Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Hannon, M. J.' 'Alcock, N.' 'Hamblin, Jacqueline' 'Jackson, Alexander' _publ_contact_author_name 'Dr M J Hannon' _publ_contact_author_address ; Department of Chemistry University of Warwick Gibbet Hill Road COVENTRY CV4 7AL UK ; _publ_contact_author_email 'M.J.HANNON@WARWICK.AC.UK' _publ_section_title ; Triple Helicates and planar dimers arising from silver(I) coordination to directly linked bis-pyridylimine ligands ; data_febim _database_code_CSD 173888 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H30 F24 Fe2 N16 O8 P4' _chemical_formula_weight 1554.38 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' 'Fe' 'Fe' 0.3463 0.8444 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 22.74680(10) _cell_length_b 41.1307(7) _cell_length_c 13.0308(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12191.5(3) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 6139 _cell_measurement_theta_min 3 _cell_measurement_theta_max 15 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.694 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6192 _exptl_absorpt_coefficient_mu 0.716 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15169 _diffrn_reflns_av_R_equivalents 0.0924 _diffrn_reflns_av_sigmaI/netI 0.0776 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 48 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5165 _reflns_number_gt 4140 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0300P)^2^+225.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(4) _refine_ls_number_reflns 5165 _refine_ls_number_parameters 448 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.1109 _refine_ls_R_factor_gt 0.0809 _refine_ls_wR_factor_ref 0.1739 _refine_ls_wR_factor_gt 0.1547 _refine_ls_goodness_of_fit_ref 1.198 _refine_ls_restrained_S_all 1.198 _refine_ls_shift/su_max 0.135 _refine_ls_shift/su_mean 0.006 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 Fe1 Fe 0.27974(5) 0.21078(3) 1.01003(9) 0.0255(3) Uani 1 1 d . . . N11 N 0.3121(3) 0.24719(15) 0.9360(5) 0.0270(16) Uani 1 1 d . . . C12 C 0.3366(4) 0.2428(2) 0.8495(7) 0.037(2) Uani 1 1 d . . . H12A H 0.3545 0.2596 0.8106 0.044 Uiso 1 1 calc R . . C13 C 0.3342(4) 0.2085(2) 0.8165(7) 0.035(2) Uani 1 1 d . . . N14 N 0.3021(3) 0.18901(16) 0.8807(5) 0.0274(16) Uani 1 1 d . . . C15 C 0.2923(4) 0.1587(2) 0.8486(6) 0.0305(19) Uani 1 1 d . . . H15A H 0.2695 0.1446 0.8904 0.037 Uiso 1 1 calc R . . C16 C 0.3143(4) 0.1470(2) 0.7562(8) 0.040(2) Uani 1 1 d . . . H16A H 0.3064 0.1253 0.7361 0.048 Uiso 1 1 calc R . . C17 C 0.3465(5) 0.1662(3) 0.6952(8) 0.057(3) Uani 1 1 d . . . H17A H 0.3620 0.1581 0.6325 0.069 Uiso 1 1 calc R . . C18 C 0.3570(5) 0.1981(2) 0.7251(8) 0.056(3) Uani 1 1 d . . . H18A H 0.3794 0.2123 0.6831 0.068 Uiso 1 1 calc R . . N21 N 0.2001(3) 0.22154(15) 0.9713(5) 0.0270(15) Uani 1 1 d . . . C22 C 0.1591(4) 0.20180(19) 0.9981(7) 0.032(2) Uani 1 1 d . . . H22A H 0.1186 0.2060 0.9858 0.039 Uiso 1 1 calc R . . C23 C 0.1795(4) 0.1728(2) 1.0483(6) 0.0292(19) Uani 1 1 d . . . N24 N 0.2382(3) 0.17220(16) 1.0655(5) 0.0269(15) Uani 1 1 d . . . C25 C 0.2614(4) 0.1463(2) 1.1121(7) 0.040(2) Uani 1 1 d . . . H25A H 0.3026 0.1456 1.1237 0.048 Uiso 1 1 calc R . . C26 C 0.2266(5) 0.1203(2) 1.1443(7) 0.045(2) Uani 1 1 d . . . H26A H 0.2441 0.1022 1.1776 0.054 Uiso 1 1 calc R . . C27 C 0.1671(5) 0.1210(3) 1.1277(8) 0.051(3) Uani 1 1 d . . . H27A H 0.1430 0.1035 1.1497 0.061 Uiso 1 1 calc R . . C28 C 0.1428(4) 0.1475(2) 1.0784(7) 0.038(2) Uani 1 1 d . . . H28A H 0.1018 0.1484 1.0653 0.046 Uiso 1 1 calc R . . N31 N 0.2718(3) 0.23796(16) 1.1298(5) 0.0303(16) Uani 1 1 d . . . C32 C 0.3134(4) 0.2387(2) 1.1970(7) 0.032(2) Uani 1 1 d . . . H32A H 0.3131 0.2525 1.2556 0.039 Uiso 1 1 calc R . . C33 C 0.3610(4) 0.2163(2) 1.1737(6) 0.032(2) Uani 1 1 d . . . N34 N 0.3546(3) 0.20057(17) 1.0806(5) 0.0302(17) Uani 1 1 d . . . C35 C 0.3971(4) 0.1806(2) 1.0517(7) 0.035(2) Uani 1 1 d . . . H35A H 0.3932 0.1694 0.9883 0.042 Uiso 1 1 calc R . . C36 C 0.4474(4) 0.1754(2) 1.1108(9) 0.045(3) Uani 1 1 d . . . H36A H 0.4774 0.1613 1.0866 0.054 Uiso 1 1 calc R . . C37 C 0.4534(4) 0.1906(2) 1.2036(8) 0.042(2) Uani 1 1 d . . . H37A H 0.4867 0.1868 1.2458 0.051 Uiso 1 1 calc R . . C38 C 0.4096(4) 0.2117(2) 1.2339(7) 0.042(2) Uani 1 1 d . . . H38A H 0.4132 0.2231 1.2970 0.050 Uiso 1 1 calc R . . P1 P -0.04057(14) 0.30852(8) 0.7852(2) 