Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _publ_contact_author_email BUXH@NANKAI.EDU.CN _publ_contact_author_name 'Prof Xianhe Bu' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_address ; Department of Chemistry Nankai University Weijin Road Tianjin 300071 CHINA ; _publ_section_title ; Polymeric Silver(I) Complexes with Pyridyl Dithioether Ligands: Experimental and Theoretical Investigations on the Coordination Properties of the Ligands ; loop_ _publ_author_name 'Bu Xianhe' 'Ya-Bo Xie' 'Chong Zhang' data_020904c _database_code_depnum_ccdc_archive 'CCDC 223559' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H28 Ag2 B2 F8 N4 S4' _chemical_formula_weight 914.12 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.690(3) _cell_length_b 10.188(4) _cell_length_c 10.689(4) _cell_angle_alpha 68.023(6) _cell_angle_beta 86.283(6) _cell_angle_gamma 66.403(6) _cell_volume 800.2(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 847 _cell_measurement_theta_min 3.68 _cell_measurement_theta_max 26.33 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.897 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 452 _exptl_absorpt_coefficient_mu 1.558 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.688293 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 4497 _diffrn_reflns_av_R_equivalents 0.0163 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 26.40 _reflns_number_total 3216 _reflns_number_gt 2619 _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^)+(0.0396P)^2^+0.6198P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3216 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0459 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0827 _refine_ls_wR_factor_gt 0.0754 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 0.38291(4) 0.60640(3) 0.31418(3) 0.04864(11) Uani 1 1 d . . . S1 S 0.56885(13) 0.26124(10) 0.28602(10) 0.0474(2) Uani 1 1 d . . . S2 S 0.64983(12) -0.32806(10) 0.42957(10) 0.0445(2) Uani 1 1 d . . . N1 N 0.5590(3) 0.5396(3) 0.1703(3) 0.0384(6) Uani 1 1 d . . . N2 N 0.7855(3) -0.6271(3) 0.5239(3) 0.0387(6) Uani 1 1 d . . . C1 C 0.6035(5) 0.6509(4) 0.0840(4) 0.0437(8) Uani 1 1 d . . . H1 H 0.5512 0.7501 0.0846 0.052 Uiso 1 1 calc R . . C2 C 0.7219(5) 0.6251(4) -0.0043(4) 0.0497(9) Uani 1 1 d . . . H2 H 0.7499 0.7048 -0.0625 0.060 Uiso 1 1 calc R . . C3 C 0.7990(5) 0.4780(5) -0.0053(4) 0.0532(10) Uani 1 1 d . . . H3 H 0.8804 0.4573 -0.0644 0.064 Uiso 1 1 calc R . . C4 C 0.7557(5) 0.3629(4) 0.0806(4) 0.0484(9) Uani 1 1 d . . . H4 H 0.8064 0.2634 0.0804 0.058 Uiso 1 1 calc R . . C5 C 0.6349(4) 0.3966(4) 0.1682(3) 0.0386(7) Uani 1 1 d . . . C6 C 0.6748(5) 0.0912(4) 0.2446(4) 0.0459(8) Uani 1 1 d . . . H6A H 0.6462 0.1161 0.1499 0.055 Uiso 1 1 calc R . . H6B H 0.7961 0.0545 0.2604 0.055 Uiso 1 1 calc R . . C7 C 0.6172(5) -0.0321(4) 0.3342(4) 0.0448(8) Uani 1 1 d . . . H7A H 0.4973 0.0019 0.3128 0.054 Uiso 1 1 calc R . . H7B H 0.6365 -0.0495 0.4286 0.054 Uiso 1 1 calc R . . C8 C 0.7144(5) -0.1818(4) 0.3119(4) 0.0435(8) Uani 1 1 d . . . H8A H 0.8348 -0.2135 0.3283 0.052 Uiso 1 1 calc R . . H8B H 0.6893 -0.1672 0.2193 0.052 Uiso 1 1 calc R . . C9 C 0.8009(4) -0.5038(4) 0.4281(3) 0.0361(7) Uani 1 1 d . . . C10 C 0.9216(5) -0.5188(4) 0.3368(4) 0.0451(8) Uani 1 1 d . . . H10 H 0.9334 -0.4322 0.2733 0.054 Uiso 1 1 calc R . . C11 C 1.0237(5) -0.6660(5) 0.3429(4) 0.0520(9) Uani 1 1 d . . . H11 H 1.1061 -0.6797 0.2833 0.062 Uiso 1 1 calc R . . C12 C 1.0033(5) -0.7907(4) 0.4363(4) 0.0518(9) Uani 1 1 d . . . H12 H 1.0689 -0.8900 0.4394 0.062 Uiso 1 1 calc R . . C13 C 0.8846(5) -0.7676(4) 0.5258(4) 0.0467(9) Uani 1 1 d . . . H13 H 0.8726 -0.8534 0.5905 0.056 Uiso 1 1 calc R . . B1 B 0.1963(6) 1.0079(5) 0.1098(5) 0.0495(10) Uani 1 1 d . . . F1 F 0.1866(4) 0.8640(3) 0.1407(3) 0.0936(9) Uani 1 1 d . . . F2 F 0.1016(4) 1.1204(3) -0.0126(3) 0.0775(8) Uani 1 1 d . . . F3 F 0.3611(3) 0.9930(4) 0.0959(4) 0.0984(11) Uani 1 1 d . . . F4 F 0.1397(5) 1.0692(3) 0.2072(3) 0.1004(11) 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 0.04839(17) 0.04223(17) 0.05000(18) -0.02106(13) 0.01740(13) -0.01194(12) S1 0.0607(6) 0.0357(5) 0.0487(5) -0.0218(4) 0.0194(4) -0.0192(4) S2 0.0488(5) 0.0333(4) 0.0506(5) -0.0192(4) 0.0180(4) -0.0148(4) N1 0.0404(15) 0.0327(14) 0.0444(16) -0.0214(13) 0.0041(13) -0.0107(12) N2 0.0412(15) 0.0345(14) 0.0406(16) -0.0160(13) 0.0082(12) -0.0148(12) C1 0.050(2) 0.0327(17) 0.049(2) -0.0175(16) 0.0027(17) -0.0151(16) C2 0.059(2) 0.041(2) 0.049(2) -0.0145(17) 0.0120(18) -0.0238(18) C3 0.057(2) 0.053(2) 0.051(2) -0.0250(19) 0.0224(19) -0.0213(19) C4 0.050(2) 0.0379(19) 0.054(2) -0.0233(18) 0.0114(17) -0.0102(16) C5 0.0423(18) 0.0318(16) 0.0385(19) -0.0153(15) 0.0025(15) -0.0099(14) C6 0.058(2) 0.0336(18) 0.045(2) -0.0182(16) 0.0104(17) -0.0144(16) C7 0.050(2) 0.0345(18) 0.049(2) -0.0185(16) 0.0097(17) -0.0147(16) C8 0.054(2) 0.0350(18) 0.044(2) -0.0181(16) 0.0130(17) -0.0196(16) C9 0.0376(17) 0.0360(17) 0.0375(18) -0.0184(15) 0.0043(14) -0.0138(14) C10 0.049(2) 0.044(2) 0.042(2) -0.0194(17) 0.0128(16) -0.0176(17) C11 0.052(2) 0.057(2) 0.047(2) -0.0297(19) 0.0193(18) -0.0153(19) C12 0.059(2) 0.040(2) 0.050(2) -0.0233(18) 0.0076(18) -0.0072(17) C13 0.054(2) 0.0346(18) 0.048(2) -0.0182(16) 0.0070(17) -0.0124(16) B1 0.047(2) 0.034(2) 0.053(3) -0.0182(19) 0.004(2) -0.0010(18) F1 0.110(2) 0.0535(16) 0.097(2) -0.0171(16) -0.0170(19) -0.0201(16) F2 0.0896(19) 0.0558(15) 0.0671(17) -0.0018(13) -0.0094(14) -0.0275(14) F3 0.0570(16) 0.083(2) 0.156(3) -0.059(2) 0.0107(18) -0.0159(15) F4 0.159(3) 0.0650(18) 0.0739(19) -0.0420(16) 0.044(2) -0.0324(19) _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 2.195(3) . ? Ag1 N2 2.209(3) 2_656 ? Ag1 F1 2.534(3) . ? S1 C5 1.748(3) . ? S1 C6 1.813(3) . ? S2 C9 1.751(3) . ? S2 C8 1.814(4) . ? N1 C1 1.344(5) . ? N1 C5 1.346(4) . ? N2 C13 1.336(4) . ? N2 C9 1.341(4) . ? N2 Ag1 2.209(3) 2_656 ? C1 C2 1.365(5) . ? C1 H1 0.9300 . ? C2 C3 1.379(5) . ? C2 H2 0.9300 . ? C3 C4 1.365(5) . ? C3 H3 0.9300 . ? C4 C5 1.386(5) . ? C4 H4 0.9300 . ? C6 C7 1.512(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.520(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.387(5) . ? C10 C11 1.382(5) . ? C10 H10 0.9300 . ? C11 C12 1.360(6) . ? C11 H11 0.9300 . ? C12 C13 1.372(5) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? B1 F4 1.375(5) . ? B1 F3 1.382(5) . ? B1 F2 1.401(5) . ? B1 F1 1.413(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N2 169.23(10) . 2_656 ? N1 Ag1 F1 95.40(11) . . ? N2 Ag1 F1 93.11(11) 2_656 . ? C5 S1 C6 102.70(16) . . ? C9 S2 C8 104.66(16) . . ? C1 N1 C5 118.0(3) . . ? C1 N1 Ag1 115.7(2) . . ? C5 N1 Ag1 126.1(2) . . ? C13 N2 C9 118.2(3) . . ? C13 N2 Ag1 119.3(2) . 2_656 ? C9 N2 Ag1 122.3(2) . 2_656 ? N1 C1 C2 123.1(3) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C1 C2 C3 118.4(3) . . ? C1 C2 H2 120.8 . . ? C3 C2 H2 120.8 . . ? C4 C3 C2 119.8(3) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 118.9(3) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 C4 121.8(3) . . ? N1 C5 S1 113.9(2) . . ? C4 C5 S1 124.3(3) . . ? C7 C6 S1 107.7(2) . . ? C7 C6 H6A 110.2 . . ? S1 C6 H6A 110.2 . . ? C7 C6 H6B 110.2 . . ? S1 C6 H6B 110.2 . . ? H6A C6 H6B 108.5 . . ? C6 C7 C8 109.6(3) . . ? C6 C7 H7A 109.7 . . ? C8 C7 H7A 109.7 . . ? C6 C7 H7B 109.7 . . ? C8 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? C7 C8 S2 107.5(2) . . ? C7 C8 H8A 110.2 . . ? S2 C8 H8A 110.2 . . ? C7 C8 H8B 110.2 . . ? S2 C8 H8B 110.2 . . ? H8A C8 H8B 108.5 . . ? N2 C9 C10 122.1(3) . . ? N2 C9 S2 112.6(2) . . ? C10 C9 S2 125.3(3) . . ? C11 C10 C9 118.2(3) . . ? C11 C10 H10 120.9 . . ? C9 C10 H10 120.9 . . ? C12 C11 C10 119.8(3) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 118.9(3) . . ? C11 C12 H12 120.5 . . ? C13 C12 H12 120.5 . . ? N2 C13 C12 122.8(3) . . ? N2 C13 H13 118.6 . . ? C12 C13 H13 118.6 . . ? F4 B1 F3 107.1(4) . . ? F4 B1 F2 106.4(3) . . ? F3 B1 F2 106.6(4) . . ? F4 B1 F1 113.4(4) . . ? F3 B1 F1 110.7(3) . . ? F2 B1 F1 112.2(4) . . ? B1 F1 Ag1 125.6(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ag1 N1 C1 -172.9(5) 2_656 . . . ? F1 Ag1 N1 C1 45.0(3) . . . . ? N2 Ag1 N1 C5 1.6(7) 2_656 . . . ? F1 Ag1 N1 C5 -140.5(3) . . . . ? C5 N1 C1 C2 -0.3(5) . . . . ? Ag1 N1 C1 C2 174.6(3) . . . . ? N1 C1 C2 C3 0.2(6) . . . . ? C1 C2 C3 C4 0.2(6) . . . . ? C2 C3 C4 C5 -0.4(6) . . . . ? C1 N1 C5 C4 0.1(5) . . . . ? Ag1 N1 C5 C4 -174.3(3) . . . . ? C1 N1 C5 S1 179.2(3) . . . . ? Ag1 N1 C5 S1 4.9(4) . . . . ? C3 C4 C5 N1 0.3(6) . . . . ? C3 C4 C5 S1 -178.8(3) . . . . ? C6 S1 C5 N1 174.0(3) . . . . ? C6 S1 C5 C4 -6.9(4) . . . . ? C5 S1 C6 C7 -176.0(3) . . . . ? S1 C6 C7 C8 -175.0(3) . . . . ? C6 C7 C8 S2 176.4(3) . . . . ? C9 S2 C8 C7 -165.8(3) . . . . ? C13 N2 C9 C10 -3.4(5) . . . . ? Ag1 N2 C9 C10 171.9(3) 2_656 . . . ? C13 N2 C9 S2 174.5(3) . . . . ? Ag1 N2 C9 S2 -10.1(3) 2_656 . . . ? C8 S2 C9 N2 171.5(2) . . . . ? C8 S2 C9 C10 -10.6(4) . . . . ? N2 C9 C10 C11 2.5(5) . . . . ? S2 C9 C10 C11 -175.2(3) . . . . ? C9 C10 C11 C12 0.3(6) . . . . ? C10 C11 C12 C13 -2.1(6) . . . . ? C9 N2 C13 C12 1.6(5) . . . . ? Ag1 N2 C13 C12 -173.9(3) 2_656 . . . ? C11 C12 C13 N2 1.2(6) . . . . ? F4 B1 F1 Ag1 -75.1(4) . . . . ? F3 B1 F1 Ag1 45.3(5) . . . . ? F2 B1 F1 Ag1 164.3(3) . . . . ? N1 Ag1 F1 B1 -92.6(3) . . . . ? N2 Ag1 F1 B1 94.0(3) 2_656 . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.687 _refine_diff_density_min -0.432 _refine_diff_density_rms 0.073 data_p-1 _database_code_depnum_ccdc_archive 'CCDC 223560' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H16 Ag Cl N2 O4 S2' _chemical_formula_sum 'C14 H16 Ag Cl N2 O4 S2' _chemical_formula_weight 483.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.634(2) _cell_length_b 9.967(2) _cell_length_c 11.967(2) _cell_angle_alpha 96.45(3) _cell_angle_beta 94.23(3) _cell_angle_gamma 104.63(3) _cell_volume 870.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 945 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 25.97 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.846 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 484 _exptl_absorpt_coefficient_mu 1.572 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6853 _exptl_absorpt_correction_T_max 0.7041 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 director' _diffrn_measurement_method 'Omig and Phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3754 _diffrn_reflns_av_R_equivalents 0.0197 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.50 _reflns_number_total 3141 _reflns_number_gt 2922 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0463P)^2^+2.3856P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.004(1) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3141 _refine_ls_number_parameters 227 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0515 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1222 _refine_ls_wR_factor_gt 0.1184 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _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 1.62147(6) 0.53636(4) 0.86835(3) 0.0575(2) Uani 1 1 d . . . Cl1 Cl 1.8870(2) 0.88056(14) 0.75563(13) 0.0609(4) Uani 1 1 d . . . S1 S 1.62018(18) 0.29984(13) 1.02420(12) 0.0511(3) Uani 1 1 d . . . S2 S 1.4577(2) 0.22891(16) 0.72865(12) 0.0610(4) Uani 1 1 d . . . N1 N 1.7870(6) 0.5611(4) 1.0305(4) 0.0458(9) Uani 1 1 d . . . N2 N 1.4578(6) 0.4823(5) 0.7033(4) 0.0490(10) Uani 1 1 d . . . C1 C 1.9001(8) 0.6847(6) 1.0754(5) 0.0564(13) Uani 1 1 d . . . H1A H 1.8945 0.7634 1.0417 0.068 Uiso 1 1 calc R . . C2 C 2.0225(8) 0.7014(6) 1.1676(5) 0.0611(14) Uani 1 1 d . . . H2A H 2.0989 0.7890 1.1959 0.073 Uiso 1 1 calc R . . C3 C 2.0304(8) 0.5871(6) 1.2174(5) 0.0574(13) Uani 1 1 d . . . H3A H 2.1145 0.5959 1.2799 0.069 Uiso 1 1 calc R . . C4 C 1.9147(7) 0.4578(6) 1.1758(5) 0.0514(12) Uani 1 1 d . . . H4A H 1.9190 0.3786 1.2092 0.062 Uiso 1 1 calc R . . C5 C 1.7926(6) 0.4502(5) 1.0831(4) 0.0429(10) Uani 1 1 d . . . C6 C 1.6797(10) 0.1582(6) 1.0876(6) 0.0743(19) Uani 1 1 d D . . H6A H 1.7751 0.1708 1.1479 0.089 Uiso 1 1 d R . . C7 C 1.5945(16) 0.0204(10) 1.0080(14) 0.095(4) Uani 0.70 1 d PD . 1 H7A H 1.6398 0.0299 0.9349 0.114 Uiso 0.70 1 calc PR . 1 H7B H 1.6365 -0.0538 1.0380 0.114 Uiso 0.70 1 calc PR . 