.7(13) . . . . ? C8 C6 C7 C2 178.8(7) . . . . ? C3 C2 C7 C6 -0.7(12) . . . . ? C1 C2 C7 C6 177.3(7) . . . . ? C5 C6 C8 O5 -164.4(10) . . . . ? C7 C6 C8 O5 19.4(10) . . . . ? O5 C9 C10 C11 179.0(7) . . . . ? C14 C9 C10 C11 -1.3(11) . . . . ? C9 C10 C11 C12 0.3(11) . . . . ? C10 C11 C12 C13 1.7(12) . . . . ? C11 C12 C13 C14 -2.7(12) . . . . ? C11 C12 C13 C15 173.6(7) . . . . ? C12 C13 C14 C9 1.6(11) . . . . ? C15 C13 C14 C9 -174.4(7) . . . . ? C10 C9 C14 C13 0.4(11) . . . . ? O5 C9 C14 C13 -179.9(6) . . . . ? C12 C13 C15 N6 -35.7(11) . . . . ? C14 C13 C15 N6 140.5(8) . . . . ? C12 C13 C15 O4 143.9(7) . . . . ? C14 C13 C15 O4 -39.9(11) . . . . ? N5 C16 C17 C22 -148.2(7) . . . . ? O4 C16 C17 C22 33.6(11) . . . . ? N5 C16 C17 C18 30.4(12) . . . . ? O4 C16 C17 C18 -147.8(7) . . . . ? C22 C17 C18 C19 0.1(11) . . . . ? C16 C17 C18 C19 -178.5(7) . . . . ? C17 C18 C19 C20 0.9(13) . . . . ? C18 C19 C20 C21 0.0(12) . . . . ? C19 C20 C21 O6 179.7(7) . . . . ? C19 C20 C21 C22 -1.9(11) . . . . ? O6 C21 C22 C17 -178.6(6) . . . . ? C20 C21 C22 C17 2.9(10) . . . . ? C18 C17 C22 C21 -2.0(11) . . . . ? C16 C17 C22 C21 176.5(6) . . . . ? O6 C23 C24 C25 -3.7(11) . . . . ? O6 C23 C24 C30 178.4(8) . . . . ? C30 C24 C25 C26 -0.3(13) . . . . ? C23 C24 C25 C26 -178.1(7) . . . . ? C24 C25 C26 C28 1.1(12) . . . . ? C24 C25 C26 C27 177.1(7) . . . . ? C25 C26 C27 N8 -165(28) . . . . ? C28 C26 C27 N8 11(29) . . . . ? C25 C26 C28 C29 1.0(15) . . . . ? C27 C26 C28 C29 -175.1(10) . . . . ? C26 C28 C29 C30 -3.9(19) . . . . ? C28 C29 C30 C24 5(2) . . . . ? C25 C24 C30 C29 -2.7(17) . . . . ? C23 C24 C30 C29 175.3(11) . . . . ? N3 C31 C32 C33 26(12) . . . . ? N3 C31 C32 C37 -153(12) . . . . ? C37 C32 C33 C34 0.3(11) . . . . ? C31 C32 C33 C34 -178.6(7) . . . . ? C32 C33 C34 C35 0.4(12) . . . . ? C33 C34 C35 C36 0.7(13) . . . . ? C34 C35 C36 C37 -2.5(12) . . . . ? C34 C35 C36 C38 177.5(7) . . . . ? C33 C32 C37 C36 -2.1(11) . . . . ? C31 C32 C37 C36 176.9(7) . . . . ? C35 C36 C37 C32 3.0(10) . . . . ? C38 C36 C37 C32 -177.0(7) . . . . ? C35 C36 C38 O2 176.4(6) . . . . ? C37 C36 C38 O2 -3.6(10) . . . . ? O2 C39 C40 C41 -179.8(7) . . . . ? C44 C39 C40 C41 -1.0(12) . . . . ? C39 C40 C41 C42 0.8(12) . . . . ? C40 C41 C42 C43 -1.4(11) . . . . ? C41 C42 C43 C44 2.4(11) . . . . ? C41 C42 C43 C45 -176.8(6) . . . . ? O2 C39 C44 C43 -179.3(6) . . . . ? C40 C39 C44 C43 1.8(10) . . . . ? C42 C43 C44 C39 -2.6(10) . . . . ? C45 C43 C44 C39 176.5(6) . . . . ? C42 C43 C45 N1 33.1(10) . . . . ? C44 C43 C45 N1 -146.1(7) . . . . ? C42 C43 C45 O1 -144.0(7) . . . . ? C44 C43 C45 O1 36.8(10) . . . . ? N2 C46 C47 C48 -34.4(11) . . . . ? O1 C46 C47 C48 146.4(7) . . . . ? N2 C46 C47 C52 141.7(7) . . . . ? O1 C46 C47 C52 -37.6(10) . . . . ? C52 C47 C48 C49 -2.3(11) . . . . ? C46 C47 C48 C49 173.7(7) . . . . ? C47 C48 C49 C50 0.6(12) . . . . ? C48 