0.0601(9) Uani 1 1 d D . . F11 F -0.0031(3) 0.27592(17) 0.7842(7) 0.099(3) Uani 1 1 d D . . F12 F -0.0776(4) 0.34053(19) 0.7853(7) 0.116(3) Uani 1 1 d D . . F13 F -0.0005(5) 0.3216(2) 0.8717(8) 0.154(5) Uani 1 1 d D . . F14 F -0.0824(4) 0.29346(19) 0.6992(6) 0.105(3) Uani 1 1 d D . . F15 F -0.0823(4) 0.2918(3) 0.8656(8) 0.167(5) Uani 1 1 d D . . F16 F -0.0012(4) 0.3223(2) 0.6981(7) 0.127(4) Uani 1 1 d D . . P2 P 0.13232(11) 0.16957(6) 0.7164(2) 0.0403(6) Uani 1 1 d D . . F21 F 0.1686(3) 0.14040(15) 0.6706(5) 0.072(2) Uani 1 1 d D . . F22 F 0.0953(2) 0.19904(15) 0.7638(6) 0.081(2) Uani 1 1 d D . . F23 F 0.1891(3) 0.19084(15) 0.7255(8) 0.107(4) Uani 1 1 d D . . F24 F 0.0742(3) 0.14864(16) 0.7143(6) 0.089(3) Uani 1 1 d D . . F25 F 0.1448(4) 0.1560(2) 0.8283(5) 0.110(3) Uani 1 1 d D . . F26 F 0.1190(4) 0.1828(2) 0.6078(6) 0.126(4) Uani 1 1 d D . . O11A O -0.0725(5) 0.2085(3) 1.0002(10) 0.076(4) Uani 0.697(15) 1 d P . . O11B O 0.0481(11) 0.2470(6) 0.993(2) 0.064(9) Uiso 0.303(15) 1 d PD . . O12 O 0.0119(5) 0.2096(2) 0.9517(8) 0.096(3) Uani 1 1 d D . . C01 C -0.0296(10) 0.2533(3) 1.0502(11) 0.114(7) Uani 1 1 d D . . N01A N -0.0265(6) 0.2201(4) 0.9966(9) 0.042(3) Uani 0.697(15) 1 d P . . N01B N -0.0012(14) 0.2360(7) 0.996(2) 0.048(8) Uiso 0.303(15) 1 d PD . . O21A O -0.2656(10) 0.1924(6) 0.821(2) 0.246(13) Uani 1.00(2) 1 d P . . O22 O -0.2084(6) 0.1640(4) 0.8391(11) 0.131(5) Uani 1.00(2) 1 d P . . C002 C -0.2921(7) 0.1536(4) 0.9344(14) 0.103(6) Uani 1.00(2) 1 d P . . N002 N -0.2392(12) 0.1706(4) 0.898(2) 0.237(19) Uani 1.00(2) 1 d P . . C03D C -0.2928(17) 0.2562(9) 1.018(4) 0.119(11) Uiso 0.50 1 d P . . C03C C -0.2500 0.2500 1.091(5) 0.103(15) Uiso 0.50 2 d SP . . C03B C -0.2500 0.2500 1.013(5) 0.114(16) Uiso 0.50 2 d SP . . C03A C -0.2845(16) 0.2394(9) 0.932(3) 0.119(12) Uiso 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 Fe1 0.0256(5) 0.0227(5) 0.0283(6) 0.0010(5) 0.0001(5) -0.0008(5) N11 0.023(4) 0.019(3) 0.040(4) 0.002(3) 0.005(3) 0.004(3) C12 0.035(5) 0.029(5) 0.047(6) 0.005(4) 0.020(5) 0.003(4) C13 0.041(5) 0.027(5) 0.038(5) -0.007(4) 0.014(4) 0.010(4) N14 0.023(4) 0.023(4) 0.036(4) 0.003(3) -0.003(3) 0.004(3) C15 0.034(5) 0.025(4) 0.032(5) 0.005(4) -0.003(4) -0.002(4) C16 0.056(6) 0.030(4) 0.035(5) -0.003(4) -0.003(5) 0.004(4) C17 0.073(8) 0.048(6) 0.050(7) -0.001(5) 0.022(6) 0.016(6) C18 0.092(9) 0.025(5) 0.053(6) 0.005(5) 0.037(6) 0.009(5) N21 0.026(4) 0.026(4) 0.029(4) -0.003(3) 0.004(3) -0.001(3) C22 0.022(4) 0.038(5) 0.037(5) 0.000(4) -0.004(4) -0.002(4) C23 0.037(5) 0.023(4) 0.027(4) -0.003(3) 0.006(4) -0.006(4) N24 0.029(4) 0.026(4) 0.025(4) 0.007(3) 0.005(3) 0.006(3) C25 0.041(5) 0.036(5) 0.044(6) 0.004(4) -0.008(5) 0.002(4) C26 0.071(7) 0.021(5) 0.042(6) 0.002(4) -0.003(5) 0.002(5) C27 0.048(6) 0.048(6) 0.057(7) 0.011(5) 0.017(5) -0.014(5) C28 0.050(6) 0.032(5) 0.033(5) 0.005(4) 0.006(4) -0.009(4) N31 0.027(4) 0.029(4) 0.035(4) -0.001(3) 0.000(3) 0.000(3) C32 0.034(5) 0.035(5) 0.028(5) 0.002(4) -0.002(4) 0.007(4) C33 0.029(5) 0.040(5) 0.026(4) 0.004(4) -0.009(4) -0.002(4) N34 0.025(4) 0.030(4) 0.035(4) 0.003(3) -0.002(3) -0.005(3) C35 0.033(5) 0.025(4) 0.046(5) 0.006(4) -0.005(4) 0.004(4) C36 0.021(5) 0.040(5) 0.074(8) 0.016(5) 0.001(5) 0.008(4) C37 0.035(5) 0.050(6) 0.042(6) 0.015(5) -0.015(5) 0.000(5) C38 0.040(5) 0.044(5) 0.041(6) 0.010(4) -0.008(5) -0.004(5) P1 0.067(2) 0.0627(19) 0.0510(19) -0.0075(14) -0.0044(15) 0.0107(16) F11 0.099(6) 0.079(5) 0.119(7) -0.002(5) -0.028(5) 0.023(4) F12 0.132(7) 0.112(7) 0.103(7) -0.039(6) -0.039(6) 0.071(6) F13 0.201(11) 0.091(7) 0.170(10) -0.067(7) -0.125(9) 0.044(7) F14 0.105(6) 0.086(6) 0.126(7) 0.009(5) -0.060(6) -0.012(5) F15 0.143(10) 0.240(14) 0.117(9) 0.058(9) 0.042(8) 0.047(10) F16 0.118(7) 0.114(7) 0.148(9) 0.046(6) 0.056(7) -0.004(6) P2 0.0404(14) 0.0360(13) 0.0446(14) -0.0050(11) -0.0047(12) 0.0007(11) F21 0.077(4) 0.054(4) 0.084(5) -0.007(4) 0.010(4) 0.022(4) F22 0.045(3) 0.065(4) 0.133(7) -0.059(5) 0.004(4) -0.002(3) F23 0.039(4) 0.054(4) 0.229(11) -0.014(6) 0.006(5) 0.001(3) F24 0.061(4) 0.062(4) 0.144(8) -0.046(5) 0.007(4) -0.018(3) F25 0.156(8) 0.111(7) 0.061(5) -0.001(5) -0.009(5) 0.006(6) F26 0.189(10) 0.128(8) 0.061(5) 0.027(5) -0.012(6) 0.072(7) O11A 0.064(8) 0.106(10) 0.059(8) -0.007(7) 0.006(7) -0.024(7) O12 0.120(9) 0.088(7) 0.080(7) -0.014(6) 0.009(7) -0.004(6) C01 0.23(2) 0.051(8) 0.057(8) -0.023(7) 0.001(11) -0.024(11) N01A 