1 C7' C 1.508(2) 0.0287(14) 1.0643(11) 0.034(3) Uani 0.30 1 d PD . 2 H7'A H 1.5226 -0.0427 1.1103 0.041 Uiso 0.30 1 calc PR . 2 H7'B H 1.3993 0.0568 1.0821 0.041 Uiso 0.30 1 calc PR . 2 C8 C 1.4112(8) 0.5859(6) 0.6551(5) 0.0600(14) Uani 1 1 d . . . H8A H 1.4617 0.6781 0.6880 0.072 Uiso 1 1 calc R . . C9 C 1.2915(9) 0.5597(7) 0.5589(6) 0.0687(16) Uani 1 1 d . . . H9A H 1.2615 0.6332 0.5274 0.082 Uiso 1 1 calc R . . C10 C 1.2163(8) 0.4240(7) 0.5097(5) 0.0649(15) Uani 1 1 d . . . H10A H 1.1350 0.4041 0.4445 0.078 Uiso 1 1 calc R . . C11 C 1.2635(8) 0.3182(6) 0.5584(5) 0.0581(13) Uani 1 1 d . . . H11A H 1.2143 0.2255 0.5263 0.070 Uiso 1 1 calc R . . C12 C 1.3847(7) 0.3496(6) 0.6554(4) 0.0468(11) Uani 1 1 d . . . C13 C 1.4010(8) 0.0688(5) 0.6311(5) 0.0560(13) Uani 1 1 d . . . H13A H 1.4115 -0.0076 0.6725 0.067 Uiso 1 1 calc R . . H13B H 1.2751 0.0498 0.5996 0.067 Uiso 1 1 calc R . . C14 C 1.5192(7) 0.0716(5) 0.5352(4) 0.0505(12) Uani 1 1 d . . . H14A H 1.6463 0.1013 0.5657 0.061 Uiso 1 1 calc R . . H14B H 1.4969 0.1390 0.4872 0.061 Uiso 1 1 calc R . . O1 O 1.8164(10) 0.7557(8) 0.7921(9) 0.170(4) Uani 1 1 d . . . O2 O 1.9838(11) 0.9757(7) 0.8453(7) 0.151(4) Uani 1 1 d . . . O3 O 1.7499(12) 0.9248(8) 0.7030(7) 0.155(4) Uani 1 1 d . . . O4 O 2.0064(11) 0.8469(12) 0.6831(6) 0.180(4) 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 0.0600(3) 0.0592(3) 0.0502(3) 0.00690(19) -0.00086(19) 0.0118(2) Cl1 0.0682(8) 0.0477(7) 0.0614(8) 0.0086(6) -0.0094(6) 0.0098(6) S1 0.0543(7) 0.0415(6) 0.0541(7) 0.0060(5) -0.0055(6) 0.0097(5) S2 0.0812(10) 0.0541(8) 0.0468(7) 0.0013(6) -0.0056(7) 0.0224(7) N1 0.047(2) 0.043(2) 0.047(2) 0.0049(18) 0.0039(17) 0.0117(17) N2 0.051(2) 0.050(2) 0.045(2) 0.0058(19) 0.0052(18) 0.0131(19) C1 0.060(3) 0.043(3) 0.065(3) 0.008(2) 0.007(3) 0.010(2) C2 0.054(3) 0.050(3) 0.071(4) -0.004(3) 0.002(3) 0.004(2) C3 0.052(3) 0.060(3) 0.055(3) -0.004(3) -0.001(2) 0.012(2) C4 0.053(3) 0.053(3) 0.049(3) 0.009(2) 0.003(2) 0.016(2) C5 0.044(2) 0.040(2) 0.044(3) 0.001(2) 0.0055(19) 0.0114(19) C6 0.087(4) 0.040(3) 0.086(5) 0.006(3) -0.030(4) 0.011(3) C7 0.085(8) 0.051(6) 0.143(13) 0.026(7) -0.018(10) 0.010(6) C7' 0.049(10) 0.027(7) 0.020(7) 0.003(5) 0.010(7) -0.001(7) C8 0.068(3) 0.054(3) 0.059(3) 0.012(3) 0.012(3) 0.013(3) C9 0.073(4) 0.072(4) 0.066(4) 0.024(3) 0.005(3) 0.023(3) C10 0.063(3) 0.075(4) 0.057(3) 0.013(3) -0.005(3) 0.020(3) C11 0.062(3) 0.061(3) 0.049(3) 0.002(3) -0.003(2) 0.017(3) C12 0.045(3) 0.055(3) 0.041(3) 0.004(2) 0.006(2) 0.014(2) C13 0.072(4) 0.040(3) 0.053(3) 0.005(2) 0.004(3) 0.011(2) C14 0.058(3) 0.040(3) 0.053(3) 0.007(2) 0.002(2) 0.011(2) O1 0.125(6) 0.123(6) 0.267(11) 0.130(7) -0.001(6) 0.000(4) O2 0.179(7) 0.097(4) 0.159(6) -0.059(4) -0.105(6) 0.068(5) O3 0.197(8) 0.124(5) 0.147(6) -0.002(4) -0.097(6) 0.090(5) O4 0.110(5) 0.306(13) 0.096(5) -0.009(7) 0.024(4) 0.016(7) _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 2.190(4) . ? Ag1 N2 2.193(4) . ? Cl1 O1 1.359(6) . ? Cl1 O3 1.373(6) . ? Cl1 O2 1.377(6) . ? Cl1 O4 1.379(8) . ? S1 C5 1.762(5) . ? S1 C6 1.814(6) . ? S2 C12 1.741(5) . ? S2 C13 1.805(5) . ? N1 C5 1.340(6) . ? N1 C1 1.341(7) . ? N2 C12 1.341(7) . ? N2 C8 1.347(7) . ? C1 C2 1.359(8) . ? C1 H1A 0.9300 . ? C2 C3 1.356(8) . ? C2 H2A 0.9300 . ? C3 C4 1.380(8) . ? C3 H3A 0.9300 . ? C4 C5 1.378(7) . ? C4 H4A 0.9300 . ? C6 C7 1.543(12) . ? C6 C7' 1.573(14) . ? C6 H6A 0.9600 . ? C7 C7 1.39(2) 2_857 ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7' C7' 1.57(3) 2_857 ? C7' H7'A 0.9700 . ? C7' H7'B 0.9700 . ? C8 C9 1.373(9) . ? C8 H8A 0.9300 . ? C9 C10 1.373(9) . ? C9 H9A 0.9300 . ? C10 C11 1.371(8) . ? C10 H10A 0.9300 . ? C11 C12 1.383(7) . ? C11 H11A 0.9300 . ? C13 C14 1.509(8) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C14 1.521(10) 2_856 ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? 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 N2 172.3(2) . . ? O1 Cl1 O3 109.7(5) . . ? O1 Cl1 O2 109.6(6) . . ? O3 Cl1 O2 112.8(4) . . ? O1 Cl1 O4 101.7(7) . . ? O3 Cl1 O4 113.3(6) . . ? O2 Cl1 O4 109.2(5) . . ? C5 S1 C6 104.5(3) . . ? C12 S2 C13 105.2(3) . . ? C5 N1 C1 117.2(4) . . ? C5 N1 Ag1 121.0(3) . . ? C1 N1 Ag1 121.5(4) . . ? C12 N2 C8 118.7(5) . . ? C12 N2 Ag1 122.6(3) . . ? C8 N2 Ag1 118.2(4) . . ? N1 C1 C2 123.6(5) . . ? N1 C1 H1A 118.2 . . ? C2 C1 H1A 118.2 . . ? C3 C2 C1 118.4(5) . . ? C3 C2 H2A 120.8 . . ? C1 C2 H2A 120.8 . . ? C2 C3 C4 120.4(5) . . ? C2 C3 H3A 119.8 . . ? C4 C3 H3A 119.8 . . ? C5 C4 C3 117.6(5) . . ? C5 C4 H4A 121.2 . . ? C3 C4 H4A 121.2 . . ? N1 C5 C4 122.8(5) . . ? N1 C5 S1 112.0(4) . . ? C4 C5 S1 125.1(4) . . ? C7 C6 C7' 37.0(6) . . ? C7 C6 S1 108.3(6) . . ? C7' C6 S1 107.2(7) . . ? C7 C6 H6A 125.0 . . ? C7' C6 H6A 124.1 . . ? S1 C6 H6A 124.4 . . ? C7 C7 C6 115.7(15) 2_857 . ? C7 C7 H7A 108.4 2_857 . ? C6 C7 H7A 108.4 . . ? C7 C7 H7B 108.4 2_857 . ? C6 C7 H7B 108.4 . . ? H7A C7 H7B 107.4 . . ? C7' C7' C6 106.6(13) 2_857 . ? C7' C7' H7'A 110.4 2_857 . ? C6 C7' H7'A 110.4 . . ? C7' C7' H7'B 110.4 2_857 . ? C6 C7' H7'B 110.4 . . ? H7'A C7' H7'B 108.6 . . ? N2 C8 C9 122.1(6) . . ? N2 C8 H8A 119.0 . . ? C9 C8 H8A 119.0 . . ? C8 C9 C10 119.4(6) . . ? C8 C9 H9A 120.3 . . ? C10 C9 H9A 120.3 . . ? C11 C10 C9 118.7(6) . . ? C11 C10 H10A 120.6 . . ? C9 C10 H10A 120.6 . . ? C10 C11 C12 119.8(6) . . ? C10 C11 H11A 120.1 . . ? C12 C11 H11A 120.1 . . ? N2 C12 C11 121.3(5) . . ? N2 C12 S2 112.8(4) . . ? C11 C12 S2 125.9(4) . . ? C14 C13 S2 114.1(4) . . ? C14 C13 H13A 108.7 . . ? S2 C13 H13A 108.7 . . ? C14 C13 H13B 108.7 . . ? S2 C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? C13 C14 C14 111.4(5) . 2_856 ? C13 C14 H14A 109.3 . . ? C14 C14 H14A 109.3 2_856 . ? C13 C14 H14B 109.3 . . ? C14 C14 H14B 109.3 2_856 . ? H14A C14 H14B 108.0 . . ? 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 N2 Ag1 N1 C5 -21.9(13) . . . . ? N2 Ag1 N1 C1 151.4(10) . . . . ? N1 Ag1 N2 C12 14.6(14) . . . . ? N1 Ag1 N2 C8 -173.6(10) . . . . ? C5 N1 C1 C2 2.5(8) . . . . ? Ag1 N1 C1 C2 -171.1(5) . . . . ? N1 C1 C2 C3 -0.3(9) . . . . ? C1 C2 C3 C4 -1.0(9) . . . . ? C2 C3 C4 C5 -0.1(8) . . . . ? C1 N1 C5 C4 -3.6(7) . . . . ? Ag1 N1 C5 C4 170.0(4) . . . . ? C1 N1 C5 S1 173.4(4) . . . . ? Ag1 N1 C5 S1 -13.0(5) . . . . ? C3 C4 C5 N1 2.4(8) . . . . ? C3 C4 C5 S1 -174.2(4) . . . . ? C6 S1 C5 N1 169.1(4) . . . . ? C6 S1 C5 C4 -13.9(6) . . . . ? C5 S1 C6 C7 -155.5(7) . . . . ? C5 S1 C6 C7' 165.5(6) . . . . ? C7' C6 C7 C7 30.6(13) . . . 2_857 ? S1 C6 C7 C7 -63.9(18) . . . 2_857 ? C7 C6 C7' C7' -25.1(10) . . . 2_857 ? S1 C6 C7' C7' 72.8(17) . . . 2_857 ? C12 N2 C8 C9 0.1(8) . . . . ? Ag1 N2 C8 C9 -172.1(5) . . . . ? N2 C8 C9 C10 -0.1(10) . . . . ? C8 C9 C10 C11 0.0(10) . . . . ? C9 C10 C11 C12 0.1(9) . . . . ? C8 N2 C12 C11 0.0(8) . . . . ? Ag1 N2 C12 C11 171.8(4) . . . . ? C8 N2 C12 S2 -179.6(4) . . . . ? Ag1 N2 C12 S2 -7.8(5) . . . . ? C10 C11 C12 N2 0.0(9) . . . . ? C10 C11 C12 S2 179.4(5) . . . . ? C13 S2 C12 N2 -163.5(4) . . . . ? C13 S2 C12 C11 17.0(6) . . . . ? C12 S2 C13 C14 72.0(5) . . . . ? S2 C13 C14 C14 172.8(5) . . . 2_856 ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.650 _refine_diff_density_min -0.515 _refine_diff_density_rms 0.096 data_021218f _database_code_depnum_ccdc_archive 'CCDC 223561' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H19 Ag F6 N3 P S2' _chemical_formula_weight 570.30 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' 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' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.856(3) _cell_length_b 10.821(3) _cell_length_c 12.864(4) _cell_angle_alpha 66.487(5) _cell_angle_beta 78.556(5) _cell_angle_gamma 82.009(6) _cell_volume 1105.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 940 _cell_measurement_theta_min 2.70 _cell_measurement_theta_max 19.23 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas None _exptl_crystal_density_diffrn 1.713 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 568 _exptl_absorpt_coefficient_mu 1.230 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.727381 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 6445 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_sigmaI/netI 0.1480 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 26.43 _reflns_number_total 4501 _reflns_number_gt 1862 _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^)+(0.0524P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4501 _refine_ls_number_parameters 328 _refine_ls_number_restraints 330 _refine_ls_R_factor_all 0.1859 _refine_ls_R_factor_gt 0.0644 _refine_ls_wR_factor_ref 0.1502 _refine_ls_wR_factor_gt 0.1153 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 1.031 _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 0.26320(8) 1.00321(7) 0.44280(5) 0.0759(3) Uani 1 1 d . A . S1 S 0.0199(3) 0.7703(3) 0.5415(2) 0.0917(9) Uani 1 1 d . . . S2 S 0.4593(2) 1.1906(2) 0.49366(16) 0.0592(6) Uani 1 1 d . . . N1 N 0.1400(8) 0.9057(7) 0.6254(6) 0.0671(19) Uani 1 1 d . . . N2 N 0.4067(7) 1.1737(6) 0.3101(5) 0.0581(17) Uani 1 1 d . . . N3 N 0.2399(9) 0.9336(9) 0.2876(7) 0.093(3) Uani 1 1 d . . . C1 C 0.1653(10) 0.9449(9) 0.7051(8) 0.074(3) Uani 1 1 d . A . H1 H 0.2203 1.0210 0.6826 0.089 Uiso 1 1 calc R . . C2 C 0.1141(11) 0.8784(11) 0.8189(9) 0.089(3) Uani 1 1 d . . . H2 H 0.1360 0.9072 0.8731 0.106 Uiso 1 1 calc R A . C3 C 0.0300(11) 0.7688(11) 0.8520(8) 0.087(3) Uani 1 1 d . A . H3 H -0.0076 0.7228 0.9292 0.104 Uiso 1 1 calc R . . C4 C 0.0012(10) 0.7270(10) 0.7706(8) 0.080(3) Uani 1 1 d . . . H4 H -0.0537 0.6511 0.7920 0.096 Uiso 1 1 calc R A . C5 C 0.0550(9) 0.7992(9) 0.6570(7) 0.067(2) Uani 1 1 d . A . C6 C -0.0347(12) 0.6012(10) 0.5989(9) 0.097(3) Uani 0.56(4) 1 d PU A 1 H6A H 0.0242 0.5416 0.6582 0.116 Uiso 0.56(4) 1 calc PR A 1 H6B H -0.1443 0.5945 0.6276 0.116 Uiso 0.56(4) 1 calc PR A 1 C7 C 0.014(3) 0.576(2) 0.4821(17) 0.058(7) Uani 0.56(4) 1 d PU . 1 H7A H -0.0503 0.6334 0.4255 0.070 Uiso 0.56(4) 1 calc PR A 1 H7B H 0.1210 0.5931 0.4505 0.070 Uiso 0.56(4) 1 calc PR A 1 C6' C -0.0347(12) 0.6012(10) 0.5989(9) 0.097(3) Uani 0.44(4) 1 d PU A 2 H6'A H 0.0462 0.5459 0.6410 0.116 Uiso 0.44(4) 1 calc PR A 2 H6'B H -0.1266 0.5971 0.6552 0.116 Uiso 0.44(4) 1 calc PR A 2 C7' C -0.069(4) 0.528(4) 0.523(3) 0.070(8) Uani 0.44(4) 1 d PU . 2 H7'A H -0.1370 0.4560 0.5698 0.084 Uiso 0.44(4) 1 calc PR A 2 H7'B H -0.1207 0.5914 0.4613 0.084 Uiso 0.44(4) 1 calc PR A 2 C8 C 0.4571(8) 1.4506(7) 0.4913(6) 0.054(2) Uani 1 1 d . . . H8A H 0.4390 1.4860 0.4123 0.064 Uiso 1 1 calc R . . H8B H 0.3575 1.4396 0.5406 0.064 Uiso 1 1 calc R . . C9 C 0.5462(9) 1.3152(7) 0.5179(6) 0.059(2) Uani 1 1 d . . . H9A H 0.5602 1.2797 0.5978 0.071 Uiso 1 1 calc R . . H9B H 0.6478 1.3286 0.4716 0.071 Uiso 1 1 calc R . . C10 C 0.4859(9) 1.2452(8) 0.3438(6) 0.053(2) Uani 1 1 d . A . C11 C 0.5717(9) 1.3487(8) 0.2667(7) 0.067(2) Uani 1 1 d . . . H11 H 0.6233 1.3978 0.2923 0.080 Uiso 1 1 calc R A . C12 C 0.5813(10) 1.3796(9) 0.1520(8) 0.077(3) Uani 1 1 d . A . H12 H 0.6404 1.4493 0.0991 0.092 Uiso 1 1 calc R . . C13 C 0.5045(11) 1.3087(10) 0.1152(7) 0.080(3) Uani 1 1 d . . . H13 H 0.5100 1.3284 0.0373 0.096 Uiso 1 1 calc R A . C14 C 0.4190(10) 1.2075(9) 0.1959(7) 0.071(2) Uani 1 1 d . A . H14 H 0.3660 1.1590 0.1708 0.085 Uiso 1 1 calc R . . C15 C 0.2357(10) 0.8936(9) 0.2213(8) 0.074(3) Uani 1 1 d . A . C16 C 0.2363(12) 0.8418(11) 0.1318(8) 0.113(4) Uani 1 1 d . . . H16A H 0.2945 0.8983 0.0612 0.169 Uiso 1 1 calc R A . H16B H 0.1321 0.8421 0.1207 0.169 Uiso 1 1 calc R . . H16C H 0.2826 0.7513 0.1547 0.169 Uiso 1 1 calc R . . P1 P 0.2665(3) 0.2445(3) 0.84854(19) 0.0825(8) Uani 1 1 d D . . F1 F 0.3978(16) 0.3383(14) 0.7757(11) 0.135(5) Uani 0.643(12) 1 d PDU B 1 F2 F 0.1390(11) 0.1415(11) 0.9267(8) 0.096(4) Uani 0.643(12) 1 d PDU B 1 F3 F 0.1578(15) 0.3656(11) 0.8596(13) 0.168(5) Uani 0.643(12) 1 d PDU B 1 F4 F 0.1953(14) 0.2642(14) 0.7386(7) 0.140(5) Uani 0.643(12) 1 d PDU B 1 F5 F 0.3665(11) 0.1183(10) 0.8317(11) 0.129(4) Uani 0.643(12) 1 d PDU B 1 F6 F 0.3269(13) 0.2061(15) 0.9628(7) 0.134(5) Uani 0.643(12) 1 d PDU B 1 F1' F 0.4424(13) 0.2906(18) 0.8043(14) 0.096(8) Uani 0.357(12) 1 d PDU B 2 F2' F 0.1009(15) 0.208(2) 0.8896(15) 0.129(9) Uani 0.357(12) 1 d PDU