C49 C50 C51 1.3(13) . . . . ? C49 C50 C51 O3 178.7(7) . . . . ? C49 C50 C51 C52 -1.6(12) . . . . ? O3 C51 C52 C47 179.6(6) . . . . ? C50 C51 C52 C47 -0.1(11) . . . . ? C48 C47 C52 C51 2.0(10) . . . . ? C46 C47 C52 C51 -173.9(7) . . . . ? O3 C53 C54 C59 -177.7(6) . . . . ? O3 C53 C54 C55 2.7(9) . . . . ? C59 C54 C55 C56 0.7(12) . . . . ? C53 C54 C55 C56 -179.7(7) . . . . ? C54 C55 C56 C57 0.6(13) . . . . ? C55 C56 C57 C58 -1.9(12) . . . . ? C56 C57 C58 C59 1.9(11) . . . . ? C56 C57 C58 C60 -179.5(7) . . . . ? C55 C54 C59 C58 -0.7(10) . . . . ? C53 C54 C59 C58 179.7(6) . . . . ? C57 C58 C59 C54 -0.7(11) . . . . ? C60 C58 C59 C54 -179.3(6) . . . . ? C57 C58 C60 N4 159(32) . . . . ? C59 C58 C60 N4 -22(33) . . . . ? O7 C61 C62 C63 6.8(19) . . . . ? C61 C62 C63 C64 7.7(18) . . . . ? C62 C63 C64 O7 -19.8(16) . . . . ? C68 C67 C66 C65 51(2) . . . . ? C67 C66 C65 O8 -33(2) . . . . ? C66 C65 O8 C68 6(4) . . . . ? O1 C45 N1 N2 -0.8(8) . . . . ? C43 C45 N1 N2 -178.1(6) . . . . ? O1 C45 N1 Ag2 -165.6(4) . . . . ? C43 C45 N1 Ag2 17.1(11) . . . . ? N5 Ag2 N1 C45 174.5(6) . . . . ? N7 Ag2 N1 C45 34.4(7) 2_554 . . . ? N4 Ag2 N1 C45 -65.9(7) 2 . . . ? N5 Ag2 N1 N2 11.1(5) . . . . ? N7 Ag2 N1 N2 -129.0(4) 2_554 . . . ? N4 Ag2 N1 N2 130.7(4) 2 . . . ? O1 C46 N2 N1 -1.0(8) . . . . ? C47 C46 N2 N1 179.7(6) . . . . ? O1 C46 N2 Ag1 165.1(5) . . . . ? C47 C46 N2 Ag1 -14.2(11) . . . . ? C45 N1 N2 C46 1.0(7) . . . . ? Ag2 N1 N2 C46 168.4(5) . . . . ? C45 N1 N2 Ag1 -167.2(5) . . . . ? Ag2 N1 N2 Ag1 0.2(6) . . . . ? N6 Ag1 N2 C46 -172.7(6) . . . . ? N8 Ag1 N2 C46 -36.1(7) 2_554 . . . ? N3 Ag1 N2 C46 72.6(7) 2 . . . ? N6 Ag1 N2 N1 -8.2(5) . . . . ? N8 Ag1 N2 N1 128.4(5) 2_554 . . . ? N3 Ag1 N2 N1 -122.9(5) 2 . . . ? C32 C31 N3 Ag1 -103(12) . . . 2_554 ? C58 C60 N4 Ag2 -17(33) . . . 2_554 ? O4 C16 N5 N6 -0.1(7) . . . . ? C17 C16 N5 N6 -178.4(7) . . . . ? O4 C16 N5 Ag2 -175.9(4) . . . . ? C17 C16 N5 Ag2 5.7(12) . . . . ? N7 Ag2 N5 C16 -74.2(8) 2_554 . . . ? N1 Ag2 N5 C16 159.6(6) . . . . ? N4 Ag2 N5 C16 34.9(7) 2 . . . ? N7 Ag2 N5 N6 110.3(5) 2_554 . . . ? N1 Ag2 N5 N6 -15.9(5) . . . . ? N4 Ag2 N5 N6 -140.6(4) 2 . . . ? O4 C15 N6 N5 -1.2(8) . . . . ? C13 C15 N6 N5 178.4(7) . . . . ? O4 C15 N6 Ag1 167.3(5) . . . . ? C13 C15 N6 Ag1 -13.1(11) . . . . ? C16 N5 N6 C15 0.7(7) . . . . ? Ag2 N5 N6 C15 177.4(5) . . . . ? C16 N5 N6 Ag1 -168.7(5) . . . . ? Ag2 N5 N6 Ag1 8.0(6) . . . . ? N8 Ag1 N6 C15 73.1(7) 2_554 . . . ? N2 Ag1 N6 C15 -163.7(6) . . . . ? N3 Ag1 N6 C15 -40.0(7) 2 . . . ? N8 Ag1 N6 N5 -120.1(5) 2_554 . . . ? N2 Ag1 N6 N5 3.1(6) . . . . ? N3 Ag1 N6 N5 126.8(5) 2 . . . ? C2 C1 N7 Ag2 75(52) . . . 2 ? C26 C27 N8 Ag1 -85(29) . . . 