0.028(6) 0.066(9) 0.033(7) 0.024(6) 0.006(6) 0.002(7) O21A 0.20(2) 0.22(2) 0.31(3) 0.04(2) 0.08(2) -0.054(19) O22 0.114(10) 0.151(13) 0.128(11) 0.004(10) 0.008(9) 0.012(9) C002 0.080(10) 0.097(12) 0.132(14) 0.053(10) 0.052(10) 0.015(9) N002 0.29(3) 0.070(11) 0.35(4) -0.023(15) 0.29(3) 0.003(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N11 1.928(7) . y Fe1 N31 1.928(7) . y Fe1 N21 1.932(7) . y Fe1 N14 1.975(7) . y Fe1 N34 1.980(7) . y Fe1 N24 1.983(7) . y Fe1 Fe1 37.928(2) 14_545 y N11 C12 1.271(11) . ? N11 N21 1.394(9) 14 ? C12 C13 1.474(12) . ? C13 C18 1.369(13) . ? C13 N14 1.370(11) . ? N14 C15 1.334(10) . ? C15 C16 1.390(13) . ? C16 C17 1.338(14) . ? C17 C18 1.388(14) . ? N21 C22 1.285(10) . ? N21 N11 1.394(9) 14 ? C22 C23 1.437(12) . ? C23 N24 1.354(11) . ? C23 C28 1.390(12) . ? N24 C25 1.335(11) . ? C25 C26 1.395(13) . ? C26 C27 1.371(14) . ? C27 C28 1.380(13) . ? N31 C32 1.291(11) . ? N31 N31 1.401(13) 14 ? C32 C33 1.452(12) . ? C33 C38 1.370(12) . ? C33 N34 1.382(11) . ? N34 C35 1.323(11) . ? C35 C36 1.396(12) . ? C36 C37 1.369(14) . ? C37 C38 1.377(14) . ? P1 F13 1.546(8) . ? P1 F16 1.553(8) . ? P1 F12 1.563(7) . ? P1 F15 1.574(9) . ? P1 F11 1.589(7) . ? P1 F14 1.595(7) . ? P2 F26 1.546(7) . ? P2 F23 1.564(6) . ? P2 F21 1.573(6) . ? P2 F24 1.579(6) . ? P2 F25 1.587(7) . ? P2 F22 1.600(6) . ? O11A N01A 1.150(16) . ? O11B N01B 1.21(3) . ? O12 N01A 1.136(14) . ? O12 N01B 1.26(3) . ? C01 N01B 1.20(3) . ? C01 N01A 1.54(2) . ? N01A N01B 0.87(3) . ? O21A N002 1.48(4) . ? O21A O22 1.77(3) . ? O22 N002 1.080(17) . ? C002 N002 1.47(2) . ? C03D C03B 1.01(4) . ? C03D C03A 1.33(5) . ? C03D C03C 1.39(6) . ? C03D C03D 2.01(8) 14_455 ? C03C C03B 1.02(7) . ? C03C C03D 1.39(6) 14_455 ? C03B C03D 1.01(4) 14_455 ? C03B C03A 1.38(6) 14_455 ? C03B C03A 1.38(6) . ? C03A C03A 1.80(7) 14_455 ? 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 N11 Fe1 N31 89.4(3) . . y N11 Fe1 N21 92.9(3) . . y N31 Fe1 N21 89.4(3) . . y N11 Fe1 N14 80.0(3) . . y N31 Fe1 N14 167.9(3) . . y N21 Fe1 N14 97.0(3) . . y N11 Fe1 N34 93.9(3) . . y N31 Fe1 N34 80.1(3) . . y N21 Fe1 N34 167.4(3) . . y N14 Fe1 N34 94.5(3) . . y N11 Fe1 N24 170.4(3) . . y N31 Fe1 N24 97.1(3) . . y N21 Fe1 N24 80.3(3) . . y N14 Fe1 N24 94.1(3) . . y N34 Fe1 N24 94.0(3) . . y N11 Fe1 Fe1 142.2(2) . 14_545 ? N31 Fe1 Fe1 125.2(2) . 14_545 ? N21 Fe1 Fe1 101.27(19) . 14_545 ? N14 Fe1 Fe1 63.64(19) . 14_545 ? N34 Fe1 Fe1 79.6(2) . 14_545 ? N24 Fe1 Fe1 35.25(19) . 14_545 ? C12 N11 N21 120.8(7) . 14 ? C12 N11 Fe1 120.0(6) . . ? N21 N11 Fe1 118.4(5) 14 . ? N11 C12 C13 112.3(8) . . ? C18 C13 N14 123.4(9) . . ? C18 C13 C12 122.6(9) . . ? N14 C13 C12 113.7(7) . . ? C15 N14 C13 116.5(7) . . ? C15 N14 Fe1 130.4(6) . . ? C13 N14 Fe1 113.1(5) . . ? N14 C15 C16 122.2(8) . . ? C17 C16 C15 120.6(9) . . ? C16 C17 C18 118.9(9) . . ? C13 C18 C17 118.4(9) . . ? C22 N21 N11 121.9(7) . 14 ? C22 N21 Fe1 117.7(6) . . ? N11 N21 Fe1 119.0(5) 14 . ? N21 C22 C23 114.4(7) . . ? N24 C23 C28 122.1(8) . . ? N24 C23 C22 114.2(7) . . ? C28 C23 C22 123.8(8) . . ? C25 N24 C23 118.6(7) . . ? C25 N24 Fe1 128.1(6) . . ? C23 N24 Fe1 113.2(5) . . ? N24 C25 C26 121.7(9) . . ? C27 C26 C25 119.7(9) . . ? C26 C27 C28 119.1(9) . . ? C27 C28 C23 118.8(9) . . ? C32 N31 N31 120.2(7) . 14 ? C32 N31 Fe1 119.6(6) . . ? N31 N31 Fe1 118.5(3) 14 . ? N31 C32 C33 112.9(8) . . ? C38 C33 N34 121.5(8) . . ? C38 C33 C32 124.7(8) . . ? N34 C33 C32 113.7(7) . . ? C35 N34 C33 117.6(7) . . ? C35 N34 Fe1 128.9(6) . . ? C33 N34 Fe1 113.5(5) . . ? N34 C35 C36 122.5(9) . . ? C37 C36 C35 119.9(9) . . ? C36 C37 C38 117.9(9) . . ? C33 C38 C37 120.5(9) . . ? F13 P1 F16 93.8(6) . . ? F13 P1 F12 91.4(4) . . ? F16 P1 F12 90.2(5) . . ? F13 P1 F15 91.3(6) . . ? F16 P1 F15 174.2(6) . . ? F12 P1 F15 92.4(5) . . ? F13 P1 F11 89.0(4) . . ? F16 P1 F11 89.6(5) . . ? F12 P1 F11 179.6(5) . . ? F15 P1 F11 87.7(5) . . ? F13 P1 F14 177.2(5) . . ? F16 P1 F14 88.4(5) . . ? F12 P1 F14 90.4(4) . . ? F15 P1 F14 86.5(5) . . ? F11 P1 F14 89.2(4) . . ? F26 P2 F23 92.0(5) . . ? F26 P2 F21 91.4(4) . . ? F23 P2 F21 91.3(4) . . ? F26 P2 F24 90.6(5) . . ? F23 P2 F24 176.5(5) . . ? F21 P2 F24 90.9(4) . . ? F26 P2 F25 179.0(6) . . ? F23 P2 F25 88.8(5) . . ? F21 P2 F25 89.2(4) . . ? F24 P2 F25 88.5(5) . . ? F26 P2 F22 89.0(5) . . ? F23 P2 F22 89.0(3) . . ? F21 P2 F22 179.5(5) . . ? F24 P2 F22 88.8(3) . . ? F25 P2 F22 90.4(4) . . ? N01A O12 N01B 42.1(14) . . ? N01B C01 N01A 34.4(16) . . ? N01B N01A O12 77(2) . . ? N01B N01A O11A 156(3) . . ? O12 N01A O11A 124.2(17) . . ? N01B N01A C01 51(2) . . ? O12 N01A C01 127.4(15) . . ? O11A N01A C01 107.9(14) . . ? N01A N01B C01 95(3) . . ? N01A N01B O11B 153(3) . . ? C01 N01B O11B 107(3) . . ? N01A N01B O12 61.2(19) . . ? C01 N01B O12 155(3) . . ? O11B N01B O12 95(2) . . ? N002 O21A O22 37.6(10) . . ? N002 O22 O21A 56.8(19) . . ? O22 N002 C002 130(2) . . ? O22 N002 O21A 86(2) . . ? C002 N002 O21A 100(2) . . ? C03B C03D C03A 71(4) . . ? C03B C03D C03C 47(4) . . ? C03A C03D C03C 113(4) . . ? C03B C03D C03D 4(5) . 