B 2 F3' F 0.2534(18) 0.3179(18) 0.9338(12) 0.095(6) Uani 0.357(12) 1 d PDU B 2 F4' F 0.2225(19) 0.3851(13) 0.7546(13) 0.122(8) Uani 0.357(12) 1 d PDU B 2 F5' F 0.291(2) 0.1823(19) 0.7578(15) 0.139(9) Uani 0.357(12) 1 d PDU B 2 F6' F 0.333(2) 0.1152(17) 0.9370(18) 0.238(15) Uani 0.357(12) 1 d PDU 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 0.0848(5) 0.0809(5) 0.0572(4) -0.0172(4) -0.0063(3) -0.0260(4) S1 0.0749(17) 0.130(2) 0.0715(16) -0.0333(16) -0.0113(13) -0.0270(17) S2 0.0782(15) 0.0571(13) 0.0448(11) -0.0214(10) -0.0046(10) -0.0132(12) N1 0.066(5) 0.074(5) 0.059(4) -0.027(4) -0.003(4) -0.001(4) N2 0.068(4) 0.072(5) 0.037(4) -0.022(3) -0.010(3) -0.009(4) N3 0.106(6) 0.110(7) 0.069(5) -0.031(5) -0.017(5) -0.029(5) C1 0.085(7) 0.071(6) 0.066(6) -0.030(6) 0.001(5) -0.007(5) C2 0.094(8) 0.097(8) 0.079(8) -0.044(7) -0.009(6) 0.002(7) C3 0.092(7) 0.099(8) 0.051(6) -0.025(6) 0.015(5) 0.003(7) C4 0.071(6) 0.104(8) 0.062(6) -0.030(6) 0.008(5) -0.026(6) C5 0.051(5) 0.078(7) 0.070(6) -0.031(5) -0.001(5) -0.003(5) C6 0.105(7) 0.092(7) 0.105(7) -0.044(6) -0.051(6) 0.022(6) C7 0.064(13) 0.034(13) 0.070(11) 0.000(8) -0.031(9) -0.010(10) C6' 0.105(7) 0.092(7) 0.105(7) -0.044(6) -0.051(6) 0.022(6) C7' 0.062(15) 0.060(17) 0.091(15) -0.026(12) -0.032(12) 0.002(13) C8 0.066(5) 0.044(5) 0.051(4) -0.023(4) 0.001(4) -0.002(4) C9 0.085(6) 0.050(5) 0.046(5) -0.019(4) -0.013(4) -0.010(5) C10 0.060(5) 0.049(5) 0.048(5) -0.016(4) -0.011(4) 0.002(4) C11 0.079(6) 0.062(6) 0.056(6) -0.018(5) -0.003(5) -0.018(5) C12 0.088(7) 0.075(6) 0.056(6) -0.017(5) 0.007(5) -0.020(5) C13 0.093(7) 0.095(8) 0.044(5) -0.021(6) -0.002(5) -0.011(6) C14 0.080(6) 0.080(7) 0.057(6) -0.028(5) -0.011(5) -0.010(5) C15 0.083(7) 0.082(7) 0.064(6) -0.028(6) -0.022(5) -0.016(5) C16 0.134(9) 0.122(9) 0.098(8) -0.047(7) -0.041(7) -0.011(8) P1 0.099(2) 0.094(2) 0.0496(15) -0.0212(15) -0.0008(14) -0.0277(19) F1 0.152(9) 0.105(8) 0.122(8) -0.028(6) 0.028(7) -0.041(7) F2 0.092(6) 0.087(6) 0.088(6) -0.011(5) 0.004(5) -0.028(5) F3 0.186(9) 0.121(7) 0.157(9) -0.044(6) 0.005(7) 0.051(7) F4 0.168(8) 0.162(9) 0.089(6) -0.033(6) -0.062(6) 0.012(7) F5 0.116(7) 0.122(7) 0.152(8) -0.076(6) 0.006(6) 0.017(6) F6 0.159(8) 0.175(9) 0.082(6) -0.042(6) -0.051(5) -0.038(7) F1' 0.060(9) 0.100(11) 0.103(11) -0.014(8) -0.023(7) 0.010(7) F2' 0.108(12) 0.153(14) 0.135(13) -0.052(9) -0.028(8) -0.036(9) F3' 0.099(10) 0.108(10) 0.091(9) -0.055(8) 0.005(7) -0.030(8) F4' 0.124(11) 0.124(11) 0.108(10) -0.033(8) -0.041(8) 0.019(8) F5' 0.167(13) 0.135(12) 0.138(12) -0.085(9) -0.002(9) -0.009(9) F6' 0.254(18) 0.222(17) 0.225(17) -0.072(11) -0.042(10) -0.010(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 2.269(6) . ? Ag1 N2 2.283(6) . ? Ag1 N3 2.450(9) . ? S1 C5 1.727(9) . ? S1 C6 1.776(10) . ? S2 C10 1.753(7) . ? S2 C9 1.796(7) . ? N1 C1 1.322(10) . ? N1 C5 1.344(9) . ? N2 C10 1.348(9) . ? N2 C14 1.349(9) . ? N3 C15 1.108(9) . ? C1 C2 1.361(11) . ? C1 H1 0.9300 . ? C2 C3 1.364(12) . ? C2 H2 0.9300 . ? C3 C4 1.371(12) . ? C3 H3 0.9300 . ? C4 C5 1.375(11) . ? C4 H4 0.9300 . ? C6 C7 1.60(2) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C7 1.56(5) 2_566 ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7' C7' 1.41(7) 2_566 ? C7' H7'A 0.9700 . ? C7' H7'B 0.9700 . ? C8 C8 1.502(13) 2_686 ? C8 C9 1.508(9) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.367(9) . ? C11 C12 1.364(10) . ? C11 H11 0.9300 . ? C12 C13 1.356(11) . ? C12 H12 0.9300 . ? C13 C14 1.365(10) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C16 1.467(12) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? P1 F2' 1.508(11) . ? P1 F5' 1.532(11) . ? P1 F6' 1.537(12) . ? P1 F6 1.543(8) . ? P1 F1 1.549(9) . ? P1 F3 1.552(9) . ? P1 F3' 1.570(10) . ? P1 F4' 1.576(11) . ? P1 F4 1.587(8) . ? P1 F5 1.587(9) . ? P1 F2 1.592(7) . ? P1 F1' 1.624(11) . ? 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 N2 148.2(3) . . ? N1 Ag1 N3 123.3(3) . . ? N2 Ag1 N3 88.1(2) . . ? C5 S1 C6 105.4(5) . . ? C10 S2 C9 104.0(4) . . ? C1 N1 C5 119.0(7) . . ? C1 N1 Ag1 119.3(6) . . ? C5 N1 Ag1 121.4(6) . . ? C10 N2 C14 116.6(7) . . ? C10 N2 Ag1 120.4(5) . . ? C14 N2 Ag1 123.0(5) . . ? C15 N3 Ag1 174.8(9) . . ? N1 C1 C2 122.7(9) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C1 C2 C3 118.8(9) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C2 C3 C4 119.5(9) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C4 C5 118.9(9) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 C4 121.1(8) . . ? N1 C5 S1 112.9(6) . . ? C4 C5 S1 126.0(8) . . ? C7 C6 S1 96.4(11) . . ? C7 C6 H6A 112.5 . . ? S1 C6 H6A 112.5 . . ? C7 C6 H6B 112.5 . . ? S1 C6 H6B 112.5 . . ? H6A C6 H6B 110.0 . . ? C7 C7 C6 104(2) 2_566 . ? C7 C7 H7A 110.9 2_566 . ? C6 C7 H7A 110.9 . . ? C7 C7 H7B 110.9 2_566 . ? C6 C7 H7B 110.9 . . ? H7A C7 H7B 108.9 . . ? C7' C7' H7'A 109.4 2_566 . ? C7' C7' H7'B 109.4 2_566 . ? H7'A C7' H7'B 108.0 . . ? C8 C8 C9 111.4(8) 2_686 . ? C8 C8 H8A 109.3 2_686 . ? C9 C8 H8A 109.3 . . ? C8 C8 H8B 109.3 2_686 . ? C9 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? C8 C9 S2 115.6(5) . . ? C8 C9 H9A 108.4 . . ? S2 C9 H9A 108.4 . . ? C8 C9 H9B 108.4 . . ? S2 C9 H9B 108.4 . . ? H9A C9 H9B 107.5 . . ? N2 C10 C11 122.0(7) . . ? N2 C10 S2 111.7(6) . . ? C11 C10 S2 126.3(6) . . ? C12 C11 C10 119.5(8) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C13 C12 C11 120.0(8) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 118.0(8) . . ? C12 C13 H13 121.0 . . ? C14 C13 H13 121.0 . . ? N2 C14 C13 123.9(8) . . ? N2 C14 H14 118.1 . . ? C13 C14 H14 118.1 . . ? N3 C15 C16 177.8(10) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? F2' P1 F5' 93.6(7) . . ? F2' P1 F6' 94.9(7) . . ? F5' P1 F6' 92.3(8) . . ? F2' P1 F6 101.9(8) . . ? F5' P1 F6 134.0(9) . . ? F6' P1 F6 43.8(8) . . ? F2' P1 F1 154.9(9) . . ? F5' P1 F1 88.6(9) . . ? F6' P1 F1 110.0(9) . . ? F6 P1 F1 94.3(7) . . ? F2' P1 F3 68.2(8) . . ? F5' P1 F3 130.7(9) . . ? F6' P1 F3 133.0(9) . . ? F6 P1 F3 95.2(7) . . ? F1 P1 F3 91.6(7) . . ? F2' P1 F3' 91.3(7) . . ? F5' P1 F3' 174.4(7) . . ? F6' P1 F3' 89.8(7) . . ? F6 P1 F3' 47.0(6) . . ? F1 P1 F3' 85.8(7) . . ? F3 P1 F3' 49.4(7) . . ? F2' P1 F4' 93.2(7) . . ? F5' P1 F4' 89.1(7) . . ? F6' P1 F4' 171.7(9) . . ? F6 P1 F4' 132.1(7) . . ? F1 P1 F4' 61.9(7) . . ? F3 P1 F4' 49.2(6) . . ? F3' P1 F4' 88.0(7) . . ? F2' P1 F4 73.0(8) . . ? F5' P1 F4 42.3(8) . . ? F6' P1 F4 129.7(9) . . ? F6 P1 F4 172.2(7) . . ? F1 P1 F4 92.5(7) . . ? F3 P1 F4 88.4(7) . . ? F3' P1 F4 137.6(8) . . ? F4' P1 F4 55.0(6) . . ? F2' P1 F5 108.1(8) . . ? F5' P1 F5 45.0(8) . . ? F6' P1 F5 49.8(8) . . ? F6 P1 F5 89.0(7) . . ? F1 P1 F5 91.0(7) . . ? F3 P1 F5 174.8(7) . . ? F3' P1 F5 135.4(8) . . ? F4' P1 F5 128.9(7) . . ? F4 P1 F5 87.0(6) . . ? F2' P1 F2 28.4(7) . . ? F5' P1 F2 91.1(8) . . ? F6' P1 F2 66.7(8) . . ? F6 P1 F2 83.5(6) . . ? F1 P1 F2 176.7(7) . . ? F3 P1 F2 91.1(6) . . ? F3' P1 F2 94.5(6) . . ? F4' P1 F2 121.4(7) . . ? F4 P1 F2 89.5(6) . . ? F5 P1 F2 86.5(6) . . ? F2' P1 F1' 177.3(8) . . ? F5' P1 F1' 88.3(7) . . ? F6' P1 F1' 86.9(7) . . ? F6 P1 F1' 78.1(8) . . ? F1 P1 F1' 23.1(8) . . ? F3 P1 F1' 109.2(8) . . ? F3' P1 F1' 86.8(6) . . ? F4' P1 F1' 84.9(6) . . ? F4 P1 F1' 107.3(7) . . ? F5 P1 F1' 74.5(8) . . ? F2 P1 F1' 153.6(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ag1 N1 C1 -12.8(9) . . . . ? N3 Ag1 N1 C1 176.6(6) . . . . ? N2 Ag1 N1 C5 174.4(5) . . . . ? N3 Ag1 N1 C5 3.8(7) . . . . ? N1 Ag1 N2 C10 19.7(8) . . . . ? N3 Ag1 N2 C10 -168.1(6) . . . . ? N1 Ag1 N2 C14 -161.0(6) . . . . ? N3 Ag1 N2 C14 11.2(6) . . . . ? N1 Ag1 N3 C15 -71(9) . . . . ? N2 Ag1 N3 C15 114(9) . . . . ? C5 N1 C1 C2 2.8(13) . . . . ? Ag1 N1 C1 C2 -170.2(7) . . . . ? N1 C1 C2 C3 -1.7(14) . . . . ? C1 C2 C3 C4 1.0(14) . . . . ? C2 C3 C4 C5 -1.6(14) . . . . ? C1 N1 C5 C4 -3.4(12) . . . . ? Ag1 N1 C5 C4 169.4(6) . . . . ? C1 N1 C5 S1 175.0(6) . . . . ? Ag1 N1 C5 S1 -12.2(8) . . . . ? C3 C4 C5 N1 2.8(13) . . . . ? C3 C4 C5 S1 -175.3(7) . . . . ? C6 S1 C5 N1 161.4(6) . . . . ? C6 S1 C5 C4 -20.3(9) . . . . ? C5 S1 C6 C7 -155.8(10) . . . . ? S1 C6 C7 C7 175(2) . . . 2_566 ? C8 C8 C9 S2 -177.2(6) 2_686 . . . ? C10 S2 C9 C8 73.0(6) . . . . ? C14 N2 C10 C11 1.4(11) . . . . ? Ag1 N2 C10 C11 -179.3(6) . . . . ? C14 N2 C10 S2 179.9(6) . . . . ? Ag1 N2 C10 S2 -0.8(7) . . . . ? C9 S2 C10 N2 -170.7(5) . . . . ? C9 S2 C10 C11 7.8(8) . . . . ? N2 C10 C11 C12 -1.5(12) . . . . ? S2 C10 C11 C12 -179.9(7) . . . . ? C10 C11 C12 C13 0.7(13) . . . . ? C11 C12 C13 C14 0.1(14) . . . . ? C10 N2 C14 C13 -0.5(12) . . . . ? Ag1 N2 C14 C13 -179.8(6) . . . . ? C12 C13 C14 N2 -0.2(13) . . . . ? Ag1 N3 C15 C16 -74(31) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.43 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.481 _refine_diff_density_min -0.362 _refine_diff_density_rms 0.080 data_020912e _database_code_depnum_ccdc_archive 'CCDC 223562' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H19 Ag B Cl3 F4 N2 S2' _chemical_formula_weight 604.48 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 15.725(10) _cell_length_b 16.132(10) _cell_length_c 18.870(12) _cell_angle_alpha 90.00 _cell_angle_beta 97.024(17) _cell_angle_gamma 90.00 _cell_volume 4751(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 753 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 22.23 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.690 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2400 _exptl_absorpt_coefficient_mu 1.399 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6790 _exptl_absorpt_correction_T_max 0.7673 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 8950 _diffrn_reflns_av_R_equivalents 0.0893 _diffrn_reflns_av_sigmaI/netI 0.1295 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4007 _reflns_number_gt 1714 _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^)+(0.0438P)^2^+36.9377P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4007 _refine_ls_number_parameters 299 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1929 _refine_ls_R_factor_gt 0.0750 _refine_ls_wR_factor_ref 0.1730 _refine_ls_wR_factor_gt 0.1314 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 0.81212(6) 0.19840(6) 0.42321(4) 0.0745(4) Uani 1 1 d . . . B1 B 0.7527(9) 0.6916(8) 0.2933(7) 0.100(6) Uani 1 1 d D . . C1 C 0.7995(8) 0.3761(7) 0.3624(6) 0.079(4) Uani 1 1 d . . . H1 H 0.7778 0.3466 0.3218 0.095 Uiso 1 1 calc R . . C2 C 0.8059(9) 0.4585(7) 0.3553(6) 0.083(4) Uani 1 1 d . . . H2 H 0.7937 0.4846 0.3113 0.100 Uiso 1 1 calc R . . C3 C 0.8319(8) 0.5028(6) 0.4177(7) 0.079(4) Uani 1 1 d . . . H3 H 0.8330 0.5604 0.4171 0.095 Uiso 1 1 calc R . . C4 C 0.8560(8) 0.4603(6) 0.4804(5) 0.069(4) Uani 1 1 d . . . H4 H 0.8769 0.4883 0.5219 0.083 Uiso 1 1 calc R . . C5 C 0.8486(5) 0.3782(6) 0.4798(5) 0.042(2) Uani 1 1 d . . . C6 C 0.9273(7) 0.3805(6) 0.6246(5) 0.064(3) Uani 1 1 d . . . H6A H 0.9729 0.4108 0.6058 0.077 Uiso 1 1 calc R . . H6B H 0.8868 0.4203 0.6394 0.077 Uiso 1 1 calc R . . C7 C 0.9636(7) 0.3297(6) 0.6871(5) 0.061(3) Uani 1 1 d . . . H7A H 1.0085 0.2944 0.6731 0.073 Uiso 1 1 calc R . . H7B H 0.9190 0.2943 0.7017 0.073 Uiso 1 1 calc R . . C8 C 1.0000 0.3833(9) 0.7500 0.066(4) Uani 1 2 d S . . H8A H 0.9552 0.4186 0.7643 0.079 Uiso 0.50 1 calc PR . . H8B H 1.0448 0.4186 0.7357 0.079 Uiso 0.50 1 calc PR . . C9 C 0.7965(8) 0.0207(7) 0.3627(7) 0.073(4) Uani 1 1 d . . . H9 H 0.7754 0.0496 0.3216 0.088 Uiso 1 1 calc R . . C10 C 0.7942(9) -0.0638(7) 0.3611(8) 0.092(4) Uani 1 1 d . . . H10 H 0.7691 -0.0910 0.3203 0.110 Uiso 1 1 calc R . . C11 C 0.8284(10) -0.1089(8) 0.4189(7) 0.104(5) Uani 1 1 d . . . H11 H 0.8296 -0.1665 0.4176 0.124 Uiso 1 1 calc R . . C12 C 0.8605(8) -0.0664(6) 0.4785(7) 0.076(4) Uani 1 1 d . . . H12 H 0.8835 -0.0949 0.5193 0.091 Uiso 1 1 calc R . . C13 C 0.8590(7) 0.0221(7) 0.4784(6) 0.064(3) Uani 1 1 d . . . C14 C 0.9358(8) 0.0129(7) 0.6196(5) 0.076(4) Uani 1 1 d . . . H14A H 0.8894 -0.0233 0.6293 0.091 Uiso 1 1 calc R . . H14B H 0.9823 -0.0208 0.6060 0.091 Uiso 1 1 calc R . . C15 C 0.9666(9) 0.0651(7) 0.6855(6) 0.085(4) Uani 1 1 d . . . H15A H 0.9196 0.0991 0.6976 0.102 Uiso 1 1 calc R . . H15B H 1.0120 0.1019 0.6743 0.102 Uiso 1 1 calc R . . C16 C 1.0000 0.0116(9) 0.7500 0.066(4) Uani 1 2 d S . . H16A H 0.9542 -0.0238 0.7624 0.080 Uiso 0.50 1 calc PR . . H16B H 1.0458 -0.0238 0.7376 0.080 Uiso 0.50 1 calc PR . . C17 C 0.9285(9) 0.7051(9) 0.6206(8) 0.118(5) Uani 1 1 d . . . H17 H 0.8765 0.7199 0.6414 0.141 Uiso 1 1 calc R . . Cl1 Cl 0.9608(3) 0.6099(3) 0.6499(3) 0.169(2) Uani 1 1 d . . . Cl2 Cl 1.0049(3) 0.7802(3) 0.6430(5) 0.234(4) Uani 1 1 d . . . Cl3 Cl 0.9051(5) 0.7041(4) 0.5277(3) 0.236(3) Uani 1 1 d . . . F1 F 0.6891(10) 0.6361(8) 0.3068(13) 0.114(6) Uani 0.50 1 d PD . . F2 F 0.7160(14) 0.7704(8) 0.2942(10) 0.104(5) Uani 0.50 1 d PD . . F3 F 0.8284(9) 0.6851(13) 0.3389(10) 0.122(6) Uani 0.50 1 d PD . . F4 F 0.7664(15) 0.6844(14) 0.2220(8) 0.136(9) Uani 0.50 1 d PD . . N1 N 0.8213(6) 0.3319(4) 0.4220(5) 0.053(2) Uani 1 1 d . . . N2 N 0.8272(6) 0.0637(4) 0.4199(5) 0.052(2) Uani 1 1 d . . . S1 S 0.87418(18) 0.31403(16) 0.55624(14) 0.0614(8) Uani 1 1 d . . . S2 S 0.8995(2) 0.08579(18) 0.54928(16) 0.0806(10) Uani 1 1 d . . . F1' F 0.8033(11) 0.6271(8) 0.2769(10) 0.097(5) Uani 0.50 1 d P . . F2' F 0.738(2) 0.6893(19) 0.3571(10) 0.180(10) Uani 0.50 1 d P . . F3' F 0.806(3) 0.7619(13) 0.2835(16) 0.221(13) Uani 0.50 1 d P . . F4' F 0.695(2) 0.701(2) 0.2439(16) 0.216(13) Uani 0.50 1 d P . . 