2 ? N2 C46 O1 C45 0.5(8) . . . . ? C47 C46 O1 C45 179.9(7) . . . . ? N1 C45 O1 C46 0.2(8) . . . . ? C43 C45 O1 C46 177.6(6) . . . . ? C44 C39 O2 C38 178.7(6) . . . . ? C40 C39 O2 C38 -2.5(10) . . . . ? C36 C38 O2 C39 -173.3(6) . . . . ? C50 C51 O3 C53 176.7(6) . . . . ? C52 C51 O3 C53 -3.0(10) . . . . ? C54 C53 O3 C51 -179.6(6) . . . . ? N6 C15 O4 C16 1.1(8) . . . . ? C13 C15 O4 C16 -178.5(7) . . . . ? N5 C16 O4 C15 -0.6(8) . . . . ? C17 C16 O4 C15 177.9(6) . . . . ? C10 C9 O5 C8 2.8(10) . . . . ? C14 C9 O5 C8 -176.9(6) . . . . ? C6 C8 O5 C9 178.5(6) . . . . ? C20 C21 O6 C23 -4.5(10) . . . . ? C22 C21 O6 C23 177.0(6) . . . . ? C24 C23 O6 C21 -177.5(6) . . . . ? C63 C64 O7 C61 25.1(15) . . . . ? C62 C61 O7 C64 -20.7(18) . . . . ? C65 O8 C68 C67 25(4) . . . . ? C66 C67 C68 O8 -42.3(19) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.987 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.105 #===End data_11 _database_code_depnum_ccdc_archive 'CCDC 791147' #TrackingRef '- CIF_1.1.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30.50 H22 Ag Cl2 N4 O7.50' _chemical_formula_weight 743.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 24.744(4) _cell_length_b 13.627(2) _cell_length_c 19.476(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.663(3) _cell_angle_gamma 90.00 _cell_volume 6407(2) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4153 _cell_measurement_theta_min 2.420 _cell_measurement_theta_max 22.255 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.541 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2992 _exptl_absorpt_coefficient_mu 0.849 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6761 _exptl_absorpt_correction_T_max 0.8832 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16467 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.50 _reflns_number_total 5940 _reflns_number_gt 4110 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1201P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5940 _refine_ls_number_parameters 424 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0796 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.1852 _refine_ls_wR_factor_gt 0.1649 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.033 _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 0.430179(17) 0.55247(3) 0.18929(2) 0.0716(2) Uani 1 1 d . . . C1 C 0.5189(2) -0.3065(4) 0.1304(3) 0.0632(12) Uani 1 1 d . . . C2 C 0.54973(18) -0.2429(3) 0.0950(2) 0.0547(11) Uani 1 1 d . . . C3 C 0.58318(19) -0.2846(4) 0.0546(2) 0.0591(12) Uani 1 1 d . . . H3 H 0.5865 -0.3524 0.0520 0.071 Uiso 1 1 calc R . . C4 C 0.6114(2) -0.2236(4) 0.0184(3) 0.0622(13) Uani 1 1 d . . . H4 H 0.6342 -0.2503 -0.0088 0.075 Uiso 1 1 calc R . . C5 C 0.60616(18) -0.1236(4) 0.0222(3) 0.0591(12) Uani 1 1 d . . . H5 H 0.6258 -0.0835 -0.0024 0.071 Uiso 1 1 calc R . . C6 C 0.57199(17) -0.0808(3) 0.0620(2) 0.0494(10) Uani 1 1 d . . . C7 C 0.54389(17) -0.1407(3) 0.0984(2) 0.0524(10) Uani 1 1 d . . . H7 H 0.5210 -0.1138 0.1254 0.063 Uiso 1 1 calc R . . C8 