14_455 ? C03A C03D C03D 74(3) . 14_455 ? C03C C03D C03D 43(3) . 14_455 ? C03B C03C C03D 47(3) . . ? C03B C03C C03D 47(3) . 14_455 ? C03D C03C C03D 93(5) . 14_455 ? C03D C03B C03D 172(10) . 14_455 ? C03D C03B C03C 86(5) . . ? C03D C03B C03C 86(5) 14_455 . ? C03D C03B C03A 121(6) . 14_455 ? C03D C03B C03A 65(4) 14_455 14_455 ? C03C C03B C03A 139(3) . 14_455 ? C03D C03B C03A 65(4) . . ? C03D C03B C03A 121(6) 14_455 . ? C03C C03B C03A 139(3) . . ? C03A C03B C03A 81(5) 14_455 . ? C03D C03A C03B 44(2) . . ? C03D C03A C03A 83(3) . 14_455 ? C03B C03A C03A 49(3) . 14_455 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.739 _refine_diff_density_min -0.604 _refine_diff_density_rms 0.096 data_kezagc _database_code_CSD 173889 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H42 Ag2 F12 N12 P2' _chemical_formula_weight 1220.56 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' '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 12.813(2) _cell_length_b 23.504(2) _cell_length_c 16.140(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.878(5) _cell_angle_gamma 90.00 _cell_volume 4854.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 3 _cell_measurement_theta_max 20 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.670 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2440 _exptl_absorpt_coefficient_mu 0.964 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 0.86 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cooler (Cosier & Glazer, 1986). The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.0 cm. Coverage of the unique set is over 97% complete to at least 26\% in \q. Crystal decay was found to be negligible by by repeating the initial frames at t data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for met atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 14569 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_sigmaI/netI 0.0404 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 28.65 _reflns_number_total 5689 _reflns_number_gt 4169 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.0486P)^2^+7.7619P] 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 5689 _refine_ls_number_parameters 336 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0650 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.1059 _refine_ls_wR_factor_gt 0.0962 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.024232(19) 0.362214(12) -0.386447(16) 0.03836(10) Uani 1 1 d . . . N11 N -0.1022(2) 0.43146(13) -0.44633(17) 0.0432(7) Uani 1 1 d . . . C12 C -0.1442(3) 0.42882(18) -0.5238(2) 0.0505(9) Uani 1 1 d . . . H12A H -0.1042 0.4121 -0.5654 0.061 Uiso 1 1 calc R . . C13 C -0.2426(3) 0.44910(17) -0.5465(2) 0.0515(10) Uani 1 1 d . . . H13A H -0.2693 0.4467 -0.6024 0.062 Uiso 1 1 calc R . . C14 C -0.3004(3) 0.47265(18) -0.4870(3) 0.0556(10) Uani 1 1 d . . . H14A H -0.3691 0.4860 -0.5005 0.067 Uiso 1 1 calc R . . C15 C -0.2579(3) 0.47695(16) -0.4061(2) 0.0464(9) Uani 1 1 d . . . H15A H -0.2966 0.4940 -0.3640 0.056 Uiso 1 1 calc R . . C16 C -0.1584(3) 0.45596(14) -0.3883(2) 0.0345(7) Uani 1 1 d . . . C17 C -0.1081(2) 0.45996(14) -0.30241(19) 0.0326(7) Uani 1 1 d . . . N18 N -0.0223(2) 0.43313(11) -0.28999(15) 0.0301(5) Uani 1 1 d . . . N21 N 0.1865(2) 0.37185(12) -0.44744(16) 0.0359(6) Uani 1 1 d . . . C22 C 0.1962(3) 0.38051(16) -0.5286(2) 0.0457(9) Uani 1 1 d . . . H22A H 0.1346 0.3864 -0.5627 0.055 Uiso 1 1 calc R . . C23 C 0.2911(3) 0.38126(17) -0.5651(2) 0.0522(10) Uani 1 1 d . . . H23A H 0.2942 0.3862 -0.6234 0.063 Uiso 1 1 calc R . . C24 C 0.3797(3) 0.3748(2) -0.5169(3) 0.0641(13) Uani 1 1 d . . . H24A H 0.4462 0.3755 -0.5404 0.077 Uiso 1 1 calc R . . C25 C 0.3712(3) 0.3671(2) -0.4320(3) 0.0597(12) Uani 1 1 d . . . H25A H 0.4323 0.3636 -0.3965 0.072 Uiso 1 1 calc R . . C26 C 0.2738(3) 0.36450(14) -0.3999(2) 