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 0.1126(8) 0.0460(5) 0.0622(5) 0.0065(5) 0.0003(5) 0.0026(6) B1 0.150(19) 0.057(12) 0.094(15) 0.022(11) 0.019(14) 0.048(15) C1 0.113(10) 0.053(8) 0.058(7) 0.027(6) -0.039(7) -0.004(7) C2 0.154(13) 0.047(8) 0.040(7) 0.023(6) -0.017(7) 0.002(8) C3 0.126(11) 0.011(5) 0.098(10) 0.015(6) 0.009(9) 0.024(6) C4 0.121(10) 0.030(6) 0.049(7) 0.028(5) -0.020(7) 0.010(6) C5 0.037(6) 0.020(5) 0.065(7) 0.001(5) -0.008(5) 0.000(4) C6 0.073(8) 0.044(7) 0.073(8) 0.008(6) -0.003(6) 0.022(6) C7 0.059(7) 0.050(7) 0.068(8) 0.007(6) -0.014(6) 0.007(6) C8 0.072(11) 0.042(10) 0.077(11) 0.000 -0.014(9) 0.000 C9 0.103(10) 0.049(8) 0.069(9) 0.025(7) 0.012(8) 0.018(7) C10 0.123(12) 0.035(7) 0.114(12) -0.003(7) -0.001(9) 0.013(7) C11 0.165(14) 0.059(9) 0.079(10) -0.002(9) -0.017(10) 0.012(10) C12 0.101(10) 0.032(7) 0.088(10) 0.008(6) -0.011(8) 0.020(6) C13 0.078(8) 0.043(7) 0.072(8) 0.006(6) 0.013(7) 0.011(6) C14 0.114(10) 0.060(8) 0.047(7) 0.017(6) -0.020(7) 0.024(7) C15 0.123(11) 0.043(8) 0.085(10) 0.005(7) -0.008(8) 0.008(7) C16 0.080(12) 0.051(10) 0.063(11) 0.000 -0.013(9) 0.000 C17 0.111(11) 0.087(10) 0.163(15) 0.028(11) 0.048(10) 0.003(10) Cl1 0.195(5) 0.079(3) 0.214(5) 0.030(3) -0.046(4) 0.002(3) Cl2 0.146(4) 0.088(4) 0.494(12) -0.044(5) 0.141(6) -0.021(3) Cl3 0.410(10) 0.144(5) 0.168(5) 0.047(4) 0.094(6) 0.074(6) F1 0.139(15) 0.041(9) 0.165(18) 0.036(10) 0.036(14) -0.029(9) F2 0.151(15) 0.057(10) 0.111(13) -0.007(9) 0.039(12) 0.019(10) F3 0.078(11) 0.142(17) 0.141(15) 0.056(15) -0.005(11) 0.005(12) F4 0.149(16) 0.17(2) 0.099(14) -0.101(15) 0.056(13) -0.051(16) N1 0.083(6) 0.017(4) 0.056(5) 0.010(4) -0.004(5) 0.014(4) N2 0.082(7) 0.020(4) 0.052(5) 0.000(4) 0.002(5) 0.014(4) S1 0.087(2) 0.0318(17) 0.0628(17) 0.0117(13) -0.0028(15) 0.0034(15) S2 0.117(3) 0.0392(18) 0.076(2) 0.0060(15) -0.0264(19) 0.0103(18) F1' 0.145(15) 0.052(10) 0.092(11) 0.001(9) 0.003(11) 0.023(9) F2' 0.24(3) 0.22(3) 0.084(13) 0.016(17) 0.037(15) 0.11(2) F3' 0.37(4) 0.065(15) 0.23(3) -0.019(16) 0.07(3) 0.04(2) F4' 0.24(3) 0.26(4) 0.14(2) 0.07(3) -0.01(2) 0.09(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.158(7) . ? Ag1 N2 2.187(7) . ? B1 F4' 1.22(3) . ? B1 F2' 1.25(2) . ? B1 F1' 1.369(19) . ? B1 F3 1.385(9) . ? B1 F1 1.389(9) . ? B1 F4 1.393(9) . ? B1 F2 1.397(9) . ? B1 F3' 1.43(3) . ? C1 N1 1.340(11) . ? C1 C2 1.341(14) . ? C1 H1 0.9300 . ? C2 C3 1.396(15) . ? C2 H2 0.9300 . ? C3 C4 1.379(13) . ? C3 H3 0.9300 . ? C4 C5 1.329(12) . ? C4 H4 0.9300 . ? C5 N1 1.349(11) . ? C5 S1 1.781(9) . ? C6 C7 1.491(12) . ? C6 S1 1.801(10) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.523(12) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C7 1.523(12) 2_756 ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N2 1.324(13) . ? C9 C10 1.365(14) . ? C9 H9 0.9300 . ? C10 C11 1.366(16) . ? C10 H10 0.9300 . ? C11 C12 1.361(15) . ? C11 H11 0.9300 . ? C12 C13 1.428(13) . ? C12 H12 0.9300 . ? C13 N2 1.336(12) . ? C13 S2 1.743(11) . ? C14 C15 1.530(14) . ? C14 S2 1.813(10) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.532(13) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C15 1.532(13) 2_756 ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 Cl1 1.690(14) . ? C17 Cl2 1.722(15) . ? C17 Cl3 1.746(16) . ? C17 H17 0.9800 . ? F1 F2' 1.43(3) . ? F1 F4' 1.59(3) . ? F2 F3' 1.46(4) . ? F2 F4' 1.48(4) . ? F2 F2' 1.77(3) . ? F3 F2' 1.50(3) . ? F3 F1' 1.51(2) . ? F3 F3' 1.63(3) . ? F4 F4' 1.26(3) . ? F4 F1' 1.46(2) . ? F4 F3' 1.77(3) . ? 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 N2 169.4(3) . . ? F4' B1 F2' 122(2) . . ? F4' B1 F1' 108(2) . . ? F2' B1 F1' 111.9(16) . . ? F4' B1 F3 168(2) . . ? F2' B1 F3 69.1(15) . . ? F1' B1 F3 66.7(12) . . ? F4' B1 F1 74.6(19) . . ? F2' B1 F1 65.5(16) . . ? F1' B1 F1 90.1(13) . . ? F3 B1 F1 114.8(14) . . ? F4' B1 F4 57.4(15) . . ? F2' B1 F4 173(2) . . ? F1' B1 F4 63.6(13) . . ? F3 B1 F4 111.8(17) . . ? F1 B1 F4 108.9(16) . . ? F4' B1 F2 68.6(18) . . ? F2' B1 F2 83.9(14) . . ? F1' B1 F2 161.3(14) . . ? F3 B1 F2 112.8(17) . . ? F1 B1 F2 106.1(13) . . ? F4 B1 F2 101.5(14) . . ? F4' B1 F3' 101(2) . . ? F2' B1 F3' 109(2) . . ? F1' B1 F3' 102.1(16) . . ? F3 B1 F3' 70.8(16) . . ? F1 B1 F3' 167.8(16) . . ? F4 B1 F3' 77.3(15) . . ? F2 B1 F3' 61.9(13) . . ? N1 C1 C2 126.7(11) . . ? N1 C1 H1 116.7 . . ? C2 C1 H1 116.7 . . ? C1 C2 C3 116.1(10) . . ? C1 C2 H2 121.9 . . ? C3 C2 H2 121.9 . . ? C4 C3 C2 119.4(9) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C5 C4 C3 118.3(10) . . ? C5 C4 H4 120.9 . . ? C3 C4 H4 120.9 . . ? C4 C5 N1 125.3(9) . . ? C4 C5 S1 124.2(8) . . ? N1 C5 S1 110.5(6) . . ? C7 C6 S1 109.8(7) . . ? C7 C6 H6A 109.7 . . ? S1 C6 H6A 109.7 . . ? C7 C6 H6B 109.7 . . ? S1 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? C6 C7 C8 112.1(8) . . ? C6 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 . . ? C6 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C7 C8 C7 110.8(11) . 2_756 ? C7 C8 H8A 109.5 . . ? C7 C8 H8A 109.5 2_756 . ? C7 C8 H8B 109.5 . . ? C7 C8 H8B 109.5 2_756 . ? H8A C8 H8B 108.1 . . ? N2 C9 C10 123.2(11) . . ? N2 C9 H9 118.4 . . ? C10 C9 H9 118.4 . . ? C9 C10 C11 120.4(13) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C12 C11 C10 117.6(12) . . ? C12 C11 H11 121.2 . . ? C10 C11 H11 121.2 . . ? C11 C12 C13 119.9(11) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? N2 C13 C12 120.5(10) . . ? N2 C13 S2 113.7(8) . . ? C12 C13 S2 125.7(9) . . ? C15 C14 S2 106.2(7) . . ? C15 C14 H14A 110.5 . . ? S2 C14 H14A 110.5 . . ? C15 C14 H14B 110.5 . . ? S2 C14 H14B 110.5 . . ? H14A C14 H14B 108.7 . . ? C14 C15 C16 112.3(9) . . ? C14 C15 H15A 109.2 . . ? C16 C15 H15A 109.2 . . ? C14 C15 H15B 109.2 . . ? C16 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? C15 C16 C15 111.3(13) 2_756 . ? C15 C16 H16A 109.4 2_756 . ? C15 C16 H16A 109.4 . . ? C15 C16 H16B 109.4 2_756 . ? C15 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? Cl1 C17 Cl2 112.7(9) . . ? Cl1 C17 Cl3 109.8(9) . . ? Cl2 C17 Cl3 108.0(8) . . ? Cl1 C17 H17 108.8 . . ? Cl2 C17 H17 108.8 . . ? Cl3 C17 H17 108.8 . . ? B1 F1 F2' 52.7(12) . . ? B1 F1 F4' 47.9(13) . . ? F2' F1 F4' 91.5(17) . . ? B1 F2 F3' 60.3(12) . . ? B1 F2 F4' 50.2(11) . . ? F3' F2 F4' 88.9(17) . . ? B1 F2 F2' 44.6(9) . . ? F3' F2 F2' 84.7(16) . . ? F4' F2 F2' 82.9(14) . . ? B1 F3 F2' 51.3(10) . . ? B1 F3 F1' 56.2(10) . . ? F2' F3 F1' 92.3(15) . . ? B1 F3 F3' 56.0(15) . . ? F2' F3 F3' 88.5(18) . . ? F1' F3 F3' 87.6(14) . . ? F4' F4 B1 54.6(13) . . ? F4' F4 F1' 100.9(17) . . ? B1 F4 F1' 57.4(11) . . ? F4' F4 F3' 84(2) . . ? B1 F4 F3' 52.4(12) . . ? F1' F4 F3' 84.6(14) . . ? C1 N1 C5 114.0(8) . . ? C1 N1 Ag1 122.0(7) . . ? C5 N1 Ag1 124.0(6) . . ? C9 N2 C13 118.3(8) . . ? C9 N2 Ag1 120.9(7) . . ? C13 N2 Ag1 120.5(7) . . ? C5 S1 C6 105.8(4) . . ? C13 S2 C14 103.4(5) . . ? B1 F1' F4 59.0(8) . . ? B1 F1' F3 57.2(8) . . ? F4 F1' F3 101.6(11) . . ? B1 F2' F1 61.8(11) . . ? B1 F2' F3 59.7(11) . . ? F1 F2' F3 105.7(16) . . ? B1 F2' F2 51.5(10) . . ? F1 F2' F2 87.2(13) . . ? F3 F2' F2 89.7(17) . . ? B1 F3' F2 57.8(14) . . ? B1 F3' F3 53.2(10) . . ? F2 F3' F3 97(2) . . ? B1 F3' F4 50.3(10) . . ? F2 F3' F4 84(2) . . ? F3 F3' F4 85.1(15) . . ? B1 F4' F4 68.1(15) . . ? B1 F4' F2 61.2(16) . . ? F4 F4' F2 103(3) . . ? B1 F4' F1 57.4(11) . . ? F4 F4' F1 104(2) . . ? F2 F4' F1 92.8(18) . . ? 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 -5(2) . . . . ? C1 C2 C3 C4 5.4(19) . . . . ? C2 C3 C4 C5 -4.0(18) . . . . ? C3 C4 C5 N1 1.9(17) . . . . ? C3 C4 C5 S1 -178.4(8) . . . . ? S1 C6 C7 C8 -173.2(6) . . . . ? C6 C7 C8 C7 180.0(10) . . . 2_756 ? N2 C9 C10 C11 -3(2) . . . . ? C9 C10 C11 C12 3(2) . . . . ? C10 C11 C12 C13 -1(2) . . . . ? C11 C12 C13 N2 -0.8(18) . . . . ? C11 C12 C13 S2 -178.5(10) . . . . ? S2 C14 C15 C16 -179.8(7) . . . . ? C14 C15 C16 C15 178.0(12) . . . 2_756 ? F4' B1 F1 F2' -137(2) . . . . ? F1' B1 F1 F2' 114.1(16) . . . . ? F3 B1 F1 F2' 49.9(17) . . . . ? F4 B1 F1 F2' 176(2) . . . . ? F2 B1 F1 F2' -75.3(16) . . . . ? F3' B1 F1 F2' -65(9) . . . . ? F2' B1 F1 F4' 137(2) . . . . ? F1' B1 F1 F4' -109(2) . . . . ? F3 B1 F1 F4' -173(3) . . . . ? F4 B1 F1 F4' -46.8(19) . . . . ? F2 B1 F1 F4' 61.8(19) . . . . ? F3' B1 F1 F4' 72(9) . . . . ? F4' B1 F2 F3' -117(2) . . . . ? F2' B1 F2 F3' 115(2) . . . . ? F1' B1 F2 F3' -33(5) . . . . ? F3 B1 F2 F3' 51.1(19) . . . . ? F1 B1 F2 F3' 178(2) . . . . ? F4 B1 F2 F3' -68.7(19) . . . . ? F2' B1 F2 F4' -128(3) . . . . ? F1' B1 F2 F4' 83(5) . . . . ? F3 B1 F2 F4' 168(2) . . . . ? F1 B1 F2 F4' -66(2) . . . . ? F4 B1 F2 F4' 47.8(19) . . . . ? F3' B1 F2 F4' 117(2) . . . . ? F4' B1 F2 F2' 128(3) . . . . ? F1' B1 F2 F2' -148(6) . . . . ? F3 B1 F2 F2' -64.2(18) . . . . ? F1 B1 F2 F2' 62.3(16) . . . . ? F4 B1 F2 F2' 176(2) . . . . ? F3' B1 F2 F2' -115(2) . . . . ? F4' B1 F3 F2' 168(12) . . . . ? F1' B1 F3 F2' -127(2) . . . . ? F1 B1 F3 F2' -48.2(18) . . . . ? F4 B1 F3 F2' -173(2) . . . . ? F2 B1 F3 F2' 73.5(19) . . . . ? F3' B1 F3 F2' 120(2) . . . . ? F4' B1 F3 F1' -65(12) . . . . ? F2' B1 F3 F1' 127(2) . . . . ? F1 B1 F3 F1' 78.7(16) . . . . ? F4 B1 F3 F1' -46.0(14) . . . . ? F2 B1 F3 F1' -159.7(15) . . . . ? F3' B1 F3 F1' -113.0(16) . . . . ? F4' B1 F3 F3' 48(12) . . . . ? F2' B1 F3 F3' -120(2) . . . . ? F1' B1 F3 F3' 113.0(16) . . . . ? F1 B1 F3 F3' -168.3(18) . . . . ? F4 B1 F3 F3' 67.0(18) . . . . ? F2 B1 F3 F3' -46.6(15) . . . . ? F2' B1 F4 F4' 88(18) . . . . ? F1' B1 F4 F4' 137(3) . . . . ? F3 B1 F4 F4' -176(3) . . . . ? F1 B1 F4 F4' 57(2) . . . . ? F2 B1 F4 F4' -55(2) . . . . ? F3' B1 F4 F4' -112(2) . . . . ? F4' B1 F4 F1' -137(3) . . . . ? F2' B1 F4 F1' -49(18) . . . . ? F3 B1 F4 F1' 47.5(14) . . . . ? F1 B1 F4 F1' -80.4(15) . . . . ? F2 B1 F4 F1' 168.0(17) . . . . ? F3' B1 F4 F1' 110.6(18) . . . . ? F4' B1 F4 F3' 112(2) . . . . ? F2' B1 F4 F3' -159(18) . . . . ? F1' B1 F4 F3' -110.6(18) . . . . ? F3 B1 F4 F3' -63.0(19) . . . . ? F1 B1 F4 F3' 169.0(18) . . . . ? F2 B1 F4 F3' 57.4(16) . . . . ? C2 C1 N1 C5 2.9(18) . . . . ? C2 C1 N1 Ag1 -177.2(11) . . . . ? C4 C5 N1 C1 -1.2(15) . . . . ? S1 C5 N1 C1 179.1(8) . . . . ? C4 C5 N1 Ag1 179.0(8) . . . . ? S1 C5 N1 Ag1 -0.8(10) . . . . ? N2 Ag1 N1 C1 90.7(18) . . . . ? N2 Ag1 N1 C5 -89.5(18) . . . . ? C10 C9 N2 C13 1.4(17) . . . . ? C10 C9 N2 Ag1 -171.2(9) . . . . ? C12 C13 N2 C9 0.7(16) . . . . ? S2 C13 N2 C9 178.7(8) . . . . ? C12 C13 N2 Ag1 173.4(8) . . . . ? S2 C13 N2 Ag1 -8.7(11) . . . . ? N1 Ag1 N2 C9 -100.0(18) . . . . ? N1 Ag1 N2 C13 87.5(18) . . . . ? C4 C5 S1 C6 -9.9(10) . . . . ? N1 C5 S1 C6 169.9(7) . . . . ? C7 C6 S1 C5 -171.1(7) . . . . ? N2 C13 S2 C14 179.3(8) . . . . ? C12 C13 S2 C14 -2.9(11) . . . . ? C15 C14 S2 C13 -176.2(8) . . . . ? F4' B1 F1' F4 37(2) . . . . ? F2' B1 F1' F4 175(3) . . . . ? F3 B1 F1' F4 -131.8(15) . . . . ? F1 B1 F1' F4 111.1(16) . . . . ? F2 B1 F1' F4 -39(5) . . . . ? F3' B1 F1' F4 -69.1(17) . . . . ? F4' B1 F1' F3 169(2) . . . . ? F2' B1 F1' F3 -54(2) . . . . ? F1 B1 F1' F3 -117.2(15) . . . . ? F4 B1 F1' F3 