C 0.56695(19) 0.0289(3) 0.0606(3) 0.0545(11) Uani 1 1 d . . . H8A H 0.6029 0.0582 0.0790 0.065 Uiso 1 1 calc R . . H8B H 0.5538 0.0512 0.0126 0.065 Uiso 1 1 calc R . . C9 C 0.51940(16) 0.1567(3) 0.1060(2) 0.0479(10) Uani 1 1 d . . . C10 C 0.54390(18) 0.2284(3) 0.0731(2) 0.0537(11) Uani 1 1 d . . . H10 H 0.5692 0.2111 0.0462 0.064 Uiso 1 1 calc R . . C11 C 0.53074(19) 0.3260(3) 0.0803(3) 0.0599(12) Uani 1 1 d . . . H11 H 0.5474 0.3740 0.0580 0.072 Uiso 1 1 calc R . . C12 C 0.49325(18) 0.3531(3) 0.1200(2) 0.0543(11) Uani 1 1 d . . . H12 H 0.4844 0.4188 0.1243 0.065 Uiso 1 1 calc R . . C13 C 0.46894(16) 0.2804(3) 0.1535(2) 0.0441(9) Uani 1 1 d . . . C14 C 0.48168(16) 0.1823(3) 0.1463(2) 0.0482(10) Uani 1 1 d . . . H14 H 0.4651 0.1339 0.1683 0.058 Uiso 1 1 calc R . . C15 C 0.43018(15) 0.3097(3) 0.1960(2) 0.0434(9) Uani 1 1 d . . . C16 C 0.37183(17) 0.2901(3) 0.2617(2) 0.0455(10) Uani 1 1 d . . . C17 C 0.33712(16) 0.2395(3) 0.3014(2) 0.0466(10) Uani 1 1 d . . . C18 C 0.31485(19) 0.2941(3) 0.3487(2) 0.0583(12) Uani 1 1 d . . . H18 H 0.3219 0.3610 0.3539 0.070 Uiso 1 1 calc R . . C19 C 0.2824(2) 0.2482(4) 0.3876(3) 0.0644(13) Uani 1 1 d . . . H19 H 0.2676 0.2843 0.4197 0.077 Uiso 1 1 calc R . . C20 C 0.27139(19) 0.1491(4) 0.3796(2) 0.0578(11) Uani 1 1 d . . . H20 H 0.2485 0.1192 0.4054 0.069 Uiso 1 1 calc R . . C21 C 0.29395(17) 0.0946(3) 0.3339(2) 0.0489(10) Uani 1 1 d . . . C22 C 0.32780(15) 0.1406(3) 0.2946(2) 0.0458(9) Uani 1 1 d . . . H22 H 0.3439 0.1040 0.2641 0.055 Uiso 1 1 calc R . . C23 C 0.2527(2) -0.0538(3) 0.3619(3) 0.0600(13) Uani 1 1 d . . . H23A H 0.2143 -0.0364 0.3432 0.072 Uiso 1 1 calc R . . H23B H 0.2624 -0.0342 0.4109 0.072 Uiso 1 1 calc R . . C24 C 0.26009(17) -0.1619(3) 0.3561(2) 0.0499(10) Uani 1 1 d . . . C25 C 0.2343(2) -0.2239(4) 0.3952(3) 0.0615(12) Uani 1 1 d . . . H25 H 0.2114 -0.1971 0.4224 0.074 Uiso 1 1 calc R . . C26 C 0.2414(2) -0.3234(4) 0.3950(3) 0.0735(14) Uani 1 1 d . . . H26 H 0.2232 -0.3632 0.4215 0.088 Uiso 1 1 calc R . . C27 C 0.2755(2) -0.3649(4) 0.3557(2) 0.0622(12) Uani 1 1 d . . . H27 H 0.2812 -0.4324 0.3560 0.075 Uiso 1 1 calc R . . C28 C 0.30075(18) -0.3045(3) 0.3161(2) 0.0523(10) Uani 1 1 d . . . C29 C 0.29347(17) -0.2032(3) 0.3157(2) 0.0509(10) Uani 1 1 d . . . H29 H 0.3110 -0.1636 0.2883 0.061 Uiso 1 1 calc R . . C30 C 0.3375(2) -0.3445(4) 0.2751(3) 0.0610(12) Uani 1 1 d . . . Cl1 Cl 0.15203(5) 0.02691(9) 0.48358(7) 0.0645(3) Uani 1 1 d . . . N1 N 0.37859(15) 0.3831(3) 0.25722(19) 0.0528(9) Uani 1 1 d . . . N2 N 0.41730(14) 0.3942(3) 0.21409(19) 0.0504(8) Uani 1 1 d . . . N3 N 0.4937(2) -0.3566(3) 0.1586(3) 0.0795(13) Uani 1 1 d . . . N4 N 0.3669(2) -0.3751(3) 0.2435(3) 0.0785(13) Uani 1 1 d . . . O1 O 0.40282(11) 0.2377(2) 0.22440(15) 0.0458(7) Uani 1 1 d . . . O2 O 0.52922(14) 0.0584(2) 0.10229(19) 0.0622(9) Uani 1 1 d . . . O3 O 