0.0352(7) Uani 1 1 d . . . C27 C 0.2612(2) 0.35079(14) -0.3106(2) 0.0339(7) Uani 1 1 d . . . N28 N 0.1728(2) 0.33095(12) -0.29251(16) 0.0325(6) Uani 1 1 d . . . N29 N 0.1589(2) 0.31659(12) -0.20994(15) 0.0323(6) Uani 1 1 d . . . C117 C -0.1578(3) 0.49429(19) -0.2377(2) 0.0548(10) Uani 1 1 d . . . H11A H -0.1149 0.4923 -0.1858 0.082 Uiso 1 1 calc R . . H11B H -0.2276 0.4792 -0.2288 0.082 Uiso 1 1 calc R . . H11C H -0.1635 0.5340 -0.2560 0.082 Uiso 1 1 calc R . . C210 C 0.1462(2) 0.26341(14) -0.19689(19) 0.0319(7) Uani 1 1 d . . . C211 C 0.1261(2) 0.24709(14) -0.10964(19) 0.0310(7) Uani 1 1 d . . . N212 N 0.0640(2) 0.28144(12) -0.06706(16) 0.0342(6) Uani 1 1 d . . . C213 C 0.0508(3) 0.26848(16) 0.0123(2) 0.0405(8) Uani 1 1 d . . . H21A H 0.0064 0.2921 0.0429 0.049 Uiso 1 1 calc R . . C214 C 0.0978(3) 0.22303(16) 0.0521(2) 0.0436(8) Uani 1 1 d . . . H21B H 0.0874 0.2161 0.1091 0.052 Uiso 1 1 calc R . . C215 C 0.1602(3) 0.18752(16) 0.0085(2) 0.0438(8) Uani 1 1 d . . . H21C H 0.1939 0.1558 0.0346 0.053 Uiso 1 1 calc R . . C216 C 0.1726(3) 0.19917(15) -0.0749(2) 0.0394(8) Uani 1 1 d . . . H21D H 0.2126 0.1745 -0.1075 0.047 Uiso 1 1 calc R . . C217 C 0.3529(3) 0.35702(18) -0.2501(2) 0.0494(9) Uani 1 1 d . . . H21E H 0.3323 0.3463 -0.1945 0.074 Uiso 1 1 calc R . . H21F H 0.3767 0.3967 -0.2494 0.074 Uiso 1 1 calc R . . H21G H 0.4097 0.3322 -0.2666 0.074 Uiso 1 1 calc R . . C218 C 0.1535(3) 0.21820(16) -0.2610(2) 0.0469(9) Uani 1 1 d . . . H21H H 0.1668 0.2357 -0.3146 0.070 Uiso 1 1 calc R . . H21I H 0.0878 0.1969 -0.2656 0.070 Uiso 1 1 calc R . . H21J H 0.2109 0.1923 -0.2449 0.070 Uiso 1 1 calc R . . P1 P -0.5000 0.45546(7) 0.2500 0.0527(4) Uani 1 2 d S . . F11 F -0.3820(3) 0.4419(3) 0.2502(3) 0.155(2) Uani 1 1 d . A . F12 F -0.5092(5) 0.4038(3) 0.1833(4) 0.103(2) Uani 0.678(11) 1 d P A 1 F13 F -0.5059(8) 0.4968(3) 0.1803(6) 0.164(5) Uani 0.678(11) 1 d P A 1 F12B F -0.4866(10) 0.4545(12) 0.1590(8) 0.133(10) Uani 0.322(11) 1 d P A 2 F13B F -0.4139(9) 0.5062(6) 0.2619(10) 0.125(7) Uani 0.322(11) 1 d P A 2 P2 P 0.5000 0.16842(7) -0.2500 0.0527(4) Uani 1 2 d S . . F21 F 0.4038(2) 0.16855(17) -0.19332(19) 0.1011(11) Uani 1 1 d . . . F22 F 0.5504(3) 0.12088(17) -0.1930(2) 0.1192(13) Uani 1 1 d . . . F23 F 0.4442(3) 0.21432(17) -0.3081(2) 0.1258(15) 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 0.03054(14) 0.05236(17) 0.03201(15) -0.00923(12) -0.00010(10) -0.00005(12) N11 0.0424(16) 0.0584(19) 0.0286(15) 0.0016(13) 0.0008(12) 0.0028(14) C12 0.056(2) 0.068(3) 0.0275(18) 0.0032(17) -0.0016(16) -0.005(2) C13 0.060(2) 0.058(2) 0.036(2) 0.0143(18) -0.0138(18) -0.010(2) C14 0.053(2) 0.054(2) 0.058(3) 0.012(2) -0.021(2) 0.0040(19) C15 0.044(2) 0.049(2) 0.046(2) 0.0019(17) -0.0048(17) 0.0070(17) C16 0.0354(16) 0.0353(17) 0.0326(17) 0.0053(14) -0.0005(14) -0.0003(13) C17 0.0308(16) 0.0376(17) 0.0292(16) 0.0005(13) 0.0014(13) 0.0008(13) N18 0.0330(13) 0.0342(14) 0.0231(12) 0.0022(10) 0.0015(10) -0.0018(11) N21 0.0349(14) 0.0479(17) 0.0252(13) 0.0034(12) 0.0025(11) -0.0039(12) C22 0.053(2) 0.057(2) 0.0264(17) 0.0036(16) 0.0014(16) -0.0090(18) C23 0.072(3) 0.055(2) 0.0310(19) 0.0054(17) 0.0207(19) 0.004(2) C24 0.051(2) 0.091(3) 0.054(3) 0.025(2) 0.029(2) 0.017(2) C25 0.039(2) 0.093(3) 0.049(2) 0.024(2) 0.0161(18) 0.015(2) C26 0.0335(16) 0.0429(18) 0.0296(16) 0.0045(14) 0.0067(13) 0.0044(14) C27 0.0293(15) 0.0435(19) 0.0295(16) 0.0050(13) 0.0058(13) 0.0050(13) N28 0.0332(14) 0.0433(16) 0.0212(13) 0.0036(11) 0.0042(11) 0.0050(12) N29 0.0346(14) 0.0405(16) 0.0222(13) 0.0034(11) 0.0046(11) 0.0045(12) C117 0.046(2) 0.072(3) 0.046(2) -0.014(2) -0.0004(18) 0.023(2) C210 0.0263(15) 0.0419(19) 0.0275(16) 0.0009(14) 0.0017(12) -0.0004(13) C211 0.0281(15) 0.0389(17) 0.0261(15) 0.0019(13) 0.0011(12) -0.0033(13) N212 0.0304(13) 0.0485(16) 0.0240(13) 0.0051(12) 0.0038(11) 0.0070(12) C213 0.0398(18) 0.056(2) 0.0257(17) 0.0049(15) 0.0073(14) 0.0062(16) C214 0.052(2) 0.052(2) 0.0268(17) 0.0084(15) 0.0039(15) -0.0016(17) C215 0.051(2) 0.042(2) 0.0390(19) 0.0103(16) 0.0025(16) 0.0044(16) C216 0.0439(19) 0.0397(19) 0.0349(18) 0.0036(15) 0.0051(15) 0.0025(15) C217 0.0363(18) 0.073(3) 0.038(2) 0.0139(18) -0.0037(15) 0.0014(18) C218 0.063(2) 0.043(2) 0.0351(19) -0.0047(16) 0.0078(18) -0.0034(18) P1 0.0361(7) 0.0744(10) 0.0480(8) 0.000 0.0072(6) 0.000 F11 0.071(2) 0.261(7) 0.132(4) -0.009(4) 0.003(2) 0.021(3) F12 0.122(5) 0.111(5) 