131.8(15) . . . . ? F2 B1 F1' F3 92(5) . . . . ? F3' B1 F1' F3 62.7(16) . . . . ? F4' F4 F1' B1 -35(2) . . . . ? F3' F4 F1' B1 48.2(15) . . . . ? F4' F4 F1' F3 -74(2) . . . . ? B1 F4 F1' F3 -39.8(12) . . . . ? F3' F4 F1' F3 8.4(18) . . . . ? F2' F3 F1' B1 38.7(13) . . . . ? F3' F3 F1' B1 -49.8(16) . . . . ? B1 F3 F1' F4 40.7(12) . . . . ? F2' F3 F1' F4 79.4(17) . . . . ? F3' F3 F1' F4 -9(2) . . . . ? F4' B1 F2' F1 51(3) . . . . ? F1' B1 F2' F1 -79.6(17) . . . . ? F3 B1 F2' F1 -132.0(17) . . . . ? F4 B1 F2' F1 -33(18) . . . . ? F2 B1 F2' F1 110.8(14) . . . . ? F3' B1 F2' F1 168.3(18) . . . . ? F4' B1 F2' F3 -177(3) . . . . ? F1' B1 F2' F3 52.3(18) . . . . ? F1 B1 F2' F3 132.0(17) . . . . ? F4 B1 F2' F3 99(18) . . . . ? F2 B1 F2' F3 -117.3(18) . . . . ? F3' B1 F2' F3 -59.7(19) . . . . ? F4' B1 F2' F2 -60(2) . . . . ? F1' B1 F2' F2 169.6(19) . . . . ? F3 B1 F2' F2 117.3(18) . . . . ? F1 B1 F2' F2 -110.8(14) . . . . ? F4 B1 F2' F2 -144(18) . . . . ? F3' B1 F2' F2 57.5(16) . . . . ? F4' F1 F2' B1 -30.4(17) . . . . ? B1 F1 F2' F3 -41.8(14) . . . . ? F4' F1 F2' F3 -72(2) . . . . ? B1 F1 F2' F2 47.1(9) . . . . ? F4' F1 F2' F2 16.8(19) . . . . ? F1' F3 F2' B1 -41.7(14) . . . . ? F3' F3 F2' B1 45.8(17) . . . . ? B1 F3 F2' F1 42.9(13) . . . . ? F1' F3 F2' F1 1(2) . . . . ? F3' F3 F2' F1 89(2) . . . . ? B1 F3 F2' F2 -44.1(11) . . . . ? F1' F3 F2' F2 -85.8(15) . . . . ? F3' F3 F2' F2 1.7(18) . . . . ? F3' F2 F2' B1 -52.0(19) . . . . ? F4' F2 F2' B1 37(2) . . . . ? B1 F2 F2' F1 -55.6(12) . . . . ? F3' F2 F2' F1 -107.6(19) . . . . ? F4' F2 F2' F1 -18(2) . . . . ? B1 F2 F2' F3 50.1(13) . . . . ? F3' F2 F2' F3 -2(2) . . . . ? F4' F2 F2' F3 88(2) . . . . ? F4' B1 F3' F2 58(2) . . . . ? F2' B1 F3' F2 -71.9(19) . . . . ? F1' B1 F3' F2 169.7(16) . . . . ? F3 B1 F3' F2 -130.6(19) . . . . ? F1 B1 F3' F2 -11(10) . . . . ? F4 B1 F3' F2 110.6(18) . . . . ? F4' B1 F3' F3 -171(2) . . . . ? F2' B1 F3' F3 58.7(15) . . . . ? F1' B1 F3' F3 -59.8(14) . . . . ? F1 B1 F3' F3 120(9) . . . . ? F4 B1 F3' F3 -118.8(19) . . . . ? F2 B1 F3' F3 130.6(19) . . . . ? F4' B1 F3' F4 -52.5(16) . . . . ? F2' B1 F3' F4 177(2) . . . . ? F1' B1 F3' F4 59.0(15) . . . . ? F3 B1 F3' F4 118.8(19) . . . . ? F1 B1 F3' F4 -122(9) . . . . ? F2 B1 F3' F4 -110.6(18) . . . . ? F4' F2 F3' B1 -43.4(13) . . . . ? F2' F2 F3' B1 39.6(13) . . . . ? B1 F2 F3' F3 -37.8(13) . . . . ? F4' F2 F3' F3 -81.2(19) . . . . ? F2' F2 F3' F3 1.8(19) . . . . ? B1 F2 F3' F4 46.5(10) . . . . ? F4' F2 F3' F4 3.1(17) . . . . ? F2' F2 F3' F4 86.1(15) . . . . ? F2' F3 F3' B1 -42.5(15) . . . . ? F1' F3 F3' B1 49.9(11) . . . . ? B1 F3 F3' F2 40.4(16) . . . . ? F2' F3 F3' F2 -2(2) . . . . ? F1' F3 F3' F2 90.3(18) . . . . ? B1 F3 F3' F4 -42.6(13) . . . . ? F2' F3 F3' F4 -85(2) . . . . ? F1' F3 F3' F4 7.3(16) . . . . ? F4' F4 F3' B1 49.2(16) . . . . ? F1' F4 F3' B1 -52.4(13) . . . . ? F4' F4 F3' F2 -4(2) . . . . ? B1 F4 F3' F2 -52.8(13) . . . . ? F1' F4 F3' F2 -105.2(16) . . . . ? F4' F4 F3' F3 94(2) . . . . ? B1 F4 F3' F3 44.8(13) . . . . ? F1' F4 F3' F3 -7.6(16) . . . . ? F2' B1 F4' F4 -172(3) . . . . ? F1' B1 F4' F4 -40(2) . . . . ? F3 B1 F4' F4 21(13) . . . . ? F1 B1 F4' F4 -125(2) . . . . ? F2 B1 F4' F4 120(2) . . . . ? F3' B1 F4' F4 67(2) . . . . ? F2' B1 F4' F2 68(2) . . . . ? F1' B1 F4' F2 -160.4(16) . . . . ? F3 B1 F4' F2 -99(12) . . . . ? F1 B1 F4' F2 114.6(16) . . . . ? F4 B1 F4' F2 -120(2) . . . . ? F3' B1 F4' F2 -53.6(14) . . . . ? F2' B1 F4' F1 -47(2) . . . . ? F1' B1 F4' F1 85.0(16) . . . . ? F3 B1 F4' F1 146(11) . . . . ? F4 B1 F4' F1 125(2) . . . . ? F2 B1 F4' F1 -114.6(16) . . . . ? F3' B1 F4' F1 -168.2(17) . . . . ? F1' F4 F4' B1 36(2) . . . . ? F3' F4 F4' B1 -47.4(16) . . . . ? B1 F4 F4' F2 51.0(14) . . . . ? F1' F4 F4' F2 87(2) . . . . ? F3' F4 F4' F2 4(2) . . . . ? B1 F4 F4' F1 -45.4(14) . . . . ? F1' F4 F4' F1 -10(3) . . . . ? F3' F4 F4' F1 -93(2) . . . . ? F3' F2 F4' B1 51.0(18) . . . . ? F2' F2 F4' B1 -33.8(16) . . . . ? B1 F2 F4' F4 -55.3(16) . . . . ? F3' F2 F4' F4 -4(2) . . . . ? F2' F2 F4' F4 -89(2) . . . . ? B1 F2 F4' F1 50.1(11) . . . . ? F3' F2 F4' F1 101.1(19) . . . . ? F2' F2 F4' F1 16.3(18) . . . . ? F2' F1 F4' B1 32.8(18) . . . . ? B1 F1 F4' F4 51.6(19) . . . . ? F2' F1 F4' F4 84(3) . . . . ? B1 F1 F4' F2 -53.0(15) . . . . ? F2' F1 F4' F2 -20(2) . . . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 0.582 _refine_diff_density_min -0.882 _refine_diff_density_rms 0.093 data_021224d _database_code_depnum_ccdc_archive 'CCDC 223563' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16.50 H20 Ag F3 N2 O3.50 S3' _chemical_formula_weight 563.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.382(5) _cell_length_b 21.700(6) _cell_length_c 14.334(5) _cell_angle_alpha 90.00 _cell_angle_beta 117.854(8) _cell_angle_gamma 90.00 _cell_volume 4780(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 978 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 21.45 _exptl_crystal_description Flake _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2264 _exptl_absorpt_coefficient_mu 1.149 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7100 _exptl_absorpt_correction_T_max 0.8199 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 11124 _diffrn_reflns_av_R_equivalents 0.0694 _diffrn_reflns_av_sigmaI/netI 0.0918 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4207 _reflns_number_gt 2015 _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^)+(0.1015P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00019(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4207 _refine_ls_number_parameters 347 _refine_ls_number_restraints 215 _refine_ls_R_factor_all 0.1543 _refine_ls_R_factor_gt 0.0678 _refine_ls_wR_factor_ref 0.2043 _refine_ls_wR_factor_gt 0.1636 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.022 _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 1.10091(4) 0.41999(3) 1.19248(6) 0.0798(4) Uani 1 1 d . . . N1 N 1.0145(4) 0.4995(3) 1.1310(5) 0.0582(19) Uani 1 1 d . . . N2 N 0.3221(5) 0.1643(3) 0.7920(6) 0.0647(19) Uani 1 1 d . . . S1 S 0.89458(13) 0.42046(11) 1.10156(19) 0.0648(6) Uani 1 1 d . . . S2 S 0.47255(16) 0.21526(11) 0.8684(2) 0.0812(8) Uani 1 1 d . . . C1 C 1.0470(6) 0.5547(5) 1.1318(8) 0.077(3) Uani 1 1 d . . . H1 H 1.1068 0.5579 1.1562 0.093 Uiso 1 1 calc R . . C2 C 0.9980(7) 0.6077(5) 1.0988(8) 0.093(3) Uani 1 1 d . . . H2 H 1.0230 0.6455 1.0983 0.112 Uiso 1 1 calc R . . C3 C 0.9111(7) 0.6021(5) 1.0668(9) 0.096(4) Uani 1 1 d . . . H3 H 0.8758 0.6369 1.0459 0.116 Uiso 1 1 calc R . . C4 C 0.8752(6) 0.5456(4) 1.0653(8) 0.076(3) Uani 1 1 d . . . H4 H 0.8159 0.5414 1.0431 0.091 Uiso 1 1 calc R . . C5 C 0.9301(6) 0.4948(4) 1.0980(6) 0.058(2) Uani 1 1 d . . . C6 C 0.7781(5) 0.4226(4) 1.0208(8) 0.074(3) Uani 1 1 d . . . H6A H 0.7520 0.4459 1.0565 0.089 Uiso 1 1 calc R . . H6B H 0.7638 0.4428 0.9544 0.089 Uiso 1 1 calc R . . C7 C 0.7425(5) 0.3580(4) 1.0003(8) 0.064(2) Uani 1 1 d . . . H7A H 0.7665 0.3354 1.0663 0.077 Uiso 1 1 calc R . . H7B H 0.7605 0.3374 0.9536 0.077 Uiso 1 1 calc R . . C8 C 0.6444(5) 0.3573(4) 0.9510(7) 0.067(2) Uani 1 1 d . . . H8A H 0.6267 0.3785 0.9974 0.080 Uiso 1 1 calc R . . H8B H 0.6207 0.3797 0.8848 0.080 Uiso 1 1 calc R . . C9 C 0.6067(5) 0.2934(4) 0.9304(7) 0.065(2) Uani 1 1 d . . . H9A H 0.6334 0.2699 0.9955 0.078 Uiso 1 1 calc R . . H9B H 0.6207 0.2731 0.8799 0.078 Uiso 1 1 calc R . . C10 C 0.5087(5) 0.2931(4) 0.8880(7) 0.069(3) Uani 1 1 d . . . H10A H 0.4809 0.3155 0.8217 0.083 Uiso 1 1 calc R . . H10B H 0.4936 0.3131 0.9378 0.083 Uiso 1 1 calc R . . C11 C 0.3601(5) 0.2201(4) 0.8142(7) 0.060(2) Uani 1 1 d . . . C12 C 0.3126(6) 0.2743(4) 0.7966(8) 0.085(3) Uani 1 1 d . . . H12 H 0.3403 0.3124 0.8134 0.102 Uiso 1 1 calc R . . C13 C 0.2243(7) 0.2702(5) 0.7540(10) 0.098(4) Uani 1 1 d . . . H13 H 0.1911 0.3058 0.7411 0.117 Uiso 1 1 calc R . . C14 C 0.1833(6) 0.2123(5) 0.7296(9) 0.094(3) Uani 1 1 d . . . H14 H 0.1232 0.2087 0.7007 0.112 Uiso 1 1 calc R . . C15 C 0.2347(6) 0.1622(4) 0.7499(8) 0.079(3) Uani 1 1 d . . . H15 H 0.2081 0.1237 0.7338 0.095 Uiso 1 1 calc R . . S3 S 0.2975(4) 0.5347(4) 0.2977(6) 0.091(3) Uani 0.771(11) 1 d PDU . 1 O1 O 0.2429(6) 0.4841(4) 0.2569(11) 0.121(5) Uani 0.771(11) 1 d PDU . 1 O2 O 0.3185(11) 0.5480(8) 0.4047(8) 0.192(7) Uani 0.771(11) 1 d PDU . 1 O3 O 0.2737(12) 0.5878(6) 0.2347(12) 0.124(6) Uani 0.771(11) 1 d PDU . 1 C16 C 0.4013(6) 0.5093(5) 0.3107(10) 0.116(4) Uani 0.771(11) 1 d PDU . 1 F1 F 0.4290(5) 0.4569(4) 0.3695(9) 0.161(5) Uani 0.771(11) 1 d PDU . 1 F2 F 0.3903(8) 0.4989(6) 0.2100(9) 0.192(6) Uani 0.771(11) 1 d PDU . 1 F3 F 0.4598(10) 0.5570(5) 0.3603(13) 0.213(8) Uani 0.771(11) 1 d PDU . 1 S3' S 0.2995(14) 0.5239(11) 0.2736(19) 0.086(7) Uani 0.229(11) 1 d PDU . 2 O1' O 0.267(3) 0.4818(14) 0.189(3) 0.157(17) Uani 0.229(11) 1 d PDU . 2 O2' O 0.258(4) 0.518(2) 0.338(4) 0.192(19) Uani 0.229(11) 1 d PDU . 2 O3' O 0.298(4) 0.5856(12) 0.240(3) 0.092(13) Uani 0.229(11) 1 d PDU . 2 C16' C 0.4024(17) 0.5333(17) 0.391(2) 0.154(13) Uani 0.229(11) 1 d PDU . 2 F1' F 0.418(3) 0.488(2) 0.464(3) 0.25(2) Uani 0.229(11) 1 d PDU . 2 F2' F 0.457(3) 0.5314(17) 0.346(4) 0.150(14) Uani 0.229(11) 1 d PDU . 2 F3' F 0.396(4) 0.591(2) 0.426(4) 0.245(19) Uani 0.229(11) 1 d PDU . 2 O4 O 0.4193(15) 0.7080(11) 0.5921(15) 0.153(7) Uani 0.50 1 d PDU . . H4A H 0.4579 0.7144 0.6522 0.230 Uiso 0.50 1 calc PR . . C17 C 0.386(2) 0.6455(12) 0.585(3) 0.163(11) Uani 0.50 1 d PDU . . H17A H 0.4021 0.6304 0.6546 0.245 Uiso 0.50 1 calc PR . . H17B H 0.4107 0.6193 0.5518 0.245 Uiso 0.50 1 calc PR . . H17C H 0.3240 0.6457 0.5439 0.245 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0525(5) 0.0531(5) 0.1187(7) -0.0094(4) 0.0272(4) -0.0038(3) N1 0.046(4) 0.049(5) 0.070(5) -0.001(4) 0.018(4) -0.009(3) N2 0.062(5) 0.051(5) 0.079(5) -0.003(4) 0.030(4) -0.011(3) S1 0.0446(12) 0.0542(13) 0.0870(16) 0.0005(12) 0.0235(11) -0.0015(10) S2 0.0560(14) 0.0474(14) 0.129(2) -0.0040(14) 0.0340(14) -0.0048(11) C1 0.056(6) 0.068(7) 0.093(8) 0.005(6) 0.023(5) -0.005(5) C2 0.076(7) 0.075(8) 0.100(8) 0.018(6) 0.018(6) -0.026(6) C3 0.069(7) 0.069(7) 0.125(9) 0.024(6) 0.023(6) 0.005(5) C4 0.056(6) 0.056(6) 0.099(7) 0.007(5) 0.023(5) -0.011(5) C5 0.055(5) 0.057(6) 0.053(5) -0.002(4) 0.017(4) 0.002(4) C6 0.048(5) 0.065(6) 0.095(7) -0.003(5) 0.021(5) 0.002(4) C7 0.046(5) 0.054(6) 0.085(6) -0.005(5) 0.024(4) -0.009(4) C8 0.056(5) 0.051(5) 0.088(7) -0.001(5) 0.028(5) -0.004(4) C9 0.060(5) 0.054(6) 0.077(6) -0.002(5) 0.029(5) -0.007(4) C10 0.066(6) 0.056(6) 0.084(7) -0.003(5) 0.033(5) -0.007(4) C11 0.052(5) 0.051(6) 0.071(6) -0.001(4) 0.023(4) -0.004(4) C12 0.063(6) 0.053(6) 0.123(9) 0.003(6) 0.030(6) 0.001(5) C13 0.064(7) 0.065(7) 0.148(10) 0.011(7) 0.036(7) 0.016(5) C14 0.055(6) 0.074(8) 0.132(10) -0.003(7) 0.027(6) 0.006(6) C15 0.067(7) 0.055(6) 0.117(8) -0.015(6) 0.044(6) -0.016(5) S3 0.064(3) 0.084(5) 0.119(4) -0.009(3) 0.037(3) -0.023(3) O1 0.054(5) 0.068(6) 0.203(13) -0.007(7) 0.028(7) -0.019(5) O2 0.216(17) 0.247(18) 0.157(9) -0.059(10) 0.125(12) -0.088(13) O3 0.085(9) 0.071(7) 0.194(12) 0.012(7) 0.049(8) -0.002(6) C16 0.063(8) 0.085(10) 0.190(13) 0.005(9) 0.051(10) -0.026(6) F1 0.065(5) 0.108(7) 0.239(11) 0.041(8) 0.012(6) 0.004(5) F2 0.206(13) 0.180(12) 0.251(11) 0.008(9) 0.158(11) 0.051(9) F3 0.077(6) 0.111(10) 0.382(18) -0.011(11) 0.049(10) -0.055(8) S3' 0.086(11) 0.041(9) 0.141(15) 0.026(9) 0.061(9) 0.007(8) O1' 0.19(3) 0.048(17) 0.18(3) -0.005(18) 0.04(2) 0.00(2) O2' 0.19(3) 0.22(4) 0.23(3) 0.06(3) 0.16(3) -0.03(3) O3' 0.14(3) 0.041(12) 0.11(2) 0.006(14) 0.067(18) -0.003(17) C16' 0.131(19) 0.16(3) 0.14(2) 0.015(14) 0.035(12) 0.02(2) F1' 0.22(3) 0.30(3) 0.16(3) 0.08(3) 0.031(19) -0.01(3) F2' 0.091(15) 0.07(2) 0.28(3) -0.01(2) 0.07(2) -0.053(19) F3' 0.27(4) 0.23(3) 0.20(3) -0.10(2) 0.08(2) -0.03(3) O4 0.173(11) 0.179(11) 0.129(10) -0.001(8) 0.088(8) 0.024(8) C17 0.177(14) 0.186(15) 0.153(14) -0.014(9) 0.099(10) 0.011(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 2.185(7) . ? Ag1 N2 2.216(7) 7_657 ? Ag1 O1 2.598(8) 1_656 ? Ag1 S1 2.917(3) 2_757 ? N1 C5 1.317(10) . ? N1 C1 1.322(11) . ? N2 C11 1.343(10) . ? N2 C15 1.348(10) . ? N2 Ag1 2.216(7) 7_657 ? S1 C5 1.736(9) . ? S1 C6 1.803(8) . ? S1 Ag1 2.917(3) 2_757 ? S2 C11 1.736(8) . ? S2 C10 1.779(9) . ? C1 C2 1.377(14) . ? C1 H1 0.9300 . ? C2 C3 1.364(14) . ? C2 H2 0.9300 . ? C3 C4 1.371(13) . ? C3 H3 0.9300 . ? C4 C5 1.389(12) . ? C4 H4 0.9300 . ? C6 C7 1.504(11) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.509(10) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.503(11) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.519(11) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.391(12) . ? C12 C13 1.364(13) . ? C12 H12 0.9300 . ? C13 C14 1.405(14) . ? C13 H13 0.9300 . ? C14 C15 1.350(12) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? S3 O1 1.389(7) . ? S3 O3 1.402(7) . ? S3 O2 1.430(8) . ? S3 C16 1.811(9) . ? O1 Ag1 2.598(8) 1_454 ? C16 F1 1.363(9) . ? C16 F2 1.384(9) . ? C16 F3 1.391(8) . ? S3' O1' 1.411(10) . ? S3' O2' 1.418(10) . ? S3' O3' 1.419(10) . ? S3' C16' 1.804(10) . ? C16' F1' 1.372(10) . ? C16' F3' 1.378(10) . ? C16' F2' 1.380(10) . ? O4 C17 1.457(10) . ? O4 H4A 0.8200 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? 