0.28740(13) -0.0039(2) 0.32336(18) 0.0620(8) Uani 1 1 d . . . O4 O 0.1340(3) 0.1050(6) 0.4414(4) 0.189(3) Uani 1 1 d . . . O5 O 0.20999(18) 0.0401(3) 0.5116(3) 0.0956(13) Uani 1 1 d . . . O6 O 0.12625(19) 0.0165(3) 0.5410(3) 0.1030(14) Uani 1 1 d . . . O7 O 0.1438(2) -0.0631(4) 0.4451(3) 0.1202(18) Uani 1 1 d . . . C31 C 0.3760(8) 0.8294(7) 0.1370(7) 0.146(7) Uani 0.50 1 d PD A 1 H31A H 0.3994 0.7832 0.1191 0.176 Uiso 0.50 1 calc PR A 1 H31B H 0.3487 0.7916 0.1545 0.176 Uiso 0.50 1 calc PR A 1 Cl2 Cl 0.4153(3) 0.8898(9) 0.2048(4) 0.235(4) Uani 0.50 1 d PD A 1 Cl3 Cl 0.3440(4) 0.8958(8) 0.0722(5) 0.261(5) Uani 0.50 1 d PD A 1 O8 O 0.3508(12) 0.9588(18) 0.1433(11) 0.34(2) Uani 0.50 1 d P B 2 H8C H 0.3849 0.9764 0.1552 0.513 Uiso 0.50 1 d PR B 2 H8D H 0.3429 0.8973 0.1415 0.513 Uiso 0.50 1 d PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0904(4) 0.0424(3) 0.0942(4) -0.00241(18) 0.0466(3) -0.00503(17) C1 0.064(3) 0.050(3) 0.077(3) -0.001(2) 0.021(3) 0.003(2) C2 0.053(3) 0.049(3) 0.060(3) -0.002(2) 0.011(2) 0.002(2) C3 0.056(3) 0.054(3) 0.067(3) -0.006(2) 0.014(2) 0.012(2) C4 0.061(3) 0.066(3) 0.063(3) -0.007(2) 0.021(2) 0.019(2) C5 0.055(3) 0.062(3) 0.065(3) -0.001(2) 0.023(2) 0.009(2) C6 0.043(2) 0.049(2) 0.055(3) -0.005(2) 0.0095(19) 0.0034(18) C7 0.048(2) 0.057(3) 0.053(3) -0.007(2) 0.015(2) 0.006(2) C8 0.049(2) 0.053(3) 0.067(3) -0.005(2) 0.023(2) 0.002(2) C9 0.046(2) 0.044(2) 0.055(3) -0.0035(19) 0.0162(19) 0.0000(18) C10 0.052(2) 0.052(3) 0.062(3) -0.007(2) 0.022(2) -0.005(2) C11 0.067(3) 0.049(3) 0.071(3) 0.000(2) 0.032(2) -0.012(2) C12 0.062(3) 0.038(2) 0.067(3) -0.003(2) 0.025(2) -0.0020(19) C13 0.046(2) 0.040(2) 0.047(2) -0.0028(18) 0.0142(18) -0.0034(17) C14 0.047(2) 0.048(2) 0.051(2) -0.0001(19) 0.0154(19) -0.0010(18) C15 0.046(2) 0.039(2) 0.045(2) -0.0015(17) 0.0106(18) -0.0025(16) C16 0.046(2) 0.045(2) 0.046(2) -0.0039(18) 0.0119(18) 0.0031(17) C17 0.042(2) 0.048(2) 0.050(2) -0.0031(19) 0.0101(18) -0.0011(18) C18 0.069(3) 0.042(2) 0.071(3) -0.012(2) 0.032(2) -0.006(2) C19 0.074(3) 0.054(3) 0.076(3) -0.017(2) 0.041(3) -0.004(2) C20 0.061(3) 0.056(3) 0.065(3) -0.006(2) 0.030(2) -0.006(2) C21 0.046(2) 0.045(2) 0.058(3) -0.004(2) 0.016(2) -0.0041(18) C22 0.044(2) 0.045(2) 0.052(2) -0.0051(18) 0.0177(18) 0.0015(17) C23 0.063(3) 0.048(3) 0.081(3) -0.001(2) 0.041(3) -0.007(2) C24 0.049(2) 0.048(2) 0.056(3) 0.001(2) 0.018(2) -0.0019(18) C25 0.068(3) 0.055(3) 0.070(3) -0.003(2) 0.035(2) -0.004(2) C26 0.095(4) 0.058(3) 0.077(3) 0.011(3) 0.039(3) -0.010(3) C27 0.075(3) 0.046(3) 0.064(3) 0.004(2) 0.014(3) 0.000(2) C28 0.052(2) 0.049(2) 0.055(3) -0.003(2) 0.008(2) -0.0004(19) C29 0.051(2) 0.046(2) 0.059(3) -0.002(2) 0.017(2) -0.0048(18) C30 0.064(3) 0.046(3) 0.074(3) -0.005(2) 0.018(3) 0.005(2) Cl1 0.0725(8) 0.0615(7) 0.0651(8) -0.0028(6) 0.0272(6) -0.0069(6) N1 0.062(2) 0.041(2) 