0.076(3) -0.035(3) 0.014(3) -0.012(4) F13 0.239(12) 0.109(5) 0.138(8) 0.084(5) -0.040(8) -0.019(7) F12B 0.080(7) 0.26(3) 0.059(7) -0.075(13) 0.027(6) -0.021(13) F13B 0.091(9) 0.135(11) 0.154(13) -0.040(9) 0.057(9) -0.074(8) P2 0.0665(10) 0.0650(10) 0.0270(7) 0.000 0.0050(7) 0.000 F21 0.082(2) 0.162(3) 0.0620(18) 0.0163(19) 0.0260(16) -0.020(2) F22 0.149(3) 0.136(3) 0.068(2) 0.025(2) -0.041(2) 0.028(3) F23 0.147(3) 0.132(3) 0.104(3) 0.066(2) 0.058(2) 0.070(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 N212 2.315(3) 6 y Ag1 N21 2.356(3) . y Ag1 N18 2.377(3) . y Ag1 N11 2.460(3) . y Ag1 N28 2.485(3) . y N11 C12 1.337(4) . ? N11 C16 1.340(4) . ? C12 C13 1.380(5) . ? C13 C14 1.360(6) . ? C14 C15 1.392(5) . ? C15 C16 1.385(5) . ? C16 C17 1.502(4) . ? C17 N18 1.275(4) . ? C17 C117 1.487(5) . ? N18 N18 1.385(5) 6 ? N21 C26 1.336(4) . ? N21 C22 1.337(4) . ? C22 C23 1.377(5) . ? C23 C24 1.353(6) . ? C24 C25 1.391(6) . ? C25 C26 1.376(5) . ? C26 C27 1.493(4) . ? C27 N28 1.272(4) . ? C27 C217 1.497(5) . ? N28 N29 1.395(3) . ? N29 C210 1.279(4) . ? C210 C218 1.489(5) . ? C210 C211 1.494(4) . ? C211 N212 1.346(4) . ? C211 C216 1.380(5) . ? N212 C213 1.336(4) . ? N212 Ag1 2.315(3) 6 ? C213 C214 1.370(5) . ? C214 C215 1.374(5) . ? C215 C216 1.390(5) . ? P1 F13 1.485(6) 6_456 ? P1 F13 1.485(6) . ? P1 F12B 1.488(12) . ? P1 F12B 1.488(12) 6_456 ? P1 F11 1.545(4) . ? P1 F11 1.545(4) 6_456 ? P1 F12 1.623(5) . ? P1 F12 1.623(5) 6_456 ? P1 F13B 1.629(9) 6_456 ? P1 F13B 1.629(9) . ? F11 F13B 1.579(15) . ? P2 F22 1.566(3) 6_655 ? P2 F22 1.566(3) . ? P2 F21 1.571(3) . ? P2 F21 1.571(3) 6_655 ? P2 F23 1.577(3) 6_655 ? P2 F23 1.577(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 N212 Ag1 N21 111.74(9) 6 . y N212 Ag1 N18 130.74(9) 6 . y N21 Ag1 N18 117.52(9) . . y N212 Ag1 N11 96.54(10) 6 . y N21 Ag1 N11 110.48(10) . . y N18 Ag1 N11 67.13(9) . . y N212 Ag1 N28 107.59(9) 6 . y N21 Ag1 N28 67.54(9) . . y N18 Ag1 N28 91.01(9) . . y N11 Ag1 N28 154.80(10) . . y C12 N11 C16 117.9(3) . . ? C12 N11 Ag1 124.3(3) . . ? C16 N11 Ag1 112.1(2) . . ? N11 C12 C13 123.5(4) . . ? C14 C13 C12 118.4(4) . . ? C13 C14 C15 119.4(4) . . ? C16 C15 C14 118.8(4) . . ? N11 C16 C15 122.0(3) . . ? N11 C16 C17 116.9(3) . . ? C15 C16 C17 121.2(3) . . ? N18 C17 C117 123.6(3) . . ? N18 C17 C16 116.1(3) . . ? C117 C17 C16 120.2(3) . . ? C17 N18 N18 117.3(3) . 6 ? C17 N18 Ag1 119.1(2) . . ? N18 N18 Ag1 120.31(15) 6 . ? C26 N21 C22 117.8(3) . . ? C26 N21 Ag1 118.6(2) . . ? C22 N21 Ag1 123.4(2) . . ? N21 C22 C23 123.3(4) . . ? C24 C23 C22 119.0(4) . . ? C23 C24 C25 118.4(4) . . ? C26 C25 C24 119.6(4) . . ? N21 C26 C25 121.7(3) . . ? N21 C26 C27 117.0(3) . . ? C25 C26 C27 121.2(3) . . ? N28 C27 C26 116.2(3) . . ? N28 C27 C217 124.3(3) . . ? C26 C27 C217 119.3(3) . . ? C27 N28 N29 117.8(3) . . ? C27 N28 Ag1 114.5(2) . . ? N29 N28 Ag1 121.58(18) . . ? C210 N29 N28 114.7(3) . . ? N29 C210 C218 124.7(3) . . ? N29 C210 C211 115.8(3) . . ? C218 C210 C211 119.4(3) . . ? N212 C211 C216 122.4(3) . . ? N212 C211 C210 117.5(3) . . ? C216 C211 C210 120.1(3) . . ? C213 N212 C211 117.4(3) . . ? C213 N212 Ag1 114.5(2) . 6 ? C211 N212 Ag1 128.2(2) . 6 ? N212 C213 C214 123.6(3) . . ? C213 C214 C215 119.1(3) . . ? C214 C215 C216 118.3(3) . . ? C211 C216 C215 119.1(3) . . ? F13 P1 F13 98.3(8) 6_456 . ? F13 P1 F12B 138.9(13) 6_456 . ? F13 P1 F12B 42.7(9) . . ? F13 P1 F12B 42.7(9) 6_456 6_456 ? F13 P1 F12B 138.9(13) . 6_456 ? F12B P1 F12B 178(2) . 6_456 ? F13 P1 F11 96.9(4) 6_456 . ? F13 P1 F11 98.5(5) . . ? F12B P1 F11 80.6(6) . . ? F12B P1 F11 99.0(5) 6_456 . ? F13 P1 F11 98.5(5) 6_456 6_456 ? F13 P1 F11 96.9(4) . 6_456 ? F12B P1 F11 99.0(5) . 6_456 ? F12B P1 F11 80.6(6) 6_456 6_456 ? F11 P1 F11 156.3(5) . 6_456 ? F13 P1 F12 172.2(6) 6_456 . ? F13 P1 F12 89.3(4) . . ? F12B P1 F12 48.9(9) . . ? F12B P1 F12 129.5(13) 6_456 . ? F11 P1 F12 83.5(3) . . ? F11 P1 F12 78.8(3) 6_456 . ? F13 P1 F12 89.3(4) 6_456 6_456 ? F13 P1 F12 172.2(6) . 6_456 ? F12B P1 F12 129.5(13) . 6_456 ? F12B P1 F12 48.9(9) 6_456 6_456 ? F11 P1 F12 78.8(3) . 6_456 ? F11 P1 F12 83.5(3) 6_456 6_456 ? F12 P1 F12 83.1(5) . 6_456 ? F13 P1 F13B 67.6(6) 6_456 6_456 ? F13 P1 F13B 54.8(5) . 6_456 ? F12B P1 F13B 90.3(9) . 6_456 ? F12B P1 F13B 90.9(10) 6_456 6_456 ? F11 P1 F13B 143.8(7) . 6_456 ? F11 P1 F13B 59.6(5) 6_456 6_456 ? F12 P1 F13B 116.3(6) . 