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 N2 164.1(3) . 7_657 ? N1 Ag1 O1 94.6(3) . 1_656 ? N2 Ag1 O1 88.7(3) 7_657 1_656 ? N1 Ag1 S1 95.39(19) . 2_757 ? N2 Ag1 S1 99.90(19) 7_657 2_757 ? O1 Ag1 S1 93.8(4) 1_656 2_757 ? C5 N1 C1 118.3(8) . . ? C5 N1 Ag1 121.5(5) . . ? C1 N1 Ag1 120.0(6) . . ? C11 N2 C15 117.6(8) . . ? C11 N2 Ag1 120.8(6) . 7_657 ? C15 N2 Ag1 121.2(6) . 7_657 ? C5 S1 C6 105.4(4) . . ? C5 S1 Ag1 101.0(3) . 2_757 ? C6 S1 Ag1 98.1(4) . 2_757 ? C11 S2 C10 104.7(4) . . ? N1 C1 C2 124.0(9) . . ? N1 C1 H1 118.0 . . ? C2 C1 H1 118.0 . . ? C3 C2 C1 116.9(10) . . ? C3 C2 H2 121.6 . . ? C1 C2 H2 121.6 . . ? C2 C3 C4 120.6(10) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C3 C4 C5 118.0(9) . . ? C3 C4 H4 121.0 . . ? C5 C4 H4 121.0 . . ? N1 C5 C4 122.2(8) . . ? N1 C5 S1 114.5(6) . . ? C4 C5 S1 123.3(7) . . ? C7 C6 S1 109.8(6) . . ? C7 C6 H6A 109.7 . . ? S1 C6 H6A 109.7 . . ? C7 C6 H6B 109.7 . . ? S1 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? C6 C7 C8 111.9(7) . . ? C6 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 . . ? C6 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C9 C8 C7 113.3(7) . . ? C9 C8 H8A 108.9 . . ? C7 C8 H8A 108.9 . . ? C9 C8 H8B 108.9 . . ? C7 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C8 C9 C10 112.7(7) . . ? C8 C9 H9A 109.0 . . ? C10 C9 H9A 109.0 . . ? C8 C9 H9B 109.0 . . ? C10 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? C9 C10 S2 108.3(6) . . ? C9 C10 H10A 110.0 . . ? S2 C10 H10A 110.0 . . ? C9 C10 H10B 110.0 . . ? S2 C10 H10B 110.0 . . ? H10A C10 H10B 108.4 . . ? N2 C11 C12 122.3(8) . . ? N2 C11 S2 112.2(6) . . ? C12 C11 S2 125.5(7) . . ? C13 C12 C11 118.3(9) . . ? C13 C12 H12 120.8 . . ? C11 C12 H12 120.8 . . ? C12 C13 C14 120.3(9) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C15 C14 C13 117.3(9) . . ? C15 C14 H14 121.4 . . ? C13 C14 H14 121.4 . . ? N2 C15 C14 124.2(9) . . ? N2 C15 H15 117.9 . . ? C14 C15 H15 117.9 . . ? O1 S3 O3 116.2(7) . . ? O1 S3 O2 113.1(7) . . ? O3 S3 O2 112.0(7) . . ? O1 S3 C16 104.7(8) . . ? O3 S3 C16 107.3(10) . . ? O2 S3 C16 102.0(9) . . ? S3 O1 Ag1 157.1(8) . 1_454 ? F1 C16 F2 110.2(8) . . ? F1 C16 F3 110.0(8) . . ? F2 C16 F3 111.5(8) . . ? F1 C16 S3 111.4(8) . . ? F2 C16 S3 107.3(8) . . ? F3 C16 S3 106.3(10) . . ? O1' S3' O2' 112.4(11) . . ? O1' S3' O3' 112.4(11) . . ? O2' S3' O3' 112.0(11) . . ? O1' S3' C16' 134(3) . . ? O2' S3' C16' 89(3) . . ? O3' S3' C16' 94(3) . . ? F1' C16' F3' 113.0(11) . . ? F1' C16' F2' 113.6(11) . . ? F3' C16' F2' 113.3(11) . . ? F1' C16' S3' 113(3) . . ? F3' C16' S3' 103(3) . . ? F2' C16' S3' 99(3) . . ? C17 O4 H4A 109.5 . . ? O4 C17 H17A 109.5 . . ? O4 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O4 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ag1 N1 C5 86.8(11) 7_657 . . . ? O1 Ag1 N1 C5 -171.6(7) 1_656 . . . ? S1 Ag1 N1 C5 -77.3(6) 2_757 . . . ? N2 Ag1 N1 C1 -97.1(11) 7_657 . . . ? O1 Ag1 N1 C1 4.5(8) 1_656 . . . ? S1 Ag1 N1 C1 98.8(7) 2_757 . . . ? C5 N1 C1 C2 -1.0(15) . . . . ? Ag1 N1 C1 C2 -177.2(8) . . . . ? N1 C1 C2 C3 2.2(17) . . . . ? C1 C2 C3 C4 -1.9(17) . . . . ? C2 C3 C4 C5 0.5(17) . . . . ? C1 N1 C5 C4 -0.5(13) . . . . ? Ag1 N1 C5 C4 175.6(7) . . . . ? C1 N1 C5 S1 -179.3(7) . . . . ? Ag1 N1 C5 S1 -3.2(9) . . . . ? C3 C4 C5 N1 0.8(15) . . . . ? C3 C4 C5 S1 179.5(8) . . . . ? C6 S1 C5 N1 -164.5(6) . . . . ? Ag1 S1 C5 N1 93.8(6) 2_757 . . . ? C6 S1 C5 C4 16.7(9) . . . . ? Ag1 S1 C5 C4 -85.0(8) 2_757 . . . ? C5 S1 C6 C7 168.5(7) . . . . ? Ag1 S1 C6 C7 -87.6(7) 2_757 . . . ? S1 C6 C7 C8 169.2(7) . . . . ? C6 C7 C8 C9 -179.4(8) . . . . ? C7 C8 C9 C10 175.9(8) . . . . ? C8 C9 C10 S2 -179.4(7) . . . . ? C11 S2 C10 C9 -177.1(6) . . . . ? C15 N2 C11 C12 1.0(13) . . . . ? Ag1 N2 C11 C12 174.3(7) 7_657 . . . ? C15 N2 C11 S2 179.7(7) . . . . ? Ag1 N2 C11 S2 -7.0(9) 7_657 . . . ? C10 S2 C11 N2 178.5(6) . . . . ? C10 S2 C11 C12 -2.9(10) . . . . ? N2 C11 C12 C13 -0.9(15) . . . . ? S2 C11 C12 C13 -179.4(8) . . . . ? C11 C12 C13 C14 0.5(17) . . . . ? C12 C13 C14 C15 -0.1(18) . . . . ? C11 N2 C15 C14 -0.7(14) . . . . ? Ag1 N2 C15 C14 -173.9(9) 7_657 . . . ? C13 C14 C15 N2 0.2(17) . . . . ? O3 S3 O1 Ag1 -66(3) . . . 1_454 ? O2 S3 O1 Ag1 65(2) . . . 1_454 ? C16 S3 O1 Ag1 176(2) . . . 1_454 ? O1 S3 C16 F1 -54.9(11) . . . . ? O3 S3 C16 F1 -178.9(9) . . . . ? O2 S3 C16 F1 63.2(10) . . . . ? O1 S3 C16 F2 65.9(10) . . . . ? O3 S3 C16 F2 -58.1(10) . . . . ? O2 S3 C16 F2 -176.0(9) . . . . ? O1 S3 C16 F3 -174.8(10) . . . . ? O3 S3 C16 F3 61.2(11) . . . . ? O2 S3 C16 F3 -56.7(11) . . . . ? O1' S3' C16' F1' -70(4) . . . . ? O2' S3' C16' F1' 51(3) . . . . ? O3' S3' C16' F1' 163(3) . . . . ? O1' S3' C16' F3' 167(3) . . . . ? O2' S3' C16' F3' -71(3) . . . . ? O3' S3' C16' F3' 41(3) . . . . ? O1' S3' C16' F2' 51(4) . . . . ? O2' S3' C16' F2' 172(3) . . . . ? O3' S3' C16' F2' -76(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.831 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.115 data_020915b _database_code_depnum_ccdc_archive 'CCDC 223564' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H40 Ag2 B2 F8 N4 S4' _chemical_formula_weight 998.28 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2 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' _cell_length_a 17.502(12) _cell_length_b 17.831(13) _cell_length_c 13.250(9) _cell_angle_alpha 90.00 _cell_angle_beta 106.446(12) _cell_angle_gamma 90.00 _cell_volume 3966(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 903 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 21.21 _exptl_crystal_description Flake _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.672 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 1.265 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7860 _exptl_absorpt_correction_T_max 0.8839 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 6915 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0683 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6326 _reflns_number_gt 3228 _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^)+(0.1286P)^2^+4.1109P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.3(11) _refine_ls_number_reflns 6326 _refine_ls_number_parameters 357 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.1473 _refine_ls_R_factor_gt 0.0730 _refine_ls_wR_factor_ref 0.2508 _refine_ls_wR_factor_gt 0.1974 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 28.674 _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 1.0000 0.2390(10) 0.5000 0.085(6) Uani 1 2 d S . . Ag2 Ag 0.7413(8) 0.8624(8) 0.7557(7) 0.094(5) Uani 1 1 d . . . Ag3 Ag 0.5000 0.2460(11) 1.0000 0.107(8) Uani 1 2 d S . . S1 S 1.060(2) 0.369(2) 0.661(3) 0.086(15) Uani 1 1 d D . . S2 S 0.681(2) 0.725(2) 0.608(3) 0.075(13) Uani 1 1 d D . . S3 S 0.810(2) 0.740(2) 0.927(3) 0.081(13) Uani 1 1 d D . . S4 S 0.432(3) 0.377(3) 0.842(4) 0.11(2) Uani 1 1 d D . . N1 N 0.985(3) 0.243(4) 0.661(4) 0.07(4) Uani 1 1 d G . . C1 C 0.947(5) 0.187(4) 0.700(6) 0.08(5) Uani 1 1 d G . . H1 H 0.9316 0.1430 0.6617 0.091 Uiso 1 1 calc R . . C2 C 0.931(6) 0.196(7) 0.797(7) 0.10(7) Uani 1 1 d G . . H2 H 0.9055 0.1581 0.8227 0.126 Uiso 1 1 calc R . . C3 C 0.954(6) 0.261(8) 0.854(6) 0.13(8) Uani 1 1 d G . . H3 H 0.9437 0.2674 0.9186 0.153 Uiso 1 1 calc R . . C4 C 0.993(7) 0.318(6) 0.815(6) 0.11(7) Uani 1 1 d G . . H4 H 1.0080 0.3616 0.8536 0.130 Uiso 1 1 calc R . . C5 C 1.008(5) 0.309(4) 0.719(6) 0.09(5) Uani 1 1 d GD . . C6 C 1.016(6) 0.452(6) 0.686(13) 0.13(8) Uani 1 1 d D . . H6A H 1.0147 0.4530 0.7588 0.158 Uiso 1 1 calc R . . H6B H 1.0476 0.4949 0.6753 0.158 Uiso 1 1 calc R . . C7 C 0.932(7) 0.457(6) 0.612(17) 0.19(14) Uani 1 1 d D . . H7A H 0.8947 0.4297 0.6401 0.226 Uiso 1 1 calc R . . H7B H 0.9300 0.4370 0.5431 0.226 Uiso 1 1 calc R . . C8 C 0.915(7) 0.542(7) 0.607(12) 0.250 Uiso 1 1 d D . . H8A H 0.9633 0.5700 0.6368 0.300 Uiso 1 1 calc R . . H8B H 0.8917 0.5577 0.5347 0.300 Uiso 1 1 calc R . . C9 C 0.856(7) 0.553(7) 0.671(12) 0.22(13) Uani 1 1 d D . . H9A H 0.8854 0.5499 0.7449 0.260 Uiso 1 1 calc R . . H9B H 0.8184 0.5120 0.6556 0.260 Uiso 1 1 calc R . . C10 C 0.809(6) 0.628(6) 0.653(15) 0.15(8) Uani 1 1 d D . . H10A H 0.8177 0.6506 0.7215 0.183 Uiso 1 1 calc R . . H10B H 0.8352 0.6599 0.6136 0.183 Uiso 1 1 calc R . . C11 C 0.719(6) 0.635(6) 0.598(11) 0.08(5) Uani 1 1 d D . . H11A H 0.6909 0.5988 0.6290 0.099 Uiso 1 1 calc R . . H11B H 0.7093 0.6221 0.5243 0.099 Uiso 1 1 calc R . . N2 N 0.756(2) 0.852(2) 0.597(3) 0.06(3) Uani 1 1 d G . . C12 C 0.730(2) 0.785(2) 0.546(3) 0.06(4) Uani 1 1 d GD . . C13 C 0.747(3) 0.768(3) 0.452(3) 0.07(5) Uani 1 1 d G . . H13 H 0.7293 0.7227 0.4175 0.088 Uiso 1 1 calc R . . C14 C 0.790(3) 0.818(3) 0.409(3) 0.10(7) Uani 1 1 d G . . H14 H 0.8009 0.8067 0.3461 0.116 Uiso 1 1 calc R . . C15 C 0.816(2) 0.885(3) 0.460(3) 0.12(7) Uani 1 1 d G . . H15 H 0.8445 0.9191 0.4313 0.141 Uiso 1 1 calc R . . C16 C 0.799(2) 0.902(3) 0.554(3) 0.09(6) Uani 1 1 d G . . H16 H 0.8164 0.9474 0.5880 0.107 Uiso 1 1 calc R . . N3 N 0.735(3) 0.867(3) 0.918(3) 0.07(4) Uani 1 1 d G . . C17 C 0.695(4) 0.925(4) 0.953(3) 0.10(6) Uani 1 1 d G . . H17 H 0.6758 0.9659 0.9091 0.116 Uiso 1 1 calc R . . C18 C 0.683(4) 0.922(5) 1.052(3) 0.10(7) Uani 1 1 d G . . H18 H 0.6566 0.9606 1.0751 0.123 Uiso 1 1 calc R . . C19 C 0.712(4) 0.861(5) 1.118(3) 0.11(6) Uani 1 1 d G . . H19 H 0.7039 0.8588 1.1841 0.128 Uiso 1 1 calc R . . C20 C 0.751(4) 0.803(4) 1.083(3) 0.08(5) Uani 1 1 d G . . H20 H 0.7704 0.7624 1.1269 0.096 Uiso 1 1 calc R . . C21 C 0.763(3) 0.806(4) 0.984(3) 0.07(5) Uani 1 1 d GD . . C22 C 0.769(5) 0.656(3) 0.955(4) 0.13(8) Uani 1 1 d GD . . H22A H 0.7947 0.6141 0.9314 0.151 Uiso 1 1 calc R . . H22B H 0.7786 0.6512 1.0306 0.151 Uiso 1 1 calc R . . C23 C 0.678(7) 0.650(6) 0.902(18) 0.18(11) Uani 1 1 d D . . H23A H 0.6485 0.6804 0.9397 0.213 Uiso 1 1 calc R . . H23B H 0.6644 0.6663 0.8296 0.213 Uiso 1 1 calc R . . C24 C 0.660(7) 0.566(7) 0.91(2) 0.27(14) Uani 1 1 d D . . H24A H 0.6915 0.5367 0.8752 0.325 Uiso 1 1 calc R . . H24B H 0.6739 0.5510 0.9837 0.325 Uiso 1 1 calc R . . C25 C 0.571(7) 0.555(6) 0.858(16) 0.24(11) Uani 1 1 d D . . H25A H 0.5578 0.5645 0.7829 0.284 Uiso 1 1 calc R . . H25B H 0.5393 0.5869 0.8891 0.284 Uiso 1 1 calc R . . C26 C 0.560(6) 0.471(7) 0.881(18) 0.21(16) Uani 1 1 d D . . H26A H 0.5682 0.4622 0.9554 0.250 Uiso 1 1 calc R . . H26B H 0.5957 0.4393 0.8554 0.250 Uiso 1 1 calc R . . C27 C 0.472(6) 0.461(6) 0.816(14) 0.15(10) Uani 1 1 d D . . H27A H 0.4678 0.4638 0.7415 0.177 Uiso 1 1 calc R . . H27B H 0.4404 0.5024 0.8318 0.177 Uiso 1 1 calc R . . N4 N 0.505(4) 0.249(4) 0.840(5) 0.09(4) Uani 1 1 d G . . C28 C 0.482(6) 0.315(5) 0.783(6) 0.09(6) Uani 1 1 d GD . . C29 C 0.494(7) 0.324(7) 0.685(7) 0.16(10) Uani 1 1 d G . . H29 H 0.4788 0.3679 0.6472 0.190 Uiso 1 1 calc R . . C30 C 0.529(7) 0.266(9) 0.642(6) 0.23(12) Uani 1 1 d G . . H30 H 0.5370 0.2721 0.5764 0.281 Uiso 1 1 calc R . . C31 C 0.552(6) 0.200(7) 0.699(7) 0.13(10) Uani 1 1 d G . . H31 H 0.5751 0.1619 0.6701 0.156 Uiso 1 1 calc R . . C32 C 0.540(5) 0.192(5) 0.797(7) 0.08(6) Uani 1 1 d G . . H32 H 0.5549 0.1474 0.8347 0.100 Uiso 1 1 calc R . . B1 B 0.751(5) 1.073(5) 0.741(7) 0.07(5) Uani 1 1 d D . . F1 F 0.742(5) 1.147(3) 0.761(7) 0.15(6) Uani 1 1 