0.063(2) -0.0021(17) 0.0301(18) 0.0014(16) N2 0.058(2) 0.040(2) 0.057(2) 0.0011(16) 0.0224(18) -0.0002(16) N3 0.082(3) 0.059(3) 0.103(4) 0.003(3) 0.035(3) -0.005(2) N4 0.085(3) 0.057(3) 0.101(3) -0.013(2) 0.035(3) 0.007(2) O1 0.0464(15) 0.0393(15) 0.0559(17) -0.0012(13) 0.0204(13) -0.0014(12) O2 0.070(2) 0.0463(18) 0.083(2) 0.0017(15) 0.0429(18) 0.0087(14) O3 0.075(2) 0.0457(18) 0.077(2) -0.0055(16) 0.0438(17) -0.0067(15) O4 0.199(6) 0.149(6) 0.195(7) 0.094(6) -0.011(5) 0.014(5) O5 0.084(3) 0.107(3) 0.097(3) -0.005(2) 0.022(2) -0.019(2) O6 0.116(3) 0.094(3) 0.123(4) -0.019(3) 0.079(3) -0.006(3) O7 0.124(4) 0.122(4) 0.129(4) -0.074(3) 0.060(3) -0.038(3) C31 0.25(2) 0.029(6) 0.134(13) -0.001(7) -0.015(13) 0.000(8) Cl2 0.194(6) 0.358(12) 0.130(4) -0.013(6) -0.015(4) -0.061(8) Cl3 0.280(9) 0.246(10) 0.234(8) 0.092(8) 0.010(7) -0.092(8) O8 0.46(4) 0.41(3) 0.178(17) 0.076(18) 0.117(19) 0.37(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 N3 2.185(5) 1_565 ? Ag1 N2 2.248(3) . ? Ag1 N4 2.294(5) 1_565 ? C1 N3 1.144(6) . ? C1 C2 1.428(7) . ? C2 C3 1.382(6) . ? C2 C7 1.403(6) . ? C3 C4 1.375(7) . ? C3 H3 0.9300 . ? C4 C5 1.372(7) . ? C4 H4 0.9300 . ? C5 C6 1.394(6) . ? C5 H5 0.9300 . ? C6 C7 1.367(6) . ? C6 C8 1.500(6) . ? C7 H7 0.9300 . ? C8 O2 1.422(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O2 1.367(5) . ? C9 C10 1.379(6) . ? C9 C14 1.389(6) . ? C10 C11 1.383(6) . ? C10 H10 0.9300 . ? C11 C12 1.382(6) . ? C11 H11 0.9300 . ? C12 C13 1.394(6) . ? C12 H12 0.9300 . ? C13 C14 1.388(6) . ? C13 C15 1.454(5) . ? C14 H14 0.9300 . ? C15 N2 1.266(5) . ? C15 O1 1.375(5) . ? C16 N1 1.283(5) . ? C16 O1 1.369(5) . ? C16 C17 1.449(6) . ? C17 C22 1.369(6) . ? C17 C18 1.388(6) . ? C18 C19 1.370(6) . ? C18 H18 0.9300 . ? C19 C20 1.380(7) . ? C19 H19 0.9300 . ? C20 C21 1.368(6) . ? C20 H20 0.9300 . ? C21 O3 1.362(5) . ? C21 C22 1.400(6) . ? C22 H22 0.9300 . ? C23 O3 1.429(5) . ? C23 C24 1.492(6) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C29 1.380(6) . ? C24 C25 1.383(6) . ? C25 C26 1.368(7) . ? C25 H25 0.9300 . ? C26 C27 1.379(7) . ? C26 H26 0.9300 . ? C27 C28 1.368(6) . ? C27 H27 0.9300 . ? C28 C29 1.392(6) . ? C28 C30 1.443(7) . ? C29 H29 0.9300 . ? C30 N4 1.130(6) . ? Cl1 O4 1.359(6) . ? Cl1 O6 1.412(4) . ? Cl1 O7 1.429(4) . ? Cl1 O5 1.429(4) . ? N1 N2 1.414(5) . ? N3 Ag1 2.185(5) 1_545 ? N4 Ag1 2.294(5) 1_545 ? C31 Cl3 1.613(8) . ? C31 Cl2 1.674(8) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H8D 1.2520 . ? Cl2 H8C 1.6046 . ? Cl3 H8D 1.3582 . ? O8 H8C 0.8592 . ? O8 H8D 0.8596 . ? 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 N3 Ag1 N2 138.33(15) 1_565 . ? N3 Ag1 N4 119.10(18) 1_565 1_565 ? N2 Ag1 N4 99.82(15) . 