6_456 ? F12 P1 F13B 130.7(6) 6_456 6_456 ? F13 P1 F13B 54.8(5) 6_456 . ? F13 P1 F13B 67.6(6) . . ? F12B P1 F13B 90.9(10) . . ? F12B P1 F13B 90.3(9) 6_456 . ? F11 P1 F13B 59.6(5) . . ? F11 P1 F13B 143.8(7) 6_456 . ? F12 P1 F13B 130.7(6) . . ? F12 P1 F13B 116.3(6) 6_456 . ? F13B P1 F13B 85.9(11) 6_456 . ? P1 F11 F13B 62.8(4) . . ? F11 F13B P1 57.6(4) . . ? F22 P2 F22 88.9(3) 6_655 . ? F22 P2 F21 91.8(2) 6_655 . ? F22 P2 F21 88.4(2) . . ? F22 P2 F21 88.4(2) 6_655 6_655 ? F22 P2 F21 91.8(2) . 6_655 ? F21 P2 F21 179.8(3) . 6_655 ? F22 P2 F23 177.1(2) 6_655 6_655 ? F22 P2 F23 88.7(2) . 6_655 ? F21 P2 F23 89.91(18) . 6_655 ? F21 P2 F23 89.94(18) 6_655 6_655 ? F22 P2 F23 88.7(2) 6_655 . ? F22 P2 F23 177.1(2) . . ? F21 P2 F23 89.94(18) . . ? F21 P2 F23 89.91(18) 6_655 . ? F23 P2 F23 93.7(4) 6_655 . ? _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 28.65 _diffrn_measured_fraction_theta_full 0.911 _refine_diff_density_max 0.792 _refine_diff_density_min -0.728 _refine_diff_density_rms 0.079 data_latrif _database_code_CSD 173890 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H10 Ag F3 N4 O3 S' _chemical_formula_weight 467.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.9563(5) _cell_length_b 19.8349(10) _cell_length_c 9.3583(5) _cell_angle_alpha 90.00 _cell_angle_beta 107.4800(10) _cell_angle_gamma 90.00 _cell_volume 1585.71(15) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 7170 _cell_measurement_theta_min 3 _cell_measurement_theta_max 20 _exptl_crystal_description blocks _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.957 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 1.458 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cooler (Cosier & Glazer, 1986). The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.0 cm. Coverage of the unique set is over 97% complete to at least 26\% in \q. Crystal decay was found to be negligible by by repeating the initial frames at t data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for met atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 180(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 'Siemens SMART diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 9277 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 28.48 _reflns_number_total 3697 _reflns_number_gt 3032 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL PC (Siemens, 1994)' _computing_publication_material 'SHELXTL PC (Siemens, 1994)' _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^)+(0.0270P)^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 0.0008(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3697 _refine_ls_number_parameters 227 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0311 _refine_ls_R_factor_gt 0.0223 _refine_ls_wR_factor_ref 0.0529 _refine_ls_wR_factor_gt 0.0506 _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_restrained_S_all 0.944 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.240873(17) 0.438673(7) -0.000205(16) 0.02767(6) Uani 1 1 d . . . N1 N 0.38446(18) 0.50659(8) 0.17764(18) 0.0243(3) Uani 1 1 d . . . C2 C 0.5392(2) 0.49484(10) 0.2282(2) 0.0299(5) Uani 1 1 d . . . H2A H 0.5814 0.4610 0.1798 0.036 Uiso 1 1 calc R . . C3 C 0.6404(2) 0.52919(11) 0.3466(3) 0.0374(5) Uani 1 1 d . . . H3A H 0.7489 0.5187 0.3793 0.045 Uiso 1 1 calc R . . C4 C 0.5802(3) 0.57928(12) 0.4164(3) 0.0383(5) Uani 1 1 d . . . H4A H 0.6466 0.6037 0.4984 0.046 Uiso 1 1 calc R . . C5 C 0.4214(2) 0.59318(11) 0.3646(2) 0.0316(5) Uani 1 1 d . . . H5A H 0.3778 0.6278 0.4099 0.038 Uiso 1 1 calc R . . C6 C 0.3261(2) 0.55596(9) 0.2454(2) 0.0228(4) Uani 1 1 d . . . C7 C 0.1568(2) 0.56882(9) 0.1871(2) 0.0219(4) Uani 1 1 d . . . H7A H 0.0896 0.5370 0.1231 0.026 Uiso 1 1 calc R . . N8 N 0.10150(18) 0.62300(8) 0.22358(18) 0.0254(4) Uani 1 1 d . . . N9 N -0.06285(18) 0.62836(8) 0.16224(17) 0.0229(3) Uani 1 1 d . . . C10 C -0.1138(2) 0.68388(10) 0.2014(2) 0.0234(4) Uani 1 1 d . . . H10A H -0.0409 0.7155 0.2593 0.028 Uiso 1 1 calc R . . C11 C -0.2813(2) 0.69967(9) 0.1591(2) 0.0231(4) Uani 1 1 d . . . N12 N -0.38288(18) 0.65577(8) 0.06905(18) 0.0255(4) Uani 1 1 d . . . C13 C -0.5351(2) 0.66943(10) 0.0364(2) 0.0303(5) Uani 1 1 d . . . H13A H -0.6073 0.6389 -0.0262 0.036 Uiso 1 1 calc R . . C14 C -0.5943(2) 0.72611(11) 0.0891(2) 0.0345(5) Uani 1 1 d . . . H14A H -0.7039 0.7338 0.0633 0.041 Uiso 1 1 calc R . . C15 C -0.4896(2) 0.77078(11) 0.1798(3) 0.0362(5) Uani 1 1 d . . . H15A H -0.5260 0.8101 0.2168 0.043 Uiso 1 1 calc R . . C16 