d D . . F2 F 0.792(4) 1.071(6) 0.665(5) 0.18(5) Uani 1 1 d D . . F3 F 0.683(4) 1.036(6) 0.709(11) 0.38(17) Uani 1 1 d D . . F4 F 0.800(7) 1.040(6) 0.828(7) 0.282 Uiso 1 1 d D . . B2 B 1.0000 0.5419 1.0000 0.250 Uiso 1 2 d SD . . F5 F 0.9337 0.5845 0.9539 0.166 Uiso 1 1 d D . . F6 F 1.0031 0.4862 0.9290 0.254 Uiso 1 1 d D . . B3 B 0.9881 0.0157 0.4605 0.250 Uiso 0.50 1 d PD . . F7 F 1.0112 0.0867 0.5034 0.250 Uiso 0.50 1 d PD . . F8 F 0.9318 0.0042 0.3851 0.250 Uiso 0.50 1 d PD . . F9 F 1.0214 0.0000 0.5625 0.250 Uiso 0.50 1 d PD . . F10 F 1.0693 0.0291 0.4572 0.250 Uiso 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.119(12) 0.083(11) 0.056(7) 0.000 0.028(7) 0.000 Ag2 0.143(10) 0.081(8) 0.060(6) -0.001(6) 0.031(6) 0.000(9) Ag3 0.186(18) 0.080(12) 0.048(7) 0.000 0.024(10) 0.000 S1 0.06(2) 0.07(2) 0.12(3) -0.02(2) 0.01(2) 0.00(2) S2 0.07(2) 0.07(2) 0.08(2) -0.009(19) 0.026(17) 0.00(2) S3 0.09(2) 0.08(3) 0.080(19) 0.01(2) 0.034(17) 0.01(2) S4 0.10(3) 0.09(3) 0.12(3) 0.03(3) 0.00(3) -0.01(3) N1 0.06(6) 0.06(6) 0.07(6) -0.04(5) 0.01(5) 0.01(6) C1 0.07(9) 0.08(10) 0.07(8) -0.01(7) 0.00(7) 0.01(8) C2 0.07(8) 0.17(18) 0.10(8) -0.01(10) 0.06(6) -0.01(10) C3 0.13(10) 0.20(19) 0.09(8) 0.04(10) 0.07(7) 0.05(12) C4 0.10(11) 0.14(15) 0.09(10) -0.03(10) 0.03(9) 0.01(11) C5 0.06(7) 0.13(12) 0.08(7) -0.05(8) 0.03(6) -0.01(8) C6 0.08(10) 0.09(12) 0.23(19) -0.06(12) 0.04(11) 0.00(10) C7 0.13(15) 0.05(10) 0.4(3) 0.00(16) 0.08(18) 0.04(11) C9 0.4(3) 0.08(14) 0.3(2) 0.02(16) 0.20(19) 0.0(2) C10 0.24(16) 0.06(9) 0.19(14) -0.02(9) 0.11(12) 0.07(10) C11 0.09(9) 0.06(9) 0.10(9) -0.01(8) 0.04(8) 0.01(8) N2 0.05(6) 0.07(7) 0.06(5) 0.03(5) 0.00(5) 0.02(6) C12 0.04(7) 0.09(9) 0.05(6) 0.00(6) 0.00(6) 0.02(7) C13 0.05(7) 0.09(10) 0.07(8) -0.02(7) 0.02(6) 0.02(7) C14 0.06(9) 0.14(15) 0.07(9) -0.01(10) -0.01(8) 0.03(10) C15 0.12(12) 0.15(16) 0.09(9) 0.05(10) 0.05(9) 0.02(12) C16 0.07(8) 0.09(11) 0.12(10) 0.03(9) 0.04(8) 0.00(8) N3 0.07(6) 0.07(7) 0.07(6) -0.01(6) 0.02(5) -0.02(6) C17 0.06(8) 0.10(11) 0.13(12) -0.04(9) 0.03(8) 0.02(8) C18 0.14(13) 0.09(10) 0.08(9) -0.01(8) 0.03(9) 0.04(10) C19 0.11(9) 0.15(14) 0.07(7) 0.05(9) 0.05(6) 0.04(11) C20 0.10(10) 0.08(9) 0.05(6) 0.04(6) 0.02(7) 0.03(9) C21 0.06(8) 0.05(7) 0.07(7) -0.01(6) -0.02(7) 0.00(7) C22 0.10(11) 0.07(10) 0.23(18) 0.05(11) 0.08(11) 0.02(9) C23 0.2(2) 0.09(12) 0.2(2) 0.04(13) 0.05(17) -0.08(13) C24 0.2(2) 0.2(2) 0.4(3) 0.20(18) 0.1(2) 0.0(2) C25 0.24(18) 0.19(18) 0.16(17) 0.08(15) -0.13(15) -0.15(14) C26 0.05(11) 0.2(2) 0.4(4) 0.0(2) -0.01(17) -0.05(12) C27 0.13(16) 0.09(13) 0.19(19) 0.05(13) 0.00(15) -0.03(12) N4 0.08(7) 0.12(9) 0.07(6) 0.05(6) 0.00(6) -0.02(8) C28 0.07(9) 0.13(12) 0.07(8) 0.06(8) 0.01(7) -0.02(9) C29 0.15(15) 0.2(2) 0.09(9) 0.07(12) 0.04(10) -0.02(17) C30 0.16(12) 0.5(3) 0.07(8) -0.08(14) 0.07(8) -0.21(15) C31 0.08(11) 0.2(3) 0.06(8) -0.01(12) 0.03(8) -0.01(14) C32 0.06(9) 0.13(13) 0.06(8) 0.02(8) 0.00(7) -0.01(9) B1 0.09(10) 0.03(7) 0.09(10) 0.02(7) 0.03(8) -0.03(7) F1 0.13(8) 0.06(6) 0.26(14) -0.02(7) 0.06(8) -0.01(6) F2 0.19(7) 0.20(12) 0.21(9) -0.07(9) 0.14(6) -0.10(8) F3 0.09(7) 0.2(2) 0.8(5) 0.0(3) 0.13(14) -0.05(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 2.22(6) 2_756 ? Ag1 N1 2.22(6) . ? Ag2 N3 2.19(4) . ? Ag2 N2 2.20(4) . ? Ag3 N4 2.15(6) 2_657 ? Ag3 N4 2.15(6) . ? S1 C5 1.72(9) . ? S1 C6 1.75(12) . ? S2 C12 1.72(6) . ? S2 C11 1.76(10) . ? S3 C21 1.73(7) . ? S3 C22 1.76(7) . ? S4 C28 1.73(10) . ? S4 C27 1.74(13) . ? N1 C1 1.3900 . ? N1 C5 1.3900 . ? C1 C2 1.3900 . ? C1 H1 0.9300 . ? C2 C3 1.3900 . ? C2 H2 0.9300 . ? C3 C4 1.3900 . ? C3 H3 0.9300 . ? C4 C5 1.3900 . ? C4 H4 0.9300 . ? C6 C7 1.53(15) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.54(15) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.52(18) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.55(15) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.54(13) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? N2 C12 1.3900 . ? N2 C16 1.3900 . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C13 H13 0.9300 . ? C14 C15 1.3900 . ? C14 H14 0.9300 . ? C15 C16 1.3900 . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? N3 C21 1.3900 . ? N3 C17 1.3902 . ? C17 C18 1.3900 . ? C17 H17 0.9300 . ? C18 C19 1.3900 . ? C18 H18 0.9300 . ? C19 C20 1.3900 . ? C19 H19 0.9300 . ? C20 C21 1.3901 . ? C20 H20 0.9300 . ? C22 C23 1.54(13) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.54(15) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.53(15) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.54(16) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.56(14) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? N4 C28 1.3900 . ? N4 C32 1.3900 . ? C28 C29 1.3900 . ? C29 C30 1.3900 . ? C29 H29 0.9300 . ? C30 C31 1.3900 . ? C30 H30 0.9300 . ? C31 C32 1.3900 . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? B1 F3 1.32(11) . ? B1 F1 1.35(10) . ? B1 F4 1.37(11) . ? B1 F2 1.39(12) . ? B2 F5 1.3762(7) 2_757 ? B2 F5 1.3762(7) . ? B2 F6 1.3797(7) . ? B2 F6 1.3797(7) 2_757 ? B3 F9 0.41256(19) 2_756 ? B3 B3 1.0111(7) 2_756 ? B3 F8 1.2057(6) . ? B3 F9 1.3411(9) . ? B3 F7 1.3522(9) 2_756 ? B3 F7 1.3997(9) . ? B3 F10 1.4539(10) . ? B3 F10 1.6958(8) 2_756 ? F7 F7 0.3766(3) 2_756 ? F7 B3 1.3522(9) 2_756 ? F7 F10 1.6781(7) . ? F7 F9 1.7193(11) . ? F8 F9 0.9146(5) 2_756 ? F9 B3 0.41256(19) 2_756 ? F9 F8 0.9146(5) 2_756 ? F9 F9 1.6130(11) 2_756 ? F9 F10 1.6195(10) 2_756 ? F10 F9 1.6195(10) 2_756 ? F10 B3 1.6958(8) 2_756 ? 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 176(4) 2_756 . ? N3 Ag2 N2 176(2) . . ? N4 Ag3 N4 177(4) 2_657 . ? C5 S1 C6 97(6) . . ? C12 S2 C11 106(5) . . ? C21 S3 C22 102(4) . . ? C28 S4 C27 100(7) . . ? C1 N1 C5 120.0 . . ? C1 N1 Ag1 122(3) . . ? C5 N1 Ag1 117(3) . . ? C2 C1 N1 120.0 . . ? C2 C1 H1 120.0 . . ? N1 C1 H1 120.0 . . ? C1 C2 C3 120.00(5) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C4 C3 C2 120.0 . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 120.0 . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 N1 120.0 . . ? C4 C5 S1 127(4) . . ? N1 C5 S1 113(4) . . ? C7 C6 S1 108(9) . . ? C7 C6 H6A 110.0 . . ? S1 C6 H6A 110.0 . . ? C7 C6 H6B 110.0 . . ? S1 C6 H6B 110.0 . . ? H6A C6 H6B 108.4 . . ? C6 C7 C8 103(9) . . ? C6 C7 H7A 111.2 . . ? C8 C7 H7A 111.2 . . ? C6 C7 H7B 111.2 . . ? C8 C7 H7B 111.2 . . ? H7A C7 H7B 109.1 . . ? C9 C8 C7 105(10) . . ? C9 C8 H8A 110.7 . . ? C7 C8 H8A 110.7 . . ? C9 C8 H8B 110.7 . . ? C7 C8 H8B 110.7 . . ? H8A C8 H8B 108.8 . . ? C8 C9 C10 116(10) . . ? C8 C9 H9A 108.2 . . ? C10 C9 H9A 108.2 . . ? C8 C9 H9B 108.2 . . ? C10 C9 H9B 108.2 . . ? H9A C9 H9B 107.4 . . ? C11 C10 C9 125(10) . . ? C11 C10 H10A 106.1 . . ? C9 C10 H10A 106.1 . . ? C11 C10 H10B 106.1 . . ? C9 C10 H10B 106.1 . . ? H10A C10 H10B 106.3 . . ? C10 C11 S2 114(8) . . ? C10 C11 H11A 108.8 . . ? S2 C11 H11A 108.8 . . ? C10 C11 H11B 108.8 . . ? S2 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? C12 N2 C16 120.0 . . ? C12 N2 Ag2 115.3(13) . . ? C16 N2 Ag2 124.0(12) . . ? N2 C12 C13 120.0 . . ? N2 C12 S2 116(2) . . ? C13 C12 S2 124(2) . . ? C12 C13 C14 120.0 . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C15 C14 C13 120.0 . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 120.0 . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 N2 120.0 . . ? C15 C16 H16 120.0 . . ? N2 C16 H16 120.0 . . ? C21 N3 C17 120.0 . . ? C21 N3 Ag2 118.1(12) . . ? C17 N3 Ag2 121.4(12) . . ? C18 C17 N3 120.0 . . ? C18 C17 H17 120.0 . . ? N3 C17 H17 120.0 . . ? C17 C18 C19 120.0 . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C20 C19 C18 120.0 . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C21 120.0 . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? N3 C21 C20 120.0 . . ? N3 C21 S3 113.2(17) . . ? C20 C21 S3 126.8(17) . . ? C23 C22 S3 113(6) . . ? C23 C22 H22A 108.9 . . ? S3 C22 H22A 108.9 . . ? C23 C22 H22B 108.9 . . ? S3 C22 H22B 108.9 . . ? H22A C22 H22B 107.7 . . ? C24 C23 C22 103(8) . . ? C24 C23 H23A 111.1 . . ? C22 C23 H23A 111.1 . . ? C24 C23 H23B 111.1 . . ? C22 C23 H23B 111.1 . . ? H23A C23 H23B 109.1 . . ? C25 C24 C23 107(10) . . ? C25 C24 H24A 110.3 . . ? C23 C24 H24A 110.3 . . ? C25 C24 H24B 110.3 . . ? C23 C24 H24B 110.3 . . ? H24A C24 H24B 108.5 . . ? C24 C25 C26 102(9) . . ? C24 C25 H25A 111.4 . . ? C26 C25 H25A 111.4 . . ? C24 C25 H25B 111.4 . . ? C26 C25 H25B 111.4 . . ? H25A C25 H25B 109.3 . . ? C25 C26 C27 99(10) . . ? C25 C26 H26A 111.9 . . ? C27 C26 H26A 111.9 . . ? C25 C26 H26B 111.9 . . ? C27 C26 H26B 111.9 . . ? H26A C26 H26B 109.6 . . ? C26 C27 S4 112(9) . . ? C26 C27 H27A 109.1 . . ? S4 C27 H27A 109.1 . . ? C26 C27 H27B 109.1 . . ? S4 C27 H27B 109.1 . . ? H27A C27 H27B 107.9 . . ? C28 N4 C32 120.0 . . ? C28 N4 Ag3 118(4) . . ? C32 N4 Ag3 122(4) . . ? N4 C28 C29 120.0 . . ? N4 C28 S4 114(5) . . ? C29 C28 S4 126(5) . . ? C28 C29 C30 120.0 . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C31 C30 C29 120.0 . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C30 C31 C32 120.0 . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C31 C32 N4 120.0 . . ? C31 C32 H32 120.0 . . ? N4 C32 H32 120.0 . . ? F3 B1 F1 114(8) . . ? F3 B1 F4 110(9) . . ? F1 B1 F4 110(8) . . ? F3 B1 F2 111(9) . . ? F1 B1 F2 106(9) . . ? F4 B1 F2 105(8) . . ? F5 B2 F5 112.95(5) 2_757 . ? F5 B2 F6 120.62(3) 2_757 . ? F5 B2 F6 106.61(4) . . ? F5 B2 F6 106.61(4) 2_757 2_757 ? F5 B2 F6 120.62(3) . 2_757 ? F6 B2 F6 87.91(6) . 2_757 ? F9 B3 B3 136.59(3) 2_756 2_756 ? F9 B3 F8 37.681(17) 2_756 . ? B3 B3 F8 149.131(15) 2_756 . ? F9 B3 F9 124.89(4) 2_756 . ? B3 B3 F9 12.203(12) 2_756 . ? F8 B3 F9 145.042(18) . . ? F9 B3 F7 149.096(13) 2_756 2_756 ? B3 B3 F7 70.97(2) 2_756 2_756 ? F8 B3 F7 112.073(16) . 2_756 ? F9 B3 F7 83.17(3) . 2_756 ? F9 B3 F7 157.431(7) 2_756 . ? B3 B3 F7 65.96(2) 2_756 . ? F8 B3 F7 124.380(12) . . ? F9 B3 F7 77.67(3) . . ? F7 B3 F7 15.608(14) 2_756 . ? F9 B3 F10 106.40(2) 2_756 . ? B3 B3 F10 84.92(3) 2_756 . ? F8 B3 F10 125.42(4) . . ? F9 B3 F10 85.12(3) . . ? F7 B3 F10 86.890(13) 2_756 . ? F7 B3 F10 72.010(11) . . ? F9 B3 F10 112.48(4) 2_756 2_756 ? B3 B3 F10 58.65(4) 2_756 2_756 ? F8 B3 F10 93.60(6) . 2_756 ? F9 B3 F10 63.19(5) . 2_756 ? F7 B3 F10 65.687(14) 2_756 2_756 ? F7 B3 F10 76.53(2) . 2_756 ? F10 B3 F10 139.31(2) . 2_756 ? F7 F7 B3 89.380(6) 2_756 2_756 ? F7 F7 B3 75.012(13) 2_756 . ? B3 F7 B3 43.07(4) 2_756 . ? F7 F7 F10 127.59(3) 2_756 . ? B3 F7 F10 67.06(4) 2_756 . ? B3 F7 F10 55.49(4) . . ? F7 F7 F9 94.346(7) 2_756 . ? B3 F7 F9 7.079(5) 2_756 . ? B3 F7 F9 49.65(4) . . ? F10 F7 F9 67.69(4) . . ? F9 F8 B3 16.005(12) 2_756 . ? B3 F9 F8 126.31(3) 2_756 2_756 ? B3 F9 B3 31.203(15) 2_756 . ? F8 F9 B3 142.015(16) 2_756 . ? B3 F9 F9 43.00(3) 2_756 2_756 ? F8 F9 F9 146.637(13) 2_756 2_756 ? B3 F9 F9 12.110(12) . 2_756 ? B3 F9 F10 59.458(14) 2_756 2_756 ? F8 F9 F10 136.25(3) 2_756 2_756 ? B3 F9 F10 69.158(19) . 2_756 ? F9 F9 F10 71.66(2) 2_756 2_756 ? B3 F9 F7 23.824(8) 2_756 . ? F8 F9 F7 103.14(2) 2_756 . ? B3 F9 F7 52.687(12) . . ? F9 F9 F7 64.80(2) 2_756 . ? F10 F9 F7 70.601(16) 2_756 . ? B3 F10 F9 14.145(11) . 2_756 ? B3 F10 F7 52.50(3) . . ? F9 F10 F7 65.63(4) 2_756 . ? B3 F10 B3 36.43(2) . 2_756 ? F9 F10 B3 47.65(3) 2_756 2_756 ? F7 F10 B3 47.25(3) . 2_756 ? 