1_565 ? N3 C1 C2 179.2(5) . . ? C3 C2 C7 121.1(4) . . ? C3 C2 C1 118.4(4) . . ? C7 C2 C1 120.5(4) . . ? C4 C3 C2 118.5(4) . . ? C4 C3 H3 120.8 . . ? C2 C3 H3 120.8 . . ? C5 C4 C3 120.7(4) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 121.3(5) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C7 C6 C5 118.6(4) . . ? C7 C6 C8 123.6(4) . . ? C5 C6 C8 117.8(4) . . ? C6 C7 C2 119.9(4) . . ? C6 C7 H7 120.1 . . ? C2 C7 H7 120.1 . . ? O2 C8 C6 109.6(4) . . ? O2 C8 H8A 109.8 . . ? C6 C8 H8A 109.8 . . ? O2 C8 H8B 109.8 . . ? C6 C8 H8B 109.8 . . ? H8A C8 H8B 108.2 . . ? O2 C9 C10 124.6(4) . . ? O2 C9 C14 115.2(4) . . ? C10 C9 C14 120.2(4) . . ? C9 C10 C11 119.8(4) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C12 C11 C10 121.0(4) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C11 C12 C13 118.9(4) . . ? C11 C12 H12 120.6 . . ? C13 C12 H12 120.6 . . ? C14 C13 C12 120.5(4) . . ? C14 C13 C15 121.0(4) . . ? C12 C13 C15 118.5(4) . . ? C13 C14 C9 119.6(4) . . ? C13 C14 H14 120.2 . . ? C9 C14 H14 120.2 . . ? N2 C15 O1 111.2(3) . . ? N2 C15 C13 130.3(4) . . ? O1 C15 C13 118.5(3) . . ? N1 C16 O1 112.5(4) . . ? N1 C16 C17 127.4(4) . . ? O1 C16 C17 120.1(4) . . ? C22 C17 C18 120.5(4) . . ? C22 C17 C16 121.7(4) . . ? C18 C17 C16 117.8(4) . . ? C19 C18 C17 119.3(4) . . ? C19 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? C18 C19 C20 120.6(4) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C21 C20 C19 120.4(4) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? O3 C21 C20 125.5(4) . . ? O3 C21 C22 115.1(4) . . ? C20 C21 C22 119.4(4) . . ? C17 C22 C21 119.8(4) . . ? C17 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? O3 C23 C24 109.5(4) . . ? O3 C23 H23A 109.8 . . ? C24 C23 H23A 109.8 . . ? O3 C23 H23B 109.8 . . ? C24 C23 H23B 109.8 . . ? H23A C23 H23B 108.2 . . ? C29 C24 C25 118.2(4) . . ? C29 C24 C23 122.9(4) . . ? C25 C24 C23 118.9(4) . . ? C26 C25 C24 121.9(5) . . ? C26 C25 H25 119.1 . . ? C24 C25 H25 119.1 . . ? C25 C26 C27 120.2(5) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C28 C27 C26 118.4(5) . . ? C28 C27 H27 120.8 . . ? C26 C27 H27 120.8 . . ? C27 C28 C29 121.7(4) . . ? C27 C28 C30 120.4(4) . . ? C29 C28 C30 117.9(4) . . ? C24 C29 C28 119.6(4) . . ? C24 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? N4 C30 C28 179.1(6) . . ? O4 Cl1 O6 114.4(4) . . ? O4 Cl1 O7 111.4(5) . . ? O6 Cl1 O7 107.0(3) . . ? O4 Cl1 O5 107.5(4) . . ? O6 Cl1 O5 107.5(3) . . ? O7 Cl1 O5 108.9(3) . . ? C16 N1 N2 105.2(3) . . ? C15 N2 N1 108.2(3) . . ? C15 N2 Ag1 139.2(3) . . ? N1 N2 Ag1 112.1(2) . . ? C1 N3 Ag1 166.1(5) . 1_545 ? C30 N4 Ag1 174.0(5) . 1_545 ? C16 O1 C15 102.9(3) . . ? C9 O2 C8 117.0(3) . . ? C21 O3 C23 117.0(3) . . ? Cl3 C31 Cl2 116.2(7) . . ? Cl3 C31 H31A 108.2 . . ? Cl2 C31 H31A 108.2 . . ? Cl3 C31 H31B 108.2 . . ? Cl2 C31 H31B 108.2 . . ? H31A C31 H31B 107.4 . . ? Cl3 C31 H8D 54.9 . . ? Cl2 C31 H8D 81.8 . . ? H31A C31 H8D 163.1 . . ? H31B C31 H8D 81.3 . . ? C31 Cl2 H8C 76.8 . . ? C31 Cl3 H8D 48.9 . . ? H8C O8 H8D 119.0 . . ? 