C -0.3308(2) 0.75742(10) 0.2162(2) 0.0297(4) Uani 1 1 d . . . H16A H -0.2567 0.7873 0.2791 0.036 Uiso 1 1 calc R . . S1 S 0.96787(6) 0.38741(2) 0.21128(6) 0.02575(11) Uani 1 1 d . . . O1 O 0.93094(19) 0.32320(8) 0.13738(16) 0.0403(4) Uani 1 1 d . . . O2 O 0.85158(18) 0.43923(7) 0.15621(17) 0.0375(4) Uani 1 1 d . . . O3 O 1.12799(17) 0.40883(8) 0.23953(17) 0.0398(4) Uani 1 1 d . . . C01 C 0.9546(2) 0.37084(11) 0.3981(2) 0.0327(5) Uani 1 1 d . . . F1 F 1.05327(19) 0.32208(7) 0.46532(15) 0.0569(4) Uani 1 1 d . . . F2 F 0.81055(18) 0.35257(8) 0.39404(17) 0.0583(4) Uani 1 1 d . . . F3 F 0.99014(17) 0.42546(7) 0.48581(15) 0.0466(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02425(9) 0.02597(9) 0.03083(10) -0.00917(6) 0.00533(6) -0.00191(6) N1 0.0193(8) 0.0239(8) 0.0286(9) -0.0019(7) 0.0054(7) 0.0009(6) C2 0.0200(10) 0.0297(11) 0.0384(12) -0.0033(9) 0.0062(9) 0.0022(8) C3 0.0186(11) 0.0402(13) 0.0471(14) -0.0030(10) 0.0002(9) 0.0015(9) C4 0.0262(12) 0.0446(13) 0.0355(13) -0.0097(10) -0.0040(9) -0.0039(9) C5 0.0257(11) 0.0350(12) 0.0310(12) -0.0097(9) 0.0037(9) -0.0009(9) C6 0.0203(9) 0.0234(10) 0.0238(10) -0.0004(8) 0.0052(7) 0.0006(7) C7 0.0190(9) 0.0249(10) 0.0206(9) -0.0027(7) 0.0042(7) -0.0016(7) N8 0.0177(8) 0.0280(9) 0.0281(9) -0.0038(7) 0.0032(7) 0.0007(6) N9 0.0165(8) 0.0271(9) 0.0238(8) -0.0015(7) 0.0041(6) 0.0004(6) C10 0.0231(10) 0.0241(10) 0.0216(10) -0.0011(8) 0.0044(8) -0.0001(8) C11 0.0240(10) 0.0217(9) 0.0234(10) 0.0012(7) 0.0066(8) 0.0010(7) N12 0.0216(8) 0.0253(9) 0.0277(9) -0.0038(7) 0.0046(7) 0.0005(6) C13 0.0234(11) 0.0310(11) 0.0343(12) -0.0046(9) 0.0056(9) -0.0008(8) C14 0.0229(11) 0.0373(12) 0.0412(13) -0.0040(10) 0.0068(9) 0.0065(9) C15 0.0305(12) 0.0329(12) 0.0436(14) -0.0095(10) 0.0085(10) 0.0078(9) C16 0.0274(11) 0.0244(10) 0.0343(12) -0.0070(8) 0.0047(9) 0.0012(8) S1 0.0224(2) 0.0284(3) 0.0253(3) 0.0052(2) 0.00542(19) 0.00211(19) O1 0.0480(10) 0.0337(9) 0.0324(9) -0.0041(7) 0.0019(7) 0.0024(7) O2 0.0337(9) 0.0371(9) 0.0396(9) 0.0105(7) 0.0078(7) 0.0108(7) O3 0.0250(8) 0.0518(10) 0.0447(10) 0.0080(8) 0.0137(7) -0.0032(7) C01 0.0303(12) 0.0359(12) 0.0317(12) 0.0009(9) 0.0089(9) -0.0058(9) F1 0.0801(11) 0.0523(9) 0.0346(8) 0.0193(7) 0.0119(7) 0.0204(8) F2 0.0473(9) 0.0793(11) 0.0556(9) -0.0030(8) 0.0264(7) -0.0303(8) F3 0.0519(9) 0.0509(9) 0.0364(8) -0.0133(6) 0.0122(6) -0.0111(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 2.2255(16) . Y Ag1 N9 2.2710(15) 3_565 Y Ag1 N12 2.4564(16) 3_565 Y N1 C2 1.343(2) . ? N1 C6 1.354(2) . ? C2 C3 1.382(3) . ? C3 C4 1.384(3) . ? C4 C5 1.385(3) . ? C5 C6 1.395(3) . ? C6 C7 1.472(3) . ? C7 N8 1.272(2) . ? N8 N9 1.414(2) . ? N9 C10 1.287(2) . ? N9 Ag1 2.2710(15) 3_565 ? C10 C11 1.466(3) . ? C11 N12 1.355(2) . ? C11 C16 1.391(3) . ? N12 C13 1.332(2) . ? N12 Ag1 2.4565(16) 3_565 ? C13 C14 1.395(3) . ? C14 C15 1.381(3) . ? C15 C16 1.386(3) . ? S1 O1 1.4397(15) . ? S1 O3 1.4419(15) . ? S1 O2 1.4437(15) . ? S1 C01 1.818(2) . ? C01 F2 1.329(2) . ? C01 F1 1.334(3) . ? C01 F3 1.338(2) . ? 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 N9 170.36(6) . 3_565 Y N1 Ag1 N12 115.43(5) . 3_565 Y N9 Ag1 N12 72.14(5) 3_565 3_565 Y C2 N1 C6 117.57(17) . . ? C2 N1 Ag1 117.49(13) . . ? C6 N1 Ag1 124.79(12) . . ? N1 C2 C3 123.76(19) . . ? C4 C3 C2 118.5(2) . . ? C3 C4 C5 118.8(2) . . ? C4 C5 C6 119.44(19) . . ? N1 C6 C5 121.87(18) . . ? N1 C6 C7 116.84(16) . . ? C5 C6 C7 121.29(17) . . ? N8 C7 C6 119.22(17) . . ? C7 N8 N9 113.35(15) . . ? C10 N9 N8 111.34(15) . . ? C10 N9 Ag1 116.94(12) . 3_565 ? N8 N9 Ag1 131.56(11) . 3_565 ? N9 C10 C11 121.87(17) . . ? N12 C11 C16 122.45(18) . . ? N12 C11 C10 118.16(17) . . ? C16 C11 C10 119.35(17) . . ? C13 N12 C11 117.47(17) . . ? C13 N12 Ag1 132.05(13) . 3_565 ? C11 N12 Ag1 110.46(12) . 3_565 ? N12 C13 C14 123.68(19) . . ? C15 C14 C13 118.32(19) . . ? C14 C15 C16 119.08(19) . . ? C15 C16 C11 119.01(19) . . ? O1 S1 O3 114.90(10) . . ? O1 S1 O2 114.92(9) . . ? O3 S1 O2 115.27(10) . . ? O1 S1 C01 103.30(10) . . ? O3 S1 C01 103.05(9) . . ? O2 S1 C01 102.91(10) . . ? F2 C01 F1 108.43(18) . . ? F2 C01 F3 106.78(18) . . ? F1 C01 F3 107.22(18) . . ? F2 C01 S1 111.41(15) . . ? F1 C01 S1 111.03(15) . . ? F3 C01 S1 111.77(15) . . ? _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 28.48 _diffrn_measured_fraction_theta_full 0.920 _refine_diff_density_max 0.452 _refine_diff_density_min -0.324 _refine_diff_density_rms 0.063