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 151(4) 2_756 . . . ? N1 Ag1 N1 C5 -22(3) 2_756 . . . ? C5 N1 C1 C2 0.0 . . . . ? Ag1 N1 C1 C2 -173(3) . . . . ? N1 C1 C2 C3 0.0 . . . . ? C1 C2 C3 C4 0.0 . . . . ? C2 C3 C4 C5 0.0 . . . . ? C3 C4 C5 N1 0.0 . . . . ? C3 C4 C5 S1 -176(6) . . . . ? C1 N1 C5 C4 0.0 . . . . ? Ag1 N1 C5 C4 173(3) . . . . ? C1 N1 C5 S1 176(5) . . . . ? Ag1 N1 C5 S1 -11(5) . . . . ? C6 S1 C5 C4 -44(6) . . . . ? C6 S1 C5 N1 140(6) . . . . ? C5 S1 C6 C7 -74(12) . . . . ? S1 C6 C7 C8 -156(12) . . . . ? C6 C7 C8 C9 -107(14) . . . . ? C7 C8 C9 C10 -162(11) . . . . ? C8 C9 C10 C11 110(17) . . . . ? C9 C10 C11 S2 171(14) . . . . ? C12 S2 C11 C10 61(12) . . . . ? N3 Ag2 N2 C12 78(33) . . . . ? N3 Ag2 N2 C16 -93(33) . . . . ? C16 N2 C12 C13 0.0 . . . . ? Ag2 N2 C12 C13 -170.7(12) . . . . ? C16 N2 C12 S2 178(2) . . . . ? Ag2 N2 C12 S2 7(2) . . . . ? C11 S2 C12 N2 -136(4) . . . . ? C11 S2 C12 C13 41(5) . . . . ? N2 C12 C13 C14 0.0 . . . . ? S2 C12 C13 C14 -177(3) . . . . ? C12 C13 C14 C15 0.0 . . . . ? C13 C14 C15 C16 0.0 . . . . ? C14 C15 C16 N2 0.0 . . . . ? C12 N2 C16 C15 0.0 . . . . ? Ag2 N2 C16 C15 169.8(13) . . . . ? N2 Ag2 N3 C21 -29(34) . . . . ? N2 Ag2 N3 C17 158(32) . . . . ? C21 N3 C17 C18 0.0 . . . . ? Ag2 N3 C17 C18 172.2(13) . . . . ? N3 C17 C18 C19 0.0 . . . . ? C17 C18 C19 C20 0.0 . . . . ? C18 C19 C20 C21 0.0 . . . . ? C17 N3 C21 C20 0.0 . . . . ? Ag2 N3 C21 C20 -172.5(12) . . . . ? C17 N3 C21 S3 180(2) . . . . ? Ag2 N3 C21 S3 7(2) . . . . ? C19 C20 C21 N3 0.0 . . . . ? C19 C20 C21 S3 -180(3) . . . . ? C22 S3 C21 N3 -133.6(16) . . . . ? C22 S3 C21 C20 46(4) . . . . ? C21 S3 C22 C23 63(10) . . . . ? S3 C22 C23 C24 164(14) . . . . ? C22 C23 C24 C25 -179(17) . . . . ? C23 C24 C25 C26 -175(20) . . . . ? C24 C25 C26 C27 -174(18) . . . . ? C25 C26 C27 S4 -169(13) . . . . ? C28 S4 C27 C26 -71(14) . . . . ? N4 Ag3 N4 C28 -19(4) 2_657 . . . ? N4 Ag3 N4 C32 152(4) 2_657 . . . ? C32 N4 C28 C29 0.0 . . . . ? Ag3 N4 C28 C29 171(3) . . . . ? C32 N4 C28 S4 175(6) . . . . ? Ag3 N4 C28 S4 -14(6) . . . . ? C27 S4 C28 N4 141(6) . . . . ? C27 S4 C28 C29 -45(6) . . . . ? N4 C28 C29 C30 0.0 . . . . ? S4 C28 C29 C30 -174(7) . . . . ? C28 C29 C30 C31 0.0 . . . . ? C29 C30 C31 C32 0.0 . . . . ? C30 C31 C32 N4 0.0 . . . . ? C28 N4 C32 C31 0.0 . . . . ? Ag3 N4 C32 C31 -171(4) . . . . ? F9 B3 F7 F7 72.338(16) 2_756 . . 2_756 ? B3 B3 F7 F7 -105.662(17) 2_756 . . 2_756 ? F8 B3 F7 F7 40.81(3) . . . 2_756 ? F9 B3 F7 F7 -109.294(19) . . . 2_756 ? F10 B3 F7 F7 161.880(16) . . . 2_756 ? F10 B3 F7 F7 -44.28(3) 2_756 . . 2_756 ? F9 B3 F7 B3 178.000(8) 2_756 . . 2_756 ? F8 B3 F7 B3 146.469(16) . . . 2_756 ? F9 B3 F7 B3 -3.632(3) . . . 2_756 ? F7 B3 F7 B3 105.662(17) 2_756 . . 2_756 ? F10 B3 F7 B3 -92.46(3) . . . 2_756 ? F10 B3 F7 B3 61.38(4) 2_756 . . 2_756 ? F9 B3 F7 F10 -89.54(3) 2_756 . . . ? B3 B3 F7 F10 92.46(3) 2_756 . . . ? F8 B3 F7 F10 -121.07(4) . . . . ? F9 B3 F7 F10 88.83(3) . . . . ? F7 B3 F7 F10 -161.880(16) 2_756 . . . ? F10 B3 F7 F10 153.841(14) 2_756 . . . ? F9 B3 F7 F9 -178.369(7) 2_756 . . . ? B3 B3 F7 F9 3.632(3) 2_756 . . . ? F8 B3 F7 F9 150.101(14) . . . . ? F7 B3 F7 F9 109.294(19) 2_756 . . . ? F10 B3 F7 F9 -88.83(3) . . . . ? F10 B3 F7 F9 65.01(4) 2_756 . . . ? B3 B3 F8 F9 -98.65(3) 2_756 . . 2_756 ? F9 B3 F8 F9 -77.37(4) . . . 2_756 ? F7 B3 F8 F9 171.769(5) 2_756 . . 2_756 ? F7 B3 F8 F9 160.831(13) . . . 2_756 ? F10 B3 F8 F9 69.26(2) . . . 2_756 ? F10 B3 F8 F9 -123.043(15) 2_756 . . 2_756 ? F9 B3 F9 B3 -164.881(15) 2_756 . . 2_756 ? F8 B3 F9 B3 -118.23(3) . . . 2_756 ? F7 B3 F9 B3 1.064(1) 2_756 . . 2_756 ? F7 B3 F9 B3 15.882(14) . . . 2_756 ? F10 B3 F9 B3 88.506(17) . . . 2_756 ? F10 B3 F9 B3 -65.102(12) 2_756 . . 2_756 ? F9 B3 F9 F8 120.009(13) 2_756 . . 2_756 ? B3 B3 F9 F8 -75.11(3) 2_756 . . 2_756 ? F8 B3 F9 F8 166.661(7) . . . 2_756 ? F7 B3 F9 F8 -74.05(3) 2_756 . . 2_756 ? F7 B3 F9 F8 -59.228(13) . . . 2_756 ? F10 B3 F9 F8 13.396(11) . . . 2_756 ? F10 B3 F9 F8 -140.21(3) 2_756 . . 2_756 ? B3 B3 F9 F9 164.881(15) 2_756 . . 2_756 ? F8 B3 F9 F9 46.652(19) . . . 2_756 ? F7 B3 F9 F9 165.945(14) 2_756 . . 2_756 ? F7 B3 F9 F9 -179.237(3) . . . 2_756 ? F10 B3 F9 F9 -106.613(6) . . . 2_756 ? F10 B3 F9 F9 99.78(2) 2_756 . . 2_756 ? F9 B3 F9 F10 -99.78(2) 2_756 . . 2_756 ? B3 B3 F9 F10 65.102(12) 2_756 . . 2_756 ? F8 B3 F9 F10 -53.13(4) . . . 2_756 ? F7 B3 F9 F10 66.166(11) 2_756 . . 2_756 ? F7 B3 F9 F10 80.98(2) . . . 2_756 ? F10 B3 F9 F10 153.61(2) . . . 2_756 ? F9 B3 F9 F7 179.237(3) 2_756 . . . ? B3 B3 F9 F7 -15.882(14) 2_756 . . . ? F8 B3 F9 F7 -134.111(19) . . . . ? F7 B3 F9 F7 -14.819(14) 2_756 . . . ? F10 B3 F9 F7 72.624(6) . . . . ? F10 B3 F9 F7 -80.98(2) 2_756 . . . ? F7 F7 F9 B3 45.57(2) 2_756 . . 2_756 ? B3 F7 F9 B3 -20.548(8) . . . 2_756 ? F10 F7 F9 B3 -83.49(5) . . . 2_756 ? F7 F7 F9 F8 -146.78(2) 2_756 . . 2_756 ? B3 F7 F9 F8 167.658(3) 2_756 . . 2_756 ? B3 F7 F9 F8 147.110(11) . . . 2_756 ? F10 F7 F9 F8 84.16(5) . . . 2_756 ? F7 F7 F9 B3 66.115(17) 2_756 . . . ? B3 F7 F9 B3 20.548(8) 2_756 . . . ? F10 F7 F9 B3 -62.95(4) . . . . ? F7 F7 F9 F9 66.292(17) 2_756 . . 2_756 ? B3 F7 F9 F9 20.725(8) 2_756 . . 2_756 ? B3 F7 F9 F9 0.2 . . . 2_756 ? F10 F7 F9 F9 -62.77(4) . . . 2_756 ? F7 F7 F9 F10 -12.003(11) 2_756 . . 2_756 ? B3 F7 F9 F10 -57.57(3) 2_756 . . 2_756 ? B3 F7 F9 F10 -78.12(3) . . . 2_756 ? F10 F7 F9 F10 -141.06(2) . . . 2_756 ? B3 B3 F10 F9 137.23(3) 2_756 . . 2_756 ? F8 B3 F10 F9 -36.58(2) . . . 2_756 ? F9 B3 F10 F9 124.98(4) . . . 2_756 ? F7 B3 F10 F9 -151.611(9) 2_756 . . 2_756 ? F7 B3 F10 F9 -156.418(6) . . . 2_756 ? F10 B3 F10 F9 162.465(7) 2_756 . . 2_756 ? F9 B3 F10 F7 156.418(6) 2_756 . . . ? B3 B3 F10 F7 -66.35(2) 2_756 . . . ? F8 B3 F10 F7 119.842(18) . . . . ? F9 B3 F10 F7 -78.60(4) . . . . ? F7 B3 F10 F7 4.807(3) 2_756 . . . ? F10 B3 F10 F7 -41.117(2) 2_756 . . . ? F9 B3 F10 B3 -137.23(3) 2_756 . . 2_756 ? F8 B3 F10 B3 -173.809(6) . . . 2_756 ? F9 B3 F10 B3 -12.248(12) . . . 2_756 ? F7 B3 F10 B3 71.16(2) 2_756 . . 2_756 ? F7 B3 F10 B3 66.35(2) . . . 2_756 ? F10 B3 F10 B3 25.23(2) 2_756 . . 2_756 ? F7 F7 F10 B3 -22.282(13) 2_756 . . . ? B3 F7 F10 B3 47.80(3) 2_756 . . . ? F9 F7 F10 B3 55.44(3) . . . . ? F7 F7 F10 F9 -16.120(9) 2_756 . . 2_756 ? B3 F7 F10 F9 53.97(3) 2_756 . . 2_756 ? B3 F7 F10 F9 6.162(4) . . . 2_756 ? F9 F7 F10 F9 61.61(3) . . . 2_756 ? F7 F7 F10 B3 -70.09(4) 2_756 . . 2_756 ? B3 F7 F10 B3 -47.80(3) . . . 2_756 ? F9 F7 F10 B3 7.641(4) . . . 2_756 ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 0.745 _refine_diff_density_min -0.509 _refine_diff_density_rms 0.101 data_021202d _database_code_depnum_ccdc_archive 'CCDC 223565' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H20 Ag F6 N2 P S2' _chemical_formula_weight 557.30 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 13.731(3) _cell_length_b 19.097(4) _cell_length_c 8.870(2) _cell_angle_alpha 90.00 _cell_angle_beta 113.614(5) _cell_angle_gamma 90.00 _cell_volume 2131.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 890 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 19.56 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.737 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 1.272 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.853219 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 5016 _diffrn_reflns_av_R_equivalents 0.0573 _diffrn_reflns_av_sigmaI/netI 0.0935 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 26.41 _reflns_number_total 2169 _reflns_number_gt 1114 _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^)+(0.0810P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0005(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2169 _refine_ls_number_parameters 130 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1323 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1606 _refine_ls_wR_factor_gt 0.1157 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 0.964 _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 0.55406(4) 0.7500 0.0733(4) Uani 1 2 d S . . S1 S 0.41471(14) 0.42808(9) 0.8831(2) 0.0628(6) Uani 1 1 d . . . N1 N 0.3362(4) 0.5477(3) 0.7452(6) 0.0534(13) Uani 1 1 d . . . C1 C 0.2612(6) 0.5969(4) 0.6801(9) 0.070(2) Uani 1 1 d . . . H1 H 0.2811 0.6397 0.6512 0.084 Uiso 1 1 calc R . . C2 C 0.1580(7) 0.5873(5) 0.6544(10) 0.086(2) Uani 1 1 d . . . H2 H 0.1083 0.6229 0.6117 0.103 Uiso 1 1 calc R . . C3 C 0.1286(7) 0.5217(6) 0.6945(11) 0.092(3) Uani 1 1 d . . . H3 H 0.0576 0.5124 0.6722 0.110 Uiso 1 1 calc R . . C4 C 0.2044(6) 0.4713(4) 0.7666(10) 0.078(2) Uani 1 1 d . . . H4 H 0.1862 0.4286 0.7985 0.093 Uiso 1 1 calc R . . C5 C 0.3083(5) 0.4854(3) 0.7907(8) 0.0533(16) Uani 1 1 d . . . C6 C 0.3565(6) 0.3420(3) 0.8166(9) 0.073(2) Uani 1 1 d . . . H6A H 0.4101 0.3067 0.8699 0.087 Uiso 1 1 calc R . . H6B H 0.2993 0.3352 0.8531 0.087 Uiso 1 1 calc R . . C7 C 0.3136(6) 0.3308(4) 0.6342(9) 0.071(2) Uani 1 1 d . . . H7A H 0.3683 0.3419 0.5948 0.086 Uiso 1 1 calc R . . H7B H 0.2542 0.3622 0.5805 0.086 Uiso 1 1 calc R . . C8 C 0.2774(6) 0.2559(4) 0.5896(9) 0.078(2) Uani 1 1 d . . . H8A H 0.3388 0.2253 0.6332 0.094 Uiso 1 1 calc R . . H8B H 0.2298 0.2433 0.6416 0.094 Uiso 1 1 calc R . . P1 P 0.5000 0.21776(13) 0.2500 0.0649(8) Uani 1 2 d S . . F1 F 0.3787(4) 0.2174(2) 0.1297(7) 0.1071(17) Uani 1 1 d . . . F2 F 0.5000 0.2960(3) 0.2500 0.208(6) Uani 1 2 d S . . F3 F 0.5273(5) 0.2130(4) 0.0960(8) 0.154(3) Uani 1 1 d . . . F4 F 0.5000 0.1357(4) 0.2500 0.137(3) 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 0.0640(6) 0.0604(6) 0.1077(9) 0.000 0.0473(5) 0.000 S1 0.0626(12) 0.0575(11) 0.0648(13) -0.0017(8) 0.0217(10) -0.0043(8) N1 0.053(3) 0.054(3) 0.051(4) -0.003(3) 0.019(3) 0.000(3) C1 0.070(5) 0.072(5) 0.067(5) 0.002(4) 0.025(4) 0.011(4) C2 0.071(6) 0.105(7) 0.076(6) 0.010(5) 0.024(5) 0.027(5) C3 0.053(5) 0.130(8) 0.092(7) -0.003(6) 0.030(5) 0.000(5) C4 0.064(5) 0.088(6) 0.083(6) 0.006(5) 0.032(5) -0.010(4) C5 0.053(4) 0.062(4) 0.045(4) -0.004(3) 0.019(3) -0.007(3) C6 0.087(6) 0.052(4) 0.072(6) -0.004(4) 0.025(5) -0.012(4) C7 0.078(5) 0.061(4) 0.070(6) -0.010(4) 0.025(4) -0.014(4) C8 0.091(6) 0.066(5) 0.077(5) -0.009(4) 0.033(5) -0.012(4) P1 0.0537(17) 0.0561(17) 0.077(2) 0.000 0.0179(16) 0.000 F1 0.062(3) 0.120(4) 0.114(4) -0.009(3) 0.008(3) 0.010(3) F2 0.182(9) 0.044(4) 0.247(12) 0.000 -0.073(8) 0.000 F3 0.097(5) 0.260(8) 0.114(5) 0.002(5) 0.052(4) -0.024(4) F4 0.133(7) 0.081(5) 0.160(8) 0.000 0.019(6) 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 2.236(5) . ? Ag1 N1 2.236(5) 2_656 ? S1 C5 1.745(7) . ? S1 C6 1.820(7) . ? N1 C1 1.341(8) . ? N1 C5 1.360(8) . ? C1 C2 1.354(10) . ? C1 H1 0.9300 . ? C2 C3 1.405(12) . ? C2 H2 0.9300 . ? C3 C4 1.373(11) . ? C3 H3 0.9300 . ? C4 C5 1.381(9) . ? C4 H4 0.9300 . ? C6 C7 1.499(10) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.514(9) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C8 1.478(14) 7_556 ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? P1 F2 1.494(7) . ? P1 F3 1.557(6) 2_655 ? P1 F3 1.557(6) . ? P1 F4 1.568(8) . ? P1 F1 1.577(4) . ? P1 F1 1.578(4) 2_655 ? 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 173.8(3) . 2_656 ? C5 S1 C6 103.8(3) . . ? C1 N1 C5 118.8(6) . . ? C1 N1 Ag1 124.2(5) . . ? C5 N1 Ag1 116.3(4) . . ? N1 C1 C2 123.2(8) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C1 C2 C3 117.8(8) . . ? C1 C2 H2 121.1 . . ? C3 C2 H2 121.1 . . ? C4 C3 C2 120.0(8) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 118.6(8) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? N1 C5 C4 121.4(6) . . ? N1 C5 S1 113.9(5) . . ? C4 C5 S1 124.7(6) . . ? C7 C6 S1 114.2(5) . . ? C7 C6 H6A 108.7 . . ? S1 C6 H6A 108.7 . . ? C7 C6 H6B 108.7 . . ? S1 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? C6 C7 C8 111.2(6) . . ? C6 C7 H7A 109.4 . . ? C8 C7 H7A 109.4 . . ? C6 C7 H7B 109.4 . . ? C8 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? C8 C8 C7 113.4(8) 7_556 . ? C8 C8 H8A 108.9 7_556 . ? C7 C8 H8A 108.9 . . ? C8 C8 H8B 108.9 7_556 . ? C7 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? F2 P1 F3 93.3(3) . 2_655 ? F2 P1 F3 93.3(3) . . ? F3 P1 F3 173.3(6) 2_655 . ? F2 P1 F4 180.000(1) . . ? F3 P1 F4 86.7(3) 2_655 . ? F3 P1 F4 86.7(3) . . ? F2 P1 F1 90.27(19) . . ? F3 P1 F1 91.9(3) 2_655 . ? F3 P1 F1 88.0(3) . . ? F4 P1 F1 89.73(19) . . ? F2 P1 F1 90.27(19) . 2_655 ? F3 P1 F1 88.0(3) 2_655 2_655 ? F3 P1 F1 91.9(3) . 2_655 ? F4 P1 F1 89.73(19) . 2_655 ? F1 P1 F1 179.5(4) . 2_655 ? 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 -152.3(5) 2_656 . . . ? N1 Ag1 N1 C5 18.1(4) 2_656 . . . ? C5 N1 C1 C2 -1.2(10) . . . . ? Ag1 N1 C1 C2 169.0(6) . . . . ? N1 C1 C2 C3 -1.7(12) . . . . ? C1 C2 C3 C4 3.9(13) . . . . ? C2 C3 C4 C5 -3.2(12) . . . . ? C1 N1 C5 C4 2.0(9) . . . . ? Ag1 N1 C5 C4 -169.0(5) . . . . ? C1 N1 C5 S1 -176.8(5) . . . . ? Ag1 N1 C5 S1 12.2(6) . . . . ? C3 C4 C5 N1 0.2(11) . . . . ? C3 C4 C5 S1 178.9(6) . . . . ? C6 S1 C5 N1 -146.1(5) . . . . ? C6 S1 C5 C4 35.1(7) . . . . ? C5 S1 C6 C7 62.6(6) . . . . ? S1 C6 C7 C8 173.9(5) . . . . ? C6 C7 C8 C8 173.0(9) . . . 7_556 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.590 _refine_diff_density_min -0.329 _refine_diff_density_rms 0.106