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 N3 C1 C2 C3 -146(47) . . . . ? N3 C1 C2 C7 31(48) . . . . ? C7 C2 C3 C4 0.9(7) . . . . ? C1 C2 C3 C4 177.7(5) . . . . ? C2 C3 C4 C5 -0.3(7) . . . . ? C3 C4 C5 C6 -0.6(8) . . . . ? C4 C5 C6 C7 0.8(7) . . . . ? C4 C5 C6 C8 -177.5(5) . . . . ? C5 C6 C7 C2 -0.2(6) . . . . ? C8 C6 C7 C2 178.0(4) . . . . ? C3 C2 C7 C6 -0.6(7) . . . . ? C1 C2 C7 C6 -177.4(4) . . . . ? C7 C6 C8 O2 -0.1(6) . . . . ? C5 C6 C8 O2 178.2(4) . . . . ? O2 C9 C10 C11 179.7(4) . . . . ? C14 C9 C10 C11 -0.1(7) . . . . ? C9 C10 C11 C12 0.0(7) . . . . ? C10 C11 C12 C13 0.4(7) . . . . ? C11 C12 C13 C14 -0.8(7) . . . . ? C11 C12 C13 C15 179.1(4) . . . . ? C12 C13 C14 C9 0.7(6) . . . . ? C15 C13 C14 C9 -179.2(4) . . . . ? O2 C9 C14 C13 179.9(4) . . . . ? C10 C9 C14 C13 -0.3(6) . . . . ? C14 C13 C15 N2 172.7(4) . . . . ? C12 C13 C15 N2 -7.2(7) . . . . ? C14 C13 C15 O1 -5.3(6) . . . . ? C12 C13 C15 O1 174.8(4) . . . . ? N1 C16 C17 C22 171.3(4) . . . . ? O1 C16 C17 C22 -9.8(6) . . . . ? N1 C16 C17 C18 -10.9(7) . . . . ? O1 C16 C17 C18 168.0(4) . . . . ? C22 C17 C18 C19 -1.4(7) . . . . ? C16 C17 C18 C19 -179.2(4) . . . . ? C17 C18 C19 C20 -0.6(8) . . . . ? C18 C19 C20 C21 1.7(8) . . . . ? C19 C20 C21 O3 177.9(4) . . . . ? C19 C20 C21 C22 -0.8(7) . . . . ? C18 C17 C22 C21 2.3(6) . . . . ? C16 C17 C22 C21 -180.0(4) . . . . ? O3 C21 C22 C17 -180.0(4) . . . . ? C20 C21 C22 C17 -1.2(6) . . . . ? O3 C23 C24 C29 -3.3(7) . . . . ? O3 C23 C24 C25 173.8(4) . . . . ? C29 C24 C25 C26 0.5(7) . . . . ? C23 C24 C25 C26 -176.8(5) . . . . ? C24 C25 C26 C27 0.7(8) . . . . ? C25 C26 C27 C28 -1.4(8) . . . . ? C26 C27 C28 C29 1.0(7) . . . . ? C26 C27 C28 C30 178.9(5) . . . . ? C25 C24 C29 C28 -0.9(7) . . . . ? C23 C24 C29 C28 176.3(4) . . . . ? C27 C28 C29 C24 0.1(7) . . . . ? C30 C28 C29 C24 -177.8(4) . . . . ? C27 C28 C30 N4 -118(41) . . . . ? C29 C28 C30 N4 60(41) . . . . ? O1 C16 N1 N2 -0.5(5) . . . . ? C17 C16 N1 N2 178.5(4) . . . . ? O1 C15 N2 N1 -0.3(4) . . . . ? C13 C15 N2 N1 -178.4(4) . . . . ? O1 C15 N2 Ag1 -171.8(3) . . . . ? C13 C15 N2 Ag1 10.1(7) . . . . ? C16 N1 N2 C15 0.5(5) . . . . ? C16 N1 N2 Ag1 174.5(3) . . . . ? N3 Ag1 N2 C15 -32.6(6) 1_565 . . . ? N4 Ag1 N2 C15 167.9(5) 1_565 . . . ? N3 Ag1 N2 N1 156.2(3) 1_565 . . . ? N4 Ag1 N2 N1 -3.3(3) 1_565 . . . ? C2 C1 N3 Ag1 54(48) . . . 1_545 ? C28 C30 N4 Ag1 76(42) . . . 1_545 ? N1 C16 O1 C15 0.3(4) . . . . ? C17 C16 O1 C15 -178.8(4) . . . . ? N2 C15 O1 C16 0.1(4) . . . . ? C13 C15 O1 C16 178.4(3) . . . . ? C10 C9 O2 C8 -0.8(7) . . . . ? C14 C9 O2 C8 179.0(4) . . . . ? C6 C8 O2 C9 -179.3(4) . . . . ? C20 C21 O3 C23 1.8(7) . . . . ? C22 C21 O3 C23 -179.4(4) . . . . ? C24 C23 O3 C21 -167.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.842 _refine_diff_density_min -0.482 _refine_diff_density_rms 0.111